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MICROCOPY RESOLUTION TEST CHART
NATIONAL QURE AU OF STANDARDS -1963
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1.
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ORNU P'_ 3,00
Cort- 670905.-20
JUN 2 2 1969
CESTI PRICES
20. 12.00 un 65
H.C.
FORMATI. ON AND CHARACTERIZATION OF AN A15-TYPE STRUCTURE
IN CHEMICAL VAPOR DEPOSITED TUNGSTEN-RHENIUM ALLOYS2
•
J. I. Federer and J. E. Spruiel12
Metals and Ceramics Division
Oak Ridge National Laboratory
Oak Ridge, Tennessee
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LEGAL NOTICE
This report we prepared as an account of Gororadioat sponsored work. Neither the United
Stato, por the Commission, nor any person acting a bohalt of the Commission:
A, Maken any warranty or representation, expressed or implied, with respect to the accu.
racy, completeness, or unofulness of the Information contained in this ruport, or that the use
of may lalormation, apparatus, method, or proceso decloud lo this roport may not infringo
primtaly owned rights; or
B. Assumes any liabilties with respect to the uko of, or for damage romuitas from the
' un of any information, apparatus, method, or procedo diaolond ta two report.
As und in the above, "porono scttag on behall of the Commission" Includes any on-
ployw or contractor of the Commission, or omployho of such contractor, to the extent that
such employee or contractor of the Commission, or employee of much contractor preparo,
denominatas, or provides accouto, any Information purwant to his employment or contract
with the Commission, or his employment with such contractor.
21 pages
5 tables
5 figures
Y
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DISTRIBUTION OE THIS DOCUMENT IS ORCIMITED
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SAVOLETT
UNITATEAU
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A
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A15 PHASE IN TUNGSTEN-RHENIUM ALLOYS
J. I. Federer
Metals and Ceramics Division
Post Office Box X
Oak Ridge National Laboratory
Oak Ridge, Tennessee 37830
.
r
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3
AESTRACT
An A15-type phase in vapor-deposited tungsten-rhenium alloys was
identified by X-ray diffraction, metallography, and hardness measurements.
The composition range of this A15-type phase varied with temperatura, but
was near to W3Re; in the temperature range investigated, 1000 to 1500°C,
the phase occurred alone or coexisted with the tungsten-rich terminal solid
solution (B) or with sigma phase (o). The phase was about four times as
hard as ß, limiting the usefulness of alloys containing the phase as a
major constituent. Transformation to B or to B + o phases during long time
ánneals at deposition temperatures showed that the phase was metasteble.
Based upon a proposed reason for formation during deposition, the phase
would not be expected to form in B or B + o phase alloys subjected to
service at elevated temperatures.
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I.
INTRODUCTION
Chemical vapor deposition of tungsten-rhenium alloys is being investi-
gated as a fabrication method to supplement present metalworking techniques.
Potential applications include the deposition of material in suitable form
for subsequent mechanical working (extrusion, drawing, rolling, etc.),
coatings for diffusion and corrosion barriers, and complex shapes that are
difficult to fabricate by other methods. Early in this investigation a
previously unreported cubic phase was found in tungsten-rich as-deposited
alloys occurring alone or coexisting with the tungsten-rich terminal solid
solution. Later, the new phase was identified as an A15-type phase; that
is, having the same type crystal structure as W30 (refs. 1 and 2). .
The lattice parameter of the new phase is approximately the same as
for W30, which has an oxygen content of about 3 wt %. Analyses showed,
however, that tungsten-rhenium deposits typically contained a total inter- ..
stitial (0,8,0,) content of about 30 ppra; about 10 ppm F, and traces of
several metals. Thus, the A15 phase found in this study could not be W30.
Literature references to phases having the same crystal structure as
W30 use the terms A15-type structure, ß tungsten-type structure, and Cr30-
type structure (3,4). Since the tungsten-rich terminal solid solution is
labelled B on presently accepted tungsten-rhenium phase diagrams, the
term A15 is used for the new phase found in this study. This type of
structure occurs frequently In binary systems involving transition elements.
