SRI-MME-93-261-7244.02

CGF CARTRIDGE DEVELOPMENT

VOLUME I

Final Report To:

NASA MARSHALL SPACE FLIGHT CENTER

Marshall Space Flight Center, AL 35812

Contract Number NAS8-39026

By:

SOUTHERN RESEARCH INSTITUTE

2000 Ninth Avenue South

Birmingham, AL 35205

Written By:

Carl A. Dixon

Assistant Engineer

Approved By:

R. Koenig

arch DirectorThermophysical Research Department

March 1993

TABLE OF CONTENTS

I.0 INTRODUCTION

2.0 INVESTIGATION OF WELDING/BRAZING MOLYBDENUM AND TZM ALLOY

2.1 EVALUATION OF TZM AS A POTENTIAL SOLUTION

2.2 CONCLUSIONS OF THE WELDING/BRAZING INVESTIGATION

2.3 REFERENCES FOR RECRYSTALLIZATION STUDY

3.0 EVALUATION OF TZM AS A CARTRIDGE MATERIAL

3.1 CONCLUSIONS

EVALUATION OF WC-103 AS AN ALTERNATE TO TZM

4.1 CONCLUSIONS

5.0 SURVEY OF OXIDATION RESISTANT COATINGS FOR TZM AND WC-103

5.1 CONCLUSIONS

6.0 CHEMICAL COMPATIBILITY STUDIES

7.0 FINAL DESIGN OF CGF CARTRIDGE

8.0 SUPPORT WORK

9.0 FUTURE IMPROVEMENTS

9.1 LITERATURE SEARCH FOR ALTERNATE CARTRIDGE MATERIALS

9.2 IMPROVED AMPOULE DESIGN

9.3 COMPUTERIZED MATERIALS DATABASE DEVELOPMENT

LIST OF APPENDICES

4.0

i

2

12

31

33

34

35

39

39

40

41

42

43

45

46

46

54

60

61

Ii

LIST OF ILLUSTRATIONS

2.0.4

2.0.7

2.0.8

2.1.1

2.1.2

2.1.3

2.1.4

2.1.5

2.1.6

2.1.7

2.1.8

2.1.9

2.1.10

2.1.11

Cross-Section of Crystal Growth Cartridge Showing Placement

of Adjustment Block and End Cap

Photomicrograph (25x) of a Cross-Section of Molybdenum Tube

Photomicrograph (25x) of a Cross-Section of Molybdenum TubeHeat Treated at I065°C for One Hour

Photomicrograph (25x) of Adjustment Block Brazed to

Molybdenum Tube

Quartz Dilatometer for Measuring Thermal Expansion to 1500°F

Thermal Expansion of PM-TZM (Same as Literature Values for

Molybdenum)

Thermal Expansion of 304L Stainless Steel (from TPRLHandbook)

Photomicrograph (25x) of Electron Beam Weld Area of

Molybdenum Tube

Photomicrograph (25x) of a Bar Section of Arc-Cast TZM Alloy

Photomicrograph (25x) of a Bar Section of PM-TZM

Typical Hot Zone Cavities Available

Standard Char Cycle

Photomicrograph (25x) of a Bar Section of Arc-Cast TZM AlloyHeat Soaked at 1370°C for 50 Hours

Photomicrograph (25x) of a Bar Section of PM-TZM Heat Treated

at 1370°C for 50 Hours

Photomicrograph (25x) of Virgin PM-TZM in LongitudinalDirection of Bar

Photomicrograph (lOOx) of an Actual PM-TZM Cartridge Run inthe CGF for 90 Hours at 1260°C

Photomicrograph (100x) of Virgin PM-TZM Showing MicrohardnessIndentations

Photomicrograph (100x) of PM-TZM Bar Heat Treated at 1370°C

for One Hour Showing Hard Outside Coating

Schematic of Ring-Flex Test

4

5

7

8

9

i0

ii

14

15

16

17

18

19

20

21

22

23

24

iii

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2.1.12

2.1.13

2.1.14

3.0.1

3.0.2

3.0.3

7.0.1

9.2.1

9.2.2

9.2.3

9.2.4

LIST OF ILLUSTRATIONS (Continued)

Load-Deflection of Arc-Cast Molybdenum Cartridge Rings

Load-Deflectlon of PM-TZM Cartridge Rings

Photomicrograph (100x) of Hardness Indentation in 80 Hours1370°C Heat Soaked PM-TZM

Graphite Dilatometer for Measuring Thermal Expansion to5500°F

Unit Thermal Expansion of FBD Zirconia Insulation from CGF

Molybdenum Oxide Test Facility

CGF Cartridge Schematic

Prototype Ampoule

Alternate Sealing Technique for Re-deslgned Ampoule

Ampoule Failure Sensing Mechanism for Non-conductlve

Ampoules

Ampoule Failure Sensing Mechanism for Conductive Ampoules

25

26

27

36

37

38

44

56

57

58

59

iv

Table

2.1.1

2.1.2

2.1.3

2.2.1

9.1.1

9.1.2

9.1.3

9.1.4

9.1.5

LIST OF TABLES

PM-TZMMicro-Hardness, I00 Gram Load

Arc-Cast Micro-Hardness, i00 Gram Load

PM-TZM NASA CGF Cartridge Micro-Hardness (100 gm Load)

Brazes for Molybdenum and TZM

Candidate Materials Considered for CGF Tube

Immediate Minimum Goals (Refractory Metals)

Immediate Minimum Goals (Ceramics)

Long Term Preferred Goals (Refractory Metals)

Long Term Preferred Goals (Ceramics)

28

29

30

32

49

5O

51

52

53

V

1.0 INTRODUCTION

This is Volume I of a final report for work performed by the Southern

Research Institute (SRI) for the NASA Marshall Space Flight Center (NASA/MSFC)

under contract number NAS8-39026. This report will present a summary of SRI's

research efforts in the development of crystal growth cartridges for the Crystal

Growth Furnace (CGF) used for experiments aboard USML-1.

2.0 INVESTIGATION OF WELDING/BRAglNG MOLYBDENUM AND TZM ALT_)Y

SRI's initial efforts on the CGF cartridge development program involved

investigating the welding and brazing techniques of molybdenum tubes.

NASA/MSFC's initial cartridge design is shown in Figure 2.0.1. A molybdenum

tube, fabricated by rolling, was fitted with a spherical end cap (electron-beam

welded) and a 304L stainless steel adjustment block (vacuum brazed). During the

welding and brazing operations, however, the molybdenum tube recrystalllzed and

became extremely brittle. Hoop stresses generated by both the welding and

brazing operations caused failures of the cartridge.

Figure 2.0.2 is a photomicrograph of a section of a NASA/MSFC supplied

molybdenum cartridge. This cartridge had not been heat treated. As can be seen,

the molybdenum had an aligned grain structure due to the rolling process with

which it was formed.

Figure 2.0.3 is a photomicrograph of a sample from the same cartridge but

heat treated to I065°C for one hour. This was the temperature and time at which

the cartridge was brazed in a vacuum furnace. As can be seen, the molybdenum had

recrystallized. The original grain structure was replaced by randomly oriented

large grains yielding a brittle structure.

Figure 2.0.4 is a photomicrograph of a section of the adjustment block

brazed to the molybdenum tube. Note the recrystallization of the molybdenum.

Also note that the molybdenum tube had crimped slightly and pulled away from the

braze and adjustment block. This crimping was due to the large circumferential

stresses put on the tube by a thermal expansion mismatch between the stainless

steel and the molybdenum.

Figure 2.0.5 is a schematic of one of the quartz dilatometers available at

SRI. The quartz dilatometer is capable of measuring thermal expansion up to

980°C with a precision of 10 .5 cm/cm. Thermal expansion measurements can be

performed on solid rods, tubes, and spheres.

Figure 2.0.6 is the thermal expansion of molybdenum measured in SRI's

quartz dilatometer. Figure 2.0.7 is the thermal expansion curve for 304L

stainless steel from literature. At 760°C the expansion of the stainless steel

is 14.0 x 10 -3 cm/cm. The expansion of the molybdenum is about 4.4 x 10 -3 cm/cm

at the same temperature. The large thermal expansion of the stainless steel

caused a gap of about 0.0114 centimeters (at 760°C) between the adjustment block

and the tube. This gap then filled with braze. Upon cooling, the braze

solidified and the stainless steel adjustment block contracted, placing large

hoop compressive and flexural stresses on the tube. Assuming equal compliance

between the molybdenum tube and stainless steel adjustment block, the compressive

elastic hoop stresses exceed the yield strength of both materials. This stress

caused the tube crimping or collapse. The flexural stress where the molybdenum

exits the adjustment block was about 2070 MPa (again, elastic analysis). Thus

one would also expect collapse of the molybdenum tube due to flexural stress.

Attempts were made by NASA/MSFC to place a 304L stainless steel mandrel in

the tube to prevent collapse, but, with the thermal expansion mismatch, the

stainless steel mandrel's expansion created extensive stresses and failure of the

molybdenum tube during heat up.

Figure 2.0.8 is a photomicrograph of the joint where the spherical end cap

was electron beam welded to the tube. The large grain structure is easily

visible at the heat affected zone.

In summary, the problems associated with the molybdenum tube/stainless

steel adjustment block design were;

i] Recrystallization of the molybdenum tube during brazing.

2] Compressive hoop and axial stresses from the stainless steel

adjustment block.

3] Tensile stresses from the stainless steel mandrel.

4] Recrystallization of the electron beam welded joint at the

spherical end cap.

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2.1 EVALUATION OF TZM AS A POTENTIAL SOLUTION

The recrystalllzatlon temperature of molybdenum can be increased by

alloying it with 0.5% titanium and 0.1% zirconium. The small amounts of titanium

and zirconium inhibit grain growth. Recrystallization temperatures 1,2 for this

alloy, known as TZM, become significant around 1370°C.

TZM alloy can be produced by two methods: Arc-cast and powder metallurgy.

Historically, powder metallurgy techniques yield TZM with a lower density than

arc-cast. However, current technology produces powder metallurgy TZM (PM-TZM)

with the same density and approximate mechanical properties as arc-cast TZM 1.2

PM-TZM is much more readily available and less expensive than arc-cast TZM.

Figure 2.1.1 is a photomicrograph of a piece of arc-cast TZM alloy taken

from a solid rod. The fine grain structure is evident.

Figure 2.1.2 is a photomicrograph of a piece of PM-TZM taken from a solid

rod. Note that its grain structure is similar to that of arc-cast TZM. The

small voids are created by the powder metallurgy process. The manufacturer

claims that these voids have minimal effect on material properties.

Figure 2.1.3 shows the dimensions of the hot zone cavities of the high

temperature furnaces available at SRI. SRI's high temperature furnaces use

graphite resistance heaters and is capable of reaching temperatures up to 2760°C.

Heat soaks can be performed both in air, in an inert gas, or in a prescribed

environment (such as the CGF's). Figure 2.1.4 shows the standard cycles used to

heat soak specimens.

Figure 2.1.5 is a photomicrograph of a piece of arc-cast TZM that had been

heat treated to 1370°C for fifty hours. Slight changes in grain structure were

evident but nowhere near as drastic as seen in pure molybdenum.

Figure 2.1.6 is a photomicrograph of a piece of PM-TZM that had also been

heat treated to 1370°C for fifty hours. Again, there was only slight recrystal-

lization.

12

Figure 2.1.7 is a photomicrograph of a piece of PM-TZMIn the longitudinal

direction of a solid bar. Figure 2.1.8 is a photomicrograph of a section of a

PM-TZM cartridge run in the CGF for 90 hours at 1260°C. A comparison of these

two figures shows no significant recrystalllzatlon.

A series of microhardness tests were run on samples of virgin and heat-

soaked TZM. Figure 2.1.9 is a photomicrograph of a section of virgin PM-TZMbar.

The hardness indentations are visible. Tables 2.1.1 and 2.1.2 summarize the

mlcrohardness readings for PM-TZMand arc-cast TZM. The outside surface of heat-

soaked materials apparently had a thin hard coating. This is shown in Figure

2.1.10. The composition of the coating was not known. The data from Tables

2.1.1 and 2.1.2 indicated that continued exposure to hlgh temperatures increases

the hardness of the TZM. Microhardness was also run on the PM-TZM tube that was

run in the CGF for 90 hours. Hardness readings were taken from areas at both the

brazed joint and the end cap. Table 2.1.3 summarizes this data. As expected,

there was less change than seen in the 1370°C environment.

Figure 2.1.11 is a schematic of a test technique to qualitatively evaluate

ring flexure of samples cut from CGF cartridges. A series of dead weight loads

was employed to obtain deformations. Ring samples 0.50 inches wide were cut from

an arc-cast molybdenum cartridge and a PM-TZMcartridge. Ring samples from both

cartridges were heat treated to 2500°F for six hours. Figure 2.1.12 is the load-

deflection curve for the arc-cast molybdenum rings. The effect of heat treating

was to lower the strain to failure. Figure 2.1.13 is the load-deflection curve

for the PM-TZM rings. Failure could not be obtained with this geometry and

facility (load limited).

To evaluate TZM's ductility, SRI's scanning electron microscope was used

to photograph the hardness indentations in the 80 hour heat soaked specimen.

Figure 2.1.14 is a photomicrograph (3000x) of such an indentation. A brittle

material would have cracks propagating from the corners of the indentation. A

ductile material would have flow lines around the periphery. Neither of these

effects were seen.

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2.2 CONCLUSIONS OF THE WELDING/BRAZING INVESTIGATION

Based upon the recrystalllzatlon study and the simple ring flexure test,

PM-TZMwas considered to be an acceptable cartridge material. The electron beam

welding of the end cap was eliminated by machining the tubes with a closed

spherical end from a solid bar of PM-TZM. It was decided that a re-design of

the adjustment block was required to eliminate the stresses built up during

brazing the adjustment block to the cartridge tube. The new adjustment block

configuration was designed by NASA/MSFC and was constructed from PM-TZM to

eliminate the thermal expansion mismatch. SRI also researched some brazing

alloys recommended 1,3 for molybdenum and TZM. These alloys are listed in Table

2.2.1 in decreasing order of brazing temperature. Brazing pure molybdenum with

these materials would have resulted in some recrystalllzation. TZM, however,

posed no problems.

31

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2.3 REFERENCES FOR RECRYSTALLIZATION STUDY

i. "Fabricating Molybdenum and TZM Alloys", Climax Specialty Metals.

2. "Molybdenum", Metallwerk Plansee GmbH.

3. "Brazing Molybdenum", American Society for Metals (1959).

. L.H. Stone, A.H. Freedman, and E.B. Mlkus, "Recrystalllzatlon Behavior and

Brazing of the TEM Alloy".

33

3.0 EVALUATION OF TZM AS A CARTRIDGE MATERIAL

Upon completion of NASA/MSFC's re-deslgn of the adjustment block, SRI

arranged to have several test cartridges assembled for ground testing. SRI

purchased bar stock of TZM from Climax Specialty Metals in Chicago. Some of this

bar stock was subcontracted to a machine shop to be gun-drilled and ground to

form the cartridge tube with a closed spherical end. SRI machined the adjustment

blocks in-house from the remainder of the TZM bar stock. The adjustment blocks

and cartridge tubes were then sent to NASA/MSFC for brazing and ground testing.

The TZM cartridge did not have the problems with recrystallization and

brittleness that the previous molybdenum/stainless steel design suffered.

However, there were some difficulties with TZM.

The TZM alloy was very difficult to machine. TZM is hard enough that tools

wear out very quickly. The tools also required constant cooling with a tapping

fluid to machine the alloy. TZM is a fairly brittle material. This brittleness

often prevented the material from chipping cleanly and occasionally caused

fracture of the part as holes were bored through. Machining the TZM was

expensive in both man-hours and tooling.

During high temperature ground tests of the CGF with a TZM cartridge, the

low density zirconia insulation in the adiabatic zone of the CGF crumbled and

formed a yellow powder. An investigation of the yellow powder by SRI's X-ray

diffraction facility showed the presence of large amounts of monoclinic zirconia.

Commercial zirconia insulation has a yttria stabilizer added to maintain the

zirconia in a stable cubic crystal form. It was apparent from this analysis that

something was causing the stable cubic zirconia to break down into the less

stable monoclinic form (which is yellow in color).

The transformation from cubic to monoclinic zirconia is accompanied by a

three-fold volume change. As a check on the stability of the zirconia insulation

supplied by the manufacture to NASA/MSFC, thermal expansion measurements were

made on zirconia samples taken from spare parts of the CGF. In order to reach

temperatures higher than 980°C, SRI's graphite dilatometer (Figure 3.0.1) was

used in conjunction with the quartz dilatometer. The graphite dilatometer is

34

capable of measuring thermal expansion from about 815°C to 2760°C. Figure 3.0.2

is the thermal expansion curve for the zlrconla insulation. The thermal

expansion coefficient is uniform, indicating a stable material with no phase

changes. Therefore, since the breakdown occurred only when a TZM cartridge was

used, it was surmised that the TZMwas somehow attacking the zlrconla insulation.

A literature search on molybdenum and TZM showed that the volatile oxide

formed by molybdenum can act as a catalyst for certain chemlcal reactions. Since

the TZM cartridge readily oxidizes in the CGF, a test was designed to evaluate

the effects of molybdenum oxide on zlrconia insulation.

Figure 3.0.3 is a schematic of the molybdenum oxide test facility.

Shavings of TZM were packed in the forward end of the furnace. A block of

zirconla insulation (i cc) was set in the rear of the furnace. The entire

assembly was heated to 1200°C. Air was then purged into the forward end of the

furnace through the TZMshavlngs. The large surface area of the shavings allowed

the generation of copious amounts of molybdenum oxide that then passed over the

zirconia insulation. The test was run for two hours. By the end of the test,

the zirconla insulation had crumbled into a yellow powder. X-ray diffraction

showed the powder to be monocllnlc zirconia.

The above test showed that the molybdenum oxide generated by the TZM alloy

was attacking the zirconla insulation. The chemical mechanism of the attack is

not known.

3,1 CONCLUSIONS

There were two possible courses of action in response to the difficulties

experienced in using TEM as the CGF cartridge material. Either an alternate

material could be selected or a coating of some sort could be applied to the

cartridge to prevent oxidation. The adjustment block would require no coating

since it operated at only a few hundred degrees centigrade and thus did not

oxidize at all.

35

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38

4.0 EVALUATION OF WC-103 AS AN ALTERNATE TO TEM

WC-103 is a niobium/hafnium alloy produced by Teledyne Wah-Chang in Albany,

Oregon. WC-103 will not recrystallize during electron beam welding or brazing

operations. This eliminated the need for machining cartridge tubes from solid

rods as with the TZM. Tubes could be bought directly from Teledyne Wah-Chang,

then the endcaps could be e-beam welded. This greatly reduced the manufacturing

cost of CGF cartridges. Some of that savings was offset, however, by the greater

cost of WC-103.

WC-103 is a more ductile alloy than TZM. This made machining the

adjustment blocks considerably easier. The greater ductility also meant that the

WC-103 cartridges were less susceptible to breakage when jarred than the TZM

cartridges.

