RCF Analysis TMS 2011
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Transcript of RCF Analysis TMS 2011
ANALYSIS OF CARBON FIBER RECOVERED FROM OPTIMIZED
PROCESSES OF COMMERCIAL SCALE RECYCLING FACILITIESJoseph Heil, Davis Litzenberger, Dr. Jerry Cuomo
TMS 2011 San Diego, CaliforniaMarch 3, 2011
Institute for Maintenance Science and Technology
February 27-March 3, 2011 – San Diego, California
2
Outline
• Recycling Overview• Test Methods• Samples Tested• Test Results
• Electron Microscopy• Filament Testing
• Questions
February 27-March 3, 2011 – San Diego, California
3
Overview of CF Recycling
Uncured Trim ScrapCured Trim ScrapEnd of Life Material
Carbon Fiber Recycling
Single Blind Testing & Analysis
Samples of CF for Testing
February 27-March 3, 2011 – San Diego, California
4
Characterization MethodsMethod Information Determined
SEMScanning Electron Microscopy
Fiber diameter,contamination
Surface texture, defects
EDS Energy Dispersive Spectroscopy
Elemental composition of bulk
XPSX-Ray Photoelectron Spectroscopy
Atomic Percent %’s of Carbon Bonding
Tensile Test3 gauge lengths
Fiber Tensile Properties Failure Probability
February 27-March 3, 2011 – San Diego, California
5
Outline• Test Methods• Samples Tested• Test Results
• Electron Microscopy• Filament Testing
• Questions
February 27-March 3, 2011 – San Diego, California
6
Outline• Test Methods• Mechanical Test Results from 2006 - 2008• Samples Tested• Test Results
• Electron Microscopy• Filament Testing
• Questions
February 27-March 3, 2011 – San Diego, California
7
Samples Tested
Sample Name SourceRCF 10 Uncured T300 prepreg Fabric
V-T300 Sized Cytec T300 sample from Boeing
RCF 11 Uncured T700G prepreg fabric
V-T700G Sized sample from Boeing
*RCF 12, 13 Uncured prepreg fabric
RCF 14, 15, 16 T-800s prepreg left, center, & right side of furnace
VCF 17, 18, 19 Soxhlet extraction of prepregs “14-16”
V-T800s Sized sample from Boeing
RCF-recycled carbon fiber VCF- virgin carbon fiber
*RCFs 12 & 13 are standard modulus fibers but their morphologies after recycling left them unidentifiable.
February 27-March 3, 2011 – San Diego, California
8
Outline• Test Methods• Samples Tested• Test Results
• Electron Microscopy• Filament Testing
• Questions
February 27-March 3, 2011 – San Diego, California
9
T300 Prepreg Fabric
• Striations clearly present• Fiber appears coated
February 27-March 3, 2011 – San Diego, California
10
T700G Prepreg Fabric
RCF 11 V-T700G
• No pitting observed• Changes in shade of fiber suggests thin coating of resin
February 27-March 3, 2011 – San Diego, California
11
RCF 12 & 13
• RCF 12 & 13 have surfaces that have been heavily damaged• Not identifiable based on morphology or tensile properties
RCF 12 RCF 13
February 27-March 3, 2011 – San Diego, California
12
T800s Prepreg Left Side of Furnace
• RCF 14 has residual matrix material; size is usually <500nm• On occasion pits were seen suggesting fiber damage• Silicon in residual material
VCF 17RCF 14
February 27-March 3, 2011 – San Diego, California
13
T800s Prepreg Center of Furnace
• RCF 15 is comparatively densely covered with char • EDS indicated silicon, aluminum, sodium, and chlorine • No pitting or otherwise noticeable defects
RCF 15 VCF 18
February 27-March 3, 2011 – San Diego, California
14
T800s Prepreg Right Side of Furnace
• RCF 16 has large amounts of resins stuck in-between the fibers with a lesser amount stuck on the fibers
• Some particulates >500nm • Surface appears textured• Calcium was identified in particulate based on EDS
RCF 16 VCF 19
February 27-March 3, 2011 – San Diego, California
15
Outline• Test Methods• Samples Tested• Test Results
• Electron Microscopy• Filament Testing
• Questions
February 27-March 3, 2011 – San Diego, California
16
Standard Modulus Fiber Tensile Strength
RCF10 RCF11 RCF12 RCF13 VT3000
500
1000
1500
2000
2500
3000
3500 3,371
2,494
1,144 1,258
2,960
2,405 2,535
1,217 1,256
2,841
6mm25mm
Tens
ile S
treg
nth
(Mpa
)
T300 T700G
• RCFs 10 & 11 compare favorable to virgin T300 fiber• Tensile testing confirms damage to RCF 12 & RCF 13
February 27-March 3, 2011 – San Diego, California
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T800s Fiber Tensile Strength
• 30-50% fiber strength retention vs. ~70% from previous work
RCF14 RCF15 RCF16 VCF17 VCF18 VCF190
1000
2000
3000
4000
5000
6000
2,398 2,498
1,774
5,6986,020
5,124
1,635
2,621 2,490
5,0204,593 4,418
6mm
25mm
Te
ns
ile
