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ORNL-TM-2483.txt
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& e f
P rsartcey—of
OAK RIDGE NATIONAL LABORATORY
operated by
UNION CARBIDE CORPORATION %
NUCLEAR DIVISION
for the _
U.S. ATOMIC ENERGY COMMISSION (}4 c
ORNL- TM- 2483
i6
PE men
BT T MAR 2
e et MMM i s TR - i L
e s P
PREIRRADIATION AND POSTIRRADIATION MECHANICAL
PROPERTIES OF HASTELLOY N WELDS
H. E. McCoy
D. A. Canonico
—_———————— LEGAL NOTICE ——————— —
This report was prepored os an gccount of Government sponsored work. Majther the United States,
nor the Commission, nor any person acting on behalf of the Commission:
A. Makes any warranty or representation, expressed or implisd, with respect to the occuracy,
completeness, or usefulness of the information ceontoined in this report, or that the use of
any information, opparctus, method, or process disclosed in this report may not infringe
privotely owned rights; or
B. Assumas any liabilities with respect 1o the use of, or for domages resulting from the use of
any information, apporatus, methed, or process disclosed in this report.
As used in the ohove, "'person acting on behalf of the Commission” includes any employe= or
contractor of the Commission, ot employee of such controctor, to the extent that such employes
or contractor of the Commission, or employee of such contractor prepores, disseminates, or
pravides occess to, any information pursuont to his employment or contract with the Commissien,
or his employment with sueh contractor,
ORNL-TM-2483
Contract No. W-7405-eng-26
METALS AND CERAMICS DIVISION
PREIRRADIATION AND POSTIRRADIATION MECHANICAL
PROPERTIES OF HASTELLOY N WELDS
H. E. McCoy and D. A. Canonico
Submitted to the Welding Journal without the Appendix.
MARCH 1969
OAK RIDGE NATIONAL LABORATORY
Oak Ridge, Tennessee
operated by
UNION CARBIDE CORPORATTION
for the
U.S. ATOMIC ENERGY COMMISSION
A 0 BN A e et
[P
e ¥Ry
R R 1
iii
CONTENTS
Abstract .
Introduction .
Experimental Details .
Experimental Results .
Tensile Properties
Creep-Rupture Properties
Postweld Heat Treatments
Metallography . . « « « « + « « &
SUMMAYY « « o« e e e e e e e e e
Acknowledgments
References .
Appendix .
PREIRRADIATION AND POSTIRRADIATION MECHANICAL
PROPERTIES OF HASTELLOY N WELDS
H. E. McCoy and D. A. Canonico
ABSTRACT
Welds were made by the TIG process in several heats
of Hastelloy N. The mechanical properties of transverse
weld samples and the base metal were compared in tensile
tests over the range of 75 to 1600°F and in creep tests at
1200°F. The as-fabricated welds exhibited lower fracture
strains than the base metal under all test conditions, but
the properties of the welds were improved markedly by post-
weld heat treatments. The postirradiation tensile and
creep properties of the welds and base metal at elevated
temperatures were about the same, although the properties
were widely different before irradiation.
INTRODUCTION
Hastelloy N is a trade name given the solid-solution-strengthened
nickel-base alloy developed at the Oak Ridge National Laboratory specif-
ically for use in molten fluoride salts up to 1500°F (ref. 1). The
alloy was originally designated INOR-8 and has a nominal composition of
Ni—17% Mo—7% Cr—5% Fe. This material is the primary metallic structural
material in the Molten Salt Reactor Experiment (MSRE) which achieved
criticality on June 1, 1965, at Oak Ridge, Tennesse.? This alloy has
been used for numerous other applications, and we anticipate that a
slightly modified composition will be used in a future molten salt
breeder reactor experiment.
The weldability of this material has received considerable atten-
3,4
tion in our program. We found it necessary to establish a weldability
test to determine whether specific heats of material could be joined
satisfactorily. Through this screening process, it was possible to
select heats for use in fabricating the MSRE components.
During the past few years we have found that Hastelloy N as well
as other nickel- and iron-base alloys are subject to a type of neutron
irradiation damage that decreases the creep-rupture strength and fracture
556 Thisg damage 1is rather general for
strain at elevated temperatures.
all austenitic iron- and nickel-base alloys and is attributed to the
production of helium within the material due to the interaction of a
neutron of thermal energy with '“B to produce “Li and “He (refs. 7-14).
The property changes due to the helium must be evaluated for base metal
and welds.
In the present paper, we shall show how the mechanical properties
of transverse welds differ from those of the base metal and what types
of annealing treatments can be used to improve the properties of welds.