At least 39 such phases were known in 1958 (ref. 4). The nominal composi-
tion for A15 phases 18 A3B. In some binary systems the phases have a
narrow composition range around the stoichiometric compositions (5).
..
Tungsten-rhenium alloys containing primarily the A15 phase were sub-
stantially more brittle than the solid solution at room temperature as
evidenced by the relative' ease of crushing the two types of deposits to
powder for x-ray diffraction studies. Mechanical properties might also
be affected at higher temperatures. For these reasons optimum use of
vapor-ceposited alloys requires characterization of the A15 phase. A
study was initiated, therefore, of the practical aspects of the phase
including hardness, temperature and composition limits for formation during
deposition, and stability and transtormation products during annealing and
aging treatments. In addition, x-ray studies confirmed the crystal
structure type.
II. EXPERIMENTAL PROCEDURE
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:
Alloys were deposited at temperatures in the range of 1000 to 1500°C
in a search for the highest temperature at which the A15 phase forms.
The deposition pressure .was 5 torrs, the volumetric H2-to-(WF6+ReF6) ratio
was 15, the volumetric WF6-to-ReFr ratio was varied from 0.7 to 10 in order
to obtain different alloys, and the deposition time for each alloy was
2 hr. The deposition apparatus is shown schematically in Fig. 1. The
deposits formed on the outside of 0.32.5-in.-OD by 3-in.-long alumina
mandrels heated by contact with resistance-heated 1/8-in.-diam carbon rods.
No reaction occurred between the deposits and alumina mandrels, and the
deposits could be mechanical.ly removed without difficulty. The deposition
temperatures were measured by an optical pyrometer calibrated for the
experimental conditions. Although the deposits coated the entire 3-in.-
long mandrel, only the center 1-in.-long section for which the temperatures
were observed during deposition was used for evaluation. A Dehye-Scherrer
X-ray pattern was prepared from each deposit for the purpose of phase
identification, and a portion of the same powder was analyzed gravi-
metrically for rhenium content.
III. COMPOSITION AND TEMPERATURE RANGE
OF FORMATION OF THE A15 PHASE
The phases found in as-deposited alloys are listed in Table I. These
data show that the deposits usually consisted of either the tungsten-rich
terminal solid solution (b), the A15 phase, or a mixture of the two phases.
Sigma phase (o) occurred in some deposits of high chenium content, and
occurred along with the A15 and 8 phases in two deposits at 1500°C.
Three sol·ld phases can coexist in a binary system only at a eutectoid or
peritectoid temperature or under conditions of nonequilibrim.
Phases present in various as-deposited alloys are also shown in
relation to a portion of the tungsten-rhenlum phase diagram in Fig. 2.
Phase boundaries involving the as-deposited phases are shown as broken .
lines in the 200O to 1500°C region, while previously established equili. .
brium phase boundaries are shown as solid lines. Figure 2 shows that the
homogeneity range of the A15 phase is relatively wide and is not centered
about the nominal composition A3B. Vapor-deposited alloys containing
26% Re, the approximate optimim composition for ductility in wrought alloys,
contain amounts of the A15 phase dependent upon deposition temperature.
The phase was previously found to be dominant in alloys containing 15 and
26% Re and was the only phase in an alloy containing 37% Re, all deposited
at 600°C (refs. 1 and 2).
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The A15 phase has not been found in alloys prepared by the usual
powder metallurgy and arc-casting techniques and is not show on the
presently accepted phase diagram (6). The first reason proposed to explain
the absence of the phase in these alloys was that low diffusion rates
below 1500°C caused the transformation to equilibrium products to be slow.
Thus, 1f the A15 phase were an equilibrium phase, the usual alloy prepara-
tion techniques ordinarily would not allow sufficient time for formation.
An alternate explanation is that the A15 phase is a nonequilibrium phase
that can be formed only by vapor deposition or similar technique. Annealing
treatments, which will now be described, showed conclusively that the A15
phase is a nonequilibrium phase.
