Hurst, Bernadette J. Puleo€¦ · G57, 40.00 mg CMAS SiO Wellman -Aygun Smialek Braue 0 49 mole%;...
Transcript of Hurst, Bernadette J. Puleo€¦ · G57, 40.00 mg CMAS SiO Wellman -Aygun Smialek Braue 0 49 mole%;...
![Page 1: Hurst, Bernadette J. Puleo€¦ · G57, 40.00 mg CMAS SiO Wellman -Aygun Smialek Braue 0 49 mole%; such as NASA’s CMAS (with NiO DSC:020 OES Measured by EDS [#] Type Date/time :](https://reader033.fdocuments.us/reader033/viewer/2022060211/5f04cb127e708231d40fbc15/html5/thumbnails/1.jpg)
National Aeronautics and Space Adm
inistration
Calcium
-Magnesium
-Alum
ino-Silicates (CM
AS) R
eaction M
echanisms and R
esistance of Advanced Turbine Environm
ental B
arrier Coatings for SiC
SiC C
eramic M
atrix Com
posites
Dongm
ing Zhu Gustavo C
osta Bryan J H
arder Valerie L Wiesner Janet B
H
urst Bernadette J P
uleo
Materials and S
tructures Division
NA
SA
John H G
lenn Research C
enter C
leveland Ohio 44135
Advanced Ceram
ic Matrix C
omposites
Science and Technology of Materials D
esign Applications Performance and Integration
An EC
I Conference Santa Fe N
M
Novem
ber 8 2017
ww
wnasagov
1
Temperature
Capability
National Aeronautics and Space Adm
inistration
NA
SA Environm
ental Barrier Coatings (E
BCs) and C
eramic
Matrix C
omposite (C
MC
) System
Developm
entminus
Emphasize m
aterial temperature capability perform
ance and long-term
durability-Highly loaded E
BC
-CM
Cs w
ith temperature capability of 2700degF
(1482degC)
bull 2700-3000degF (1482-1650degC) turbine and C
MC
combustor coatings
bull 2700degF (1482degC) E
BC
bond coat technology for supporting next generation ndashR
ecession lt5 mgcm
2 per 1000 h ndashC
oating and component strength requirem
ents 15-30 ksi or 100-207 Mpa
ndashResistance to C
alcium M
agnesium A
lumino-S
ilicate (CM
AS
) Step increase in the m
aterialrsquos temperature capability
Temperature
3000degF SiC
SiC
CM
C airfoil
Capability (TE(TEBBC)C) ssuurfarfaccee
and combustor
3000degF+ (1650degC+)
technologies 2700degF S
iCS
iC thin turbine
2700degF (1482qC)
2700degF (1482degC) G
en III SiCSiC
CM
Cs
EB
C system
s for CM
C
airfoils
2400degF (1316degC) G
en I and Gen II SiC
SiC
CM
Cs
2000degF (1093degC) PtAl and N
iAl bond coats
Gen II ndash
Currentcomm
ercialG
en IIIG
en IV
Increase in T across TEBC
Single Crystal Superalloy
Ceramic M
atrix Composite
Gen II ndash Current com
mercial
Gen III
Gen IV
Increase in T across TEBC
Single Crystal Superalloy
Ceramic M
atrix Composite
2800ordmF com
bustor TB
C
2500ordmF Turbine TB
C
GGenen II
YYearear
ww
wnasagov
2
National Aeronautics and Space Adm
inistration
Outline
bullN
ASA environm
ental barrier coating (EBC
) development the C
MAS
relevance and importance
minus E
BC
systems
minus C
MA
S com
positions
bullSom
e generalized CM
AS related failures
bullC
MAS degradation of environm
ental barrier coating (EBC
) systems rare
earth silicates ndash
Ytterbium
silicate and yttrium silicate E
BC
s ndash
Som
e reactions kinetics and mechanism
s
bullC
urrent advanced EBC
s HfO
2 -and Rare Earth -Silicon based 2700degF+
capable bond coats ndash
Som
e CM
AS
durability tests and results
bull Sum
mary
ww
wnasagov
3
National Aeronautics and Space Adm
inistration
EBC-C
MA
S D
egradation is of Concern w
ith Increasing O
perating Temperatures
minusEm
phasize improving tem
perature capability performance and long-term
durability of ceram
ic turbine airfoils bull
Increased gas inlet temperatures for net generation engines lead to significant C
MA
S -
related coating durability issues ndash CM
AS
infiltration and reactions
Marcus P B
orom et al S
urf Coat
Technol 86-87 1996
Current airfoil C
MA
S attack
region -R D
arolia International M
aterials Review
s 2013
ww
wnasagov
4
National Aeronautics and Space Adm
inistration
Calcium
Magnesium
Alumino-Silicate (C
MAS) System
s Used
in Laboratory Tests minus
N
AS
A m
odified version (NA
SA
CM
AS
) and the Air Force -P
owder Technology Incorporated
PTI 02 C
MA
S currently being used for advanced coating developm
ents minus
C
MA
S S
iO2 content typically ranging from
43-49 mole
such as NASArsquos CMAS (with N
iO
and FeO)
NA
SA m
odified CM
AS
AR
FL PTI CM
AS 02
(higher SiO2 )
GEB
orom
Wellm
an
Kram
er
Aygun Smialek
Rai
Braue
AR
FL PTI 11717A
02
Fully reacted A
s received
AFR
L02 particle size
distribution (34
Quartz 30
Gypsum
17
Aplite 14
Dolom
ite 5
Salt) Percentile Size (μm
) 10 25 +-10 50 85 +-20 90 405 +-30
Fully reacted C
MA
S EDS
ww
wnasagov
5
National Aeronautics and Space Adm
inistration
Calcium
Magnesium
Alumino-Silicate (C
MAS) System
s Used
in Laboratory Tests -Continued
minus
NA
SA
modified version (N
AS
A C
MA
S)
minus
CM
AS
SiO
2 content typically ranging from 43-49 m
ole such as N
ASArsquos CMAS (with N
iO
and FeO)
NA
SA
CM
AS
Com
positions
NA
SA m
odified CM
AS
AR
FL PTI CM
AS 02
(higher SiO2 )
GEB
orom
Wellm
an
Kram
er
Aygun Smialek
Rai
Braue
Method
Content (m
ol)
CaO
M
gO
Al2 O3
SiO2
Fe2 O
3 N
iO
(DesignedTargeted)
338 90
67 460
30 15
Measured by IC
P-O
ES 38 r 2
90 r 05 69 r 03
41 r 2 38 r 02
137 r 007
Measured by ED
S 36 r 1
84 r 03 75 r 02
43 r 1 39 r 01
15 r 01
Created w
ith NE
TZSC
H P
roteus software
[] Type [11] D
ynamic
Range
2550(Km
in)1500 A
cqRate
7500 S
TC
0 P
1N2O
2 500
Corr
DS
C020
[] Type [13] D
ynamic
Range
150050(Km
in)25 A
cqRate
7500 S
TC
0 P
1N2O
2 500
Corr
DS
C020
Project
Identity D
atetime
Laboratory O
perator S
ample
G57
6282016 91511 AM
G
lenn Research C
enter C
osta G
57 4000 mg
Reference
Material
Corrtem
pcal S
ensfile S
ample carTC
M
odetype of meas R
ef Al2O
30 mg
baseline for YS
Z 5 C_m
in up tp 1500 C 06-24-16bd8 TC
ALZE
RO
TMX
sensitivity from
sapphire_Pt crucible 1500C
air 01-06-16ed8 D
SC
Cp S
S
DS
C sam
ple with correction
Segm
ents C
rucible A
tmosphere
M range
3 DS
CTG
pan Pt
N2O
2 500mlm
in 5000 microV
Instrument N
ETZS
CH
DS
C 404F1 File C
NE
TZSC
HP
roteusdata5CostaS
amplesG
62dd8 Rem
ark Third DS
C run since O
ct 2014 1x evacbackfill
200 400
600 800
1000 1200
1400 Tem
perature degC
-10
-08
-06
-04
-02
00
02
04
DS
C (m
Wm
g)
0 50
100
150
200
250
Flow (m
lmin)
Main
exo
DSC
traces of CM
AS during heating and cooling up
to 1500 qC at 5 qC
min
ww
wnasagov
6
National Aeronautics and Space Adm
inistration
Advanced N
AS
A E
BC
Developm
ents
Improved tem
perature capability sintering phase stability recession resistance and high tem
perature strength
Advanced com
positions amp processing for com
bined therm
omechanical loading and environm
ents higher stability and increased toughness tow
ards prime-reliant
Gen I (E
PM)
RampD
Award
Gen II (U
EET)
2000-2004 Advanced EBC
(U
EET) 2000-2005 R
ampD Aw
ard (2007)
Advanced EBC (FAP)
2005-2011 R
ampD Aw
ard (2007) coating turbine developm
ent
Advanced EBC
(FAP -ERA)
2007 -present
Advanced (FAP ERA)
Patent13923450 PC
TUS1346946 and subsequent patents
Engine C
omponents
Com
bustor C
ombustor
(Vane) C
ombustor
Vane Vane Blade
-VaneBlade EB
Cs
-Equivalent APS com
bustor EBC
s
Airfoil components
Top Coat
BSAS (APS) R
E2 Si2 O
7 or R
E2 SiO
5 (APS)
-(HfY
bGdY
) 2 O3
-ZrO2 H
fO2 +R
E
silicates -ZrO
2 HfO
2 +BS
AS
(APS and EBPVD
)
RE-H
fO2 -Alum
ino silicate
(APS andor 100
EB-
PVD)
RE-H
fO2 -X
advanced top coat R
E-HfO
2 Silica (EB
-PVD etc vapor
deposition)
Advanced EBC
s
Interlayer --
--R
E-HfO
2 ZrO2 -
aluminosilicate
layered systems
Nanocom
posite graded oxidesilicate
--
EBC
M
ullite+ BSAS R
E2 Si2 O
7 and or BSAS+M
ullite
RE
silicates or R
E-Hf m
ullite R
E doped m
ullite-HfO
2 or R
E silicates
Multi-com
ponent R
E silicate systems
Multicom
ponent R
E-silicate + Hf self
grown
Bond C
oat Si
Si O
xide+Si bond coat
HfO
2 -Si-X
doped mulliteSi
SiC nanotube
Optim
ized HfO
2 -Si-X bond coat 2700degF bond coats
RE-Si+H
f systems
Thickness 10-15 m
il 10-15 m
il 15-20 m
il 10 m
il 5 m
il 1 -3 m
ils
Surface T U
p to 2400degF 2400degF
3000degF2400CM
C
2700degF2400F CM
C
2700-3000degF
Bond Coat T
Limited to
2462degF Lim
it to 2462degF
Limit to 2642degF
Proven at 2600degF + Advancem
ents targeting 2700degF
2700degF
Challenges overcom
e by advancem
ents
ww
wnasagov
7
National Aeronautics and Space Adm
inistration
CM
AS
Related D
egradations in EBC
s
Cross-section
50 mm
minus C
MAS effects
bull S
ignificantly reduce melting points of the E
BC
s and bond coats bull
More detrim
ental effects with thin airfoil E
BC
s bull
CM
AS
weakens the coating system
s reducing strength and toughness bullM
AS
increase EB
C diffusivities and perm
eability thus less protective as an environmental
barrier bullC
MA
S interactions w
ith heat flux thermal cycling erosion and therm
omechanical fatigue
Reaction layer spallations
Accelerated C
MC
failure when C
MA
S intact w
ith CM
Cs
Such as yttrium silicate
Coating
surface
EB
C and degradations
CM
AS induced m
elting and failure$w
ww
nasagov 8
National Aeronautics and Space Adm
inistration
CM
AS R
elated Degradations in E
BCs -C
ontinued minus
CM
AS effects on EBC
temperature capability
bull S
ilicate reactions with N
aO2 and A
l2 O3 silicate
Phase diagram
s showing yttrium
di-silicate reactions w
ith SiO
2 NaO
and Al2 O
3
ww
wnasagov
9
National Aeronautics and Space Adm
inistration
CM
AS R
elated Degradations in E
BCs -C
ontinued minus
CM
AS effects on EBC
temperature capability
bullRare earths generally have lim
ited temperature capability below
1500degC in the R
E2 O
3 -A
l2 O3 -S
iO2 based system
s bull
Sm
aller ionic size RE
s have higher melting points
Solidus temperature in Ln
2 Si2 O7 -A
l6 Si2 O13 -
SiO2 system
as function of ionic radius
Y Murakam
i and H Yam
amoto J C
eram Soc Jpn 101 [10] 1101-1106 (1993)
ww
wnasagov
10
National Aeronautics and Space Adm
inistration
Rare Earth D
issolutions in CM
AS Melts
ZrO2 -30Y
2 O3 -15Sm
2 O3 -15Yb
2 O3
ZrO2 -30Y
2 O3 -15N
d2 O
3 -15Yb2 O
3 -03Sc2 O
3
ZrO2 -96Y
2 O3 -22G
d2 O
3 -21Yb2 O
3
Ionic potential trend of RE
Radius size trend of RE
minus Large ionic size rare earths show
ed higher concentration dissolutions in the CM
AS
m
elt for ZrO2 -R
E2 O
3 oxide systems
ZrO2 -R
EO15 -H
f more endotherm
ic
Gustavo and Zhu International C
onference on Advanced C
eramics and C
omposites 2016
ww
wnasagov
11
Front CM
AS side
National Aeronautics and Space Adm
inistration
CM
AS Related D
egradations in EBC
coated CM
Cs ndash
Laboratory Heat Flux Tests
minusC
MAS effects on EB
C-C
MC
temperature capability tested in laser high heat
flux creep-rupture rig bull
Accelerated failure of C
MC
in loading high heat flux conditions
EBC
coated CV
I-MI C
MC
with N
dYb silicate R
ESi bond coat tested Tsurface 2600degF TC
MC
2450degF
Front heated CM
AS
side B
ack cooled side
Creep strain
Time h
Front CM
AS
side
200h
05
ww
wnasagov
12
National Aeronautics and Space Adm
inistration
EBC
CM
AS
Surface Initial N
ucleation Dissolution R
eactions ndash
Ytterbium
-and yttrium-silicate silicates reactions and dissolutions in C
AM
S
ndash M
ore sluggish dissolution of ytterbium as com
pared to yttrium
Ytterbium
di-silicate surface CM
AS m
elts 50 Y
tterbium di-silicate surface C
MA
S melts 5 h
h 1300degC
1500degC$
Yttrium
mono-silicate surface C
MA
S Y
ttrium silicate surface C
MA
S melts 5 h
melts 50 h 1300degC
1500degC
A
hlborg and Zhu Surface amp C
oatings Technology 237 (2013) 79ndash87 w
ww
nasagov 13
National Aeronautics and Space Adm
inistration
Rare E
arth Apatite G
rain Grow
th ndash
Grain grow
th of apatite phase at 1500degC at various tim
es
Ytterbium
silicate system
50 hr 150 hr
200 hr
200 hr50 hr
150 hr
Yttrium
silicate system$
ww
wnasagov
14
National Aeronautics and Space Adm
inistration
Effect of C
MA
S R
eactions on Grain B
oundary Phases
ndash C
MA
S and grain boundary phase has higher A
l2 O3
content (17-22 mole
) bull
Eutectic region w
ith high Al2 O
3 content ~1200degC m
elting point bull
Loss of SiO
2 due to volatility
200 hr 1500degC
NA
SA
modified
CM
AS
Grain
boundary final phase ndash low
SiO
2 and high A
lumina
ww
wnasagov
15
National Aeronautics and Space Adm
inistration
Rare E
arth Dissolution in C
MA
S M
elts ndash
Non stoichiom
etric characteristics of the CM
AS
ndash rare earth silicate reacted apatite phases ndash up to 200 h testing
ndash D
ifference in partitioning of ytterbium vs yttrium
in apatite bull
Average AE
OR
E2 O
3 ratio ~ 068 for ytterbium silicate ndash C
MA
S system
bull
Average AE
OR
E2 O
3 ratio ~ 022 for yttrium silicate ndash C
MA
S system
C
omposition in apatite (100 hr)
SiO2
Ahlborg and Zhu Surface amp
Coatings Technology 237 (2013) 79ndash87
RE
2 O3
AEO
Yttrium
Silicate EBC
Com
position in apatite (100 hr)
Ytterbium
Silicate EBC
ww
wnasagov
16
National Aeronautics and Space Adm
inistration
Advanced N
AS
A E
BC
Developm
ents
NA
SA advanced E
BC
systems em
phasizing high stability HfO
2 -and ZrO2 -R
E2 O
3 -
EBC layer 2 region
EB
Cs
Mol
Mol
SiO
2 EB
C system
RE
2 Si2-x O
7-2x such as (YbG
dY) 2 S
i2-x O7-2x
-Controlled dissolution and m
aintaining coating stability
(YbGdY) 2 S
i2-x O7-2x in
CM
AS
1300degC
(a)
(b)
ww
wnasagov
17
National Aeronautics and Space Adm
inistration E
xample of N
AS
A A
dvanced Environm
ental Barrier C
oating on S
iCSiC
CM
C System
s
Advanced EB
C coated vanes
HfO
2 -(YbG
dY)2 O
3
(YbG
dY)2 Si2-x O
7-2x
RESi(O
)+Hf B
ond Coat
Gd Y
b Y
O
Si
Yb
Gd Y
Si
Hf
A
lternating layered HfO
2 -Multicom
ponent Rare E
arth silicate EB
Cs used for fundam
ental stability studies
2700degF capable YbG
d-YbO+H
f based bond coats C
oated onto SiC
SiC
CM
C substrates using E
B-P
VD
The bond coat region
ww
wnasagov
18
National Aeronautics and Space Adm
inistration
CM
AS
Resistant Tests
ndash JE
Ts test of more advanced coating system
s at 2700F
Plasma sprayed (G
dY)2 Si2 O
7 2450 cycles
Special processed Yb
2 Si2 O7 spalling at 450 C
ycles EB
-PVD
(YbG
dY)2 Si2 O
7 total 4450 JETS cycles 100h
2450 4450
450
Hybrid H
f-rare earth aluminate silicate com
pleted 4450 cycles 100h
Hybrid H
ybrid Zr-rare earth silicate completed 4450
cycles 100h
2450 4450
2450 with
CM
AS 2450
ww
wnasagov
19
National Aeronautics and Space Adm
inistration
High S
tability and CM
AS
Resistance are E
nsured by Advanced H
igh M
elting Point C
oating and Multi-C
omponent C
ompositions A
rea A
Area B
ndash G
enerally improved C
MA
S
resistance of NAS
A R
ESi
System
at 1500degC 100 hr
ndash S
ilica-rich phase precipitation ndash
Rare earth elem
ent leaching into the m
elts (low concentration
~9mol
)
Surface side of the C
MA
S melts
EDS E
ww
wnasagov
20
National Aeronautics and Space Adm
inistration
Advanced E
BC
-CM
C S
ystem D
emonstrated 300 hr H
igh Cycle and
Low Fatigue D
urability in High H
eat Flux 2700degF Test Conditions
Specimen after 300 h testing
-A turbine airfoil E
BC
with H
fO2 -rare earth silicate and G
dYbSi bond coat on C
VI-M
I CM
C
substrate system selected for heat flux durability testing
-Laser high heat flux rig H
igh Cycle and Low
Cycle Fatigue test perform
ed at Stress
amplitude 10 ksi fatigue frequency 3 H
z at EB
C and 1 hr therm
al gradient cycles -
Tested EB
C surface tem
perature 1537degC (2800degF) and T bond coat tem
perature 1482degC
(2700degF) with C
MA
S
-D
emonstrated 300 hour durability at 2700degF+
-D
etermined fatigue-creep and therm
al conductivity behavior of the EB
C-C
MC
system
Specimen in rig testing
Test Condition Sum
mary
-EB
CC
VI-M
I Fatigue$loading 10 ksi (69 M
Pa) R
=005 with 1 hr Therm
al LC
F$-
TEB
C-surface 1537degC
(2800degF)$-
Tbond coat 1482degC
(2700degF)$-
Tback C
MC
surface 1250degC
(2282degF)
ww
wnasagov
21
National Aeronautics and Space Adm
inistration
Advanced E
BC
-CM
C Fatigue Test w
ith CM
AS
and in Steam
Jet Tested 300 h D
urability in High H
eat Flux Fatigue Test Conditions
-A
dvanced Hf-N
dYb silicate-N
dYbS
i bond coat EB
C coatings on 3D
architecture C
VI-P
IP S
iC-S
iC C
MC
(EB
-PV
D processing)
-Further understanding w
ater vapor -environmental interactions necessary
Surface view C
MA
S 35m
gcm2)
Back view
CM
AS
35mgcm
2)
ww
wnasagov
National Aeronautics and Space Adm
inistration
EBC
System
Designs ndash E
ffects of Com
posites and Clustered
Com
positions -
An alternating H
fO2 -and R
E-silicate coatings (EB
-PV
D processing) ndash H
fO2 -layer
infiltration and rare earth silicate layer melting
EB
-PV
D P
rocessed EB
Cs alternating H
fO2 -rich and ytterbium
silicate layer systems for
CM
AS
and impact resistance
ww
wnasagov
National Aeronautics and Space Adm
inistration
Sum
mary
bullC
MA
S degradation rem
ains a challenge for emerging turbine engine
environmental barrier coating ndash S
iCSiC
CM
C com
ponent systems
bullC
MA
S leads to low
er melting point of E
BC and bond coat system
s with
accelerated EBC
and CM
C degradations
bullN
AS
A advanced E
BC com
positions showed som
e promise for C
MA
S
resistance at temperatures up to 1500degC
in high velocity high heat flux and m
echanical loading tests bull
Currently focus on better understanding of E
BC com
positions and EBC
-CM
AS
interactions particularly with hafnium
zirconium and rare
earth silicates for improved tem
perature capability and CM
AS
resistance bull
Also standardize C
MA
S testing and quantify C
MA
S induced life debits
helping validate life modeling
bullC
ontrolling the compositions for C
MA
S resistance w
hile maintaining
high toughness continued to be a key emphasis
ww
wnasagov
24
National Aeronautics and Space Adm
inistration
Acknow
ledgements
bullThe w
ork was supported by N
ASA Fundam
ental Aeronautics Program (FAP)
Transformational Tools and Technologies (TTT) Project
bullThe authors are grateful to D
r Michael H
elminiak in the assistant of JETS tests
ww
wnasagov
25
National Aeronautics and Space Adm
inistration
CM
AS
Reaction K
inetics in Bond C
oats ndash S
iO2 rich phase partitioning in the C
MA
S m
elts ndash R
are earth content leaching low even at 1500degC
ndash M
ore advanced compositions are being im
plemented for im
proved thermom
echanical ndash
CM
AS Partitioning on R
E-Si bond coat 1500degC
100hr
RE incorporations
CM
AS
resistance
ww
wnasagov
26
National Aeronautics and Space Adm
inistration Strength R
esults of Selected EBC and EBC
Bond Coats
-CM
AS
Reaction R
esulted in Strength Reduction in Silicates
Selected E
BC
systems
ndashH
fO2 -R
E-S
i along with co-doped rare earth silicates and rare earth alum
ino-silicates for optim
ized strength stability and temperature capability
ndashC
MA
S infiltrations can reduce the strength
350 646-Specially alloy toughened t like H
fO2
648-EBC Bond Coat Constituent 300
659-AE9762
150
EBC
s
EBC
s
HfO
2 -Si (Si-rich)
Yb
2 Si 2 O 7
250658-EBC H
fO2-Rare Earth-A
lumino Silicate
660-Y2Si2O
7657-Zr-RE silicate 669-Y
b2Si2O7
Strength MPa
200696-EBC Bond Coat Constituent
100681-H
fO2-Si
669-9762 with CM
AS 1350C 50hr reacted
693-HfO
2-Si with CM
AS 1350C 50hr reacted
5000
200 400
600 800
1000 1200
1400 1600
Temperature degC
Strength test data compared
Yb
2 Si2 O7 C
MA
S reacted tensile Y
b2 Si2 O
7 CM
AS reacted
specimen fracture surface
surface w
ww
nasagov 27
National Aeronautics and Space Adm
inistration
High Stability and C
MAS R
esistance Observed from
the Rare
Earth S
ilicon High M
elting Point C
oating Com
positions
ndashD
emonstrated C
MA
S resistance
of NAS
A R
E-Si S
ystem at
1500degC 100 hr
ndash S
ilica-rich phase precipitation ndash
Rare earth elem
ent leaching into the m
elts (low concentration ~9
Surface side of the m
ol)
CM
AS m
elts
Area A
Area B
ww
wnasagov
28
![Page 2: Hurst, Bernadette J. Puleo€¦ · G57, 40.00 mg CMAS SiO Wellman -Aygun Smialek Braue 0 49 mole%; such as NASA’s CMAS (with NiO DSC:020 OES Measured by EDS [#] Type Date/time :](https://reader033.fdocuments.us/reader033/viewer/2022060211/5f04cb127e708231d40fbc15/html5/thumbnails/2.jpg)
Temperature
Capability
National Aeronautics and Space Adm
inistration
NA
SA Environm
ental Barrier Coatings (E
BCs) and C
eramic
Matrix C
omposite (C
MC
) System
Developm
entminus
Emphasize m
aterial temperature capability perform
ance and long-term
durability-Highly loaded E
BC
-CM
Cs w
ith temperature capability of 2700degF
(1482degC)
bull 2700-3000degF (1482-1650degC) turbine and C
MC
combustor coatings
bull 2700degF (1482degC) E
BC
bond coat technology for supporting next generation ndashR
ecession lt5 mgcm
2 per 1000 h ndashC
oating and component strength requirem
ents 15-30 ksi or 100-207 Mpa
ndashResistance to C
alcium M
agnesium A
lumino-S
ilicate (CM
AS
) Step increase in the m
aterialrsquos temperature capability
Temperature
3000degF SiC
SiC
CM
C airfoil
Capability (TE(TEBBC)C) ssuurfarfaccee
and combustor
3000degF+ (1650degC+)
technologies 2700degF S
iCS
iC thin turbine
2700degF (1482qC)
2700degF (1482degC) G
en III SiCSiC
CM
Cs
EB
C system
s for CM
C
airfoils
2400degF (1316degC) G
en I and Gen II SiC
SiC
CM
Cs
2000degF (1093degC) PtAl and N
iAl bond coats
Gen II ndash
Currentcomm
ercialG
en IIIG
en IV
Increase in T across TEBC
Single Crystal Superalloy
Ceramic M
atrix Composite
Gen II ndash Current com
mercial
Gen III
Gen IV
Increase in T across TEBC
Single Crystal Superalloy
Ceramic M
atrix Composite
2800ordmF com
bustor TB
C
2500ordmF Turbine TB
C
GGenen II
YYearear
ww
wnasagov
2
National Aeronautics and Space Adm
inistration
Outline
bullN
ASA environm
ental barrier coating (EBC
) development the C
MAS
relevance and importance
minus E
BC
systems
minus C
MA
S com
positions
bullSom
e generalized CM
AS related failures
bullC
MAS degradation of environm
ental barrier coating (EBC
) systems rare
earth silicates ndash
Ytterbium
silicate and yttrium silicate E
BC
s ndash
Som
e reactions kinetics and mechanism
s
bullC
urrent advanced EBC
s HfO
2 -and Rare Earth -Silicon based 2700degF+
capable bond coats ndash
Som
e CM
AS
durability tests and results
bull Sum
mary
ww
wnasagov
3
National Aeronautics and Space Adm
inistration
EBC-C
MA
S D
egradation is of Concern w
ith Increasing O
perating Temperatures
minusEm
phasize improving tem
perature capability performance and long-term
durability of ceram
ic turbine airfoils bull
Increased gas inlet temperatures for net generation engines lead to significant C
MA
S -
related coating durability issues ndash CM
AS
infiltration and reactions
Marcus P B
orom et al S
urf Coat
Technol 86-87 1996
Current airfoil C
MA
S attack
region -R D
arolia International M
aterials Review
s 2013
ww
wnasagov
4
National Aeronautics and Space Adm
inistration
Calcium
Magnesium
Alumino-Silicate (C
MAS) System
s Used
in Laboratory Tests minus
N
AS
A m
odified version (NA
SA
CM
AS
) and the Air Force -P
owder Technology Incorporated
PTI 02 C
MA
S currently being used for advanced coating developm
ents minus
C
MA
S S
iO2 content typically ranging from
43-49 mole
such as NASArsquos CMAS (with N
iO
and FeO)
NA
SA m
odified CM
AS
AR
FL PTI CM
AS 02
(higher SiO2 )
GEB
orom
Wellm
an
Kram
er
Aygun Smialek
Rai
Braue
AR
FL PTI 11717A
02
Fully reacted A
s received
AFR
L02 particle size
distribution (34
Quartz 30
Gypsum
17
Aplite 14
Dolom
ite 5
Salt) Percentile Size (μm
) 10 25 +-10 50 85 +-20 90 405 +-30
Fully reacted C
MA
S EDS
ww
wnasagov
5
National Aeronautics and Space Adm
inistration
Calcium
Magnesium
Alumino-Silicate (C
MAS) System
s Used
in Laboratory Tests -Continued
minus
NA
SA
modified version (N
AS
A C
MA
S)
minus
CM
AS
SiO
2 content typically ranging from 43-49 m
ole such as N
ASArsquos CMAS (with N
iO
and FeO)
NA
SA
CM
AS
Com
positions
NA
SA m
odified CM
AS
AR
FL PTI CM
AS 02
(higher SiO2 )
GEB
orom
Wellm
an
Kram
er
Aygun Smialek
Rai
Braue
Method
Content (m
ol)
CaO
M
gO
Al2 O3
SiO2
Fe2 O
3 N
iO
(DesignedTargeted)
338 90
67 460
30 15
Measured by IC
P-O
ES 38 r 2
90 r 05 69 r 03
41 r 2 38 r 02
137 r 007
Measured by ED
S 36 r 1
84 r 03 75 r 02
43 r 1 39 r 01
15 r 01
Created w
ith NE
TZSC
H P
roteus software
[] Type [11] D
ynamic
Range
2550(Km
in)1500 A
cqRate
7500 S
TC
0 P
1N2O
2 500
Corr
DS
C020
[] Type [13] D
ynamic
Range
150050(Km
in)25 A
cqRate
7500 S
TC
0 P
1N2O
2 500
Corr
DS
C020
Project
Identity D
atetime
Laboratory O
perator S
ample
G57
6282016 91511 AM
G
lenn Research C
enter C
osta G
57 4000 mg
Reference
Material
Corrtem
pcal S
ensfile S
ample carTC
M
odetype of meas R
ef Al2O
30 mg
baseline for YS
Z 5 C_m
in up tp 1500 C 06-24-16bd8 TC
ALZE
RO
TMX
sensitivity from
sapphire_Pt crucible 1500C
air 01-06-16ed8 D
SC
Cp S
S
DS
C sam
ple with correction
Segm
ents C
rucible A
tmosphere
M range
3 DS
CTG
pan Pt
N2O
2 500mlm
in 5000 microV
Instrument N
ETZS
CH
DS
C 404F1 File C
NE
TZSC
HP
roteusdata5CostaS
amplesG
62dd8 Rem
ark Third DS
C run since O
ct 2014 1x evacbackfill
200 400
600 800
1000 1200
1400 Tem
perature degC
-10
-08
-06
-04
-02
00
02
04
DS
C (m
Wm
g)
0 50
100
150
200
250
Flow (m
lmin)
Main
exo
DSC
traces of CM
AS during heating and cooling up
to 1500 qC at 5 qC
min
ww
wnasagov
6
National Aeronautics and Space Adm
inistration
Advanced N
AS
A E
BC
Developm
ents
Improved tem
perature capability sintering phase stability recession resistance and high tem
perature strength
Advanced com
positions amp processing for com
bined therm
omechanical loading and environm
ents higher stability and increased toughness tow
ards prime-reliant
Gen I (E
PM)
RampD
Award
Gen II (U
EET)
2000-2004 Advanced EBC
(U
EET) 2000-2005 R
ampD Aw
ard (2007)
Advanced EBC (FAP)
2005-2011 R
ampD Aw
ard (2007) coating turbine developm
ent
Advanced EBC
(FAP -ERA)
2007 -present
Advanced (FAP ERA)
Patent13923450 PC
TUS1346946 and subsequent patents
Engine C
omponents
Com
bustor C
ombustor
(Vane) C
ombustor
Vane Vane Blade
-VaneBlade EB
Cs
-Equivalent APS com
bustor EBC
s
Airfoil components
Top Coat
BSAS (APS) R
E2 Si2 O
7 or R
E2 SiO
5 (APS)
-(HfY
bGdY
) 2 O3
-ZrO2 H
fO2 +R
E
silicates -ZrO
2 HfO
2 +BS
AS
(APS and EBPVD
)
RE-H
fO2 -Alum
ino silicate
(APS andor 100
EB-
PVD)
RE-H
fO2 -X
advanced top coat R
E-HfO
2 Silica (EB
-PVD etc vapor
deposition)
Advanced EBC
s
Interlayer --
--R
E-HfO
2 ZrO2 -
aluminosilicate
layered systems
Nanocom
posite graded oxidesilicate
--
EBC
M
ullite+ BSAS R
E2 Si2 O
7 and or BSAS+M
ullite
RE
silicates or R
E-Hf m
ullite R
E doped m
ullite-HfO
2 or R
E silicates
Multi-com
ponent R
E silicate systems
Multicom
ponent R
E-silicate + Hf self
grown
Bond C
oat Si
Si O
xide+Si bond coat
HfO
2 -Si-X
doped mulliteSi
SiC nanotube
Optim
ized HfO
2 -Si-X bond coat 2700degF bond coats
RE-Si+H
f systems
Thickness 10-15 m
il 10-15 m
il 15-20 m
il 10 m
il 5 m
il 1 -3 m
ils
Surface T U
p to 2400degF 2400degF
3000degF2400CM
C
2700degF2400F CM
C
2700-3000degF
Bond Coat T
Limited to
2462degF Lim
it to 2462degF
Limit to 2642degF
Proven at 2600degF + Advancem
ents targeting 2700degF
2700degF
Challenges overcom
e by advancem
ents
ww
wnasagov
7
National Aeronautics and Space Adm
inistration
CM
AS
Related D
egradations in EBC
s
Cross-section
50 mm
minus C
MAS effects
bull S
ignificantly reduce melting points of the E
BC
s and bond coats bull
More detrim
ental effects with thin airfoil E
BC
s bull
CM
AS
weakens the coating system
s reducing strength and toughness bullM
AS
increase EB
C diffusivities and perm
eability thus less protective as an environmental
barrier bullC
MA
S interactions w
ith heat flux thermal cycling erosion and therm
omechanical fatigue
Reaction layer spallations
Accelerated C
MC
failure when C
MA
S intact w
ith CM
Cs
Such as yttrium silicate
Coating
surface
EB
C and degradations
CM
AS induced m
elting and failure$w
ww
nasagov 8
National Aeronautics and Space Adm
inistration
CM
AS R
elated Degradations in E
BCs -C
ontinued minus
CM
AS effects on EBC
temperature capability
bull S
ilicate reactions with N
aO2 and A
l2 O3 silicate
Phase diagram
s showing yttrium
di-silicate reactions w
ith SiO
2 NaO
and Al2 O
3
ww
wnasagov
9
National Aeronautics and Space Adm
inistration
CM
AS R
elated Degradations in E
BCs -C
ontinued minus
CM
AS effects on EBC
temperature capability
bullRare earths generally have lim
ited temperature capability below
1500degC in the R
E2 O
3 -A
l2 O3 -S
iO2 based system
s bull
Sm
aller ionic size RE
s have higher melting points
Solidus temperature in Ln
2 Si2 O7 -A
l6 Si2 O13 -
SiO2 system
as function of ionic radius
Y Murakam
i and H Yam
amoto J C
eram Soc Jpn 101 [10] 1101-1106 (1993)
ww
wnasagov
10
National Aeronautics and Space Adm
inistration
Rare Earth D
issolutions in CM
AS Melts
ZrO2 -30Y
2 O3 -15Sm
2 O3 -15Yb
2 O3
ZrO2 -30Y
2 O3 -15N
d2 O
3 -15Yb2 O
3 -03Sc2 O
3
ZrO2 -96Y
2 O3 -22G
d2 O
3 -21Yb2 O
3
Ionic potential trend of RE
Radius size trend of RE
minus Large ionic size rare earths show
ed higher concentration dissolutions in the CM
AS
m
elt for ZrO2 -R
E2 O
3 oxide systems
ZrO2 -R
EO15 -H
f more endotherm
ic
Gustavo and Zhu International C
onference on Advanced C
eramics and C
omposites 2016
ww
wnasagov
11
Front CM
AS side
National Aeronautics and Space Adm
inistration
CM
AS Related D
egradations in EBC
coated CM
Cs ndash
Laboratory Heat Flux Tests
minusC
MAS effects on EB
C-C
MC
temperature capability tested in laser high heat
flux creep-rupture rig bull
Accelerated failure of C
MC
in loading high heat flux conditions
EBC
coated CV
I-MI C
MC
with N
dYb silicate R
ESi bond coat tested Tsurface 2600degF TC
MC
2450degF
Front heated CM
AS
side B
ack cooled side
Creep strain
Time h
Front CM
AS
side
200h
05
ww
wnasagov
12
National Aeronautics and Space Adm
inistration
EBC
CM
AS
Surface Initial N
ucleation Dissolution R
eactions ndash
Ytterbium
-and yttrium-silicate silicates reactions and dissolutions in C
AM
S
ndash M
ore sluggish dissolution of ytterbium as com
pared to yttrium
Ytterbium
di-silicate surface CM
AS m
elts 50 Y
tterbium di-silicate surface C
MA
S melts 5 h
h 1300degC
1500degC$
Yttrium
mono-silicate surface C
MA
S Y
ttrium silicate surface C
MA
S melts 5 h
melts 50 h 1300degC
1500degC
A
hlborg and Zhu Surface amp C
oatings Technology 237 (2013) 79ndash87 w
ww
nasagov 13
National Aeronautics and Space Adm
inistration
Rare E
arth Apatite G
rain Grow
th ndash
Grain grow
th of apatite phase at 1500degC at various tim
es
Ytterbium
silicate system
50 hr 150 hr
200 hr
200 hr50 hr
150 hr
Yttrium
silicate system$
ww
wnasagov
14
National Aeronautics and Space Adm
inistration
Effect of C
MA
S R
eactions on Grain B
oundary Phases
ndash C
MA
S and grain boundary phase has higher A
l2 O3
content (17-22 mole
) bull
Eutectic region w
ith high Al2 O
3 content ~1200degC m
elting point bull
Loss of SiO
2 due to volatility
200 hr 1500degC
NA
SA
modified
CM
AS
Grain
boundary final phase ndash low
SiO
2 and high A
lumina
ww
wnasagov
15
National Aeronautics and Space Adm
inistration
Rare E
arth Dissolution in C
MA
S M
elts ndash
Non stoichiom
etric characteristics of the CM
AS
ndash rare earth silicate reacted apatite phases ndash up to 200 h testing
ndash D
ifference in partitioning of ytterbium vs yttrium
in apatite bull
Average AE
OR
E2 O
3 ratio ~ 068 for ytterbium silicate ndash C
MA
S system
bull
Average AE
OR
E2 O
3 ratio ~ 022 for yttrium silicate ndash C
MA
S system
C
omposition in apatite (100 hr)
SiO2
Ahlborg and Zhu Surface amp
Coatings Technology 237 (2013) 79ndash87
RE
2 O3
AEO
Yttrium
Silicate EBC
Com
position in apatite (100 hr)
Ytterbium
Silicate EBC
ww
wnasagov
16
National Aeronautics and Space Adm
inistration
Advanced N
AS
A E
BC
Developm
ents
NA
SA advanced E
BC
systems em
phasizing high stability HfO
2 -and ZrO2 -R
E2 O
3 -
EBC layer 2 region
EB
Cs
Mol
Mol
SiO
2 EB
C system
RE
2 Si2-x O
7-2x such as (YbG
dY) 2 S
