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COMPATIBILITY TESTS OF MATERIALS FOR
USE IN BEARINGS, SEALS, AND VALVES IN

FUSED FLUORIDE SALTS AT 1200°F

¥.p To;

W. C. Tunnell

 

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LEGAL NOTICE

This report was prepared as an account of Government sponscred work. Neither the United States,

nor the Commission, nor any person acting on behalf of the Commission:

A. Magkes any warranty or representation, express or implied, with respect to the accuracy,
completeness, or usefulness of the information contained in this report, or that the use of
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As used in the ocbove, '‘person acting on behalf of the Commission®' includes any employee or

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or distributes, or provides access to, any information pursuant to his employment or contract

with the Commission.

 

 
 

ORNL-2103

This document consists of 74 pages.

Copy /’36 of 250 copies. Series A,

Contract No. W-7405-eng-26

AIRCRAFT REACTOR ENGINEERING DIVISION

COMPATIBILITY TESTS OF MATERIALS FOR USE IN BEARINGS, SEALS,

AND VALVES IN FUSED FLUORIDE SALTS AT 1200°F

W. C. Tunnell

DATE ISSUED

SEP 271 190a

 

OAK RIDGE NATIONAL LABORATORY
Operated by
UNION CARBIDE NUCLEAR COMPANY
A Division of Union Carbide and Carbon Corporation
Peost Office Box P
Oak Ridge, Tennessee

   
  
    

 

MARTIN MARIETTA ENERGY SYSTEMS LIBRARIES

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. Browning

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. Charpie

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ORNL-2103

C-84 — Reactors-Special Features of Aircraft Reactors

INTERNAL DISTRIBUTION

Affel

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95. A. M:Weinberg
    
  
  
   
  

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96. J.%. White 112, R. G

acPherson
97. G. B Whitman 113. W. l "Osborn

  
  
   
  
  
    
  

98. E. PRWigner (consultant} 114. W Scott

99. G. C.Williams 115. #_""‘" Smith

100. J. C. Wlson 116. .‘ K. Stair

101, C. E. Weaters 1174BE. Storto

102. E. S. Belis ] ;” W. C. Tunnell

103. R. B. Bridfs .ff" D. R. Ward

104. A, A, AbbaRello p/0. J. Zasler

105. L. P. Carperfar 121, H. Inouye

106. W. G. Cobb & 122. W. H. Cook

107. J. A, Conlin . -]24 ORNL - Y-12 Technical Library
108. G. A, Cristy p Document Reference Section
109. S. M. DeCamp 25-]34 Laboratory Records Department
110. B. L. Greenstreet J 135, Laboratory Records, ORNL R.C,
111, J. W. Kingsley ’ 136-137. Central Research Library

EXTERNAL DIZERIBUTION
P lant Represeny ive, Baltimore
flant Represeffitive, Burbank
140, AF { Repre ' ahve, Marietta
141-143, AF PRt Repre; tohve, Santa Monica
144-145. AF Pl Repr il nfcmve, Seattle
146. AF PlarfiRen entofive, Wood-Ridge
147. Air Mater(@l
148. Air ReseaNillhnd Development Command (RDGN)
149, Air Technif® Intelligence Center
150. Allison Djn
151-153. ANP Proj £t Wifice, Fort Worth
154. Albuque ; e (QRerations Office
155. Argonn /" ationq@l aboratory
156. Armed bial Weapons Project, Sandia
157. Armeg ; Forces Spe lWeapons Project, Washington
158. Assi #a Secretaryqt the Air Force, R&D
159-164. Atofllt Energy ComnW@sion, Washington
165. Ba ’f le Memorial Insflite
166-167. Bffs Plant (WAPD) W&
168. feau of Aeronautics W&
169. Jeau of Aeronautics (CE v
170.
171.4

  
   

138. A
139. AF

       
    
     
  

 

  

   
       
  
     
     
    
  
       
     
 
 

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Blrcau of Aeronautics Genflnl Representative
Thicago Operations Office ¥
17 '_,-"7: hicago Patent Group ":1;.,\
1748 Chief of Naval Research %
f Convair-General Dynamics Corf
b. Engineer Research and DevelopM@int Laboratories
; General Electric Company (ANPDY@
#4380, Hartford Area Office :
.',{;T; Headquarters, Air Force Special Weains Cenfter
‘:;’.'"i 182. ldaho Operations Office B
& 183. Knolls Atomic Power Laboratory §
% 184. Lockland Area Office

        
      
  
 

   
  
 

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185.
186.
187.
188.
189,
190.
191,
192,
193.
194,
195.
196-199,
200.
201.
202.
203.
204,
205-222.
223-247.
248,
249,
250,

   
  
  
  
 
 
  

Los Alamos Je
National Advidk
National Advisily
Naval Air Deve \@
Naval Research &

   
   
   
   
     
   

North American Aviltion, 4 % (Aerophysics Division)
¢, (Canoga Park)
Nuclear Development} ation of America
Office of the Chief of '
Patent Branch, Washig

USAF Project R o

Wright Air Devg ;pment Cenf'_
Division o ' . hhent, AEC, ORC
Richard G. J&

Technical | _search Group, New

 
 

CONTENTS

A B SIIACT oottt ettt e e e a e e s e b e bt
Materials Requirements ........ccoiiiiiiiiiiiiiiicer et ere e
Self-Welding and Friction Effects ...
T @St APPAFGIUS ooviuiiiiieieeeeieieie e et sstrasesereetebes e se e e et e s st b ettt
Selection of Materials ..o e ettt e aa et b etr e e et e rea et rnes
T @5t PrOCEAUIE oottt ettt et s e n et e b e eenen e ebe e ebaeebneente e
Criteria for Rating Materials ...t e
Evaluation of ResuUlEs ..ot

Conclusions and Recommendations .o e

Ot W W LW N et aad e

Acknowledgment ...
Appendix A. Index for Tests of Various Pin and Plate Combinations..........cccooocoo. 19
Appendix B. Material Compatibility Tests — Correlation Series ..o, 23
Appendix C. Photographic Record of Wear Patterns ..., 29

 
 
COMPATIBILITY TESTS OF MATERIALS FOR USE IN BEARINGS, SEALS, AND
VALVES IN FUSED FLUORIDES AT 1200°F

W. C. Tunnell

ABSTRACT

A series of tests were made for selecting combinations of materials compatible for possible

use in journal bearings, face seals, and valve seats operating in fused fluoride salts at 1500°F.