WC-103 mechanical properties are not as good as TZM (see tables in Section

6.1 for numerical data). However, its properties were deemed sufficient for use

in the CGF.

There was only one major drawback to using WC-103 as a CGF cartridge

material. The alloy oxidizes extensively at temperatures above about 230°C. In

tests run in SRI's high temperature furnace, a WC-103 sample was heated to 1200°C

and held for i hour in an environment simulating the CGF. The WC-103 broke down

completely into a whitish powder. Obviously, such disintegration of the car-

tridge in the CGF would result in failure of the experiment. However, a coating

could be applied to the WC-103 tube to prevent oxidation.

4,_ CONCLUSIONS

The WC-103 appeared to be a viable candidate if the oxidation problem could

be solved with some sort of coating. The greater machinability and higher

recrystallization temperature of the WC-103 made it desirable over TZM. However,

TZM did possess better mechanical properties.

39

5.0 SURVEY OF OXIDATION R_SIST_ COATINGS FOR TgM AND WC-10_

Since both the TZM and WC-103 oxidized readily in the CGF environment, a

survey was made of oxidation resistant coatings that could be applied to

cartridges of these materials. This would allow either of the materials to be

successfully used in the CGF.

The survey yielded two types of coatings that could be applied to the

cartridges; i) a silicide coating and 2) a chemical-vapor-deposited (CVD) iridium

coating. These two coatings had thermal expansion coefficients that matched

those of the base materials. The thermal expansion match was necessary to avoid

cracks in the coatings at elevated temperatures.

Plasma sprayed silicide coatings were available from a company called VAC-

HYD, based in Los Angeles, California. The silicide coatings were available

which had been formulated to have compatible thermal expansion coefficients with

both TZM and WC-103. The actual compositions of these coatings were proprietary.

The CVD iridium coating was available from a company called ULTRAMET based

in Pacomla, California. Iridium is a high temperature, oxidation resistant

metal. The thermal expansion of iridium is compatible with both TZM and WC-103.

Sample coupons of both TZM and WC-103 were sent to VAC-HYD for silicide

coatings. A sample coupon of TZMwas sent to ULTRAMET for a CVD iridium coating.

The returned samples were then inspected by SRI. It was noted that the

silicide coatings were soft and easily rubbed off. The silicide coatings also

had a tendency to crack if mishandled. The CVD iridium coating on the TZM,

however, did not have any flaws and appeared to be quite rugged.

SRI then performed oxidation testing in the high temperature furnace on all

the samples. The coupons were heated to 1200°C in air and held at temperature

for eight hours. No oxidation was seen on any of the samples.

Since the silicide coatings were inexpensive and quickly available, a WC-

103 cartridge was sent to VAC-HYD for coating. An inspection of the returned

4O

cartridge showed the silicide coating had a tendency to chip off. There were

numerous small cracks in the coating. This cartridge was then sent to NASA/MSFC

for ground testing.

Since VAC-HYD's silicide coatings were easily damaged, another source of

silicide coatings was sought. HITEMCO, based in New York, was able to provide

suitable silicide coatings. HITEMCO's coatings were dipped rather than sprayed.

The dipped coatings were considerably more rugged than the VAC-HYD's sprayed

coatings. HITEMCO's coatings were also much less expensive than VAC-HYD's

sprayed coatings ($250 per tube vs. $500 per tube). The dipped coatings provided

adequate oxidation protection of the cartridges in the CGF.

A TZM cartridge was sent to ULTRAMET for an iridium coating. Upon

inspection of the returned cartridge, the coating was durable and without

defects. Testing at NASA/MSFC indicating that the iridium coating protected the

TZMfrom oxidation. The zirconia insulation was not attacked.

5.1 CONCLUSIONS

Both the silicide and iridium coatings provided adequate protection from

oxidation for both TZM and WC-103. The iridium is much more durable than the

silicide coatings which require careful handling to avoid damage. However, the

iridium coating's cost is prohibitive. The single TZM tube that was iridium

coated cost around $25,000. This cost was broken into two parts; a $15,000 setup

charge, then $i0,000 per tube for the iridium coating. HITEMCO's silicide

coatings, on the other hand, cost only around $250 per tube. This savings in

cost of coating was deemed sufficient to offset the extra care required in

handling the siliclde coated tubes.

41

6,0 CHEMICAL COMPATIBILITY STUD;E$

Two semiconductor materials were scheduled to be run aboard USML-I. They

were gallium arsenide (GaAs) and cadmium zinc telluride (CdZnTe). Chemical

compatibility between these semiconductors and the CGF cartridge material is of

importance in the event of an ampoule failure during the experiment. Such a

failure would result in direct contact of the molten semiconductor and cartridge.

If the metal were attacked too extensively the cartridge would fail releasing

molten semiconductor into the CGF, ruining the facility. Also the molten

semiconductor could possibly escape the CGF entirely, posing a threat to shuttle

personnel. The investigation of chemical compatibility was subcontracted by SRI

to Dr. Rosalia Andrews of the Department of Materials Science and Engineering at

the University of Alabama at Birmingham. Chemical compatibility studies were

conducted as shown in the following matrix;

Silicide Hot Pressed

Coated Boron

WC-I03 WC-103 WC-103 TZM WC-103 Nitride

GaAs @ 24 hours 12 hours 6 hours --- 24 hours 24 hours

1260°C

CdZnTe @ 90 hours 24 hours 12 hours 90 hours 90 hours

I170°C

All compatibility test reports are contained in Appendix A.

42

7.0 FINAL DESIGN OF CGF CARTRIDGE

The flnal design of the CGF cartridge is shown in Figure 7.0.1. The

selected materials were WC-103 for both the cartridge and the adjustment block.

The cartridge was coated inside and out with a slllclde coating by HITEMCO. The

WC-103 end cap was e-beamwelded and the adjustment block was brazed.

43

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8.0 SUPPORT WORK

In addition to the extensive research effort performed under this contract,

SRI also carried out support work for NASA/MSFC. This support work consisted

mainly of machine shop time to fabricate test articles and flight hardware in

support of the USML-I schedule.

45

9.0 FUTURE IMPROVEMENTS

The following sections are some efforts directed toward improving the

current CGF cartridge design for future USML missions.

9,1 LITERATURE SEARCH FOR ALTERNATE CARTRIDGE MATERIALS

WC-I03 proved to be a workable material for use as a CGF cartridge when

protected by a silicide coating. However, the silicide coating was easily

damaged. It was decided to begin to conduct a survey of alternate cartridge

materials for use in later USML flights. Table 9.1.1 is a preliminary list of

candidate materials selected by NASA/MSFC and SRI as being most likely to qualify

as cartridge materials. These materials were selected primarily for their high

operating temperatures.

As a preliminary step in selecting alternate cartridge materials, a

literature search for thermal, mechanical, oxidative, and chemical properties was

performed on the materials listed in Table 9.1.1. Appendix B of this report

contains all available data on the candidate metals and metal alloys. Appendix

C lists all data on the candidate ceramic materials. Blank spaces were left

where data was not available. Data is presented in both International System

(SI) and British Gravitational (BG) units. No information on chemical compati-

bility with semiconductor crystal compounds was found for any of the candidate

materials. Appendix D summarizes thermal and mechanical properties for the

candidate materials both at room temperature and at elevated temperatures.

Appendix E lists the references used in the literature search.

Table 9.1.2 lists the candidate metals and metal alloys subject to a

preliminary screening based upon the following conditions;

i)

2)

The material must survive at 1350°C in a mildly oxidizing

environment. The CGF environment has about one-half percent

oxygen.

The material must withstand thermal shock. The translating

hot zone of the CGF subjects the cartridge to large thermal

gradients.

46

3)

4)

5)

The material must be commercially available.

The material must be machinable.

The material must be able to be formed into a sealed tube.

The tube must maintain its shape (not be too malleable).

As can be seen in Table 9.1.2, only one metal survives the preliminary

screening. The downfall of many of the metals is the oxidation requirement.

Most of the metals and metal alloys oxidize at elevated temperatures.

Table 9.1.3 presents the candidate ceramic materials subject to the same

screening conditions. Only two materials survived. The downfall of the ceramics

is the thermal gradient requirement. Most ceramics are very susceptible to

thermal shock and cracking at elevated temperatures. The final two selections,

silicon carbide and silicon nitride, present a problem in that they can only be

formed into tubes with about a six millimeter wall thickness. This is a much

thicker wall than the current design allows.

Tables 9.1.4 and 9.1.5 contain the metal and ceramic candidates

(respectively) subjected to a higher temperature requirement (1575°C) in

anticipation of future USML flights that will require greater temperatures. As

can be seen, the results of the second screening are the same as the first.

It is evident from this preliminary study and experience with TZM and WC-

103 that candidate metals and metal alloys must have some form of oxidation

protection if they are to survive at high temperatures in the CGF environment.

Iridium, though not subject to oxidation, is too expensive to be a feasible

cartridge material. Many of the metals rejected in the preliminary screening

could become viable candidates with an oxidation resistant coating. However, a

more durable coating than the silicide coatings used with WC-103 would be

desired.

Silicon nitride and silicon carbide seem to be two good potential ceramic

cartridge materials. These materials are oxidation resistant, have high

operating temperatures, and are not susceptible to thermal shock. However, the

thick-wall requirement would necessitate the redesign of the ampoule and

47

thermocouple assembly currently used in the CGF. A silicon nitride tube was

ordered and fabricated by Ceradyne Inc. in Costa Mesa, California, under this

contract for future evaluation as a CGF cartridge.

48

TABLE 9.1.1

CANDIDATE MATERIALS OONSIDERED FOR OGF TUBE

METALS CERAMICS

Iridium

Niobium

Niobium (we-103)Platinum

Platinum/20% Iridium

Platinum/20% RhodiumRhenium

Rhodium

Tantalum

Tantalum/10% TungstenTantalum/Rhenium

Tungsten

Tungsten/25% RheniumTZM

Aluminum Oxide

Aluminum Oxide/SiC Whiskers

Beryllium Oxide (Impressed)

Boron Nitride (HP Grade)OLromium Bonded Aluminum Oxide

Quartz (Fused Silica)

Silicon Carbide (Sintered Alpha)

Silicon Nitride (Hot Pressed)

Zirconium Oxide (Sintered; MgO Stabilized)

49

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9.2 IMPROVED AMPOULE DESIGN

The semiconductor crystals are contained in a sealed quartz ampoule in the

current CGF design. However, quartz becomes soft at around 1260°C, enabling the

vapor pressure of the crystal material to "balloon" the ampoule. This difficulty

was overcome by pressurizing the CGF cartridge to prevent the ampoule's

ballooning. Another problem with the quartz ampoule was its chemical

incompatibility with galllumarsenide (GaAs) at elevated temperatures. The GaAs

attacked the quartz severely leading to failure of the ampoule. To prevent

failure, a pyrolytic boron nitrlde sleeve was inserted into the ampoule.

Pyrolytic boron nitride does not react with GaAs and the sleeve prevented the

attack of the quartz. An effort was made to improve the ampoule design for

future USML missions which will require higher temperatures.

The redesigned CGF ampoule must meet three requirements. First, the

material must survive the CGF operating temperature and be chemically inert with

the semiconductor crystals it contains. Second, the ampoule must be sealable.

An added improvement would be to include a failure sensing device that would

alert the operator of an ampoule failure during the experiment. These three

requirements were addressed by SRI.

Only ceramic materials were considered as candidate ampoules due to the

oxidation problems experienced with most metals and metal alloys. Pyrolitic

boron nitride was successfully used with GaAs in ground testing of the CGF for

USML-I. However, pyrolytic boron nitride is not available in pieces large enough

to construct an ampoule. Hot pressed boron nitride is available but the chemical

compatibility with semiconductor crystals must be determined. SRI had an ampoule

constructed from boron nitride for evaluation under this contract. This ampoule

is shown in Figure 9.2.1. Testing is ongoing. Also, from the literature search

described in Section 8.1 of this report, silicon carbide and silicon nitride seem

to be viable candidates as well.

Future experiments may require consideration of other ceramics to ensure

chemical compatibility with other semiconductor crystals. SRI possesses a

complex finite-element analysis computer program (NISA) that can be used to

54

ensure the ampoule configuration (wall thickness) and material properties are

sufficient to contain various semiconductors during the CGF experiments.

Ceramics are not as easily sealed as quartz. The prototype ampoule was

designed with a threaded cap and a small crushable platinum seal (chemically

inert with most semiconductors) equipped with nodes that would penetrate the

ampoule material upon tightening the cap (Figure 9.2.1) thus sealing the ampoule.

Another proposed technique would be to machine a slightly oversized plug, cool

it to cryogenic temperature, then insert it into a slightly heated ampoule. Upon

reaching thermal equilibrium, the plug would tightly seal the ampoule (Figure

9.2.2).

The failure sensing device devised by SRI consisted of a metallic circuit

etched on the outside of the ampoule (Figure 9.2.3). Upon failure of the

ampoule, the circuit would either be broken by cracks or attacked by the escaping

semiconductor. Either case would result in a broken circuit that would alert the

operator of ampoule failure. For conductive ampoule materials, such a silicon

carbide, the metal circuit could be placed inside a permeable insulator and

placed near the ampoule (Figure 9.2.4). Again, if the ampoule fails, the

semiconductor would attack the circuit and break it, signalling an alert. SRI

has completed the preliminary design work on such a circuit but no prototypes

have been constructed.

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59

9.3 COMPUTERIZED MATERIALS DATABASE DEVELOPMENT

SRI has developed a computer program that maintains a database on

mechanical and thermal properties of candidate cartridge and ampoule materials.

The database currently contains all of the information listed in Appendixes B and

C. The program is capable of switching between SI and BG units. Provisions for

adding candidate materials to the database have been made. The program will be

especially useful in selecting appropriate ampoule materials for specific semi-

conductor crystals since chemical compatibility information can be maintained.

6O

LIST OF APPENDICES

APPENDIX A

APPENDIX B

APPENDIX C

APPENDIX D

APPENDIX E

CHEMICAL COMPATIBILITY STUDIES

CGF CARTRIDGE CANDIDATE METALS AND METAL ALI_YS

CGF CARTRIDGE CANDIDATE CERAMIC MATERIALS

CANDIDATE CARTRIDGE MATERIALS SUMMARY TABLES

LITERATURE SEARCH REFERENCES

61

APPENDIX A

CHEMICAL COMPATIBILITY STUDIES

A-I

Progress Report

Chemical Compatibility Studies

of GaAs and CdZnTe

with WC-103 and TZM

by:

Rosalia N. Andrews, Ph.D., P.E.

Department of Materials Science and Engineering

University of Alabama at Birmingham

Birmingham, Alabama 35294

February 10, 1992

A-2

Introduction

The purpose of this investigation was to evaluate the chemical compatibility of both GaAs

and CdZnTe with the alloys WC-103 and TZM. These two alloys are candidate cartridge

materials for use in the Crystal Growth Furnace (CGF) during crystal growth experiments

aboard USML-1. WC-103 is an 89%Nb - 10%Hf- 1%Ti alloy and TZM is a Mo - 0.5%Ti -

0.19%Zr alloy.

The chemical compatibility issue is of critical importance in the event of an ampule

failure during crystal growth experiments. Such a failure, would result in the metal and molten

semiconductor being in direct contact, possibly over an extended period of time at high

temperatures. The extent of any semiconductor/metal reaction is thus a critical safety issue

question. This investigation was undertaken to determine the occurrence of any reactions or

metal loss at the molten semiconductor/metal interface during long term contact. This study

fully evaluated the chemical compatibility of GaAs and CdZnTe with WC-103 at 1260"C and

1170°C, respectively and also provides preliminary data for the chemical compatibility of

CdZnTe with TZM.

Experimental Procedure

The metal-semiconductor reaction couple was loaded into the appropriate crucible

(Pyrolytic Boron Nitride (PBN) for GaAs and Quartz for CdZnTe), then covered and sealed in

an evacuated quartz ampule. The design of the test configuration is shown in Figure #1. This

configuration simulates very closely the actual conditions that would occur in the event of an

unexpected ampule failure at elevated temperatures. Namely, the metal would be exposed to a

A-3

2:

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A-4

semi-infinite supply of molten semiconductor for the duration of the growth experiment at an

elevated temperature. The longest duration for the CdZnTe experiment would be 90 hours and

that for the GaAs would be 24 hours at temperature. The test matrix utilized in this study is

shown in Table # 1 and was selected to determine the progressive semiconductor/metal attack as

a function of time.

Table I

WC- 103 WC- 103 WC- 103 TZM

GaAs 24 Hours 12 Hours 6 Hours

1260"

CdZnTe 90 Hours 24 Hours 12 Hours 90 Hours

1170"

All GaAs compatibility tests were performed at 1260°C and all CdZnTe compatibility

tests were performed at 1170 ° C.

CdZnTe couples are shown in

The heating and cooling profiles followed for both GaAs and

Figures 2 and 3, respectively. After processing, all

semiconductor/metal reaction couples were examined both optically and with Scanning Electron

Microscopy (SEM) and Energy Dispersive Spectroscopy (EDS) to determine both the extent of

metal loss, the presence of any semiconductor/metal reaction zone, and the resultant chemical

compatibility of the couple.

Details of the sample preparation, ampule loading and characterization techniques used

in this study are given below.

A-5

1400

1200fI000

aoo I----V - _ \ :

600

_'°°II \\ '.,_oo_j \ \ \

O r f , _. _ i _0 10 20 30 40 60

Time (hours)

6 hours" _.'12 hours ..... 24 hours

Figure 2. Furnace Heating Schedule for GaAs Compatibility Tests; 6, 12, and 24

hour runs at 1260°C.

Figure 3.

,200[...........................

E

oo 20 40 60 80 lO0 12o

Time (hours)

12 hours "-"-- 24 hours ..... 90 hours

Furnace Heating Schedule for CdZnTe Compatibility Tests; 12, 24, and90 hour runs at l l70°C.

A-6

Semiconductor/Metal Couple Preparation

Metal coupons of approximately 10ram x 10mm x 5mm were cut from a slab of WC-103

or TZM and were ground and polished using successively, 240, 400 and 600 grit SiC, f611owed

by 9.5_m, 5.0/_m and 1.0/zm alumina polish. The coupons were then cleaned with distilled

watei" and methanol. A schematic of the metal coupon is shown in Figure 4.

Height

II0 mm

I

/ /

Front Face

i_'_ 10 mm

Length

_I _ _

Figure 4. Schematic of metal coupon used in compatibility studies.

For the GaAs experiments, pyrolytic boron nitride boats and lids were used to contain

the metal/semiconductor couple. The boats and lids were rinsed in distilled water and then

soaked in aqua regia (3 parts concentrated HCI and I part concentrated HNO3) overnight. Upon

removing the pyrolytic boron nitride from the aqua regia, the pieces were rinsed several times

A-7

in warm distilled water and subsequently placed in a furnace and heated in air at 700°C for 3

hours.