We shall also show how neutron irradiation alters the mechanical proper-
ties of the welds and the base metal. The mechanical properties measured
in this study were tensile properties over the temperature range of 75
to 1600°F and creep properties at 1200°F.
ok b e R A R PR B R R e vt SR et ke R e ok e G e 1 e b R AR 20, Rttt L e L
EXPERIMENTAL DETAILS
Several heats of Hastelloy N were used in this study and their
chemical compositions and other pertinent details are given in Table 1.
Heats 65-552 and 2477 were wvacuum melted; all others were air melted.
All base metal was annealed for 1 hr at 2150°F prior to testing unless
otherwise specified.
Seven weldments were involved in this study and the details are
given in Table 2. The welds were all highly restrained and made by the
manual tungsten-arc welding process. A standard welding procedure was
used on all the welds, although some deviation was necessary in welds 7
and & because of the type of filler metal being used. The joint configu-
ration and pass sequence are shown in Fig. 1. The primary working
direction in the plates was perpendicular to the weld axis.
We used small mechanical property samples throughout the study,
since this geometry was required for the irradiation experiments (Fig. 1).
The samples were cut perpendicular to the weld axis and parallel to the
stringers. Three layers of specimens were cut from all the welds except
No. 3; we could find no systematic variation in properties from top to
bottom. However, the gage portions of the transverse weld specimens did
contain different amounts of weld metal since the joint tapered (Fig. 1).
The tensile tests were run in an Instron Universal testing machine
1
(10,000-1b capacity) at strain rates of 0.05 or 0.002 min~ The strain
measurements were taken from the crosshead travel. A similar machine
was located in a hot cell for testing the irradiated samples. The labo-
ratory creep-rupture tests were run in standard lever-arm creep machines.
The strain measurements were taken from the pull-rod displacement after
Table 1. Chemical Analysis of Test Materials
Heat . Composition
Designa- Meltl?g
etiin Fractice Cr Fe Mo c si Co W (w;n%j v P S AL Ti Cu B (pgm) N
5065 Air 7.2 3.9 16.5 0.065 0.e0 0.08 0.04 0.55 0,22 0.004 0.007 0.01 0.01 0.01 10-37 16 110
5067 Air 7.4 4.0 17.3 0.060 0.43 0.08 0.06 0.50 0.30 0.013 0.007 0.01L 0.01 0.015 10-24 12 100
5101 Air 6.9 3.9 16.4 0.05 0.63 0.05 0.44 0.34 0,001 0.009 - 0.022 — 3.5
5055 Air 7.9 3.8 16.2 0.06 0.6l 0.03 0.69 0.21 0.006 0.008 0.06 0.02 50
2477 Vacuum 7.05 4.25 16.3 0.057 0.015 0.14 0.47 0.04 0.008 0.003 0.055 0.10 0.10 8 5 7
65-552 Vacuum 6.89 4.06 16.2 0.045 0.16 0.050 0.006 0.45 < 0.0005 0.002 0.006 0.25 0.5 1.3 9
aCom.bined amount of eluminum and titanium.
Table 2. Identification of Welds Made in This Study
Weld Thickness
Nurber Base Metal Filler Metal of.Weld
{in.)
1 5065, 5067 5101 1
3 2477 2477 1/2
4 5065, 5067 5101 1
5 5065, 5067 5055 1
6 5065 65-552 11/8
7 5065 5055 + Al,052 11/8
5065 5055 + WC? 11/8
8piller material was 1/8 in. wire of heat 5055 plasma
sprayed with 0.002 in. of indicated material.
the load was applied. The postirradiation creep-rupture tests were run
in 1ever-arm creep machines located in the ORNL hot cells. The strain
was measured by an extensometer with rods attached to the upper and lower
specimen grips. The relative movement of these two rods was measured by
a linear differential transformer. All tests were run in an air environ-
ment. We used a standard equilibrating time of 1/2 hr for each test
prior to loading.
The irradiations were conducted in two facilities: the ETR,
Idaho Falls, Idaho, and the ORR, Oak Ridge, Tennessee. A core facility
was used in the ETR where the thermal and fast (> 1 Mev) fluxes were
each 3.2 X 10%* neutrons em™? sec™!. The fluence obtained there was
5 x 10°° neutrons/cmz. The ETR experiments were uninstrumented and the
design temperatures were either less than 300°F or 1112 + 180°F. A
core facility was also used in the ORR where the thermal flux was
ORNL-DWG 68-12878R
DIMENSIONS IN INCHES
<
FILLET WELDED TO STRONG BACK TO PRODUCE HIGH RESTRAINT WELD
29
1, +O L
- Ya 16 MAX
JOINT DESIGN AND WELDING SEQUENCE
+0.0000 in.
Q.0008 in.
Q.0000 in.
0.0005 in.
+Q.0000C in,
Q.Q00% in.
! e >
@® @® !
nE 3 @
N o 63
o s 53
|
i £
! oX
- — — Q= _
t ~(E
S
\ |
|
00008
\— 01875 R(TYP)
~—-3in. 1425 in.