The test apparatus was designed to impose on the test specimen conditions similar tc those that

will be encountered in starting journal bearings and face seals from rest or in opening valves

which have been seoted for a considerable time.

These conditions are considered to be those

most likely to cause damage to the working surfaces.

Thirty=six combinations of ten different materials were tested in fused fluoride salts at 1200°F

with the use of an apparatus consisting of a pin sliding against a rotating plate under a fixed

[oad. The following combinations of materials showed sufficient promise to warrant further testing

at higher temperatures:

Kennametal 151A vs Adamas A
Adamas A vs Kennametal 138A
Kennametal 151A vs Norbide B4C

Kennametal 151A vs Carboloy 608
Kennametal 151A vs Kennametal 151A

Kennametal 151A vs High-Density Graphite

 

MATERIALS REQUIREMENTS

A basic requirement of materials used for pump
journal bearings, face-type shaft seals, and valve
seats in contact with fused fluoride salts at high
In addition
the materials must resist wear, galling, and self-
welding under severe operating conditions. There-

temperatures is corrosion resistance.

fore screening tests were developed to ascertain
the design limitations that materials might impose
on the Aircraft Reactor Test, in which a fused salt
mixture i s to be circulated at 1500°F, The selected
corrosion-resistant materials were screened for
compatibility under conditions that simulated, in
a general way, the operation of journal bearings,
face-type seals with boundary lubrication, or valve
seats under load in fused fluoride salts at 1200
to 1500°F.

It was originaily planned that the materials would
be given a preliminary screening test at 1200°F,
that those proving to be compatible would then
be further tested at 1350 and 1500°F, and that
any material proving to be compatible at 1500°F
would be tested as actual bearing pump and valve
components. However, tests at 1200°F were the
only ones performed, because the work was stopped
by higher priority projects.

SELF-WELDING AND FRICTION EFFECTS

In considering materials for high-temperature ap-
plication, it is recognized that any formed, smooth
surface has microscopic asperities. Also, it has
been reliably demonstrated that two such surfaces
in intimate sliding contact will generate sufficient
heat to cause welding and shearing of these minute
asperities as they come in contact under the ex-
treme unit pressures, or that the asperities will
shear without welding, or that they will slide “‘up
and over'’ each other and create frictional forces,
metal transfer, and/or surface damage. A similar
condition exists in a valve poppet and seat, and
it is intensified when the assembly is subjected to
a high temperature with high unit pressures at the
minute contact points; that is, a *‘weld'’ forms
through diffusion bonding of the metals. When the
valve is to be opened, the welds must be broken;
surface damage and metal transfer result,
metal

Some
combinations apparently resist diffusion
bonding, or welding, but such resistant combi-
nations can be determined only through tests. In
a study of the friction of metals the conclusion
has been that the magnitude of the frictional forces
and the extent and type of surface domage caused

by sliding are determined primarily by the relative
physical properties of the two sliding surfaces.!

In particular, the behavior is very dependent upon
the relative hardnesses of the sliding surfaces,
and, if the sliding speed is high, the relative
softening or melting points are quite important.
Properly designed, hydrodynamically lubricated
bearings operate with a thin layer of the lubricant
separating the two sliding surfaces, except in
cases of extreme loads or of starting and stopping
under load, when the thin film may be destroyed
or interrupted and metal-to-metal contact may
occur. The bearing then operates in what is called
a '‘boundary region’’ of lubrication, and an analy-
sis of the friction developed becomes complicated.
The phenomena invelved cannot be explained by
any presently known lubrication theory. Surface
finish and the chemical and physical properties
of the. sliding surfaces become critical in this
situation, and hardnesses, shear strengths, and
melting points of the materials are important.

TEST APPARATUS

The test apparatus, which was modified from
apparatus previously used for testing seals, con-
sisted of an Inconel sump tank, an Inconel operat-
ing pot, and a concentric spindle shaft and sliding
shaft arrangement inserted in the operating pot
and externally supported by ball bearings (Fig. 1).
The 2%4“' specimen plate was rotated in the
operating pot and was held against a ]/2-in.-dia
stationary pin specimen. The contact pressure
of the plate on the pin couid be adjusted by on
external spring. The surface of the plate speci-
men was lapped flat, to within three light bands,
and the end of the stationary pin specimen was
ground to a Y%-in.radius cylindrical surface so
that theoretical line contact between the speci-
mens could be obtained. The pin was mounted
so that contact would occur at a mean radius of
1 in. from the center of the plate. The mean slid-
ing speed (7.4 fps) used by Vail at KAPL? was
selected for use in these tests, At the specified
sliding speed of 7.4 fps, the plate rotated at
850 rpm.

The test apparatus was calibrated {tests Nos. 1
and 2) by use of acetylene tetrabromide (1.1-2,2
TEB) as the liquid, a Graphitar 14 plate, and an

 

1F. P. Bowden and D. Tabor, The Friction and Lubri-
cation of Solids, p 78, Clarendon Press, Oxford, 1950.

2p, B. Vail, Compatibility of Materials in Liquid
Metal, KAPL-589 (Aug. 18, 1951).

UNCLASSIFIED
DWG 22338

  

LOADING SPRING ———

DRIVE WHEEL

-BALL BEARINGS

SPINDLE SHAFT

 

 

 

 

SLIDING SHAFT

ROTATING PLATE —

Fig. 1. Bearing Materials Compatibility Tester,

[nconel pin. Contact pressure was applied in vary-
ing steps until, with a 10-lb load on the load
spring and an initial Hertz stress of about 15,000
psi, the hydrodynamic film was interrupted and a
With the
load requirement established, a series of six cor-
relation tests {tests Nos. 3 through 8, Appendix B)
were conducted in which type 416 stainless steel
plates were used in combination with six different

boundary lubricated condition existed.
pin materials: babbit, die steel, high-speed tool
steel, Stellite 6, Stellite Star J, and Superoilite.
The fluid used was regular-grade Texaco Regal
““A’ oil, without additives, which has a viscosity
of 40 to 44 SSU at 210°F. The correlation tests
were run at room temperature and were each of
2-hr duration.
agreement with the KAPL data for the same ma-
terial combinations.

