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ORNL-2264.txt
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JSECRET cp fi
ORNL.2264
AEC RESEARCH AND DEVELOPMENT REPORT - P
v A
TR
3 445k 0022989 3
INCONEL AS A STRUCTURAL MATERIAL FOR A
HIGH.-TEMPERATURE FUSED.SALT REACTOR
J. R. Weir, Jr.
D. A. Douglas
W. D. Manly
M..m..,.(,..cmDEGLAS‘:EE:E
By AUTHORITY OF: fiafi (; ? :—?;__\);J? = f
CENTRAL RESEARCH LIBRARY
DOCUMENT COLLECTION
LIBRARY LOAN COPY
DO NOT TRANSFER TO ANOTHER PERSON
If you wish someone else to see “this
~ document, send in name with document
: .und the library will arrange o Iodn
OAK RIDGE NATIONAL LABORATORY
OPERATED BY
UNION CARBIDE NUCLEAR COMPANY
A Division of Union Carbide and Carbon Corpurufi@‘r\:
uce NG
POST OFFICE BOX X * OAK RIDGE, TENNESSEE
RESTRICTED.DATA
ORNL.-2264
This document consists of 78 pages.
Copy\_,c_-nf 191 copies. Series A.
Contract No. W-7405-eng-26
METALLURGY DIVISION
INCONEL AS A STRUCTURAL MATERIAL FOR A
HIGH-TEMPERATURE FUSED-SALT REACTOR
DATE ISSUED
JUN 41357
ATIONAL LAEDRATORY LIBS.
OAK RIDGE NATIONAL LABORATORY
UNION cmmgfl'%fibfia COMPANY 3 yys5& 00229489 3
A Division of Union Carbide and Corben Corporati
Post Office Box X
Oak Ridge, Tennessee
CONTENTS
SUMMARY . .coocuonnssmmmsisse
Corrosion Resistance........c..ccoeeeennns
B ORI, comoirsmnsrnesmomemmarbefearertrr i ns e s e A i vmun i b prson i st s mesarmmssbensiiepr s b
B b FR DB R oLl s sessmninssssk B ek B LN B B o e o R DR
Effects Produced by Neutron and Gamma Flux ..........
Mechanical Properties of the Alloy in Contact with Various Environments at
High Temperatures...................
MATERIALS AND EQUIPMENT ....cccoommninn
TESTING EQUIPMENT ......ccovvnrvnnenes
RESULTS AND INTERPRETATION ...cccccccmmmsnisnisasins:
Creep-Rupture Tests ..........
Effect of a Biaxial Stress System on the Stress-Rupture Properties ........ccoovevivinnrrnnnne
Effect of Section Thickness on the Creep-Rupture Properties in the Various Media .................
Effect of Welding on the Creep-Rupture Strength...cccccviniecnniance
Variations in Strength Among Various Heats of Inconel. ..o
Tensile Properties of Inconel...............
Some Physical Properties of Inconel..............
Design Data...c.ccccevereereneinscniiinnnnnnanens
DISCUSSION iiccicviiins
CONCLUSIONS AND RECOMMENDATIONS .....ocooorrcecierrecererereienes
ACKNOWLEDGMENTS :....cocemssernssicsansanss
MR R = =
43
45
53
56
62
63
67
71
71
INCONEL AS A STRUCTURAL MATERIAL FOR A HIGH-TEMPERATURE FUSED-SALT REACTOR
J. R. Weir, Jr.
SUMMARY
A prototype aircraft reactor test unit is being
constructed in which fused fluoride salt No. 30
{NqF-ZrF4+UF4, 50-46-4 mole %) is used as the
fuel and as the primary-circuit heat transfer fluid,
with sodium and NaK used as the secondary-
circuit heat transfer media. Inconel was selected
as the material to be used for the construction of
this reactor, and an extensive testing program was
initiated to evaluate its high-temperature mechani-
cal properties.
The elevated-temperature creep-rupture properties
were evaluated at 1300, 1500, and 1650°F in
various reactor environments. The tests were
carried out under constant load conditions, since
this type of test produces more realistic design
data. The data were obtained in the inert gas
argon, and the results of creep data obtained in
environments of sodium, fused salt No. 30, and
air are compared with the argon data as a reference
for determining environmental effects.
The fused salt, which is corrosive to Inconel,
was found to reduce the creep strength and to
decrease the rupture life in comparision with tests
conducted in argon. High-purity sodium is inert
to Inconel in an isothermal system, and creep
results in this medium compare well with data
obtained in argon. The results of creep tests in
an air environment indicate that thin-sheet Inconel
is strengthened by this oxidizing environment.