The GaAs was cleaned in a solution consisting of 2 parts H2SO4, 1 part peroxide, and

1 part distilled H20. After soaking for 2 minutes, the GaAs was removed and thoroughly rinsed

with distilled water, with a final rinse in methanol. The CdZnTe was used in the as-received

condition. Both semiconductor materials were stored in a vacuum desiccator.

The quartz ampule, plug, and support slide used in all experiments were initially cleaned

in distilled water and methanol. They were then rinsed in hydrofluoric acid for 30 seconds

followed by thorough rinsing in distilled water. A final methanol rinse was used. The quartz

boats and lids used for the CdZnTe experiments were also cleaned using the above procedure.

The weight of the empty boats as well as the weight and dimensions of the metal coupon

were recorded prior to each compatibility run. To load the boats, the metal coupon was first

placed into the boat on edge so that the front and back faces did not touch any portion of the

boat. The boat was then filled with crushed semiconductor. The boat was then repeatedly

tapped and filled until the semiconductor was level with the top of the boat. The filled boat was

then weighed.

The filled boat was covered using the appropriate lid and secured to a support slide using

quartz yarn. After the boat was secured to the slide, the boat and slide were placed in the

ampule and positioned at the very end of the ampule. Once the boat was in place, the quartz

plug was slid to the end of the ampule so that it was in contact with the square end of the

support slide. The loaded ampule was then slowly evacuated down to 3x10 -6 Torr. Argon gas

was used to back fill the ampule to atmospheric pressure. The ampule was again evacuated and

A-8

backfilled two more times. A final vacuumof 3x107 Tort wasachievedprior to the actual

sealingof theampule.

An oxygen-hydrogentorchwasusedto sealtheampule. Thequartzampulewasheated

so that it collapsedonto the quartz plug and formeda seal betweenthe two surfaces. The

sealingwasdonein severalstepsso that theend of the ampulecontainingthe boat could be

cooled. Distilled waterwasusedto cool the endof theampule. To avoid thermallyshocking

the quartz, the waterwasnot applieddirectly to the regionbeingsealed. The cooling of the

ampulehelpedto preventvaporizationof thesemiconductorduring thesealingprocedure.

A diamondwire sawwas thenusedto cut the excesslengthoff of theampuleand the

ampulewasthencleanedwith methanolto removeany residue. A graphiteplug wasground to

fit into thequartzplug, and the ampule(with thegraphiteplug in place)was then loadedinto

a graphitecontainmentvessel. This graphitecontainerwas usedto hold the sealedquartz

ampuleto minimize anyballooningeffect of thequartzwhich mayoccurat high temperatures.

A graphitelid was thenscrewedinto placesothat it just touchedtheendof thequartzampule,

butdid not rotatetheampule. Figures5 and6 iliustratea loadedboatandampule,respectively

astheyarebeingpreparedfor placementin thefurnace.

Thegraphitevesselwasthenloadedinto thefurnacesuchthattheboatwasin thecentral

constanttemperatureregionof thefurnace. An externalthermocouplewasinsertedthroughthe

endcapson the aluminafurnacetubeand argongasat a flow rateof 90 cc/min, wasstarted.

Thefurnacecontrollerwasthenprogrammedfor theproperheatingprofile. The heatingprofile

usedfor the GaAs experimentsand for the CdZnTe experimentswas shownpreviously in

Figures2 and3, respectively.

A-9

Figure 5. Loaded PBN boat with lid.

Figure 6. Quartz ampule assembly for compatibility tests.

A-IO

After the entire heating profile was run and the ampule was again at room temperature,

the graphite vessel was removed from the furnace. The quartz ampule was removed and was

cut open using a diamond cut off wheel. The boat was removed and a photograph was taken

of the boat. The lid was then removed and another photo was taken. Figures 7 and 8 are

representative photos of an ampule and boat as they were removed from the furnace. After

removing the semiconductor/metal coupon from the boat, the combination was sectioned using

a diamond cut off saw and one half of the sample was mounted in an electrically conductive

mounting compound. The mounted half was then ground using 240, 400, and 600 grit SiC with

final polishing done using 9.5 _m, 5.0 #m, and 1.0 _m alumina polish. The sample was then

cleaned in methanol.

A photograph was taken of the mounted sample to show the overall cross section.

Optical photographs were then taken of each side of the metal coupon and its bottom to show

the microstructure in the region of the metal/semiconductor interface. Optical photographs were

taken of all samples at magnifications of 31.25X, 100X, and 200X.

The mounted samples were also examined in the scanning electron microscope, (SEM).

Compositional analysis was performed at various locations across the metal semiconductor

interface using a KEVEX microanalysis system. All SEM/KEVEX analysis was performed at

an accelerating voltage of 16 KeV and a take off angle of 15 °. This technique clearly showed

any reaction or diffusion zone at the interface between the semiconductor and the metal coupon.

Additionally, X-ray maps were taken across the semiconductor/metal interface to more

graphically show the reactions taking place.

The final dimensions of the metal coupon were also measured using a micrometer stage

and optical microscope so that the amount of metal loss and thickness of any reaction zone could

be accurately determined.

A-II

Figure 7. Quartz ampule assemble as removed from furnace after compatibility tests.

IIIIIIIIIIIIIIIIIIIIIIIIIIIIII)1Iltlil))IliltJlPIftJ)ldlltllIr)l(Pl!4111!!rf'rlirlF!,J 10 20 30 x,O t,_ .61_ 7_ .i 3LG 13;i'

Figure 8. PBN boat removed from ampule after compatibility test.

A-12

Results and Discussion

GaAs/WC-103 Compatibility Tests

Three GaAs/WC-103 compatibility tests were conducted to determine the

reactivity/compatibility of molten GaAs in contact with WC-103 at 1260°C. Details of the

experimental set-up and test procedures were described previously. The three runs conducted

and analyzed were for 6, 12, and 24 hours at 1260°C. The results are presented below.

6 hour GaAs/WC-103

An optical micrograph showing a cross-section of the 6 hour GaAs/WC-103 reaction

couple is shown in Figure 9. An optical micrograph of the reaction zone at the

metal/semiconductor interface is shown in Figure 10. As can be seen in Figure 10, the metal

was severely attacked by the semiconductor. It is also apparent that reaction products have

formed at the metal/semiconductor interface and that some of these products have begun to break

off into the adjacent semiconductor. SEM/EDS analysis across the interface was performed and

the compositional results obtained from Figure A1 are shown in Figure A2 (Appendix A).

Points 3, 4, and 5 on Figure A2, (zones 1, 2, 3, on plots) indicate that the reaction

products formed are indeed a mixture of semiconductor and metal. In this run, the average

thickness of metal lost was 0.7 mm or 2.76 mils. Since the proposed metal cartridge for use in

the CGF crystal growth experiments aboard USML-1 is 27 mils thick, the metal loss observed

was normalized to this thickness. Thus, for a 27 mil thick metal sample, the amount of metal

loss observed for a 6 hour run would amount to a 10% reduction in thickness.

A-13

Figure 9. Cross section of a GaAs/WC-103 reaction couple after a 6 hour compatibility run

at 1260" C.

Figure 10. Metal/semiconductor interface region in a GaAs/WC-103 compatibility test

carried out for 6 hours at 1260°C. i = metal, 2 = interface/reaction zone, and

3 = semiconductor.

A-14

!2 hour GaAs/WC-102

For the 12 hour run, Figure I1 again shows a severe attack present at the

metal/semiconductor interface. The reaction products formed at this interface have also spalled

off and floated into the adjacent semiconductor. In the compositional analysis performed across

the interface (Figures A3 and A4 in Appendix A), it is observed that metal is present a

considerable distance away from the metal/semiconductor interface (points 8 and I0 for example)

and that reaction products which break off from the reaction zone are a mixture of metal and

semiconductor.

In this couple, the average thickness of metal lost was 0.08 mm or 3.15 mils. On a 27

mil thick metal sample, this would correspond to a 12% reduction in thickness.

Figure 11. Metal/semiconductor interface region in a GaAs/WC-103 compatibility testcarried out for 12 hours at 1260°C. 1 = metal, 2 = interface/reaction zone and3 = semiconductor.

A-15

24 hour (_aA_/WC-103

The 24 hour GaAs/WC-103 couple showed a very severe reaction at the

metal/semiconductor interface, as can be seen in Figure 12. It is obvious in this micrograph that

reaction products formed at the interface between the metal and semiconductor and then broke

off and floated into the adjacent molten semiconductor.

Figure 12. Metal/semiconductor interface region in a GaAs/WC-103 compatibility test

carried out for 24 hours at 1260°C. 1 = metal, 2 = interface/reaction zone, and3 = semiconductor.

The SEM/EDS analysis confirms this observation (Figures A5 and A6 in Appendix A).

For example, points 4, 6, and 7 on Figure A6 indicate a mixture of metal and semiconductor

in the reaction products which were not adherent to the metal surface.

In this couple, a reduction in metal thickness of 0.17 mm or 6.69 mils. was observed.

In a 27 rail thick metal sample, this would result in a 25% reduction in thickness.

A-16

Summary - GaAs/WC-103

In all GaAs runs there was a measurable amount of metal loss due to interaction between

the metal coupon and semiconductor. The average metal loss for the various times averaged at

several locations along the sample are summarized in Table II.

Table II

Time at Temperature Average Thicknessof Metal Lost

mm (mils)

6 hours 0.07 (2.76)

12 hours 0.08 (3.15)

24 hours 0.17 (6.69)

Figure 13 shows a plot of the average thickness of metal lost as a function of time at

temperature. Metal loss due to the formation of a non adherent reaction layer is expected to

exhibit a linear relationship with time. Although there is limited data, there does appear to be

a linear relationship between metal lost and time at temperature for this metal/semiconductor.

combination.0.2

O.15

EE

(n(/)

o o.1_J

0.05

Figure 13.

J0

o 6

/

I I I

10 15 20 26

Time (hours)

Average thickness of metal lost as a function of time for GaAs/WC-103 couplestested at 1260 ° C.

A-17

In summary, in the region adjacent to the metal surface, an appreciable reaction was

observed in all test samples. The metal was severely attacked and the reaction products formed

were observed to break off and float into the surrounding semiconductor. Using the 24 hour run

as the most severe test, our resutts indicate that on a 27 mil thick WC-103 sample, an average

of 6.69 mils (25% of the thickness) may be lost if the metal and molten semiconductor are held

in contact for 24 hours at 1260°C.

CdZnTe/WC-103 Compatibility Tests

Two CdZnTe/WC-103 compatibility tests have been completed. These runs were for 12,

24, and 90 hours at 1170°C. The results of these tests are presented below:

24 hour CdZnTe/WC-103

A cross-section of the 24 hour CdZnTe/WC-103 couple is shown in Figure 14. This

macrograph shows the presence of a well defined reaction zone at the metal/semiconductor

interface. Figure 15 indicates the presence of an adherent reaction zone.

The SEM/EDS analysis, shown in Figures A7 and A8 in Appendix A, verifies the well

defined reaction zone at the metal/semiconductor interface. This reaction zone is a mixture of

semiconductor and metal. This reaction zone, as stated above, was adherent and did not appear

to break off into the semiconductor as was observed consistently with the GaAs/WC- 103 reaction

couples.

A-18

Figure 14. Cross section of a CdZnTe/WC-103 reaction couple after a 24 hour compatibilitytest at 1170 ° C.

Figure 15. Metal/semiconductor interface

for 24 hours at 1170°C. I

semicond UCtOF.

n :t CdZnTe/WC- 103 compatibility test carried out= mctatl, 2 = FC;ICIiOI1 (lllltlS]OI1 zone, and ._ =

A-19

The reaction zone was small, with a measured thickness of 0.062 mm (2.441 miis). This

reaction zone did not appear to effect the integrity of the metal. In fact, there was no

measurable reduction in the dimensions of the metal coupon.

90 Hour CdZnTe/WC-103

A photography of a cross section and an optical micrograph of the reaction zone observed

in the 90 hour CdZnTe/WC-102_ run are shown in Figures 16 and 17, respectively. As seen in

Figure 17, a well defined reaction layer was formed. The reaction layer was approximately

0.112 mm or 4.409 mils thick. As in the 24 hour run, the reaction or diffusion layer formed

did not affect the integrity of the metal or change its dimensions to any measurable degree. (If

anything, it appeared as if the thickness of the metal had increased slightly.) The compositional

analysis, which is shown in Figures A9 and A10 in Appendix A, likewise indicates the presence

of an adherent reaction zone at the metal/semiconductor interface.

Figure 16. Cross section of a GaAs/WC-103 reaction couple after a 90 hour compatibilitytest at 1260°C.

A-20

Figure 17. Metal/semiconductor interface in a CdZnTe/WC-103 compatibility test carried out

for 90 hours at 1170"C. 1 = metal, 2 -- reaction/diffusion zone, and 3 =semiconductor.

Summary - CdZnTe/WC-103

Table III summarizes the average reaction zone thickness observed for the CdZnTe/WC-

103 runs completed to date.

Table III

Time at Temperature Average Reaction ZoneThickness

mm (mils)

12 hours * *

24 hours 0.062 (2.441)

90 hours 0.112 (4.409)

•To be completed

A-21

As seen in Table lII, the reaction layer thickness for the 90 hour run is approximately

twice the thickness obtained for the 24 hour run. These results are consistent with the

anticipated kinetics for a diffusion controlled process where the reactants must diffuse through

the reaction layer in order for the reaction to proceed. A plot of reaction zone thickness as a

function of time =a shows a nearly linear relationship (Figure 18). The composition of the

reaction or diffusion zone is clearly seen to be a mixture of semiconductor and metal as

evidenced by a compositional analysis in this region (Figure A10). Even though a measurable

reaction layer was observed to form with this combination, any loss of metal was undeteetable.

As a result, the CdZnTe/WC-103 combination appears to be a workable solution to

semiconductor containment in the event of" an ampule failure.

0.12

0.1

E o.osE

_Dc-

O 0.06N

c-O

O 0.04

0.02

I I I I

0 2 4 6 8 10

Time'1/2 (hours)

Figure 18. Reaction/diffusion zone thickness as a function of time ,,2for CdZnTe/WC-103

reaction couples tested at 1170"C.

A-22

CdZnTe/TZM Compatibility Tests

One 90 hour run was completed for the CdZnTe/TZM compatibility tests. A cross

section of the metal coupon is shown in Figure 19. From this macrograph, along with the

micrograph shown in Figure 20, there does not appear to be any reaction or diffusion zone

which is adherent to the semiconductor/metal interface. As seen in the micrographs, a "stringer"

is observed in the semiconductor region a short distance from the interface. This stringer is

approximately 0.023 mm (0.906 mils) thick and from the SEM/EDS data is seen to be

Molybdenum rich. It is postulated that this stringer originated as a reaction layer at the

metal/semiconductor interface and over time broke away and floated into the molten

semiconductor. The stringer remained in tact and was observed on all sides of the metal

coupon. The SEM/EDS analysis across the semiconductor/metal interface is shown in Figures

All and AI2 in Appendix A.

Results of the measurements on the metal coupon indicate no significant effect on the

thickness or integrity of the metal.

Summary - CdZnTe/TZM

The CdZnTe/TZM couple, from a semiconductor/metal compatibility standpoint shows

minimal reaction for 90 hours at 1170°C.

zone formed or any loss of metal thickness.

There does not appear to be any significant reaction

Thus, from the compatibility tests conducted in this

study, the CdZnTe/TZM combination is determined to be a suitable semiconductor/cartridge

combination.

A-23

Figure 19. Cross section of a CdZnTe/TZM reaction couple after a 24 hour compatibility test

at 1170°C.

Figure 20. Metal/semiconductor interface in a CdZnTe/TZM compatibility test carried out

for 24 hours at I170°C. 1 = metal, 2 = "stringer", and 3 = semiconductor•

A-24

Conclusions

Based upon the results of the experiments conducted in this study, the following

conclusions have been made:

1. There was a considerable reaction between the GaAs and the WC-103 couple for

all three runs (6 hours, 12 hours, and 24 hours) at 1260°C. Reaction products

formed at the metal/semiconductor interface and these products broke off and

floated into the molten semiconductor. Metal loss ranged from 0.07 mm (2.76

mils) to 0.17 mm (6.69 mils) for the three runs. In the worst case situation,

where the WC-103 was exposed to molten GaAs for 24 hours, it was determined

that a 27 mil thick cartridge would undergo a 25% reduction in thickness.

. In the CdZnTe/WC-103 reaction couples run at 24 and 90 hours at 1170°C, a

reaction or diffusion zone was observed to form at the metal/semiconductor

interface. This zone was adherent to the metal surface. The average thickness

varied from 0.062 mm (2.441 mils) for the 24 hour run to 0.112 mm (4.409 mils)

for the 90 hour run. There did not appear to be any significant loss of metal for

either reaction couple.

, The CdZnTe/TZM reaction couple run for 90 hours at 1170°C showed minimal

reaction at the metal/semiconductor interface. There did not appear to be any

measurable change in the dimensions of the metal in the couple.

A-25

Appendix A

SEM and EDS analysis of GaAs/WC-103, CdZnTe/WC-103,

and CdZnTe/TZM reaction couples.

A-26

Figure AI. SEM micrograph of GaAs/WC-103 couple tested at 1260"C for 6 hours.

Numbers indicate points where compositional analysis was performed.

A-27

Figure A2. Compositional spectra across the semiconductor/metal interface of a GaAs/WC-

103 reaction couple tested at 1260°C for 6 hours.

A-28

_AS6S-S[H[-| Preset, 200 sees_Vert, 2057 counts Dtsp, t (lapsed, IGe secs

Ga

10-Dec-t?gt 11:01:59

_RRSGS-S(MZ-2 Preset- 280 secsVert- 2238 counts Olsp- 1 (lapeed. 118 sees

Ga

Quan_ex)

J

4- 9.000 Range- 20.468 key 20.229 -kIntegral 8 - 181968

! !8-De¢-1991 t1:04:$2

! GRnS6S-ZONE- !, Vert. 4765 counts

I t_b' $u._nlex )

Ast

,iT'_,J/!