i2-x O7-2x
-Controlled dissolution and m
aintaining coating stability
(YbGdY) 2 S
i2-x O7-2x in
CM
AS
1300degC
(a)
(b)
ww
wnasagov
17
National Aeronautics and Space Adm
inistration E
xample of N
AS
A A
dvanced Environm
ental Barrier C
oating on S
iCSiC
CM
C System
s
Advanced EB
C coated vanes
HfO
2 -(YbG
dY)2 O
3
(YbG
dY)2 Si2-x O
7-2x
RESi(O
)+Hf B
ond Coat
Gd Y
b Y
O
Si
Yb
Gd Y
Si
Hf
A
lternating layered HfO
2 -Multicom
ponent Rare E
arth silicate EB
Cs used for fundam
ental stability studies
2700degF capable YbG
d-YbO+H
f based bond coats C
oated onto SiC
SiC
CM
C substrates using E
B-P
VD
The bond coat region
ww
wnasagov
18
National Aeronautics and Space Adm
inistration
CM
AS
Resistant Tests
ndash JE
Ts test of more advanced coating system
s at 2700F
Plasma sprayed (G
dY)2 Si2 O
7 2450 cycles
Special processed Yb
2 Si2 O7 spalling at 450 C
ycles EB
-PVD
(YbG
dY)2 Si2 O
7 total 4450 JETS cycles 100h
2450 4450
450
Hybrid H
f-rare earth aluminate silicate com
pleted 4450 cycles 100h
Hybrid H
ybrid Zr-rare earth silicate completed 4450
cycles 100h
2450 4450
2450 with
CM
AS 2450
ww
wnasagov
19
National Aeronautics and Space Adm
inistration
High S
tability and CM
AS
Resistance are E
nsured by Advanced H
igh M
elting Point C
oating and Multi-C
omponent C
ompositions A
rea A
Area B
ndash G
enerally improved C
MA
S
resistance of NAS
A R
ESi
System
at 1500degC 100 hr
ndash S
ilica-rich phase precipitation ndash
Rare earth elem
ent leaching into the m
elts (low concentration
~9mol
)
Surface side of the C
MA
S melts
EDS E
ww
wnasagov
20
National Aeronautics and Space Adm
inistration
Advanced E
BC
-CM
C S
ystem D
emonstrated 300 hr H
igh Cycle and
Low Fatigue D
urability in High H
eat Flux 2700degF Test Conditions
Specimen after 300 h testing
-A turbine airfoil E
BC
with H
fO2 -rare earth silicate and G
dYbSi bond coat on C
VI-M
I CM
C
substrate system selected for heat flux durability testing
-Laser high heat flux rig H
igh Cycle and Low
Cycle Fatigue test perform
ed at Stress
amplitude 10 ksi fatigue frequency 3 H
z at EB
C and 1 hr therm
al gradient cycles -
Tested EB
C surface tem
perature 1537degC (2800degF) and T bond coat tem
perature 1482degC
(2700degF) with C
MA
S
-D
emonstrated 300 hour durability at 2700degF+
-D
etermined fatigue-creep and therm
al conductivity behavior of the EB
C-C
MC
system
Specimen in rig testing
Test Condition Sum
mary
-EB
CC
VI-M
I Fatigue$loading 10 ksi (69 M
Pa) R
=005 with 1 hr Therm
al LC
F$-
TEB
C-surface 1537degC
(2800degF)$-
Tbond coat 1482degC
(2700degF)$-
Tback C
MC
surface 1250degC
(2282degF)
ww
wnasagov
21
National Aeronautics and Space Adm
inistration
Advanced E
BC
-CM
C Fatigue Test w
ith CM
AS
and in Steam
Jet Tested 300 h D
urability in High H
eat Flux Fatigue Test Conditions
-A
dvanced Hf-N
dYb silicate-N
dYbS
i bond coat EB
C coatings on 3D
architecture C
VI-P
IP S
iC-S
iC C
MC
(EB
-PV
D processing)
-Further understanding w
ater vapor -environmental interactions necessary
Surface view C
MA
S 35m
gcm2)
Back view
CM
AS
35mgcm
2)
ww
wnasagov
National Aeronautics and Space Adm
inistration
EBC
System
Designs ndash E
ffects of Com
posites and Clustered
Com
positions -
An alternating H
fO2 -and R
E-silicate coatings (EB
-PV
D processing) ndash H
fO2 -layer
infiltration and rare earth silicate layer melting
EB
-PV
D P
rocessed EB
Cs alternating H
fO2 -rich and ytterbium
silicate layer systems for
CM
AS
and impact resistance
ww
wnasagov
National Aeronautics and Space Adm
inistration
Sum
mary
bullC
MA
S degradation rem
ains a challenge for emerging turbine engine
environmental barrier coating ndash S
iCSiC
CM
C com
ponent systems
bullC
MA
S leads to low
er melting point of E
BC and bond coat system
s with
accelerated EBC
and CM
C degradations
bullN
AS
A advanced E
BC com
positions showed som
e promise for C
MA
S
resistance at temperatures up to 1500degC
in high velocity high heat flux and m
echanical loading tests bull
Currently focus on better understanding of E
BC com
positions and EBC
-CM
AS
interactions particularly with hafnium
zirconium and rare
earth silicates for improved tem
perature capability and CM
AS
resistance bull
Also standardize C
MA
S testing and quantify C
MA
S induced life debits
helping validate life modeling
bullC
ontrolling the compositions for C
MA
S resistance w
hile maintaining
high toughness continued to be a key emphasis
ww
wnasagov
24
National Aeronautics and Space Adm
inistration
Acknow
ledgements
bullThe w
ork was supported by N
ASA Fundam
ental Aeronautics Program (FAP)
Transformational Tools and Technologies (TTT) Project
bullThe authors are grateful to D
r Michael H
elminiak in the assistant of JETS tests
ww
wnasagov
25
National Aeronautics and Space Adm
inistration
CM
AS
Reaction K
inetics in Bond C
oats ndash S
iO2 rich phase partitioning in the C
MA
S m
elts ndash R
are earth content leaching low even at 1500degC
ndash M
ore advanced compositions are being im
plemented for im
proved thermom
echanical ndash
CM
AS Partitioning on R
E-Si bond coat 1500degC
100hr
RE incorporations
CM
AS
resistance
ww
wnasagov
26
National Aeronautics and Space Adm
inistration Strength R
esults of Selected EBC and EBC
Bond Coats
-CM
AS
Reaction R
esulted in Strength Reduction in Silicates
Selected E
BC
systems
ndashH
fO2 -R
E-S
i along with co-doped rare earth silicates and rare earth alum
ino-silicates for optim
ized strength stability and temperature capability
ndashC
MA
S infiltrations can reduce the strength
350 646-Specially alloy toughened t like H
fO2
648-EBC Bond Coat Constituent 300
659-AE9762
150
EBC
s
EBC
s
HfO
2 -Si (Si-rich)
Yb
2 Si 2 O 7
250658-EBC H
fO2-Rare Earth-A
lumino Silicate
660-Y2Si2O
7657-Zr-RE silicate 669-Y
b2Si2O7
Strength MPa
200696-EBC Bond Coat Constituent
100681-H
fO2-Si
669-9762 with CM
AS 1350C 50hr reacted
693-HfO
2-Si with CM
AS 1350C 50hr reacted
5000
200 400
600 800
1000 1200
1400 1600
Temperature degC
Strength test data compared
Yb
2 Si2 O7 C
MA
S reacted tensile Y
b2 Si2 O
7 CM
AS reacted
specimen fracture surface
surface w
ww
nasagov 27
National Aeronautics and Space Adm
inistration
High Stability and C
MAS R
esistance Observed from
the Rare
Earth S
ilicon High M
elting Point C
oating Com
positions
ndashD
emonstrated C
MA
S resistance
of NAS
A R
E-Si S
ystem at
1500degC 100 hr
ndash S
ilica-rich phase precipitation ndash
Rare earth elem
ent leaching into the m
elts (low concentration ~9
Surface side of the m
ol)
CM
AS m
elts
Area A
Area B
ww
wnasagov
28
![Page 3: Hurst, Bernadette J. Puleo€¦ · G57, 40.00 mg CMAS SiO Wellman -Aygun Smialek Braue 0 49 mole%; such as NASA’s CMAS (with NiO DSC:020 OES Measured by EDS [#] Type Date/time :](https://reader033.fdocuments.us/reader033/viewer/2022060211/5f04cb127e708231d40fbc15/html5/thumbnails/3.jpg)
National Aeronautics and Space Adm
inistration
Outline
bullN
ASA environm
ental barrier coating (EBC
) development the C
MAS
relevance and importance
minus E
BC
systems
minus C
MA
S com
positions
bullSom
e generalized CM
AS related failures
bullC
MAS degradation of environm
ental barrier coating (EBC
) systems rare
earth silicates ndash
Ytterbium
silicate and yttrium silicate E
BC
s ndash
Som
e reactions kinetics and mechanism
s
bullC
urrent advanced EBC
s HfO
2 -and Rare Earth -Silicon based 2700degF+
capable bond coats ndash
Som
e CM
AS
durability tests and results
bull Sum
mary
ww
wnasagov
3
National Aeronautics and Space Adm
inistration
EBC-C
MA
S D
egradation is of Concern w
ith Increasing O
perating Temperatures
minusEm
phasize improving tem
perature capability performance and long-term
durability of ceram
ic turbine airfoils bull
Increased gas inlet temperatures for net generation engines lead to significant C
MA
S -
related coating durability issues ndash CM
AS
infiltration and reactions
Marcus P B
orom et al S
urf Coat
Technol 86-87 1996
Current airfoil C
MA
S attack
region -R D
arolia International M
aterials Review
s 2013
ww
wnasagov
4
National Aeronautics and Space Adm
inistration
Calcium
Magnesium
Alumino-Silicate (C
MAS) System
s Used
in Laboratory Tests minus
N
AS
A m
odified version (NA
SA
CM
AS
) and the Air Force -P
owder Technology Incorporated
PTI 02 C
MA
S currently being used for advanced coating developm
ents minus
C
MA
S S
iO2 content typically ranging from
43-49 mole
such as NASArsquos CMAS (with N
iO
and FeO)
NA
SA m
odified CM
AS
AR
FL PTI CM
AS 02
(higher SiO2 )
GEB
orom
Wellm
an
Kram
er
Aygun Smialek
Rai
Braue
AR
FL PTI 11717A
02
Fully reacted A
s received
AFR
L02 particle size
distribution (34
Quartz 30
Gypsum
17
Aplite 14
Dolom
ite 5
Salt) Percentile Size (μm
) 10 25 +-10 50 85 +-20 90 405 +-30
Fully reacted C
MA
S EDS
ww
wnasagov
5
National Aeronautics and Space Adm
inistration
Calcium
Magnesium
Alumino-Silicate (C
MAS) System
s Used
in Laboratory Tests -Continued
minus
NA
SA
modified version (N
AS
A C
MA
S)
minus
CM
AS
SiO
2 content typically ranging from 43-49 m
ole such as N
ASArsquos CMAS (with N
iO
and FeO)
NA
SA
CM
AS
Com
positions
NA
SA m
odified CM
AS
AR
FL PTI CM
AS 02
(higher SiO2 )
GEB
orom
Wellm
an
Kram
er
Aygun Smialek
Rai
Braue
Method
Content (m
ol)
CaO
M
gO
Al2 O3
SiO2
Fe2 O
3 N
iO
(DesignedTargeted)
338 90
67 460
30 15
Measured by IC
P-O
ES 38 r 2
90 r 05 69 r 03
41 r 2 38 r 02
137 r 007
Measured by ED
S 36 r 1
84 r 03 75 r 02
43 r 1 39 r 01
15 r 01
Created w
ith NE
TZSC
H P
roteus software
[] Type [11] D
ynamic
Range
2550(Km
in)1500 A
cqRate
7500 S
TC
0 P
1N2O
2 500
Corr
DS
C020
[] Type [13] D
ynamic
Range
150050(Km
in)25 A
cqRate
7500 S
TC
0 P
1N2O
2 500
Corr
DS
C020
Project
Identity D
atetime
Laboratory O
perator S
ample
G57
6282016 91511 AM
G
lenn Research C
enter C
osta G
57 4000 mg
Reference
Material
Corrtem
pcal S
ensfile S
ample carTC
M
odetype of meas R
ef Al2O
30 mg
baseline for YS
Z 5 C_m
in up tp 1500 C 06-24-16bd8 TC
ALZE
RO
TMX
sensitivity from
sapphire_Pt crucible 1500C
air 01-06-16ed8 D
SC
Cp S
S
DS
C sam
ple with correction
Segm
ents C
rucible A
tmosphere
M range
3 DS
CTG
pan Pt
N2O
2 500mlm
in 5000 microV
Instrument N
ETZS
CH
DS
C 404F1 File C
NE
TZSC
HP
roteusdata5CostaS
amplesG
62dd8 Rem
ark Third DS
C run since O
ct 2014 1x evacbackfill
200 400
600 800
1000 1200
1400 Tem
perature degC
-10
-08
-06
-04
-02
00
02
04
DS
C (m
Wm
g)
0 50
100
150
200
250
Flow (m
lmin)
Main
exo
DSC
traces of CM
AS during heating and cooling up
to 1500 qC at 5 qC
min
ww
wnasagov
6
National Aeronautics and Space Adm
inistration
Advanced N
AS
A E
BC
Developm
ents
Improved tem
perature capability sintering phase stability recession resistance and high tem
perature strength
Advanced com
positions amp processing for com
bined therm
omechanical loading and environm
ents higher stability and increased toughness tow
ards prime-reliant
Gen I (E
PM)
RampD
Award
Gen II (U
EET)
2000-2004 Advanced EBC
(U
EET) 2000-2005 R
ampD Aw
ard (2007)
Advanced EBC (FAP)
2005-2011 R
ampD Aw
ard (2007) coating turbine developm
ent
Advanced EBC
(FAP -ERA)
2007 -present
Advanced (FAP ERA)
Patent13923450 PC
TUS1346946 and subsequent patents
Engine C
omponents
Com
bustor C
ombustor
(Vane) C
ombustor
Vane Vane Blade
-VaneBlade EB
Cs
-Equivalent APS com
bustor EBC
s
Airfoil components
Top Coat
BSAS (APS) R
E2 Si2 O
7 or R
E2 SiO
5 (APS)
-(HfY
bGdY
) 2 O3
-ZrO2 H
fO2 +R
E
silicates -ZrO
2 HfO
2 +BS
AS
(APS and EBPVD
)
RE-H
fO2 -Alum
ino silicate
(APS andor 100
EB-
PVD)
RE-H
fO2 -X
advanced top coat R
E-HfO
2 Silica (EB
-PVD etc vapor
deposition)
Advanced EBC
s
Interlayer --
--R
E-HfO
2 ZrO2 -
aluminosilicate
layered systems
Nanocom
posite graded oxidesilicate
--
EBC
M
ullite+ BSAS R
E2 Si2 O
7 and or BSAS+M
ullite
RE
silicates or R
E-Hf m
ullite R
E doped m
ullite-HfO
2 or R
E silicates
Multi-com
ponent R
E silicate systems
Multicom
ponent R
E-silicate + Hf self
grown
Bond C
oat Si
Si O
xide+Si bond coat
HfO
2 -Si-X
doped mulliteSi
SiC nanotube
Optim
ized HfO
2 -Si-X bond coat 2700degF bond coats
RE-Si+H
f systems
Thickness 10-15 m
il 10-15 m
il 15-20 m
il 10 m
il 5 m
il 1 -3 m
ils
Surface T U
p to 2400degF 2400degF
3000degF2400CM
C
2700degF2400F CM
C
2700-3000degF
Bond Coat T
Limited to
2462degF Lim
it to 2462degF
Limit to 2642degF
Proven at 2600degF + Advancem
ents targeting 2700degF
2700degF
Challenges overcom
e by advancem
ents
ww
wnasagov
7
National Aeronautics and Space Adm
inistration
CM
AS
Related D
egradations in EBC
s
Cross-section
50 mm
minus C
MAS effects
bull S
ignificantly reduce melting points of the E
BC
s and bond coats bull
More detrim
ental effects with thin airfoil E
BC
s bull
CM
AS
weakens the coating system
s reducing strength and toughness bullM
AS
increase EB
C diffusivities and perm
eability thus less protective as an environmental
barrier bullC
MA
S interactions w
ith heat flux thermal cycling erosion and therm
omechanical fatigue
Reaction layer spallations
Accelerated C
MC
failure when C
MA
S intact w
ith CM
Cs
Such as yttrium silicate
Coating
surface
EB
C and degradations
CM
AS induced m
elting and failure$w
ww
nasagov 8
National Aeronautics and Space Adm
inistration
CM
AS R
elated Degradations in E
BCs -C
ontinued minus
CM
AS effects on EBC
temperature capability
bull S
ilicate reactions with N
aO2 and A
l2 O3 silicate
Phase diagram
s showing yttrium
di-silicate reactions w
ith SiO
2 NaO
and Al2 O
3
ww
wnasagov
9
National Aeronautics and Space Adm
inistration
CM
AS R
elated Degradations in E
BCs -C
ontinued minus
CM
AS effects on EBC
temperature capability
bullRare earths generally have lim
ited temperature capability below
1500degC in the R
E2 O
3 -A
l2 O3 -S
iO2 based system
s bull
Sm
aller ionic size RE
s have higher melting points
Solidus temperature in Ln
2 Si2 O7 -A
l6 Si2 O13 -
SiO2 system
as function of ionic radius
Y Murakam
i and H Yam
amoto J C
eram Soc Jpn 101 [10] 1101-1106 (1993)
ww
wnasagov
10
National Aeronautics and Space Adm
inistration
Rare Earth D
issolutions in CM
AS Melts
ZrO2 -30Y
2 O3 -15Sm
2 O3 -15Yb
2 O3
ZrO2 -30Y
2 O3 -15N
d2 O
3 -15Yb2 O
3 -03Sc2 O
3
ZrO2 -96Y
2 O3 -22G
d2 O
3 -21Yb2 O
3
Ionic potential trend of RE
Radius size trend of RE
minus Large ionic size rare earths show
ed higher concentration dissolutions in the CM
AS
m
elt for ZrO2 -R
E2 O
3 oxide systems
ZrO2 -R
EO15 -H
f more endotherm
ic
Gustavo and Zhu International C
onference on Advanced C
eramics and C
omposites 2016
ww
wnasagov
11
Front CM
AS side
National Aeronautics and Space Adm
inistration
CM
AS Related D
egradations in EBC
coated CM
Cs ndash
Laboratory Heat Flux Tests
minusC
MAS effects on EB
C-C
MC
temperature capability tested in laser high heat
flux creep-rupture rig bull
Accelerated failure of C
MC
in loading high heat flux conditions
EBC
coated CV
I-MI C
MC
with N
dYb silicate R
ESi bond coat tested Tsurface 2600degF TC
MC
2450degF
Front heated CM
AS
side B
ack cooled side
Creep strain
Time h
Front CM
AS
side
200h
05
ww
wnasagov
12
National Aeronautics and Space Adm
inistration
EBC
CM
AS
Surface Initial N
ucleation Dissolution R
eactions ndash
Ytterbium
-and yttrium-silicate silicates reactions and dissolutions in C
AM
S
ndash M
ore sluggish dissolution of ytterbium as com
pared to yttrium
Ytterbium
di-silicate surface CM
AS m
elts 50 Y
tterbium di-silicate surface C
MA
S melts 5 h
h 1300degC
1500degC$
Yttrium
mono-silicate surface C
MA
S Y
ttrium silicate surface C
MA
S melts 5 h
melts 50 h 1300degC
1500degC
A
hlborg and Zhu Surface amp C
oatings Technology 237 (2013) 79ndash87 w
ww
nasagov 13
National Aeronautics and Space Adm
inistration
Rare E
arth Apatite G
rain Grow
th ndash
Grain grow
th of apatite phase at 1500degC at various tim
es
Ytterbium
silicate system
50 hr 150 hr
200 hr
200 hr50 hr
150 hr
Yttrium
silicate system$
ww
wnasagov
14
National Aeronautics and Space Adm
inistration
Effect of C
MA
S R
eactions on Grain B
oundary Phases
ndash C
MA
S and grain boundary phase has higher A
l2 O3
content (17-22 mole
) bull
Eutectic region w
ith high Al2 O
3 content ~1200degC m
elting point bull
Loss of SiO
2 due to volatility
200 hr 1500degC
NA
SA
modified
CM
AS
Grain
boundary final phase ndash low
SiO
2 and high A
lumina
ww
wnasagov
15
National Aeronautics and Space Adm
inistration
Rare E
arth Dissolution in C
MA
S M
elts ndash
Non stoichiom
etric characteristics of the CM
AS
ndash rare earth silicate reacted apatite phases ndash up to 200 h testing
ndash D
ifference in partitioning of ytterbium vs yttrium
in apatite bull
Average AE
OR
E2 O
3 ratio ~ 068 for ytterbium silicate ndash C
MA
S system
bull
Average AE
OR
E2 O
3 ratio ~ 022 for yttrium silicate ndash C
MA
S system
C
omposition in apatite (100 hr)
SiO2
Ahlborg and Zhu Surface amp
Coatings Technology 237 (2013) 79ndash87
RE
2 O3
AEO
Yttrium
Silicate EBC
Com
position in apatite (100 hr)
Ytterbium
Silicate EBC
ww
wnasagov
16
National Aeronautics and Space Adm
inistration
Advanced N
AS
A E
BC
Developm
ents
NA
SA advanced E
BC
systems em
phasizing high stability HfO
2 -and ZrO2 -R
E2 O
3 -
EBC layer 2 region
EB
Cs
Mol
Mol
SiO
2 EB
C system
RE
2 Si2-x O
7-2x such as (YbG
dY) 2 S
i2-x O7-2x
-Controlled dissolution and m
aintaining coating stability
(YbGdY) 2 S
i2-x O7-2x in
CM
AS
1300degC
(a)
(b)
ww
wnasagov
17
National Aeronautics and Space Adm
inistration E
xample of N
AS
A A
dvanced Environm
ental Barrier C
oating on S
iCSiC
CM
C System
s
Advanced EB
C coated vanes
HfO
2 -(YbG
dY)2 O
3
(YbG
dY)2 Si2-x O
7-2x
RESi(O
)+Hf B
ond Coat
Gd Y
b Y
O
Si
Yb
Gd Y
Si
Hf
A
lternating layered HfO
2 -Multicom
ponent Rare E
arth silicate EB
Cs used for fundam
ental stability studies
2700degF capable YbG
d-YbO+H
f based bond coats C
oated onto SiC
SiC
CM
C substrates using E
B-P
VD
The bond coat region
ww
wnasagov
18
National Aeronautics and Space Adm
inistration
CM
AS
Resistant Tests
ndash JE
Ts test of more advanced coating system
s at 2700F
Plasma sprayed (G
dY)2 Si2 O
7 2450 cycles
Special processed Yb
2 Si2 O7 spalling at 450 C
ycles EB
-PVD
(YbG
dY)2 Si2 O
7 total 4450 JETS cycles 100h
2450 4450
450
Hybrid H
f-rare earth aluminate silicate com
pleted 4450 cycles 100h
Hybrid H
ybrid Zr-rare earth silicate completed 4450
cycles 100h
2450 4450
2450 with
CM
AS 2450
ww
wnasagov
19
National Aeronautics and Space Adm
inistration
High S
tability and CM
AS
Resistance are E
nsured by Advanced H
igh M
elting Point C
oating and Multi-C
omponent C
ompositions A
rea A
Area B
ndash G
enerally improved C
MA
S
resistance of NAS
A R
ESi
System
at 1500degC 100 hr
ndash S
ilica-rich phase precipitation ndash
Rare earth elem
ent leaching into the m
elts (low concentration
~9mol
)
Surface side of the C
MA
S melts
EDS E
ww
wnasagov
20
National Aeronautics and Space Adm
inistration
Advanced E
BC
-CM
C S
ystem D
emonstrated 300 hr H
igh Cycle and
Low Fatigue D
urability in High H
eat Flux 2700degF Test Conditions
Specimen after 300 h testing
-A turbine airfoil E
BC
with H
fO2 -rare earth silicate and G
dYbSi bond coat on C
VI-M
I CM
C
substrate system selected for heat flux durability testing
-Laser high heat flux rig H
igh Cycle and Low
Cycle Fatigue test perform
ed at Stress
amplitude 10 ksi fatigue frequency 3 H
z at EB
C and 1 hr therm
al gradient cycles -
Tested EB
C surface tem
perature 1537degC (2800degF) and T bond coat tem
perature 1482degC
(2700degF) with C
MA
S
-D
emonstrated 300 hour durability at 2700degF+
-D
etermined fatigue-creep and therm
al conductivity behavior of the EB
C-C
MC
system
Specimen in rig testing
Test Condition Sum
mary
-EB
CC
VI-M
I Fatigue$loading 10 ksi (69 M
Pa) R
=005 with 1 hr Therm
al LC
F$-
TEB
C-surface 1537degC
(2800degF)$-
Tbond coat 1482degC
(2700degF)$-
Tback C
MC
surface 1250degC
(2282degF)
ww
wnasagov
21
National Aeronautics and Space Adm
inistration
Advanced E
BC
-CM
C Fatigue Test w
ith CM
AS
and in Steam
Jet Tested 300 h D
urability in High H
eat Flux Fatigue Test Conditions
-A
dvanced Hf-N
dYb silicate-N
dYbS
i bond coat EB
C coatings on 3D
architecture C
VI-P
IP S
iC-S
iC C
MC
(EB
-PV
D processing)
-Further understanding w
ater vapor -environmental interactions necessary
Surface view C
MA
S 35m
gcm2)
Back view
CM
AS
35mgcm
2)
ww
wnasagov
National Aeronautics and Space Adm
inistration
EBC
System
Designs ndash E
ffects of Com
posites and Clustered
Com
positions -
An alternating H
fO2 -and R
E-silicate coatings (EB
-PV
D processing) ndash H
fO2 -layer
infiltration and rare earth silicate layer melting
EB
-PV
D P
rocessed EB
Cs alternating H
fO2 -rich and ytterbium
silicate layer systems for
CM
AS
and impact resistance
ww
wnasagov
National Aeronautics and Space Adm
inistration
Sum
mary
bullC
MA
S degradation rem
ains a challenge for emerging turbine engine
environmental barrier coating ndash S
iCSiC
CM
C com
ponent systems
bullC
MA
S leads to low
er melting point of E
BC and bond coat system
s with
accelerated EBC
and CM
C degradations
bullN
AS
A advanced E
BC com
positions showed som
e promise for C
MA
S
resistance at temperatures up to 1500degC
in high velocity high heat flux and m
echanical loading tests bull
Currently focus on better understanding of E
BC com
positions and EBC
-CM
AS
interactions particularly with hafnium
zirconium and rare
earth silicates for improved tem
perature capability and CM
AS
resistance bull
Also standardize C
MA
S testing and quantify C
MA
S induced life debits
helping validate life modeling
bullC
ontrolling the compositions for C
MA
S resistance w
hile maintaining
high toughness continued to be a key emphasis
ww
wnasagov
24
National Aeronautics and Space Adm
inistration
Acknow
ledgements
bullThe w
ork was supported by N
ASA Fundam
ental Aeronautics Program (FAP)
Transformational Tools and Technologies (TTT) Project
bullThe authors are grateful to D
r Michael H
elminiak in the assistant of JETS tests
ww
wnasagov
25
National Aeronautics and Space Adm
inistration
CM
AS
Reaction K
inetics in Bond C
oats ndash S
iO2 rich phase partitioning in the C
MA
S m
elts ndash R
are earth content leaching low even at 1500degC
ndash M
ore advanced compositions are being im
plemented for im
proved thermom
echanical ndash
CM
AS Partitioning on R
E-Si bond coat 1500degC
100hr
RE incorporations
CM
AS
resistance
ww
wnasagov
26
National Aeronautics and Space Adm
inistration Strength R
esults of Selected EBC and EBC
Bond Coats
-CM
AS
Reaction R
esulted in Strength Reduction in Silicates
Selected E
BC
systems
ndashH
fO2 -R
E-S
i along with co-doped rare earth silicates and rare earth alum
ino-silicates for optim
ized strength stability and temperature capability
ndashC
MA
S infiltrations can reduce the strength
350 646-Specially alloy toughened t like H
fO2
648-EBC Bond Coat Constituent 300
659-AE9762
150
EBC
s
EBC
s
HfO
2 -Si (Si-rich)
Yb
2 Si 2 O 7
250658-EBC H
fO2-Rare Earth-A
lumino Silicate
660-Y2Si2O
7657-Zr-RE silicate 669-Y
b2Si2O7
Strength MPa
200696-EBC Bond Coat Constituent
100681-H
fO2-Si
669-9762 with CM
AS 1350C 50hr reacted
693-HfO
2-Si with CM
AS 1350C 50hr reacted
5000
200 400
600 800
1000 1200
1400 1600
Temperature degC
Strength test data compared
Yb
2 Si2 O7 C
MA
S reacted tensile Y
b2 Si2 O
7 CM
AS reacted
specimen fracture surface
surface w
ww
nasagov 27
National Aeronautics and Space Adm
inistration
High Stability and C
MAS R
esistance Observed from
the Rare
Earth S
ilicon High M
elting Point C
oating Com
positions
ndashD
emonstrated C
MA
S resistance
of NAS
A R
E-Si S
ystem at
1500degC 100 hr
ndash S
ilica-rich phase precipitation ndash
Rare earth elem
ent leaching into the m
elts (low concentration ~9
Surface side of the m
ol)
CM
AS m
elts
Area A
Area B
ww
wnasagov
28
![Page 4: Hurst, Bernadette J. Puleo€¦ · G57, 40.00 mg CMAS SiO Wellman -Aygun Smialek Braue 0 49 mole%; such as NASA’s CMAS (with NiO DSC:020 OES Measured by EDS [#] Type Date/time :](https://reader033.fdocuments.us/reader033/viewer/2022060211/5f04cb127e708231d40fbc15/html5/thumbnails/4.jpg)
National Aeronautics and Space Adm
inistration
EBC-C
MA
S D
egradation is of Concern w
ith Increasing O
perating Temperatures
minusEm
phasize improving tem
perature capability performance and long-term
durability of ceram
ic turbine airfoils bull
Increased gas inlet temperatures for net generation engines lead to significant C
MA
S -
related coating durability issues ndash CM
AS
infiltration and reactions
Marcus P B
orom et al S
urf Coat
Technol 86-87 1996
Current airfoil C
MA
S attack
region -R D
arolia International M
aterials Review
s 2013
ww
wnasagov
4
National Aeronautics and Space Adm
inistration
Calcium
Magnesium
Alumino-Silicate (C
MAS) System
s Used
in Laboratory Tests minus
N
AS
A m
odified version (NA
SA
CM
AS
) and the Air Force -P
owder Technology Incorporated
PTI 02 C
MA
S currently being used for advanced coating developm
ents minus
C
MA
S S
iO2 content typically ranging from
43-49 mole
such as NASArsquos CMAS (with N
iO
and FeO)
NA
SA m
odified CM
AS
AR
FL PTI CM
AS 02
(higher SiO2 )
GEB
orom
Wellm
an
Kram
er
Aygun Smialek
Rai
Braue
AR
FL PTI 11717A
02
Fully reacted A
s received
AFR
L02 particle size
distribution (34
Quartz 30
Gypsum
17
Aplite 14
Dolom
ite 5
Salt) Percentile Size (μm
) 10 25 +-10 50 85 +-20 90 405 +-30
Fully reacted C
MA
S EDS
ww
wnasagov
5
National Aeronautics and Space Adm
inistration
Calcium
Magnesium
Alumino-Silicate (C
MAS) System
s Used
in Laboratory Tests -Continued
minus
NA
SA
modified version (N
AS
A C
MA
S)
minus
CM
AS
SiO
2 content typically ranging from 43-49 m
ole such as N
ASArsquos CMAS (with N
iO
and FeO)
NA
SA
CM
AS
Com
positions
NA
SA m
odified CM
AS
AR
FL PTI CM
AS 02
(higher SiO2 )
GEB
orom
Wellm
an
Kram
er
Aygun Smialek
Rai
Braue
Method
Content (m
ol)
CaO
M
gO
Al2 O3
SiO2
Fe2 O
3 N
iO
(DesignedTargeted)
338 90
67 460
30 15
Measured by IC
P-O
ES 38 r 2
90 r 05 69 r 03
41 r 2 38 r 02
137 r 007
Measured by ED
S 36 r 1
84 r 03 75 r 02
43 r 1 39 r 01
15 r 01
Created w
ith NE
TZSC
H P
roteus software
[] Type [11] D
ynamic
Range
2550(Km
in)1500 A
cqRate
7500 S
TC
0 P
1N2O
2 500
Corr
DS
C020
[] Type [13] D
ynamic
Range
150050(Km
in)25 A
cqRate
7500 S
TC
0 P
1N2O
2 500
Corr
DS
C020
Project
Identity D
atetime
Laboratory O
perator S
ample
G57
6282016 91511 AM
G
lenn Research C
enter C
osta G
57 4000 mg
Reference
Material
Corrtem
pcal S
ensfile S
ample carTC
M
odetype of meas R
ef Al2O
30 mg
baseline for YS
Z 5 C_m
in up tp 1500 C 06-24-16bd8 TC
ALZE
RO
TMX
sensitivity from
sapphire_Pt crucible 1500C
air 01-06-16ed8 D
SC
Cp S
S
DS
C sam
ple with correction
Segm
ents C
rucible A
tmosphere
M range
3 DS
CTG
pan Pt
N2O
2 500mlm
in 5000 microV
Instrument N
ETZS
CH
DS
C 404F1 File C
NE
TZSC
HP
roteusdata5CostaS
amplesG
62dd8 Rem
ark Third DS
C run since O
ct 2014 1x evacbackfill
200 400
600 800
1000 1200
1400 Tem
perature degC
-10
-08
-06
-04
-02
00
02
04
DS
C (m
Wm
g)
0 50
100
150
200
250
Flow (m
lmin)
Main
exo
DSC
traces of CM
AS during heating and cooling up
to 1500 qC at 5 qC
min
ww
wnasagov
6
National Aeronautics and Space Adm
inistration
Advanced N
AS
A E
BC
Developm
ents
Improved tem
perature capability sintering phase stability recession resistance and high tem
perature strength
Advanced com
positions amp processing for com
bined therm
omechanical loading and environm
ents higher stability and increased toughness tow
ards prime-reliant
Gen I (E
PM)
RampD
Award
Gen II (U
EET)
2000-2004 Advanced EBC
(U
EET) 2000-2005 R
ampD Aw
ard (2007)
Advanced EBC (FAP)
2005-2011 R
ampD Aw
ard (2007) coating turbine developm
ent
Advanced EBC
(FAP -ERA)
2007 -present
Advanced (FAP ERA)
Patent13923450 PC
TUS1346946 and subsequent patents
Engine C
omponents
Com
bustor C
ombustor
(Vane) C
ombustor
Vane Vane Blade
-VaneBlade EB
Cs
-Equivalent APS com
bustor EBC
s
Airfoil components
Top Coat
BSAS (APS) R
E2 Si2 O
7 or R
E2 SiO
5 (APS)
-(HfY
bGdY
) 2 O3
-ZrO2 H
fO2 +R
E
silicates -ZrO
2 HfO
2 +BS
AS
(APS and EBPVD
)
RE-H
fO2 -Alum
ino silicate
(APS andor 100
EB-
PVD)
RE-H
fO2 -X
advanced top coat R
E-HfO
2 Silica (EB
-PVD etc vapor
deposition)
Advanced EBC
s
Interlayer --
--R
E-HfO
2 ZrO2 -
aluminosilicate
layered systems
Nanocom
posite graded oxidesilicate
--
EBC
M
ullite+ BSAS R
E2 Si2 O
7 and or BSAS+M
ullite
RE
silicates or R
E-Hf m
ullite R
E doped m
ullite-HfO
2 or R
E silicates
Multi-com
ponent R
E silicate systems
Multicom
ponent R
E-silicate + Hf self
grown
Bond C
oat Si
Si O
xide+Si bond coat
HfO
2 -Si-X
doped mulliteSi
SiC nanotube
Optim
ized HfO
2 -Si-X bond coat 2700degF bond coats
RE-Si+H
f systems
Thickness 10-15 m
il 10-15 m
il 15-20 m
il 10 m
il 5 m
il 1 -3 m
ils
Surface T U
p to 2400degF 2400degF
3000degF2400CM
C
2700degF2400F CM
C
2700-3000degF
Bond Coat T
Limited to
2462degF Lim
it to 2462degF
Limit to 2642degF
Proven at 2600degF + Advancem
ents targeting 2700degF
2700degF
Challenges overcom
e by advancem
ents
ww
wnasagov
7
National Aeronautics and Space Adm
inistration
CM
AS
Related D
egradations in EBC
s
Cross-section
50 mm
minus C
MAS effects
bull S
ignificantly reduce melting points of the E
BC
s and bond coats bull
More detrim
ental effects with thin airfoil E
BC
s bull
CM
AS
weakens the coating system
s reducing strength and toughness bullM
AS
increase EB
C diffusivities and perm
eability thus less protective as an environmental
barrier bullC
MA
S interactions w
ith heat flux thermal cycling erosion and therm
omechanical fatigue
Reaction layer spallations
Accelerated C
MC
failure when C
MA
S intact w
ith CM
Cs
Such as yttrium silicate
Coating
surface
EB
C and degradations
CM
AS induced m
elting and failure$w
ww
nasagov 8
National Aeronautics and Space Adm
inistration
CM
AS R
elated Degradations in E
BCs -C
ontinued minus
CM
AS effects on EBC
temperature capability
bull S
ilicate reactions with N
aO2 and A
l2 O3 silicate
Phase diagram
s showing yttrium
di-silicate reactions w
ith SiO
2 NaO
and Al2 O
3
ww
wnasagov
9
National Aeronautics and Space Adm
inistration
CM
AS R
elated Degradations in E
BCs -C
ontinued minus
CM
AS effects on EBC
temperature capability
bullRare earths generally have lim
ited temperature capability below
1500degC in the R
E2 O
3 -A
l2 O3 -S
iO2 based system
s bull
Sm
aller ionic size RE
s have higher melting points
Solidus temperature in Ln
2 Si2 O7 -A
l6 Si2 O13 -
SiO2 system
as function of ionic radius
Y Murakam
i and H Yam
amoto J C
eram Soc Jpn 101 [10] 1101-1106 (1993)
ww
wnasagov
10
National Aeronautics and Space Adm
inistration
Rare Earth D
issolutions in CM
AS Melts
ZrO2 -30Y
2 O3 -15Sm
2 O3 -15Yb
2 O3
ZrO2 -30Y
2 O3 -15N
d2 O
3 -15Yb2 O
3 -03Sc2 O
3
ZrO2 -96Y
2 O3 -22G
d2 O
3 -21Yb2 O
3
Ionic potential trend of RE
Radius size trend of RE
minus Large ionic size rare earths show
ed higher concentration dissolutions in the CM
AS
m
elt for ZrO2 -R
E2 O
3 oxide systems
ZrO2 -R
EO15 -H
f more endotherm
ic
Gustavo and Zhu International C
onference on Advanced C
eramics and C
omposites 2016
ww
wnasagov
11
Front CM
AS side
National Aeronautics and Space Adm
inistration
CM
AS Related D
egradations in EBC
coated CM
Cs ndash
Laboratory Heat Flux Tests
minusC
MAS effects on EB
C-C
MC
temperature capability tested in laser high heat
flux creep-rupture rig bull
Accelerated failure of C
MC
in loading high heat flux conditions
EBC
coated CV
I-MI C
MC
with N
dYb silicate R
ESi bond coat tested Tsurface 2600degF TC
MC
2450degF
Front heated CM
AS
side B
ack cooled side