In thicker sections this environment does not
appreciably affect the creep rate but does prolong
the rupture life at lower stress levels. The results
of creep-rupture tests conducted with sheet speci-
mens of various thickness indicate that the dele-
terious effect of the fused salts on the strength
of Inconel becomes more pronounced as the speci-
men thickness is decreased.
Variations in structure resulting from annealing
treatments have an effect on the creep properties.
The data indicate that the fine-grained material
has superior strength at low temperatures and high
stresses and that the coarse-grained material has
better strength at high temperatures and low
stresses.
D. A. Douglas
W. D. Manly
Considerable variation in properties may be
expected from different heats of Inconel. Appar-
ently these variations in strength result from
small differences in chemical composition or
fabrication procedures.
Tests in the sodium environment show that the
liquid-metal coolants are inert under isothermal
conditions if there is no contamination from oxygen.
Sodium contaminated with oxygen decarburizes
Inconel, thus decreasing the creep properties and
rupture life.
Air tests reveal that in large sections the data
will correspond very well with the argon data but
that thin sections are significantly strengthened
by the oxidizing environment.
INTRODUCTION
The use of a circulating-fuel type of nuclear
reactor as an energy source in aircraft propulsioen
systems imposes wupon the structural material
metallurgical restrictions which limit the appli-
cability of certain types of alloys. The general
factors which must be considered in the selection
of an alloy for this application are corrosion
resistance, fabricability, nuclear properties, radi-
ation damage, and elevated-temperature strength.
In the following discussion the importance of each
of these topics will be pointed out and it will be
shown that the selection of Inconel as a structural
material was based on these criteria.
Corrosion Resistance
The interaction between the structural material
and the circulating fluids is of major importance,
since all the reactor components in contact with
these fluids must operate without leakage through-
out the proposed 1000-hr operating life. In liquid
media, corrosion phenomena such as dissimilar-
metal transfer and temperature-induced mass
transfer, as well as general solution, occur. The
mode and rate of attack will depend upon such
factors as the temperature, the thermodynamic
activity and the solubility of the various metallic
phases and elemental constituents of the alloy,
and the chemical reactions involving the liquid,
impurties of the liquid, and the elemental con-
stituents of the alloy. The base metal must also
be alloyed such that, in the presence of air moving
at high velocity, the oxide formed will be protective.
Fabricability
The alloy or alloys to be used in the construc-
tion of reactors of this type must be amenable to
welding, brazing, and hot and cold forming.
Welding. — The weldability of an alloy is de-
pendent primarily upon the physical and mechanical
properties of the base metal during and after
welding. During the welding operation stresses
may be induced in the weld zone by volume changes
resulting from the thermal coefficient of expansion,
the allotropic phase transformations, and the
solution and precipitation of gases and minor
phases. The stresses may result in failure of the
weld if the strength of the weld is low at temper-
atures near the melting point or if the weld is
weokened by porosity, low-melting eutectics, or
gross oxidation. Some of the problems asscciated
with welding can be alleviated by carefully se-
lecting the alloying el ements to include deoxidizers
and solid-solution strengtheners and by controlling
the residual elements.
Brazing. — Alloys which are best suited for
hydrogen-furnace brazing must have easily reducible
oxides, form no stable hydrides, contain no alloying
element which will form a brittle intermetallic
compound with the brazing alloy, and be metal-
lurgically stable at the brazing temperature, since
further heat treatment involving any higher temper-
ature is not possible.
Hot and Cold Forming. — Hot-forming operations
such as tube or pipe extrusion and rolling must
be performed at temperatures high encugh to render
the material weak so that prohibitively high-press
capacities and roll pressures will not be involved.
On the other hand, the temperature at which the
material becomes ‘‘hot short'’ must be avoided.
These two factors place a lower and upper temper-
ature limitation on the hot-working range of the
alloy. For both practicality and quality control,
the best alloys are those with a wide temperature
range in which hot work is possible. It is also
desirable to have the metal ductile and soft at
room temperature so that cold rolling and machining
operations may be more easily accomplished.
Although not a major consideration, the castability
of the alloy may be important, since casting is
less expensive ond less time consuming than
forging and machining operations. The use of
casting as a means of forming may be limited
by the sometimes poor corrosion resistance and
ductility of cast structures.
Nuclear Properties
In order to attain high neutron efficiency in the
core of a reactor, the structural material in this
region must have a low neutron cross section,
a requirement which limits the use of elements
such as cobalt, tungsten, and manganese. The
restriction of the use of cobalt is unfortunate
since it is one of the most potent agents used to
obtain strength at high temperatures.
Effects Produced by Neutron and Gamma Flux
Although the data in the field are meager, it is
known that neutron and gamma flux may affect the
creep and tensile properties, the oxidation resist-
ance, and the corrosion resistance of the materials
exposed to this flux.
effects depends, of course, upon the flux density,
the temperature, and the particular material in-
volved.