A pin-wear classification guide (Fig. 2) was
prepared by taking cuts of known amounts off the
wearing nose of an unused test pin and then photo-
graphing the pin. The photographs provided a
reference to which photographs of the tested pins
could be compared to determine visually the extent
of wear,

The results were in reasonable

SELECTION OF MATERIALS

An examination of work by Vail® with sodium
and sodium-potassium alloy at temperatures up to
950°F and recommendations made by the Materials
Chemistry Section and the Ceramics Department
of ORNL were used as the basis for selecting
materials, Samples of materials that were ex-
pected to be corrosion resistant were obtained
and were exposed to the fluoride salt in static
capsule or seesaw tests? for 100 hr, The ma-
terials selected and the results of the corrosion
tests are presented in Table 1,

TEST PROCEDURE

The test specimens were cleaned with alcohol
and then slowly heated to 1200°F in a purging
stream of dry, pure helium, After the operating
pot and specimens were heated, a fluoride mixture
at 1200°F was introduced into the pot and brought
to the level-control probe. The rotation of the
submerged plate specimen was started, and the
system temperature was allowed to come to equi-
librium at 1200°F, Contact was then established
between the pin and plote specimens, with a
10-Ib contact load being applied for 120 min,
during which time the specimens remained sub-
merged in the molten fluoride salt, The load was
released, and the fluoride mixture was allowed
to drain back into the sump pot and freeze. The

 

3p. B. Vail, Compatibility of Materials in Liquid
Metal, Second Report, KAPL-1021 (Jan. 5, 1954).
4A. desS. Brasunas, A Simplified Apparatus for Making

Thermal Gradient Dynamic Corrosion Tests, ORNL CF-
52-3-123 (March 13, 1952).

system was allowed to cool to room temperature
under a helium atmosphere before the specimens
were removed for examination. Photographs were
taken of the pin and the plate after each run (see
Appendix C), and enlargements were made of the
pin-surface and plate-surface photographs to show

the wear pattern.

A Faxfilm replica was also made of each plate
and pin. The process consisted in applying a
clear solvent to the surface to be recorded, pressing
a piece of soluble plastic tope against the solvent
and surface, allowing a few seconds for reaction
and drying, and then mounting the tape in slides
for projection.

A sample of the fluoride was recovered after
each run, and a spectrographic analysis was made,
with special emphasis given to the constituents
of the compatibility specimens., There was no in-
crease of metal content, except in the case of the
oxides, which were recognized as being soluble
in the fluoride.

CRITERIA FOR RATING MATERIALS

The compatibility of pairs of materials operating
in contact with each other was established as a
relative measure of resistance to mechanical dam-
age, such as wear, galling, and self-welding. For
the purpose of classifying materials according to
test results, arbitrary group standards were estab-
lished, as follows:

Group A ~ Only slight wear on the narrow-band
pin specimen; no spalling of either specimen; no
galling or smearing tendency; no appreciable change
in surface flatness of the plate; no change in
surface finish, except an improvement (polishing
or superfinishing); no appreciable reduction in
hardness as indicated by the Rockwell hardness
tester; and no evidence of erosion or corrosion by
spectrographic or visual means.

Group B ~ Slight wear indications on either
specimen; no spalling; no smearing or metal pickup;
slight scoring and surface roughening; no appreci-
able reduction in Rockwell hardness; no evidence
of erosion or corrosion by spectrographic or visual
means.

Group C — More extensive wear than on speci-
mens of Group B; some possible roughening of
either surface or of both; some metal pickup, smear-
ing, scoring, or spalling readily apparent; no
evidence of erosion or corrosion by spectrographic
or visual means.
UNCLASSIFIED
PHOTO 18266

 

0.001-IN. CUT 0.002-IN, CUT 0.003-IN. CUT

  

0.005IN. CUT 0.010-IN. CUT

  

0.015IN. QUT 0.030-IN. CUT

Fig. 2. Pin-Wear Classification Guide. Machine cuts of various amounts on an Inconel pin specimen.
Group D -~ Excessive wear of either specimen;
metal pickup; scoring or smearing; roughening of
surfaces; reduction in hardness; deterioration of
surface finish; corrosion or erosionreadily apparent.

EVALUATION OF RESULTS

From the post-test photographs (presented in
Appendix C), a very clear indication of the com-
patibility of the test materials was obtained. Wear,
smearing, or metal buildup, galling or self-welding,
spalling, and cracking are all identifiable in the
photographs. The extent of pin wear may be ob-
served by comparison of the test photograph with
Fig. 2. The hardness readings and the spectro-
graphic analyses were effective in indicating the
compatibility of the specimens,

The test data, presented in Tables 2 and 3,
showed that, in general, pairs of unlike materials
were more compatible than pairs of like materials.
Thirty-six combinations of ten different materials
were tested, and the following were considered
suitable for further testing at higher temperature:

Kennametal 151A vs Adamas A

Adamas A vs Kennametal 138A

Kennametal 151A vs Norbide B4C
Kennametal 151A vs Carboloy 608
Kennametal 151A vs Kennametal 151A
Kennametal 151A vs High-Density Graphite

The repetition of various tests showed that the
results were reproducible and indicated that the
test apparatus and methods used were consistent
and reliable.

No single property or combination of properties,
such as surface finish, hardness, or chemical
composition, was found which was characteristic
of the best materials. It is felt that tests of ad-
ditional combinations of carbides would be produc-

tive and that tests of available borides, nitrides,
and silicides would greatly increase the chances
of finding ideal combinations of materials for the
desired applications.

CONCLUSIONS AND RECOMMENDATIONS

From the results obtained at 1200°F it is con-
cluded that several of the combinations of ma-
terials tested were sufficiently compatible under
the conditions imposed on them to warrant further
testing at 1350 to 1500°F, as was originally
planned (see ‘‘Materials Requirements'’). There-
fore the following recommendations are made:

1. Resume the compatibility screening tests
reported herein and test additional promising com-
binations of carbides, as well as combinations
of borides, nitrides, and silicides, which alsc
offer promise,

2. Run a series of tests on the screened com-
binations at 1350 and 1500°F, successively screen-
ing and retaining the most promising.

3. Test the material combinations which show
promise at 1500°F as journal bearings, face seals,
and valve seats in apparatus designed to simulate
operation in an actual reactor circuit.