Preset- 200 secsDlsp, I (|opsed- 100 secs

As/

Hb T i C,a _ A_

0.000 Range- 20, 460 keVIntegral 0

1i6 118Z0,220 -_

203670A-28_

!_o[,e¢-1991 11:07:18

_;AAS6S-ZONE-2Vert- 5Z28 counts

Hb

,_u._nt _ x )

Asl

t-

Preset. 20e secs

Dlsp, I Elapsed. IBB secs

,00_ Range- ;_.468 key Z_.Z2_ -_Integral g 7.07360

_e-[,ec-199L [t:gS:37

GRAS6S-ZOME-3 Preset. 2Be secsVert. 5302 counts Dlsp, I Elapsed. lee secs

Hb

_uantex)

Asl _ _ As

I I 14 16 I 8 Ila I1Z I 14I 4- 0.008 Range- 20.468 key

Integra| 0

116 118Zeo228 -_

Z_9Z75

!_-Dec-199L L1:11:37

GARS6S-ZOflE-4Ver_- 10194 counts

Hb

HI

Nt

Hi

T,/

4-

Preset- 280 secsDlsp- I Elapsed, lee secs

14b T I He Hf Hf

112 _ 14

.OOO _'_nge, 20.460 key

I16 118

20.7.20 -).A-28b

' :_-[,ec-1991 11:13:26

';AAS6_'METAL-I Pretet. 2e0 secs_rto 957? counts DIspo I Elapsed, lee secs

rib

HY

r41o

H'_ llb T l Hf

14 m : e lie lle I 14 Is6 Jle4- O.el_8 Range- 28.460 key ZS.ZZ8 -t"

Inte$ral B • ZTe428

1_-0ec-1991 11:15"07

SARS6S-METAL-2 PreseLl 208 secsVert- 1e988 counts Dlsp. 1 Elapsed. 110 sees

Nb

H;_b

I Htf Nb T| H_ Hf

_ j_a Hf

Z Id _ 1 8 110 iIZ 114 116 1184- 0.000 Range- 28.460 key 20.Z20 -F

[nLegral 0 290254"

_8-Jan-1992 16:14:56

';AAS6S-METAL-3 Preset. 180',,_,. 98Olco.n,, D,,.. I _l.ps,d. 10e::::Mb

Tt Hf Hf

i 4- O.gO0 Ra, ng."- 20.46g keYr_, ..... i n

116 lie19.900 -b A-28c

Figure A3. SEM micrograph of GaAs/WC-103 couple tested at 1260°C for 12 hours.

Numbers indicate points where compositional analysis was performed.

A-29

Figure A4. Compositional spectra across the semiconductor/metal interface of a GaAs/WC-

103 reaction couple tested at 1260°C for 12 hours.

A-30

_1-Dec'1991 14:48:46

:_AASI2S-I Preset- t00 sees

'Vert, 2084 counts Disp. 1 Elapsed. 100 secs

_a

k|

tks Ga

___a iJ 2 14 I 6 18 I 16 118

4- 0.000 Range- 20.46e keV 19.9e0 -_

Inteiral 0 - 168980

Z1-Dec-1991 t4:SZ:ZO

GkkS]ZS-Z Preset l |00 $ecs

Vert. 257 counts Drip- I [|apsed, [00 secs

_a

Ga

ks As

As Lj.As

12 14 16 10 I 10" 112 114 I16 118

_- 0.000 Range. 20.468 key 19.900-_

Intesra| 0 ZIZ20

2[-Dec-1991 14:_4:20

.Execution time , 3 seconds

_GkAS12S-3

Yert, _|76 counts O|sp, 1

_aQuant_x)

Preset, 100 secs

Elapsed- 100 secs

k s la

_3,; .12 14 16 18 I 10 112 114

4- 0.800 Ran9e- 20. 460 keV

116 lib

19.9B8 TFA-30a

21-Dec-1991 15:06:30Execution time - 2 secondsGRRS12S-4Vert, 4907 counts Dlsp- I

fib

J,

Presetm

Elapsed.

tog eecs108 secs

Hf

Hi Ga As

H,] TI HfHfH,

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116 110

20.220 -_Z21887

21-Dec-1991 15:00:0g

GAAS12S-S Preset-

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180 secs100 secs

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IZ 14 16 18 I18 112 1144- 0.000 Range- Z0.460 key

|ntegra| 0

116 118

ZO,ZZO -_• 169497

$7-Feb-199Z 15:03:0Z[xecutLOn time • 2 seconds_AAS1ZS°6 Preset.vert, 2125 counts DIsp- 1 Elapsed-

Ga

As

4keV

[nteqra}

100 secs100 sece

116" 11820.2Z8 -F

171_qAA-30b

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key

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preset. 100 secs(lapsed- t00 secs

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A-30c

71-D_c-1991 15:23:58C,ecutlon time • 3 seconds_QA5125-10Vert- 4401 counts Disp- 1

Hb

IH¢

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IBO secs100 secs

HT

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116 lie20.460 -_

- Z29439

21-Dec-1991 15:Z5:15

GAAS125-11 Preset,

Vert. 2166 counts Disp- 1 [{apsed-Ga

10B secs100 sees

_s

Ga

12 14 l 6 IB4-

_s

iGa

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As

I11 I 12 1140.320 Range- 20.460 keV

Inlegra| 0

I1G 11820.460 -_

• 158112

21-Dec-1991 15:Z6:20

Execution t|me • 3 secondsGAAS12S-12Vert, 2248 counts OISD. i

Ga

Ouantex)

Preset-C]apsed-

I_s

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I _' |4 | 6 I B 110 ) 12 114

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]16

180 secs100 secs

20.4GQ -_172523

A-30d

121-Dec-1991 15:27:23Execution ilme • 3 secondsGAAS125-13Vert. 2134 counts DIIp. I

Ga

Ouantex)

Prelet-Elapsed-

lee secslee secs

As

JAs As

I Z 14 I 6 I 0 I|g I IZ I 144- 0.320 Range- ZO. 460 keV

Zntegra! O

116 I 1'820.466 -_

17Z6Z3

21-0ec-1991LS:Zg:teExecution time - Z secondsGARS1ZS-14Vert- Z135 counts Oispo |

Ga

Ouantex)

Preset- 196 sec$Elapsed- 100 secs

As

iAs _ Go

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L In:egra| e . 172915 J

21-Dec-1991 15:30:14Execution _tme • 2 seconds_AASI2S-ISVe_t- 2102 counts Dlsp. 1

Ga

Ouantex>

As

12 14 I 6 184- O. 3ZO Range-

Preset. lOO secsElapsed. 10e secs

As

Go

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I11_ 11'6

20.460 keyInLegral 0

I _820.468 -_

178571 A-30

21-De¢-1991 15:31:17Execution time • 3 secondsGAAS125-16Vert. 2161 counts Dlsp, I

Ga

Ouantex)

As

Preset. 188 secsElapsed- 188 secs

As

4- 0,320 Range- 20.468 keV ZQ.468 -_Inte9ra| 8 171193

21-Dec-1991 15:32:36

Execution time • 2 seconds

GAASIZS'17 Preset. leg secsVert- 5497 counts Dlsp- 1 Elapsed, 188 secs

Hb

Hf

Hf

As

As

H¢

HFHf As

TI Hf Hf Hf

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ZI-Dec-1991 15:35:15

Execution time • 2 seconds

bAASI2S°I8 Preset. 190 secsVert= 5345 counts Oisp. 1 Elapsed. 188 secs

Nb

Hf

Hf

Hf ASi

Hf I TI HfHfHf Hf

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Integral B

116 t 18

Z0.468 -_2EB768 A-30f

21-00c-1991 tS:36:ZZExc¢ut|on time • 3 seconds

GAAS125-19 Preset. 100 secsVert. 5505 counts Olsa- I Elapsed, 100 secs

Hb

Hf

iHf

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T i G,d_

Hf

As

TI Hf G_ LTl Hf Hf HfHf geHf

IZ 14 I 6 18 I1_ I IZ 114 116 I 184- 0.3Z0 Ran$e- 20.460 keV 20.460 -_

]ntesral 0 • ZZ$048

ZI-Dec-199! IS:38:27

Execution time - 2 secondsGAASIZS-Z8

Vcrt. 10935 counts Olsp. 1Hf

IHf

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ix_b

"!lHII ti

, He|.6 T, ,e HeHe H, ,b

IZ 14 I 6 IB 110 I 1Z 114 116 I IB4- 0,320 Range. 20.460 keY

Z0,460 -_Inte$ra] 0 Z93736

Preset, 100 secsElapsed- 100 sees

!21-Dec-1991 15:39:3!

Executionst?_l time . 3 seconds 1GAA____- Preset, 100 sec dVert, 10261 counts Olep. I Elapsed.

Hf 100 secs /

')uantex)

Hf

rib

iF/,f

H[I_ TIHb

He"/rtb T, Hf HfHf Hf

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Nb

Hb Hb

_'12 114 JIG I 10 --

A-30g

_l-Dec-1991 15:48:36

[Aecutlon time * _ secondsGAASIZS-Z2

Vert. 10Z84 counts Oisp. IHf

H(

rib

Hb

Hb H_ Ti

t'b "_ Hb T| H@ H'Hf HF

T i H/l_Xf yHr Hr HrH,_I ! -_ --_--_

iZ Id i6 18 i18(- 8.888 Range- ZS.46e keV

Preset=elapsed.

Hb

112 114 I16

Integral 0

100 sec_100 sec:

Hb

Nb

11820.Z20 -_

_08687

r_!-'-_'e¢-19_gl 15:41:44

E_eCution time • I secondsGAnSI2S-Z3

vert. 9B06 counts Olsp. iHf

Ouantex)

Nb

Preset.Elapsed.

100 secs

100 secs

feb

IZ 14 16 18 I10-- IL2 f 14(- O.OOO Range- 20.460 keV

Integral 8

Hb

Hb Nb

116 ilO

20.220 -_288Z58

A-30h

Figure A5. SEM micrograph of GaAs/WC-103 couple tested at 1260°C for 24 hours.

Numbers indicate points where compositional analysis was pertbrmed.

A-31

Figure A6. Compositional spectra across the semiconductor/metal interface of a GaAs/WC-

103 reaction couple tested at 1260°C for 24 hours.

A-32

_9-Jan-1992 09:36:55

3_asnZ4s-I Preset° 100 seesVert. Z053 counts Olsp- Elapsed. 100 seesOuantex) Ga

As

IZ 14 i 6 18 110 I IZ 114 116 I 184- 8,000 Range- 20.460 key 20o140 -_

Integral B 161344

14-Veb-1992 17:Z5:48

9aasnZ4s-2 Preset= 100 seesVert- 89 counts Elapsed. 100 secsOlspo

r;b

Ga

Ga

IZ 14 16 18 110 _' 114 116 118(- 0.00_ Range- 20.460 key ZO.Z20 -_

Integral 8 0

)_9-Jan-199Z 09:41:58

3_asnZ4s-3 Preset. 100 seesVert. 1951 counts Dlsp- Elapsed, 100 sees

Ca

Nb

12 14 I 6 18 116 I IZ----_4 116 I 184- 0.800 Range- 20.460 ke',' ZO.14B -I,

Integral 0 104730A-32a

IT-Feb-1992 IZ:ZS:58

9aasnZ4s-4Vert, 33 counts DIsp-

fib

I in iz 14 m is4- 0.888 Range-

GQ

Ga

,,428.468 key

IntegraI B

116

188 secs188 secsi

118Ee.z2e -_

2489

29-1an-1992 09:46:35

9aasnZ4s-5 Preset-Vert- Z138 COUnts Disp= (lapsed,

_a

As

IZ 14 I 6 I 8 118 I IZ 1144- e.888 Range- Z8. 468 keV

Integral 8

188 secs188 secs

116 118Z8.148 -_

166931

39-/an-199Z 89:52:06

g_asn24s-6 Preset-Vert, $115 coun_# Dlsp- I (lapsed-

Mb

As

Ti As

IZ 14 I 6 18 110 I J2 114_- _.£10e Range- Z0.468 keV

Inte,lral @

116

188 see,188 sec*

118Z0.140 -_

ZI7331 A-32b

_9-]an-tgSZ 89:55:08

9aasn24s-7 Preset-V_rt, 4980 ¢ount$ Olsp- 1 Elapsed-

Nb

198 secs168 =ec=

As

Tt

TI A=l Xf _a.

Jr_2____I= 14 I 6 18 Itg I 12 114

4- 8.808 Range- Z0,468 keY[ntegra| e

116 11828,148 -_

228972

29-Jan-199Z 09:57:37

saasnZ4=-8 Preset=VePt- 18876 counte Dlsp= 1 Elapsed-

Hb

189 sees100 sac=

TI Hf

Tt

12 14 I 6 18 118_- O.OEO Range- 20.460 key

I 1Z ' Ill' 116 I iBZO.t4O -_

Integral O 283313

29-Jan-1992 09:59:19

9aasnZ4s-9Veer. 18093 counts

HbDlsp- 1

TI HF

Tl

12 14 I 6 18 110 'J 12(- 0.000 Range- 20,46(] keV

Preset.Elapsed.

lOO sacslOO sacs

114 116 118

• . 2o.l_p_:_ A-32,

Figure A7. SEM micrograph of CdZnTe/WC-103 couple tested at l l70°C for 24 hours.

Numbers indicate points where compositional analysis was performed.

A-33

Figure A8. Compositional spectra across the semiconductor/metal interface ofa CdZnTe/WC-

103 reaction couple tested at I170°C for 24 hours.

A-34

_l-De_-1991 14:21:0e

CZT24S-I Preset-Vert, 4.597 counts Ols_, 1 Elapsed,

CdCd

n2

i I. 14 I 5 18 I lU IIZ i 114 116 libi 4- 8,008 Range- 20 460 key 19 988[ " Intesral S - "Z$$|'53

lBe sec_168 secs

21-0ec-1991 14:Z3:18

CZT245-2Vert,

Ouantex)

Cd

4- O, 000

Preset. 100 sacs5566 counts Olsp, 1 Elapsed. 118 see

Cd

Te

Te

Cd

Te

Te

14 I 6 18 I 10Range. ZO.d6E keV

112 'm 114 115 118

19.900 -kIntesral O - ZOISG7

21-['ec-1991 14:Z4:23

CZTZ4S-3Preset. tOOvet,. 3865oo,nt. D,.o. _ Elapsed. ::_:

Te 100

|TaTs

Te

_- O.OeO Range2 ,_0.460"" keY'_ ,1_ 11419. 900 -),

Inteara) 0 _A_lqA-34a

21-Dec-1991 14:25:27

CZTZ45-4 Preset- Ie8 secsVert. 48Z4 counts DIsD- ! Elapsed. 188 secs

CdTe

Ouantex)

Te

_Te

Hb(

I £/I

14- 8.83B Range- 20.466 key 19.9B8-_Integr'a| 8 • Z61187

._l-Dec-t991 14:ZG:45

CZT245-5 Preset- 188 seesVer.t, 5185 counts DIsp, ; Elapsed- 188 sees

CdCd

TeQuan_ex)

Te

Cd

Te

Te

zn14 I 6 18 I 18 IIZ "114 I 15 I1B4- • Range, Z0.468 keV 19.908 -_

Integr.al 8 286143

21-Dec-1991 14:Z7:49

CZTZaS-6Vet.t, 5351 counts

CdCd

Te

_uantex)

Te

Cd

Te

4- O. ee8

Preset- 18e seesDisp. 1 Elapsed= 18e see1

Te

Te n 114I_ I12

Range- 20.46e keY

Integral 0

116 11819,900 -_

273041 A-34b

31-Dec-1991 14:29:14

CZT24S-? Preset, IB8 sacsVert. 5198 counts Dlep- ! Elapsed. |80 secs

_dCd

&Te

Te

Te

19.9B8 -_4- e. OOO Range- 20.460 keyIntegral e 266550

Ouantex)

_1-Dec-199! 14:30:43

CZT24S-8Vert. 5163 counts

CdCd

Te

Te

Preset- 100 secsDlsp- ! Elapsed, lOO sacs

eTe

Te

4- 0.800 Range. 20.468 key 19.900-_]ntegrsl O 264311

21-Dec-1991 14:31:48

CZTZ4$-9Vert. 5262 counts

CdCd

Te

O,Jan rex > jTe

c'."re

_,J,P4- O. 0G0

Preset- 100 sacsDlsp- 1 Elapsed. 1B9 sac

Te

_ Te n

14 I 6 18 I 10 112 114Range- 20.460 keV

Integral

116 I1019900 -_

267795A-34c

Preset. 190 sec_DJsp. i Elapsed, IZO secs

CZT245-18Vert. 6L90 count=

CdCd

Te

Ou_nt_x ) l

Te

c3Te

Te

I ,Jl, . ,, ,,,_,,_,_I- 0.000 Range. 20.460 keV 19.900 -_

Integral O 313449

21-Dec-1991 14:33:56

CZT24S-11 Preset. 108 secsVert. 5197 counts OJsp. | Elapsed- 100 secs

"CdCd

Te

Te

4- 0.008 Range. 20.468 key 19,900 -FIntegral O 260427

121-Dec-199! 14:3S:0e

CZT24S-t2 Preset. 100 secVert. 5123 counts Dtsp, 1 Elapsed. 100 sees

Te

Quantex)

Te

4- 0.800 Range- 20.460 key 19.9(]0 -I,Integral 0 22D907 A-34d

21-[,e¢-1991 14:36:06

CZTZ4$-I3

Vert. 4_4 Counts

Te

IOu_ntex)

I

fib re

T

Cd

TI ]

t- 8. roe

Preset- 19e sec$Dlsp. 1 Elapsed. 180 secs

Te

I 114Ranae, ZE.468 keV

]ntesrel E

116 11819.909 -)

• 225613

2L-Dec-1991 1d:37:18

CZT24S-14Vert- 447 countz

Te

Quantex )

HT

r_b

Te

Te

Te Te

Cj

t- e. eoe

Preset- le8 secsOlsp- I Elapsed. leo secs

14 I 6 Ie I 18 I1Z 114Ran$e- 2B.46e keV

Integral 8

116 11819.968 -_

218049

31-Dec-1991 14:38:Z4

CZT24S-ISVeer. 60Z9 counts

Ouantex )

Preset- lee sec$Dlsp, 1 Elapsed- IBe secs

Te Te

j --' tetl

Hf NbJ ,Te Hf

A J • I --I__12 14 16 18 I 10 112 lid

[ :- 0.000 Range. Z0,460 keV

L__ ................ Integral 0

116 IlB19.900 -_

197007 A-34,

_I-Dec-1991 %4:39:29

CZT24S-16 Preset.Vert* 6618 counts Plsp- I Elapsed*

Nb

_uan_x)

LeO secs10Q sees

Hfii

tlb

2 14 16 IB I 10 112 1144- 0.000 Range- 20.468 keY

Int.egra I 0

116 11819.989 -_

186154

Zl-bec-1991 1,::40:32

CZT245-17 Preset-Vert. 6773 counts Dlsp. 1 Elapsed.

_b

Ouan_ex)

100 sees108 secs

j Hfii

! rib;L

I HF TI Hf

Ti / _

J "- 14 16 18 I 10

_- 0.000 Range- Z0.460 keYIIZ 114 116 118

19.900 -_Integral 0 1905S2

Vert. r.lb6S46 counts

Dlsp. I

Hf Hb T I Hf

_- O, 000 Range • 20.46B keY

Preset. 100 secsElapsed. 100 secs

r{_-- 114 ;L6 i1819.900 -_ A-34f

Figure A9. SEM micrograph of CdZnTe/WC-103 couple tested at 1170°C for 90 hours.

Numbers indicate points where compositional analysis was performed.

A-35

Figure A 10. Compositional spectra across the semiconductor/metal interface ofa CdZnTe/WC-103 reaction couple tested at 1170°C for 90 hours.

A-36

6-Feb-199;' 2(?.:I-1:08

C,ZTgOS- I

Vet&, 597 counts Dlsp. |Cd Te

tCdTe

_ZI Z 14 16 I 8 Ile IIZ I 14 '

4- e.6ee Range- 2e. 46B keyIntegral I

_reset-Elapsed.