The importance of these
Mechanical Properties of the Alloy in Contact with
Various Environments at High Temperatures
Some of the more important considerations in the
selection of an alloy for aircraft reactor application
are its strength and ductility at high temperatures
in such environments as air, sodium, NaK, and the
proposed liquid fuel. The advantages to be gained
from the use of high-strength alloys are a decrease
in reactor weight, an increased design margin of
safety, and a longer life expectancy for critically
stressed components.
Commercial high-temperature alloys may be
classified into the two broad categories of second-
phase-hardened ond solid-solution-hardened alloys.
At low temperatures the phose-hardened alloys
have the advantage of being generally stronger
than the solid-solution-hardened alloys, although
As the temperature is increased,
however, they tend to lose their strength because
of the instability of the precipitate and therefore
lose this advantage.
A survey of the commercial high-temperature
alloys, based on the factors discussed above as
the criteria for selection, yielded Inconel as the
most promising reactor material. It then became
the responsibility of the Mechanical Properties
Group to obtain the necessary data needed for the
less ductile.
2 " &}@:
design of a prototype reactor using fused fluoride
No. 30 (NuF-ZrF‘-UFd, 50-46-4 mole %) as the
fuel and as the primary-circuit heat transfer fluid,
with sodium and NaK as the secondary-circuit heat
transfer media.
This report is a summary of the work of the
Mechanical Properties Group in an effort to obtain
the necessary mechanical properties data for
Inconel in the temperature range 1200 to 1650°F.
MATERIALS AND EQUIPMENT
The reactor design is such that formed sheet and
tubular materials are used to a great extent in the
construction. Since it follows that any surface
reaction which might occur between the liquid-
metal coolants and Inconel or between fused
fluorides and Inconel would have a greater effect
on the strength of a thin sheet than on the strength
of a heavier section, it was decided that the testing
of thin sheet and tube materials would produce the
most useful design data.
The basic design of the sheet and tube specimens
used in testing is shown in Fig. 1. The machining
methods used to form these specimens are described
in ORNL-2053.7 The ASTM specification for the
chemical composition of Inconel is reproduced in
Table 1. Also listed are the chemical compositions
of the various materials which have been tested.
TESTING EQUIPMENT
The equipment used for creep-rupture tests and
for tests of the tubular specimens in the various
liquid and goeeous environments is described in
detail in ORNL-2053.2
RESULTS AND INTERPRETATION
Creep-Rupture Tests
For the purpose of obtaining the basic design
data a large quantity of 0.060-in.-thick sheet
Inconel was obtained. The chemical composition
of this heat (designated as heat B) of Inconel is
given in Table 1. Specimens from this heat of
Inconel were creep-rupture tested at 1300, 1500,
and 1650°F (except for tests in sodium, which did
lD. A. Douglas and W. D. Manly, A Laboratory for the
High Temperature Creep Testing of Metals and Alloys
in Controlled Environments, ORNL-2053 (Sept. 18, 1956).
21pid., p 9.
Table 1. Chemical Composition (%) of Various Heats of Inconel
0.060-in.-Sheet
iy A.S.'I'M | Seacimbes 0.0 20-i.n.-5hee| Tl.-lbfl
Specification Tk R Specimens Specimens
Ni 72 (min) 78 76 76 76
Cr 1417 14.9 15.4 14.8 16.0
Fe 6-10 6.4 7.4 8.1 7.6
Mn 1.0 (max) 0.31 0.23 0.29
G 0.15 (max) 0.04 0.04 0.02 0.04
Cu 0.5 (max) 0.13 0.09 0.13 0.13
Si 0.5 (max) 0.18 0.21 0.09 0.22
S 0.01 (max) 0.007 0.007 0.007 0.007
Al 0.08 0.19 0.15
T 0.16 0.33 0.20
B 0.091 0.094
N, 0.091 0.027
UNCLASSIFIED
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ALL DIMENSIONS ARE IN INCHES
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TUBE BURST SPECIMEN
Fig. 1. Drawing of Sheet and Tubular Types of Specimen.
not exceed 1500°F) in the environments and con-
ditions listed below:
Specimen Condition Environment
As-received Argon
Fused salt No, 30
Sodium
Air
Annealed at 2050°F for 2 hr Argon
Fused salt Neo. 30
The material designated ‘‘as-received’’ was
tested in the condition in which it was received
from International Nickel Company, Inc. The INCO
sheet fabrication procedure consists of
1. hot working from 18 x 18 in. ingot to 20% over
finish size,
passing through the 1900°F hot zone of the
annealing furnace in 3% min,
. pickling in an HNO,-HF mixture,
20% cold working to size,
passing through the 1900°F hot zone of the
annealing furnace in 4]’2 min,
2.