IV. STABILITY OF THE A15 PHASE
The temperature stability of the as-deposited structures was deter-
mined by annealing alloys containing from 14.8 to 57.2% Re at temperatures
.
powder patterns. The results of these anneals are shown in Table II. At
all temperatures investigated above 1300°C the A15 phase transformed to B
or B +0. In alloys annealed at 1300°C for 700 hr. the amount of A15 phase
was always less than in the as-deposited condition. This is shown by the
change in intensity ratios of the (211) A15 reflection to the (200) B .
reflection presented in Table III. In addition, lines corresponding to
o phase appeared in the x-ray patterns of some of the alloys following the
annealing treatment at 1300°C (Table II). The results of these annealing
studies show that the A15 phase is metastable and decomposes into products
consistent with an extrapolation of the presently accepted equilibrium
phase boundaries to 1300°C.

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V. MICROSTRUCTURES AND HARDNESS
.
The microstructure of a1oy deposits varied with kind and amount of
phases present. The single-phase ß deposit shown in Fig. 3& nas a fine-
grained structure in the first deposition region and coarse columnar grains
similar to those of unalloyed tungsten deposits. The two phases, B and
A15, are clearly distinguished in Fig. 3b. The matrix or continuous phase
in this structure is the B phase as shown by the larger hardness indenta-
tion. The hardness of the A15 phase is much greater than that of other
VA
phases encountered in both as-deposited and annealed alloys. Although
..
:
not clearly shown in Fig. 3b because the B phase is under-etched, the
overall grain structure of the deposits containing both the B. and A15
phases was similar to the all B phase deposits. Because of this similarity
and the nature of the interaction of the two phases with the etchant,
differentiation between the B and A15 phases was difficult when the samples ·
were heavily etched.
Figure 3c shows the microstructure of a deposit consisting primarily
of the A15 phase. The minor constituent, B phase, was confined to the
small slightly darker areas and a thin layer on the last deposited surface
(top) of the deposit.
In addition to the transformation previously discussed, recrystalliza-
tion and/or grain growth occurred during annealing. Figure 4 shows typi-
cal microstructures of alloys annealed at 1500°C for 1000 hr. The grains
of the single-phase B alloy shown in Fig. 4a are still elongated in the
growth direction but are much larger than in the as-deposited condition
(Fig. 3a). The microstructure of Fig. 4b shows the transformation products
of the A15 phase, namely o în a B matrix.
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The diamond pyramid hardnesses of alloys deposited at 1100°C and
annealed at 1500°C are compared in Table IV. These data show that the
hardness of the B phase increases gradually with increasing rhenium con-
tent, and the hardness of the alloy increases abruptly when the A15 phase
becomes the major constituent. Annealing at 1500°C resulted in a large
decrease in hardness, even in alloys having o as the major phase.
VI. LATTICE PARAMETER AND CRYSTAL STRUCTURE TYPE
Debye-Scherrer patterns from the new phase found in this investigation
..could be indexed assuming a cubic unit cell. Lattice parameters of this
.
cubic cell were calculated by use of a computer program involving a Nelson-
Riley extrapolation. Values ranged between 4.9817 1 0.0005 A and
5,0196 $ 0.003 A depending upon the rhenium content of the alloy as shown
in Fig. 5. The structure was identified as an A15-type by comparison of
calculated and experimental x-ray intensities. The typical cubic A15-type
structure has eight atoms in the unit cell with A atoms in the positions
2,0,; 3:2,0; 0,32 2,0,2; 3; 3,0; 0,32 and B atoms in the positions
0,0,0 and zzz (ref. 4). X-ray diffraction can be used to establish if
the eight atoms in the unit cell occupy the eight sites listeá above but
cannot distinguish between an ordered and a disordered arrangement of the
atoms. This is true because the x-ray atomic scattering factors of tungsten
and rhenium are nearly identical, and, therefore, the x-ray intensities
computed for the ordered and random arrangements are essentially the same.
X-ray intensities were calculated from the expression
I = cp 1 +.cos? 20 72
"Feli
sina cos e hk.