ACKNOWLEDGMENT

The work of D. B, Vail of the Knolls Atomic
Power Laboratory (reports KAPL-58% and - 021)
on the compatibility of materials in sodium and
in NaK was of considerable value in the initial
selection of materials to be tested. It was also
used to check and to validate the calibration of
the apparatus used.

The data presented herein were obtained by
P. G. Smith and J. W, Kingsley of ORNL and by

W. K. Stair, consultant, the University of Tennessee,
TABLE 1. CONDITIONS AND RESULTS OF CORROSION TESTS OF SELECTED ALLOYS, CERMETS, AND CERAMICS IN FUSED FLUORIDE SALTS

 

 

Fluoride Salt Mixtures Used: 1. NuF-ZrF4-UF4 (50-46-4 mole %)
2. NoF-ZrF4-UF4 {46-50-4 mole %) ,
3. NaF-ZrF4-UF4 (53.5-40-6.5 mole %)
4. NaF-KF-LiF-UF, (10.9-43.5-44.5-1.1 mole %)
Material Typical Composition Fl-uoride Salt Type Depth of Corrosion
Manufacturer Mixture Used of Attack Comments
ldentification {wt %) a ) Reference
(see above) Test (mils)
Adamas Carbide Corp. AA 97 WC=3 Co 1 Seesaw 0 Hot zone, 1500°F; cold zone, b
1328°F
A 94 WC—6 Co 1 Seesaw 0 Hot zone, 1490°F; cold zone, b
1355°F
66 60 WC=12 Co-28 TaC 1 Seesaw 1 Hot zone, 1500°F; cold zone, b
1319°F
Borolite Corp. MoSi2 Nickel-bonded 3 Seesaw 0 c
SiC 3 Static 0 d
TiB2 3 Seesaw 2 d
ZrB2 3 Seesaw 2 d
Carboloy Dept., General 44A 94 WC=6 Co 2 Static 0 e
Electric Co.
55A 87 WC-13 Co 2 Static 0 e
608 83 CryCy~2 WC=15 Ni 2 Static Some surface roughening e
1 Seesaw 4 Attack on exposed surface /
779 91 WC~9 Co 2 Static 0 Some evidence of spalling e
907 74 WCa6 Co-20 TaC 2 Static 0 Some evidence of spalling e
X350S 98 Cr3C2—2 wC 1 Seesaw 0 Specimen extremely brittle f
The Carborundum Company BN 3 Static 2to 5 d
Mo,B 501 3 Seesaw 16 d
Electro Metallurgical Cr3C2 3 Static 0 CraC, particles did not d
Company appear well bonded in
as-received condition
5i3N4 3 Static 2tc 5 d
TiC 3 Static 0 TiC particles did not appear d

to be formed or bonded as

well as could have been
TABLE 1. (continued)

 

 

) ) . Fluoride Salt Type Depth of )
Manufacturer M?f?”al, Typical Composition Mixture Used of Attack Comments Corrosion
ldentification (wt %) a ) Reference
(see above) Test {mils)
Electro Metallurgical ZrC 3 Static Penetrated Small incipient cracks in d
Company ZrC particles throughout
specimen
Firth Sterling, Inc. FS 27 43 TiC-50 Ni-7 Cr,0, 1 Seesaw 2to5 e
Haynes Stellite Company 1 46 Co-31 Cr=13 W— 1 Static 10 €
1 Ni~3 Fe-2.45C
3 46 Co=31 Cr=13 W~ 4 Static 6 e
3 Ni-3 Fe-2.45C
2 Static 29
6 56 Co~30 Cr=5 W= 1 Static 15 e
3 Ni~3 Fe-1,25C
12 56 Co=31 Cr=8 W- 1 Static 13 e
2 Fe-1.35C
19 52 Co~31 Cr=10 W= 4 Static 2 e
3 Fe-1.8C
2 Static 29 e
21 65 Co—25 to 30 Cr-4.5 to 1 Static 5 e
6.5 Mo-=2 Fe=1.5 to
3.5 Ni-=0.2 C
25 40 Co=20 Cr—-15 W- 4 Static 0 e
10 Ni—3 Fe~1 Mo~
0.1C
] Static 5 e
40 13.5 Cr—4.5 Fe—4 Si- 1 Static 5 e
1 Co=3.2 B=Bal Ni
41 12 Cr~4.5 Fe—~4 Si- 1 Static 23 e
1 Co-2.25 B~Bal Ni
Hastelloy B 63 Ni—=28 Mo—6 Fe=1 Cr 4 Static 5 e
1 Static 5 e
Hastelloy C 55 Ni~17 Mo—16 Cr— 4 Static 2 e
6 Fe—4 W7 to 10 5i
1 Static 1 e
TABLE 1. (continued)

 

 

_ . . Fluoride Salt  Type Depth of
Manufacturer Material Typical Composition Mixture Used of Atrock Commente Corrosion
ldentification (wt %) a . Reference
(see above) Test {mils)
Haynes Stellite Company Hastelloy D 83 Ni~4 Ca=1 Fe=1 Cr 1 Static 1.5 e
Kennametal, Inc. 138A 65 TiC=20 Co= 1 Seesaw 0.5 to 1 May have been slight attack g
15 NbTiTcC3 on binder
150A 80 TiC~10 Ni-~ 1 Seesaw 4 /
10 NbTiTaC,
3 Seesaw 0 c
3 Seesaw 0 d
151A 70 TiC=20 Ni~ Seesaw 1to2 f
10 NbTiTaC3
1 Seesaw 6 Blisters on surface c
3 Seesaw 0 d
3 Seesaw 0 d
1528 64 TiC-30 Ni- 1 Seesaw 2 f
6 NbTiTaC,
1 Seesaw 4t07 Erratic attack c
3 Seesaw 0 d
3 Seesaw 0 d
153B 54 TiC—-40 Ni- 1 Seesaw 3 Uniform attack above TiC g
6 NbTiTaC3 particle surface
1618 ? TiC=? Ni=? Mo 1 Seesaw 0 Only 208°F temperature dif- g
ferential on capsule
1628 64 TiC=25 Ni—=5 Mo~ ] Seesaw 9 Portions of surface appeared f
6 NbTiTaC3 to be ploted
3 Seesaw 0 d
3 Seesaw 0 d
D4675 97.5 WC=-2.5 Co 1 Seesaw 1 Slight subsurface voids c
3 Seesaw 0 d
Metamic LT-1 77 Cr-~23 A|203 1 Seesaw Completely penetrated b
Norton Company Norbide B,C 3 Static 5 One side of specimen d

showed unidentified phase

14 mils deep
TABLE 1. (continued)