Creep strain
Time h
Front CM
AS
side
200h
05
ww
wnasagov
12
National Aeronautics and Space Adm
inistration
EBC
CM
AS
Surface Initial N
ucleation Dissolution R
eactions ndash
Ytterbium
-and yttrium-silicate silicates reactions and dissolutions in C
AM
S
ndash M
ore sluggish dissolution of ytterbium as com
pared to yttrium
Ytterbium
di-silicate surface CM
AS m
elts 50 Y
tterbium di-silicate surface C
MA
S melts 5 h
h 1300degC
1500degC$
Yttrium
mono-silicate surface C
MA
S Y
ttrium silicate surface C
MA
S melts 5 h
melts 50 h 1300degC
1500degC
A
hlborg and Zhu Surface amp C
oatings Technology 237 (2013) 79ndash87 w
ww
nasagov 13
National Aeronautics and Space Adm
inistration
Rare E
arth Apatite G
rain Grow
th ndash
Grain grow
th of apatite phase at 1500degC at various tim
es
Ytterbium
silicate system
50 hr 150 hr
200 hr
200 hr50 hr
150 hr
Yttrium
silicate system$
ww
wnasagov
14
National Aeronautics and Space Adm
inistration
Effect of C
MA
S R
eactions on Grain B
oundary Phases
ndash C
MA
S and grain boundary phase has higher A
l2 O3
content (17-22 mole
) bull
Eutectic region w
ith high Al2 O
3 content ~1200degC m
elting point bull
Loss of SiO
2 due to volatility
200 hr 1500degC
NA
SA
modified
CM
AS
Grain
boundary final phase ndash low
SiO
2 and high A
lumina
ww
wnasagov
15
National Aeronautics and Space Adm
inistration
Rare E
arth Dissolution in C
MA
S M
elts ndash
Non stoichiom
etric characteristics of the CM
AS
ndash rare earth silicate reacted apatite phases ndash up to 200 h testing
ndash D
ifference in partitioning of ytterbium vs yttrium
in apatite bull
Average AE
OR
E2 O
3 ratio ~ 068 for ytterbium silicate ndash C
MA
S system
bull
Average AE
OR
E2 O
3 ratio ~ 022 for yttrium silicate ndash C
MA
S system
C
omposition in apatite (100 hr)
SiO2
Ahlborg and Zhu Surface amp
Coatings Technology 237 (2013) 79ndash87
RE
2 O3
AEO
Yttrium
Silicate EBC
Com
position in apatite (100 hr)
Ytterbium
Silicate EBC
ww
wnasagov
16
National Aeronautics and Space Adm
inistration
Advanced N
AS
A E
BC
Developm
ents
NA
SA advanced E
BC
systems em
phasizing high stability HfO
2 -and ZrO2 -R
E2 O
3 -
EBC layer 2 region
EB
Cs
Mol
Mol
SiO
2 EB
C system
RE
2 Si2-x O
7-2x such as (YbG
dY) 2 S
i2-x O7-2x
-Controlled dissolution and m
aintaining coating stability
(YbGdY) 2 S
i2-x O7-2x in
CM
AS
1300degC
(a)
(b)
ww
wnasagov
17
National Aeronautics and Space Adm
inistration E
xample of N
AS
A A
dvanced Environm
ental Barrier C
oating on S
iCSiC
CM
C System
s
Advanced EB
C coated vanes
HfO
2 -(YbG
dY)2 O
3
(YbG
dY)2 Si2-x O
7-2x
RESi(O
)+Hf B
ond Coat
Gd Y
b Y
O
Si
Yb
Gd Y
Si
Hf
A
lternating layered HfO
2 -Multicom
ponent Rare E
arth silicate EB
Cs used for fundam
ental stability studies
2700degF capable YbG
d-YbO+H
f based bond coats C
oated onto SiC
SiC
CM
C substrates using E
B-P
VD
The bond coat region
ww
wnasagov
18
National Aeronautics and Space Adm
inistration
CM
AS
Resistant Tests
ndash JE
Ts test of more advanced coating system
s at 2700F
Plasma sprayed (G
dY)2 Si2 O
7 2450 cycles
Special processed Yb
2 Si2 O7 spalling at 450 C
ycles EB
-PVD
(YbG
dY)2 Si2 O
7 total 4450 JETS cycles 100h
2450 4450
450
Hybrid H
f-rare earth aluminate silicate com
pleted 4450 cycles 100h
Hybrid H
ybrid Zr-rare earth silicate completed 4450
cycles 100h
2450 4450
2450 with
CM
AS 2450
ww
wnasagov
19
National Aeronautics and Space Adm
inistration
High S
tability and CM
AS
Resistance are E
nsured by Advanced H
igh M
elting Point C
oating and Multi-C
omponent C
ompositions A
rea A
Area B
ndash G
enerally improved C
MA
S
resistance of NAS
A R
ESi
System
at 1500degC 100 hr
ndash S
ilica-rich phase precipitation ndash
Rare earth elem
ent leaching into the m
elts (low concentration
~9mol
)
Surface side of the C
MA
S melts
EDS E
ww
wnasagov
20
National Aeronautics and Space Adm
inistration
Advanced E
BC
-CM
C S
ystem D
emonstrated 300 hr H
igh Cycle and
Low Fatigue D
urability in High H
eat Flux 2700degF Test Conditions
Specimen after 300 h testing
-A turbine airfoil E
BC
with H
fO2 -rare earth silicate and G
dYbSi bond coat on C
VI-M
I CM
C
substrate system selected for heat flux durability testing
-Laser high heat flux rig H
igh Cycle and Low
Cycle Fatigue test perform
ed at Stress
amplitude 10 ksi fatigue frequency 3 H
z at EB
C and 1 hr therm
al gradient cycles -
Tested EB
C surface tem
perature 1537degC (2800degF) and T bond coat tem
perature 1482degC
(2700degF) with C
MA
S
-D
emonstrated 300 hour durability at 2700degF+
-D
etermined fatigue-creep and therm
al conductivity behavior of the EB
C-C
MC
system
Specimen in rig testing
Test Condition Sum
mary
-EB
CC
VI-M
I Fatigue$loading 10 ksi (69 M
Pa) R
=005 with 1 hr Therm
al LC
F$-
TEB
C-surface 1537degC
(2800degF)$-
Tbond coat 1482degC
(2700degF)$-
Tback C
MC
surface 1250degC
(2282degF)
ww
wnasagov
21
National Aeronautics and Space Adm
inistration
Advanced E
BC
-CM
C Fatigue Test w
ith CM
AS
and in Steam
Jet Tested 300 h D
urability in High H
eat Flux Fatigue Test Conditions
-A
dvanced Hf-N
dYb silicate-N
dYbS
i bond coat EB
C coatings on 3D
architecture C
VI-P
IP S
iC-S
iC C
MC
(EB
-PV
D processing)
-Further understanding w
ater vapor -environmental interactions necessary
Surface view C
MA
S 35m
gcm2)
Back view
CM
AS
35mgcm
2)
ww
wnasagov
National Aeronautics and Space Adm
inistration
EBC
System
Designs ndash E
ffects of Com
posites and Clustered
Com
positions -
An alternating H
fO2 -and R
E-silicate coatings (EB
-PV
D processing) ndash H
fO2 -layer
infiltration and rare earth silicate layer melting
EB
-PV
D P
rocessed EB
Cs alternating H
fO2 -rich and ytterbium
silicate layer systems for
CM
AS
and impact resistance
ww
wnasagov
National Aeronautics and Space Adm
inistration
Sum
mary
bullC
MA
S degradation rem
ains a challenge for emerging turbine engine
environmental barrier coating ndash S
iCSiC
CM
C com
ponent systems
bullC
MA
S leads to low
er melting point of E
BC and bond coat system
s with
accelerated EBC
and CM
C degradations
bullN
AS
A advanced E
BC com
positions showed som
e promise for C
MA
S
resistance at temperatures up to 1500degC
in high velocity high heat flux and m
echanical loading tests bull
Currently focus on better understanding of E
BC com
positions and EBC
-CM
AS
interactions particularly with hafnium
zirconium and rare
earth silicates for improved tem
perature capability and CM
AS
resistance bull
Also standardize C
MA
S testing and quantify C
MA
S induced life debits
helping validate life modeling
bullC
ontrolling the compositions for C
MA
S resistance w
hile maintaining
high toughness continued to be a key emphasis
ww
wnasagov
24
National Aeronautics and Space Adm
inistration
Acknow
ledgements
bullThe w
ork was supported by N
ASA Fundam
ental Aeronautics Program (FAP)
Transformational Tools and Technologies (TTT) Project
bullThe authors are grateful to D
r Michael H
elminiak in the assistant of JETS tests
ww
wnasagov
25
National Aeronautics and Space Adm
inistration
CM
AS
Reaction K
inetics in Bond C
oats ndash S
iO2 rich phase partitioning in the C
MA
S m
elts ndash R
are earth content leaching low even at 1500degC
ndash M
ore advanced compositions are being im
plemented for im
proved thermom
echanical ndash
CM
AS Partitioning on R
E-Si bond coat 1500degC
100hr
RE incorporations
CM
AS
resistance
ww
wnasagov
26
National Aeronautics and Space Adm
inistration Strength R
esults of Selected EBC and EBC
Bond Coats
-CM
AS
Reaction R
esulted in Strength Reduction in Silicates
Selected E
BC
systems
ndashH
fO2 -R
E-S
i along with co-doped rare earth silicates and rare earth alum
ino-silicates for optim
ized strength stability and temperature capability
ndashC
MA
S infiltrations can reduce the strength
350 646-Specially alloy toughened t like H
fO2
648-EBC Bond Coat Constituent 300
659-AE9762
150
EBC
s
EBC
s
HfO
2 -Si (Si-rich)
Yb
2 Si 2 O 7
250658-EBC H
fO2-Rare Earth-A
lumino Silicate
660-Y2Si2O
7657-Zr-RE silicate 669-Y
b2Si2O7
Strength MPa
200696-EBC Bond Coat Constituent
100681-H
fO2-Si
669-9762 with CM
AS 1350C 50hr reacted
693-HfO
2-Si with CM
AS 1350C 50hr reacted
5000
200 400
600 800
1000 1200
1400 1600
Temperature degC
Strength test data compared
Yb
2 Si2 O7 C
MA
S reacted tensile Y
b2 Si2 O
7 CM
AS reacted
specimen fracture surface
surface w
ww
nasagov 27
National Aeronautics and Space Adm
inistration
High Stability and C
MAS R
esistance Observed from
the Rare
Earth S
ilicon High M
elting Point C
oating Com
positions
ndashD
emonstrated C
MA
S resistance
of NAS
A R
E-Si S
ystem at
1500degC 100 hr
ndash S
ilica-rich phase precipitation ndash
Rare earth elem
ent leaching into the m
elts (low concentration ~9
Surface side of the m
ol)
CM
AS m
elts
Area A
Area B
ww
wnasagov
28
![Page 5: Hurst, Bernadette J. Puleo€¦ · G57, 40.00 mg CMAS SiO Wellman -Aygun Smialek Braue 0 49 mole%; such as NASA’s CMAS (with NiO DSC:020 OES Measured by EDS [#] Type Date/time :](https://reader033.fdocuments.us/reader033/viewer/2022060211/5f04cb127e708231d40fbc15/html5/thumbnails/5.jpg)
National Aeronautics and Space Adm
inistration
Calcium
Magnesium
Alumino-Silicate (C
MAS) System
s Used
in Laboratory Tests minus
N
AS
A m
odified version (NA
SA
CM
AS
) and the Air Force -P
owder Technology Incorporated
PTI 02 C
MA
S currently being used for advanced coating developm
ents minus
C
MA
S S
iO2 content typically ranging from
43-49 mole
such as NASArsquos CMAS (with N
iO
and FeO)
NA
SA m
odified CM
AS
AR
FL PTI CM
AS 02
(higher SiO2 )
GEB
orom
Wellm
an
Kram
er
Aygun Smialek
Rai
Braue
AR
FL PTI 11717A
02
Fully reacted A
s received
AFR
L02 particle size
distribution (34
Quartz 30
Gypsum
17
Aplite 14
Dolom
ite 5
Salt) Percentile Size (μm
) 10 25 +-10 50 85 +-20 90 405 +-30
Fully reacted C
MA
S EDS
ww
wnasagov
5
National Aeronautics and Space Adm
inistration
Calcium
Magnesium
Alumino-Silicate (C
MAS) System
s Used
in Laboratory Tests -Continued
minus
NA
SA
modified version (N
AS
A C
MA
S)
minus
CM
AS
SiO
2 content typically ranging from 43-49 m
ole such as N
ASArsquos CMAS (with N
iO
and FeO)
NA
SA
CM
AS
Com
positions
NA
SA m
odified CM
AS
AR
FL PTI CM
AS 02
(higher SiO2 )
GEB
orom
Wellm
an
Kram
er
Aygun Smialek
Rai
Braue
Method
Content (m
ol)
CaO
M
gO
Al2 O3
SiO2
Fe2 O
3 N
iO
(DesignedTargeted)
338 90
67 460
30 15
Measured by IC
P-O
ES 38 r 2
90 r 05 69 r 03
41 r 2 38 r 02
137 r 007
Measured by ED
S 36 r 1
84 r 03 75 r 02
43 r 1 39 r 01
15 r 01
Created w
ith NE
TZSC
H P
roteus software
[] Type [11] D
ynamic
Range
2550(Km
in)1500 A
cqRate
7500 S
TC
0 P
1N2O
2 500
Corr
DS
C020
[] Type [13] D
ynamic
Range
150050(Km
in)25 A
cqRate
7500 S
TC
0 P
1N2O
2 500
Corr
DS
C020
Project
Identity D
atetime
Laboratory O
perator S
ample
G57
6282016 91511 AM
G
lenn Research C
enter C
osta G
57 4000 mg
Reference
Material
Corrtem
pcal S
ensfile S
ample carTC
M
odetype of meas R
ef Al2O
30 mg
baseline for YS
Z 5 C_m
in up tp 1500 C 06-24-16bd8 TC
ALZE
RO
TMX
sensitivity from
sapphire_Pt crucible 1500C
air 01-06-16ed8 D
SC
Cp S
S
DS
C sam
ple with correction
Segm
ents C
rucible A
tmosphere
M range
3 DS
CTG
pan Pt
N2O
2 500mlm
in 5000 microV
Instrument N
ETZS
CH
DS
C 404F1 File C
NE
TZSC
HP
roteusdata5CostaS
amplesG
62dd8 Rem
ark Third DS
C run since O
ct 2014 1x evacbackfill
200 400
600 800
1000 1200
1400 Tem
perature degC
-10
-08
-06
-04
-02
00
02
04
DS
C (m
Wm
g)
0 50
100
150
200
250
Flow (m
lmin)
Main
exo
DSC
traces of CM
AS during heating and cooling up
to 1500 qC at 5 qC
min
ww
wnasagov
6
National Aeronautics and Space Adm
inistration
Advanced N
AS
A E
BC
Developm
ents
Improved tem
perature capability sintering phase stability recession resistance and high tem
perature strength
Advanced com
positions amp processing for com
bined therm
omechanical loading and environm
ents higher stability and increased toughness tow
ards prime-reliant
Gen I (E
PM)
RampD
Award
Gen II (U
EET)
2000-2004 Advanced EBC
(U
EET) 2000-2005 R
ampD Aw
ard (2007)
Advanced EBC (FAP)
2005-2011 R
ampD Aw
ard (2007) coating turbine developm
ent
Advanced EBC
(FAP -ERA)
2007 -present
Advanced (FAP ERA)
Patent13923450 PC
TUS1346946 and subsequent patents
Engine C
omponents
Com
bustor C
ombustor
(Vane) C
ombustor
Vane Vane Blade
-VaneBlade EB
Cs
-Equivalent APS com
bustor EBC
s
Airfoil components
Top Coat
BSAS (APS) R
E2 Si2 O
7 or R
E2 SiO
5 (APS)
-(HfY
bGdY
) 2 O3
-ZrO2 H
fO2 +R
E
silicates -ZrO
2 HfO
2 +BS
AS
(APS and EBPVD
)
RE-H
fO2 -Alum
ino silicate
(APS andor 100
EB-
PVD)
RE-H
fO2 -X
advanced top coat R
E-HfO
2 Silica (EB
-PVD etc vapor
deposition)
Advanced EBC
s
Interlayer --
--R
E-HfO
2 ZrO2 -
aluminosilicate
layered systems
Nanocom
posite graded oxidesilicate
--
EBC
M
ullite+ BSAS R
E2 Si2 O
7 and or BSAS+M
ullite
RE
silicates or R
E-Hf m
ullite R
E doped m
ullite-HfO
2 or R
E silicates
Multi-com
ponent R
E silicate systems
Multicom
ponent R
E-silicate + Hf self
grown
Bond C
oat Si
Si O
xide+Si bond coat
HfO
2 -Si-X
doped mulliteSi
SiC nanotube
Optim
ized HfO
2 -Si-X bond coat 2700degF bond coats
RE-Si+H
f systems
Thickness 10-15 m
il 10-15 m
il 15-20 m
il 10 m
il 5 m
il 1 -3 m
ils
Surface T U
p to 2400degF 2400degF
3000degF2400CM
C
2700degF2400F CM
C
2700-3000degF
Bond Coat T
Limited to
2462degF Lim
it to 2462degF
Limit to 2642degF
Proven at 2600degF + Advancem
ents targeting 2700degF
2700degF
Challenges overcom
e by advancem
ents
ww
wnasagov
7
National Aeronautics and Space Adm
inistration
CM
AS
Related D
egradations in EBC
s
Cross-section
50 mm
minus C
MAS effects
bull S
ignificantly reduce melting points of the E
BC
s and bond coats bull
More detrim
ental effects with thin airfoil E
BC
s bull
CM
AS
weakens the coating system
s reducing strength and toughness bullM
AS
increase EB
C diffusivities and perm
eability thus less protective as an environmental
barrier bullC
MA
S interactions w
ith heat flux thermal cycling erosion and therm
omechanical fatigue
Reaction layer spallations
Accelerated C
MC
failure when C
MA
S intact w
ith CM
Cs
Such as yttrium silicate
Coating
surface
EB
C and degradations
CM
AS induced m
elting and failure$w
ww
nasagov 8
National Aeronautics and Space Adm
inistration
CM
AS R
elated Degradations in E
BCs -C
ontinued minus
CM
AS effects on EBC
temperature capability
bull S
ilicate reactions with N
aO2 and A
l2 O3 silicate
Phase diagram
s showing yttrium
di-silicate reactions w
ith SiO
2 NaO
and Al2 O
3
ww
wnasagov
9
National Aeronautics and Space Adm
inistration
CM
AS R
elated Degradations in E
BCs -C
ontinued minus
CM
AS effects on EBC
temperature capability
bullRare earths generally have lim
ited temperature capability below
1500degC in the R
E2 O
3 -A
l2 O3 -S
iO2 based system
s bull
Sm
aller ionic size RE
s have higher melting points
Solidus temperature in Ln
2 Si2 O7 -A
l6 Si2 O13 -
SiO2 system
as function of ionic radius
Y Murakam
i and H Yam
amoto J C
eram Soc Jpn 101 [10] 1101-1106 (1993)
ww
wnasagov
10
National Aeronautics and Space Adm
inistration
Rare Earth D
issolutions in CM
AS Melts
ZrO2 -30Y
2 O3 -15Sm
2 O3 -15Yb
2 O3
ZrO2 -30Y
2 O3 -15N
d2 O
3 -15Yb2 O
3 -03Sc2 O
3
ZrO2 -96Y
2 O3 -22G
d2 O
3 -21Yb2 O
3
Ionic potential trend of RE
Radius size trend of RE
minus Large ionic size rare earths show
ed higher concentration dissolutions in the CM
AS
m
elt for ZrO2 -R
E2 O
3 oxide systems
ZrO2 -R
EO15 -H
f more endotherm
ic
Gustavo and Zhu International C
onference on Advanced C
eramics and C
omposites 2016
ww
wnasagov
11
Front CM
AS side
National Aeronautics and Space Adm
inistration
CM
AS Related D
egradations in EBC
coated CM
Cs ndash
Laboratory Heat Flux Tests
minusC
MAS effects on EB
C-C
MC
temperature capability tested in laser high heat
flux creep-rupture rig bull
Accelerated failure of C
MC
in loading high heat flux conditions
EBC
coated CV
I-MI C
MC
with N
dYb silicate R
ESi bond coat tested Tsurface 2600degF TC
MC
2450degF
Front heated CM
AS
side B
ack cooled side
Creep strain
Time h
Front CM
AS
side
200h
05
ww
wnasagov
12
National Aeronautics and Space Adm
inistration
EBC
CM
AS
Surface Initial N
ucleation Dissolution R
eactions ndash
Ytterbium
-and yttrium-silicate silicates reactions and dissolutions in C
AM
S
ndash M
ore sluggish dissolution of ytterbium as com
pared to yttrium
Ytterbium
di-silicate surface CM
AS m
elts 50 Y
tterbium di-silicate surface C
MA
S melts 5 h
h 1300degC
1500degC$
Yttrium
mono-silicate surface C
MA
S Y
ttrium silicate surface C
MA
S melts 5 h
melts 50 h 1300degC
1500degC
A
hlborg and Zhu Surface amp C
oatings Technology 237 (2013) 79ndash87 w
ww
nasagov 13
National Aeronautics and Space Adm
inistration
Rare E
arth Apatite G
rain Grow
th ndash
Grain grow
th of apatite phase at 1500degC at various tim
es
Ytterbium
silicate system
50 hr 150 hr
200 hr
200 hr50 hr
150 hr
Yttrium
silicate system$
ww
wnasagov
14
National Aeronautics and Space Adm
inistration
Effect of C
MA
S R
eactions on Grain B
oundary Phases
ndash C
MA
S and grain boundary phase has higher A
l2 O3
content (17-22 mole
) bull
Eutectic region w
ith high Al2 O
3 content ~1200degC m
elting point bull
Loss of SiO
2 due to volatility
200 hr 1500degC
NA
SA
modified
CM
AS
Grain
boundary final phase ndash low
SiO
2 and high A
lumina
ww
wnasagov
15
National Aeronautics and Space Adm
inistration
Rare E
arth Dissolution in C
MA
S M
elts ndash
Non stoichiom
etric characteristics of the CM
AS
ndash rare earth silicate reacted apatite phases ndash up to 200 h testing
ndash D
ifference in partitioning of ytterbium vs yttrium
in apatite bull
Average AE
OR
E2 O
3 ratio ~ 068 for ytterbium silicate ndash C
MA
S system
bull
Average AE
OR
E2 O
3 ratio ~ 022 for yttrium silicate ndash C
MA
S system
C
omposition in apatite (100 hr)
SiO2
Ahlborg and Zhu Surface amp
Coatings Technology 237 (2013) 79ndash87
RE
2 O3
AEO
Yttrium
Silicate EBC
Com
position in apatite (100 hr)
Ytterbium
Silicate EBC
ww
wnasagov
16
National Aeronautics and Space Adm
inistration
Advanced N
AS
A E
BC
Developm
ents
NA
SA advanced E
BC
systems em
phasizing high stability HfO
2 -and ZrO2 -R
E2 O
3 -
EBC layer 2 region
EB
Cs
Mol
Mol
SiO
2 EB
C system
RE
2 Si2-x O
7-2x such as (YbG
dY) 2 S
i2-x O7-2x
-Controlled dissolution and m
aintaining coating stability
(YbGdY) 2 S
i2-x O7-2x in
CM
AS
1300degC
(a)
(b)
ww
wnasagov
17
National Aeronautics and Space Adm
inistration E
xample of N
AS
A A
dvanced Environm
ental Barrier C
oating on S
iCSiC
CM
C System
s
Advanced EB
C coated vanes
HfO
2 -(YbG
dY)2 O
3
(YbG
dY)2 Si2-x O
7-2x
RESi(O
)+Hf B
ond Coat
Gd Y
b Y
O
Si
Yb
Gd Y
Si
Hf
A
lternating layered HfO
2 -Multicom
ponent Rare E
arth silicate EB
Cs used for fundam
ental stability studies
2700degF capable YbG
d-YbO+H
f based bond coats C
oated onto SiC
SiC
CM
C substrates using E
B-P
VD
The bond coat region
ww
wnasagov
18
National Aeronautics and Space Adm
inistration
CM
AS
Resistant Tests
ndash JE
Ts test of more advanced coating system
s at 2700F
Plasma sprayed (G
dY)2 Si2 O
7 2450 cycles
Special processed Yb
2 Si2 O7 spalling at 450 C
ycles EB
-PVD
(YbG
dY)2 Si2 O
7 total 4450 JETS cycles 100h
2450 4450
450
Hybrid H
f-rare earth aluminate silicate com
pleted 4450 cycles 100h
Hybrid H
ybrid Zr-rare earth silicate completed 4450
cycles 100h
2450 4450
2450 with
CM
AS 2450
ww
wnasagov
19
National Aeronautics and Space Adm
inistration
High S
tability and CM
AS
Resistance are E
nsured by Advanced H
igh M
elting Point C
oating and Multi-C
omponent C
ompositions A
rea A
Area B
ndash G
enerally improved C
MA
S
resistance of NAS
A R
ESi
System
at 1500degC 100 hr
ndash S
ilica-rich phase precipitation ndash
Rare earth elem
ent leaching into the m
elts (low concentration
~9mol
)
Surface side of the C
MA
S melts
EDS E
ww
wnasagov
20
National Aeronautics and Space Adm
inistration
Advanced E
BC
-CM
C S
ystem D
emonstrated 300 hr H
igh Cycle and
Low Fatigue D
urability in High H
eat Flux 2700degF Test Conditions
Specimen after 300 h testing
-A turbine airfoil E
BC
with H
fO2 -rare earth silicate and G
dYbSi bond coat on C
VI-M
I CM
C
substrate system selected for heat flux durability testing
-Laser high heat flux rig H
igh Cycle and Low
Cycle Fatigue test perform
ed at Stress
amplitude 10 ksi fatigue frequency 3 H
z at EB
C and 1 hr therm
al gradient cycles -
Tested EB
C surface tem
perature 1537degC (2800degF) and T bond coat tem
perature 1482degC
(2700degF) with C
MA
S
-D
emonstrated 300 hour durability at 2700degF+
-D
etermined fatigue-creep and therm
al conductivity behavior of the EB
C-C
MC
system
Specimen in rig testing
Test Condition Sum
mary
-EB
CC
VI-M
I Fatigue$loading 10 ksi (69 M
Pa) R
=005 with 1 hr Therm
al LC
F$-
TEB
C-surface 1537degC
(2800degF)$-
Tbond coat 1482degC
(2700degF)$-
Tback C
MC
surface 1250degC
(2282degF)
ww
wnasagov
21
National Aeronautics and Space Adm
inistration
Advanced E
BC
-CM
C Fatigue Test w
ith CM
AS
and in Steam
Jet Tested 300 h D
urability in High H
eat Flux Fatigue Test Conditions
-A
dvanced Hf-N
dYb silicate-N
dYbS
i bond coat EB
C coatings on 3D
architecture C
VI-P
IP S
iC-S
iC C
MC
(EB
-PV
D processing)
-Further understanding w
ater vapor -environmental interactions necessary
Surface view C
MA
S 35m
gcm2)
Back view
CM
AS
35mgcm
2)
ww
wnasagov
National Aeronautics and Space Adm
inistration
EBC
System
Designs ndash E
ffects of Com
posites and Clustered
Com
positions -
An alternating H
fO2 -and R
E-silicate coatings (EB
-PV
D processing) ndash H
fO2 -layer
infiltration and rare earth silicate layer melting
EB
-PV
D P
rocessed EB
Cs alternating H
fO2 -rich and ytterbium
silicate layer systems for
CM
AS
and impact resistance
ww
wnasagov
National Aeronautics and Space Adm
inistration
Sum
mary
bullC
MA
S degradation rem
ains a challenge for emerging turbine engine
environmental barrier coating ndash S
iCSiC
CM
C com
ponent systems
bullC
MA
S leads to low
er melting point of E
BC and bond coat system
s with
accelerated EBC
and CM
C degradations
bullN
AS
A advanced E
BC com
positions showed som
e promise for C
MA
S
resistance at temperatures up to 1500degC
in high velocity high heat flux and m
echanical loading tests bull
Currently focus on better understanding of E
BC com
positions and EBC
-CM
AS
interactions particularly with hafnium
zirconium and rare
earth silicates for improved tem
perature capability and CM
AS
resistance bull
Also standardize C
MA
S testing and quantify C
MA
S induced life debits
helping validate life modeling
bullC
ontrolling the compositions for C
MA
S resistance w
hile maintaining
high toughness continued to be a key emphasis
ww
wnasagov
24
National Aeronautics and Space Adm
inistration
Acknow
ledgements
bullThe w
ork was supported by N
ASA Fundam
ental Aeronautics Program (FAP)
Transformational Tools and Technologies (TTT) Project
bullThe authors are grateful to D
r Michael H
elminiak in the assistant of JETS tests
ww
wnasagov
25
National Aeronautics and Space Adm
inistration
CM
AS
Reaction K
inetics in Bond C
oats ndash S
iO2 rich phase partitioning in the C
MA
S m
elts ndash R
are earth content leaching low even at 1500degC
ndash M
ore advanced compositions are being im
plemented for im
proved thermom
echanical ndash
CM
AS Partitioning on R
E-Si bond coat 1500degC
100hr
RE incorporations
CM
AS
resistance
ww
wnasagov
26
National Aeronautics and Space Adm
inistration Strength R
esults of Selected EBC and EBC
Bond Coats
-CM
AS
Reaction R
esulted in Strength Reduction in Silicates
Selected E
BC
systems
ndashH
fO2 -R
E-S
i along with co-doped rare earth silicates and rare earth alum
ino-silicates for optim
ized strength stability and temperature capability
ndashC
MA
S infiltrations can reduce the strength
350 646-Specially alloy toughened t like H
fO2
648-EBC Bond Coat Constituent 300
659-AE9762
150
EBC
s
EBC
s
HfO
2 -Si (Si-rich)
Yb
2 Si 2 O 7
250658-EBC H
fO2-Rare Earth-A
lumino Silicate
660-Y2Si2O
7657-Zr-RE silicate 669-Y
b2Si2O7
Strength MPa
200696-EBC Bond Coat Constituent
100681-H
fO2-Si
669-9762 with CM
AS 1350C 50hr reacted
693-HfO
2-Si with CM
AS 1350C 50hr reacted
5000
200 400
600 800
1000 1200
1400 1600
Temperature degC
Strength test data compared
Yb
2 Si2 O7 C
MA
S reacted tensile Y
b2 Si2 O
7 CM
AS reacted
specimen fracture surface
surface w
ww
nasagov 27
National Aeronautics and Space Adm
inistration
High Stability and C
MAS R
esistance Observed from
the Rare
Earth S
ilicon High M
elting Point C
oating Com
positions
ndashD
emonstrated C
MA
S resistance
of NAS
A R
E-Si S
ystem at
1500degC 100 hr
ndash S
ilica-rich phase precipitation ndash
Rare earth elem
ent leaching into the m
elts (low concentration ~9
Surface side of the m
ol)
CM
AS m
elts
Area A
Area B
ww
wnasagov
28
![Page 6: Hurst, Bernadette J. Puleo€¦ · G57, 40.00 mg CMAS SiO Wellman -Aygun Smialek Braue 0 49 mole%; such as NASA’s CMAS (with NiO DSC:020 OES Measured by EDS [#] Type Date/time :](https://reader033.fdocuments.us/reader033/viewer/2022060211/5f04cb127e708231d40fbc15/html5/thumbnails/6.jpg)
National Aeronautics and Space Adm
inistration
Calcium
Magnesium
Alumino-Silicate (C
MAS) System
s Used
in Laboratory Tests -Continued
minus
NA
SA
modified version (N
AS
A C
MA
S)
minus
CM
AS
SiO
2 content typically ranging from 43-49 m
ole such as N
ASArsquos CMAS (with N
iO
and FeO)
NA
SA
CM
AS
Com
positions
NA
SA m
odified CM
AS
AR
FL PTI CM
AS 02
(higher SiO2 )
GEB
orom
Wellm
an
Kram
er
Aygun Smialek
Rai
Braue
Method
Content (m
ol)
CaO
M
gO
Al2 O3
SiO2
Fe2 O
3 N
iO
(DesignedTargeted)
338 90
67 460
30 15
Measured by IC
P-O
ES 38 r 2
90 r 05 69 r 03
41 r 2 38 r 02
137 r 007
Measured by ED
S 36 r 1
84 r 03 75 r 02
43 r 1 39 r 01
15 r 01
Created w
ith NE
TZSC
H P
roteus software
[] Type [11] D
ynamic
Range
2550(Km
in)1500 A
cqRate
7500 S
TC
0 P
1N2O
2 500
Corr
DS
C020
[] Type [13] D
ynamic
Range
150050(Km
in)25 A
cqRate
7500 S
TC
0 P
1N2O
2 500
Corr
DS
C020
Project
Identity D
atetime
Laboratory O
perator S
ample
G57
6282016 91511 AM
G
lenn Research C
enter C
osta G
57 4000 mg
Reference
Material
Corrtem
pcal S
ensfile S
ample carTC
M
odetype of meas R
ef Al2O
30 mg
baseline for YS
Z 5 C_m
in up tp 1500 C 06-24-16bd8 TC
ALZE
RO
TMX
sensitivity from
sapphire_Pt crucible 1500C
air 01-06-16ed8 D
SC
Cp S
S
DS
C sam
ple with correction
Segm
ents C
rucible A
tmosphere
M range
3 DS
CTG
pan Pt
N2O
2 500mlm
in 5000 microV
Instrument N
ETZS
CH
DS
C 404F1 File C
NE
TZSC
HP
roteusdata5CostaS
amplesG
62dd8 Rem
ark Third DS
C run since O
ct 2014 1x evacbackfill
200 400
600 800
1000 1200
1400 Tem
perature degC
-10
-08
-06
-04
-02
00
02
04
DS
C (m
Wm
g)
0 50
100
150
200
250
Flow (m
lmin)
Main
exo
DSC
traces of CM
AS during heating and cooling up
to 1500 qC at 5 qC
min
ww
wnasagov
6
National Aeronautics and Space Adm
inistration
Advanced N
AS
A E
BC
Developm
ents
Improved tem
perature capability sintering phase stability recession resistance and high tem
perature strength
Advanced com
positions amp processing for com
bined therm
omechanical loading and environm
ents higher stability and increased toughness tow
ards prime-reliant
Gen I (E
PM)
RampD
Award
Gen II (U
EET)
2000-2004 Advanced EBC
(U
EET) 2000-2005 R
ampD Aw
ard (2007)
Advanced EBC (FAP)
2005-2011 R
ampD Aw
ard (2007) coating turbine developm
ent
Advanced EBC
(FAP -ERA)
2007 -present
Advanced (FAP ERA)
Patent13923450 PC
TUS1346946 and subsequent patents
Engine C
omponents
Com
bustor C
ombustor
(Vane) C
ombustor
Vane Vane Blade
-VaneBlade EB
Cs
-Equivalent APS com
bustor EBC
s
Airfoil components
Top Coat
BSAS (APS) R
E2 Si2 O
7 or R
E2 SiO
5 (APS)
-(HfY
bGdY
) 2 O3
-ZrO2 H
fO2 +R
E
silicates -ZrO
2 HfO
2 +BS
AS
(APS and EBPVD
)
RE-H
fO2 -Alum
ino silicate
(APS andor 100
EB-
PVD)
RE-H
fO2 -X
advanced top coat R
E-HfO
2 Silica (EB
-PVD etc vapor
deposition)
Advanced EBC
s
Interlayer --
--R
E-HfO
2 ZrO2 -
aluminosilicate
layered systems
Nanocom
posite graded oxidesilicate
--
EBC
M
ullite+ BSAS R
E2 Si2 O
7 and or BSAS+M
ullite
RE
silicates or R
E-Hf m
ullite R
E doped m
ullite-HfO
2 or R
E silicates
Multi-com
ponent R
E silicate systems
Multicom
ponent R
E-silicate + Hf self
grown
Bond C
oat Si
Si O
xide+Si bond coat
HfO
2 -Si-X
doped mulliteSi
SiC nanotube
Optim
ized HfO
2 -Si-X bond coat 2700degF bond coats
RE-Si+H
f systems
Thickness 10-15 m
il 10-15 m
il 15-20 m
il 10 m
il 5 m
il 1 -3 m
ils
Surface T U
p to 2400degF 2400degF
3000degF2400CM
C
2700degF2400F CM
C
2700-3000degF
Bond Coat T
Limited to
2462degF Lim
it to 2462degF
Limit to 2642degF
Proven at 2600degF + Advancem
ents targeting 2700degF
2700degF
Challenges overcom
e by advancem
ents
ww
wnasagov
7
National Aeronautics and Space Adm
inistration
CM
AS
Related D
egradations in EBC
s
Cross-section
50 mm
minus C
MAS effects
bull S
ignificantly reduce melting points of the E
BC
s and bond coats bull
More detrim
ental effects with thin airfoil E
BC
s bull
CM
AS
weakens the coating system
s reducing strength and toughness bullM
AS
increase EB
C diffusivities and perm
eability thus less protective as an environmental
barrier bullC
MA
S interactions w
ith heat flux thermal cycling erosion and therm
omechanical fatigue
Reaction layer spallations
Accelerated C
MC
failure when C
MA
S intact w
ith CM
Cs
Such as yttrium silicate
Coating
surface
EB
C and degradations
CM
AS induced m
elting and failure$w
ww
nasagov 8
National Aeronautics and Space Adm
inistration
CM
AS R
elated Degradations in E
BCs -C
ontinued minus
CM
AS effects on EBC
temperature capability
bull S
ilicate reactions with N
aO2 and A
l2 O3 silicate
Phase diagram
s showing yttrium
di-silicate reactions w
ith SiO
2 NaO
and Al2 O
3
ww
wnasagov
9
National Aeronautics and Space Adm
inistration
CM
AS R
elated Degradations in E
BCs -C
ontinued minus
CM
AS effects on EBC
temperature capability
bullRare earths generally have lim
ited temperature capability below
1500degC in the R
E2 O
3 -A
l2 O3 -S
iO2 based system
s bull
Sm
aller ionic size RE
s have higher melting points
Solidus temperature in Ln
2 Si2 O7 -A
l6 Si2 O13 -
SiO2 system
as function of ionic radius
Y Murakam
i and H Yam
amoto J C
eram Soc Jpn 101 [10] 1101-1106 (1993)
ww
wnasagov
10
National Aeronautics and Space Adm
inistration
Rare Earth D
issolutions in CM
AS Melts
ZrO2 -30Y
2 O3 -15Sm
2 O3 -15Yb
2 O3
ZrO2 -30Y
2 O3 -15N
d2 O
3 -15Yb2 O
3 -03Sc2 O
3
ZrO2 -96Y
2 O3 -22G
d2 O
3 -21Yb2 O
3
Ionic potential trend of RE
Radius size trend of RE
minus Large ionic size rare earths show
ed higher concentration dissolutions in the CM
AS
m
elt for ZrO2 -R
E2 O
3 oxide systems
ZrO2 -R
EO15 -H
f more endotherm
ic
Gustavo and Zhu International C
onference on Advanced C
eramics and C
omposites 2016
ww
wnasagov
11
Front CM
AS side
National Aeronautics and Space Adm
inistration
CM
AS Related D
egradations in EBC
coated CM
Cs ndash
Laboratory Heat Flux Tests
minusC
MAS effects on EB
C-C
MC
temperature capability tested in laser high heat
flux creep-rupture rig bull
Accelerated failure of C
MC
in loading high heat flux conditions
EBC
coated CV
I-MI C
MC
with N
dYb silicate R
ESi bond coat tested Tsurface 2600degF TC
MC
2450degF
Front heated CM
AS
side B
ack cooled side
Creep strain
Time h
Front CM
AS
side
200h
05
ww
wnasagov
12
National Aeronautics and Space Adm
inistration
EBC
CM
AS
Surface Initial N
ucleation Dissolution R
eactions ndash
Ytterbium
-and yttrium-silicate silicates reactions and dissolutions in C
AM