I09 secs18B secs

116 11828.228 -_

• e

6-reb-199_ 22:44:23

CZTgOS-2Ver_. G606 counts

Cd

Te

Preset-

Dlsp, 1 Elapsed.

C

Te

Te

Te

t- 0.88B Range- 28.460 keY ZB.Z2B -_Integral [ - Q

6-reb-199Z 2_:$6:32

CZT90$-3 Preset- 188 secsVert, G579 counts Dlsp- [ Elapsed, leB secs

Cd

Te

Cd

Te

Te

Te

14- O.OQ_ Range, 20.460 keV E0.2_0 -_Integral ! 0

A-36

6-reb-19?2 Z2:SO:51 ICZTgOS-4 Preset. leo sec;Vert- 11153 counts Plsp. 1 [lapsed. 170 #ecs

Cd

_e

CO

Te

Te

Te

4- 0,880 Range- 20.460 key 28.228 b]ntegro| 1 - -_

I -Feb-1992 Z2:Z8:36

CZT90S-5

Veer. 6845 countsCd

Preset- 188 secsDlsp- 1 Elapsed. le4 sec:

I e

Te

Te

Te

_- 0.0BB Range- 2B.468 key ZS.Z28 -_Integral I 8

G-Feb-1992 22:Z2:03

CZT90S-6Veer. 6479 counts

Cd

Te

Preset. leo secsOlsp- I [lapsed- 190 sec#

tITTe

4- O.BOg Range- :20.468 keV Zg._.2g -I,Integral i 0 A-36b

6-feb- 1992 22:Z4:59

CZTgOS-7 Preset. [88 secsVert. 6479 counts Olsp. I EI6psed- 108 secs

Cd

Te

Cc

4- O.OgO Range- Z0.468 keY 28.228 -)Integral | 0

6-feb-1992 22:Z6:SJ

CZT98S-8

Vert- 5014 countsTe

Nb

Te

! Te

T, C_IT_

Preset. 100 secDisp- 1 Elapsed- 189 secs

IZ 14 16 18 lie IlZ I 14 115 ItO(- o.ee0 Range. ZO.46e key ZO.Z20 -F

[ntesrel t 0

6-1feb- [ 992 22:30:05

CZT98$-9Vert, 574 count#

Te

Ib

Te

¢dl

N

I 2 14 IG4- 0, _]OQ Range -

Preset. lOB seesDlsp. I Elapsed. ]00 secs

Hf

I0 11820.460 key

fIT---T]4 Jr6 11o20.220 -_

Integral 1 0A-36

6-reb-199Z 22:32:55

CZT90$-IOV:rt* 5856 counts

Te

_b

re

Te

Ca

I 2 14 16(- 0,080 Range-

Preset- 100 secsOlzp. I Elapsed- ]00 secz

18 118 112 114 116 lIBZ0.468 keV ZS.ZZ8 -k

Integral 1 0

6-Feb- L992 Z2:34:40

CZT9OS-[1'err t- 5"/'88 count#

Te

Nb

Te

Cd

._/IZ

t- 6. ee8

Preset= 108 secsOlsp- 1 Elapsed. 188 secs

Te

14 16 I 8 118Range- ?'8.468 keV

112 I 14 116 li820.Z28 -k

Integral 1

6-reb-199z LL:39:38

CZTgOS-lZVer_- 8558 counts

Nb

DAsp. L

Ti Hf

12 14 16 I B I1e 112O.8Oe Rangel 20.468 key

Preset. LOB secsElapsedl L80 Sees

]14 116 ]18_O.Z20 -_

Integral 1 0 A-36d

Preset= tg8 secDisp. I Elapsed. 181 lees

6-Feb-1992 11:4l:22

_ZT90S-13Veer. 8760 counts

Mb

T! J Ti Hf

I Z 24 16 18 Ill IIZ " 114 116 t184- 8.888 Ranse- 20.46B key 28.22B -_

lntegrel 1 - e

6-reb-199Z 1|:44:52

CZT90S-14 Preset- 180 eeceVert- 859Z Counts Ollp. 1 (lapsed- 180 eels

INb

t TI Hf Hf

,-[_,22 14 16 18 lib

(- 0.eel RanBe - 20,460 keV112 1[4

]ntegral t

116 It8

A-36

Figure All. SEM micrograph of CdZnTe/TZM couple tested at 1170°C for 90 hours.

Numbers indicate points where compositional analysis was performed.

A-37

Figure A12. Compositional spectra across the semiconductor/metal interface of a

CdZnTe/TZM reaction couple tested at 1170"C for 90 hours.

A-38

IO-Teb-199Z Z1:84:57

TZM-CZTgBS-I Preset- 188 seesVert, 5797 counts Dlsp. 1 Elapsed- 180 secs

C'd

dl TM

4- 0.B88 Range- 2B.4G8 keV 19.9B8 -_Intesral 8 Z913B8

lO-reb-1992 21:B6:11 IPreset. 108 secs I

TZM-CZT9OS-Z

Vert. 6379 counts Olspo I _lapsed= 100 secs I_dT_

Cd

Te

Te

• u o 19o98B -_Integral 8 • 3213_3

10-leeb- 1992 21:11:,15

TZM-CZTgBS-3Vert. 4329 count*

le

,J

{- O. 000

Preset- 108 secsDlzp. ! glapeed. IB8 secs

T¢

14 16 18 I 10 I1Z 114Range- 20.460 keV

[nteara|

116 lib19.?OB -_

PTA_qQ A-38;

lO-Feb-1992 2t:08:54 - " I

Tz.-czT�es-_ P,;:::,:, leo se_.Vert. 5833 counts [_llp- i -.-. • |80 secs

C'd

d Te

I1).

t- 0.000 a ge, 2 . 60 • 19.9 0 -_Integral 0 Z94079

|8-Feb-1992 21:10:18

TZM-CZT90S-5 Preset= 100 seesVert- 5314 ¢ountl DIIp- l Elapsed- 108 secs

_dTe

Cd

Te

Te

Te

4- 0.000 Range- Z0.460 key 19.900 -kIntegral 0 • 293766

10-reb-1992 21:13:00

TZM-CZT90S-6Vert- 6Z39 counts

¢'d

I"

Te

JIZ 14 16

4- 0. 808 Range -

Preset. 180 sec_Dlsp, 1 Elapsed- 100 secs

2n

10 i 10 H2_-_4 I 16 lib

Z0.460 keV 19.900 -_Integral 0 313366 A-38b

lO-Feb-l.qgz 21:14:11

rZM-CZTg95-7Vert. 66Z3 counts

C'd

Preset- 188 sacsDlsp- | Clapsed. 188 secs

d

Te

Te

Te

19.988 -F|ntegral 8 - 29S682

18-Feb-199Z 21:15:34

TZh-CZT98S-8 Preset- 188 secsVert. 6449 counts Dlsp. ! Elapsedo [88 sacsde

Te

Cd

Te

Te

, Inte,r,, 8 .

1e-Feb-1992 21:21:87

TZM-CZT985-9 Preset- 188 sacsVert- 778 counts Dlsp, 1 Elapsed. 18B sac

Mo

Te

14 16 18 I 10 IIZ 1141- 0.808 Range- 20.4i_0 keV

Integral 0

I 16 11819.980 -F

623_5 i A-38

1S-Feb-1992 21:Z3:41

TZM-CZT985-IgVert. 18914 counts

Mo

T! TI

IZ 14 164- 6.g88 Rangeo

Preset- 188 secsD|sp- I Elapsed- ]Sg secs

18 I 18 112 114 116 11828.468 key 19.988 -)

Integral 8 • 263398

Preset- 188 sec:Dlsp. 1 Elapsed. 180 sees

18-F'eb- 1992 21:24:45

TZM-CZTggS-I 1Vert. 11163 counts

Mo

2'J "IZ 14 16 18 I 18 I1 :_ 114 116 118

4- 8.888 Range- 20.468 ke9 19.988 -_Integral 8 267187

lg-Feb- 1992 21:25:52

TZM-CZTgBS-12Verto 11114 counts

Mo

Tz TI

I_ 14 16_- 0.000 Range.

Preset. 188 secsDlsp. 1 Elapsed. 188 secs

80.468 key 19.900 -_[ntegral g Z66098 A-38d

[8-feb-|992 21:Z6:56

TZM-CZTgOS-13Vert. 1114 counts

Mo

TI T|

IZ 14 16 IB 118(- 8.e08 Range- Z0.468 keV

Preset- 188 sac:Dlsp. I Elapsed, IBO sacs

11"2 114 116 1|8 :19.996 -_

Intesrai 8 266898

Preaet= 189 sacsDtsp, 1 Elapsed- 188 sec

10-Feb-1992 Z1:ZS:S5

TZH-CZTge$-14Vert- 11114 counts

Ho

T! TI

IZ It 16 18 118 112 114 116 1184- 8.808 Range- Z0.468 keV 19.900 -_

Integral 8 Z66098

10-Feb-1992 21:Z9:04

TZMlCZTgOS-JSVert= 11114 counts

Mo

t, II ,,,4 ,64 0.006 Range.

Preset- 188 seosDlsp. I [lapsed. 180 secs

18 ! _ 112 114 ; IG 118

20.468 keV 19.900 -FIntegral O 266098

A-38e

!O-Feb-1992 21:3_:14

TZM-CZTgeS-16 Prese%- 100 secsVert- 11114 count* Dlsp- I Elapsed. 100 sec$

Mo

T| Tl

12 14 16 18 I 10 i 112 114 116 lIB(- 0.000 Range- Z0.460 keV 19.9B0 -_

Inte9ral 0 286098

1e-Feb-1992 21:38:15

t zm-czt90-Ioose-1 Preset- 180 secsVert. 4301 counts D|sp, 1 Elapsed, 180 $ec$

C'd

l]Cd

Te

Te

Te

4- 8.080 Range- 20.460 keV 19.988 -_Integral 6 Z13860

A-38f

Chemical Compatibility ofCdZnTe with Silicide Coated WC-103

Addendum to:

Progress Report

on:

Chemical Compatibility Studiesof GaAs & CdZnTe

with WC-103 & TZM

by:

Rosalia N. Andrews, Ph.D., P.E.Department of Materials Science and Engineering

University of Alabama at BirminghamBirmingham, Alabama 35294

April 20, 1992

A-39

Original Progress Report:February 10, 1992

Introduction

The following report summarizes the results obtained for the CdZnTe/ silicide coatedWC-103 compatibility test run at 1170°C for 90 hours. WC-I03 test coupons of9.960x9.962x4.978mm were obtained from Southern Research Institute. Two surfaces of these

coupons were polished using a procedure identical to that discussed in the initial reportsubmitted on February 10, 1992. This initial report should be referred to for details onprocedure. Following surface preparation, test coupons were sent to HITEMCO for silicidecoating. Samples were given a heat treatment of one hour at 1566"C (2850" C) after coatingto ensure bonding of the sillcide coating.

Sample/semiconductor compatibility tests were accomplished by immersion of the test couponsin molten CdZnTe for 90 hours at 1170"C using a procedure identical to that discussed in thereport of February 10, 1992.

90 hour CdZnTe/Silicide Coated WC-103 Compatibility Test

An optical micrograph of the reaction zone observed for the 90 hour CdZnTe/silicidecoated WC-103 couple is shown in Figure 1. The original thickness of the metal coupon was4.930 ram. The final thickness of the pure metal was - 4.883 ram. However, this reductionin metal thickness did not appear to be due to a reaction between the metal and semiconductor.Apparently the reduction in metal thickness resulted due to interdiffusion between the silicidecoating (original thickness 0.056ram or 2.2 mils) and the base metal. The thickness of theinitial silicide coating was seen to increase during the compatibility test resulting in a finalthickness Of 0.079mm or 3.1 mils. After testing, base metal from the coupon was foundthroughout the silieide coating implying the layer had changed to a mixture of silicide and WC-103. See Figure 2 and EDS plots 1-16.

Figure 1. Metal/silicide coating/semiconductor interface in a CdZnTe/silicidecoated WC-I03 compatibility test carded out for 90 hours at 1170C.

A-40

There does not appear to be any significant reaction between the CdZnTe and the silicidecoating. Note also that in those regions where there is a scratch or defect in the silic;decoating, the semiconductor has penetrated. Therefore, it is imperative that no defects arepresent in the coating as applied and that utmost care be taken in the handling of the coatedcartridges to prevent damage to the coating. I understand there has been some considerationgiven to only coating the outside surface of the cartridges. This approach would provide nobarrier to the attack of the WC-103 by the CdZnTe semiconductor in the event of an ampoulefailure. While the silicide coating would not be chemically attacked in the event the WC-103was totally consumed by the molten semiconductor, it would not appear that the silicide coatingis in, and of itself, sufficiently substantial from a mechanical standpoint to withstand the

significant .v'a:por pressure of the semiconductor. In summary, the silicide coating appears tobe effective m reducing and/or eliminating WC-103/CdZnTe reaction and if applied to theinterior of the cartridge should enhance the ability of the cartridge to function more effectivelyas a second level of containment.

Figure 2. SEM micrograph of CdZnTe/silicide coated WC-103 tested for 90 hours at

1170"C. Numbers indicate where compositional analysis was performed.

A-41

Summary of Findings to Date for WC-103 Cartridge Material - Recommendations

1)

2)

3)

From a semiconductor/metal compatibility standpoint, the CdZnTe/WC-103 coupleappears to be a workable solution to semiconductor containment in the event of anampoule failure. However, some evidence of a variation in the degree of attack withsurface finish was noted during testing. It appears that best results are obtained with ahighly polished surface.

From a compatibility standpoint the CdZnTe/silieide coated WC-103 couple also appearsto be a workable solution to the semiconductor containment problem in case of anampoule failure. It is recommended that the inside of the cartridge be coated with asilicide layer at least 4-5 mils thick. To be effective, this coating must be perfect andcare must be taken not to scratch the coating after application.

Due to the vigorous reaction of GaAs with WC-103, which results in metal reactionproducts which spall off, I do not recommend that WC-103 be used in combination

with GaAs. Optional coatings or cartridge liners should be investigated for thismetal/semiconductor combination.

A-42

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Chemical Compatibility of (3aAs with Silicide Coat_ WC-103and Hot Pressed Boron Nitride

Addendum to:

Progress Report

on:

Chemical Compatibility Studies

of GaAs & CdZnTe

with WC-103 & TZM

by :

Rosalia N. Andrews, Ph.D., P.E.

Sherrie A. Beske, Research Assistant

Department of Materials Science and Engineering

University of Alabama at Birmingham

Birmingham, Alabama 35294

April 1, 1993

Original Progress Report:

February i0, 1992

A-61

Introduotion

The following report summarizes the results obtained for the

GaAs/silicide coated WC-103 and GaAs/hot pressed boron nitride

compatibility tests run at 1260°C for 24 hours. WC-103 test coupons

of i0.Ii0 x 10.120 x 5.044 mm and hot pressed BN test coupons ofi0.000 x 9.995 x 5.000 mm were obtained from Southern Research

Institute. The WC-103 coupon surfaces were polished using a

procedure identical to that discussed in the initial report

submitted on February i0, 1992. This initial report should be

referred to for details on experimental procedure. Following

surface preparation of the WC-103, test coupons were sent to

HITEMCO for silicide coating. Samples were given a heat treatment

by HITEMCO of one hour at 1566°C (28500F) after coating to ensure

bonding of the silicide coating. Two surfaces of the hot pressed

BN coupons were abraded with #98 Scotch Brite and rinsed three

times with methanol. The coupons were then heated with a heat gun

to remove any residual methanol.

Sample/semiconductor compatibility tests were accomplished by

immersion of the test coupons in molten GaAs for 24 hours at 1260°C

using a procedure identical to that discussed in the report of

February i0, 1992.

24 hour GaAs/Silioide Coated WC-103 Compatibility Test

An optical micrograph of the reaction zone observed for the 24 hour

GaAs/silicide coated WC-103 couple is shown in Figure i. Theinitial thickness of the bare metal was -4.932 mm. A silicide

coating of -0.056 mm (2.205 mils) was applied to each side of the

coupon. The total thickness of the coated metal coupon was thus

5.044 mm. The final thickness of the remaining metal coupon after

the compatibility test was -4.757 mm. The total loss of coupon

thickness was 0.287 mm (11.299 mils). Considering attack from one

side of the sample, as would be seen in a cartridge assembly, this

amounts to a thickness loss of of 0.144 mm (5.565 mils).

After completion of the compatibility test, no silicide coating

could be found using EDS analysis. Several locations in the pure

semiconductor, the reaction product, and in the metal were

analyzed. No traces of silicon, iron, or chromium, the principle

components of the silicide coating, were found at any of the

locations. Traces of arsenic were found in the metal coupon, with

the concentration of arsenic becoming negligible at - 0.07 mm (2.76

mils) away from the interface. See Figure 2 and EDS plots 1-12.

A-62

The silicide coating did not prevent GaAs attack of the WC-103. On

exposure to molten GaAs for 24 hours at 1260°C, a 27 mil thick WC-

103 cartridge with a 2.205 mil thick silicide coating (total

thickness 29.205 mils) would experience approximately a 20%

reduction in thickness. Also, there would be arsenic penetration

into 0.07 mm (2.76 mils) of the remaining metal thickness.

Figure 1. Metal/silicide coating/semiconductor interface in a

GaAs/silicide coated WC-103 compatibility test carried

out for 24 hours at 1260°C. l=metal,2=reaction zone, and

3=semiconductor

A-63

Figure 2. SEM micrograph of GaAs/silicide coated WC-103 tested for

24 hours at 12600C. Numbers indicate where compositional

analysis was performed.

A-64

24 hour Ge_s/Hot Pressed BN Compatibility Test

The GaAs/hot pressed BN couple as removed from the boat after the

compatibility test is shown in Figure 3. On initial observation,

it did not appear that the ceramic coupon was wet by the GaAs. An

optical micrograph of the semiconductor/BN interface for the 24

hour GaAs/hot pressed BN couple is shown in Figure 4. There did

not appear to be any visible reaction product. The original

thickness of the hot pressed BN coupon was 5.000 mm. The final

thickness of the coupon was - 5.000 mm. Thus, no loss in material

thickness occurred due to exposure to GaAs.

Figure 3. GaAs/hot pressed BN couple after compatibilitytest carried out for 24 hours at 1260°C.

A-65

The semiconductor/BN interface was examined using EDS analysis.

Traces of arsenic were found at 0.21 mm into the ceramic coupon,

but at 0.30 mm, the traces of arsenic became negliglble. Binding

elements used in hot pressed BN were also found throughout the

ceramic coupon. See Figure 5 and EDS plots 13-22.

There did not appear to be any visible reaction between GaAs and

the hot pressed BN. For a 27 mil thick BN cartridge exposed to

molten GaAs at 1260°C for 24 hours, there would be no reduction in

thickness. There would, however, be traces of arsenic penetration

up to 0.30 mm (11.81 mils) into the cartridge.