 

 

. . . Fluoride Salt  Type Depth of )
Manufactorer Mcrh.enu! Typical Composition Mixture Used of Attack Commente Corrosion
Identification (wt %) Reference
(see above) Test? (mils)
ORNL Ceramics Laboratory SiC-Si
Sintercast Corp. of America 1 50 TiC=50 Co-base 1 Seesaw 0.5 to 2 Random penetration, voids g
binder between TiC and binder
4 48 TiC-52 Co-base 1 Seesaw 1 Possible phase change g
binder within particle
5 48 TiC=52 Ni-base 1 Seesaw 0 g
binder
8 48 TiC=52 Ni-base 1 Seesaw 2 Some TiC without binder g
binder observed; not attacked
10 47 TiC=53 Ni-base 1 Seesaw 5 Some attack on binder; g
binder TiC particles separated
Vascoloy-Ramet Corp. EE 80 WC=-10 TiC=10 Co 1 Seesaw 0 Hot zone, 1500°F; cold zone, b
1346°F
EH 54 WC—40 TiC=6 Co 1 Seesaw 0 Hot zone, 1500°F; cold zone, b
1445°F
2A3 89 WC-11 Co 1 Seesaw 0 Hot zone, 1500°F; cold zone, b
1328°F (55 hr only)
2A7 95.5 WC~4.5 Co 1 Seesaw 0 Hot zone, 1500°F; cold zone, b
1355°F; spalling to a depth
of 1 to 1.5 mils
Unidentified TiN 3 Static 2 d
Copper 4 Static 0 Negligible attack i
Graphite 4 Static 0 Negligible attack i
Graph-i-tite 1 Static 2 d
3 Static 2 d

 

NOTE: See following page for references.
oL

9Static tests: specimen submerged in fluoride salt sealed in Inconel capsule for 100 hr at 1500°F. Seesaw test: tilting Inconel capsule filled with
fluoride salt; temperatures of specimen end (hot zone) and other end (cold zone), as specified; tests of 100-hr duration.

bMemorandum, D. C. Vreeland to W. D. Manly, Results of Corrosion Tests with Various Tungsten Carbide Cermets (Nov. 25, 1953).

“Data presented at conference at ORNL, May 25, 1954, by ORNL Metallurgy Division representatives.
dPersoncfl communication from W. H, Cook.

(Dec. 22, 1953).

“Memorandum, D. C. Vreeland to W. D. Manly, Summary of Corrosion Resistance of Some Hard Facing Alloys, Cermets, and Ceramics in Various Media
fMemorandum, E. E. Hoffman to W. D. Manly, Cermets Seesaw Tested in Fluoride #30 in Inconel Containers.

EMemorandum, W. H. Cock to W. D. Manly, Dynamic Testing of Some Nickel-Base Bonded and Cobalt-Base Bonded Litanium Carbide Specimens in Fluo-
ride #30 (April 20, 1954).

Memorandum, D. C. Vreeland to W. D. Manly, Results of Corrosion Tests with Metamic LT-1 Cermet (Nov. 24, 1953).
'D. C. Vreeland, E. E. Hoffman, and L. D. Dyer, Met. Quar. Prog. Rep. Oct. 31, 1952, ORNL-1437, p 25.
TABLE 2. SUMMARY OF DATA OF MATERIALS COMPATIBILITY TEST

 

 

 

I

Metal
Pin Plate Plate Surface Pickup,
Test Pin Plate Hardness* Pin Wear Hardness Finish** Spalling, Group
- e —_— . Remarks
No. Identification \dentification Before After Resistance PBefore After Before After and Classification
Test Test Test Test Test Test Galling
Resistance
] Incone! Graphitar 14 Calibration run for
load reguirement
using TEB
2 Copper Graphitar 14 One-hour operatiaon,
10-1b load, room
temperature TEB
3 Babbit Type 416 Good 18-20 18 Good Correlation test in oil,
stainless steel 2 hr at 850 rpm, room
temperature
4 Ontario die Type 416 Poor 1820 150=160 Poor Correlation test in oil,
steel stainless steel 2 hr at 850 rpm,
room tempetature
5 Stellite 6 Type 416 Poor 18-24 175-225 Poor Correlation test in oil,
stainless steel 2 hr at 850 rpm,
room temperature
6 Stellite Type 416 ' Poor 20-28 125-150 Poor Correlation test in oil,
Star J stainless steel 2 hr ot 850 rpm,
room temperature
7 High-Speed Type 416 Poor 2432 160 Poor Correlation test in oil,
tool steel stainless steel 2 hr at 850 rpm,
t;oom temperature
8 Superoilite Type 416 Goed 16--24 30--35 Fair Correlation test in oil,
stainless steel 2 hr at 850 rpm,
room temperature
9 Inconel Graphitar 14 Good Friction test, 18°F

temperature rise in

oil

*Hardness determined on Rockwell Hardness Tester. This machine was not available for use from the beginning of investigation.

**Surface finish determined by use of The Brush Development Co. Profilometer in pin. rms.
Zt

TABLE 2. (continued)

 

 

 

 

Metal
Pin Plate Plate Surface Pickup,
& .
Test Pin Plate Hardness Pin Wear Hardness Finish** Spalling, Group
No. ldentification ldentification Before After Resistance Before After Before After and Remarks Classification
Test Test Test Test Test Test Galling
Resistance
10 Inconel Graphitar 14 Good Operation for 20 hr,
10-1b load, oil,
room temperature
1 inconel Graphitar 14 Good Good First test using fuel C
No. 30, metal buildup
on pin
12 Carboloy 608 Kennametal 71 Rc 4 Excessive metal
135A buildup preventing
contact
13 Kennametal Kennametal 71 Rc Excessive metal
138A 138A buildup preventing
contact
14 Inconel Graphitar 14 Goced Good Temperature calibra- C
tion; pin 38°F
cooler than liquid
15 Carboloy 608 Kennametal 10-12 Metal buildup investi-
151A gation; Ni plate pot,
Inconel sump
16 Carboloy 608 Kennametal 70 Rc 10 Metal buildup investi-
151A gation; type 316
stainless steel pot,
Inconel sump
17 Carboloy 608 Kennametal 72 Rc 7=10 Metal buildup investi-
151A gation; Ni pot, Ni
sump
18 Carboloy 608 Kennametal 71 RC 7-10 Metal buildup investi-
151A gation; Incenel pot,

*Hardness determined on Rockwell Hardness Tester.