S
ndash M
ore sluggish dissolution of ytterbium as com
pared to yttrium
Ytterbium
di-silicate surface CM
AS m
elts 50 Y
tterbium di-silicate surface C
MA
S melts 5 h
h 1300degC
1500degC$
Yttrium
mono-silicate surface C
MA
S Y
ttrium silicate surface C
MA
S melts 5 h
melts 50 h 1300degC
1500degC
A
hlborg and Zhu Surface amp C
oatings Technology 237 (2013) 79ndash87 w
ww
nasagov 13
National Aeronautics and Space Adm
inistration
Rare E
arth Apatite G
rain Grow
th ndash
Grain grow
th of apatite phase at 1500degC at various tim
es
Ytterbium
silicate system
50 hr 150 hr
200 hr
200 hr50 hr
150 hr
Yttrium
silicate system$
ww
wnasagov
14
National Aeronautics and Space Adm
inistration
Effect of C
MA
S R
eactions on Grain B
oundary Phases
ndash C
MA
S and grain boundary phase has higher A
l2 O3
content (17-22 mole
) bull
Eutectic region w
ith high Al2 O
3 content ~1200degC m
elting point bull
Loss of SiO
2 due to volatility
200 hr 1500degC
NA
SA
modified
CM
AS
Grain
boundary final phase ndash low
SiO
2 and high A
lumina
ww
wnasagov
15
National Aeronautics and Space Adm
inistration
Rare E
arth Dissolution in C
MA
S M
elts ndash
Non stoichiom
etric characteristics of the CM
AS
ndash rare earth silicate reacted apatite phases ndash up to 200 h testing
ndash D
ifference in partitioning of ytterbium vs yttrium
in apatite bull
Average AE
OR
E2 O
3 ratio ~ 068 for ytterbium silicate ndash C
MA
S system
bull
Average AE
OR
E2 O
3 ratio ~ 022 for yttrium silicate ndash C
MA
S system
C
omposition in apatite (100 hr)
SiO2
Ahlborg and Zhu Surface amp
Coatings Technology 237 (2013) 79ndash87
RE
2 O3
AEO
Yttrium
Silicate EBC
Com
position in apatite (100 hr)
Ytterbium
Silicate EBC
ww
wnasagov
16
National Aeronautics and Space Adm
inistration
Advanced N
AS
A E
BC
Developm
ents
NA
SA advanced E
BC
systems em
phasizing high stability HfO
2 -and ZrO2 -R
E2 O
3 -
EBC layer 2 region
EB
Cs
Mol
Mol
SiO
2 EB
C system
RE
2 Si2-x O
7-2x such as (YbG
dY) 2 S
i2-x O7-2x
-Controlled dissolution and m
aintaining coating stability
(YbGdY) 2 S
i2-x O7-2x in
CM
AS
1300degC
(a)
(b)
ww
wnasagov
17
National Aeronautics and Space Adm
inistration E
xample of N
AS
A A
dvanced Environm
ental Barrier C
oating on S
iCSiC
CM
C System
s
Advanced EB
C coated vanes
HfO
2 -(YbG
dY)2 O
3
(YbG
dY)2 Si2-x O
7-2x
RESi(O
)+Hf B
ond Coat
Gd Y
b Y
O
Si
Yb
Gd Y
Si
Hf
A
lternating layered HfO
2 -Multicom
ponent Rare E
arth silicate EB
Cs used for fundam
ental stability studies
2700degF capable YbG
d-YbO+H
f based bond coats C
oated onto SiC
SiC
CM
C substrates using E
B-P
VD
The bond coat region
ww
wnasagov
18
National Aeronautics and Space Adm
inistration
CM
AS
Resistant Tests
ndash JE
Ts test of more advanced coating system
s at 2700F
Plasma sprayed (G
dY)2 Si2 O
7 2450 cycles
Special processed Yb
2 Si2 O7 spalling at 450 C
ycles EB
-PVD
(YbG
dY)2 Si2 O
7 total 4450 JETS cycles 100h
2450 4450
450
Hybrid H
f-rare earth aluminate silicate com
pleted 4450 cycles 100h
Hybrid H
ybrid Zr-rare earth silicate completed 4450
cycles 100h
2450 4450
2450 with
CM
AS 2450
ww
wnasagov
19
National Aeronautics and Space Adm
inistration
High S
tability and CM
AS
Resistance are E
nsured by Advanced H
igh M
elting Point C
oating and Multi-C
omponent C
ompositions A
rea A
Area B
ndash G
enerally improved C
MA
S
resistance of NAS
A R
ESi
System
at 1500degC 100 hr
ndash S
ilica-rich phase precipitation ndash
Rare earth elem
ent leaching into the m
elts (low concentration
~9mol
)
Surface side of the C
MA
S melts
EDS E
ww
wnasagov
20
National Aeronautics and Space Adm
inistration
Advanced E
BC
-CM
C S
ystem D
emonstrated 300 hr H
igh Cycle and
Low Fatigue D
urability in High H
eat Flux 2700degF Test Conditions
Specimen after 300 h testing
-A turbine airfoil E
BC
with H
fO2 -rare earth silicate and G
dYbSi bond coat on C
VI-M
I CM
C
substrate system selected for heat flux durability testing
-Laser high heat flux rig H
igh Cycle and Low
Cycle Fatigue test perform
ed at Stress
amplitude 10 ksi fatigue frequency 3 H
z at EB
C and 1 hr therm
al gradient cycles -
Tested EB
C surface tem
perature 1537degC (2800degF) and T bond coat tem
perature 1482degC
(2700degF) with C
MA
S
-D
emonstrated 300 hour durability at 2700degF+
-D
etermined fatigue-creep and therm
al conductivity behavior of the EB
C-C
MC
system
Specimen in rig testing
Test Condition Sum
mary
-EB
CC
VI-M
I Fatigue$loading 10 ksi (69 M
Pa) R
=005 with 1 hr Therm
al LC
F$-
TEB
C-surface 1537degC
(2800degF)$-
Tbond coat 1482degC
(2700degF)$-
Tback C
MC
surface 1250degC
(2282degF)
ww
wnasagov
21
National Aeronautics and Space Adm
inistration
Advanced E
BC
-CM
C Fatigue Test w
ith CM
AS
and in Steam
Jet Tested 300 h D
urability in High H
eat Flux Fatigue Test Conditions
-A
dvanced Hf-N
dYb silicate-N
dYbS
i bond coat EB
C coatings on 3D
architecture C
VI-P
IP S
iC-S
iC C
MC
(EB
-PV
D processing)
-Further understanding w
ater vapor -environmental interactions necessary
Surface view C
MA
S 35m
gcm2)
Back view
CM
AS
35mgcm
2)
ww
wnasagov
National Aeronautics and Space Adm
inistration
EBC
System
Designs ndash E
ffects of Com
posites and Clustered
Com
positions -
An alternating H
fO2 -and R
E-silicate coatings (EB
-PV
D processing) ndash H
fO2 -layer
infiltration and rare earth silicate layer melting
EB
-PV
D P
rocessed EB
Cs alternating H
fO2 -rich and ytterbium
silicate layer systems for
CM
AS
and impact resistance
ww
wnasagov
National Aeronautics and Space Adm
inistration
Sum
mary
bullC
MA
S degradation rem
ains a challenge for emerging turbine engine
environmental barrier coating ndash S
iCSiC
CM
C com
ponent systems
bullC
MA
S leads to low
er melting point of E
BC and bond coat system
s with
accelerated EBC
and CM
C degradations
bullN
AS
A advanced E
BC com
positions showed som
e promise for C
MA
S
resistance at temperatures up to 1500degC
in high velocity high heat flux and m
echanical loading tests bull
Currently focus on better understanding of E
BC com
positions and EBC
-CM
AS
interactions particularly with hafnium
zirconium and rare
earth silicates for improved tem
perature capability and CM
AS
resistance bull
Also standardize C
MA
S testing and quantify C
MA
S induced life debits
helping validate life modeling
bullC
ontrolling the compositions for C
MA
S resistance w
hile maintaining
high toughness continued to be a key emphasis
ww
wnasagov
24
National Aeronautics and Space Adm
inistration
Acknow
ledgements
bullThe w
ork was supported by N
ASA Fundam
ental Aeronautics Program (FAP)
Transformational Tools and Technologies (TTT) Project
bullThe authors are grateful to D
r Michael H
elminiak in the assistant of JETS tests
ww
wnasagov
25
National Aeronautics and Space Adm
inistration
CM
AS
Reaction K
inetics in Bond C
oats ndash S
iO2 rich phase partitioning in the C
MA
S m
elts ndash R
are earth content leaching low even at 1500degC
ndash M
ore advanced compositions are being im
plemented for im
proved thermom
echanical ndash
CM
AS Partitioning on R
E-Si bond coat 1500degC
100hr
RE incorporations
CM
AS
resistance
ww
wnasagov
26
National Aeronautics and Space Adm
inistration Strength R
esults of Selected EBC and EBC
Bond Coats
-CM
AS
Reaction R
esulted in Strength Reduction in Silicates
Selected E
BC
systems
ndashH
fO2 -R
E-S
i along with co-doped rare earth silicates and rare earth alum
ino-silicates for optim
ized strength stability and temperature capability
ndashC
MA
S infiltrations can reduce the strength
350 646-Specially alloy toughened t like H
fO2
648-EBC Bond Coat Constituent 300
659-AE9762
150
EBC
s
EBC
s
HfO
2 -Si (Si-rich)
Yb
2 Si 2 O 7
250658-EBC H
fO2-Rare Earth-A
lumino Silicate
660-Y2Si2O
7657-Zr-RE silicate 669-Y
b2Si2O7
Strength MPa
200696-EBC Bond Coat Constituent
100681-H
fO2-Si
669-9762 with CM
AS 1350C 50hr reacted
693-HfO
2-Si with CM
AS 1350C 50hr reacted
5000
200 400
600 800
1000 1200
1400 1600
Temperature degC
Strength test data compared
Yb
2 Si2 O7 C
MA
S reacted tensile Y
b2 Si2 O
7 CM
AS reacted
specimen fracture surface
surface w
ww
nasagov 27
National Aeronautics and Space Adm
inistration
High Stability and C
MAS R
esistance Observed from
the Rare
Earth S
ilicon High M
elting Point C
oating Com
positions
ndashD
emonstrated C
MA
S resistance
of NAS
A R
E-Si S
ystem at
1500degC 100 hr
ndash S
ilica-rich phase precipitation ndash
Rare earth elem
ent leaching into the m
elts (low concentration ~9
Surface side of the m
ol)
CM
AS m
elts
Area A
Area B
ww
wnasagov
28
![Page 7: Hurst, Bernadette J. Puleo€¦ · G57, 40.00 mg CMAS SiO Wellman -Aygun Smialek Braue 0 49 mole%; such as NASA’s CMAS (with NiO DSC:020 OES Measured by EDS [#] Type Date/time :](https://reader033.fdocuments.us/reader033/viewer/2022060211/5f04cb127e708231d40fbc15/html5/thumbnails/7.jpg)
National Aeronautics and Space Adm
inistration
Advanced N
AS
A E
BC
Developm
ents
Improved tem
perature capability sintering phase stability recession resistance and high tem
perature strength
Advanced com
positions amp processing for com
bined therm
omechanical loading and environm
ents higher stability and increased toughness tow
ards prime-reliant
Gen I (E
PM)
RampD
Award
Gen II (U
EET)
2000-2004 Advanced EBC
(U
EET) 2000-2005 R
ampD Aw
ard (2007)
Advanced EBC (FAP)
2005-2011 R
ampD Aw
ard (2007) coating turbine developm
ent
Advanced EBC
(FAP -ERA)
2007 -present
Advanced (FAP ERA)
Patent13923450 PC
TUS1346946 and subsequent patents
Engine C
omponents
Com
bustor C
ombustor
(Vane) C
ombustor
Vane Vane Blade
-VaneBlade EB
Cs
-Equivalent APS com
bustor EBC
s
Airfoil components
Top Coat
BSAS (APS) R
E2 Si2 O
7 or R
E2 SiO
5 (APS)
-(HfY
bGdY
) 2 O3
-ZrO2 H
fO2 +R
E
silicates -ZrO
2 HfO
2 +BS
AS
(APS and EBPVD
)
RE-H
fO2 -Alum
ino silicate
(APS andor 100
EB-
PVD)
RE-H
fO2 -X
advanced top coat R
E-HfO
2 Silica (EB
-PVD etc vapor
deposition)
Advanced EBC
s
Interlayer --
--R
E-HfO
2 ZrO2 -
aluminosilicate
layered systems
Nanocom
posite graded oxidesilicate
--
EBC
M
ullite+ BSAS R
E2 Si2 O
7 and or BSAS+M
ullite
RE
silicates or R
E-Hf m
ullite R
E doped m
ullite-HfO
2 or R
E silicates
Multi-com
ponent R
E silicate systems
Multicom
ponent R
E-silicate + Hf self
grown
Bond C
oat Si
Si O
xide+Si bond coat
HfO
2 -Si-X
doped mulliteSi
SiC nanotube
Optim
ized HfO
2 -Si-X bond coat 2700degF bond coats
RE-Si+H
f systems
Thickness 10-15 m
il 10-15 m
il 15-20 m
il 10 m
il 5 m
il 1 -3 m
ils
Surface T U
p to 2400degF 2400degF
3000degF2400CM
C
2700degF2400F CM
C
2700-3000degF
Bond Coat T
Limited to
2462degF Lim
it to 2462degF
Limit to 2642degF
Proven at 2600degF + Advancem
ents targeting 2700degF
2700degF
Challenges overcom
e by advancem
ents
ww
wnasagov
7
National Aeronautics and Space Adm
inistration
CM
AS
Related D
egradations in EBC
s
Cross-section
50 mm
minus C
MAS effects
bull S
ignificantly reduce melting points of the E
BC
s and bond coats bull
More detrim
ental effects with thin airfoil E
BC
s bull
CM
AS
weakens the coating system
s reducing strength and toughness bullM
AS
increase EB
C diffusivities and perm
eability thus less protective as an environmental
barrier bullC
MA
S interactions w
ith heat flux thermal cycling erosion and therm
omechanical fatigue
Reaction layer spallations
Accelerated C
MC
failure when C
MA
S intact w
ith CM
Cs
Such as yttrium silicate
Coating
surface
EB
C and degradations
CM
AS induced m
elting and failure$w
ww
nasagov 8
National Aeronautics and Space Adm
inistration
CM
AS R
elated Degradations in E
BCs -C
ontinued minus
CM
AS effects on EBC
temperature capability
bull S
ilicate reactions with N
aO2 and A
l2 O3 silicate
Phase diagram
s showing yttrium
di-silicate reactions w
ith SiO
2 NaO
and Al2 O
3
ww
wnasagov
9
National Aeronautics and Space Adm
inistration
CM
AS R
elated Degradations in E
BCs -C
ontinued minus
CM
AS effects on EBC
temperature capability
bullRare earths generally have lim
ited temperature capability below
1500degC in the R
E2 O
3 -A
l2 O3 -S
iO2 based system
s bull
Sm
aller ionic size RE
s have higher melting points
Solidus temperature in Ln
2 Si2 O7 -A
l6 Si2 O13 -
SiO2 system
as function of ionic radius
Y Murakam
i and H Yam
amoto J C
eram Soc Jpn 101 [10] 1101-1106 (1993)
ww
wnasagov
10
National Aeronautics and Space Adm
inistration
Rare Earth D
issolutions in CM
AS Melts
ZrO2 -30Y
2 O3 -15Sm
2 O3 -15Yb
2 O3
ZrO2 -30Y
2 O3 -15N
d2 O
3 -15Yb2 O
3 -03Sc2 O
3
ZrO2 -96Y
2 O3 -22G
d2 O
3 -21Yb2 O
3
Ionic potential trend of RE
Radius size trend of RE
minus Large ionic size rare earths show
ed higher concentration dissolutions in the CM
AS
m
elt for ZrO2 -R
E2 O
3 oxide systems
ZrO2 -R
EO15 -H
f more endotherm
ic
Gustavo and Zhu International C
onference on Advanced C
eramics and C
omposites 2016
ww
wnasagov
11
Front CM
AS side
National Aeronautics and Space Adm
inistration
CM
AS Related D
egradations in EBC
coated CM
Cs ndash
Laboratory Heat Flux Tests
minusC
MAS effects on EB
C-C
MC
temperature capability tested in laser high heat
flux creep-rupture rig bull
Accelerated failure of C
MC
in loading high heat flux conditions
EBC
coated CV
I-MI C
MC
with N
dYb silicate R
ESi bond coat tested Tsurface 2600degF TC
MC
2450degF
Front heated CM
AS
side B
ack cooled side
Creep strain
Time h
Front CM
AS
side
200h
05
ww
wnasagov
12
National Aeronautics and Space Adm
inistration
EBC
CM
AS
Surface Initial N
ucleation Dissolution R
eactions ndash
Ytterbium
-and yttrium-silicate silicates reactions and dissolutions in C
AM
S
ndash M
ore sluggish dissolution of ytterbium as com
pared to yttrium
Ytterbium
di-silicate surface CM
AS m
elts 50 Y
tterbium di-silicate surface C
MA
S melts 5 h
h 1300degC
1500degC$
Yttrium
mono-silicate surface C
MA
S Y
ttrium silicate surface C
MA
S melts 5 h
melts 50 h 1300degC
1500degC
A
hlborg and Zhu Surface amp C
oatings Technology 237 (2013) 79ndash87 w
ww
nasagov 13
National Aeronautics and Space Adm
inistration
Rare E
arth Apatite G
rain Grow
th ndash
Grain grow
th of apatite phase at 1500degC at various tim
es
Ytterbium
silicate system
50 hr 150 hr
200 hr
200 hr50 hr
150 hr
Yttrium
silicate system$
ww
wnasagov
14
National Aeronautics and Space Adm
inistration
Effect of C
MA
S R
eactions on Grain B
oundary Phases
ndash C
MA
S and grain boundary phase has higher A
l2 O3
content (17-22 mole
) bull
Eutectic region w
ith high Al2 O
3 content ~1200degC m
elting point bull
Loss of SiO
2 due to volatility
200 hr 1500degC
NA
SA
modified
CM
AS
Grain
boundary final phase ndash low
SiO
2 and high A
lumina
ww
wnasagov
15
National Aeronautics and Space Adm
inistration
Rare E
arth Dissolution in C
MA
S M
elts ndash
Non stoichiom
etric characteristics of the CM
AS
ndash rare earth silicate reacted apatite phases ndash up to 200 h testing
ndash D
ifference in partitioning of ytterbium vs yttrium
in apatite bull
Average AE
OR
E2 O
3 ratio ~ 068 for ytterbium silicate ndash C
MA
S system
bull
Average AE
OR
E2 O
3 ratio ~ 022 for yttrium silicate ndash C
MA
S system
C
omposition in apatite (100 hr)
SiO2
Ahlborg and Zhu Surface amp
Coatings Technology 237 (2013) 79ndash87
RE
2 O3
AEO
Yttrium
Silicate EBC
Com
position in apatite (100 hr)
Ytterbium
Silicate EBC
ww
wnasagov
16
National Aeronautics and Space Adm
inistration
Advanced N
AS
A E
BC
Developm
ents
NA
SA advanced E
BC
systems em
phasizing high stability HfO
2 -and ZrO2 -R
E2 O
3 -
EBC layer 2 region
EB
Cs
Mol
Mol
SiO
2 EB
C system
RE
2 Si2-x O
7-2x such as (YbG
dY) 2 S
i2-x O7-2x
-Controlled dissolution and m
aintaining coating stability
(YbGdY) 2 S
i2-x O7-2x in
CM
AS
1300degC
(a)
(b)
ww
wnasagov
17
National Aeronautics and Space Adm
inistration E
xample of N
AS
A A
dvanced Environm
ental Barrier C
oating on S
iCSiC
CM
C System
s
Advanced EB
C coated vanes
HfO
2 -(YbG
dY)2 O
3
(YbG
dY)2 Si2-x O
7-2x
RESi(O
)+Hf B
ond Coat
Gd Y
b Y
O
Si
Yb
Gd Y
Si
Hf
A
lternating layered HfO
2 -Multicom
ponent Rare E
arth silicate EB
Cs used for fundam
ental stability studies
2700degF capable YbG
d-YbO+H
f based bond coats C
oated onto SiC
SiC
CM
C substrates using E
B-P
VD
The bond coat region
ww
wnasagov
18
National Aeronautics and Space Adm
inistration
CM
AS
Resistant Tests
ndash JE
Ts test of more advanced coating system
s at 2700F
Plasma sprayed (G
dY)2 Si2 O
7 2450 cycles
Special processed Yb
2 Si2 O7 spalling at 450 C
ycles EB
-PVD
(YbG
dY)2 Si2 O
7 total 4450 JETS cycles 100h
2450 4450
450
Hybrid H
f-rare earth aluminate silicate com
pleted 4450 cycles 100h
Hybrid H
ybrid Zr-rare earth silicate completed 4450
cycles 100h
2450 4450
2450 with
CM
AS 2450
ww
wnasagov
19
National Aeronautics and Space Adm
inistration
High S
tability and CM
AS
Resistance are E
nsured by Advanced H
igh M
elting Point C
oating and Multi-C
omponent C
ompositions A
rea A
Area B
ndash G
enerally improved C
MA
S
resistance of NAS
A R
ESi
System
at 1500degC 100 hr
ndash S
ilica-rich phase precipitation ndash
Rare earth elem
ent leaching into the m
elts (low concentration
~9mol
)
Surface side of the C
MA
S melts
EDS E
ww
wnasagov
20
National Aeronautics and Space Adm
inistration
Advanced E
BC
-CM
C S
ystem D
emonstrated 300 hr H
igh Cycle and
Low Fatigue D
urability in High H
eat Flux 2700degF Test Conditions
Specimen after 300 h testing
-A turbine airfoil E
BC
with H
fO2 -rare earth silicate and G
dYbSi bond coat on C
VI-M
I CM
C
substrate system selected for heat flux durability testing
-Laser high heat flux rig H
igh Cycle and Low
Cycle Fatigue test perform
ed at Stress
amplitude 10 ksi fatigue frequency 3 H
z at EB
C and 1 hr therm
al gradient cycles -
Tested EB
C surface tem
perature 1537degC (2800degF) and T bond coat tem
perature 1482degC
(2700degF) with C
MA
S
-D
emonstrated 300 hour durability at 2700degF+
-D
etermined fatigue-creep and therm
al conductivity behavior of the EB
C-C
MC
system
Specimen in rig testing
Test Condition Sum
mary
-EB
CC
VI-M
I Fatigue$loading 10 ksi (69 M
Pa) R
=005 with 1 hr Therm
al LC
F$-
TEB
C-surface 1537degC
(2800degF)$-
Tbond coat 1482degC
(2700degF)$-
Tback C
MC
surface 1250degC
(2282degF)
ww
wnasagov
21
National Aeronautics and Space Adm
inistration
Advanced E
BC
-CM
C Fatigue Test w
ith CM
AS
and in Steam
Jet Tested 300 h D
urability in High H
eat Flux Fatigue Test Conditions
-A
dvanced Hf-N
dYb silicate-N
dYbS
i bond coat EB
C coatings on 3D
architecture C
VI-P
IP S
iC-S
iC C
MC
(EB
-PV
D processing)
-Further understanding w
ater vapor -environmental interactions necessary
Surface view C
MA
S 35m
gcm2)
Back view
CM
AS
35mgcm
2)
ww
wnasagov
National Aeronautics and Space Adm
inistration
EBC
System
Designs ndash E
ffects of Com
posites and Clustered
Com
positions -
An alternating H
fO2 -and R
E-silicate coatings (EB
-PV
D processing) ndash H
fO2 -layer
infiltration and rare earth silicate layer melting
EB
-PV
D P
rocessed EB
Cs alternating H
fO2 -rich and ytterbium
silicate layer systems for
CM
AS
and impact resistance
ww
wnasagov
National Aeronautics and Space Adm
inistration
Sum
mary
bullC
MA
S degradation rem
ains a challenge for emerging turbine engine
environmental barrier coating ndash S
iCSiC
CM
C com
ponent systems
bullC
MA
S leads to low
er melting point of E
BC and bond coat system
s with
accelerated EBC
and CM
C degradations
bullN
AS
A advanced E
BC com
positions showed som
e promise for C
MA
S
resistance at temperatures up to 1500degC
in high velocity high heat flux and m
echanical loading tests bull
Currently focus on better understanding of E
BC com
positions and EBC
-CM
AS
interactions particularly with hafnium
zirconium and rare
earth silicates for improved tem
perature capability and CM
AS
resistance bull
Also standardize C
MA
S testing and quantify C
MA
S induced life debits
helping validate life modeling
bullC
ontrolling the compositions for C
MA
S resistance w
hile maintaining
high toughness continued to be a key emphasis
ww
wnasagov
24
National Aeronautics and Space Adm
inistration
Acknow
ledgements
bullThe w
ork was supported by N
ASA Fundam
ental Aeronautics Program (FAP)
Transformational Tools and Technologies (TTT) Project
bullThe authors are grateful to D
r Michael H
elminiak in the assistant of JETS tests
ww
wnasagov
25
National Aeronautics and Space Adm
inistration
CM
AS
Reaction K
inetics in Bond C
oats ndash S
iO2 rich phase partitioning in the C
MA
S m
elts ndash R
are earth content leaching low even at 1500degC
ndash M
ore advanced compositions are being im
plemented for im
proved thermom
echanical ndash
CM
AS Partitioning on R
E-Si bond coat 1500degC
100hr
RE incorporations
CM
AS
resistance
ww
wnasagov
26
National Aeronautics and Space Adm
inistration Strength R
esults of Selected EBC and EBC
Bond Coats
-CM
AS
Reaction R
esulted in Strength Reduction in Silicates
Selected E
BC
systems
ndashH
fO2 -R
E-S
i along with co-doped rare earth silicates and rare earth alum
ino-silicates for optim
ized strength stability and temperature capability
ndashC
MA
S infiltrations can reduce the strength
350 646-Specially alloy toughened t like H
fO2
648-EBC Bond Coat Constituent 300
659-AE9762
150
EBC
s
EBC
s
HfO
2 -Si (Si-rich)
Yb
2 Si 2 O 7
250658-EBC H
fO2-Rare Earth-A
lumino Silicate
660-Y2Si2O
7657-Zr-RE silicate 669-Y
b2Si2O7
Strength MPa
200696-EBC Bond Coat Constituent
100681-H
fO2-Si
669-9762 with CM
AS 1350C 50hr reacted
693-HfO
2-Si with CM
AS 1350C 50hr reacted
5000
200 400
600 800
1000 1200
1400 1600
Temperature degC
Strength test data compared
Yb
2 Si2 O7 C
MA
S reacted tensile Y
b2 Si2 O
7 CM
AS reacted
specimen fracture surface
surface w
ww
nasagov 27
National Aeronautics and Space Adm
inistration
High Stability and C
MAS R
esistance Observed from
the Rare
Earth S
ilicon High M
elting Point C
oating Com
positions
ndashD
emonstrated C
MA
S resistance
of NAS
A R
E-Si S
ystem at
1500degC 100 hr
ndash S
ilica-rich phase precipitation ndash
Rare earth elem
ent leaching into the m
elts (low concentration ~9
Surface side of the m
ol)
CM
AS m
elts
Area A
Area B
ww
wnasagov
28
![Page 8: Hurst, Bernadette J. Puleo€¦ · G57, 40.00 mg CMAS SiO Wellman -Aygun Smialek Braue 0 49 mole%; such as NASA’s CMAS (with NiO DSC:020 OES Measured by EDS [#] Type Date/time :](https://reader033.fdocuments.us/reader033/viewer/2022060211/5f04cb127e708231d40fbc15/html5/thumbnails/8.jpg)
National Aeronautics and Space Adm
inistration
CM
AS
Related D
egradations in EBC
s
Cross-section
50 mm
minus C
MAS effects
bull S
ignificantly reduce melting points of the E
BC
s and bond coats bull
More detrim
ental effects with thin airfoil E
BC
s bull
CM
AS
weakens the coating system
s reducing strength and toughness bullM
AS
increase EB
C diffusivities and perm
eability thus less protective as an environmental
barrier bullC
MA
S interactions w
ith heat flux thermal cycling erosion and therm
omechanical fatigue
Reaction layer spallations
Accelerated C
MC
failure when C
MA
S intact w
ith CM
Cs
Such as yttrium silicate
Coating
surface
EB
C and degradations
CM
AS induced m
elting and failure$w
ww
nasagov 8
National Aeronautics and Space Adm
inistration
CM
AS R
elated Degradations in E
BCs -C
ontinued minus
CM
AS effects on EBC
temperature capability
bull S
ilicate reactions with N
aO2 and A
l2 O3 silicate
Phase diagram
s showing yttrium
di-silicate reactions w
ith SiO
2 NaO
and Al2 O
3
ww
wnasagov
9
National Aeronautics and Space Adm
inistration
CM
AS R
elated Degradations in E
BCs -C
ontinued minus
CM
AS effects on EBC
temperature capability
bullRare earths generally have lim
ited temperature capability below
1500degC in the R
E2 O
3 -A
l2 O3 -S
iO2 based system
s bull
Sm
aller ionic size RE
s have higher melting points
Solidus temperature in Ln
2 Si2 O7 -A
l6 Si2 O13 -
SiO2 system
as function of ionic radius
Y Murakam
i and H Yam
amoto J C
eram Soc Jpn 101 [10] 1101-1106 (1993)
ww
wnasagov
10
National Aeronautics and Space Adm
inistration
Rare Earth D
issolutions in CM
AS Melts
ZrO2 -30Y
2 O3 -15Sm
2 O3 -15Yb
2 O3
ZrO2 -30Y
2 O3 -15N
d2 O
3 -15Yb2 O
3 -03Sc2 O
3
ZrO2 -96Y
2 O3 -22G
d2 O
3 -21Yb2 O
3
Ionic potential trend of RE
Radius size trend of RE
minus Large ionic size rare earths show
ed higher concentration dissolutions in the CM
AS
m
elt for ZrO2 -R
E2 O
3 oxide systems
ZrO2 -R
EO15 -H
f more endotherm
ic
Gustavo and Zhu International C
onference on Advanced C
eramics and C
omposites 2016
ww
wnasagov
11
Front CM
AS side
National Aeronautics and Space Adm
inistration
CM
AS Related D
egradations in EBC
coated CM
Cs ndash
Laboratory Heat Flux Tests
minusC
MAS effects on EB
C-C
MC
temperature capability tested in laser high heat
flux creep-rupture rig bull
Accelerated failure of C
MC
in loading high heat flux conditions
EBC
coated CV
I-MI C
MC
with N
dYb silicate R
ESi bond coat tested Tsurface 2600degF TC
MC
2450degF
Front heated CM
AS
side B
ack cooled side
Creep strain
Time h
Front CM
AS
side
200h
05
ww
wnasagov
12
National Aeronautics and Space Adm
inistration
EBC
CM
AS
Surface Initial N
ucleation Dissolution R
eactions ndash
Ytterbium
-and yttrium-silicate silicates reactions and dissolutions in C
AM
S
ndash M
ore sluggish dissolution of ytterbium as com
pared to yttrium
Ytterbium
di-silicate surface CM
AS m
elts 50 Y
tterbium di-silicate surface C
MA
S melts 5 h
h 1300degC
1500degC$
Yttrium
mono-silicate surface C
MA
S Y
ttrium silicate surface C
MA
S melts 5 h
melts 50 h 1300degC
1500degC
A
hlborg and Zhu Surface amp C
oatings Technology 237 (2013) 79ndash87 w
ww
nasagov 13
National Aeronautics and Space Adm
inistration
Rare E
arth Apatite G
rain Grow
th ndash
Grain grow
th of apatite phase at 1500degC at various tim
es
Ytterbium
silicate system
50 hr 150 hr
200 hr
200 hr50 hr
150 hr
Yttrium
silicate system$
ww
wnasagov
14
National Aeronautics and Space Adm
inistration
Effect of C
MA
S R
eactions on Grain B
oundary Phases
ndash C
MA
S and grain boundary phase has higher A
l2 O3
content (17-22 mole
) bull
Eutectic region w
ith high Al2 O
3 content ~1200degC m
elting point bull
Loss of SiO
2 due to volatility
200 hr 1500degC
NA
SA
modified
CM
AS
Grain
boundary final phase ndash low
SiO
2 and high A
lumina
ww
wnasagov
15
National Aeronautics and Space Adm
inistration
Rare E
arth Dissolution in C
MA
S M
elts ndash
Non stoichiom
etric characteristics of the CM
AS
ndash rare earth silicate reacted apatite phases ndash up to 200 h testing
ndash D
ifference in partitioning of ytterbium vs yttrium
in apatite bull
Average AE
OR
E2 O
3 ratio ~ 068 for ytterbium silicate ndash C
MA
S system
bull
Average AE
OR
E2 O
3 ratio ~ 022 for yttrium silicate ndash C
MA
S system
C
omposition in apatite (100 hr)
SiO2
Ahlborg and Zhu Surface amp
Coatings Technology 237 (2013) 79ndash87
RE
2 O3
AEO
Yttrium
Silicate EBC
Com
position in apatite (100 hr)
Ytterbium
Silicate EBC
ww
wnasagov
16
National Aeronautics and Space Adm
inistration
Advanced N
AS
A E
BC
Developm
ents
NA
SA advanced E
BC
systems em
phasizing high stability HfO
2 -and ZrO2 -R
E2 O
3 -
EBC layer 2 region
EB
Cs
Mol
Mol
SiO
2 EB
C system
RE
2 Si2-x O
7-2x such as (YbG
dY) 2 S
i2-x O7-2x
-Controlled dissolution and m
aintaining coating stability
(YbGdY) 2 S
i2-x O7-2x in
CM
AS
1300degC
(a)
(b)
ww
wnasagov
17
National Aeronautics and Space Adm
inistration E
xample of N
AS
A A
dvanced Environm
ental Barrier C
oating on S
iCSiC
CM
C System
s
Advanced EB
C coated vanes
HfO
2 -(YbG
dY)2 O
3
(YbG
dY)2 Si2-x O
7-2x
RESi(O
)+Hf B
ond Coat
Gd Y
b Y
O
Si
Yb
Gd Y
Si
Hf
A
lternating layered HfO
2 -Multicom
ponent Rare E
arth silicate EB
Cs used for fundam
ental stability studies
2700degF capable YbG
d-YbO+H
f based bond coats C
oated onto SiC
SiC
CM
C substrates using E
B-P
VD
The bond coat region
ww
wnasagov
18
National Aeronautics and Space Adm
inistration
CM
AS
Resistant Tests
ndash JE
Ts test of more advanced coating system
s at 2700F
Plasma sprayed (G
dY)2 Si2 O
7 2450 cycles
Special processed Yb
2 Si2 O7 spalling at 450 C
ycles EB
-PVD
(YbG
dY)2 Si2 O
7 total 4450 JETS cycles 100h
2450 4450
450
Hybrid H
f-rare earth aluminate silicate com
pleted 4450 cycles 100h
Hybrid H
ybrid Zr-rare earth silicate completed 4450
cycles 100h
2450 4450
2450 with
CM
AS 2450
ww
wnasagov
19
National Aeronautics and Space Adm
inistration
High S
tability and CM
AS
Resistance are E
nsured by Advanced H
igh M
elting Point C
oating and Multi-C
omponent C
ompositions A
rea A
Area B
ndash G
enerally improved C
MA
S
resistance of NAS
A R
ESi
System
at 1500degC 100 hr
ndash S
ilica-rich phase precipitation ndash
Rare earth elem
ent leaching into the m
elts (low concentration
~9mol
)
Surface side of the C
MA
S melts
EDS E
ww
wnasagov
20
National Aeronautics and Space Adm
inistration
Advanced E
BC
-CM
C S
ystem D
emonstrated 300 hr H
igh Cycle and
Low Fatigue D
urability in High H
eat Flux 2700degF Test Conditions
Specimen after 300 h testing
-A turbine airfoil E
BC
with H
fO2 -rare earth silicate and G
dYbSi bond coat on C
VI-M
I CM
C
substrate system selected for heat flux durability testing
-Laser high heat flux rig H
igh Cycle and Low
Cycle Fatigue test perform
ed at Stress
amplitude 10 ksi fatigue frequency 3 H
z at EB
C and 1 hr therm
al gradient cycles -
Tested EB
C surface tem
perature 1537degC (2800degF) and T bond coat tem
perature 1482degC
(2700degF) with C
MA
S
-D
emonstrated 300 hour durability at 2700degF+
-D
etermined fatigue-creep and therm
al conductivity behavior of the EB
C-C
MC
system
Specimen in rig testing
Test Condition Sum
mary
-EB
CC
VI-M
I Fatigue$loading 10 ksi (69 M
Pa) R
=005 with 1 hr Therm
al LC
F$-
TEB
C-surface 1537degC
(2800degF)$-
Tbond coat 1482degC
(2700degF)$-
Tback C
MC
surface 1250degC
(2282degF)
ww
wnasagov
21
National Aeronautics and Space Adm
inistration
Advanced E
BC
-CM
C Fatigue Test w
ith CM
AS
and in Steam
Jet Tested 300 h D
urability in High H
eat Flux Fatigue Test Conditions
-A
dvanced Hf-N
dYb silicate-N
dYbS
i bond coat EB
C coatings on 3D
architecture C
VI-P
IP S
iC-S
iC C
MC
(EB
-PV
D processing)
-Further understanding w
ater vapor -environmental interactions necessary
Surface view C
MA
S 35m
gcm2)
Back view
CM
AS
35mgcm
2)
ww
wnasagov
National Aeronautics and Space Adm
inistration
EBC
System
Designs ndash E
ffects of Com
posites and Clustered
Com
positions -
An alternating H
fO2 -and R
E-silicate coatings (EB
-PV
D processing) ndash H
fO2 -layer
infiltration and rare earth silicate layer melting
EB
-PV
D P
rocessed EB
Cs alternating H
fO2 -rich and ytterbium
silicate layer systems for
CM
AS
and impact resistance
ww
wnasagov
National Aeronautics and Space Adm
inistration
Sum
mary
bullC
MA
S degradation rem
ains a challenge for emerging turbine engine
environmental barrier coating ndash S
iCSiC
CM
C com
ponent systems
bullC
MA
S leads to low
er melting point of E
BC and bond coat system
s with
accelerated EBC
and CM
C degradations
bullN
AS
A advanced E
BC com
positions showed som
e promise for C
MA
S
resistance at temperatures up to 1500degC
in high velocity high heat flux and m
echanical loading tests bull
Currently focus on better understanding of E
BC com
positions and EBC
-CM
AS
interactions particularly with hafnium
zirconium and rare
earth silicates for improved tem
perature capability and CM
AS
resistance bull
Also standardize C
MA
S testing and quantify C
MA
S induced life debits
helping validate life modeling
bullC
ontrolling the compositions for C
MA
