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\.?:!:J Laboratory
Novemher, 1967
ON ATJ GRAPHITE
. . . - - - - - - - - N OT I CE - - - - - - . . . ,
This r~port ~.n Ffc-pOIled U lin OICl:uunt or work
sponsored by the Unit.. d Shllc!S Gu\'ernment. Neither
the United Stairs nor the United State) Alum" Enern
Commission. nur .IllY of their I:!mploy~e5, nur any of
thelr contracturs, 5ub(onlractors, or their .:mf1oyec5.
makes any warranty. ~"pressor implied. or assumes any
JeRal liabilit)' or responsibility for the ;-:cur3cy I com.
plctc:nt:ss cr usefulness or any information, apparatus,
product or process disclosed, or represents that its usc
would not infringe privateh-· o\\':l:~tt rights,
Prepared by:
Approved by:
INFORMATION CATEGORY
UNCLASSIFIED
Date
E. L. Lay d, Manager
Materials ngineering
and Specifications
D. E. Thomas
Engineering Manager a
Systems and Technology
tV:;\. Astronuclear
\:Y Laboratory
TARIE OF CONTENTS
I. ABSTRAc'r 1
II. INTRODUCTION 2
ACKNQ1IfLEDGEMENTS 11
REFERENCES 12
TABLES 13-14
Table I - Chemical Composition 13
Table II - Physical and Mechanical Properties 14.
FIGURES 15-19
Figure 1 - Location of Specimens 15
Figure 2 - Flexure Strength Specimen 15
b
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\::J Laboratory
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\E.J Laboratory
I. ARSTP.ACT
rrerared from these samples and various rroperties evaluated. Test res'.llts
indicated that the stabilization treatment produced significant reductions in
volAtile impurities, and in thermal expansivit~·, and slight reductions in der.5it~.',
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t::;;\ Astranuclear
'& laboratory
II. INTRODUCTION
siona] stability.
general, the aim of this investigation was to determine the effects of the heat
dimensions of pressed and graphitized ATJ graphite have been reported in WANL-
(2)
TIlE-1377. Heating to 2500 C and holding for 30 I':'.inutes caused an expansion in
the across-grain direction (parallel to the molding force) of .00105 in/in which
was retained a.fter cooling to room temperature. The effect in the with-grain
2
fW\ Jlstronuclear
\t=J Laboratory
Sample Ma teria1
control of coke particle size to 0.006 inch maximum, densit,~r of 1.70 gfec
minimum, average minimwn flexure strength of 2770 psi with-grain and 2000 r-si
Density Reported
Serial No. Diameter, Inches Height. Inch'3s by Supplier glcc
Stabilization Treatment
he~ted furnace, each furnace charge consisting of two samples and about 200
production blanks. The material was heated to 2450 0 C (4,442F) in about 6 1/2
hours, held at temperature for one hour, and cooled to room tenperature in about
30 bours, the furnace atmosphere being argon throughout the cycle. Temperatures
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fW\. AstrOnl.lclear
\E) laboratory
Chemical Composition
samples !'rom tWl) stabilized and two companion untreated sections were
~nalyzed for ir.tpurities.by spectrographic analysis, and for ash content by weight
of residue after combustion in a muffle furnace. These analyses and data taken
(I)
from \vANL-TIiE-956 for comparison are shown in Table I.
The longitudinal axes of all specimens were in the across-grain direction. Figure
2 shows the configuration of the flexure strength specimen and Figure 3, of the
electrical resistivity and flexure strength in that order. For each property,
results of individual tests tor the eight specimens representing each smople are
shmm in Table I of the Appendix. The samples are arranged in the order of in-
showing test results. Each specimen is identified by the sample number combined
with a number from 1 to 8. The average value £01' each sample derived from
individual test results and the standard deviation for each set of values are
Test Procedures
1. Density Det.eminations: Density was determined from the ratio of weight to
volume, the latter calculated from dimensions, using the flexure strength
specimens (Figure 2). vleight was measured to the nearest D.OOC)! gram, and
w<.s pas,~ed longitudinally through each spcimen and the voltage drop across
a 1 1/2 inch span was measured. The resistance for each specimen was then
method with a cross-head speed of 0.02 L,ch per minute. The loads were
applied by round steel pins 0.75 inch apart for the inner span and 2.25
required for testing, not obtainable from the sample material, was formed
temperatures between 1234 C (2256F) ana 2124 C (.3855F) 'Were measured. Dat.a
were obtained during one heating cycle and, after cooling to room temperature,
the speciJnens were reheated through another cycle. The original data. are
5
tV;\ Astronuctear
\!::::J laboratory
abscissas.