**Surface finish determined by use of The Brush Development Co. Profilometer in fin. rms.

incone! sump

This machine was not available for use from the beginning of investigation.
£l

TABLE 2. (continued)

 

 

 

Metal
Pin Plate Plate Surface Pickup,
Test Pin Plate Hardness* Pin Wear Hardness Finish** Spalling, Group
No. Identification Identification Befere After Resistance Before After Before After and Remarks Classification
Test Test Test Test Test Test Galling
Resistance
19 Coarboloy 608 Kennametal 65 RC Fair 70 Rc 6—=7 67 Goed Slight taper wear on C
151A pin; plate alignment
good
20 Kennametal Adamas A 72 R_  Good 79 R, 5-7 2-3 Good Corner wear on B
15TA misaligned pin;
plate wear gocd
21 Adamas A Adamas A 77 R, 78 R, Fair 78R_ 78R, 7-10 16--18 Fair Like materials ex- C
pected to wear; plate
may be warped
22 Carboloy 608 Adamas A 70 Rc Fair 79 Rc 72 Rc 5.7 7-8 Good Good pin pattern; C
plate may be
warped
23 Adamas A Kennametal 79 R. Good 73R, 66 R, 5~7 5-7 Good Good wear patterns; B
151A slight material
buildup
24 Adamas A Kennametal 79 Rc Good 73 R. 4-5 4-5 Good Good wear pattern; B
138A very slight buildup
25 Adamas A Norbide B,C 73R, Excellent 8--10 15-20 Fair Plate scored and C
excessive spalling
26 Kennametal Kennametal 5-7 Specimens reground ?
151A 138A before photos made;
data destroyed
27 ARE moder- Adamas A 72 RC 5.7 Surface Pin reacted with fuel; D
ator BeO scale no contact existed
28 Adamas A High-Density 65 Good 1012 Fair Good wear pattern; C

Graphite

some material

buildup

*Hardness determined on Rockwell Hardness Tester. This mechine was not available for use from the beginning of investigation.

**S, 1 face finish determined by use of The Brush Development Co, Profilometer in gin. rms,
r1

TABLE 2. (continued)

 

 

 

Metal
Pin Plate Plate Surface Pickup,
Test Pin Plate Hardness* Pin Wear Hardness Finish** Spalling, Group
P ipe an = — , Remarks
No. Identification |dentification Before After Resistance Before After Before After and Classification
Test Test Test Test Test Test Galling
Resistance
29 ARE moder- ARE moder. 15-18 Pin and plate reacted; D
ator BeQ ator BeO fuel plate cracked
30 Adamas A Kearfoot A|203 70 15-18 Plate reacted with D
fuel; plate cracked
31 Adamas A Graphitar 14 7 57 Good 3-5 Fair Good wear pattern;
some material
buildup
32 Carboloy 608 Carboloy 608 58 64 Fair 61 R, 72 Rc 1-2 2-3 Good
33 Carboloy 608 Norbide B,C 58 R, Fair 2-3 Poor Material buildup; D
plate misaligned;
smearing
34 Carboloy 608 Kennametal 59 R, 70R_ Fair 59 R, 1-2 Good Pin and plate wear C
138A pattern even and
concentric
35 Adamas A Norbide B4C 68 Good 2-3 Good Dry run; inert atmos- C
phere; 900°F noted
even though no heat
had been applied
36 Kennametal Norbide B4C 56 67 Good 2-3 Fair Some scoring of plate; B
151A pin wear good
37 Kennametal Carboloy 608 57 68 Good 61 1-2 Good Only slight scoring of B
151A plate; pin wear very
good
38 Kennametal Kennametal 58 66 Good 61 1-2 Good Slight scoring; may be B8
151A 151A warping of plate; pin

weaqr even

*Hardness determined on Rockwell Hardness Tester. This machine was not available for use from the beginning of investigation.

**Surface finish determined by use of The Brush Development Co. Profilometer in pgtin. rms.
TABLE 2, (continued)

 

 

 

Metal
Pin Plate Plate Surface Pickup,
Test Pin Plate Hardness* Pin Wear Hardness Finish*~ Spalling, Group
Ne. Identification Identification Before After Resistance PBefore After Before After and Remarks Classification
Test Test Test Test Test Test Galling
Resistance
39 Kennametal Graphitar 14 57 53 Fair 5=6 Fair Spalling of plate; C
151A material buildup
40 Kennametal High-Density 56 66 Good 50-60 Good Slight scoring of B
151A Graphite plate; even wear
pattern
41 Carboloy 608 Graphitor 14 50 70 Fair 5~7 Good Some smearing on C
pin; plate wear good
42 Carboloy 608 High-Density 58 68 Fair 5060 40-50 Good Slight wear on plate; C
Graphite pin pattern even
43 Norbide BAC Adamas A Fair 72 79 1-2 1-2 Good Pin misaligned; high C
stress on plate but
no wear
44 Norbide BAC Norbide B4C Fair 2-3 40 =50 Fair Pin spalled and worn; D
little plate wear;
material buildup
45 Norbide B ,C Carboloy 608 Fair 60 70 4-5 45 Good Pin spalled; mis- C
aligned plate;
wear uneven
46 Norbide B ,C Kennametal Good 59 71 1-2 1-2 Good Plate misaligned or C
151A warped; high stress;
no wear
47 Norbide B,C Kennametal Good 58 72 1-2 2-3 Good Pin and plate wear C
138A even; slight
spalling of pin
48 Kennametal Adamas A 59 58 Fair 72 71 1-2 4.5 Fair Some smearing and C
138A plate may have

warped

*Hardness determined on Rockwell Hardness Tester, This machine was not available for use from the beginning of investigation,

5l

**Surface finish determined by use of The Brush Development Co. Profilometer in pin, rms.
91

TABLE 2, (continued)