S resistance w
hile maintaining
high toughness continued to be a key emphasis
ww
wnasagov
24
National Aeronautics and Space Adm
inistration
Acknow
ledgements
bullThe w
ork was supported by N
ASA Fundam
ental Aeronautics Program (FAP)
Transformational Tools and Technologies (TTT) Project
bullThe authors are grateful to D
r Michael H
elminiak in the assistant of JETS tests
ww
wnasagov
25
National Aeronautics and Space Adm
inistration
CM
AS
Reaction K
inetics in Bond C
oats ndash S
iO2 rich phase partitioning in the C
MA
S m
elts ndash R
are earth content leaching low even at 1500degC
ndash M
ore advanced compositions are being im
plemented for im
proved thermom
echanical ndash
CM
AS Partitioning on R
E-Si bond coat 1500degC
100hr
RE incorporations
CM
AS
resistance
ww
wnasagov
26
National Aeronautics and Space Adm
inistration Strength R
esults of Selected EBC and EBC
Bond Coats
-CM
AS
Reaction R
esulted in Strength Reduction in Silicates
Selected E
BC
systems
ndashH
fO2 -R
E-S
i along with co-doped rare earth silicates and rare earth alum
ino-silicates for optim
ized strength stability and temperature capability
ndashC
MA
S infiltrations can reduce the strength
350 646-Specially alloy toughened t like H
fO2
648-EBC Bond Coat Constituent 300
659-AE9762
150
EBC
s
EBC
s
HfO
2 -Si (Si-rich)
Yb
2 Si 2 O 7
250658-EBC H
fO2-Rare Earth-A
lumino Silicate
660-Y2Si2O
7657-Zr-RE silicate 669-Y
b2Si2O7
Strength MPa
200696-EBC Bond Coat Constituent
100681-H
fO2-Si
669-9762 with CM
AS 1350C 50hr reacted
693-HfO
2-Si with CM
AS 1350C 50hr reacted
5000
200 400
600 800
1000 1200
1400 1600
Temperature degC
Strength test data compared
Yb
2 Si2 O7 C
MA
S reacted tensile Y
b2 Si2 O
7 CM
AS reacted
specimen fracture surface
surface w
ww
nasagov 27
National Aeronautics and Space Adm
inistration
High Stability and C
MAS R
esistance Observed from
the Rare
Earth S
ilicon High M
elting Point C
oating Com
positions
ndashD
emonstrated C
MA
S resistance
of NAS
A R
E-Si S
ystem at
1500degC 100 hr
ndash S
ilica-rich phase precipitation ndash
Rare earth elem
ent leaching into the m
elts (low concentration ~9
Surface side of the m
ol)
CM
AS m
elts
Area A
Area B
ww
wnasagov
28
![Page 9: Hurst, Bernadette J. Puleo€¦ · G57, 40.00 mg CMAS SiO Wellman -Aygun Smialek Braue 0 49 mole%; such as NASA’s CMAS (with NiO DSC:020 OES Measured by EDS [#] Type Date/time :](https://reader033.fdocuments.us/reader033/viewer/2022060211/5f04cb127e708231d40fbc15/html5/thumbnails/9.jpg)
National Aeronautics and Space Adm
inistration
CM
AS R
elated Degradations in E
BCs -C
ontinued minus
CM
AS effects on EBC
temperature capability
bull S
ilicate reactions with N
aO2 and A
l2 O3 silicate
Phase diagram
s showing yttrium
di-silicate reactions w
ith SiO
2 NaO
and Al2 O
3
ww
wnasagov
9
National Aeronautics and Space Adm
inistration
CM
AS R
elated Degradations in E
BCs -C
ontinued minus
CM
AS effects on EBC
temperature capability
bullRare earths generally have lim
ited temperature capability below
1500degC in the R
E2 O
3 -A
l2 O3 -S
iO2 based system
s bull
Sm
aller ionic size RE
s have higher melting points
Solidus temperature in Ln
2 Si2 O7 -A
l6 Si2 O13 -
SiO2 system
as function of ionic radius
Y Murakam
i and H Yam
amoto J C
eram Soc Jpn 101 [10] 1101-1106 (1993)
ww
wnasagov
10
National Aeronautics and Space Adm
inistration
Rare Earth D
issolutions in CM
AS Melts
ZrO2 -30Y
2 O3 -15Sm
2 O3 -15Yb
2 O3
ZrO2 -30Y
2 O3 -15N
d2 O
3 -15Yb2 O
3 -03Sc2 O
3
ZrO2 -96Y
2 O3 -22G
d2 O
3 -21Yb2 O
3
Ionic potential trend of RE
Radius size trend of RE
minus Large ionic size rare earths show
ed higher concentration dissolutions in the CM
AS
m
elt for ZrO2 -R
E2 O
3 oxide systems
ZrO2 -R
EO15 -H
f more endotherm
ic
Gustavo and Zhu International C
onference on Advanced C
eramics and C
omposites 2016
ww
wnasagov
11
Front CM
AS side
National Aeronautics and Space Adm
inistration
CM
AS Related D
egradations in EBC
coated CM
Cs ndash
Laboratory Heat Flux Tests
minusC
MAS effects on EB
C-C
MC
temperature capability tested in laser high heat
flux creep-rupture rig bull
Accelerated failure of C
MC
in loading high heat flux conditions
EBC
coated CV
I-MI C
MC
with N
dYb silicate R
ESi bond coat tested Tsurface 2600degF TC
MC
2450degF
Front heated CM
AS
side B
ack cooled side
Creep strain
Time h
Front CM
AS
side
200h
05
ww
wnasagov
12
National Aeronautics and Space Adm
inistration
EBC
CM
AS
Surface Initial N
ucleation Dissolution R
eactions ndash
Ytterbium
-and yttrium-silicate silicates reactions and dissolutions in C
AM
S
ndash M
ore sluggish dissolution of ytterbium as com
pared to yttrium
Ytterbium
di-silicate surface CM
AS m
elts 50 Y
tterbium di-silicate surface C
MA
S melts 5 h
h 1300degC
1500degC$
Yttrium
mono-silicate surface C
MA
S Y
ttrium silicate surface C
MA
S melts 5 h
melts 50 h 1300degC
1500degC
A
hlborg and Zhu Surface amp C
oatings Technology 237 (2013) 79ndash87 w
ww
nasagov 13
National Aeronautics and Space Adm
inistration
Rare E
arth Apatite G
rain Grow
th ndash
Grain grow
th of apatite phase at 1500degC at various tim
es
Ytterbium
silicate system
50 hr 150 hr
200 hr
200 hr50 hr
150 hr
Yttrium
silicate system$
ww
wnasagov
14
National Aeronautics and Space Adm
inistration
Effect of C
MA
S R
eactions on Grain B
oundary Phases
ndash C
MA
S and grain boundary phase has higher A
l2 O3
content (17-22 mole
) bull
Eutectic region w
ith high Al2 O
3 content ~1200degC m
elting point bull
Loss of SiO
2 due to volatility
200 hr 1500degC
NA
SA
modified
CM
AS
Grain
boundary final phase ndash low
SiO
2 and high A
lumina
ww
wnasagov
15
National Aeronautics and Space Adm
inistration
Rare E
arth Dissolution in C
MA
S M
elts ndash
Non stoichiom
etric characteristics of the CM
AS
ndash rare earth silicate reacted apatite phases ndash up to 200 h testing
ndash D
ifference in partitioning of ytterbium vs yttrium
in apatite bull
Average AE
OR
E2 O
3 ratio ~ 068 for ytterbium silicate ndash C
MA
S system
bull
Average AE
OR
E2 O
3 ratio ~ 022 for yttrium silicate ndash C
MA
S system
C
omposition in apatite (100 hr)
SiO2
Ahlborg and Zhu Surface amp
Coatings Technology 237 (2013) 79ndash87
RE
2 O3
AEO
Yttrium
Silicate EBC
Com
position in apatite (100 hr)
Ytterbium
Silicate EBC
ww
wnasagov
16
National Aeronautics and Space Adm
inistration
Advanced N
AS
A E
BC
Developm
ents
NA
SA advanced E
BC
systems em
phasizing high stability HfO
2 -and ZrO2 -R
E2 O
3 -
EBC layer 2 region
EB
Cs
Mol
Mol
SiO
2 EB
C system
RE
2 Si2-x O
7-2x such as (YbG
dY) 2 S
i2-x O7-2x
-Controlled dissolution and m
aintaining coating stability
(YbGdY) 2 S
i2-x O7-2x in
CM
AS
1300degC
(a)
(b)
ww
wnasagov
17
National Aeronautics and Space Adm
inistration E
xample of N
AS
A A
dvanced Environm
ental Barrier C
oating on S
iCSiC
CM
C System
s
Advanced EB
C coated vanes
HfO
2 -(YbG
dY)2 O
3
(YbG
dY)2 Si2-x O
7-2x
RESi(O
)+Hf B
ond Coat
Gd Y
b Y
O
Si
Yb
Gd Y
Si
Hf
A
lternating layered HfO
2 -Multicom
ponent Rare E
arth silicate EB
Cs used for fundam
ental stability studies
2700degF capable YbG
d-YbO+H
f based bond coats C
oated onto SiC
SiC
CM
C substrates using E
B-P
VD
The bond coat region
ww
wnasagov
18
National Aeronautics and Space Adm
inistration
CM
AS
Resistant Tests
ndash JE
Ts test of more advanced coating system
s at 2700F
Plasma sprayed (G
dY)2 Si2 O
7 2450 cycles
Special processed Yb
2 Si2 O7 spalling at 450 C
ycles EB
-PVD
(YbG
dY)2 Si2 O
7 total 4450 JETS cycles 100h
2450 4450
450
Hybrid H
f-rare earth aluminate silicate com
pleted 4450 cycles 100h
Hybrid H
ybrid Zr-rare earth silicate completed 4450
cycles 100h
2450 4450
2450 with
CM
AS 2450
ww
wnasagov
19
National Aeronautics and Space Adm
inistration
High S
tability and CM
AS
Resistance are E
nsured by Advanced H
igh M
elting Point C
oating and Multi-C
omponent C
ompositions A
rea A
Area B
ndash G
enerally improved C
MA
S
resistance of NAS
A R
ESi
System
at 1500degC 100 hr
ndash S
ilica-rich phase precipitation ndash
Rare earth elem
ent leaching into the m
elts (low concentration
~9mol
)
Surface side of the C
MA
S melts
EDS E
ww
wnasagov
20
National Aeronautics and Space Adm
inistration
Advanced E
BC
-CM
C S
ystem D
emonstrated 300 hr H
igh Cycle and
Low Fatigue D
urability in High H
eat Flux 2700degF Test Conditions
Specimen after 300 h testing
-A turbine airfoil E
BC
with H
fO2 -rare earth silicate and G
dYbSi bond coat on C
VI-M
I CM
C
substrate system selected for heat flux durability testing
-Laser high heat flux rig H
igh Cycle and Low
Cycle Fatigue test perform
ed at Stress
amplitude 10 ksi fatigue frequency 3 H
z at EB
C and 1 hr therm
al gradient cycles -
Tested EB
C surface tem
perature 1537degC (2800degF) and T bond coat tem
perature 1482degC
(2700degF) with C
MA
S
-D
emonstrated 300 hour durability at 2700degF+
-D
etermined fatigue-creep and therm
al conductivity behavior of the EB
C-C
MC
system
Specimen in rig testing
Test Condition Sum
mary
-EB
CC
VI-M
I Fatigue$loading 10 ksi (69 M
Pa) R
=005 with 1 hr Therm
al LC
F$-
TEB
C-surface 1537degC
(2800degF)$-
Tbond coat 1482degC
(2700degF)$-
Tback C
MC
surface 1250degC
(2282degF)
ww
wnasagov
21
National Aeronautics and Space Adm
inistration
Advanced E
BC
-CM
C Fatigue Test w
ith CM
AS
and in Steam
Jet Tested 300 h D
urability in High H
eat Flux Fatigue Test Conditions
-A
dvanced Hf-N
dYb silicate-N
dYbS
i bond coat EB
C coatings on 3D
architecture C
VI-P
IP S
iC-S
iC C
MC
(EB
-PV
D processing)
-Further understanding w
ater vapor -environmental interactions necessary
Surface view C
MA
S 35m
gcm2)
Back view
CM
AS
35mgcm
2)
ww
wnasagov
National Aeronautics and Space Adm
inistration
EBC
System
Designs ndash E
ffects of Com
posites and Clustered
Com
positions -
An alternating H
fO2 -and R
E-silicate coatings (EB
-PV
D processing) ndash H
fO2 -layer
infiltration and rare earth silicate layer melting
EB
-PV
D P
rocessed EB
Cs alternating H
fO2 -rich and ytterbium
silicate layer systems for
CM
AS
and impact resistance
ww
wnasagov
National Aeronautics and Space Adm
inistration
Sum
mary
bullC
MA
S degradation rem
ains a challenge for emerging turbine engine
environmental barrier coating ndash S
iCSiC
CM
C com
ponent systems
bullC
MA
S leads to low
er melting point of E
BC and bond coat system
s with
accelerated EBC
and CM
C degradations
bullN
AS
A advanced E
BC com
positions showed som
e promise for C
MA
S
resistance at temperatures up to 1500degC
in high velocity high heat flux and m
echanical loading tests bull
Currently focus on better understanding of E
BC com
positions and EBC
-CM
AS
interactions particularly with hafnium
zirconium and rare
earth silicates for improved tem
perature capability and CM
AS
resistance bull
Also standardize C
MA
S testing and quantify C
MA
S induced life debits
helping validate life modeling
bullC
ontrolling the compositions for C
MA
S resistance w
hile maintaining
high toughness continued to be a key emphasis
ww
wnasagov
24
National Aeronautics and Space Adm
inistration
Acknow
ledgements
bullThe w
ork was supported by N
ASA Fundam
ental Aeronautics Program (FAP)
Transformational Tools and Technologies (TTT) Project
bullThe authors are grateful to D
r Michael H
elminiak in the assistant of JETS tests
ww
wnasagov
25
National Aeronautics and Space Adm
inistration
CM
AS
Reaction K
inetics in Bond C
oats ndash S
iO2 rich phase partitioning in the C
MA
S m
elts ndash R
are earth content leaching low even at 1500degC
ndash M
ore advanced compositions are being im
plemented for im
proved thermom
echanical ndash
CM
AS Partitioning on R
E-Si bond coat 1500degC
100hr
RE incorporations
CM
AS
resistance
ww
wnasagov
26
National Aeronautics and Space Adm
inistration Strength R
esults of Selected EBC and EBC
Bond Coats
-CM
AS
Reaction R
esulted in Strength Reduction in Silicates
Selected E
BC
systems
ndashH
fO2 -R
E-S
i along with co-doped rare earth silicates and rare earth alum
ino-silicates for optim
ized strength stability and temperature capability
ndashC
MA
S infiltrations can reduce the strength
350 646-Specially alloy toughened t like H
fO2
648-EBC Bond Coat Constituent 300
659-AE9762
150
EBC
s
EBC
s
HfO
2 -Si (Si-rich)
Yb
2 Si 2 O 7
250658-EBC H
fO2-Rare Earth-A
lumino Silicate
660-Y2Si2O
7657-Zr-RE silicate 669-Y
b2Si2O7
Strength MPa
200696-EBC Bond Coat Constituent
100681-H
fO2-Si
669-9762 with CM
AS 1350C 50hr reacted
693-HfO
2-Si with CM
AS 1350C 50hr reacted
5000
200 400
600 800
1000 1200
1400 1600
Temperature degC
Strength test data compared
Yb
2 Si2 O7 C
MA
S reacted tensile Y
b2 Si2 O
7 CM
AS reacted
specimen fracture surface
surface w
ww
nasagov 27
National Aeronautics and Space Adm
inistration
High Stability and C
MAS R
esistance Observed from
the Rare
Earth S
ilicon High M
elting Point C
oating Com
positions
ndashD
emonstrated C
MA
S resistance
of NAS
A R
E-Si S
ystem at
1500degC 100 hr
ndash S
ilica-rich phase precipitation ndash
Rare earth elem
ent leaching into the m
elts (low concentration ~9
Surface side of the m
ol)
CM
AS m
elts
Area A
Area B
ww
wnasagov
28
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National Aeronautics and Space Adm
inistration
CM
AS R
elated Degradations in E
BCs -C
ontinued minus
CM
AS effects on EBC
temperature capability
bullRare earths generally have lim
ited temperature capability below
1500degC in the R
E2 O
3 -A
l2 O3 -S
iO2 based system
s bull
Sm
aller ionic size RE
s have higher melting points
Solidus temperature in Ln
2 Si2 O7 -A
l6 Si2 O13 -
SiO2 system
as function of ionic radius
Y Murakam
i and H Yam
amoto J C
eram Soc Jpn 101 [10] 1101-1106 (1993)
ww
wnasagov
10
National Aeronautics and Space Adm
inistration
Rare Earth D
issolutions in CM
AS Melts
ZrO2 -30Y
2 O3 -15Sm
2 O3 -15Yb
2 O3
ZrO2 -30Y
2 O3 -15N
d2 O
3 -15Yb2 O
3 -03Sc2 O
3
ZrO2 -96Y
2 O3 -22G
d2 O
3 -21Yb2 O
3
Ionic potential trend of RE
Radius size trend of RE
minus Large ionic size rare earths show
ed higher concentration dissolutions in the CM
AS
m
elt for ZrO2 -R
E2 O
3 oxide systems
ZrO2 -R
EO15 -H
f more endotherm
ic
Gustavo and Zhu International C
onference on Advanced C
eramics and C
omposites 2016
ww
wnasagov
11
Front CM
AS side
National Aeronautics and Space Adm
inistration
CM
AS Related D
egradations in EBC
coated CM
Cs ndash
Laboratory Heat Flux Tests
minusC
MAS effects on EB
C-C
MC
temperature capability tested in laser high heat
flux creep-rupture rig bull
Accelerated failure of C
MC
in loading high heat flux conditions
EBC
coated CV
I-MI C
MC
with N
dYb silicate R
ESi bond coat tested Tsurface 2600degF TC
MC
2450degF
Front heated CM
AS
side B
ack cooled side
Creep strain
Time h
Front CM
AS
side
200h
05
ww
wnasagov
12
National Aeronautics and Space Adm
inistration
EBC
CM
AS
Surface Initial N
ucleation Dissolution R
eactions ndash
Ytterbium
-and yttrium-silicate silicates reactions and dissolutions in C
AM
S
ndash M
ore sluggish dissolution of ytterbium as com
pared to yttrium
Ytterbium
di-silicate surface CM
AS m
elts 50 Y
tterbium di-silicate surface C
MA
S melts 5 h
h 1300degC
1500degC$
Yttrium
mono-silicate surface C
MA
S Y
ttrium silicate surface C
MA
S melts 5 h
melts 50 h 1300degC
1500degC
A
hlborg and Zhu Surface amp C
oatings Technology 237 (2013) 79ndash87 w
ww
nasagov 13
National Aeronautics and Space Adm
inistration
Rare E
arth Apatite G
rain Grow
th ndash
Grain grow
th of apatite phase at 1500degC at various tim
es
Ytterbium
silicate system
50 hr 150 hr
200 hr
200 hr50 hr
150 hr
Yttrium
silicate system$
ww
wnasagov
14
National Aeronautics and Space Adm
inistration
Effect of C
MA
S R
eactions on Grain B
oundary Phases
ndash C
MA
S and grain boundary phase has higher A
l2 O3
content (17-22 mole
) bull
Eutectic region w
ith high Al2 O
3 content ~1200degC m
elting point bull
Loss of SiO
2 due to volatility
200 hr 1500degC
NA
SA
modified
CM
AS
Grain
boundary final phase ndash low
SiO
2 and high A
lumina
ww
wnasagov
15
National Aeronautics and Space Adm
inistration
Rare E
arth Dissolution in C
MA
S M
elts ndash
Non stoichiom
etric characteristics of the CM
AS
ndash rare earth silicate reacted apatite phases ndash up to 200 h testing
ndash D
ifference in partitioning of ytterbium vs yttrium
in apatite bull
Average AE
OR
E2 O
3 ratio ~ 068 for ytterbium silicate ndash C
MA
S system
bull
Average AE
OR
E2 O
3 ratio ~ 022 for yttrium silicate ndash C
MA
S system
C
omposition in apatite (100 hr)
SiO2
Ahlborg and Zhu Surface amp
Coatings Technology 237 (2013) 79ndash87
RE
2 O3
AEO
Yttrium
Silicate EBC
Com
position in apatite (100 hr)
Ytterbium
Silicate EBC
ww
wnasagov
16
National Aeronautics and Space Adm
inistration
Advanced N
AS
A E
BC
Developm
ents
NA
SA advanced E
BC
systems em
phasizing high stability HfO
2 -and ZrO2 -R
E2 O
3 -
EBC layer 2 region
EB
Cs
Mol
Mol
SiO
2 EB
C system
RE
2 Si2-x O
7-2x such as (YbG
dY) 2 S
i2-x O7-2x
-Controlled dissolution and m
aintaining coating stability
(YbGdY) 2 S
i2-x O7-2x in
CM
AS
1300degC
(a)
(b)
ww
wnasagov
17
National Aeronautics and Space Adm
inistration E
xample of N
AS
A A
dvanced Environm
ental Barrier C
oating on S
iCSiC
CM
C System
s
Advanced EB
C coated vanes
HfO
2 -(YbG
dY)2 O
3
(YbG
dY)2 Si2-x O
7-2x
RESi(O
)+Hf B
ond Coat
Gd Y
b Y
O
Si
Yb
Gd Y
Si
Hf
A
lternating layered HfO
2 -Multicom
ponent Rare E
arth silicate EB
Cs used for fundam
ental stability studies
2700degF capable YbG
d-YbO+H
f based bond coats C
oated onto SiC
SiC
CM
C substrates using E
B-P
VD
The bond coat region
ww
wnasagov
18
National Aeronautics and Space Adm
inistration
CM
AS
Resistant Tests
ndash JE
Ts test of more advanced coating system
s at 2700F
Plasma sprayed (G
dY)2 Si2 O
7 2450 cycles
Special processed Yb
2 Si2 O7 spalling at 450 C
ycles EB
-PVD
(YbG
dY)2 Si2 O
7 total 4450 JETS cycles 100h
2450 4450
450
Hybrid H
f-rare earth aluminate silicate com
pleted 4450 cycles 100h
Hybrid H
ybrid Zr-rare earth silicate completed 4450
cycles 100h
2450 4450
2450 with
CM
AS 2450
ww
wnasagov
19
National Aeronautics and Space Adm
inistration
High S
tability and CM
AS
Resistance are E
nsured by Advanced H
igh M
elting Point C
oating and Multi-C
omponent C
ompositions A
rea A
Area B
ndash G
enerally improved C
MA
S
resistance of NAS
A R
ESi
System
at 1500degC 100 hr
ndash S
ilica-rich phase precipitation ndash
Rare earth elem
ent leaching into the m
elts (low concentration
~9mol
)
Surface side of the C
MA
S melts
EDS E
ww
wnasagov
20
National Aeronautics and Space Adm
inistration
Advanced E
BC
-CM
C S
ystem D
emonstrated 300 hr H
igh Cycle and
Low Fatigue D
urability in High H
eat Flux 2700degF Test Conditions
Specimen after 300 h testing
-A turbine airfoil E
BC
with H
fO2 -rare earth silicate and G
dYbSi bond coat on C
VI-M
I CM
C
substrate system selected for heat flux durability testing
-Laser high heat flux rig H
igh Cycle and Low
Cycle Fatigue test perform
ed at Stress
amplitude 10 ksi fatigue frequency 3 H
z at EB
C and 1 hr therm
al gradient cycles -
Tested EB
C surface tem
perature 1537degC (2800degF) and T bond coat tem
perature 1482degC
(2700degF) with C
MA
S
-D
emonstrated 300 hour durability at 2700degF+
-D
etermined fatigue-creep and therm
al conductivity behavior of the EB
C-C
MC
system
Specimen in rig testing
Test Condition Sum
mary
-EB
CC
VI-M
I Fatigue$loading 10 ksi (69 M
Pa) R
=005 with 1 hr Therm
al LC
F$-
TEB
C-surface 1537degC
(2800degF)$-
Tbond coat 1482degC
(2700degF)$-
Tback C
MC
surface 1250degC
(2282degF)
ww
wnasagov
21
National Aeronautics and Space Adm
inistration
Advanced E
BC
-CM
C Fatigue Test w
ith CM
AS
and in Steam
Jet Tested 300 h D
urability in High H
eat Flux Fatigue Test Conditions
-A
dvanced Hf-N
dYb silicate-N
dYbS
i bond coat EB
C coatings on 3D
architecture C
VI-P
IP S
iC-S
iC C
MC
(EB
-PV
D processing)
-Further understanding w
ater vapor -environmental interactions necessary
Surface view C
MA
S 35m
gcm2)
Back view
CM
AS
35mgcm
2)
ww
wnasagov
National Aeronautics and Space Adm
inistration
EBC
System
Designs ndash E
ffects of Com
posites and Clustered
Com
positions -
An alternating H
fO2 -and R
E-silicate coatings (EB
-PV
D processing) ndash H
fO2 -layer
infiltration and rare earth silicate layer melting
EB
-PV
D P
rocessed EB
Cs alternating H
fO2 -rich and ytterbium
silicate layer systems for
CM
AS
and impact resistance
ww
wnasagov
National Aeronautics and Space Adm
inistration
Sum
mary
bullC
MA
S degradation rem
ains a challenge for emerging turbine engine
environmental barrier coating ndash S
iCSiC
CM
C com
ponent systems
bullC
MA
S leads to low
er melting point of E
BC and bond coat system
s with
accelerated EBC
and CM
C degradations
bullN
AS
A advanced E
BC com
positions showed som
e promise for C
MA
S
resistance at temperatures up to 1500degC
in high velocity high heat flux and m
echanical loading tests bull
Currently focus on better understanding of E
BC com
positions and EBC
-CM
AS
interactions particularly with hafnium
zirconium and rare
earth silicates for improved tem
perature capability and CM
AS
resistance bull
Also standardize C
MA
S testing and quantify C
MA
S induced life debits
helping validate life modeling
bullC
ontrolling the compositions for C
MA
S resistance w
hile maintaining
high toughness continued to be a key emphasis
ww
wnasagov
24
National Aeronautics and Space Adm
inistration
Acknow
ledgements
bullThe w
ork was supported by N
ASA Fundam
ental Aeronautics Program (FAP)
Transformational Tools and Technologies (TTT) Project
bullThe authors are grateful to D
r Michael H
elminiak in the assistant of JETS tests
ww
wnasagov
25
National Aeronautics and Space Adm
inistration
CM
AS
Reaction K
inetics in Bond C
oats ndash S
iO2 rich phase partitioning in the C
MA
S m
elts ndash R
are earth content leaching low even at 1500degC
ndash M
ore advanced compositions are being im
plemented for im
proved thermom
echanical ndash
CM
AS Partitioning on R
E-Si bond coat 1500degC
100hr
RE incorporations
CM
AS
resistance
ww
wnasagov
26
National Aeronautics and Space Adm
inistration Strength R
esults of Selected EBC and EBC
Bond Coats
-CM
AS
Reaction R
esulted in Strength Reduction in Silicates
Selected E
BC
systems
ndashH
fO2 -R
E-S
i along with co-doped rare earth silicates and rare earth alum
ino-silicates for optim
ized strength stability and temperature capability
ndashC
MA
S infiltrations can reduce the strength
350 646-Specially alloy toughened t like H
fO2
648-EBC Bond Coat Constituent 300
659-AE9762
150
EBC
s
EBC
s
HfO
2 -Si (Si-rich)
Yb
2 Si 2 O 7
250658-EBC H
fO2-Rare Earth-A
lumino Silicate
660-Y2Si2O
7657-Zr-RE silicate 669-Y
b2Si2O7
Strength MPa
200696-EBC Bond Coat Constituent
100681-H
fO2-Si
669-9762 with CM
AS 1350C 50hr reacted
693-HfO
2-Si with CM
AS 1350C 50hr reacted
5000
200 400
600 800
1000 1200
1400 1600
Temperature degC
Strength test data compared
Yb
2 Si2 O7 C
MA
S reacted tensile Y
b2 Si2 O
7 CM
AS reacted
specimen fracture surface
surface w
ww
nasagov 27
National Aeronautics and Space Adm
inistration
High Stability and C
MAS R
esistance Observed from
the Rare
Earth S
ilicon High M
elting Point C
oating Com
positions
ndashD
emonstrated C
MA
S resistance
of NAS
A R
E-Si S
ystem at
1500degC 100 hr
ndash S
ilica-rich phase precipitation ndash
Rare earth elem
ent leaching into the m
elts (low concentration ~9
Surface side of the m
ol)
CM
AS m
elts
Area A
Area B
ww
wnasagov
28
![Page 11: Hurst, Bernadette J. Puleo€¦ · G57, 40.00 mg CMAS SiO Wellman -Aygun Smialek Braue 0 49 mole%; such as NASA’s CMAS (with NiO DSC:020 OES Measured by EDS [#] Type Date/time :](https://reader033.fdocuments.us/reader033/viewer/2022060211/5f04cb127e708231d40fbc15/html5/thumbnails/11.jpg)
National Aeronautics and Space Adm
inistration
Rare Earth D
issolutions in CM
AS Melts
ZrO2 -30Y
2 O3 -15Sm
2 O3 -15Yb
2 O3
ZrO2 -30Y
2 O3 -15N
d2 O
3 -15Yb2 O
3 -03Sc2 O
3
ZrO2 -96Y
2 O3 -22G
d2 O
3 -21Yb2 O
3
Ionic potential trend of RE
Radius size trend of RE
minus Large ionic size rare earths show
ed higher concentration dissolutions in the CM
AS
m
elt for ZrO2 -R
E2 O
3 oxide systems
ZrO2 -R
EO15 -H
f more endotherm
ic
Gustavo and Zhu International C
onference on Advanced C
eramics and C
omposites 2016
ww
wnasagov
11
Front CM
AS side
National Aeronautics and Space Adm
inistration
CM
AS Related D
egradations in EBC
coated CM
Cs ndash
Laboratory Heat Flux Tests
minusC
MAS effects on EB
C-C
MC
temperature capability tested in laser high heat
flux creep-rupture rig bull
Accelerated failure of C
MC
in loading high heat flux conditions
EBC
coated CV
I-MI C
MC
with N
dYb silicate R
ESi bond coat tested Tsurface 2600degF TC
MC
2450degF
Front heated CM
AS
side B
ack cooled side
Creep strain
Time h
Front CM
AS
side
200h
05
ww
wnasagov
12
National Aeronautics and Space Adm
inistration
EBC
CM
AS
Surface Initial N
ucleation Dissolution R
eactions ndash
Ytterbium
-and yttrium-silicate silicates reactions and dissolutions in C
AM
S
ndash M
ore sluggish dissolution of ytterbium as com
pared to yttrium
Ytterbium
di-silicate surface CM
AS m
elts 50 Y
tterbium di-silicate surface C
MA
S melts 5 h
h 1300degC
1500degC$
Yttrium
mono-silicate surface C
MA
S Y
ttrium silicate surface C
MA
S melts 5 h
melts 50 h 1300degC
1500degC
A
hlborg and Zhu Surface amp C
oatings Technology 237 (2013) 79ndash87 w
ww
nasagov 13
National Aeronautics and Space Adm
inistration
Rare E
arth Apatite G
rain Grow
th ndash
Grain grow
th of apatite phase at 1500degC at various tim
es
Ytterbium
silicate system
50 hr 150 hr
200 hr
200 hr50 hr
150 hr
Yttrium
silicate system$
ww
wnasagov
14
National Aeronautics and Space Adm
inistration
Effect of C
MA
S R
eactions on Grain B
oundary Phases
ndash C
MA
S and grain boundary phase has higher A
l2 O3
content (17-22 mole
) bull
Eutectic region w
ith high Al2 O
3 content ~1200degC m
elting point bull
Loss of SiO
2 due to volatility
200 hr 1500degC
NA
SA
modified
CM
AS
Grain
boundary final phase ndash low
SiO
2 and high A
lumina
ww
wnasagov
15
National Aeronautics and Space Adm
inistration
Rare E
arth Dissolution in C
MA
S M
elts ndash
Non stoichiom
etric characteristics of the CM
AS
ndash rare earth silicate reacted apatite phases ndash up to 200 h testing
ndash D
ifference in partitioning of ytterbium vs yttrium
in apatite bull
Average AE
OR
E2 O
3 ratio ~ 068 for ytterbium silicate ndash C
MA
S system
bull
Average AE
OR
E2 O
3 ratio ~ 022 for yttrium silicate ndash C
MA
S system
C
omposition in apatite (100 hr)
SiO2
Ahlborg and Zhu Surface amp
Coatings Technology 237 (2013) 79ndash87
RE
2 O3
AEO
Yttrium
Silicate EBC
Com
position in apatite (100 hr)
Ytterbium
Silicate EBC
ww
wnasagov
16
National Aeronautics and Space Adm
inistration
Advanced N
AS
A E
BC
Developm
ents
NA
SA advanced E
BC
systems em
phasizing high stability HfO
2 -and ZrO2 -R
E2 O
3 -
EBC layer 2 region
EB
Cs
Mol
Mol
SiO
2 EB
C system
RE
2 Si2-x O
7-2x such as (YbG
dY) 2 S
i2-x O7-2x
-Controlled dissolution and m
aintaining coating stability
(YbGdY) 2 S
i2-x O7-2x in
CM
AS
1300degC
(a)
(b)
ww
wnasagov
17
National Aeronautics and Space Adm
inistration E
xample of N
AS
A A
dvanced Environm
ental Barrier C
oating on S
iCSiC
CM
C System
s
Advanced EB
C coated vanes
HfO
2 -(YbG
dY)2 O
3
(YbG
dY)2 Si2-x O
7-2x
RESi(O
)+Hf B
ond Coat
Gd Y
b Y
O
Si
Yb
Gd Y
Si
Hf
A
lternating layered HfO
2 -Multicom
ponent Rare E
arth silicate EB
Cs used for fundam
ental stability studies
2700degF capable YbG
d-YbO+H
f based bond coats C
oated onto SiC
SiC
CM
C substrates using E
B-P
VD
The bond coat region
ww
wnasagov
18
National Aeronautics and Space Adm
inistration
CM
AS
Resistant Tests
ndash JE
Ts test of more advanced coating system
s at 2700F
Plasma sprayed (G
dY)2 Si2 O
7 2450 cycles
Special processed Yb
2 Si2 O7 spalling at 450 C
ycles EB
-PVD
(YbG
dY)2 Si2 O
7 total 4450 JETS cycles 100h
2450 4450
450
Hybrid H
f-rare earth aluminate silicate com
pleted 4450 cycles 100h
Hybrid H
ybrid Zr-rare earth silicate completed 4450
cycles 100h
2450 4450
2450 with
CM
AS 2450
ww
wnasagov
19
National Aeronautics and Space Adm
inistration
High S
tability and CM
AS
Resistance are E
nsured by Advanced H
igh M
elting Point C
oating and Multi-C
omponent C
ompositions A
rea A
Area B
ndash G
enerally improved C
MA
S
resistance of NAS
A R
ESi
System
at 1500degC 100 hr
ndash S
ilica-rich phase precipitation ndash
Rare earth elem
ent leaching into the m
elts (low concentration
~9mol
)
Surface side of the C
MA
S melts
EDS E
ww
wnasagov
20
National Aeronautics and Space Adm
inistration
Advanced E
BC
-CM
C S
ystem D
emonstrated 300 hr H
igh Cycle and
Low Fatigue D
urability in High H
eat Flux 2700degF Test Conditions
Specimen after 300 h testing
-A turbine airfoil E
BC
with H
fO2 -rare earth silicate and G
dYbSi bond coat on C
VI-M
I CM
C
substrate system selected for heat flux durability testing
-Laser high heat flux rig H
igh Cycle and Low
Cycle Fatigue test perform
ed at Stress
amplitude 10 ksi fatigue frequency 3 H
z at EB
C and 1 hr therm
al gradient cycles -
Tested EB
C surface tem
perature 1537degC (2800degF) and T bond coat tem
perature 1482degC
(2700degF) with C
MA
S
-D
emonstrated 300 hour durability at 2700degF+
-D
etermined fatigue-creep and therm
al conductivity behavior of the EB
C-C
MC
system
Specimen in rig testing
Test Condition Sum
mary
-EB
CC
VI-M
I Fatigue$loading 10 ksi (69 M
Pa) R
=005 with 1 hr Therm
al LC
F$-
TEB
C-surface 1537degC
(2800degF)$-
Tbond coat 1482degC
(2700degF)$-
Tback C
MC
surface 1250degC
(2282degF)
ww
wnasagov
21
National Aeronautics and Space Adm
inistration
Advanced E
BC
-CM
C Fatigue Test w
ith CM
AS
and in Steam
Jet Tested 300 h D
urability in High H
eat Flux Fatigue Test Conditions
-A
dvanced Hf-N
dYb silicate-N
dYbS
i bond coat EB
C coatings on 3D
architecture C
VI-P
IP S
iC-S
iC C
MC
(EB
-PV
D processing)
-Further understanding w
ater vapor -environmental interactions necessary
Surface view C
MA
S 35m
gcm2)
Back view
CM
AS
35mgcm
2)
ww
wnasagov
National Aeronautics and Space Adm
inistration
EBC
System
Designs ndash E
ffects of Com
posites and Clustered
Com
positions -
An alternating H
fO2 -and R
E-silicate coatings (EB
-PV
D processing) ndash H
fO2 -layer
infiltration and rare earth silicate layer melting
EB
-PV
D P
rocessed EB
Cs alternating H
fO2 -rich and ytterbium
silicate layer systems for
CM
AS
and impact resistance
ww
wnasagov
National Aeronautics and Space Adm
inistration
Sum
mary
bullC
MA
S degradation rem
ains a challenge for emerging turbine engine
environmental barrier coating ndash S
iCSiC
CM
C com
ponent systems
bullC
MA
S leads to low
er melting point of E
BC and bond coat system
s with
accelerated EBC
and CM
C degradations
bullN
AS
A advanced E
BC com
positions showed som
e promise for C
MA
S
resistance at temperatures up to 1500degC
in high velocity high heat flux and m
echanical loading tests bull
Currently focus on better understanding of E
BC com
positions and EBC
-CM
AS
interactions particularly with hafnium
zirconium and rare
earth silicates for improved tem
perature capability and CM
AS
resistance bull
Also standardize C
MA
S testing and quantify C
MA
S induced life debits
helping validate life modeling
bullC
ontrolling the compositions for C
MA
S resistance w
hile maintaining
high toughness continued to be a key emphasis
ww
wnasagov
24
National Aeronautics and Space Adm