T.33
.
:
:
·
where
I = Integrated intensity of an hkl reflection,
c = proportionality constant,
p = multiplicity,
1 + cos28 :: Lorentz-pclarization factor
sina e cos o
F, = structure factor for the hkl reflection.
hki
Experimental integrated intensities were determined for an alloy containing
34% Re by standard techniques using a Norelco diffractometer, NaI scintil-
iation counter, and a 20 scan rate of 1/4 degree/min. Observed intensities
are compared with the calculated values for the A15 structure (both nor-
malized to the strongest, 210, reflection) in Table V. The close agree-
ment between calculated and experimental intensities confirms that the
.
atomic coordinates in the unit cell are actually those for the A15
structure.
.
Neutror. diffraction can be used to determine order in the unit celi
because the neutron scattering factor of rhenium is about double that of
tungsten, but this experiment has not yet been performed.
VII. DISCUSSION
· Nevitt (4) examined atomic size effects in about 30 A15-type structures
and found that a necessary, but not sufficient, condition for occurrence
of the structure is that the Goldschmidt coordination No. 12 radii of the
component elements do not differ by more than about 15%. The Goldschmidt
radii for tungsten and rhenium differ by only about 3% (?). Nevitt also
found a linear relationship between lattice parameters of A15-type
2.1
structures and Goldschmidt coordination No. 12 radii for the A atoms":
(assuming a nominal composition A3B). Using 1.41 A as the Goldschmidt
radius for tungsten, the lattice parameter of the tungsten-rhenium A15
phase determined from Nevitt's correlation is about 5.03 A. Experimentally
determined lattice parameters for the tungsten-rhenium A15 phase range
between 4.9817 and 5.0196 A. Thus, a necessary condition for occurrence
of the A15 phase is fulfilled in the tungsten-rhenium system and the
lattice parameter of the phase is consistent with values determined for
a large number of A15-type phases.
An Interesting question arising from this investigation is why the
metastable A15 phase, instead of the equilibrium phases forms during
deposition. Although a completely satisfactory explanation cannot be
given now, some basic considerations help to understand this phenomenon.
When two phases are in equilibrium at a constant temperature and
pressure, the compositions are constant and independent of the overall
composition of the alloy. This requires a segregation of the alloying
elements. For example, assuming that o and B are the equilibrium phases
at 1300°C for an alloy of overall composition corresponding to 30% Re,
the equilibrium composition of o would be about 43% Re and that of B about
25% Re. Such large composition differences would be unlikely to occur
between adjacent regions of a vapor deposited alloy without considerable
migration of the deposited atoms by surface and volume diffusion. At
temperatures below about 1400°C, in the tungsten-rhenium system, the time
required for such migration and segregation is probably too long for
completion during the deposition process itself, as evidenced by the fact
that equilibrium was not achieved at 1300°C in 700 hr. One might expect
LS
..
. 12
.
3. 2).
that o and B phases with nonequilibrium compositions (more nearly equal
to one another) might form. However, the A15 phase is apparently more
stable than o phase compositions below about 43% Re (Fig. 2).
The suggestion that large composition differences do not occur
between physically adjacent phases deposited at temperatures be.low about
1400°C 18 substantiated by the variation in the lattice parameters of the
A15 phase with overall composition shown in Fig. 5. This figure illus-
trates that the lattice parameter of the as-deposited A15 phase, whether,
occurring alone or coexisting with ß or o, decreases approximately linearly
with increasing rhenium content for all represented deposition temperatures.
Although the slope of the line in Fig. 5 is only -0.0014 A/% Re, the con-
sistency of the data indicates that the composition of the A15 phase varies
continually, even in two-phase regions. These observations suggest that
the composition of the phases is large.ly determined by the composition and ...
sticking factors of the reacting gases and less by surface diffusion. .
In wrought tungsten-rhenium alloys rhenium has a ductilizing effect .
that is retained at low temperatures. The W-25 at. % Re alloy, in parti-
cular, is ductile at -75°C. In the as-deposited condition this alloy con-
tains different amounts of the A15 phase, depending upon deposition
temperature, and the embritt).ing effect of this phase may limit the
usefulness of as-deposited alloys having the phase as the major constituent.