 

 

 

Metal
Plate Plate Surface Pickup,
Test Pin Plate Hardness* Pin Wear Hardness Finish** Spalling, Group
No. Identification ldentification Before After Resistance Before After Before After and Remarks Classification
Test Test Test Test Test Test Galling
Resistance
49 Kennametal Norbide B4C 60 71 Good 2--3 100150 Poor Plate scored and
138A smeared
50 Kennametal Inconel 53 65 Poor 84 RB 84 RB 4-5 200=225 Poor Pin worn excessively; D
151A plate roughened but
showed little wear
51 Adamas A Inconel 57 77 84 Rp 4=5
52 Kennametal inconel 58 66 84 RB 45
151A
53 Adamaos A Inconel 70 4-5
54 Kennametal Kennametal 61 59 2-3
138A 138A
55 (7)

 

*Hardness determined on Rockwell Hatdness Tester. This machine was not available for use from the beginning of investigation.

**S rface finish determined by use of The Brush Development Co. Profilometer in pin. rms.
TABLE 3. RESULTS OF SPECTROGRAPHIC ANALYSIS OF THE FLUORIDE AFTER VARIOUS TESTS

 

Impurities in Flucride Mixture (wt %)*

 

 

Test
No, Specimen Materials Al B Co Cr Fe Ni Si Ti W
Sump Pot No. 1
39 TiC-Ni and graphite <0.1 <0.01  <0.05 <0.05 <0.05  <0.05  <0.01 <0.05 <0.2
32 Cr,C, <0.01 T <0.05 <0.05 0.2  <0.05 0.1 £0.05 <0.02 <O0.1
45  B,C and Cr,C, <0.01 T <0.05 <0.05 0.05 <0.05  <0.05 0.2 <0.02 <0.1
46  B,C and TiC-Ni <0057 ND <005 0.1 <057 <0.05 <0.05 <0.05 <0.1
48  TiC-Co and WC 0.1 T <0.05 0.2  <0.05 0.05 0.2 <0.05 <0.1
Sump Pot No. 2
40  TiC-Ni and High-  <0.1 <0.01 <0.1 <0.1T 0.1 <0.5T  0.02 <0.01 <0.2
Density Grophite
41 Cr,C,and graphite  <0.1 <0.001 <0.1 <0.1  <0.05T <0.05  <0.01 <0.01 <0.2
42 CroCr and High- <0.1T <0.05  <0.05 0.1 0.5 <0.05 0.05 <0.02 <0.1
Density Graphite
44 B,C 0.01, <0.05P <0.05 0.2, 0.2,  <0.05 T <0.05 <0.02 <0.1
<0.01 <0.05  <0.05
47 B,Cand TiC-Co 0.05 ND  <0.05 0.2  <0.05 <0.05 <0.05 <0.05 <0.1
49  TiC-Coand B,C 0.05 ND <005 0.2  <0.05 <005  <0.05 <0.05 <0.1
50  TiC-Ni and Inconel 0.1 ND  <0.05 0.2 0.05  <0.05  <0.05 <0.05 <0.1
0.2
51 WC and Inconel <0.05 ND  <0.05 0.2  <0.05  <0.05 <0.02 <0.1

 

*T indicates a trace detected; P indicates element present; ND indicates not detected.

17
APPENDIX A

INDEX FOR TESTS OF VARIOUS PIN AND PLATE COMBINATIONS

19
Ic

INDEX FOR TESTS OF VARIOUS PIN AND PLATE COMBINATIONS

Key: For test number for pin material, read across
For test number for plate material, read down

 

wC

Plate Material and Vendor |dentification

 

P Vend CryC, TiC + Co TiC + Ni B,C Graohit High- BeO Al,0,4
Mat I:_ i Identiefr;c::ion Adamas Carboloy Kennametal Kennametal Norton rq;])4| ar Density Inconel ARE Kearfoot
arertd Grade A 608 138A 151A Norbide Graphite Moderator*  Alumina*
wC Adamas Test 21 Test 24 Test 23 Tests 25, Test 31 Test 28 Tests 51, 30
Grade A 35 53
CryC, Carboloy 608 Test 22  Test32  Test 34 Tests 16, Test 33 Test 4] Test 42
17, 18, 19
TiC + Co Kennametal Test 48 Test 49 55
138A
TiC + Ni  Kennametal Test 20 Test 37 Test 26**  Test 38 Test 36 Test 39 Test 40 Tests 50,
151A 52
B,C Norton Norbide Test 43 Test 45 Test 47 Test 46 Test 44
BeO* ARE Moderator 27 29
Inconel Tests 11,**

14*+

 

*Material eliminated because of lack of corrosion resistance,

**Photographs not included.
APPENDIX B

MATERIAL COMPATIBILITY TESTS - CORRELATION 5SERIES

Tested in Texaco Regal **A'’ oil at room temperature, under 10-1b load, at 850 rpm for 2 hr.

23
UNCLASSIFIED
PHOTO 18270

 

 

Test No. 3. Pin: Copper, Hard Drawn
Plate: Type 416 Stainless Steel, Ground Finish

UNCLASSIFIED
PHOTO 18271

 

Test No. 4. Pin: Ontario Die Steel, As-Received
Plate: Type 416 Stainless Steel, Ground Finish

25
26

Test No. 5.

UNCLASSIFIED
PHOTO 18273

Test No. 6.