Figure 4. Semiconductor/ceramic interface in a GaAs/hot pressed BN

compatibility test carried out for 24 hours at 1260°C.

l=Hot pressed BN, 3=semiconductor.

A-66

Figure 5. SEM micrograph of GaAs/hot pressed BN tested for 24 hours

at 1260°C. Numbers indicate where compositional analysis

was performed.

A-67

8umm8_ of Findings

1) The silicide coating tested in this study did not prevent GaAs

attack of the WC-103. The metal was attacked by the

semiconductor and the reaction products were observed to break

off and float into the surrounding semiconductor (a result

similar that obtaind in the uncoated GaAs\WC-103 compatibility

tests). On exposure to GaAs for 24 hours at 1260°C, a 27 mil

thick WC-103 cartridge with a 2.205 mil thick silicide coating

(total thickness of 29.205 mils) would experience

approximately a 20% reduction in thickness. Also, there would

be arsenic penetration into 0.07 mm (2.76 mils) of the

remaining metal thickness.

2) There did not appear to be any visible reaction between GaAs

and the hot pressed BN. For a 27 mil thick BN cartridge

exposed to molten GaAs at 1260°C for 24 hours, no reduction in

thickness of the BN is expected. There would, however, be

traces of arsenic penetration up to 0.30 mm (11.81 mils) into

the cartridge.

A-68

Plots 1-12. Compositional spectra across the semiconductor/metal

interface of a GaAs/silicide coated WC-103 reaction

couple tested at 12600C for 24 hours.

A-69

29-Mar-2000 18:Z2:15

E_ecutlOn time • 4 second

_._as_vc i_33_ : 1

'_'ert. 93_3 counts Dss_- 1

,)uan t e .: >

I

Preset-

Elapsed.

300 sacs

200 sets

As

14 16 18 110 112 114 116

4- 0.000 Range- 20.468 keYInte9ral 0

, =,118

20,220 -_400978

29-Mar-2080 18:31:44

Execution llme • d second

gaas_ci03si2 Preset= Z80 sacs

Vert- 9180 counts DIsp- 1 Elapsed- 288 sacs

As

4- 0.080 Range- 20.460 keV 20.220 -bIntegral 8 385222

39-Mar-2000 18:42:21

Execution time - 4 seconds

,3aaswclO3s13 Preset- 200 sets

Vert- 9409 counts DisD. 1 Elapsed. 308 secs

H$

14 IG I 8

4-

As

110 112 i-14 ''_16

0.000 Range- 70,460 keyIntegral 0

iC820. 220 -_

398870A-70

'29-Mae-2800 18:58:55

E:_cut|on time * 4 second8aaswct@3s14 Preset• Z80 secsVert- 7207 counts Dlsp• I Elapsed. 200 secs

_s

f HF

l lA,b . P| _,

4- 8.0180 Range• Z0.4_0 key ZO.Z20 -_Integral 0 • 385100

29-Mar-ZBB8 19:12:41Execution time • 4 second

gaaswc183s15

Vert 18138 counts Dlsp, 1

Hb

4-

Preset- 288 secsElapsed- 280 secs

st

12 14 16 1 8 Ile 112 I 140.800 Range- ZO. 460 keV

Integral 8

Nb

116 118

20.Z20 -_442Z28

29-Mar-2800 19:22:81

Execution time • 5 seconds_aaswclO3si6 Preset-Vert 941G counts Disp* 1 Elapsed•

200 secs200 secs

As

I 2 14 16 I 8 lie 1128.808 Range, 7'0.460 keV

Integral 8

Itb

I 14 I 16. 110ZO. 22_ -_

405735 A-71

29-Mar-2000 19:33:09

E:,ecutlon tlme • 4 second9_is_,Jc103si7

Ve,-t* 6882 counts Dlsp, 1

I

A_ _a|

As

Preset-Elapsed.

200 sacs200 _ec,

2g-Mar-2000 19:42:13Execution time - 4 second

9_a$_clO3s:O Preset,Vert, 10134 counts DIep, [ Elapsed,,)uante_

Nb

As

I

4-12 m4 16 18 I18 112 11"40.888 Ran9e- 20.468 keV

Integral 8

200 sacs200 secs

Nb

20.220 -_429024

Sg-Mar-2800 19:51:42

E;<ecutlon time • 4 second._eastucLO3=z9Vert- 8948 counts D|sp, I

_)u_nte_

feb

As

_F

4-

He

12 l-a 16 I B

R$

0.080 Range-

Rs

._A18 112

28.460 key

Integral 0

Preset- 200 secs

Elapsed, 200 sec_

rt I)

174 116A-'_r_8 '28.220 -_

441911A-72

_-Mar-_G00 20:03:56

_CUtlOn time • 4 seconds

_as_clO3s110 Preset-Vert- 10_57 counts Oisp. 1 Elapsed.0ulsnte_>

200 secs20e secs

HS

_f

4-

rtb

As

IZ 14 16 18 110 1120.000 Range- 28.460 keV

Intesrol 0

Hb

M14 T16 ',1E-20.220 -_

• 428972

39-Mar-2000 20:14:85Execution time • 5 seconds

9easwcLg3s111 Preset°Vert. 14685 counts Disp- I Elapsed-Ouantex>

Nb

_4S

(f

4-

As

Ti Hf Ga As

0.000 Range- 20.460 keyIntegral 0

Z08 secs200 secs

rtb

20.Z20 -_456064

29-Mar-2000 20:24:89Execution time • 5 second

,_eas_c103sl12 Preset-')err- 21688 counts Olsp- I Elapsed-

Nb

HT

T,_..__...---_ .

I _ 14 164- 0.8B0 Ran9e.

H_ HT

18 11028.466 keV

Z08 sec:200 secs

14b

i12 i1+ ,i_A. ,1828.Z20 -_

Integral 0 497299A-7Z

Plots 13-22. Compositional spectra across the semiconductor

/ceramic interface of a GaAs/hot pressed boron

nitride reaction couple tested at 1260°C for 24hours.

A-74

25-Mar-2000 17:28:83Execution time o 4 second

9aashpbnl Preset. 20B seesVert. 5193 counts Plsp- ! Elapsed. 288 secs

Ga

G'

As

IZ 14 16 184-

IAs

,I. .2 a_4- ,"i[ ",188.888 Range- Z8.460 keV ZO.ZZO -_

Integral 0 Z23109

Z$-Mar-Z000 17:31:29Execution time • 4 second

gaashpbnZVert- 6342 counts Disp- 1Quantex)

ot

Preset. 288 secsElapsed- 288 secs

G1As

Ga

iZ 14 iG 18 i10 IIZ "1"t44- 8.888 Range. 28.468 key

Integral 020.228 -_

25_918

25-Mar-2000 17:41:31Execution time - 4 second

gaashpbn3 Preset-Vert. 6818 counts Olsp- I Elapsed-

G&

Ga

As

Ga

A_

I 2 14 16 8 12 I 16

4- 0.888 Range- 28.468 keVIntegral 0

288 secs288 secs

l][ 828.22_ --_

261557A--7.

25-Mar~2888 17:54:03Execution time - 4 second i i

gaAshpbn4 Preset&Vert- 8552 counts Disp- 1 Elapsed.

2BO sec;280 sec;

Ca

Ga Ca

As S| _ Ga As

'"_'l_zi_'-' "16 18 _ i_ '112" _I.

4- 0.888 Range- 20.460 keVIntegral 0

116 It828.Z28 -F

134983

Z5-Mar-3888 18:Z8:38Execution time - 21 second

9aashpbnS Preset,Vert- 1B168 counts Dlsp- I ElaDsed,

Quantex)

Z00 sees288 secs

H S* Ca

J _Q_L Ga As12 14 16 18 118 112 I 14

4- 0.088 Ranse- 28.460 keYInte9ral 8

'1'16 11828.220 -F

376869

JlS-Mar-2888 18:36:29

Execution time • 4 secondgaashnbn6 Preset-

Vert- 4619 counts Disp= 1 Elapsed,Quantex)

Ca

81 Ca

FI As 5

[ _ " Integral 8

280 sec_288 secs

11820.Z2@ -F

[85881 A-76

25-Mar-2008 18:47:48E:_ecution time • 4 second

9eashDbn?Vert= 3413 counts Dispo 1

Preset. 288 =ecsElapsedl Z88 =eCS

Ca

S|

N ._

Ga As

12 14 16 18 IIB4- 8.888 Ran9e- 28.468 key

IIZ 114 1i6 118ZS.Z20 -_

Integral @ - 163367

25-Mar-2888 18:56:Z7Execution time * 4 second

_aashpbnBVert= 198 counts DisQ- I

Ca

4-

Preset- 288 secsElapsed- 288 secs

b| I

Ga

12 14 16 18 118 IIZ 114 116 1180.880 Range- E0.468 keV 20.220 -F

Integral 8 157684

_5-Mar-2888 19:21:23

Execution tlme • _ second

gaashDbnl@ Preset, 288 sec:Verto 3584 counts D|Sp= 1 Elapsed, 288 sec_Quantex)

Ca

S

5*

12 14 16 18 t184- 0.888 Ran9e- Z0.468 keV

.a ll_ 'ii6'"_le28.220 -_

Integral 8 179230A-77

25-Mar-2_e 19:28:43_xecutlon time ° 4 second

daashpbn11Vert. 3938 counts Dizp- I

guantex)

Ca

Preset-Elapsed-

288 secs288 secs

S

S! Ca

N Ga

4- '.%_'" _,o9'_. 2_.%.Jlv"112 114 l

Inte9ra| 8

li6 l I1820.220 -_

175232

A-78

APPENDIX B

CGF CARTRIDGE CANDIDATE METALS AND METAL ALLOYS

B-I

Material

Density (gm/em 3)

Hardness (Brincll)

Temperature (*C)

/R/D/UM

22.50

351

RT

Melting Point (*C) 2410

100 627 927 1227

Thermal Conductivity

(W / m-*K)

147.1 145.4 128.9 119.9 110.9

Temperature (°C)

Linear

Thermal Expansion

( 1 O- 3 cm/cm)

127

0.70

727

5.35

1327

10.68

1927

17.58

2227

21.78

1

Temperature (°C) RT

Modulus of

Elasticity

(X 10 3 MPa)

544.7

Temperature (°C) RT

Ultimate Tensile

Strength (MPa) 1999

Temperature (°C) RT

Yield Strength

NOTES: Most corrosion-resistant element known. Very brittle.

B-2

Material

Density (Ib/in 3)

Hardness (Brinell)

Temperature (_F)

/R/DRJM

0.8129

351

RT

Melting Point (_)

212 1161 1701

4370

2241 I

Thermal Conductivity

{Btu - in / h - ft 2 - *1_

1020 1008 894 831 769

'Temperature (°_ 261 1341 2421 3501 4041

Linear

Thermal Expansion

(10 -3 in (in)

0.70 5.35 10.68 17.58 21.78

Temperature (°C)

Modulus of

Elasticity (MSI)

RT

79

Temperature (°F)

Ultimate Tensile

Strength (10 3 psi)

RT

290

Temperature (*F) RT

Yield Strength

(lO3psi)

NOTES: Most corrosion-resistant element known. Very brittle.

B-3

Material

Density (gm/cm 3)

Hardness (Brinell)

T wrature

NIOBIUM

8.57

114

Melting Point (*C o) 2468

100 627 927 1227 1627 1927

Thermal Conductivity

(W / re-°K)

53.7 54.5 62.8 67.5 72.2 77.9 81.5

Temperature (*C) 127 727 1327 1927 2027

Coefficient of

Thermal Expansion

(10 -3 cm/cm)

0.78 5.61 11.02 16.87 17.88

Temperature (°C)

Modulus of

Elasticity

(X 10 3 MPa)

RT

96.5

Temperature (°C) RT

Ultimate Tensile

Strength (MPa) 645

Temperature (*C) RT [

Yield Strength

(UPa)207

NOTES: Oxidation above 230°C which causes brittleness.

B-4

Material

Density (Ib/in3)

Hardness (Brinell)

Temperature (*F)

Thermal Conductivity

_Btu- in / h- ft2 -°F_

NIOBIUM

0.3096

114

RT

372

Melting Point (°F) 4474

212

378

1160

435

1700

468

2240 2960

501 540

Temperature (*F)

Coefficient of

Thermal Expansion

{10 -3 in / in)

261

0.78

1341

5.61

2421

11.02

3501

16.87

3681

17.88

3500

565

Temperature (oF) RT

Modulus of

Elasticity (Mpsi) 14.0

Temperature (OF) RT

Ultimate Tensile

Strength (10 3 psi) 93.5

Temperature (*F)

Yield Strength

(10 3 psi)

RT

30

NOTES: Oxidation above 446°F which causes brittleness.

B-5

Material

Density (gm/cm 3)

Hardness (Brinell)

Temperature (°C)

Thermal Conductivity

(W / m-OK)

wc- 1o3 (mOSmM

8.86 Melting Point (°C) 2350

RT 815

38

954

4O

1093

42.4

1232

44.1

1304

44.6

1371

49.3

Temperature (°Q 127 727 1327 1927 2027

Linear

Thermal Expansion

(10-3 cm/cm)

Temperature (°C) RT [ 982 1093 1482

Modulus of

Elasticity

(X 10 3 MPa)

90.3 92.4 84.8 24.8

Temperature (°C) RT 538 1093 1482

Ultimate Tensile

Strength (MPa) 420 310 188 65.5

Temperature (°C) RT 538 1093 1371

Yield Strength

(MPa)

276 176 124 62

NOTES: Extensive oxidation above 230°C.

B-6

Material

Density (lb/in 3)

Hardness (Brinell)

Temperature (*F)

Thermal Conductivity

(Btu- in / h- ftz -*1_

wc- 103 (mOBn_rMALLO g)

0.3201 Melting Point (*F) 4262

RT 1500 1750 2000t

2250 2380 ] 2500

306 309 342264 277 294

Temperature (°F)

Linear

Thermal Expansion

{10 -3 in / in)

26O 1340 2420 I 3500 3680

Temperature (°F)

Modulus of

Elasticity (Mpsi)

RT 1800 2000 2700

13.1 13.4 12.3 3.6

Temperature (°F)

Ultimate Tensile

Strength (10 3 psi)

RT

61

1000

45

2000

27

2700

9.5

Temperature (OF) RT 1000 2000 2500

Yield Strength

(10 3 osi)

40 26 18 9

NOTES: Extensive oxidation above 446°F.

B-7

Material

Density (gm/cm 3)

Hardness (Brinell)

PLA T/NUA4

21.5

106

T matu

Thermal Conductivity

(W / m-OK)

RT l lool

Melting Point (°C) 1772

627 927 1227 1527

71.5 71.5 77.0 82.6 89.7 97.3

Temperature (°C) 127

Linear

Thermal Expansion

(10 -3 cm/cm)

727[ 1327 1627

0.96 6.99 14.14 18.37

Temperature (°C) RT

Modulus of

Elasticity

(x 103 MPa}

172.4

Temperature (°F) RT

Ultimate Tensile

Strength (MPa) 206.8

Temperature (°F)

Yield Strength

RT

186.2

NOTES: High oxidation resistance ; Ductile at room temperature.

B-8

Material

Density (lb/in 3)

Hardness (Brinell)

PLAT/NUM

0.7767

106

Melting Point (OF) 3222

Temperature (°F) RT 212 1160 1700 2240 2780

Thermal Conductivity

(Btu - in / h - ftz _ OF)

496 496 534 573 622 675

Temperature (*F) 260 1340 2420 2960

Linear

Thermal Expansion

10 -3 in / in)

0.96 6.99 14.14 18.37

Temperature (°F)

Modulus of

Elasticity (Mpsi)

RT

25.0

Temperature (*F)

Ultimate Tensile

Strength (10 3 psi) 30.0

Temperature (*F)

!Yield Strength

(10 3 psi)

RT

27.0

NOTES: High oxidation resistance ; Ductile at room temperature.

B-9

Material

Density (gm/cm 3)

Hardness (Brinell)

Temperature(°c)

Thermal Conductivity

(W / m-OK)

PLATINUM/2096 IRIDIUM

Melting Point (°C)

RTI I17.6

Temperature (*C) 127

Linear

Thermal Expansion

(10 -3 cm/cm)

Temperature (°C) RT

Modulus of

Elasticity

(x lo3 MPa)

Temperature (°C)

Ultimate Tensile

Strength (MPa)

RT

641.2

Temperature (°C) RT

Yield Strength

(MPa)

NOTES: Not commercially available in large quantities.

B-IO

Material

Density (lb/in 3)

Hardness (Brinell)

PLATINUM/20_ MIDIUM

Melting Point ('17 )

Temperature (_) RT

Thermal Conductivity 122

(Btu- in / h - ft 2 - °17} -

Temperature (°_

Linear

Thermal Expansion

(10 -3 in (in)

261

Temperature (*F)

Modulus of

Elasticity (Mpsi)

RT

Temperature (°F) RT

Ultimate Tensile

Strength (103 psi) 93.0

Temperature ('17 )

Yield Strength

(10 3 psi)

RT

NOTES: Not commercially available in large quantities.

B-II

Material

Density (gm/em 3)

Hardness (Brinell)

PLA T/NUM / 20_ RHOD/UM

18.7 Melting Point (°C)

Temperature (*C)

Thermal Conductivity

(W [ m-OK)

Temperature (°C) 127 l

Linear

Thermal Expansion

(10 -3 em/em)

Temperature (°C) RT

Modulus of

Elasticity

(x 10 3 MPa)

Temperature (°C)

Ultimate Tensile

Strength (MPa)

RT

482.6

Temperature (°C)

Yield Strength

(MPa)

RT

NOTES: Not commercially available in large quantities.

B-12

Material

Density (lb/in 3)

Hardness (Brinell)

Temperature ('17)

Thermal Conductivity

(Btu- in / h - ft 2 -*F)

PLATINUM� 209f, RHODIUM

0.6756 Melting Point (*F)

RT I

Temperature (°F)

Linear

Thermal Expansion

_10 -3 in / in)

261

Temperature (°F) RT

Modulus of

Elasticity (Mpsi)

Temperature (°F)

Ultimate Tensile

Strength (103 psi)

RT

70.0

Temperature (°F)_ RT

Yield Strength

_103 psi)

NOTES: Not commercially available in large quantities.