Str
en
gth
(M
Pa
)
February 27-March 3, 2011 – San Diego, California
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Standard Modulus Fiber Elastic Modulus
RCF10 RCF11 RCF12 RCF13 VT3000
50
100
150
200
250
195184
160
186181
209 213198
235
182
6mm25mm
Ela
sti
c M
od
ulu
s (
GP
a)
T300 T700G•Stiffness comparable to virgin fiber
February 27-March 3, 2011 – San Diego, California
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T800s Fiber Elastic Modulus
• Loss in stiffness not seen in previous work• Stiffer than virgin standard modulus
RCF14 RCF15 RCF16 VCF17 VCF18 VCF190
50
100
150
200
250
300
350
231
172
205
254234 224
245 238 241
299 284 2836mm
25mm
Ela
sti
c M
od
ulu
s (
GP
a)
February 27-March 3, 2011 – San Diego, California
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Summary• Recycled T300 is coated with residual resin but is strong
• Recycled T700G is clean & has high strength retention
• RCFs 12 & 13 have severe oxidative damage
• SEM observations of pitting in IM fibers does not correlate well to trends in tensile strength
• Variation in fiber properties based on location in furnace for IM fibers
•Recycled carbon fibers have high retention of their elastic modulus•Lower tensile strength retention than in previous years
February 27-March 3, 2011 – San Diego, California
21
Acknowledgments• Funded by Boeing as part of the Composites
Recycling Project; Pete George, Bill Carberry• Jerry Cuomo & Davis Litzenberger• Chuck Mooney, NCSU AIF• TMS
February 27-March 3, 2011 – San Diego, California
22
T700G Prepreg Fabric
RCF 11
V-T700G
February 27-March 3, 2011 – San Diego, California
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T800s Prepreg Left Side of Furnace
RCF 14 RCF 14(pitted area)
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T800s Prepreg Center of Furnace
VCF 18RCF 15
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T800s Prepreg Right Side of Furnace
RCF 16 VCF 19
February 27-March 3, 2011 – San Diego, California
26
Atomic Percentages
RCF11 V-T300 RCF14 VCF17 RCF15 VCF18 RCF16 VCF19 V-T800s0
10
20
30
40
50
60
70
80
90
100
84
7075
58
84 8186
82
71
11
27
17
38
1217
1116
29
C O
Ato
mic
Pe
rce
nta
ge
(%
)
• RCF 14 & VCF 17 low carbon content• Oxygen content reasonable
February 27-March 3, 2011 – San Diego, California
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Atomic Percentages
• Nitrogen from pyrolysis or captured onto active surface
• Na & Si in trace amounts• No N, Na, or Si seen on V-T800s
RCF11 V-T300 RCF14 VCF17 RCF15 VCF18 RCF16 VCF190.00
1.00
2.00
3.00
4.00
5.00
6.00
N Na SiA
tom
ic P
erc
en
tag
e (
%)
February 27-March 3, 2011 – San Diego, California
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Review of 2008 T800s Tensile Strength
ENEA/ Karborek Lab cured trim scrap
ENEA/ Karborek pi-lot cured trim scrap
Virgin T800s Milled Carbon Uncured trim
scrap
Milled Carbon cured trim scrap
0
1000
2000
3000
4000
5000
6000
5134
4654
4053
6mm
30mm
60mm
Te
ns
ile S
tre
ng
th (
MP
a)
February 27-March 3, 2011 – San Diego, California
29
Review of 2008T800s Elastic Modulus
ENEA/ Karborek Lab cured trim
scrap
ENEA/ Karborek pilot cured trim
scrap
Virgin T800s Milled Carbon Uncured trim
scrap
Milled Carbon cured trim scrap
0.00
50.00
100.00
150.00
200.00
250.00
300.00
350.00
252 257263
6mm
30mm
60mm
Yo
un
gs
Mo
du
lus
(G
Pa
)
February 27-March 3, 2011 – San Diego, California
Review of T300/AS4Tensile Strength
30
T300 AS4
Virign T300 T3-MC-UTS 0
500
1000
1500
2000
2500
3000
3500
4000
2875
24662698
20752376
1896
20mm50mm100mm
Fiber
Tens
ile S
tren
gth
(Mpa
)
Virigin AS4 A-MC-EOL A-MC(O)-EOL 0
500
1000
1500
2000
2500
3000
3500
4000 4001
2953
4148
3619
2732
36913401
2464
3143
5mm10mm20mm
Tens
ile S
tren
gth
(Mpa
)
•Favorable strength retention at shorter gauge lengths
Source material: uncured trim scrap recovered by RCF, Ltd
Source material: EOL scrap recovered by RCF, Ltd
February 27-March 3, 2011 – San Diego, California
Review of T300/AS4Elastic Modulus
31
•Fibers remain stiff after recycling
Source material: EOL scrapSource material: uncured trim scrap
T300 AS4
Virign T300 T3-MC-UTS 0
50
100
150
200
250
182
203209 217
193
216
20mm
50mm
100mm
Tens
ile M
odul
us (G
Pa)
Virigin AS4 A-MC-EOL A-MC(O)-EOL
0
50
100
150
200
250
201
165
211
230211
231
257
228224
5mm10mm20mm
Ten
sile M
od
ulu
s
Source material: uncured trim scrap recovered by RCF, Ltd
Source material: EOL scrap recovered by RCF, Ltd