 

Pin: Stellite 6
Plate: Type 416 Stainless Steel, Ground Surface

 

Pin: Stellite Star J
Plate: Type 416 Stainless Steel, Ground Surface
UNCLASSIFIED
PHOTO 18274

 

Test No. 7. Pin: High-Speed Tool Steel (Type 6-6-2)
Plate: Type 416 Stainless Steel, Ground Surfoce

UNCLASSIFIED}
PHOTO 18275

 

Test No. 8. Pin: Supercilite
Plate: Type 416 Stainless Steel, Ground Surface

27
APPENDIX C

PHOTOGRAPHIC RECORD OF WEAR PATTERNS

29
Test No. 16. Pin: Carboloy 608, Cr,C
Plate: Kennametal 151A, TiC + Ni
Pot: Type 316 Stainless Steel
Sump: Inconel
Note Material Buildup on Pin

UNCLASSIFIED
PHOTO 18276

 

31
32

Test No. 17. Pin: Carboloy 608, Cr,C,
Plate: Kennametal 151A, TiC + Ni
Pot and Sump: Nickel
Note Material Buildup on Pin

UNCLASSIFIED
PHOTO 18277

 
Test No. 18, Pin: Carboloy 608, Cr,C
Plate: Kennametal 151A, TiC + Ni
Pot and Sump: Inconel
Note Small Amount of Material Buildup on Pin

UNCLASSIFIED
PHOTO 18278

 

33
 

34

Test No. 19. Pin: Carboloy 608, Cr,C,
Plate: Kennametal 151A, TiC + Ni

UNCLASSIFIED
PHOTO 18279
Test No. 20. Pin: Kennametal 151A, TiC + Ni
Plate: Adamas Grade A, WC

UNMCLASSIFIED
FHOTO 18280

 

35
UNCLASSIFIED
PHOTO 18281

 

Test No. 21. Pin: Adomas Grade A, WC
Plate: Adamas Grade A, WC

 

 
Test No, 22, Pin: Carboloy 608, Cr,C
Plate: Adamas Grade A,

 

 

Ye

UNCLASSIFIED
PHOTO 18282

37
UNCLASSIFIED
PHOTO 18283

 

Test No. 23. Pin: Adamas Grade A, WC
Plate: Kennametal 151A, TiC + Ni

38
   

 

UNCLASSIFIED
PHOTO 18284

 

 

Test No. 24, Pin: Adamas Grade A, WC
Plate: Kennametal 138A, TiC + Co

39
UNCLASSIFIED
PHOTO 18285

 

Test No. 25. Pin: Adamas Grade A, WC
Plate: Norton Norbide, B4C

40
Test No. 27. ' Pin: ARE Moderator BeO
Plate: Adamas Grade A, WC

UNCLASSIFIED
PHOTO 1B285&

 

4]
42

Test No. 28, Pin: Adamas Grade A, WC
Plate: High-Density Graphite

UNCLASSIFIED
PHOTO 18287

 
UNCLASSIFIED
PHOTO 18288

 

Test No. 29. Pin: ARE Moderator BeO
Plate: ARE Moderator BeO
UNCLASSIFIED
PHOTO 18289

 

Test No, 30. Pin: Adamas Grade A, WC
Plate: Kearfoot Alumina, Alzfla
UNCL ASSIFIED
PHOTO 18290

 

Adamas Grade A, WC
Plate: Graphitar 14

Pin

Test No. 31.

45
UNCLASSIFIED
- PHOTO 18291

T ———
s LD

 

Test No, 32, Pin: Carboloy 608, Cr,C,
Plate: Carboloy 608, Cr,C,
 

 

Test No, 33, Pin: Carboloy 608, Cr,C,
Plate: Norton Norbide, B‘C

 

UNCLASSIFIED
PHOTO 18292
fi;

47
48

Test No. 34, Pin: Carboloy 608, Cr,C,
P late: Kennametal 138A, TiC + Co

UNCLASSIFIED
PHOTO 18293

 
 

Test No. 35. Pin: Adamas Grade A, WC
Plate: Norton Norbide, B,C

UNCLASSIFIED
PHOTO 18294

49
UMCLASSIFIED
PHOTO 18295

Ty

 

Test No, 36. Pin: Kennametal 151A, TiC + Ni
Plate: Norton Norbide, B,C
Test No. 37.

 

Pin: Kennametal 151A, TiC + Ni
Plate: Carboloy 608, Cr,C,

UNCLASSIFIED
FHOTO 18294

51
UNCLASSIFIED
FPHOTO 18297

 

Test No. 38. Pin: Kennametal 151A, TiC + Ni
Plate: Kennametal 151A, TiC + Ni

52
 

Test No. 39. Pin: Kennametal 151A, TiC + Ni
Plate: Graphitar 14

UNCLASSIFIED
PHOTO 18298

33
54

-

§
i

Test No. 40. Pin: Kennametal 151A, TiC + Ni
Plate: High-Density Graphite

UNCLASSIFIED
PHOTO 18299

 
Test No. 41, Pin: Carboloy 608, Cr 3C
Plate: Graphitar 14

UNCLASSIFIED
PHOTO 18300

 

55
UNCLASSIFIED
PHOTO 18301

 

High-Density Graphite

Test No, 42, Pin: Carboloy 608, Cr3C2
Plate
 

Test No. 43, Pin: Norton Norbide, B ,C
Plate: Adamas Grade A, WC

UNCLASSIFIED
PHOTO 18302

|

57
58

 

 

Test No. 44, Pin: Norton Norbide, B,C
Plate: Norton Norbide, B4C

UNCLASSIFIED
PHOTO 18303

5
Test No. 45.

Pin: Norton Norbide, B,C
Plate: Carboloy 608, Cr,C,

UNCLASSIFIED
FPHOTO 18304
e

'
R}

 

59
60

Test No. 46.

Pin: Norton Norbide, B4C
Plate: Kennametal 151A, TiC 4 Ni

UNCLASSIFIED
PHOTO 18305

 
UNCLASSIFIED
PHOTO 18306

 

LA

Test No. 47. Pin: Norton Norbide, B ,C
Plate: Kennametal 138A, TiC + Co

61
62

Test No. 48. Pin: Kennametal 138A, TiC + Co
Plate: Adamas Grade A, WC

UNCLASSIFIED
PHOTO 18307

 
 

Test No. 49, Pin: Kennametal 138A, TiC + Co
Plate: Norton Norbide, B, C

UNCLASSIFIED
PHOTO 18308

63
64

Test No. 50, Pin: Kennametal 151A, TiC + Ni

Plate: Inconel

UNCLASSIFIED
PHOTO 18309

 
 

Test No. 51. Pin: Adamas Grade A, WC

Plate: Inconel

UNCLASSIFIED
PHOTO 18310

63
 

66

Test No. 52. Pin: Kennametal 151A, TiC + Ni

Plate: Inconel

UNCLASSIFIED
PHOTO 18311
UNCL ASSIFIED
PHOTO 18312

 

Test No. 53, Pin: Adamas Grade A, WC

Plate: Inconel

67
 

68

Test No. 55. Pin: Kennametal 138A, TiC + Co
Plate: Inconel

UNCLASSIFIED
FHOTO 18313

3