inistration
Acknow
ledgements
bullThe w
ork was supported by N
ASA Fundam
ental Aeronautics Program (FAP)
Transformational Tools and Technologies (TTT) Project
bullThe authors are grateful to D
r Michael H
elminiak in the assistant of JETS tests
ww
wnasagov
25
National Aeronautics and Space Adm
inistration
CM
AS
Reaction K
inetics in Bond C
oats ndash S
iO2 rich phase partitioning in the C
MA
S m
elts ndash R
are earth content leaching low even at 1500degC
ndash M
ore advanced compositions are being im
plemented for im
proved thermom
echanical ndash
CM
AS Partitioning on R
E-Si bond coat 1500degC
100hr
RE incorporations
CM
AS
resistance
ww
wnasagov
26
National Aeronautics and Space Adm
inistration Strength R
esults of Selected EBC and EBC
Bond Coats
-CM
AS
Reaction R
esulted in Strength Reduction in Silicates
Selected E
BC
systems
ndashH
fO2 -R
E-S
i along with co-doped rare earth silicates and rare earth alum
ino-silicates for optim
ized strength stability and temperature capability
ndashC
MA
S infiltrations can reduce the strength
350 646-Specially alloy toughened t like H
fO2
648-EBC Bond Coat Constituent 300
659-AE9762
150
EBC
s
EBC
s
HfO
2 -Si (Si-rich)
Yb
2 Si 2 O 7
250658-EBC H
fO2-Rare Earth-A
lumino Silicate
660-Y2Si2O
7657-Zr-RE silicate 669-Y
b2Si2O7
Strength MPa
200696-EBC Bond Coat Constituent
100681-H
fO2-Si
669-9762 with CM
AS 1350C 50hr reacted
693-HfO
2-Si with CM
AS 1350C 50hr reacted
5000
200 400
600 800
1000 1200
1400 1600
Temperature degC
Strength test data compared
Yb
2 Si2 O7 C
MA
S reacted tensile Y
b2 Si2 O
7 CM
AS reacted
specimen fracture surface
surface w
ww
nasagov 27
National Aeronautics and Space Adm
inistration
High Stability and C
MAS R
esistance Observed from
the Rare
Earth S
ilicon High M
elting Point C
oating Com
positions
ndashD
emonstrated C
MA
S resistance
of NAS
A R
E-Si S
ystem at
1500degC 100 hr
ndash S
ilica-rich phase precipitation ndash
Rare earth elem
ent leaching into the m
elts (low concentration ~9
Surface side of the m
ol)
CM
AS m
elts
Area A
Area B
ww
wnasagov
28
![Page 12: Hurst, Bernadette J. Puleo€¦ · G57, 40.00 mg CMAS SiO Wellman -Aygun Smialek Braue 0 49 mole%; such as NASA’s CMAS (with NiO DSC:020 OES Measured by EDS [#] Type Date/time :](https://reader033.fdocuments.us/reader033/viewer/2022060211/5f04cb127e708231d40fbc15/html5/thumbnails/12.jpg)
Front CM
AS side
National Aeronautics and Space Adm
inistration
CM
AS Related D
egradations in EBC
coated CM
Cs ndash
Laboratory Heat Flux Tests
minusC
MAS effects on EB
C-C
MC
temperature capability tested in laser high heat
flux creep-rupture rig bull
Accelerated failure of C
MC
in loading high heat flux conditions
EBC
coated CV
I-MI C
MC
with N
dYb silicate R
ESi bond coat tested Tsurface 2600degF TC
MC
2450degF
Front heated CM
AS
side B
ack cooled side
Creep strain
Time h
Front CM
AS
side
200h
05
ww
wnasagov
12
National Aeronautics and Space Adm
inistration
EBC
CM
AS
Surface Initial N
ucleation Dissolution R
eactions ndash
Ytterbium
-and yttrium-silicate silicates reactions and dissolutions in C
AM
S
ndash M
ore sluggish dissolution of ytterbium as com
pared to yttrium
Ytterbium
di-silicate surface CM
AS m
elts 50 Y
tterbium di-silicate surface C
MA
S melts 5 h
h 1300degC
1500degC$
Yttrium
mono-silicate surface C
MA
S Y
ttrium silicate surface C
MA
S melts 5 h
melts 50 h 1300degC
1500degC
A
hlborg and Zhu Surface amp C
oatings Technology 237 (2013) 79ndash87 w
ww
nasagov 13
National Aeronautics and Space Adm
inistration
Rare E
arth Apatite G
rain Grow
th ndash
Grain grow
th of apatite phase at 1500degC at various tim
es
Ytterbium
silicate system
50 hr 150 hr
200 hr
200 hr50 hr
150 hr
Yttrium
silicate system$
ww
wnasagov
14
National Aeronautics and Space Adm
inistration
Effect of C
MA
S R
eactions on Grain B
oundary Phases
ndash C
MA
S and grain boundary phase has higher A
l2 O3
content (17-22 mole
) bull
Eutectic region w
ith high Al2 O
3 content ~1200degC m
elting point bull
Loss of SiO
2 due to volatility
200 hr 1500degC
NA
SA
modified
CM
AS
Grain
boundary final phase ndash low
SiO
2 and high A
lumina
ww
wnasagov
15
National Aeronautics and Space Adm
inistration
Rare E
arth Dissolution in C
MA
S M
elts ndash
Non stoichiom
etric characteristics of the CM
AS
ndash rare earth silicate reacted apatite phases ndash up to 200 h testing
ndash D
ifference in partitioning of ytterbium vs yttrium
in apatite bull
Average AE
OR
E2 O
3 ratio ~ 068 for ytterbium silicate ndash C
MA
S system
bull
Average AE
OR
E2 O
3 ratio ~ 022 for yttrium silicate ndash C
MA
S system
C
omposition in apatite (100 hr)
SiO2
Ahlborg and Zhu Surface amp
Coatings Technology 237 (2013) 79ndash87
RE
2 O3
AEO
Yttrium
Silicate EBC
Com
position in apatite (100 hr)
Ytterbium
Silicate EBC
ww
wnasagov
16
National Aeronautics and Space Adm
inistration
Advanced N
AS
A E
BC
Developm
ents
NA
SA advanced E
BC
systems em
phasizing high stability HfO
2 -and ZrO2 -R
E2 O
3 -
EBC layer 2 region
EB
Cs
Mol
Mol
SiO
2 EB
C system
RE
2 Si2-x O
7-2x such as (YbG
dY) 2 S
i2-x O7-2x
-Controlled dissolution and m
aintaining coating stability
(YbGdY) 2 S
i2-x O7-2x in
CM
AS
1300degC
(a)
(b)
ww
wnasagov
17
National Aeronautics and Space Adm
inistration E
xample of N
AS
A A
dvanced Environm
ental Barrier C
oating on S
iCSiC
CM
C System
s
Advanced EB
C coated vanes
HfO
2 -(YbG
dY)2 O
3
(YbG
dY)2 Si2-x O
7-2x
RESi(O
)+Hf B
ond Coat
Gd Y
b Y
O
Si
Yb
Gd Y
Si
Hf
A
lternating layered HfO
2 -Multicom
ponent Rare E
arth silicate EB
Cs used for fundam
ental stability studies
2700degF capable YbG
d-YbO+H
f based bond coats C
oated onto SiC
SiC
CM
C substrates using E
B-P
VD
The bond coat region
ww
wnasagov
18
National Aeronautics and Space Adm
inistration
CM
AS
Resistant Tests
ndash JE
Ts test of more advanced coating system
s at 2700F
Plasma sprayed (G
dY)2 Si2 O
7 2450 cycles
Special processed Yb
2 Si2 O7 spalling at 450 C
ycles EB
-PVD
(YbG
dY)2 Si2 O
7 total 4450 JETS cycles 100h
2450 4450
450
Hybrid H
f-rare earth aluminate silicate com
pleted 4450 cycles 100h
Hybrid H
ybrid Zr-rare earth silicate completed 4450
cycles 100h
2450 4450
2450 with
CM
AS 2450
ww
wnasagov
19
National Aeronautics and Space Adm
inistration
High S
tability and CM
AS
Resistance are E
nsured by Advanced H
igh M
elting Point C
oating and Multi-C
omponent C
ompositions A
rea A
Area B
ndash G
enerally improved C
MA
S
resistance of NAS
A R
ESi
System
at 1500degC 100 hr
ndash S
ilica-rich phase precipitation ndash
Rare earth elem
ent leaching into the m
elts (low concentration
~9mol
)
Surface side of the C
MA
S melts
EDS E
ww
wnasagov
20
National Aeronautics and Space Adm
inistration
Advanced E
BC
-CM
C S
ystem D
emonstrated 300 hr H
igh Cycle and
Low Fatigue D
urability in High H
eat Flux 2700degF Test Conditions
Specimen after 300 h testing
-A turbine airfoil E
BC
with H
fO2 -rare earth silicate and G
dYbSi bond coat on C
VI-M
I CM
C
substrate system selected for heat flux durability testing
-Laser high heat flux rig H
igh Cycle and Low
Cycle Fatigue test perform
ed at Stress
amplitude 10 ksi fatigue frequency 3 H
z at EB
C and 1 hr therm
al gradient cycles -
Tested EB
C surface tem
perature 1537degC (2800degF) and T bond coat tem
perature 1482degC
(2700degF) with C
MA
S
-D
emonstrated 300 hour durability at 2700degF+
-D
etermined fatigue-creep and therm
al conductivity behavior of the EB
C-C
MC
system
Specimen in rig testing
Test Condition Sum
mary
-EB
CC
VI-M
I Fatigue$loading 10 ksi (69 M
Pa) R
=005 with 1 hr Therm
al LC
F$-
TEB
C-surface 1537degC
(2800degF)$-
Tbond coat 1482degC
(2700degF)$-
Tback C
MC
surface 1250degC
(2282degF)
ww
wnasagov
21
National Aeronautics and Space Adm
inistration
Advanced E
BC
-CM
C Fatigue Test w
ith CM
AS
and in Steam
Jet Tested 300 h D
urability in High H
eat Flux Fatigue Test Conditions
-A
dvanced Hf-N
dYb silicate-N
dYbS
i bond coat EB
C coatings on 3D
architecture C
VI-P
IP S
iC-S
iC C
MC
(EB
-PV
D processing)
-Further understanding w
ater vapor -environmental interactions necessary
Surface view C
MA
S 35m
gcm2)
Back view
CM
AS
35mgcm
2)
ww
wnasagov
National Aeronautics and Space Adm
inistration
EBC
System
Designs ndash E
ffects of Com
posites and Clustered
Com
positions -
An alternating H
fO2 -and R
E-silicate coatings (EB
-PV
D processing) ndash H
fO2 -layer
infiltration and rare earth silicate layer melting
EB
-PV
D P
rocessed EB
Cs alternating H
fO2 -rich and ytterbium
silicate layer systems for
CM
AS
and impact resistance
ww
wnasagov
National Aeronautics and Space Adm
inistration
Sum
mary
bullC
MA
S degradation rem
ains a challenge for emerging turbine engine
environmental barrier coating ndash S
iCSiC
CM
C com
ponent systems
bullC
MA
S leads to low
er melting point of E
BC and bond coat system
s with
accelerated EBC
and CM
C degradations
bullN
AS
A advanced E
BC com
positions showed som
e promise for C
MA
S
resistance at temperatures up to 1500degC
in high velocity high heat flux and m
echanical loading tests bull
Currently focus on better understanding of E
BC com
positions and EBC
-CM
AS
interactions particularly with hafnium
zirconium and rare
earth silicates for improved tem
perature capability and CM
AS
resistance bull
Also standardize C
MA
S testing and quantify C
MA
S induced life debits
helping validate life modeling
bullC
ontrolling the compositions for C
MA
S resistance w
hile maintaining
high toughness continued to be a key emphasis
ww
wnasagov
24
National Aeronautics and Space Adm
inistration
Acknow
ledgements
bullThe w
ork was supported by N
ASA Fundam
ental Aeronautics Program (FAP)
Transformational Tools and Technologies (TTT) Project
bullThe authors are grateful to D
r Michael H
elminiak in the assistant of JETS tests
ww
wnasagov
25
National Aeronautics and Space Adm
inistration
CM
AS
Reaction K
inetics in Bond C
oats ndash S
iO2 rich phase partitioning in the C
MA
S m
elts ndash R
are earth content leaching low even at 1500degC
ndash M
ore advanced compositions are being im
plemented for im
proved thermom
echanical ndash
CM
AS Partitioning on R
E-Si bond coat 1500degC
100hr
RE incorporations
CM
AS
resistance
ww
wnasagov
26
National Aeronautics and Space Adm
inistration Strength R
esults of Selected EBC and EBC
Bond Coats
-CM
AS
Reaction R
esulted in Strength Reduction in Silicates
Selected E
BC
systems
ndashH
fO2 -R
E-S
i along with co-doped rare earth silicates and rare earth alum
ino-silicates for optim
ized strength stability and temperature capability
ndashC
MA
S infiltrations can reduce the strength
350 646-Specially alloy toughened t like H
fO2
648-EBC Bond Coat Constituent 300
659-AE9762
150
EBC
s
EBC
s
HfO
2 -Si (Si-rich)
Yb
2 Si 2 O 7
250658-EBC H
fO2-Rare Earth-A
lumino Silicate
660-Y2Si2O
7657-Zr-RE silicate 669-Y
b2Si2O7
Strength MPa
200696-EBC Bond Coat Constituent
100681-H
fO2-Si
669-9762 with CM
AS 1350C 50hr reacted
693-HfO
2-Si with CM
AS 1350C 50hr reacted
5000
200 400
600 800
1000 1200
1400 1600
Temperature degC
Strength test data compared
Yb
2 Si2 O7 C
MA
S reacted tensile Y
b2 Si2 O
7 CM
AS reacted
specimen fracture surface
surface w
ww
nasagov 27
National Aeronautics and Space Adm
inistration
High Stability and C
MAS R
esistance Observed from
the Rare
Earth S
ilicon High M
elting Point C
oating Com
positions
ndashD
emonstrated C
MA
S resistance
of NAS
A R
E-Si S
ystem at
1500degC 100 hr
ndash S
ilica-rich phase precipitation ndash
Rare earth elem
ent leaching into the m
elts (low concentration ~9
Surface side of the m
ol)
CM
AS m
elts
Area A
Area B
ww
wnasagov
28
![Page 13: Hurst, Bernadette J. Puleo€¦ · G57, 40.00 mg CMAS SiO Wellman -Aygun Smialek Braue 0 49 mole%; such as NASA’s CMAS (with NiO DSC:020 OES Measured by EDS [#] Type Date/time :](https://reader033.fdocuments.us/reader033/viewer/2022060211/5f04cb127e708231d40fbc15/html5/thumbnails/13.jpg)
National Aeronautics and Space Adm
inistration
EBC
CM
AS
Surface Initial N
ucleation Dissolution R
eactions ndash
Ytterbium
-and yttrium-silicate silicates reactions and dissolutions in C
AM
S
ndash M
ore sluggish dissolution of ytterbium as com
pared to yttrium
Ytterbium
di-silicate surface CM
AS m
elts 50 Y
tterbium di-silicate surface C
MA
S melts 5 h
h 1300degC
1500degC$
Yttrium
mono-silicate surface C
MA
S Y
ttrium silicate surface C
MA
S melts 5 h
melts 50 h 1300degC
1500degC
A
hlborg and Zhu Surface amp C
oatings Technology 237 (2013) 79ndash87 w
ww
nasagov 13
National Aeronautics and Space Adm
inistration
Rare E
arth Apatite G
rain Grow
th ndash
Grain grow
th of apatite phase at 1500degC at various tim
es
Ytterbium
silicate system
50 hr 150 hr
200 hr
200 hr50 hr
150 hr
Yttrium
silicate system$
ww
wnasagov
14
National Aeronautics and Space Adm
inistration
Effect of C
MA
S R
eactions on Grain B
oundary Phases
ndash C
MA
S and grain boundary phase has higher A
l2 O3
content (17-22 mole
) bull
Eutectic region w
ith high Al2 O
3 content ~1200degC m
elting point bull
Loss of SiO
2 due to volatility
200 hr 1500degC
NA
SA
modified
CM
AS
Grain
boundary final phase ndash low
SiO
2 and high A
lumina
ww
wnasagov
15
National Aeronautics and Space Adm
inistration
Rare E
arth Dissolution in C
MA
S M
elts ndash
Non stoichiom
etric characteristics of the CM
AS
ndash rare earth silicate reacted apatite phases ndash up to 200 h testing
ndash D
ifference in partitioning of ytterbium vs yttrium
in apatite bull
Average AE
OR
E2 O
3 ratio ~ 068 for ytterbium silicate ndash C
MA
S system
bull
Average AE
OR
E2 O
3 ratio ~ 022 for yttrium silicate ndash C
MA
S system
C
omposition in apatite (100 hr)
SiO2
Ahlborg and Zhu Surface amp
Coatings Technology 237 (2013) 79ndash87
RE
2 O3
AEO
Yttrium
Silicate EBC
Com
position in apatite (100 hr)
Ytterbium
Silicate EBC
ww
wnasagov
16
National Aeronautics and Space Adm
inistration
Advanced N
AS
A E
BC
Developm
ents
NA
SA advanced E
BC
systems em
phasizing high stability HfO
2 -and ZrO2 -R
E2 O
3 -
EBC layer 2 region
EB
Cs
Mol
Mol
SiO
2 EB
C system
RE
2 Si2-x O
7-2x such as (YbG
dY) 2 S
i2-x O7-2x
-Controlled dissolution and m
aintaining coating stability
(YbGdY) 2 S
i2-x O7-2x in
CM
AS
1300degC
(a)
(b)
ww
wnasagov
17
National Aeronautics and Space Adm
inistration E
xample of N
AS
A A
dvanced Environm
ental Barrier C
oating on S
iCSiC
CM
C System
s
Advanced EB
C coated vanes
HfO
2 -(YbG
dY)2 O
3
(YbG
dY)2 Si2-x O
7-2x
RESi(O
)+Hf B
ond Coat
Gd Y
b Y
O
Si
Yb
Gd Y
Si
Hf
A
lternating layered HfO
2 -Multicom
ponent Rare E
arth silicate EB
Cs used for fundam
ental stability studies
2700degF capable YbG
d-YbO+H
f based bond coats C
oated onto SiC
SiC
CM
C substrates using E
B-P
VD
The bond coat region
ww
wnasagov
18
National Aeronautics and Space Adm
inistration
CM
AS
Resistant Tests
ndash JE
Ts test of more advanced coating system
s at 2700F
Plasma sprayed (G
dY)2 Si2 O
7 2450 cycles
Special processed Yb
2 Si2 O7 spalling at 450 C
ycles EB
-PVD
(YbG
dY)2 Si2 O
7 total 4450 JETS cycles 100h
2450 4450
450
Hybrid H
f-rare earth aluminate silicate com
pleted 4450 cycles 100h
Hybrid H
ybrid Zr-rare earth silicate completed 4450
cycles 100h
2450 4450
2450 with
CM
AS 2450
ww
wnasagov
19
National Aeronautics and Space Adm
inistration
High S
tability and CM
AS
Resistance are E
nsured by Advanced H
igh M
elting Point C
oating and Multi-C
omponent C
ompositions A
rea A
Area B
ndash G
enerally improved C
MA
S
resistance of NAS
A R
ESi
System
at 1500degC 100 hr
ndash S
ilica-rich phase precipitation ndash
Rare earth elem
ent leaching into the m
elts (low concentration
~9mol
)
Surface side of the C
MA
S melts
EDS E
ww
wnasagov
20
National Aeronautics and Space Adm
inistration
Advanced E
BC
-CM
C S
ystem D
emonstrated 300 hr H
igh Cycle and
Low Fatigue D
urability in High H
eat Flux 2700degF Test Conditions
Specimen after 300 h testing
-A turbine airfoil E
BC
with H
fO2 -rare earth silicate and G
dYbSi bond coat on C
VI-M
I CM
C
substrate system selected for heat flux durability testing
-Laser high heat flux rig H
igh Cycle and Low
Cycle Fatigue test perform
ed at Stress
amplitude 10 ksi fatigue frequency 3 H
z at EB
C and 1 hr therm
al gradient cycles -
Tested EB
C surface tem
perature 1537degC (2800degF) and T bond coat tem
perature 1482degC
(2700degF) with C
MA
S
-D
emonstrated 300 hour durability at 2700degF+
-D
etermined fatigue-creep and therm
al conductivity behavior of the EB
C-C
MC
system
Specimen in rig testing
Test Condition Sum
mary
-EB
CC
VI-M
I Fatigue$loading 10 ksi (69 M
Pa) R
=005 with 1 hr Therm
al LC
F$-
TEB
C-surface 1537degC
(2800degF)$-
Tbond coat 1482degC
(2700degF)$-
Tback C
MC
surface 1250degC
(2282degF)
ww
wnasagov
21
National Aeronautics and Space Adm
inistration
Advanced E
BC
-CM
C Fatigue Test w
ith CM
AS
and in Steam
Jet Tested 300 h D
urability in High H
eat Flux Fatigue Test Conditions
-A
dvanced Hf-N
dYb silicate-N
dYbS
i bond coat EB
C coatings on 3D
architecture C
VI-P
IP S
iC-S
iC C
MC
(EB
-PV
D processing)
-Further understanding w
ater vapor -environmental interactions necessary
Surface view C
MA
S 35m
gcm2)
Back view
CM
AS
35mgcm
2)
ww
wnasagov
National Aeronautics and Space Adm
inistration
EBC
System
Designs ndash E
ffects of Com
posites and Clustered
Com
positions -
An alternating H
fO2 -and R
E-silicate coatings (EB
-PV
D processing) ndash H
fO2 -layer
infiltration and rare earth silicate layer melting
EB
-PV
D P
rocessed EB
Cs alternating H
fO2 -rich and ytterbium
silicate layer systems for
CM
AS
and impact resistance
ww
wnasagov
National Aeronautics and Space Adm
inistration
Sum
mary
bullC
MA
S degradation rem
ains a challenge for emerging turbine engine
environmental barrier coating ndash S
iCSiC
CM
C com
ponent systems
bullC
MA
S leads to low
er melting point of E
BC and bond coat system
s with
accelerated EBC
and CM
C degradations
bullN
AS
A advanced E
BC com
positions showed som
e promise for C
MA
S
resistance at temperatures up to 1500degC
in high velocity high heat flux and m
echanical loading tests bull
Currently focus on better understanding of E
BC com
positions and EBC
-CM
AS
interactions particularly with hafnium
zirconium and rare
earth silicates for improved tem
perature capability and CM
AS
resistance bull
Also standardize C
MA
S testing and quantify C
MA
S induced life debits
helping validate life modeling
bullC
ontrolling the compositions for C
MA
S resistance w
hile maintaining
high toughness continued to be a key emphasis
ww
wnasagov
24
National Aeronautics and Space Adm
inistration
Acknow
ledgements
bullThe w
ork was supported by N
ASA Fundam
ental Aeronautics Program (FAP)
Transformational Tools and Technologies (TTT) Project
bullThe authors are grateful to D
r Michael H
elminiak in the assistant of JETS tests
ww
wnasagov
25
National Aeronautics and Space Adm
inistration
CM
AS
Reaction K
inetics in Bond C
oats ndash S
iO2 rich phase partitioning in the C
MA
S m
elts ndash R
are earth content leaching low even at 1500degC
ndash M
ore advanced compositions are being im
plemented for im
proved thermom
echanical ndash
CM
AS Partitioning on R
E-Si bond coat 1500degC
100hr
RE incorporations
CM
AS
resistance
ww
wnasagov
26
National Aeronautics and Space Adm
inistration Strength R
esults of Selected EBC and EBC
Bond Coats
-CM
AS
Reaction R
esulted in Strength Reduction in Silicates
Selected E
BC
systems
ndashH
fO2 -R
E-S
i along with co-doped rare earth silicates and rare earth alum
ino-silicates for optim
ized strength stability and temperature capability
ndashC
MA
S infiltrations can reduce the strength
350 646-Specially alloy toughened t like H
fO2
648-EBC Bond Coat Constituent 300
659-AE9762
150
EBC
s
EBC
s
HfO
2 -Si (Si-rich)
Yb
2 Si 2 O 7
250658-EBC H
fO2-Rare Earth-A
lumino Silicate
660-Y2Si2O
7657-Zr-RE silicate 669-Y
b2Si2O7
Strength MPa
200696-EBC Bond Coat Constituent
100681-H
fO2-Si
669-9762 with CM
AS 1350C 50hr reacted
693-HfO
2-Si with CM
AS 1350C 50hr reacted
5000
200 400
600 800
1000 1200
1400 1600
Temperature degC
Strength test data compared
Yb
2 Si2 O7 C
MA
S reacted tensile Y
b2 Si2 O
7 CM
AS reacted
specimen fracture surface
surface w
ww
nasagov 27
National Aeronautics and Space Adm
inistration
High Stability and C
MAS R
esistance Observed from
the Rare
Earth S
ilicon High M
elting Point C
oating Com
positions
ndashD
emonstrated C
MA
S resistance
of NAS
A R
E-Si S
ystem at
1500degC 100 hr
ndash S
ilica-rich phase precipitation ndash
Rare earth elem
ent leaching into the m
elts (low concentration ~9
Surface side of the m
ol)
CM
AS m
elts
Area A
Area B
ww
wnasagov
28
![Page 14: Hurst, Bernadette J. Puleo€¦ · G57, 40.00 mg CMAS SiO Wellman -Aygun Smialek Braue 0 49 mole%; such as NASA’s CMAS (with NiO DSC:020 OES Measured by EDS [#] Type Date/time :](https://reader033.fdocuments.us/reader033/viewer/2022060211/5f04cb127e708231d40fbc15/html5/thumbnails/14.jpg)
National Aeronautics and Space Adm
inistration
Rare E
arth Apatite G
rain Grow
th ndash
Grain grow
th of apatite phase at 1500degC at various tim
es
Ytterbium
silicate system
50 hr 150 hr
200 hr
200 hr50 hr
150 hr
Yttrium
silicate system$
ww
wnasagov
14
National Aeronautics and Space Adm
inistration
Effect of C
MA
S R
eactions on Grain B
oundary Phases
ndash C
MA
S and grain boundary phase has higher A
l2 O3
content (17-22 mole
) bull
Eutectic region w
ith high Al2 O
3 content ~1200degC m
elting point bull
Loss of SiO
2 due to volatility
200 hr 1500degC
NA
SA
modified
CM
AS
Grain
boundary final phase ndash low
SiO
2 and high A
lumina
ww
wnasagov
15
National Aeronautics and Space Adm
inistration
Rare E
arth Dissolution in C
MA
S M
elts ndash
Non stoichiom
etric characteristics of the CM
AS
ndash rare earth silicate reacted apatite phases ndash up to 200 h testing
ndash D
ifference in partitioning of ytterbium vs yttrium
in apatite bull
Average AE
OR
E2 O
3 ratio ~ 068 for ytterbium silicate ndash C
MA
S system
bull
Average AE
OR
E2 O
3 ratio ~ 022 for yttrium silicate ndash C
MA
S system
C
omposition in apatite (100 hr)
SiO2
Ahlborg and Zhu Surface amp
Coatings Technology 237 (2013) 79ndash87
RE
2 O3
AEO
Yttrium
Silicate EBC
Com
position in apatite (100 hr)
Ytterbium
Silicate EBC
ww
wnasagov
16
National Aeronautics and Space Adm
inistration
Advanced N
AS
A E
BC
Developm
ents
NA
SA advanced E
BC
systems em
phasizing high stability HfO
2 -and ZrO2 -R
E2 O
3 -
EBC layer 2 region
EB
Cs
Mol
Mol
SiO
2 EB
C system
RE
2 Si2-x O
7-2x such as (YbG
dY) 2 S
i2-x O7-2x
-Controlled dissolution and m
aintaining coating stability
(YbGdY) 2 S
i2-x O7-2x in
CM
AS
1300degC
(a)
(b)
ww
wnasagov
17
National Aeronautics and Space Adm
inistration E
xample of N
AS
A A
dvanced Environm
ental Barrier C
oating on S
iCSiC
CM
C System
s
Advanced EB
C coated vanes
HfO
2 -(YbG
dY)2 O
3
(YbG
dY)2 Si2-x O
7-2x
RESi(O
)+Hf B
ond Coat
Gd Y
b Y
O
Si
Yb
Gd Y
Si
Hf
A
lternating layered HfO
2 -Multicom
ponent Rare E
arth silicate EB
Cs used for fundam
ental stability studies
2700degF capable YbG
d-YbO+H
f based bond coats C
oated onto SiC
SiC
CM
C substrates using E
B-P
VD
The bond coat region
ww
wnasagov
18
National Aeronautics and Space Adm
inistration
CM
AS
Resistant Tests
ndash JE
Ts test of more advanced coating system
s at 2700F
Plasma sprayed (G
dY)2 Si2 O
7 2450 cycles
Special processed Yb
2 Si2 O7 spalling at 450 C
ycles EB
-PVD
(YbG
dY)2 Si2 O
7 total 4450 JETS cycles 100h
2450 4450
450
Hybrid H
f-rare earth aluminate silicate com
pleted 4450 cycles 100h
Hybrid H
ybrid Zr-rare earth silicate completed 4450
cycles 100h
2450 4450
2450 with
CM
AS 2450
ww
wnasagov
19
National Aeronautics and Space Adm
inistration
High S
tability and CM
AS
Resistance are E
nsured by Advanced H
igh M
elting Point C
oating and Multi-C
omponent C
ompositions A
rea A
Area B
ndash G
enerally improved C
MA
S
resistance of NAS
A R
ESi
System
at 1500degC 100 hr
ndash S
ilica-rich phase precipitation ndash
Rare earth elem
ent leaching into the m
elts (low concentration
~9mol
)
Surface side of the C
MA
S melts
EDS E
ww
wnasagov
20
National Aeronautics and Space Adm
inistration
Advanced E
BC
-CM
C S
ystem D
emonstrated 300 hr H
igh Cycle and
Low Fatigue D
urability in High H
eat Flux 2700degF Test Conditions
Specimen after 300 h testing
-A turbine airfoil E
BC
with H
fO2 -rare earth silicate and G
dYbSi bond coat on C
VI-M
I CM
C
substrate system selected for heat flux durability testing
-Laser high heat flux rig H
igh Cycle and Low
Cycle Fatigue test perform
ed at Stress
amplitude 10 ksi fatigue frequency 3 H
z at EB
C and 1 hr therm
al gradient cycles -
Tested EB
C surface tem
perature 1537degC (2800degF) and T bond coat tem
perature 1482degC
(2700degF) with C
MA
S
-D
emonstrated 300 hour durability at 2700degF+
-D
etermined fatigue-creep and therm
al conductivity behavior of the EB
C-C
MC
system
Specimen in rig testing
Test Condition Sum
mary
-EB
CC
VI-M
I Fatigue$loading 10 ksi (69 M
Pa) R
=005 with 1 hr Therm
al LC
F$-
TEB
C-surface 1537degC
(2800degF)$-
Tbond coat 1482degC
(2700degF)$-
Tback C
MC
surface 1250degC
(2282degF)
ww
wnasagov
21
National Aeronautics and Space Adm
inistration
Advanced E
BC
-CM
C Fatigue Test w
ith CM
AS
and in Steam
Jet Tested 300 h D
urability in High H
eat Flux Fatigue Test Conditions
-A
dvanced Hf-N
dYb silicate-N
dYbS
i bond coat EB
C coatings on 3D
architecture C
VI-P
IP S
iC-S
iC C
MC
(EB
-PV
D processing)
-Further understanding w
ater vapor -environmental interactions necessary
Surface view C
MA
S 35m
gcm2)
Back view
CM
AS
35mgcm
2)
ww
wnasagov
National Aeronautics and Space Adm
inistration
EBC
System
Designs ndash E
ffects of Com
posites and Clustered
Com
positions -
An alternating H
fO2 -and R
E-silicate coatings (EB
-PV
D processing) ndash H
fO2 -layer
infiltration and rare earth silicate layer melting
EB
-PV
D P
rocessed EB
Cs alternating H
fO2 -rich and ytterbium
silicate layer systems for
CM
AS
and impact resistance
ww
wnasagov
National Aeronautics and Space Adm
inistration
Sum
mary
bullC
MA
S degradation rem
ains a challenge for emerging turbine engine
environmental barrier coating ndash S
iCSiC
CM
C com
ponent systems
bullC
MA
S leads to low
er melting point of E
BC and bond coat system
s with
accelerated EBC
and CM
C degradations
bullN
AS
A advanced E
BC com
positions showed som
e promise for C
MA
S
resistance at temperatures up to 1500degC
in high velocity high heat flux and m
echanical loading tests bull
Currently focus on better understanding of E
BC com
positions and EBC
-CM
AS
interactions particularly with hafnium
zirconium and rare
earth silicates for improved tem
perature capability and CM
AS
resistance bull
Also standardize C
MA
S testing and quantify C
MA
S induced life debits
helping validate life modeling
bullC
ontrolling the compositions for C
MA
S resistance w
hile maintaining
high toughness continued to be a key emphasis
ww
wnasagov
24
National Aeronautics and Space Adm
inistration
Acknow
ledgements
bullThe w
ork was supported by N
ASA Fundam
ental Aeronautics Program (FAP)
Transformational Tools and Technologies (TTT) Project
bullThe authors are grateful to D
r Michael H
elminiak in the assistant of JETS tests
ww
wnasagov
25
National Aeronautics and Space Adm
inistration
CM
AS
Reaction K
inetics in Bond C
oats ndash S
iO2 rich phase partitioning in the C
MA
S m
elts ndash R
are earth content leaching low even at 1500degC
ndash M
ore advanced compositions are being im
plemented for im
proved thermom
echanical ndash
CM
AS Partitioning on R
E-Si bond coat 1500degC
100hr
RE incorporations
CM
AS
resistance
ww
wnasagov
26
National Aeronautics and Space Adm
inistration Strength R
esults of Selected EBC and EBC
Bond Coats
-CM
AS
Reaction R
esulted in Strength Reduction in Silicates
Selected E
BC
systems
ndashH
fO2 -R
E-S
i along with co-doped rare earth silicates and rare earth alum
ino-silicates for optim
ized strength stability and temperature capability
ndashC
MA
S infiltrations can reduce the strength
350 646-Specially alloy toughened t like H
fO2
648-EBC Bond Coat Constituent 300
659-AE9762
150
EBC
s
EBC
s
HfO
2 -Si (Si-rich)
Yb
2 Si 2 O 7
250658-EBC H
fO2-Rare Earth-A
lumino Silicate
660-Y2Si2O
7657-Zr-RE silicate 669-Y
b2Si2O7
Strength MPa
200696-EBC Bond Coat Constituent
100681-H
fO2-Si
669-9762 with CM
AS 1350C 50hr reacted
693-HfO
2-Si with CM
AS 1350C 50hr reacted
5000
200 400
600 800
1000 1200
1400 1600
Temperature degC
Strength test data compared
Yb
2 Si2 O7 C
MA
S reacted tensile Y
b2 Si2 O
7 CM
AS reacted
specimen fracture surface
surface w
ww
nasagov 27
National Aeronautics and Space Adm
inistration
High Stability and C
MAS R
esistance Observed from
the Rare
Earth S
ilicon High M
elting Point C
oating Com
positions
ndashD
emonstrated C
MA
S resistance
of NAS
A R
E-Si S
ystem at
1500degC 100 hr
ndash S
ilica-rich phase precipitation ndash
Rare earth elem
ent leaching into the m
elts (low concentration ~9
Surface side of the m
ol)
CM
AS m
elts
Area A
Area B
ww
wnasagov
28
![Page 15: Hurst, Bernadette J. Puleo€¦ · G57, 40.00 mg CMAS SiO Wellman -Aygun Smialek Braue 0 49 mole%; such as NASA’s CMAS (with NiO DSC:020 OES Measured by EDS [#] Type Date/time :](https://reader033.fdocuments.us/reader033/viewer/2022060211/5f04cb127e708231d40fbc15/html5/thumbnails/15.jpg)
National Aeronautics and Space Adm
inistration
Effect of C
MA
S R
eactions on Grain B
oundary Phases
ndash C
MA
S and grain boundary phase has higher A
l2 O3
content (17-22 mole
) bull
Eutectic region w
ith high Al2 O
3 content ~1200degC m
elting point bull
Loss of SiO
2 due to volatility
200 hr 1500degC
NA
SA
modified
CM
AS
Grain
boundary final phase ndash low
SiO
2 and high A
lumina
ww
wnasagov
15
National Aeronautics and Space Adm
inistration
Rare E
arth Dissolution in C
MA
S M
elts ndash
Non stoichiom
etric characteristics of the CM
AS
ndash rare earth silicate reacted apatite phases ndash up to 200 h testing
ndash D
ifference in partitioning of ytterbium vs yttrium
in apatite bull
Average AE
OR
E2 O
3 ratio ~ 068 for ytterbium silicate ndash C
MA
S system
bull
Average AE
OR
E2 O
3 ratio ~ 022 for yttrium silicate ndash C
MA
S system
C
omposition in apatite (100 hr)
SiO2
Ahlborg and Zhu Surface amp
Coatings Technology 237 (2013) 79ndash87
RE
2 O3
AEO
Yttrium
Silicate EBC
Com
position in apatite (100 hr)
Ytterbium
Silicate EBC
ww
wnasagov
16
National Aeronautics and Space Adm
inistration
Advanced N
AS
A E
BC
Developm
ents
NA
SA advanced E
BC
systems em
phasizing high stability HfO
2 -and ZrO2 -R
E2 O
3 -
EBC layer 2 region
EB
Cs
Mol
Mol
SiO
2 EB
C system
RE
2 Si2-x O
7-2x such as (YbG
dY) 2 S
i2-x O7-2x
-Controlled dissolution and m
aintaining coating stability
(YbGdY) 2 S
i2-x O7-2x in
CM
AS
1300degC
(a)
(b)
ww
wnasagov
17
National Aeronautics and Space Adm
inistration E
xample of N
AS
A A
dvanced Environm
ental Barrier C
oating on S
iCSiC
CM
C System
s
Advanced EB
C coated vanes
HfO
2 -(YbG
dY)2 O
3
(YbG
dY)2 Si2-x O
7-2x
RESi(O
)+Hf B
ond Coat
Gd Y
b Y
O
Si
Yb
Gd Y
Si
Hf
A
lternating layered HfO
2 -Multicom
ponent Rare E
arth silicate EB
Cs used for fundam
ental stability studies
2700degF capable YbG
d-YbO+H
f based bond coats C
oated onto SiC
SiC
CM
C substrates using E
B-P
VD
The bond coat region
ww
wnasagov
18
National Aeronautics and Space Adm
inistration
CM
AS
Resistant Tests
ndash JE