The average coefficient of thermal expansion from room temperature to
each test temperature was calculated from the corresponding per cent expansion.
flverage coefficients for the range 20 to 2100 C (6B to 3B12F) are presented
in Table II. Individual values are shown graphically in Figure 5, Imd in
tabular form in Table 3 of the Appendix.
Specimen lengths were measured at room temperature before ~nd after
the first heating cycle. Permanent length changes expressed in per cent
are shown in Table II.
5. Hydrogen Corrosion Testi~; A specimen from each sample was prepared for
corrosion testing. However, of four specimens tested, two test runs were
incomplete because furnace fixtures failed prematurely. The remaining
specimens could not be tested, since the testing facilities were used con-
tinuQusly for qu;:.lity control tests during this period.
6
,©-r'" Astronuclear
\ 'I
,c::- Laboratory
IV. DISCUSSION
of material. The analyses for specific impurities also show the same trend in
reductions for AI, B, Ra, Ca, Fe, Si, Ti, V and Zr, although the order of magni-
tude varies considerably. For l11a1:ly impurities, changes in the content could not
be detected by spectrographic analysis, since calibration does not extend to the
content present in the four samples~ and only the upper limit is reported.
A comparison of the density decreases, up to 1.72% of the untreated
srecimen weights (from Table II), with decreases in ash content, 0.052% and
0.079% (from Table I), suggests that some carbonaceous material is volati lized
during the stabilization treatment. Loss of adsorbed moisture might account for
part of the difference, but smoke reported as observed through the furnace port
holes during the stabilization treatment is evidence of volatilization.
The average values, as determined fl'om test results and tA.bulated in
Table II, indicate that density and flexure strength were reduced somewhat in
most samples. The indicated properties do not differ greatly from those found
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fW\ Astronuclear
\E.J Laboratory
(1)
in the investigation reported in WANL-TME-956. Compared to the values given
in the previous report) densities of untreated samples are ir. the upper part of
the range, flexure strengths are slightly higher and ccefficients of thermal
(:3>
eXFansion are signi.ficantly lower. A previous investigation, not formally
reported, showed that flexure strength was affected as follows, based on across-
grain specimens in each condition:
Stabilized Untreated
Average fleJOU'e strength 3819 psi 40133 psi
Highest value 4030 psi 4420 psi
~west value 3640 psi 3410 psi
These average values are within the range found in the investigation
reported herein.
It should be noted that if the value for flexure strength of specXmen
NC-1961B-3 (Tabla I of the Appendix), 3170 psi (whi~h could be considered too low
to be rfOpresentative of the sample), were deleted, the average for this untreated
sample would be 4331 psi instead of 4186. The flexure strength value for each
of the untreated samples would then be greater than for the companion stabilized
sample.
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fV;\ Astronuclear
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The average density and the average flexure strength of each sample
are represented graphically in Figure 6. It is evident that, in general, as
density increases, flexure strength also increases. The ranges of density and
flexure strength values for the individual specimens representing each sample
are also shown. The wide spread of flexure strength values is evident, but no
marked difference in the variability of stabilized and untreated material is
apparent. However, the standard deviations shown in Table II indicate that
the stabilization treatment significantly reduces the variability of flexure
strength. The standard deviations for density values given in Table II indicate
that stabilization has little effect on its uniformity. An increase in the spread
of electrical resistance and, hence of thermal conductivity, is i~dicated.