B-13

Material

Density (gm/cm 3)

Hardness (Brinell)

Temperature (°C)

Thermal Conductivity

(W / m-OK)

R/-/ENK/M

21.0

555

Melting Point (*C) 3180

100 627 927 1227 1627 2327

48.3 46.7 44.3 45.7 47.8 50.9 59.2

Temperature (°C) 127 727 1327 1927 2527

Linear

Thermal Expansion

(10-3 cm/cm)

0.67 4.60 8.96 13.86 19.41

Temperature (°C) RT 871

Modulus of

Elasticity

(x 10 3 MPa)

468.8 375.8

Temperature (°C') RT 871 1316

Ultimate Tensile

Strength (MPa) 1931 924 455

Temperature (°C) RT

Yield Strength

fUVa)1862

NOTES: Rapid oxidation over 593°C ; High melting point and brittle intermetallic formation make

welding dissimilar materials difficult ; Ductile at room temperature ; Accomodates large

thermal expansion mismatches ; Can be diffusion bonded, electron-beam welded, brazed

and soldered. B- 14

Material

Density (lb/in 3)

Hardness (Brinell)

Temperature (_)_

Thermal Conductivity

_Btu - in / h - ft z _ 017}

RHEN/UM

0.7587

555

RT I

Melting Point ('17 ) 5756

212 1161 1701 2241 2961 4221

334.9 323.8 307.1 316.9 331.4 352.9 410.5

Temperature (OF)

Linear

Thermal Expansion(10 -3 in / in)I

261

0.67

1341

4.60

2421

8.96

3501

13.86

4581

19.41

Temperature (°F) l

Modulus of

Elasticity (Mpsi)

RT

68.0

1600

54.4

Temperature (°_

Ultimate Tensile

Strength (10 3 psi)

RT

280

1600

134

2401

66

Temperature (OF)_ J RT

Yield Strength

{10a psi)270

NOTES: Rapid oxidation over 1099"F ; High melting point and brittle intermetallic formation make

welding dissimilar materials difficult ; Ductile at room temperature ; Accomodates large

thermal expansion mismatches ; Can be diffusion bonded, electron-beam welded, brazed

and soldered. B- 15

Material

Density (gm/cm 3)

Hardness (Bfinell)

Temperature (°C)

Thermal Conductivity

(W / m-OL)

RHODIUM

12.4

401

RT

150.6

100

148.8

Melting Point (*C)

627 927

123.9 114.9

1966

1127

110.9

Temperature (°C)

Linear

Thermal Expansion

(10 -3 cm/cm)

127

0.91

427

3.78

727

7.12

1327

15.26

Temperature (°C) RT

Modulus of

Elasticity

(X 10 3 MPa)

317.2

Temperature (°C) RT

Ultimate Tensile

Strength (MPa) 2068

Temperature (°C)

Yield Strength

(Ura)

RT

N_: Oxidizes slowly if heated in air.

B-16

Material

Density (lb/in 3)

Hardness (Brincll)

Temperature (°F)_

Thermal Conductivity

(Btu- in [ h- ft z - *F}

Temperature (°F)

Linear

Thermal Expansion

(10 -3 in / in)

RHODIUM

0.4480

401

RT

1044

Melting Point ('17 )

212

1032

1161

859

1701

797

3571

2061

769

261

0.91

801

3.78

1341

7.12

2421

15.26

Temperature (°F)

Modulus of

Elasticity (Mpsi) 46.0

Temperature (°F)

Ultimate Tensile

Strength (10 3 psi)

RT

3OO

Temperature (*F)

Yield Strength

(10 3 psi)

RT

NOTES: Oxidizes slowly if heated in air.

B-17

Material

Density (gm/cm 3)

Hardness (Brinell)

Temperature (*C)

Thermal Conductivity

(W / m-°K)

TANTALUM

16.6

237

RT 100

57.5 54.5

Melting Point (*C) 2996

627 927

59.9 60.9

1227

62.1

1627

63.7

1927

64.7

2727

66.5

Temperature (°C) 127 727 1327 1927 2527 2927

Linear

Thermal Expansion

(10 -3 cm/cm)

0.69 4.85 9.41 14.88 23.00 31.26

Temperature (°C) RT 871

Modulus of

Elasticity

(x 10 3 MPa)

186.2 179.3

Temperature (°C) RT 871 1316

Ultimate Tensile

Strength (MPa) 414 207 90

Temperature (°C) RT 871

Yield Strength

(UPa)331 103

NOTES: High purity Tantalum is ductile. A stable oxide film is formed below 300°C;

A protective coating is necessary for elevated temperature service in air above 982°C.

B-18

Material

Density (lb/in 3)

Hardness (Brinell)

Temperature (_

Thermal Conductivity

!fBt -m (h- t -oF}

TANTALUM

0.5997

237

Melting Point ('F)

RT 212 1161 1701

399 378 415 422

5425

2241 2961 3501 4941

431 442 449 461

Temperature (*F) 261 1341 2421 3501 4581 5301

Linear

Thermal Expansion

_10 -3 in (in)

0.69 4.85 9.41 14.88 23.00 31.26

Temperature (*F) RT 1600

Modulus of

Elasticity (Mpsi) 27.0 26.0

Temperature (*F)

Ultimate Tensile

Strength (10 3 psi)

RT

6O

1600

30

2401

13

Temperature (*F) RT 1600

Yield Strength

(103 mi_

48 15

NOTES: High purity Tantalum is ductile. A stable oxide film is formed below 572°F;

A protective coating is necessary for elevated temperature service in air above 1800°F.

B-19

Material

Density (gm/cm 3)

Hardness (Brinell)

Temperature (°C)

Thermal Conductivity

(W / m-OK)

TANTALUM/1096 TUNGSTEN

16.8 Melting Point (oc)

RT 100 1371

56.0

1527

54.0

3047

1627

52.6

1927

48.5

2427

41.5

2927

34.6

Temperature (°C) 127 427 727 1327 1927

Linear

Thermal Expansion

(10 -3 cm/cm)

0.64 2.54 4.61 9.30 14.64

Temperature (°C) RT 871 1093 1316

Modulus of

Elasticity

(x 10 3 MPa)

170.9 127.5 105.5 80.7

Temperature (°C) RT 871 1093 1316

Ultimate Tensile

Strength (MPa) 1130 676 538 398

Temperature (*C)RT 871 1316 I

Yield Strength

(MPa)1089 621 138

NOTES: Tantalum / 10% Tungsten is attacked rapidly at high temperature by oxidizing

environments. The alloy's ductility is relatively high at room temperature.

B-20

Material

Density (lb/in3) '

Hardness (Brinell)

Temperature (_')

Thermal Conductivity

(Btu- in / h-ft 2 -'F_

TANTALUM/10_ TUNGSTEN

0.6069 Melting Point (°F)

RT 212 2500

388

2781

374

5517

2961

365

3501

336

4401

288

5301

240

Temperature (OF)

_Linear

Thermal Expansion

(10 -3 in / in)

261

0.64

801

2.54

1341

4.61

2421

9.30

3501

14.64

Temperature (°F)

Modulus of

Elasticity (Mpsi)

RT

24.8

1600

18.5

2OOO

15.3

2401

11.7

Temperature (°F) RT 1600 2000 2401

Ultimate Tensile

Strength (10 3 psi) 164 98 78 57.7

Temperature (_") RT 1600 2401

Yield Strength

(10 3 psi)

158 90 20

NOTES: Tantalum / 10% Tungsten is attacked rapidly at high temperature by oxidizing

environments. The alloy's ductility is relatively high at room temperature.

B-21

Material

Density (gm/cm 3)

Hardness (Brinell)

Temperature (°C)

Thermal Conductivity

(W / m-OK)

TANTALUM / R/-//_HJM

Melting Point (°C)

RT

Temperature (°C)

Linear

Thermal Expansion

(10 -3 cm/cm)

127

Temperature (°C) RT

Modulus of

Elasticity

(x 103MPa)

ITemperature (°C)

Ultimate Tensile

Strength (MPa)

RT

Temperature (°C)

Yield Strength

(MPa}

RT

NOTES: Not commercially available.

B-22

Material

Density (lb/in 3)

Hardness (Brinell)

Temperature (_')

_Thermal Conductivity

fBtn-m f h-ft_-°_

TANTALUM/RH/_/UM

Melting Point ('17 )

RT

Temperature (*F)

Linear

Thermal Expansion

(10 -3 in / in)

261

Temperature (°F) RT

Modulus of

Elasticity (Mpsi)

Temperature (°F)

Ultimate Tensile

Strength (10 3 psi)

RT

Temperature (_F)

Yield Strength

(103psi)

RT

NOTF_: Not commercially available.

B-23

Material

Density (gin/era 3)

Hardness (Brinell)

TUNGSTEN

19.24

443

Melting Point (*C) 3410

Temperature (°C) RT 100 627 927 1227 1327 1727 2727

Thermal Conductivity

(W / m-'K)

178.3 167.2 124.1 114.9 109.0 107.0 100.0 91.4

Temperature (°C)

Linear

Thermal Expansion

10 - s cm/em)

127

0.48

427

1.88

727

3.39

1327 1927

6.61 10.20

2527

14.69

Temperature (°C)

Modulus of

Elasticity

_X 10 3 MPa)

RT

406.8

871

379.2

Temperature (°C) RT 871 1316

Ultimate Tensile

Strength (MPa) 1517 455 310

Temperature (°C)

Yield Strength

{MPa)

RT

1517

871

103

NOTES: Oxidizes rapidly above 704°C; Extremely brittle at room temperature; welding notrecommended because of brittleness.

B-24

Material

Density (1b/in 3)

Hardness (Brinell)

Temperature (_F)

Thermal Conductivity

(Btu- in / h-ft 2 -*1_

TUNGSTEN

0.6951

443

RT

1236.2

212

1159.3

Melting Point (*F)

1161 1701

860.4 796.6

6170

2241

755.7

2421

741.9

3141

693.3

4941

633.7

Temperature (°F)

Linear

Thermal Expansion

(10 -3 in / in)

261

0.48

801

1.88

1341

3.39

2421

6.61

3501

10.20

4581

14.69

Temperature (OF)

Modulus of

Elasticity (Mpsi)

RT

59

1600

55

Temperature (oF)

Ultimate Tensile

Strength (10 3 psi)

RT 1600 2401

220 66 45

Temperature (*F)

Yield Strength

{10 3 psi)

RT

220

1600

15

NOTES: Oxidizes rapidly above 1299°F; Extremely brittle at room temperature ; welding notrecommended because of brittleness.

B-25

Material

Density (gm/cm a)

Hardness (Brinell)

Temperature (°C)

Thermal Conductivity

(W / m-*K)

TUNGSTEN / 25_ RHUNIUM

19.76 Melting Point (*C)

RT 100 627

12.8 10.4

927

10.2

3121

1227

10.0

1327

10.0

1527

10.0

1704

9.9

Temperature (°C) 127 427 727 1327 1927 2427

Linear

Thermal Expansion

(10 - 3 cm/cm)

0.53 2.05 3.68 7.42 11.96 16.54

Temperature (°C)

Modulus of

Elasticity

(x 103 MPa)

RT

413.7

Temperature (°C)

Ultimate Tensile

Strength (MPa)

RT

1669

871

1020

1316

689

Temperature (°C) RT 871

Yield Strength

_MPa)

1551 965

NOTES: Oxidizes rapidly above 704°C. The addition of Rhenium improves ductility,

bendability, and strength. Room temperature ductility is retained even afterrecrystallization.

B-26

Material

Density (lb/in 3)

Hardness (Brinell)

Temperature (_F)

TUNGS_N / 25% RHENIUM

0.7139 Melting Point (OF)

RT I 212 1161 1701

5650

2241 2421 2781 3099

Thermal Conductivity

(Btu- in / h- ft 2 -*1_

88.7 72.1 70.7 69.3 69.3 69.3 68.6

Temperature (oF)

Linear

Thermal Expansion

{I0 -s in / in)

261

0.53

801

2.05

1341

3.68

2421

7.42

3501

11.96

4401

16.54

Temperature (°F)

Modulus of

Elasticity (Mpsi)

RT

60.0

Temperature (*F) RT 1600 2401

Ultimate Tensile

Strength (103 psi) 242 148 100

Temperature (OF) RT 1600

Yield Strength

(103 psi)

1551 965

NOTES: Oxidizes rapidly above 1299"F. The addition of Rhenium improves ductility,

bendability, and strength. Room temperature ductility is retained even after

recrystallization. B- 27

Material

Density (gm/em3)

Hardness (Brinell)

TZM (Alloyed Molybdenum)

10.24 Melting Point (*C) 2610

Temperature (°C)

Thermal Conductivity

(W / re-°K)

RT

140.2

200

121.8

500

115.7

700

iii.I

I000

103.2

1200

97.9

1500

88.9

2000

75.0

Temperature (°C) 100 700 1000 1200 1500 1700 2000

Linear

Thermal Expansion

(10 -3 cm/cm)

0.92 3.75 5.83 7.42 9.79 11.67 14.58

Temperature (°C) RT 871 1093 1316

Modulus of

Elasticity

(x 103 MPa)

317.2 234.4 203.4 144.8

Temperature (°C) RT 871 1316

Ultimate Tensile

Strength (MPa) 862 586 379

_Temperature (°C) RT 871 1316

Yield Strength

_MPa)

793 379 276

NOTES: Needs protection against oxidation at temperatures above 538°C.

B-28

Material

Density (lb/in 3)

Hardness (Brinell)

7ZM (Alloyed Molybdenum)

0.3699 Melting Point (OF) 4730

Temperature (*F) RT 392 932 1292 1832 2192 2732 3632

Thermal Conductivity

(Btu-in / h- ft2 -°I_

972.1 844.5 802.2 770.3 715.5 678.8 616.4 520.0

Temperature (°F) 212 1291 1832 2192 2732 3092 3632

Linear

Thermal Expansion

(10 -3 in / in)

0.92 3.75 5.83 7.42 9.79 11.67 14.58

Temperature (°F) RT 1600 1999 2401

Modulus of

Elasticity (Mpsi) 46.0 34.0 29.5 21.0

Temperature (°F) RT 1600 2401

Ultimate Tensile

Strength (10 3 psi) 125 85 55

Temperature (°F) RT 1600 2401

Yield Strength 115 55 40

(10 3 psi_

NOTES: Needs protection against oxidation at temperatures above 1000°F.

B-29

APPENDIX C

CGF CARTRIDGE CANDIDATE CERAMIC MATERIALS

C-I

Material

Density (gm/cm 3) 3.98

Maximum Operating Temperature

Temperature (°C) RT

Thermal Conductivity

/m-OK)

ALUMINUM OXIDE (Polycrystalline)

127

26.4

327[

15.8

1950"C

527 727

7.85

927

6.5510.435.9

1227

5.66

1727

6.00

Temperature (*C)

Linear

Thermal Expansion

(10 -3 cm/cm)

127

0.75

227

1.48

327

2.25

527

3.88

727

5.65

1227

10.5

1727

14.8

Temperature (°C)

Modulus of

Elasticity

(x 103 MPa)

RT 1000 2000

345 324 290

Temperature (*C)

Ultimate Tensile

!Strength {MPa)

RT

207

NOTES: Excellent chemical stability in reducing atmosphere.

Cracks very easily with small thermal gradient.

c-2

Material ALUMINUM OXIDE (Polycrystalline)

Density (lb/in 3) 0.1438

Maximum Operating Temperature 3542°F

Temperature (°F) RT 261 621

Thermal Conductivity

(Btu- in / h - ft2 _ OF)

981 1341 1701 2241 3141

248.9 183.0 109.5 72.1 54.4 45.4 39.2 41.6

Temperature (°F)

Linear

Thermal Expansion

(10-3 in / in)

261 441 621 981 1341 2241 2961

0.75 1.48 2.25 3.88 5.65 10.5 14.8

Temperature ('q_)

Modulus of

Elasticity (Mpsi)

RT

50

1832

47

3632

42

Temperature (°F)

Ultimate Tensile

Strength (103 psi)

RT

30

NOTES: Excellent chemical stability in reducing atmosphere.

Cracks very easily with small thermal gradient.

c-3

Material ALUMINUM OXIDE with SiC WHISKERS

Density (gm/cm 3)

Maximum Operating Temperature

Thermal Conductivity

(w(m-°_:)

Teml:_'atur¢ (°C)

Lin_

Thermal Expansion

{10 -s cm/em)

Temperature (*C)

Modulus of

Elasticity

(x 10 3 MPa)

Temperature (*C)

Ultimate Tensile

S_n_ _Pa?

NOTES: Material not commercially available.

C-t_

Material ALUMINUM OXIDE with SiC WHISKERS

Density (lb/in 3)

Maximum Operating Temperature

Temperature (*F)

Thermal Conductivity

(Btu - in / h - ft2 _ OF)

Temperature (_) I

Linear

Thermal Expansion

(10 -3 in / in)

Temperature (°F)

Modulus of

Elasticity (Mpsi)

Temperature (°F)

Ultimate Tensile

Strength (10 3 psi)

NOTES: Material not commercially available.

c-5

Material

Density (gIn/cm 3) 2.85

Maximum _ting Temperature

Temperature (°C)

Thermal Conductivity

(W / m-°K)

oxngn aSOPR SEZ )

2400°C

RT I 100 I 150 327

251 188 146 111 70 47

527 727 927 1227

33 21.5

Temperature (°C)

Linear

Thermal Expansion

(10 -3 cm/em)

127 327 527 727 927

0.70 2.20 3.93 5.86 7.99

1227

11.5

1627

16.8

Temperature (°C)

Modulus of

Elasticity

(x 10 3 MPa)

RT

345

Temperature (*C) RT 649 982 1093

Ultimate Tensile

Strength (MPa) 152 120 89.6 72.3

N(YI'F_,S: Excellent thermal shock resistance; excellent chemical stability in reducingatmosphere; health hazard to machine.

c-6

Material

Density (lb/in 3) 0.1030

Maximum Operating Temperature

Temperature (°F) RT

BERYLLIUM OXIDE (ISOPRF__SSED)

4352°F

212 302 621 ] 981 1341 1701 2241

Thermal Conductivity

(Btu- in / h- ft 2 - OF)

1740 1303 1012 770 485 326 229 149

Temperature (°F) 261

Linear

Thermal Expansion 0.70

(10-3 in / in)

621 981

2.20 3.93

1341

5.86

1701

7.99

2241

11.5

2961

16.8

Temperature (*F) RT

Modulus of

Elasticity (Mpsi) 50

Temperature (*F) RT 1200 1800 2000

Ultimate Tensile

Strength (103 psi) 22.0 17.4 13.0 10.5

NOTES: Excellent thermal shock resistance; excellent chemical stability in reducing

atmosphere; health hazard to machine.

c-7

Material BORON N1TRIDE (I-1P Gradc)

Density (gm/cm 3) 1.90

Maximum Operating Temperature 1200°C

Temperature (°C) RT 316 437 557 711 978

Thermal Conductivity

(W / m-°K_

31.0 27.2 26.8 26.3 26.0 25.6

Temperature (°C)

Linear

Thermal Expansion

(lo m/ m)

127 327

0.21 0.80

527

1.67

727

2.76

927

4.03

1027

4.73

Temperature (*C)

Modulus of

Elasticity

RT

46.8

Temperature (*C)

Ultimate Tensile

Strength (MPa)

RT

NOTES: In oxidizing atmospheres the performance at maximum temperatures isbetween 985°C and 1400°C. Moisture sensitive.