Ts test of more advanced coating system
s at 2700F
Plasma sprayed (G
dY)2 Si2 O
7 2450 cycles
Special processed Yb
2 Si2 O7 spalling at 450 C
ycles EB
-PVD
(YbG
dY)2 Si2 O
7 total 4450 JETS cycles 100h
2450 4450
450
Hybrid H
f-rare earth aluminate silicate com
pleted 4450 cycles 100h
Hybrid H
ybrid Zr-rare earth silicate completed 4450
cycles 100h
2450 4450
2450 with
CM
AS 2450
ww
wnasagov
19
National Aeronautics and Space Adm
inistration
High S
tability and CM
AS
Resistance are E
nsured by Advanced H
igh M
elting Point C
oating and Multi-C
omponent C
ompositions A
rea A
Area B
ndash G
enerally improved C
MA
S
resistance of NAS
A R
ESi
System
at 1500degC 100 hr
ndash S
ilica-rich phase precipitation ndash
Rare earth elem
ent leaching into the m
elts (low concentration
~9mol
)
Surface side of the C
MA
S melts
EDS E
ww
wnasagov
20
National Aeronautics and Space Adm
inistration
Advanced E
BC
-CM
C S
ystem D
emonstrated 300 hr H
igh Cycle and
Low Fatigue D
urability in High H
eat Flux 2700degF Test Conditions
Specimen after 300 h testing
-A turbine airfoil E
BC
with H
fO2 -rare earth silicate and G
dYbSi bond coat on C
VI-M
I CM
C
substrate system selected for heat flux durability testing
-Laser high heat flux rig H
igh Cycle and Low
Cycle Fatigue test perform
ed at Stress
amplitude 10 ksi fatigue frequency 3 H
z at EB
C and 1 hr therm
al gradient cycles -
Tested EB
C surface tem
perature 1537degC (2800degF) and T bond coat tem
perature 1482degC
(2700degF) with C
MA
S
-D
emonstrated 300 hour durability at 2700degF+
-D
etermined fatigue-creep and therm
al conductivity behavior of the EB
C-C
MC
system
Specimen in rig testing
Test Condition Sum
mary
-EB
CC
VI-M
I Fatigue$loading 10 ksi (69 M
Pa) R
=005 with 1 hr Therm
al LC
F$-
TEB
C-surface 1537degC
(2800degF)$-
Tbond coat 1482degC
(2700degF)$-
Tback C
MC
surface 1250degC
(2282degF)
ww
wnasagov
21
National Aeronautics and Space Adm
inistration
Advanced E
BC
-CM
C Fatigue Test w
ith CM
AS
and in Steam
Jet Tested 300 h D
urability in High H
eat Flux Fatigue Test Conditions
-A
dvanced Hf-N
dYb silicate-N
dYbS
i bond coat EB
C coatings on 3D
architecture C
VI-P
IP S
iC-S
iC C
MC
(EB
-PV
D processing)
-Further understanding w
ater vapor -environmental interactions necessary
Surface view C
MA
S 35m
gcm2)
Back view
CM
AS
35mgcm
2)
ww
wnasagov
National Aeronautics and Space Adm
inistration
EBC
System
Designs ndash E
ffects of Com
posites and Clustered
Com
positions -
An alternating H
fO2 -and R
E-silicate coatings (EB
-PV
D processing) ndash H
fO2 -layer
infiltration and rare earth silicate layer melting
EB
-PV
D P
rocessed EB
Cs alternating H
fO2 -rich and ytterbium
silicate layer systems for
CM
AS
and impact resistance
ww
wnasagov
National Aeronautics and Space Adm
inistration
Sum
mary
bullC
MA
S degradation rem
ains a challenge for emerging turbine engine
environmental barrier coating ndash S
iCSiC
CM
C com
ponent systems
bullC
MA
S leads to low
er melting point of E
BC and bond coat system
s with
accelerated EBC
and CM
C degradations
bullN
AS
A advanced E
BC com
positions showed som
e promise for C
MA
S
resistance at temperatures up to 1500degC
in high velocity high heat flux and m
echanical loading tests bull
Currently focus on better understanding of E
BC com
positions and EBC
-CM
AS
interactions particularly with hafnium
zirconium and rare
earth silicates for improved tem
perature capability and CM
AS
resistance bull
Also standardize C
MA
S testing and quantify C
MA
S induced life debits
helping validate life modeling
bullC
ontrolling the compositions for C
MA
S resistance w
hile maintaining
high toughness continued to be a key emphasis
ww
wnasagov
24
National Aeronautics and Space Adm
inistration
Acknow
ledgements
bullThe w
ork was supported by N
ASA Fundam
ental Aeronautics Program (FAP)
Transformational Tools and Technologies (TTT) Project
bullThe authors are grateful to D
r Michael H
elminiak in the assistant of JETS tests
ww
wnasagov
25
National Aeronautics and Space Adm
inistration
CM
AS
Reaction K
inetics in Bond C
oats ndash S
iO2 rich phase partitioning in the C
MA
S m
elts ndash R
are earth content leaching low even at 1500degC
ndash M
ore advanced compositions are being im
plemented for im
proved thermom
echanical ndash
CM
AS Partitioning on R
E-Si bond coat 1500degC
100hr
RE incorporations
CM
AS
resistance
ww
wnasagov
26
National Aeronautics and Space Adm
inistration Strength R
esults of Selected EBC and EBC
Bond Coats
-CM
AS
Reaction R
esulted in Strength Reduction in Silicates
Selected E
BC
systems
ndashH
fO2 -R
E-S
i along with co-doped rare earth silicates and rare earth alum
ino-silicates for optim
ized strength stability and temperature capability
ndashC
MA
S infiltrations can reduce the strength
350 646-Specially alloy toughened t like H
fO2
648-EBC Bond Coat Constituent 300
659-AE9762
150
EBC
s
EBC
s
HfO
2 -Si (Si-rich)
Yb
2 Si 2 O 7
250658-EBC H
fO2-Rare Earth-A
lumino Silicate
660-Y2Si2O
7657-Zr-RE silicate 669-Y
b2Si2O7
Strength MPa
200696-EBC Bond Coat Constituent
100681-H
fO2-Si
669-9762 with CM
AS 1350C 50hr reacted
693-HfO
2-Si with CM
AS 1350C 50hr reacted
5000
200 400
600 800
1000 1200
1400 1600
Temperature degC
Strength test data compared
Yb
2 Si2 O7 C
MA
S reacted tensile Y
b2 Si2 O
7 CM
AS reacted
specimen fracture surface
surface w
ww
nasagov 27
National Aeronautics and Space Adm
inistration
High Stability and C
MAS R
esistance Observed from
the Rare
Earth S
ilicon High M
elting Point C
oating Com
positions
ndashD
emonstrated C
MA
S resistance
of NAS
A R
E-Si S
ystem at
1500degC 100 hr
ndash S
ilica-rich phase precipitation ndash
Rare earth elem
ent leaching into the m
elts (low concentration ~9
Surface side of the m
ol)
CM
AS m
elts
Area A
Area B
ww
wnasagov
28
![Page 16: Hurst, Bernadette J. Puleo€¦ · G57, 40.00 mg CMAS SiO Wellman -Aygun Smialek Braue 0 49 mole%; such as NASA’s CMAS (with NiO DSC:020 OES Measured by EDS [#] Type Date/time :](https://reader033.fdocuments.us/reader033/viewer/2022060211/5f04cb127e708231d40fbc15/html5/thumbnails/16.jpg)
National Aeronautics and Space Adm
inistration
Rare E
arth Dissolution in C
MA
S M
elts ndash
Non stoichiom
etric characteristics of the CM
AS
ndash rare earth silicate reacted apatite phases ndash up to 200 h testing
ndash D
ifference in partitioning of ytterbium vs yttrium
in apatite bull
Average AE
OR
E2 O
3 ratio ~ 068 for ytterbium silicate ndash C
MA
S system
bull
Average AE
OR
E2 O
3 ratio ~ 022 for yttrium silicate ndash C
MA
S system
C
omposition in apatite (100 hr)
SiO2
Ahlborg and Zhu Surface amp
Coatings Technology 237 (2013) 79ndash87
RE
2 O3
AEO
Yttrium
Silicate EBC
Com
position in apatite (100 hr)
Ytterbium
Silicate EBC
ww
wnasagov
16
National Aeronautics and Space Adm
inistration
Advanced N
AS
A E
BC
Developm
ents
NA
SA advanced E
BC
systems em
phasizing high stability HfO
2 -and ZrO2 -R
E2 O
3 -
EBC layer 2 region
EB
Cs
Mol
Mol
SiO
2 EB
C system
RE
2 Si2-x O
7-2x such as (YbG
dY) 2 S
i2-x O7-2x
-Controlled dissolution and m
aintaining coating stability
(YbGdY) 2 S
i2-x O7-2x in
CM
AS
1300degC
(a)
(b)
ww
wnasagov
17
National Aeronautics and Space Adm
inistration E
xample of N
AS
A A
dvanced Environm
ental Barrier C
oating on S
iCSiC
CM
C System
s
Advanced EB
C coated vanes
HfO
2 -(YbG
dY)2 O
3
(YbG
dY)2 Si2-x O
7-2x
RESi(O
)+Hf B
ond Coat
Gd Y
b Y
O
Si
Yb
Gd Y
Si
Hf
A
lternating layered HfO
2 -Multicom
ponent Rare E
arth silicate EB
Cs used for fundam
ental stability studies
2700degF capable YbG
d-YbO+H
f based bond coats C
oated onto SiC
SiC
CM
C substrates using E
B-P
VD
The bond coat region
ww
wnasagov
18
National Aeronautics and Space Adm
inistration
CM
AS
Resistant Tests
ndash JE
Ts test of more advanced coating system
s at 2700F
Plasma sprayed (G
dY)2 Si2 O
7 2450 cycles
Special processed Yb
2 Si2 O7 spalling at 450 C
ycles EB
-PVD
(YbG
dY)2 Si2 O
7 total 4450 JETS cycles 100h
2450 4450
450
Hybrid H
f-rare earth aluminate silicate com
pleted 4450 cycles 100h
Hybrid H
ybrid Zr-rare earth silicate completed 4450
cycles 100h
2450 4450
2450 with
CM
AS 2450
ww
wnasagov
19
National Aeronautics and Space Adm
inistration
High S
tability and CM
AS
Resistance are E
nsured by Advanced H
igh M
elting Point C
oating and Multi-C
omponent C
ompositions A
rea A
Area B
ndash G
enerally improved C
MA
S
resistance of NAS
A R
ESi
System
at 1500degC 100 hr
ndash S
ilica-rich phase precipitation ndash
Rare earth elem
ent leaching into the m
elts (low concentration
~9mol
)
Surface side of the C
MA
S melts
EDS E
ww
wnasagov
20
National Aeronautics and Space Adm
inistration
Advanced E
BC
-CM
C S
ystem D
emonstrated 300 hr H
igh Cycle and
Low Fatigue D
urability in High H
eat Flux 2700degF Test Conditions
Specimen after 300 h testing
-A turbine airfoil E
BC
with H
fO2 -rare earth silicate and G
dYbSi bond coat on C
VI-M
I CM
C
substrate system selected for heat flux durability testing
-Laser high heat flux rig H
igh Cycle and Low
Cycle Fatigue test perform
ed at Stress
amplitude 10 ksi fatigue frequency 3 H
z at EB
C and 1 hr therm
al gradient cycles -
Tested EB
C surface tem
perature 1537degC (2800degF) and T bond coat tem
perature 1482degC
(2700degF) with C
MA
S
-D
emonstrated 300 hour durability at 2700degF+
-D
etermined fatigue-creep and therm
al conductivity behavior of the EB
C-C
MC
system
Specimen in rig testing
Test Condition Sum
mary
-EB
CC
VI-M
I Fatigue$loading 10 ksi (69 M
Pa) R
=005 with 1 hr Therm
al LC
F$-
TEB
C-surface 1537degC
(2800degF)$-
Tbond coat 1482degC
(2700degF)$-
Tback C
MC
surface 1250degC
(2282degF)
ww
wnasagov
21
National Aeronautics and Space Adm
inistration
Advanced E
BC
-CM
C Fatigue Test w
ith CM
AS
and in Steam
Jet Tested 300 h D
urability in High H
eat Flux Fatigue Test Conditions
-A
dvanced Hf-N
dYb silicate-N
dYbS
i bond coat EB
C coatings on 3D
architecture C
VI-P
IP S
iC-S
iC C
MC
(EB
-PV
D processing)
-Further understanding w
ater vapor -environmental interactions necessary
Surface view C
MA
S 35m
gcm2)
Back view
CM
AS
35mgcm
2)
ww
wnasagov
National Aeronautics and Space Adm
inistration
EBC
System
Designs ndash E
ffects of Com
posites and Clustered
Com
positions -
An alternating H
fO2 -and R
E-silicate coatings (EB
-PV
D processing) ndash H
fO2 -layer
infiltration and rare earth silicate layer melting
EB
-PV
D P
rocessed EB
Cs alternating H
fO2 -rich and ytterbium
silicate layer systems for
CM
AS
and impact resistance
ww
wnasagov
National Aeronautics and Space Adm
inistration
Sum
mary
bullC
MA
S degradation rem
ains a challenge for emerging turbine engine
environmental barrier coating ndash S
iCSiC
CM
C com
ponent systems
bullC
MA
S leads to low
er melting point of E
BC and bond coat system
s with
accelerated EBC
and CM
C degradations
bullN
AS
A advanced E
BC com
positions showed som
e promise for C
MA
S
resistance at temperatures up to 1500degC
in high velocity high heat flux and m
echanical loading tests bull
Currently focus on better understanding of E
BC com
positions and EBC
-CM
AS
interactions particularly with hafnium
zirconium and rare
earth silicates for improved tem
perature capability and CM
AS
resistance bull
Also standardize C
MA
S testing and quantify C
MA
S induced life debits
helping validate life modeling
bullC
ontrolling the compositions for C
MA
S resistance w
hile maintaining
high toughness continued to be a key emphasis
ww
wnasagov
24
National Aeronautics and Space Adm
inistration
Acknow
ledgements
bullThe w
ork was supported by N
ASA Fundam
ental Aeronautics Program (FAP)
Transformational Tools and Technologies (TTT) Project
bullThe authors are grateful to D
r Michael H
elminiak in the assistant of JETS tests
ww
wnasagov
25
National Aeronautics and Space Adm
inistration
CM
AS
Reaction K
inetics in Bond C
oats ndash S
iO2 rich phase partitioning in the C
MA
S m
elts ndash R
are earth content leaching low even at 1500degC
ndash M
ore advanced compositions are being im
plemented for im
proved thermom
echanical ndash
CM
AS Partitioning on R
E-Si bond coat 1500degC
100hr
RE incorporations
CM
AS
resistance
ww
wnasagov
26
National Aeronautics and Space Adm
inistration Strength R
esults of Selected EBC and EBC
Bond Coats
-CM
AS
Reaction R
esulted in Strength Reduction in Silicates
Selected E
BC
systems
ndashH
fO2 -R
E-S
i along with co-doped rare earth silicates and rare earth alum
ino-silicates for optim
ized strength stability and temperature capability
ndashC
MA
S infiltrations can reduce the strength
350 646-Specially alloy toughened t like H
fO2
648-EBC Bond Coat Constituent 300
659-AE9762
150
EBC
s
EBC
s
HfO
2 -Si (Si-rich)
Yb
2 Si 2 O 7
250658-EBC H
fO2-Rare Earth-A
lumino Silicate
660-Y2Si2O
7657-Zr-RE silicate 669-Y
b2Si2O7
Strength MPa
200696-EBC Bond Coat Constituent
100681-H
fO2-Si
669-9762 with CM
AS 1350C 50hr reacted
693-HfO
2-Si with CM
AS 1350C 50hr reacted
5000
200 400
600 800
1000 1200
1400 1600
Temperature degC
Strength test data compared
Yb
2 Si2 O7 C
MA
S reacted tensile Y
b2 Si2 O
7 CM
AS reacted
specimen fracture surface
surface w
ww
nasagov 27
National Aeronautics and Space Adm
inistration
High Stability and C
MAS R
esistance Observed from
the Rare
Earth S
ilicon High M
elting Point C
oating Com
positions
ndashD
emonstrated C
MA
S resistance
of NAS
A R
E-Si S
ystem at
1500degC 100 hr
ndash S
ilica-rich phase precipitation ndash
Rare earth elem
ent leaching into the m
elts (low concentration ~9
Surface side of the m
ol)
CM
AS m
elts
Area A
Area B
ww
wnasagov
28
![Page 17: Hurst, Bernadette J. Puleo€¦ · G57, 40.00 mg CMAS SiO Wellman -Aygun Smialek Braue 0 49 mole%; such as NASA’s CMAS (with NiO DSC:020 OES Measured by EDS [#] Type Date/time :](https://reader033.fdocuments.us/reader033/viewer/2022060211/5f04cb127e708231d40fbc15/html5/thumbnails/17.jpg)
National Aeronautics and Space Adm
inistration
Advanced N
AS
A E
BC
Developm
ents
NA
SA advanced E
BC
systems em
phasizing high stability HfO
2 -and ZrO2 -R
E2 O
3 -
EBC layer 2 region
EB
Cs
Mol
Mol
SiO
2 EB
C system
RE
2 Si2-x O
7-2x such as (YbG
dY) 2 S
i2-x O7-2x
-Controlled dissolution and m
aintaining coating stability
(YbGdY) 2 S
i2-x O7-2x in
CM
AS
1300degC
(a)
(b)
ww
wnasagov
17
National Aeronautics and Space Adm
inistration E
xample of N
AS
A A
dvanced Environm
ental Barrier C
oating on S
iCSiC
CM
C System
s
Advanced EB
C coated vanes
HfO
2 -(YbG
dY)2 O
3
(YbG
dY)2 Si2-x O
7-2x
RESi(O
)+Hf B
ond Coat
Gd Y
b Y
O
Si
Yb
Gd Y
Si
Hf
A
lternating layered HfO
2 -Multicom
ponent Rare E
arth silicate EB
Cs used for fundam
ental stability studies
2700degF capable YbG
d-YbO+H
f based bond coats C
oated onto SiC
SiC
CM
C substrates using E
B-P
VD
The bond coat region
ww
wnasagov
18
National Aeronautics and Space Adm
inistration
CM
AS
Resistant Tests
ndash JE
Ts test of more advanced coating system
s at 2700F
Plasma sprayed (G
dY)2 Si2 O
7 2450 cycles
Special processed Yb
2 Si2 O7 spalling at 450 C
ycles EB
-PVD
(YbG
dY)2 Si2 O
7 total 4450 JETS cycles 100h
2450 4450
450
Hybrid H
f-rare earth aluminate silicate com
pleted 4450 cycles 100h
Hybrid H
ybrid Zr-rare earth silicate completed 4450
cycles 100h
2450 4450
2450 with
CM
AS 2450
ww
wnasagov
19
National Aeronautics and Space Adm
inistration
High S
tability and CM
AS
Resistance are E
nsured by Advanced H
igh M
elting Point C
oating and Multi-C
omponent C
ompositions A
rea A
Area B
ndash G
enerally improved C
MA
S
resistance of NAS
A R
ESi
System
at 1500degC 100 hr
ndash S
ilica-rich phase precipitation ndash
Rare earth elem
ent leaching into the m
elts (low concentration
~9mol
)
Surface side of the C
MA
S melts
EDS E
ww
wnasagov
20
National Aeronautics and Space Adm
inistration
Advanced E
BC
-CM
C S
ystem D
emonstrated 300 hr H
igh Cycle and
Low Fatigue D
urability in High H
eat Flux 2700degF Test Conditions
Specimen after 300 h testing
-A turbine airfoil E
BC
with H
fO2 -rare earth silicate and G
dYbSi bond coat on C
VI-M
I CM
C
substrate system selected for heat flux durability testing
-Laser high heat flux rig H
igh Cycle and Low
Cycle Fatigue test perform
ed at Stress
amplitude 10 ksi fatigue frequency 3 H
z at EB
C and 1 hr therm
al gradient cycles -
Tested EB
C surface tem
perature 1537degC (2800degF) and T bond coat tem
perature 1482degC
(2700degF) with C
MA
S
-D
emonstrated 300 hour durability at 2700degF+
-D
etermined fatigue-creep and therm
al conductivity behavior of the EB
C-C
MC
system
Specimen in rig testing
Test Condition Sum
mary
-EB
CC
VI-M
I Fatigue$loading 10 ksi (69 M
Pa) R
=005 with 1 hr Therm
al LC
F$-
TEB
C-surface 1537degC
(2800degF)$-
Tbond coat 1482degC
(2700degF)$-
Tback C
MC
surface 1250degC
(2282degF)
ww
wnasagov
21
National Aeronautics and Space Adm
inistration
Advanced E
BC
-CM
C Fatigue Test w
ith CM
AS
and in Steam
Jet Tested 300 h D
urability in High H
eat Flux Fatigue Test Conditions
-A
dvanced Hf-N
dYb silicate-N
dYbS
i bond coat EB
C coatings on 3D
architecture C
VI-P
IP S
iC-S
iC C
MC
(EB
-PV
D processing)
-Further understanding w
ater vapor -environmental interactions necessary
Surface view C
MA
S 35m
gcm2)
Back view
CM
AS
35mgcm
2)
ww
wnasagov
National Aeronautics and Space Adm
inistration
EBC
System
Designs ndash E
ffects of Com
posites and Clustered
Com
positions -
An alternating H
fO2 -and R
E-silicate coatings (EB
-PV
D processing) ndash H
fO2 -layer
infiltration and rare earth silicate layer melting
EB
-PV
D P
rocessed EB
Cs alternating H
fO2 -rich and ytterbium
silicate layer systems for
CM
AS
and impact resistance
ww
wnasagov
National Aeronautics and Space Adm
inistration
Sum
mary
bullC
MA
S degradation rem
ains a challenge for emerging turbine engine
environmental barrier coating ndash S
iCSiC
CM
C com
ponent systems
bullC
MA
S leads to low
er melting point of E
BC and bond coat system
s with
accelerated EBC
and CM
C degradations
bullN
AS
A advanced E
BC com
positions showed som
e promise for C
MA
S
resistance at temperatures up to 1500degC
in high velocity high heat flux and m
echanical loading tests bull
Currently focus on better understanding of E
BC com
positions and EBC
-CM
AS
interactions particularly with hafnium
zirconium and rare
earth silicates for improved tem
perature capability and CM
AS
resistance bull
Also standardize C
MA
S testing and quantify C
MA
S induced life debits
helping validate life modeling
bullC
ontrolling the compositions for C
MA
S resistance w
hile maintaining
high toughness continued to be a key emphasis
ww
wnasagov
24
National Aeronautics and Space Adm
inistration
Acknow
ledgements
bullThe w
ork was supported by N
ASA Fundam
ental Aeronautics Program (FAP)
Transformational Tools and Technologies (TTT) Project
bullThe authors are grateful to D
r Michael H
elminiak in the assistant of JETS tests
ww
wnasagov
25
National Aeronautics and Space Adm
inistration
CM
AS
Reaction K
inetics in Bond C
oats ndash S
iO2 rich phase partitioning in the C
MA
S m
elts ndash R
are earth content leaching low even at 1500degC
ndash M
ore advanced compositions are being im
plemented for im
proved thermom
echanical ndash
CM
AS Partitioning on R
E-Si bond coat 1500degC
100hr
RE incorporations
CM
AS
resistance
ww
wnasagov
26
National Aeronautics and Space Adm
inistration Strength R
esults of Selected EBC and EBC
Bond Coats
-CM
AS
Reaction R
esulted in Strength Reduction in Silicates
Selected E
BC
systems
ndashH
fO2 -R
E-S
i along with co-doped rare earth silicates and rare earth alum
ino-silicates for optim
ized strength stability and temperature capability
ndashC
MA
S infiltrations can reduce the strength
350 646-Specially alloy toughened t like H
fO2
648-EBC Bond Coat Constituent 300
659-AE9762
150
EBC
s
EBC
s
HfO
2 -Si (Si-rich)
Yb
2 Si 2 O 7
250658-EBC H
fO2-Rare Earth-A
lumino Silicate
660-Y2Si2O
7657-Zr-RE silicate 669-Y
b2Si2O7
Strength MPa
200696-EBC Bond Coat Constituent
100681-H
fO2-Si
669-9762 with CM
AS 1350C 50hr reacted
693-HfO
2-Si with CM
AS 1350C 50hr reacted
5000
200 400
600 800
1000 1200
1400 1600
Temperature degC
Strength test data compared
Yb
2 Si2 O7 C
MA
S reacted tensile Y
b2 Si2 O
7 CM
AS reacted
specimen fracture surface
surface w
ww
nasagov 27
National Aeronautics and Space Adm
inistration
High Stability and C
MAS R
esistance Observed from
the Rare
Earth S
ilicon High M
elting Point C
oating Com
positions
ndashD
emonstrated C
MA
S resistance
of NAS
A R
E-Si S
ystem at
1500degC 100 hr
ndash S
ilica-rich phase precipitation ndash
Rare earth elem
ent leaching into the m
elts (low concentration ~9
Surface side of the m
ol)
CM
AS m
elts
Area A
Area B
ww
wnasagov
28
![Page 18: Hurst, Bernadette J. Puleo€¦ · G57, 40.00 mg CMAS SiO Wellman -Aygun Smialek Braue 0 49 mole%; such as NASA’s CMAS (with NiO DSC:020 OES Measured by EDS [#] Type Date/time :](https://reader033.fdocuments.us/reader033/viewer/2022060211/5f04cb127e708231d40fbc15/html5/thumbnails/18.jpg)
National Aeronautics and Space Adm
inistration E
xample of N
AS
A A
dvanced Environm
ental Barrier C
oating on S
iCSiC
CM
C System
s
Advanced EB
C coated vanes
HfO
2 -(YbG
dY)2 O
3
(YbG
dY)2 Si2-x O
7-2x
RESi(O
)+Hf B
ond Coat
Gd Y
b Y
O
Si
Yb
Gd Y
Si
Hf
A
lternating layered HfO
2 -Multicom
ponent Rare E
arth silicate EB
Cs used for fundam
ental stability studies
2700degF capable YbG
d-YbO+H
f based bond coats C
oated onto SiC
SiC
CM
C substrates using E
B-P
VD
The bond coat region
ww
wnasagov
18
National Aeronautics and Space Adm
inistration
CM
AS
Resistant Tests
ndash JE
Ts test of more advanced coating system
s at 2700F
Plasma sprayed (G
dY)2 Si2 O
7 2450 cycles
Special processed Yb
2 Si2 O7 spalling at 450 C
ycles EB
-PVD
(YbG
dY)2 Si2 O
7 total 4450 JETS cycles 100h
2450 4450
450
Hybrid H
f-rare earth aluminate silicate com
pleted 4450 cycles 100h
Hybrid H
ybrid Zr-rare earth silicate completed 4450
cycles 100h
2450 4450
2450 with
CM
AS 2450
ww
wnasagov
19
National Aeronautics and Space Adm
inistration
High S
tability and CM
AS
Resistance are E
nsured by Advanced H
igh M
elting Point C
oating and Multi-C
omponent C
ompositions A
rea A
Area B
ndash G
enerally improved C
MA
S
resistance of NAS
A R
ESi
System
at 1500degC 100 hr
ndash S
ilica-rich phase precipitation ndash
Rare earth elem
ent leaching into the m
elts (low concentration
~9mol
)
Surface side of the C
MA
S melts
EDS E
ww
wnasagov
20
National Aeronautics and Space Adm
inistration
Advanced E
BC
-CM
C S
ystem D
emonstrated 300 hr H
igh Cycle and
Low Fatigue D
urability in High H
eat Flux 2700degF Test Conditions
Specimen after 300 h testing
-A turbine airfoil E
BC
with H
fO2 -rare earth silicate and G
dYbSi bond coat on C
VI-M
I CM
C
substrate system selected for heat flux durability testing
-Laser high heat flux rig H
igh Cycle and Low
Cycle Fatigue test perform
ed at Stress
amplitude 10 ksi fatigue frequency 3 H
z at EB
C and 1 hr therm
al gradient cycles -
Tested EB
C surface tem
perature 1537degC (2800degF) and T bond coat tem
perature 1482degC
(2700degF) with C
MA
S
-D
emonstrated 300 hour durability at 2700degF+
-D
etermined fatigue-creep and therm
al conductivity behavior of the EB
C-C
MC
system
Specimen in rig testing
Test Condition Sum
mary
-EB
CC
VI-M
I Fatigue$loading 10 ksi (69 M
Pa) R
=005 with 1 hr Therm
al LC
F$-
TEB
C-surface 1537degC
(2800degF)$-
Tbond coat 1482degC
(2700degF)$-
Tback C
MC
surface 1250degC
(2282degF)
ww
wnasagov
21
National Aeronautics and Space Adm
inistration
Advanced E
BC
-CM
C Fatigue Test w
ith CM
AS
and in Steam
Jet Tested 300 h D
urability in High H
eat Flux Fatigue Test Conditions
-A
dvanced Hf-N
dYb silicate-N
dYbS
i bond coat EB
C coatings on 3D
architecture C
VI-P
IP S
iC-S
iC C
MC
(EB
-PV
D processing)
-Further understanding w
ater vapor -environmental interactions necessary
Surface view C
MA
S 35m
gcm2)
Back view
CM
AS
35mgcm
2)
ww
wnasagov
National Aeronautics and Space Adm
inistration
EBC
System
Designs ndash E
ffects of Com
posites and Clustered
Com
positions -
An alternating H
fO2 -and R
E-silicate coatings (EB
-PV
D processing) ndash H
fO2 -layer
infiltration and rare earth silicate layer melting
EB
-PV
D P
rocessed EB
Cs alternating H
fO2 -rich and ytterbium
silicate layer systems for
CM
AS
and impact resistance
ww
wnasagov
National Aeronautics and Space Adm
inistration
Sum
mary
bullC
MA
S degradation rem
ains a challenge for emerging turbine engine
environmental barrier coating ndash S
iCSiC
CM
C com
ponent systems
bullC
MA
S leads to low
er melting point of E
BC and bond coat system
s with
accelerated EBC
and CM
C degradations
bullN
AS
A advanced E
BC com
positions showed som
e promise for C
MA
S
resistance at temperatures up to 1500degC
in high velocity high heat flux and m
echanical loading tests bull
Currently focus on better understanding of E
BC com
positions and EBC
-CM
AS
interactions particularly with hafnium
zirconium and rare
earth silicates for improved tem
perature capability and CM
AS
resistance bull
Also standardize C
MA
S testing and quantify C
MA
S induced life debits
helping validate life modeling
bullC
ontrolling the compositions for C
MA
S resistance w
hile maintaining
high toughness continued to be a key emphasis
ww
wnasagov
24
National Aeronautics and Space Adm
inistration
Acknow
ledgements
bullThe w
ork was supported by N
ASA Fundam
ental Aeronautics Program (FAP)
Transformational Tools and Technologies (TTT) Project
bullThe authors are grateful to D
r Michael H
elminiak in the assistant of JETS tests
ww
wnasagov
25
National Aeronautics and Space Adm
inistration
CM
AS
Reaction K
inetics in Bond C
oats ndash S
iO2 rich phase partitioning in the C
MA
S m
elts ndash R
are earth content leaching low even at 1500degC
ndash M
ore advanced compositions are being im
plemented for im
proved thermom
echanical ndash
CM
AS Partitioning on R
E-Si bond coat 1500degC
100hr
RE incorporations
CM
AS
resistance
ww
wnasagov
26
National Aeronautics and Space Adm
inistration Strength R
esults of Selected EBC and EBC
Bond Coats
-CM
AS
Reaction R
esulted in Strength Reduction in Silicates
Selected E
BC
systems
ndashH
fO2 -R
E-S
i along with co-doped rare earth silicates and rare earth alum
ino-silicates for optim
ized strength stability and temperature capability
ndashC
MA
S infiltrations can reduce the strength
350 646-Specially alloy toughened t like H
fO2
648-EBC Bond Coat Constituent 300
659-AE9762
150
EBC
s
EBC
s
HfO
2 -Si (Si-rich)
Yb
2 Si 2 O 7
250658-EBC H
fO2-Rare Earth-A
lumino Silicate
660-Y2Si2O
7657-Zr-RE silicate 669-Y
b2Si2O7
Strength MPa
200696-EBC Bond Coat Constituent
100681-H
fO2-Si
669-9762 with CM
AS 1350C 50hr reacted
693-HfO
2-Si with CM
AS 1350C 50hr reacted
5000
200 400
600 800
1000 1200
1400 1600
Temperature degC
Strength test data compared
Yb
2 Si2 O7 C
MA
S reacted tensile Y
b2 Si2 O
7 CM
AS reacted
specimen fracture surface
surface w
ww
nasagov 27
National Aeronautics and Space Adm
inistration
High Stability and C
MAS R
esistance Observed from
the Rare
Earth S
ilicon High M
elting Point C
oating Com
positions
ndashD
emonstrated C
MA
S resistance
of NAS
A R
E-Si S
ystem at
1500degC 100 hr
ndash S
ilica-rich phase precipitation ndash
Rare earth elem
ent leaching into the m
elts (low concentration ~9
Surface side of the m
ol)
CM
AS m
elts
Area A
Area B
ww
wnasagov
28
![Page 19: Hurst, Bernadette J. Puleo€¦ · G57, 40.00 mg CMAS SiO Wellman -Aygun Smialek Braue 0 49 mole%; such as NASA’s CMAS (with NiO DSC:020 OES Measured by EDS [#] Type Date/time :](https://reader033.fdocuments.us/reader033/viewer/2022060211/5f04cb127e708231d40fbc15/html5/thumbnails/19.jpg)
National Aeronautics and Space Adm
inistration
CM
AS
Resistant Tests
ndash JE
Ts test of more advanced coating system
s at 2700F
Plasma sprayed (G
dY)2 Si2 O
7 2450 cycles
Special processed Yb
2 Si2 O7 spalling at 450 C
ycles EB
-PVD
(YbG
dY)2 Si2 O
7 total 4450 JETS cycles 100h
2450 4450
450
Hybrid H
f-rare earth aluminate silicate com
pleted 4450 cycles 100h
Hybrid H
ybrid Zr-rare earth silicate completed 4450
cycles 100h
2450 4450
2450 with
CM
AS 2450
ww
wnasagov
19
National Aeronautics and Space Adm
inistration
High S
tability and CM
AS
Resistance are E
nsured by Advanced H
igh M
elting Point C
oating and Multi-C
omponent C
ompositions A
rea A
Area B
ndash G
enerally improved C
MA
S
resistance of NAS
A R
ESi
System
at 1500degC 100 hr
ndash S
ilica-rich phase precipitation ndash
Rare earth elem
ent leaching into the m
elts (low concentration
~9mol
)
Surface side of the C
MA
S melts
EDS E
ww
wnasagov
20
National Aeronautics and Space Adm
inistration
Advanced E
BC
-CM
C S
ystem D
emonstrated 300 hr H
igh Cycle and
Low Fatigue D
urability in High H
eat Flux 2700degF Test Conditions
Specimen after 300 h testing
-A turbine airfoil E
BC
with H
fO2 -rare earth silicate and G
dYbSi bond coat on C
VI-M
I CM
C
substrate system selected for heat flux durability testing
-Laser high heat flux rig H
igh Cycle and Low
Cycle Fatigue test perform
ed at Stress
amplitude 10 ksi fatigue frequency 3 H
z at EB
C and 1 hr therm
al gradient cycles -
Tested EB
C surface tem
perature 1537degC (2800degF) and T bond coat tem
perature 1482degC
(2700degF) with C
MA
S
-D
emonstrated 300 hour durability at 2700degF+
-D
etermined fatigue-creep and therm
al conductivity behavior of the EB
C-C
MC
system
Specimen in rig testing
Test Condition Sum
mary
-EB
CC
VI-M
I Fatigue$loading 10 ksi (69 M
Pa) R
=005 with 1 hr Therm
al LC
F$-
TEB
C-surface 1537degC
(2800degF)$-
Tbond coat 1482degC
(2700degF)$-
Tback C
MC
surface 1250degC
(2282degF)
ww
wnasagov
21
National Aeronautics and Space Adm
inistration
Advanced E
BC
-CM
C Fatigue Test w
ith CM
AS
and in Steam
Jet Tested 300 h D
urability in High H
eat Flux Fatigue Test Conditions
-A
dvanced Hf-N
dYb silicate-N
dYbS
i bond coat EB
C coatings on 3D
architecture C
VI-P
IP S
iC-S
iC C
MC
(EB
-PV
D processing)
-Further understanding w
ater vapor -environmental interactions necessary
Surface view C
MA
S 35m
gcm2)
Back view
CM
AS
35mgcm
2)
ww
wnasagov
National Aeronautics and Space Adm
inistration
EBC
System
Designs ndash E
ffects of Com
posites and Clustered
Com
positions -
An alternating H
fO2 -and R
E-silicate coatings (EB
-PV
D processing) ndash H
fO2 -layer
infiltration and rare earth silicate layer melting
EB
-PV
D P
rocessed EB
Cs alternating H
fO2 -rich and ytterbium
silicate layer systems for
CM
AS
and impact resistance
ww
wnasagov
National Aeronautics and Space Adm
inistration
Sum
mary
bullC
MA
S degradation rem
ains a challenge for emerging turbine engine
environmental barrier coating ndash S
iCSiC
CM
C com
ponent systems
bullC
MA
S leads to low
er melting point of E
BC and bond coat system
s with
accelerated EBC
and CM
C degradations
bullN
AS
A advanced E
BC com
positions showed som
e promise for C
MA
S
resistance at temperatures up to 1500degC
in high velocity high heat flux and m
echanical loading tests bull
Currently focus on better understanding of E
BC com
positions and EBC
-CM
AS
interactions particularly with hafnium
zirconium and rare
earth silicates for improved tem
perature capability and CM
AS
resistance bull
Also standardize C
MA
S testing and quantify C
MA
S induced life debits
helping validate life modeling
bullC
ontrolling the compositions for C
MA
S resistance w
hile maintaining
high toughness continued to be a key emphasis