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I'V;\ Astronuclear
~ LaboraTory
V. CONCLUSIONS
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fW\ Astronuclaar
\5J l~boratory
ACKfIOWIEDGEMENTS
Developnent Department for their guidance in carrying out the investigation and
preparing this report. Credit is also due to the WANL Thennophysical Properties
II
tV:;\ l\stronuclear
\EJ Laborat6rY
REFERENCES
12
~
CHEllIC.a.L COMPOSlTXaI
bh Content.. Sp:oetrographie J.nalnie. PP" --
Sample No. Weisht Per Cent !& !! !!! § !!! 1l! !A: f! ~ £2 £!:
1. .1.4122) * .049 f490 ppIl~ 1..3 L~o LJOO 2.6 7.9 l.1 L30 98 L100 UO L 30
z. 1l4J22) .00l 910 PpIl . 2.0 8.3 • • 11>5 • • •
3. NC-196u* .012 (720 PJlIl) 2.4 12 " 150
... NC-196111 .1~1 (1510 JlPIl) ." "
52
"• 9.1 17 ·• 250 . •
" ·
,. TIlE 956(1) - l. 0.) 45 5.0 15 L 0.) L) 675 L 1 LID
6. TIlE 956(2) .1)7/.16) .02/.03 78/79 2.1/1.5 6.5/4.1 l.02/lo01 L.o;/L.Ot. )75/2l:IJ !ill': .7/.4 10/6.7
--
Spectl'OUAphie Analpio. !lIIl!
--~.§§:
~ £!£ f!- In ! Y. !!.s ~ !2 !!! ~ !!! 1: f!! !!!i
1. [100 [10 L 1ft LIOO L 10 L3 Ll L 10 [ 30 L'lD [ 10 LlfX) LIOO L 100 [)O [lOO
2. " III " " " . • •
" · " " " " " ·
). " 14 " " "
10. " ." 320 " " 1.0
;. L 0.; 10
· L 1 [ 3 l 3 L 3 l 3 [ 10
t;; 6. -" .7/.4 173/115
Z2/Ll10 "
.4/1.4 ./i/.; .7/.; DoS/L.Ot. ).0/).3 -" .3/.4
10
Z.5/L.4
-" -" - -"
SpectJ'Ogr"phic Analni•• PpIl
§! ~ 2!: ~ !!:!. !! II I !! ~ ~
1- 19 )0 L 10 LIOO l.100 21 LlOO 26 [100 [100
2. 39 10 n 23
l'J
" " " 2? " " .
3. [ 3 " 10 • '.4 32 5.0
4. 250 10
" 52
"n
52
" 5.4
" " " "
.•
5. 85 10 L 10 10 75 50 [ 10 10
6. 26/19 15/11
f:.2/L.l f:.5/L·4 [10- 220/137
-- 49/35 bt~ 23/lh 1.7/1.3
.. Stabilized
L= lA,s than
@
..... :Do
m:n
cr_
0-'
-.0
m=
_ c
on
-<iii'
m...
TABlE II
* Stabilized
** Specimens .275 x .275 x 2.500 inches
II Heated to 2500 C tor 30 minutes
@ Astronuclear
- Laboratory
""
m III
m ID m +
WITH-GRAIN
ORIENTATION
m Ii] m
CODe TEST SPECIMEN
1 HYDROGEN CORROSION TEST LOB,E PER WANL DRAWING 3670865
2 THERMAL EXPANSIVITY SPECIMEN
3 SPECIMEN FOR DETERMINATIONS OF FLEXURE STRENGTH
ELECTRICAL RESISTIVITY AND DENSITY
r- 11 r ~:~
±~~5
I~----I 0---1
FIGURE 2 Flexure ~trength
l·250
3pecimen ±.005
-r
1.500 1.500
II ±.002
I
+.002
1---i
I .
+
CEMENTED JOINT l .250 + .005 OIA.