However, the A15 phase transforms on heating, and a single-phase B alloy
can be obtained at no higher temperature than is required for wrought
alloys. The A15 phase was never observed to form from B or o during
annealing, and the amount of the A15 phase always decreased in alloys
containing the phase in the as-deposited condition. These observations
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...together with the metastable nature of the A15 phase and the proposed
reason for formation during deposition lead to the conclusion that the
A15 phase is unlikely to form in alloys subjected to service in the
temperature range where the phase forms by deposition.
VIII. ACKNOWLEDGMENT
The authors wish to acknowledge the contributions of other people to
this study: R. L. Heestand and J. B. Flynn, experimental apparatus and
assistance; R. M. Steele, x-ray diffraction; W. R. Laing, chemical
analyses; C. P. Haltom, metallography; G. M. Adamson, Jr., C. F. Leitten, Jr.,
T. S. Lundy, W. R. Martin, and W. C. Robinson, counsel and review of the
manuscript; and the Metals and Ceramics Division Report Office for ..
preparation of this paper.
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IX. FOOTNOTES
1. Research sponsored by the U.6. Atomic Energy Commission under
contract with the Union Carbide Corporation.
1.
2. Consultant from the University of Tennessee.
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F
S
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X. REFERENCES
X. REFERENCES
1. J. I. Federer and R. M. Steele, "Identification of a Beta-Tungsten
Phase in Tungsten-Rhenium Alloys," Nature 205( 4971), 587–588
(Feb. 6, 1965).
2. J. I. Federer and C. F. Leitten, Jr., "Vapor Deposition and
Characterization of Tungsten-Rhenium Alloys," Nucl. Appl. 1, 575-580
(December 1965).
3. F. Laves, Crystal Structure and Atomic Size," Trans. Am. Soc. Metals
48A, 124 (1956).
4. M. V. Nevitt, "Atomic Size Effects in Cr30-Type Structures,"
Trans. AIME 212, 350 (1958).
5. P. Greenfield and P. A. Beck, "Intermediate Phases in Binary Systems
of Certain Transition Elements," Trans. AIME 206, 265 (1956).
6. J. M. Dickinson and L. S. Richardson, "The Constitution of Rherium-
Tungsten Alloys," Trans. Am. Soc. Metals 51, 758–771 (1959).
W. B. Pearson, Handbook of Lattice Spacings and Structure of M
Pergamon Press, New York, 1958. .


ts
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16
Table I
Phases in As-Deposited Tungsten-Rhenium Alloys
Deposition.
Rhenium
Phases Presenta
Temperature
7°c)
(wt %)
B
A25
Other
1000
19.1
21.9
23.0
25.6
31.6
34.0
59.0
13.5
""
tu
1100
14.8
ܩ ܩ ܩ ܩ ܩ ܩ ܩ ܩ
1200
ܠ
19.6
23,7
24.7
-26.1
28.5
42.4
11.1
13.5
16.6
18.4
25.8
37.4
44.7
50.8
21.8
22.2
23.9
31.1
37.7
43.5
52.0
57.9
8.3
26.2
28.6
34.0
37.3
57.2
59.3
03330000 2000 2001 e
mer om man voor ooo oo oooooooo
1300
ooo
1400
1500
(c)M
(O)M
Symbols refer to amounts of phases
estimated from x-ray line intensities: S is
strong; M 18 medium; W 18 weak.
Sought but not found.
.
. .
Ini
Table II.
Phases& in As-Deposited and Annealed Tungsten-Rhenium Alloys
Deposition
Temperature
7°c)
Rhenium
(wt %)
As-Deposited
2000°C
20 hr
1800°C
100 hr
Annealing History
1500°C 1450°C
1000 hr 1000 kr
1300°C
700 hr
B
A15
0
B
0
B
0
B
0
B
0
B
A15
1000
21.9
25.6
esta ca
:
34.0
SW
W
S
M W
1100
M
w
es
19.6
14.8
23.7
us to as
Š
s
24.7
ou
os
SWS
W SW SW SW M W W
S M S M . S M
s
1200,
.