*'77/5 in.
MECHANICAL PROPERTIES SPECIMEN.
Fig. 1. The INOR-8 High-Restraint Weldability Test Specimen Used
to Provide Samples for the Mechanical Properties Study.
2.5 x 10'% neutrons cm™? sec™l. The fluences obtained were
8.5 x 102° neutrons/em® thermal and 7.0 x 102° neutrons/cm? fast
(> 1 Mev). The temperature in this facility was 110°F. We could not
observe any effect of fluence over the small range involved here, so
the data are presented without reference to a particular experiment.
Irradiation temperature was important in some cases and will be indicated.
EXPERIMENTAL RESULTS
Tensile Properties¥
The variation of the fracture strain in a tensile test with test
temperature is shown in Fig. 2 for both transverse welds and base metal.
The behavior of this particular heat of base metal is typical for
Hastelloy N. The decrease in fracture strain above 1100°F is due to
ORNL-DWG 6812875
% l ]
T T T T
HEAT 5065 WELD1 WELD 4
AS PROCESSED ° A &
AFTER IRRADIATION . .
80 POST WELD ANNEAL OF 8hr
AT 1600°F
UNIRRADIATED 0
IRRADIATED -
-~
o
UNIRRADIATED BASE METALX
v ¥
o
[=]
-
-~
I
o
I
L
o
“
e
-
-
n
o
-
,/
Vo
L
|1 “NIRRADIATED BASE METAL \ \\/!
\
o \
\
FRACTURE STRAIN (%)
o
O
o
o
. \
A‘—-—- 9 \ 1
20 ——]
UNIRRADIATED WEL[;?\\\ /
0 "'\\ /
o S
o 200 400 600 800 1000 1200 1400 1600 1800
TEST TEMPERATURE (°F)
Fig. 2. Ductility of Hastelloy N Welds and Base Metal in Tensile
Tests at a Strain Rate of 0.05 min™?!.
*See Tables A-1 and A-2, Appendix, for the tabulated tensile data.
the transition from transgranular to intergranular fracture. The
recovery above 1400°F is associated with increasing grain boundary
mobility. The fracture strain of the welds is much lower. Most of the
welds fractured in the weld metal, but several samples tested at 75 and
392°F did fail in the base metal.
The fracture strain after irradiation is also shown in Fig. 2.
Since these samples were irradiated at less than 300°F, there is some
displacement damage in the base metal and the fracture strain is lower
at test temperatures of 75 and 392°F. At test temperatures of 1200 and
1600°F, where intergranular fracture predominates, the fracture strain
of the base metal is reduced dramatically. The postirradiation fracture
ductility of the irradiated welds is also shown in Fig. 2. The strain
at fracture of the welds is reduced slightly by irradiation, but the
changes are much less than those observed for the base metal. Thus,
although the ductility of the welds is much lower than that of the base
metal before irradiation, the ductilities of welds and base metal at
elevated temperatures are quite similar after irradiation.
The yield strengths of typical welds and base metal are compared
in Fig. 3. The yieldlstrengths of the transverse weld samples are con-
sistently higher than those of the base metal. This same observation
was also made by Gilliland and Venard.’ After a postweld anneal of & hr
at 1600°F, the welded and base metal samples have very similar yield
strengths.
Irradiation increases the yield strength of the base metal and
welded samples at low temperatures. This damage anneals out as the test
temperature is increased, and the welds and base metal show similar
ORNL - DWG 6B-12876
120 l .
| ! ‘
HEAT 5065 WELD1 WELD 4
s L,R,fsf‘ED'GE%EL AS PROCESSED o 0 a
0o | ¥ AFTER IRRADIATION o s
R N A POST WELD ANNEAL
7 \\\\\\ OF 8hr AT 1600°F
o 80 —— % UNIRRADIATED o
e
8 a ‘-~::::§\ IRRADIATED | | oo
= . —— —~— |, UNIRRADIATED WELDS
; — o \ T
3 40 O S —O
u UNIRRADIATED BASE METAL — &
N
20
0
0 200 400 600 BOO {000 {200 1400 1600 1800
TEST TEMPERATURE (°F)
Fig. 3. Yield Strength of Hastelloy N Welds and Base Metal in Ten-
sile Tests at a Strain Rate of 0.05 min~1.
recovery. Thus, above 1200°F the yield strengths of base metal and
welds annealed for & hr at 1600°F are equivalent and are unaffected by
irradiation.
Figure 4 shows that the ultimate tensile strength is about the same
for welded samples and for base metal. This property is not affected
significantly by postweld heat treatment at 1600°F. Irradiation causes
a slight (approx 10%) increase in the ultimate tensile strength at the
iower test temperatures and a decrease at test temperatures of 1200°F
and greater. This reduction at higher temperatures is due to the reduced
ability of the material to deform plastically after irradiation (i.e.,
fracture occurs before the stress increases to the higher wvalues noted
for unirradiated materials).