FIGURE 3 Thermal Expansivity Srectmen
612128-18
15
~~
- l---~~-
1.2 , ------. ,- , II @
:;:.-
1. 1 I- ~!
qs ea::ll
6 STABILIZED a=
] .;}~
I»
1.0 l- J ..
t-
Z
w 0.9 I- o UNTREATED
u
cr:
...
-
Q.
I 0.8 ~
p~
Z
-
0 Jb
u; 0.7 I-
Z -
~
x
~
w 0.6 I- -
-'
t.J
~
Ill:
~4ll
w 0.5 ... -
'" ::I:
t-
0.4 [ -
0.3 -
I • I I • •
0.2
1500 2000 2500 3000 3500 4000 4500
TEMPERATURE - of
I . I I I
1000 1500 2000 2500
TEMPERATURE - °c 612138-28
FIGURE 4
Average Thermal Expansion in Per Cent from
20 C (68F) to Indicated 'femperature (across-grain)
5.5 I I I I I I
-0 1
'0
-...x
-u 4 STABILIZED 0
~
i • 0 UNTREATED CO
"- 5.0 0 0 ·
i 0
-, c
z 08 ~
Q l!tt
&It o ~Q\
z A
~ 4.5
X ·
w ~~
~
-'
0
~ cg ~i
AA
CI:
w
...x
~ u..
/lAt
A 6
0 4.0
...z 6 ·
w
U
u::
u.
w
0 I I I , I I I
u
1500 2000 2500 3000 3500 4000 4500
TEMPERATURE - of
I I I I
1000 1500 2000 2500
TEMPERATURE - °c 612138-38
@
... :100
&»CI)
a _
c .....
..... 0
F~G'lIm 5 &»::J
-c
On
AveraRe ~oefficienL of Therr.~l ~x~nsion o<Cii'
~
fro;., !'oor:, to in.Hcn.ted TenT erttt.ure (<:tcross-p,rCiin) .....
5000
@
r->
II)
c:r en
_
a ...
... 0
11)::1
_c
I- -0- -I STABILIZED } !~
RANGE OF VALUES FOR INDIVIDUAL SPECIMENS ~
I---O--~ UNTREATED
4500
~
I
~ 4000
ell:
t----
_ ..... _
1 1 ----
t;
w
. • ----t--I
a:
In ::J .4
~ .1
...a
LL.
3500
3000
1.71 1.72 1. 73 1. 74 I. 75 1.76 1.77 1.78
DENSITY - GICC 612138-4B
FIGURE 6
Density vs Flexure strength (across-grain)
5.4 r- 3.00 I I I
I I I
o UNTREATED
5.3 2.95 [ 0
-
o STABLIZED
I-
o~Z -0()
52
•
t -
0()
2.90 -
Z I '0
!!!
UX)(~ 2 -x225
· [ -
.
u: w ' - ' "51 ........ 0
u...J U LL.
o~ 0..... ,2.80 0 -
U ffi i 5.0 i L 0
!O UJ:I:
'-.
t.!) I-
_ "
• 2.75
~. z -
ffi ~ ~ 4.9 -
~~ 2. 70 ~ CO 0 -
..J
4.8 .