SW
S
..
o
:
:
S
S
S
W
1300
1500
28.5
42.4
18.4
25.8
37.4.
50.8
31.1
26.2
28.6
34.0
37.3
57.2
S.
W
S .
S ...
M : M
M: M
.
...W
Wii
M
S
S
S
M
W
M
.
mounts of
"Symbols refer to amounts of phases estimated from x-ray line intensities:
Mis medium;.W is weak.
S is strong;
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....18
1-
Table III.
Ratio of Diffractometer Peak Heights of
(211) A15 to (200) B
Intensity Ratio
Deposition
Rhenium
Annealed at
Temperature
(wt %)
(°c)
As-Deposited
1300°C for
i
700 hr
1000
25
0.1
1000
2.1
.
23.
0
34.0
23.7
28.5
31.1
1100
1100
3.9
1100
: 0.1
21
0.
OS
1300
1.3
.
1500
-
26.2
0.28
-
- -
-
: Weak A15 phase reflection shown by diffractome-
ter but not by Debye-Scherrer powder pattern.
.
-
-
..
.
19
Table IV.
Hardness of As-Deposited and Annealed Alloys
. As-Depositega
Annealeab
Rhenium
(wt 96)
Hardness
Phases
Phases
Hardness
(DPH)
(DPH)
B
420
13.5.
24.8:
450
1:19.6
440
B.
450
...
.
23.27
5000
o
•630
.
A15
24.7.
B
1740C
.
..
A25C..
28.5
1630
1630B
- 42.4
.
115
1830
1030
...
C
'Deposition temperature 1100°c.
1500°C, 1000 hr.
“Major phase.
.
1
bol
.
-
.
..
...
.-.
...
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.

.
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...20
Table v.
Comparison of Calculated and Experi-
mental X-Ray Diffraction Intensities
for the A15-Type Phase
hk.
Intensity (I//1210)
Calculated Experimental,
OOOO
100
110
111
200
210
211
220
300
2
4
!..
310
311
.
E
y
222
320
321
400
410
330,411
331
420
421
332 :
422
430,500
431,510
333,511
432,520)
521
440
441,522
530
531
442,600
610
611
y R5000 0000FS kooo afavo
26
T
-
Soverlapping peaks grouped and
counted together.
LT
Sisi
wy
.
21.
21
XI. LIST OF FIGURES
-
-.
1.
..""
Fig. 1, (ORNL-DWG-67-2763) Tungsten-Rhenium Vapor Deposition
.
.
*
7
,
Apparatus.
Fig. 2. (Original drawing) Vapor-Deposited Phases Shown in Relation
to the Tungsten-Rhenium Equilibrium Phase Diagram.
Fig. 3. (-75274, Y-79798, Y-79796) Microstructures of As-Deposited
Tungsten-Rhenium Alloys. (a) Single-phase B alloy containing 20% Re
deposited at 1100°c. (b) B (principal phase) + A15 alloy containing
26% Re deposited at 1200°c. (0) A15 (p:incipal phase) + B alloy containing
28% Re deposited at 1100°C. Etchant: l part NH4OH (conca) and 1 part
H2O2 (30%).
Fig. 4. (Y-79621, Y-79623) Microstructures of Tungsten-Rhenium
Alloy Deposits Annealed at 1500°C for 1000 hr. (a) Single-phase B alloy
containing 20% Re. (b) B + o alloy containing 299 Re. Etchant:. i part
NH4OH (conca) and 1 part H2O2 (30%). .
Fig. 5. (Original drawing). Lattice Parameters of the A15 Phase as.
a Function of Rhenium Content of the Alloy.
.
.
..
-
.
.
.
...-
-
.
.
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WF6
MANOMETER
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COPPER ELECTRODE
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-
...
-
-
-
-
..
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..
.
.
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H2O OUT
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