(;-8

Material BORON N1TRIDE (liP Grade)

Density (lb/in 3) 0.0686

Maximum Operating Temperature 2192"F

Temperature (*F) RT 601 819 1035 1312 1792

Thermal Conductivity

(Btu- in / h- ft 2 -'17)

215 188 186 182 180 177

Temperature (°F) 261 621 981 1341 1701 1881

Linear

Thermal Expansion

(10 -s in/in)

0.21 0.80 1.67 2.76 4.03 4.73

Temperature (°F) RT IModulus of

Elasticity (Mpsi) 6.79

Temperature (°F)

Ultimate Tensile

Strength (10 3 psi)

NOTES: In oxidizing atmospheres the performance at maximum temperatures isbetween 1805°F and 2552°F. Moisture sensitive.

c-9

Material

Density (gn cm )

Maximum Operating Temperature

CttROMIUM BONDED ALUMINUM OXIDE

Temperature (*C) RT I

1371"C

100 150 I 327 527 I 727 927 I 1227

Thermal Conductivity

(W / rn-*K}

9.62

Temperature (*C)

Linear

Thermal Expansion

(10 -3 cm/cm)

127 727 1327 1927 2027

Temperature (°C)

Modulus of

Elasticity

(X 10 3 MPa)

283

T_nperatu_ (*C)

Ultimate Tensile

Strength (MPa)

RT

145

NOTES: Cracks easily with small thermal gradient.

C-10

Material CHROMIUM BONDED ALUMINUM OXIDE

Density (lb/in 3)

Maximum Operating Temperature 2500°F

Temperature ('17) RT 212 302 621 981 1341 1701 2241

Thermal Conductivity

(Btu- in / h- ft 2 - OF)

67

Temperature (°F)

Linear

Thermal Expansion

(10 -3 in / in)

261 1341 2421 3501 3681

Temperature (°F)

'Modulus of

Elasticity (Mpsi)

RT

41

Temperature (oF) RT

Ultimate Tensile

Strength (103 psi) 21

NOTES: Cracks easily with small thermal gradient.

C-ll

Material QUARTZ

Density (gm/cm 3) 2.65

Maximum Operating Temperature

Temperature (°C) I 100

(Fused Silica)

1200°C

350 500 70(1 900 1200 1300

'Thermal Conductivity

(W / m-OK)

0.69 1.45 1.62 1.92 2.48 4.00 4.82

Temperature (°C) 127[ 527 727 927 1027 1127

Linear

Thermal Expansion

{10 -3 cm/cm)

0.061 0.288 0.371 0.445 0.480 0.520

Temperature (°C)

Modulus of

Elasticity

(x 10 3 MPa)

RT

71.1

500

74.5

900

76.7

Temperature (oc)

Ultimate Tensile

Strength (MPa)

RT 500 90O 1100

79.3 105 158 113

NOTES:

C-12

Material QUARTZ

Density (lb/in 3) 0.0957

Maximum Operating Temperature

Temperature (OF) 212

Thermal Conductivity

(Btu- in / h- ft 2 -OF)

4.78

(Fused Silica)

662 932

10.0 11.2

2192°F

1292

13.3

1652

17.2

2192

27.7

2372

33.4

Temperature (°F)

Linear

Thermal Expansion

(10 -3 in / in)

261 981 1341 1701 1881 2061

0.061 0.288 0.371 0.445 0.480 0.520

Temperature (°F')

Modulus of

Elasticity (Mpsi)

RT 932 1652

10.3 10.8 11.1

Temperature (°F) RT 932 1652 2012

!Ultimate Tensile

Strength (10 3 psi) 11.5 15.2 22.9 16.4

NOTES:

C-13

Material

Density (gm/cm s) 3.10

Maximum Operating Temperature

$1LIOgN CARBIDE

Tempc_ture (°C) RT ] 2OO

(Sintcrcd Alpha)

40O

1650°C

I 927 1227 I 1627 1927

Thermal Conductivity

{W / m-OK)

126 103 77.5

Temperature (°C) 127 327 527 727 927 1327 1527

Linear

Thermal Expansion

(10 -3 cm/cm)

0.41 1.26 2.19 3.21 4.31 6.68 7.95

Temperature (*C)

Modulus of

Elasticity

(x 10 3 MPa)

RT

407

Temperature (*C)

Ultimate Tensile

Strength (MPa)

RT

NOTES:

C-14

Material

Density (lb/in 3) 0.1120

Maximum Operating Temperature

SILICON CARBIDE

Temperature (°F) RT

874Thermal Conductivity

!(Btu- in / h-ft 2 -OF)

392

714

(Sintered Alpha)

30020F

752

537

1701 2241 2961 3501

Temperature (°F)

Linear

Thermal Expansion

(10 -3 in / in)

261

0.41

621

1.26

981

2.19

1341 1701

3.21 4.31

2421

6.68

2781

7.95

Temperature (oF)

Modulus of

Elasticity (Mpsi)

RT

59

Temperature (oF) RT

Ultimate Tensile

Strength (103 psi)

NOTES:

C-15

Material S1LI_N NI'I'RIDE

Density (gm/cm 3) 3.29

Maximum Operating Temperature

(Hot Pressed)

1650oC

Temperature (°C) RT 100 627 927 1204 1627 1927

Thermal Conductivity

(W / m-OK)

25.0 16.0

Temperature (°C) 127 327 527 727 927 1227 1327

Linear

Thermal Expansion

( 1O- s cm/cm_

0.14 0.64 1.24 1.91 2.63 3.76 4.15

Temperature (*C)

Modulus of

Elasticity

(x 103 MPa)

310

I

Temperature (*C)

:Ultimate Tensile

Strength (MPa)

RT

C-16

Material SILICION N1TRIDE

Density (lb/in 3) 0.1189

Maximum Operating Temperature

Temperature (°F)

(Hot Pressed)

3002_F

RT 212 1161 1701 2199 2961 3501

Thermal Conductivity

(Btu- in / h - ft2 _ OF)

173.3 110.9

Temperature (°F) 261 621 I 981 1341 ] 1701 2241 2421

Linear

Thermal Expansion

(10 -3 in / in)

0.14 0.64 1.24 1.91 2.63 3.76 4.15

Temperature (°F)

Modulus of

Elasticity (Mpsi)

RT

45

Temperature (°F) RT

Ultimate Tensile

Strength (10 3 psi)

NOTES:

C-17

Material

Density (gm/cm 3) 5.37

Maximum Operating Temperature

ZM CONIUM OXIDE

Temperature (°C) RT I 100

(Sintered ; MgO Stabilized)

250ffC

600 900 1200 1627 1927

Thermal Conductivity

_W (m-°K)

1.84 2.05 2.13 2.26

Temperature (°C) 127 327 527 727 927 1027 1127

Linear

Thermal -Expansion

(10 =3 cm/cm)

0.88 2.29 3.60 4.89 6.40 7.38 8.50

Temperature (°C)

Modulus of

Elasticity

(x 10 s MPa)

RT

179

Temperature (°C)

Ultimate Tensile

Strength (MPa) 83

NOTES: Good chemical stability in reducing atmosphere.

Cracks easily with small thermal gradient.

C-18

Material ZIRCONIUM OXIDE

Density (lb/in 3) 0.1940

Maximum Operating Temperature

Temperature (°F)

Thermal Conductivity

(Bin- in / h - ft2 _ OF)

RT 212

12.7

1112

14.2

(Sintcrcd ;

4532"F

1652

14.8

MgO Stabilized)

2192

15.7

2961 3501

Temperature (°F) 261 [ 621 981 1341 1701 1881 2061

Linear

Thermal Expansion

(10-3 in / in)

0.88 2.29 3.60 4.89 6.40 7.38 8.50

Temperature (oF) RT

Modulus of

Elasticity (Mpsi) 26

Temperature (°F)

Ultimate Tensile

Strength (10 3 psi)

RT

12

NOTES: Good chemical stability in reducing atmosphere.

Cracks easily with small thermal gradient.

C-19

APPENDIX D

CANDIDATE CARTRIDGE MATERIALS SUMMARY TABLES

D-I

SELECTED PROPERTIES OF CANDIDATE REFRACTORY METALS *

Material

NIOBIUM

WC- 103

(NIOB1UM ALLOY)

IRIDIUM

PLATINUM

PLATINUM /20% IRIDIUM

PLATINUM/RHODIUM

RHENIUM

RHODIUM

TANTALUM

TANTALUM /10% TUNGSTEN

TANTALUM /RHENIUM

TUNGSTEN

8.58

8.86

22.5

Modulus Ultimateof Tensile

Elasticity Strength

(103 MPa (MP'a)

96.5 648

90.3

545

421

1,999

Linear

Yield Thermal Tlmm_ Melting

Smmgth Expansion ** Conductivity Temp.

(MPa) (10-" crn/cm) 07¢ / m-K_ (°C)

207 0.78 @ 127°C 53.7 2,468

276

0.70 @ 12"PC

21.5 206 207 186 0.96 @ 127"C

641

18.7 483

21.0 469 1,931 1,862 0.67 @ 127"(2

316

186

20O

12.4

16.6

2,068

414

1,103

1,517

16.8

19.2

69

331

1,089

1,517407

0.91 @ 1270C

0.69 @ 127°C

0.64 @ 127'C

0.48 @ 127"C

2,350

147 2,410

71.5 1,772

17.6

48.3 3,180

151

57.5

178

1,966

2,996

3,047

3,410

TUNGSTEN / 19.8 414 1,669 1,551 0.53@ 127"C 3,12125% RHENIUId

10.2 317 862 793 0.92@ 10(/'C 140 2,610

* All values at room temperattae unless otherwise noted.

** Referenced at room temperature

D-2

SELECTED PROPERTIES OF CANDIDATE REFRACTORY MEWALS *

Mate_al

NIOBIUM

WC- 103

(NIOBIUM ALLOY)

IRIDIUM

PLATINUM

PLATINUM/20_ IRIDIUM

PLATINUM/20% RHODIUM

RHODIUM

TANTALUM

TANTALUM /10% TUNGSTI_

TANTALUM /RHENIUM

TUNGSH_

TUNGSTEN /25% RHENIUM

TZM

Density(lb/i.3)

0310

0320

0.813

Modulusof

Elasticity

(M_i)14.0

13.1

79.0

Ultimate

Tensile

Strength(lO3i_

94

61

29O

Yield

Strength(lO3_

3O

4O

0.775 29.9 30 27

93

0.676 70

LinearThermal

_amion **(10 -° in/in)

0.78 @ 261"F

0.70 @ 261"F

Thermal

Conductivity

(Btu-in/h-ft2-*F)

3723

Melting

Temp.

4,474

4,262

1019.9 4,370

0.96 @ 261W 495.7 3,222

122.0

0.760 68.0 280 270 0.67 @ 261"F 334.9 5,756

0.447 45.9 300 10 0.91 @ 261"F 1044.2 3,571

0.600 27.0 60 48

0.608 29.0 160 158

220

225

115

59.00.695

0.714

0370

220

242

0.69 @ 261"F 398.7 5,425

0.64 @ 2610F 5,517

0.48 @ 261"1:: 1236.2 6,170

0.53 @ 261"F 5,650

0.92 @ 212"F125 972.1

60.0

46.0

* All values at room temperature unless otherwise nokxt.** Refea-enced at room temperature

4,730

D-3

D°4

D°5

SELECTED PROPERTIF__ OF CANDIDATE REFRACIORY MEFALS

Material

NIOBIUM

WC- 103

_[IOBIUM ALLOY)

IRIDIUM

PLATINUM

PLATINUM /

20% IRIDIUM

PLATINUM /20% RHODIUM

RHENIUM

RHODIUM

TANTALUM

TANTALUM /10% TUNGSTEN

TANTALUM /RHENIUM

TUNGSTEN

_JNGSTEN /

25% RHENIUM

TZM

AT _ATED TEMPI_TL_

Modulusof

Elasticity@ 871"(2

UltimateTensile

Strength@ 1316°C

Yield

Strength@ 871"(2

Linear

Thermal

Expansion**@ 1327"C

Thermal

Conductivity@ 1227°C

(103 MPa)

91.0

frCa,a) f_'a) (10 -3 cm / cm)

11.02

93.1 131

10.68

44.0

111

14.14 89.7

376 455 8.96 47.7

15.26

179 89.6 103 9.41 62.2

128 400 621 9.30

379 310 103 6.61 109

689 965 7.42 9.95

234 379 379 8.20 97.5

** Referenced at room temperature

D-6

SELECTED PROPERTIF_ OF CANDIDATE REFRACTORY METALSAT FJ.EVATED TEMPERATURES

Material

NIOBIUM

WC- 103

(mOBmM At_Y)IRIDIUM

PLATINUM

PLATINUM /20% IRIDIUM

PLATINUM /20% RHODIUM

RHENIUM

RHODIUM

TANTALUM

TANTALUM /10% TUNGSTEN

TANTALUM /RHENIUM

TUNGSTEN

TUNGSTEN /25% RHENIUM

TZM

Modulus

of

Elasticity@ 160(Y'F

(Mpsi)

13.2

54.5

Ultimate

Tensile

Strength@ 2400_(10 a psi)

13.5

66

26.0 13

18.5 58

55.0

34.0

45

100

55

Yield

Strength@ 160ff'F

(Io_psi)

19

15

90

15

140

55

Linear

Thermal

Expansion **@ 2421_

(lO-3 in/m)11.02

10.68

Thermal

Conductivity@ 224trF

(Btu-in /h-ft 2 o_

501

305

769

14.14 622

8.96 331

15.26

9.41 431

9.30

6.61

7.42

756

69

6768.20

** Referenced at room temperature

D-7

SELECTED PROPERTIES OF CANDIDATE CERAMIC MATERIALSAT ELEVATED TEMPERATURES

Material

AIMMINUM OXIDE

_ OXIDEWITH SiC FIBERS

BERYLLIUM OXIDE

ISOn_SS_D_BORON NITRIDE

(H-tROMIUM BONDEDALUMINUM OXIDE

QUARTZ

_(FUSEDSn_CAISILIOON CARBIDE

Sn_n_D ALeHA)_

SILIOON NrIRIDE

_(HOTPRESSED)ZIROONIUM OXIDE

Modulusof

Elasticity@ 1093"(2

324

lOOO°C344

UltimateTensile

Sumach@ 1093_E

183

72.3

113

LLnearThermal

Expansion **@ 1327°(2

11.58

10.70

12.78

6.68

4.15

Thermal

Conductivity@ 1227°C

5.66

21.5

4.00

@ 1200°C

16.0

@ 1204°C

2.26

** Referenced at mona temperature

D-8

SELECTED PROPERTIES OF CANDIDATE CERAMIC MATERIALSAT ELEVATED TEMPERATURES

Material

ALUMINUM OXIDE

AI.£JMINUM OXIDE

WrH-I SiC FIBERS

BERYIJ.JUM OXIDE

t_SOPRESSa_)

BORON NrIRIDE

fliP GRAI_)

(_IROMIUM BONDEDAIMMINI__ OXIDE

OUAR'IZ

(_Sa_ SIUCA)

SILIO3N CARBIDE

(S_ ALeI-_)

SILICON

gR_S_)

ZIRODNIUM OXIDE

(SIN'H/RED ; M_O)

Modulus

of

Elasticity@ 2000°F

(Mpsi)

47

@ 183w

50

Ultima_Tensile

Smngth@ 2000_(103 psi)

27

10.5

16

Linear

Thermal

Expansion**@ 2420':'F

(10 -3 in/in)

11.58

10.70

12.78

6.68

4.15

Thermal

Condmtivity@ 2240"F

(Btu-in / h-ft 2-*F)

39.2

149.1

27.73

@ 2192°F

110.9

@ 220&F

15.67

@ 2192°F

** l_femnced at room temperature

D-9

APPENDIX E

LITERATURE SEARCH REFERENCES

E-I

REFERENCES

I. Aerospace Structural Metals Handbook, 1988.

2. Frank P. Incropera and David P. DeWitt, Fundamental$ of Heat and Mass

Transfer, 2nd Edition, John Wiley & Sons, New York, 1985.

3. Materials Engineering Materials Selector 1991.

4. Rockwell International Materials Properties Manual, Tantalum-10W, UNSR05255, 1987.

5. Nerva Program Materials Data Book, Refractory Metals and Alloys, 1967.

6. Charles L. Mantell, En_ineerin_ Materials Handbook, McGraw-Hill Book

Company, Inch., New York, 1958.

7. Clifford A. Hampel, Rare Metals Handbook, Reinhold Publishing Corporation,1961.

8. Brush Wellman Engineered Materials, Beryllium Oxide Brochure.

9. Ceradyne, Inc., Silicon Nitride Brochure.

10. The Carborundum Company, Combat Boron Nitride Brochure.

ii. The Carborundum Company, Hexoloy Silicon Carbide Materials Brochure.

12. The TPRC Data Series, Thermophyslcal Properties of Matter, Volume I,

Thermal Conductivity, Metallic Elements and Alloys, IFI/Plenum, New York,1970.

13. The TPRC Data Series, Thermophyslcal Properties of Matter, Volume 2,

Thermal Conductivity, Nonmetallic Solids, IFI/Plenum, New York, 1970.

14. The TPRC Data Series, Thermophysical Properties of Matter, Volume 12,

Thermal ExDanslon. Metallic Elements and Alloys, IFI/Plenum, New York,1970.

15. The TPRC Data Series, Thermophyslcal Properties of Matter, Volume 13,

Thermal Expansion, Nonmetall$c SolSd_, IFI/Plenum, New York, 1970.

16. Wah Chang Albany, WC-103 Report.

E-2

NA.g l_e p_p _co _JIIL L Wxl

IXLI i' AC_twW_,O_ _

1. rim)on No

Report Documentation Page

2. Govemmem A_ No.

4. Title end Subtitle

CGF Cartridge Development, Volume I

Dixon

7. Author(=|

Carl A.

9. Pm4mmmg_gm_d=mionNm_em_Adckeu

Southern Research Institute

2000 Ninth Avenue South

Birmingham, Alabama 35255

12. SponsoringAgency Nlme lind Addm_

National Aeronautics and Space Administration

Washington, D.C. 20546-0001

NASA Marshall Space Flight Center

3. Rec_nt'e Catet_ No.

SRI-Y_E-93-261-7244.02

6. Repon Dot,

March 1993

6. Pedorming Of_lnilltion Code

B, PerformingOrg=nizetionRepot1No.

10. Work Unit No.

11. Contract or Grant NO.

NAS8-39026

13. TYPeof Reporl and Pmiocl Covered

Final Nov 90 - Dec 92

14. Sponwdng AgencyCode

lS. Sul)l_lemenu.yNorm

16. JU_w_:t

Summary of SRI's efforts in Crystal Growth Furnace cartridge developments.

Includes evaluation of molybdenum, TZM, and WC-I03 as cartridge materials, survey

of oxidation resistant coatings, chemical compatibility studies of cadmlum-zinc-

telluride and gallium-arsenide with TZM and WC-103, survey of future cartridge

materials, and suggested improvements in ampoule design.

'17. Key Worde IS_)_md by Amlhor(=)l

CGF Ampoule Ceramics

Cartridge Molybdenum Refractory

Compatibility WC-103 Metals

Oxidation TZM

19. S_udW Ciumf. l_thMmport)Unclassified

18. Oiltrfbutlon Statement

21).Secu.r_Clemdf. l_thmpegelUnclassified

21. No. of pages 22. Price

NASA FORM 1826 OCT 86