2.65 I- a 0 -
4.7 L I I I I I .L-
0
1. 71 1.72 J. 73 J. 74 1. 75 J. 76 1.77
AVERAGE DENSITY - Glee 612138-58
@
r-:z"
Dim
l:r=t
FTGHRE 7 00
D;=
-c=
On
Densi~y vs The~~l f.xransivity '< <1l
t»
... ...-
(~cross-~r~in) fro~ 20 to 2100 C (6B to 3q12F)
fW\ Astronuclear
\EJ Laboratory
APPENDIX
TABIE 1
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- Laboratory
TABIE 1 (continued)
TABIE 1 (concluded)
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- laboratory
TABIE 2
IB§RMAL EXPANSION MEASUREMENTS (across-grain)
A-41503* °C 1356 1581 1735 1831 1269 162.'3 1869 19.31 2121
Per Cent .537 .669 .757 .814 .523 .710 .8,31 .887 1.007
B-41503 °C 1345 1579 1725 1832 1259 1615 1863 1922 2107
Per Cent .575 .702 .785 .871 .5:36 .734 .878 .926 1.065
1..-41247* °C 1344 1566 1723 1819 1254 1609 1844 1913 211.3
Per Cent .544 .677 .765 .810 .532 .717 .845 .898 1.017
B-4l247 °C 1345 1566 1723 181.9 1254 1609 1844 1913 211.3
Per Cent .555 .686 .777 .834 .517 .703 .836 .880 1.020
NC-296lA* °C 1331 1554 1706 1805 1234 1590 1829 1889 209.3
Per Cent .537 .664 .744 .799 .5Cn .692 .816 .867 .989
NC.296lB °C 1359 1595 1739 1839 1273 1629 1872 1933 2124
Per Cent .565 ,688 .789 .826 .537 .731 .871 .932 1.068
A-41639* °C 1344 1566 1723 1819 1254 1609 1844 1913 2113
Per Cent .544 .677 .765 .810 .532 .717 .845 .898 1.017
E-41639 °C 1359 1595 1739 1839 127.3 1629 1872 1933 2120
Per Cent .556 .682 .771 .844- .546 .727 .873 .925 1.066
NC-196lA* Cie 1344 1579 1725 1832 1259 1615 1863 19'.2 2104
Per Cent .563 .719 .776 .842 .502 .697 .845 .880 .986
NC-196lB °C 1341 1559 1714 182lJ 1244 1608 1859 1913 2089
Pet' Cent .554 .693 .795 .892 S:J .709 .883 .945 1.084
}+ First hea.tin.g cycle ~ Second heating cycle
* Stabilized
23
@
-
Astronuclear
laborator~'
TABIE :3
COEFFICIENTS OF THERMAL EXPANSION (across-grain)
Average Coefficients of Thermal Expansion, 10-6 in/in./oC -
Sample 20°C to Indicated T~perature
A-4.1503* °C 1356 1,81 1735 1831 1269 1623 1869 19,31 2121
0( 4.02 4.28 4.42- 4.49 4.18 4.43 4.50 4.64 4.78
B-41503 °C 1345 1579 1725 1832 1259 1615 1863 1922 2107
0(
4.34 4.50 4.60 4.80 4.32 4.59 4.76 4.87 5.10 ' ,
A-4.J247·~ °C 1344 1566 1723 1819 1254 1609 1844 1913 211:3
c< 4.11 4.38 4.49 4.50 4.30 4.52 4.64 l~.74 4.86
B-4J247 °C 1345 1566 1723 1819 1254 1609 1844 1913 2113
ex 4.15 4.44 4.56 4.64 4.18 4.43 4.58 4.65 4.8B
NC-296LA* °C 1331 1554 1706 1805 1234 1590 1829 1889 2093
IX 4.09 4.33 4.42- 4.41 4.18 4.40 4.52 4.64 4.76
fo,lC-296lB °C 1.359 159.5 1739 1839 127.3 1629 1872 193.'3 2124
01.. 4.22 4.36 4.59 4.5S 4.28 4.56 4.70 4.87 5.00
."
A-41639* °C 1.344 1566 1123 lR19 1254 1609 IB44 1913 2113
0< 4.11 4.38 4.49 1~.50 4.30 4.52 4.64 4.74 4.86
8-41639 °C 1.359 1595 1739 1039 1273 1629 1812 1933 2120
0< 4.14 4.33 4.49 4.64 4.37 4.53 4.70 4.83 5.07
NC-196L\* °C 1344 1579 1725 1832 1259 1615 1863 1922 2104
c< 4.25 4.62 4.56 4.64 4.05 4.37 4.58 4.63 4.7'3
NC-196lB °C 1.341 1559 1714 1829 l244 ' 1608 1859 1913 2089
(;I( 4.20 4.50 4.69 4.94 4.19 4.47 4.80 4.99 5.26
~ First heating cycle f--=po- Second heating cycle
* Sta.bilized
24