ww
wnasagov
24
National Aeronautics and Space Adm
inistration
Acknow
ledgements
bullThe w
ork was supported by N
ASA Fundam
ental Aeronautics Program (FAP)
Transformational Tools and Technologies (TTT) Project
bullThe authors are grateful to D
r Michael H
elminiak in the assistant of JETS tests
ww
wnasagov
25
National Aeronautics and Space Adm
inistration
CM
AS
Reaction K
inetics in Bond C
oats ndash S
iO2 rich phase partitioning in the C
MA
S m
elts ndash R
are earth content leaching low even at 1500degC
ndash M
ore advanced compositions are being im
plemented for im
proved thermom
echanical ndash
CM
AS Partitioning on R
E-Si bond coat 1500degC
100hr
RE incorporations
CM
AS
resistance
ww
wnasagov
26
National Aeronautics and Space Adm
inistration Strength R
esults of Selected EBC and EBC
Bond Coats
-CM
AS
Reaction R
esulted in Strength Reduction in Silicates
Selected E
BC
systems
ndashH
fO2 -R
E-S
i along with co-doped rare earth silicates and rare earth alum
ino-silicates for optim
ized strength stability and temperature capability
ndashC
MA
S infiltrations can reduce the strength
350 646-Specially alloy toughened t like H
fO2
648-EBC Bond Coat Constituent 300
659-AE9762
150
EBC
s
EBC
s
HfO
2 -Si (Si-rich)
Yb
2 Si 2 O 7
250658-EBC H
fO2-Rare Earth-A
lumino Silicate
660-Y2Si2O
7657-Zr-RE silicate 669-Y
b2Si2O7
Strength MPa
200696-EBC Bond Coat Constituent
100681-H
fO2-Si
669-9762 with CM
AS 1350C 50hr reacted
693-HfO
2-Si with CM
AS 1350C 50hr reacted
5000
200 400
600 800
1000 1200
1400 1600
Temperature degC
Strength test data compared
Yb
2 Si2 O7 C
MA
S reacted tensile Y
b2 Si2 O
7 CM
AS reacted
specimen fracture surface
surface w
ww
nasagov 27
National Aeronautics and Space Adm
inistration
High Stability and C
MAS R
esistance Observed from
the Rare
Earth S
ilicon High M
elting Point C
oating Com
positions
ndashD
emonstrated C
MA
S resistance
of NAS
A R
E-Si S
ystem at
1500degC 100 hr
ndash S
ilica-rich phase precipitation ndash
Rare earth elem
ent leaching into the m
elts (low concentration ~9
Surface side of the m
ol)
CM
AS m
elts
Area A
Area B
ww
wnasagov
28
![Page 20: Hurst, Bernadette J. Puleo€¦ · G57, 40.00 mg CMAS SiO Wellman -Aygun Smialek Braue 0 49 mole%; such as NASA’s CMAS (with NiO DSC:020 OES Measured by EDS [#] Type Date/time :](https://reader033.fdocuments.us/reader033/viewer/2022060211/5f04cb127e708231d40fbc15/html5/thumbnails/20.jpg)
National Aeronautics and Space Adm
inistration
High S
tability and CM
AS
Resistance are E
nsured by Advanced H
igh M
elting Point C
oating and Multi-C
omponent C
ompositions A
rea A
Area B
ndash G
enerally improved C
MA
S
resistance of NAS
A R
ESi
System
at 1500degC 100 hr
ndash S
ilica-rich phase precipitation ndash
Rare earth elem
ent leaching into the m
elts (low concentration
~9mol
)
Surface side of the C
MA
S melts
EDS E
ww
wnasagov
20
National Aeronautics and Space Adm
inistration
Advanced E
BC
-CM
C S
ystem D
emonstrated 300 hr H
igh Cycle and
Low Fatigue D
urability in High H
eat Flux 2700degF Test Conditions
Specimen after 300 h testing
-A turbine airfoil E
BC
with H
fO2 -rare earth silicate and G
dYbSi bond coat on C
VI-M
I CM
C
substrate system selected for heat flux durability testing
-Laser high heat flux rig H
igh Cycle and Low
Cycle Fatigue test perform
ed at Stress
amplitude 10 ksi fatigue frequency 3 H
z at EB
C and 1 hr therm
al gradient cycles -
Tested EB
C surface tem
perature 1537degC (2800degF) and T bond coat tem
perature 1482degC
(2700degF) with C
MA
S
-D
emonstrated 300 hour durability at 2700degF+
-D
etermined fatigue-creep and therm
al conductivity behavior of the EB
C-C
MC
system
Specimen in rig testing
Test Condition Sum
mary
-EB
CC
VI-M
I Fatigue$loading 10 ksi (69 M
Pa) R
=005 with 1 hr Therm
al LC
F$-
TEB
C-surface 1537degC
(2800degF)$-
Tbond coat 1482degC
(2700degF)$-
Tback C
MC
surface 1250degC
(2282degF)
ww
wnasagov
21
National Aeronautics and Space Adm
inistration
Advanced E
BC
-CM
C Fatigue Test w
ith CM
AS
and in Steam
Jet Tested 300 h D
urability in High H
eat Flux Fatigue Test Conditions
-A
dvanced Hf-N
dYb silicate-N
dYbS
i bond coat EB
C coatings on 3D
architecture C
VI-P
IP S
iC-S
iC C
MC
(EB
-PV
D processing)
-Further understanding w
ater vapor -environmental interactions necessary
Surface view C
MA
S 35m
gcm2)
Back view
CM
AS
35mgcm
2)
ww
wnasagov
National Aeronautics and Space Adm
inistration
EBC
System
Designs ndash E
ffects of Com
posites and Clustered
Com
positions -
An alternating H
fO2 -and R
E-silicate coatings (EB
-PV
D processing) ndash H
fO2 -layer
infiltration and rare earth silicate layer melting
EB
-PV
D P
rocessed EB
Cs alternating H
fO2 -rich and ytterbium
silicate layer systems for
CM
AS
and impact resistance
ww
wnasagov
National Aeronautics and Space Adm
inistration
Sum
mary
bullC
MA
S degradation rem
ains a challenge for emerging turbine engine
environmental barrier coating ndash S
iCSiC
CM
C com
ponent systems
bullC
MA
S leads to low
er melting point of E
BC and bond coat system
s with
accelerated EBC
and CM
C degradations
bullN
AS
A advanced E
BC com
positions showed som
e promise for C
MA
S
resistance at temperatures up to 1500degC
in high velocity high heat flux and m
echanical loading tests bull
Currently focus on better understanding of E
BC com
positions and EBC
-CM
AS
interactions particularly with hafnium
zirconium and rare
earth silicates for improved tem
perature capability and CM
AS
resistance bull
Also standardize C
MA
S testing and quantify C
MA
S induced life debits
helping validate life modeling
bullC
ontrolling the compositions for C
MA
S resistance w
hile maintaining
high toughness continued to be a key emphasis
ww
wnasagov
24
National Aeronautics and Space Adm
inistration
Acknow
ledgements
bullThe w
ork was supported by N
ASA Fundam
ental Aeronautics Program (FAP)
Transformational Tools and Technologies (TTT) Project
bullThe authors are grateful to D
r Michael H
elminiak in the assistant of JETS tests
ww
wnasagov
25
National Aeronautics and Space Adm
inistration
CM
AS
Reaction K
inetics in Bond C
oats ndash S
iO2 rich phase partitioning in the C
MA
S m
elts ndash R
are earth content leaching low even at 1500degC
ndash M
ore advanced compositions are being im
plemented for im
proved thermom
echanical ndash
CM
AS Partitioning on R
E-Si bond coat 1500degC
100hr
RE incorporations
CM
AS
resistance
ww
wnasagov
26
National Aeronautics and Space Adm
inistration Strength R
esults of Selected EBC and EBC
Bond Coats
-CM
AS
Reaction R
esulted in Strength Reduction in Silicates
Selected E
BC
systems
ndashH
fO2 -R
E-S
i along with co-doped rare earth silicates and rare earth alum
ino-silicates for optim
ized strength stability and temperature capability
ndashC
MA
S infiltrations can reduce the strength
350 646-Specially alloy toughened t like H
fO2
648-EBC Bond Coat Constituent 300
659-AE9762
150
EBC
s
EBC
s
HfO
2 -Si (Si-rich)
Yb
2 Si 2 O 7
250658-EBC H
fO2-Rare Earth-A
lumino Silicate
660-Y2Si2O
7657-Zr-RE silicate 669-Y
b2Si2O7
Strength MPa
200696-EBC Bond Coat Constituent
100681-H
fO2-Si
669-9762 with CM
AS 1350C 50hr reacted
693-HfO
2-Si with CM
AS 1350C 50hr reacted
5000
200 400
600 800
1000 1200
1400 1600
Temperature degC
Strength test data compared
Yb
2 Si2 O7 C
MA
S reacted tensile Y
b2 Si2 O
7 CM
AS reacted
specimen fracture surface
surface w
ww
nasagov 27
National Aeronautics and Space Adm
inistration
High Stability and C
MAS R
esistance Observed from
the Rare
Earth S
ilicon High M
elting Point C
oating Com
positions
ndashD
emonstrated C
MA
S resistance
of NAS
A R
E-Si S
ystem at
1500degC 100 hr
ndash S
ilica-rich phase precipitation ndash
Rare earth elem
ent leaching into the m
elts (low concentration ~9
Surface side of the m
ol)
CM
AS m
elts
Area A
Area B
ww
wnasagov
28
![Page 21: Hurst, Bernadette J. Puleo€¦ · G57, 40.00 mg CMAS SiO Wellman -Aygun Smialek Braue 0 49 mole%; such as NASA’s CMAS (with NiO DSC:020 OES Measured by EDS [#] Type Date/time :](https://reader033.fdocuments.us/reader033/viewer/2022060211/5f04cb127e708231d40fbc15/html5/thumbnails/21.jpg)
National Aeronautics and Space Adm
inistration
Advanced E
BC
-CM
C S
ystem D
emonstrated 300 hr H
igh Cycle and
Low Fatigue D
urability in High H
eat Flux 2700degF Test Conditions
Specimen after 300 h testing
-A turbine airfoil E
BC
with H
fO2 -rare earth silicate and G
dYbSi bond coat on C
VI-M
I CM
C
substrate system selected for heat flux durability testing
-Laser high heat flux rig H
igh Cycle and Low
Cycle Fatigue test perform
ed at Stress
amplitude 10 ksi fatigue frequency 3 H
z at EB
C and 1 hr therm
al gradient cycles -
Tested EB
C surface tem
perature 1537degC (2800degF) and T bond coat tem
perature 1482degC
(2700degF) with C
MA
S
-D
emonstrated 300 hour durability at 2700degF+
-D
etermined fatigue-creep and therm
al conductivity behavior of the EB
C-C
MC
system
Specimen in rig testing
Test Condition Sum
mary
-EB
CC
VI-M
I Fatigue$loading 10 ksi (69 M
Pa) R
=005 with 1 hr Therm
al LC
F$-
TEB
C-surface 1537degC
(2800degF)$-
Tbond coat 1482degC
(2700degF)$-
Tback C
MC
surface 1250degC
(2282degF)
ww
wnasagov
21
National Aeronautics and Space Adm
inistration
Advanced E
BC
-CM
C Fatigue Test w
ith CM
AS
and in Steam
Jet Tested 300 h D
urability in High H
eat Flux Fatigue Test Conditions
-A
dvanced Hf-N
dYb silicate-N
dYbS
i bond coat EB
C coatings on 3D
architecture C
VI-P
IP S
iC-S
iC C
MC
(EB
-PV
D processing)
-Further understanding w
ater vapor -environmental interactions necessary
Surface view C
MA
S 35m
gcm2)
Back view
CM
AS
35mgcm
2)
ww
wnasagov
National Aeronautics and Space Adm
inistration
EBC
System
Designs ndash E
ffects of Com
posites and Clustered
Com
positions -
An alternating H
fO2 -and R
E-silicate coatings (EB
-PV
D processing) ndash H
fO2 -layer
infiltration and rare earth silicate layer melting
EB
-PV
D P
rocessed EB
Cs alternating H
fO2 -rich and ytterbium
silicate layer systems for
CM
AS
and impact resistance
ww
wnasagov
National Aeronautics and Space Adm
inistration
Sum
mary
bullC
MA
S degradation rem
ains a challenge for emerging turbine engine
environmental barrier coating ndash S
iCSiC
CM
C com
ponent systems
bullC
MA
S leads to low
er melting point of E
BC and bond coat system
s with
accelerated EBC
and CM
C degradations
bullN
AS
A advanced E
BC com
positions showed som
e promise for C
MA
S
resistance at temperatures up to 1500degC
in high velocity high heat flux and m
echanical loading tests bull
Currently focus on better understanding of E
BC com
positions and EBC
-CM
AS
interactions particularly with hafnium
zirconium and rare
earth silicates for improved tem
perature capability and CM
AS
resistance bull
Also standardize C
MA
S testing and quantify C
MA
S induced life debits
helping validate life modeling
bullC
ontrolling the compositions for C
MA
S resistance w
hile maintaining
high toughness continued to be a key emphasis
ww
wnasagov
24
National Aeronautics and Space Adm
inistration
Acknow
ledgements
bullThe w
ork was supported by N
ASA Fundam
ental Aeronautics Program (FAP)
Transformational Tools and Technologies (TTT) Project
bullThe authors are grateful to D
r Michael H
elminiak in the assistant of JETS tests
ww
wnasagov
25
National Aeronautics and Space Adm
inistration
CM
AS
Reaction K
inetics in Bond C
oats ndash S
iO2 rich phase partitioning in the C
MA
S m
elts ndash R
are earth content leaching low even at 1500degC
ndash M
ore advanced compositions are being im
plemented for im
proved thermom
echanical ndash
CM
AS Partitioning on R
E-Si bond coat 1500degC
100hr
RE incorporations
CM
AS
resistance
ww
wnasagov
26
National Aeronautics and Space Adm
inistration Strength R
esults of Selected EBC and EBC
Bond Coats
-CM
AS
Reaction R
esulted in Strength Reduction in Silicates
Selected E
BC
systems
ndashH
fO2 -R
E-S
i along with co-doped rare earth silicates and rare earth alum
ino-silicates for optim
ized strength stability and temperature capability
ndashC
MA
S infiltrations can reduce the strength
350 646-Specially alloy toughened t like H
fO2
648-EBC Bond Coat Constituent 300
659-AE9762
150
EBC
s
EBC
s
HfO
2 -Si (Si-rich)
Yb
2 Si 2 O 7
250658-EBC H
fO2-Rare Earth-A
lumino Silicate
660-Y2Si2O
7657-Zr-RE silicate 669-Y
b2Si2O7
Strength MPa
200696-EBC Bond Coat Constituent
100681-H
fO2-Si
669-9762 with CM
AS 1350C 50hr reacted
693-HfO
2-Si with CM
AS 1350C 50hr reacted
5000
200 400
600 800
1000 1200
1400 1600
Temperature degC
Strength test data compared
Yb
2 Si2 O7 C
MA
S reacted tensile Y
b2 Si2 O
7 CM
AS reacted
specimen fracture surface
surface w
ww
nasagov 27
National Aeronautics and Space Adm
inistration
High Stability and C
MAS R
esistance Observed from
the Rare
Earth S
ilicon High M
elting Point C
oating Com
positions
ndashD
emonstrated C
MA
S resistance
of NAS
A R
E-Si S
ystem at
1500degC 100 hr
ndash S
ilica-rich phase precipitation ndash
Rare earth elem
ent leaching into the m
elts (low concentration ~9
Surface side of the m
ol)
CM
AS m
elts
Area A
Area B
ww
wnasagov
28
![Page 22: Hurst, Bernadette J. Puleo€¦ · G57, 40.00 mg CMAS SiO Wellman -Aygun Smialek Braue 0 49 mole%; such as NASA’s CMAS (with NiO DSC:020 OES Measured by EDS [#] Type Date/time :](https://reader033.fdocuments.us/reader033/viewer/2022060211/5f04cb127e708231d40fbc15/html5/thumbnails/22.jpg)
National Aeronautics and Space Adm
inistration
Advanced E
BC
-CM
C Fatigue Test w
ith CM
AS
and in Steam
Jet Tested 300 h D
urability in High H
eat Flux Fatigue Test Conditions
-A
dvanced Hf-N
dYb silicate-N
dYbS
i bond coat EB
C coatings on 3D
architecture C
VI-P
IP S
iC-S
iC C
MC
(EB
-PV
D processing)
-Further understanding w
ater vapor -environmental interactions necessary
Surface view C
MA
S 35m
gcm2)
Back view
CM
AS
35mgcm
2)
ww
wnasagov
National Aeronautics and Space Adm
inistration
EBC
System
Designs ndash E
ffects of Com
posites and Clustered
Com
positions -
An alternating H
fO2 -and R
E-silicate coatings (EB
-PV
D processing) ndash H
fO2 -layer
infiltration and rare earth silicate layer melting
EB
-PV
D P
rocessed EB
Cs alternating H
fO2 -rich and ytterbium
silicate layer systems for
CM
AS
and impact resistance
ww
wnasagov
National Aeronautics and Space Adm
inistration
Sum
mary
bullC
MA
S degradation rem
ains a challenge for emerging turbine engine
environmental barrier coating ndash S
iCSiC
CM
C com
ponent systems
bullC
MA
S leads to low
er melting point of E
BC and bond coat system
s with
accelerated EBC
and CM
C degradations
bullN
AS
A advanced E
BC com
positions showed som
e promise for C
MA
S
resistance at temperatures up to 1500degC
in high velocity high heat flux and m
echanical loading tests bull
Currently focus on better understanding of E
BC com
positions and EBC
-CM
AS
interactions particularly with hafnium
zirconium and rare
earth silicates for improved tem
perature capability and CM
AS
resistance bull
Also standardize C
MA
S testing and quantify C
MA
S induced life debits
helping validate life modeling
bullC
ontrolling the compositions for C
MA
S resistance w
hile maintaining
high toughness continued to be a key emphasis
ww
wnasagov
24
National Aeronautics and Space Adm
inistration
Acknow
ledgements
bullThe w
ork was supported by N
ASA Fundam
ental Aeronautics Program (FAP)
Transformational Tools and Technologies (TTT) Project
bullThe authors are grateful to D
r Michael H
elminiak in the assistant of JETS tests
ww
wnasagov
25
National Aeronautics and Space Adm
inistration
CM
AS
Reaction K
inetics in Bond C
oats ndash S
iO2 rich phase partitioning in the C
MA
S m
elts ndash R
are earth content leaching low even at 1500degC
ndash M
ore advanced compositions are being im
plemented for im
proved thermom
echanical ndash
CM
AS Partitioning on R
E-Si bond coat 1500degC
100hr
RE incorporations
CM
AS
resistance
ww
wnasagov
26
National Aeronautics and Space Adm
inistration Strength R
esults of Selected EBC and EBC
Bond Coats
-CM
AS
Reaction R
esulted in Strength Reduction in Silicates
Selected E
BC
systems
ndashH
fO2 -R
E-S
i along with co-doped rare earth silicates and rare earth alum
ino-silicates for optim
ized strength stability and temperature capability
ndashC
MA
S infiltrations can reduce the strength
350 646-Specially alloy toughened t like H
fO2
648-EBC Bond Coat Constituent 300
659-AE9762
150
EBC
s
EBC
s
HfO
2 -Si (Si-rich)
Yb
2 Si 2 O 7
250658-EBC H
fO2-Rare Earth-A
lumino Silicate
660-Y2Si2O
7657-Zr-RE silicate 669-Y
b2Si2O7
Strength MPa
200696-EBC Bond Coat Constituent
100681-H
fO2-Si
669-9762 with CM
AS 1350C 50hr reacted
693-HfO
2-Si with CM
AS 1350C 50hr reacted
5000
200 400
600 800
1000 1200
1400 1600
Temperature degC
Strength test data compared
Yb
2 Si2 O7 C
MA
S reacted tensile Y
b2 Si2 O
7 CM
AS reacted
specimen fracture surface
surface w
ww
nasagov 27
National Aeronautics and Space Adm
inistration
High Stability and C
MAS R
esistance Observed from
the Rare
Earth S
ilicon High M
elting Point C
oating Com
positions
ndashD
emonstrated C
MA
S resistance
of NAS
A R
E-Si S
ystem at
1500degC 100 hr
ndash S
ilica-rich phase precipitation ndash
Rare earth elem
ent leaching into the m
elts (low concentration ~9
Surface side of the m
ol)
CM
AS m
elts
Area A
Area B
ww
wnasagov
28
![Page 23: Hurst, Bernadette J. Puleo€¦ · G57, 40.00 mg CMAS SiO Wellman -Aygun Smialek Braue 0 49 mole%; such as NASA’s CMAS (with NiO DSC:020 OES Measured by EDS [#] Type Date/time :](https://reader033.fdocuments.us/reader033/viewer/2022060211/5f04cb127e708231d40fbc15/html5/thumbnails/23.jpg)
National Aeronautics and Space Adm
inistration
EBC
System
Designs ndash E
ffects of Com
posites and Clustered
Com
positions -
An alternating H
fO2 -and R
E-silicate coatings (EB
-PV
D processing) ndash H
fO2 -layer
infiltration and rare earth silicate layer melting
EB
-PV
D P
rocessed EB
Cs alternating H
fO2 -rich and ytterbium
silicate layer systems for
CM
AS
and impact resistance
ww
wnasagov
National Aeronautics and Space Adm
inistration
Sum
mary
bullC
MA
S degradation rem
ains a challenge for emerging turbine engine
environmental barrier coating ndash S
iCSiC
CM
C com
ponent systems
bullC
MA
S leads to low
er melting point of E
BC and bond coat system
s with
accelerated EBC
and CM
C degradations
bullN
AS
A advanced E
BC com
positions showed som
e promise for C
MA
S
resistance at temperatures up to 1500degC
in high velocity high heat flux and m
echanical loading tests bull
Currently focus on better understanding of E
BC com
positions and EBC
-CM
AS
interactions particularly with hafnium
zirconium and rare
earth silicates for improved tem
perature capability and CM
AS
resistance bull
Also standardize C
MA
S testing and quantify C
MA
S induced life debits
helping validate life modeling
bullC
ontrolling the compositions for C
MA
S resistance w
hile maintaining
high toughness continued to be a key emphasis
ww
wnasagov
24
National Aeronautics and Space Adm
inistration
Acknow
ledgements
bullThe w
ork was supported by N
ASA Fundam
ental Aeronautics Program (FAP)
Transformational Tools and Technologies (TTT) Project
bullThe authors are grateful to D
r Michael H
elminiak in the assistant of JETS tests
ww
wnasagov
25
National Aeronautics and Space Adm
inistration
CM
AS
Reaction K
inetics in Bond C
oats ndash S
iO2 rich phase partitioning in the C
MA
S m
elts ndash R
are earth content leaching low even at 1500degC
ndash M
ore advanced compositions are being im
plemented for im
proved thermom
echanical ndash
CM
AS Partitioning on R
E-Si bond coat 1500degC
100hr
RE incorporations
CM
AS
resistance
ww
wnasagov
26
National Aeronautics and Space Adm
inistration Strength R
esults of Selected EBC and EBC
Bond Coats
-CM
AS
Reaction R
esulted in Strength Reduction in Silicates
Selected E
BC
systems
ndashH
fO2 -R
E-S
i along with co-doped rare earth silicates and rare earth alum
ino-silicates for optim
ized strength stability and temperature capability
ndashC
MA
S infiltrations can reduce the strength
350 646-Specially alloy toughened t like H
fO2
648-EBC Bond Coat Constituent 300
659-AE9762
150
EBC
s
EBC
s
HfO
2 -Si (Si-rich)
Yb
2 Si 2 O 7
250658-EBC H
fO2-Rare Earth-A
lumino Silicate
660-Y2Si2O
7657-Zr-RE silicate 669-Y
b2Si2O7
Strength MPa
200696-EBC Bond Coat Constituent
100681-H
fO2-Si
669-9762 with CM
AS 1350C 50hr reacted
693-HfO
2-Si with CM
AS 1350C 50hr reacted
5000
200 400
600 800
1000 1200
1400 1600
Temperature degC
Strength test data compared
Yb
2 Si2 O7 C
MA
S reacted tensile Y
b2 Si2 O
7 CM
AS reacted
specimen fracture surface
surface w
ww
nasagov 27
National Aeronautics and Space Adm
inistration
High Stability and C
MAS R
esistance Observed from
the Rare
Earth S
ilicon High M
elting Point C
oating Com
positions
ndashD
emonstrated C
MA
S resistance
of NAS
A R
E-Si S
ystem at
1500degC 100 hr
ndash S
ilica-rich phase precipitation ndash
Rare earth elem
ent leaching into the m
elts (low concentration ~9
Surface side of the m
ol)
CM
AS m
elts
Area A
Area B
ww
wnasagov
28
![Page 24: Hurst, Bernadette J. Puleo€¦ · G57, 40.00 mg CMAS SiO Wellman -Aygun Smialek Braue 0 49 mole%; such as NASA’s CMAS (with NiO DSC:020 OES Measured by EDS [#] Type Date/time :](https://reader033.fdocuments.us/reader033/viewer/2022060211/5f04cb127e708231d40fbc15/html5/thumbnails/24.jpg)
National Aeronautics and Space Adm
inistration
Sum
mary
bullC
MA
S degradation rem
ains a challenge for emerging turbine engine
environmental barrier coating ndash S
iCSiC
CM
C com
ponent systems
bullC
MA
S leads to low
er melting point of E
BC and bond coat system
s with
accelerated EBC
and CM
C degradations
bullN
AS
A advanced E
BC com
positions showed som
e promise for C
MA
S
resistance at temperatures up to 1500degC
in high velocity high heat flux and m
echanical loading tests bull
Currently focus on better understanding of E
BC com
positions and EBC
-CM
AS
interactions particularly with hafnium
zirconium and rare
earth silicates for improved tem
perature capability and CM
AS
resistance bull
Also standardize C
MA
S testing and quantify C
MA
S induced life debits
helping validate life modeling
bullC
ontrolling the compositions for C
MA
S resistance w
hile maintaining
high toughness continued to be a key emphasis
ww
wnasagov
24
National Aeronautics and Space Adm
inistration
Acknow
ledgements
bullThe w
ork was supported by N
ASA Fundam
ental Aeronautics Program (FAP)
Transformational Tools and Technologies (TTT) Project
bullThe authors are grateful to D
r Michael H
elminiak in the assistant of JETS tests
ww
wnasagov
25
National Aeronautics and Space Adm
inistration
CM
AS
Reaction K
inetics in Bond C
oats ndash S
iO2 rich phase partitioning in the C
MA
S m
elts ndash R
are earth content leaching low even at 1500degC
ndash M
ore advanced compositions are being im
plemented for im
proved thermom
echanical ndash
CM
AS Partitioning on R
E-Si bond coat 1500degC
100hr
RE incorporations
CM
AS
resistance
ww
wnasagov
26
National Aeronautics and Space Adm
inistration Strength R
esults of Selected EBC and EBC
Bond Coats
-CM
AS
Reaction R
esulted in Strength Reduction in Silicates
Selected E
BC
systems
ndashH
fO2 -R
E-S
i along with co-doped rare earth silicates and rare earth alum
ino-silicates for optim
ized strength stability and temperature capability
ndashC
MA
S infiltrations can reduce the strength
350 646-Specially alloy toughened t like H
fO2
648-EBC Bond Coat Constituent 300
659-AE9762
150
EBC
s
EBC
s
HfO
2 -Si (Si-rich)
Yb
2 Si 2 O 7
250658-EBC H
fO2-Rare Earth-A
lumino Silicate
660-Y2Si2O
7657-Zr-RE silicate 669-Y
b2Si2O7
Strength MPa
200696-EBC Bond Coat Constituent
100681-H
fO2-Si
669-9762 with CM
AS 1350C 50hr reacted
693-HfO
2-Si with CM
AS 1350C 50hr reacted
5000
200 400
600 800
1000 1200
1400 1600
Temperature degC
Strength test data compared
Yb
2 Si2 O7 C
MA
S reacted tensile Y
b2 Si2 O
7 CM
AS reacted
specimen fracture surface
surface w
ww
nasagov 27
National Aeronautics and Space Adm
inistration
High Stability and C
MAS R
esistance Observed from
the Rare
Earth S
ilicon High M
elting Point C
oating Com
positions
ndashD
emonstrated C
MA
S resistance
of NAS
A R
E-Si S
ystem at
1500degC 100 hr
ndash S
ilica-rich phase precipitation ndash
Rare earth elem
ent leaching into the m
elts (low concentration ~9
Surface side of the m
ol)
CM
AS m
elts
Area A
Area B
ww
wnasagov
28
![Page 25: Hurst, Bernadette J. Puleo€¦ · G57, 40.00 mg CMAS SiO Wellman -Aygun Smialek Braue 0 49 mole%; such as NASA’s CMAS (with NiO DSC:020 OES Measured by EDS [#] Type Date/time :](https://reader033.fdocuments.us/reader033/viewer/2022060211/5f04cb127e708231d40fbc15/html5/thumbnails/25.jpg)
National Aeronautics and Space Adm
inistration
Acknow
ledgements
bullThe w
ork was supported by N
ASA Fundam
ental Aeronautics Program (FAP)
Transformational Tools and Technologies (TTT) Project
bullThe authors are grateful to D
r Michael H
elminiak in the assistant of JETS tests
ww
wnasagov
25
National Aeronautics and Space Adm
inistration
CM
AS
Reaction K
inetics in Bond C
oats ndash S
iO2 rich phase partitioning in the C
MA
S m
elts ndash R
are earth content leaching low even at 1500degC
ndash M
ore advanced compositions are being im
plemented for im
proved thermom
echanical ndash
CM
AS Partitioning on R
E-Si bond coat 1500degC
100hr
RE incorporations
CM
AS
resistance
ww
wnasagov
26
National Aeronautics and Space Adm
inistration Strength R
esults of Selected EBC and EBC
Bond Coats
-CM
AS
Reaction R
esulted in Strength Reduction in Silicates
Selected E
BC
systems
ndashH
fO2 -R
E-S
i along with co-doped rare earth silicates and rare earth alum
ino-silicates for optim
ized strength stability and temperature capability
ndashC
MA
S infiltrations can reduce the strength
350 646-Specially alloy toughened t like H
fO2
648-EBC Bond Coat Constituent 300
659-AE9762
150
EBC
s
EBC
s
HfO
2 -Si (Si-rich)
Yb
2 Si 2 O 7
250658-EBC H
fO2-Rare Earth-A
lumino Silicate
660-Y2Si2O
7657-Zr-RE silicate 669-Y
b2Si2O7
Strength MPa
200696-EBC Bond Coat Constituent
100681-H
fO2-Si
669-9762 with CM
AS 1350C 50hr reacted
693-HfO
2-Si with CM
AS 1350C 50hr reacted
5000
200 400
600 800
1000 1200
1400 1600
Temperature degC
Strength test data compared
Yb
2 Si2 O7 C
MA
S reacted tensile Y
b2 Si2 O
7 CM
AS reacted
specimen fracture surface
surface w
ww
nasagov 27
National Aeronautics and Space Adm
inistration
High Stability and C
MAS R
esistance Observed from
the Rare
Earth S
ilicon High M
elting Point C
oating Com
positions
ndashD
emonstrated C
MA
S resistance
of NAS
A R
E-Si S
ystem at
1500degC 100 hr
ndash S
ilica-rich phase precipitation ndash
Rare earth elem
ent leaching into the m
elts (low concentration ~9
Surface side of the m
ol)
CM
AS m
elts
Area A
Area B
ww
wnasagov
28
![Page 26: Hurst, Bernadette J. Puleo€¦ · G57, 40.00 mg CMAS SiO Wellman -Aygun Smialek Braue 0 49 mole%; such as NASA’s CMAS (with NiO DSC:020 OES Measured by EDS [#] Type Date/time :](https://reader033.fdocuments.us/reader033/viewer/2022060211/5f04cb127e708231d40fbc15/html5/thumbnails/26.jpg)
National Aeronautics and Space Adm
inistration
CM
AS
Reaction K
inetics in Bond C
oats ndash S
iO2 rich phase partitioning in the C
MA
S m
elts ndash R
are earth content leaching low even at 1500degC
ndash M
ore advanced compositions are being im
plemented for im
proved thermom
echanical ndash
CM
AS Partitioning on R
E-Si bond coat 1500degC
100hr
RE incorporations
CM
AS
resistance
ww
wnasagov
26
National Aeronautics and Space Adm
inistration Strength R
esults of Selected EBC and EBC
Bond Coats
-CM
AS
Reaction R
esulted in Strength Reduction in Silicates
Selected E
BC
systems
ndashH
fO2 -R
E-S
i along with co-doped rare earth silicates and rare earth alum
ino-silicates for optim
ized strength stability and temperature capability
ndashC
MA
S infiltrations can reduce the strength
350 646-Specially alloy toughened t like H
fO2
648-EBC Bond Coat Constituent 300
659-AE9762
150
EBC
s
EBC
s
HfO
2 -Si (Si-rich)
Yb
2 Si 2 O 7
250658-EBC H
fO2-Rare Earth-A
lumino Silicate
660-Y2Si2O
7657-Zr-RE silicate 669-Y
b2Si2O7
Strength MPa
200696-EBC Bond Coat Constituent
100681-H
fO2-Si
669-9762 with CM
AS 1350C 50hr reacted
693-HfO
2-Si with CM
AS 1350C 50hr reacted
5000
200 400
600 800
1000 1200
1400 1600
Temperature degC
Strength test data compared
Yb
2 Si2 O7 C
MA
S reacted tensile Y
b2 Si2 O
7 CM
AS reacted
specimen fracture surface
surface w
ww
nasagov 27
National Aeronautics and Space Adm
inistration
High Stability and C
MAS R
esistance Observed from
the Rare
Earth S
ilicon High M
elting Point C
oating Com
positions
ndashD
emonstrated C
MA
S resistance
of NAS
A R
E-Si S
ystem at
1500degC 100 hr
ndash S
ilica-rich phase precipitation ndash
Rare earth elem
ent leaching into the m
elts (low concentration ~9
Surface side of the m
ol)
CM
AS m
elts
Area A
Area B
ww
wnasagov
28
![Page 27: Hurst, Bernadette J. Puleo€¦ · G57, 40.00 mg CMAS SiO Wellman -Aygun Smialek Braue 0 49 mole%; such as NASA’s CMAS (with NiO DSC:020 OES Measured by EDS [#] Type Date/time :](https://reader033.fdocuments.us/reader033/viewer/2022060211/5f04cb127e708231d40fbc15/html5/thumbnails/27.jpg)
National Aeronautics and Space Adm
inistration Strength R
esults of Selected EBC and EBC
Bond Coats
-CM
AS
Reaction R
esulted in Strength Reduction in Silicates
Selected E
BC
systems
ndashH
fO2 -R
E-S
i along with co-doped rare earth silicates and rare earth alum
ino-silicates for optim
ized strength stability and temperature capability
ndashC
MA
S infiltrations can reduce the strength
350 646-Specially alloy toughened t like H
fO2
648-EBC Bond Coat Constituent 300
659-AE9762
150
EBC
s
EBC
s
HfO
2 -Si (Si-rich)
Yb
2 Si 2 O 7
250658-EBC H
fO2-Rare Earth-A
lumino Silicate
660-Y2Si2O
7657-Zr-RE silicate 669-Y
b2Si2O7
Strength MPa
200696-EBC Bond Coat Constituent
100681-H
fO2-Si
669-9762 with CM
AS 1350C 50hr reacted
693-HfO
2-Si with CM
AS 1350C 50hr reacted
5000
200 400
600 800
1000 1200
1400 1600
Temperature degC
Strength test data compared
Yb
2 Si2 O7 C
MA
S reacted tensile Y
b2 Si2 O
7 CM
AS reacted
specimen fracture surface
surface w
ww
nasagov 27
National Aeronautics and Space Adm
inistration
High Stability and C
MAS R
esistance Observed from
the Rare
Earth S
ilicon High M
elting Point C
oating Com
positions
ndashD
emonstrated C
MA
S resistance
of NAS
A R
E-Si S
ystem at
1500degC 100 hr
ndash S
ilica-rich phase precipitation ndash
Rare earth elem
ent leaching into the m
elts (low concentration ~9
Surface side of the m
ol)
CM
AS m
elts
Area A
Area B
ww
wnasagov
28
![Page 28: Hurst, Bernadette J. Puleo€¦ · G57, 40.00 mg CMAS SiO Wellman -Aygun Smialek Braue 0 49 mole%; such as NASA’s CMAS (with NiO DSC:020 OES Measured by EDS [#] Type Date/time :](https://reader033.fdocuments.us/reader033/viewer/2022060211/5f04cb127e708231d40fbc15/html5/thumbnails/28.jpg)
National Aeronautics and Space Adm
inistration
High Stability and C
MAS R
esistance Observed from
the Rare
Earth S
ilicon High M
elting Point C
oating Com
positions
ndashD
emonstrated C
MA
S resistance
of NAS
A R
E-Si S
ystem at
1500degC 100 hr
ndash S
ilica-rich phase precipitation ndash
Rare earth elem
ent leaching into the m
elts (low concentration ~9
Surface side of the m
ol)
CM
AS m
elts
Area A
Area B
ww
wnasagov
28