6. pickling in an HNO,-HF mixture,
7. roller leveling.
The microstructure resulting from this treatment
is shown by the photomicrographs of the as-received
material in Figs. 2 and 3. The material in this
condition is fine-grained, having an ASTM grain
size number of 6 to 7. The fine precipitate seen
within the grains at a magnification of 100 dia
(Fig. 2) appears at 500 dia (Fig. 3) as precipitate
originally present in the grain boundaries before
the material was given the mill anneal.
The material designated as ‘‘annealed” was
annealed ot 2050°F for 2 hr before it was tested.
The microstructure of the annealed material is
shown in Fig. 4. This high-temperature anneal
results in the solution of the carbide precipitates
seen in the as-received material and
coarsening to an ASTM grain size number of 1.
Tests in Argon. — The creep-rupture data ob-
tained in an atmosphere of pure argon are used as
a basis for comparison in studying the effect of
other environments on the creep-rupture properties
of Inconel. The argon atmosphere is considered
to have no effect on the properties of a metal at
high temperature, since no interaction between the
in grain
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Fig. 2. Photomicrograph of As<Received Inconel. 100X. Electrolytically etched with 10% oxalic acid.
UNCLASSIFIE
o Y-13965
Fig. 4, Photomicrograph of Annealed Inconel. 100X. Electrolytically etched with 10% oxalic acid.
D
metal and argon is possible. However, if the gas
contains a high level of impurities such as O,
Co,, H20, or sz the properties of the metal may
be altered as a result of interaction with these
impurities. The argon used as an environment in
the creep-rupture testing of Inconel was purified
by being scrubbed with liquid sodium. This pro-
cedure for gas purification is described in detail
in ORNL-2053.2
The results of creep-rupture testing of Inconel
(heat B) in the as-received and annealed conditions
tested in argon at 1300, 1500, and 1650°F are
presented as graphs of stress vs time to 0.5, 1, 2,
5, 10% elongation and rupture in Figs. 5 through 10.
At the stress levels for which these design curves
are drawn, the as-received material is seen to have
better creep properties than the annealed material
at all three temperatures in that at approximately
the same stress level the time to the various
elongations is greater. The stiffness exhibited
by the as-received material may be attributed to
residual cold work and to the precipitate which
20,000
10,000
5000
STRESS (psi)
2000
1000
20 50
exists in the microstructure, neither of which is
present in the annealed material.
The stress-rupture properties of the as-received
and annealed materials tested ot 1300, 1500, and
1650°F in argon are compared in Fig. 11. The as-
received material is seen to have better rupture
properties at 1300 ond 1500°F, whereas the an-
nealed material exhibits better rupture properties
at 1650°F. Selected representative microstructures
of material taken from stressed and unstressed
portions of as-received and annealed specimens
tested at 1300, 1500, and 1650°F are presented in
Figs. 12 through 29.
The photomicrographs of specimens tested at
1300°F (Figs. 12-17) indicate that transgranular
slip is the principal mode of deformation at this
temperature for both the as-received and the an-
nealed material. A tendency for precipitation to
occur in primary slip planes and in previous grain-
boundary areas left segregated by the short high-
temperature annealing treatment is seen in the
case of the annealed material.
UNCLASSIFIED
ORNL-LR-DWG 19142
RUPTURE
100 200 500 {000 2000 5000 10,000
TIME (hr)
Fig. 5. Design Curve for As-Received Inconel Tested in Argon at 1300°F.
STRESS (psil
30,000
20,000
10,000
RUPTURE
i
E 5000
2000
1000
1 2 5 10 20 50 100 200 500 1000 2000 5000 10,000
TIME (hr)
Fig. 6. Design Curve for Annealed Inconel Tested in Argon at 1300°F,
UNCLASSIFIED
) ORNL-LR-DWG 19143
20,000
10,000 | [ t
0.5% 1% | 2% 5% 10% RUPTURE
--..._‘_-_‘- R Ty Ll _— -.,."-‘
—] — L1 \\"“--_____H "“"-..,__
—— P
"'-.-...____ ‘-‘;::‘:‘."“*- \"‘"---.._ “---.__H fi‘\.\
\\‘_‘\h‘""'fi T -E\""' \\
Pt M
Hh““uhhx\:\‘“‘%h M R
"‘--u...“.| S = -..“'
" —— el T
SRR
"‘h.__‘\x N"""; \ ‘\'\
SRS O
H‘“\b\%\‘
' ; gt
2000 SN
1000 L | y
1 2 5 10 20 50 100 200 500 1000 2000 5000 10,000
TIME (hr)
Fig. 7. Design Curve for As-Received Inconel Tested in Argon at 1500°F.
UNCLASSIFIED
ORML-LR-DWG 15383