Thus, the effects of welding on the strength parameters measured by
standard tensile tests are relatively small and the most significant
factor is the reduction in the fracture strain. The fracture strains
observed for the welds involved in this study are summarized in Fig. 5.
FRACTURE STRAIN (%)
140
120
100
80
60
40
ULTIMATE TENSILE STRESS (1000 psi)
20
Fig. 4.
10
ORNL-DWG 68-12877
o
g
0 -._--'-'-1
e ; b\o\q\
‘\
g \
5
&
- HEAT 5065 WELD { WELD 4 A
AS PROCESSED o o A
AFTER IRRADIATION . a
[ POST WELD ANNEAL
OF 8 hr AT 1600°F
UNIRRADIATED o
I IRRADIATED .
0 200 400 600 800 1000 1200 1400 1600 1800
TEST TEMPERATURE {°F)
Ultimate Tensile Strength of Hastelloy N Welds and Base
Metal in Tensile Tests at a Strain Rate of 0.05 min~?!.
ORNL -DWG 68- 12888
80
T B As wELDED - — = .
72 7?,, ANNEALED 8hr AT 1600°F o ]
o 8 | AS WELDED - IRRADIATED
R e - T TTTT 7T T ANNEALED 8hr AT 1600°F - IRRADIATED 13 T T
64 Fu—O—F — e = —0
- E T ®©
I <L_ E . - b —— _ -a
w Y < _J
T w o
56 " 7?-7 - =
~ & 33
11 R | -
48 - x ***2 ® *'&*nn *ul':
l " o g w 8 o
T .88 755
x = oW
40 = ] - ! 75 I -
| Y
: = =I
ST
\ J \ J -
Y
7°F 1200°F
Fig. 5. Comparison of the Fracture Strains of Welds and Base Metal
in Tensile Tests at a Strain Rate of 0.05 min~>.
ek e A G S e R Tk IS L e o e
11
Welds 1, 4, and 5 involve air-melted materials with relatively high
boron levels. Heat 2477, a vacuum-melted heat containing & ppm B, was
used as the base and filler metal in weld 3. Weld 6 utilized filler
metal from heat ©65-552, a vacuum-melted heat containing 1 ppm B, and
base metal from heat 5065, an air-melted heat. Welds 7 and 8 utilized
air-melted base and filler materials. The filler rod for weld 7 was
plasma-spray-coated with Al,03 in an effort to reduce the interdendritic
spacing in the cast weld metal and to provide additional sites for helium
collection. However, most of the Al,03 floated on the weld and had to
be removed mechanically before making the next pass; the aluminum content
of the deposited weld metal was only 0.06% compared with 0.84% for a
typical cross section from the filler metal before deposition. Weld 8
involved a filler material coated with WC. The deposited weld metal
contained 2% W and 0.1% C, so the WC coating dissolved in the melt
altered the properties of the weld appreciably.
The fracture strains shown in Fig. 5 are compared for
1. base metal given a standard solution anneal of 1 hr at 2150°F,
2. base metal given the 1 hr at 2150°F treatment followed by an anneal
of 8 hr at 1600°F,
3. transverse weld samples in the as-welded condition, and
4. transverse weld samples annealed for & hr at 1600°F.
These properties are considered for unirradiated and irradiated condi-
tions where data are available.
At a test temperature of 75°F the following points are illustrated
in Fig. 5.
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1. The fracture strains of all welds are lower than those of the
base metal.
2. Welds 1, 4, and 5 all involved air-melted alloys and exhibited
the lowest fracture strains.
3. Welds 3 and 6 involved vacuum-melted weld metal and have the
best properties.
4. Welds 7 and 8, which involved air-melted alloys with the filler
metal modified with Al,05; and WC, exhibited intermediate properties.
5. Postweld heat treatments generally improved the properties.
6. Irradiation decreased the fracture strain of all welds and
base metal. The welds had lower postirradiation ductilities than the
base metals, but the welds were affected less by irradiation.
7. The postirradiation ductilities of welds did not depend
appreciably on whether they had received a postweld heat treatment prior
to irradiation.
8. The postirradiation properties of all welds except No. 8 were
equivalent.
Figure 5 also illustrates several important points at a tensile
test temperature of 1200°F.
1. The fracture strains of all welds were lower than those of the
base metal.
2. The as-welded ductilities of all welds except No. 8 were about
equivalent, ranging from 12 to 18%. Weld & had 25% strain at fracture
under these conditions.
i3
3. A postweld heat treatment of 8 hr at 1600°F markedly improved
the fracture strain, with values of 22 to 30% being observed. Weld &
again was better.
4. After irradiation, all welds were less ductile than the base
metal. There were some differences in the ductilities of the welds, but
no consistent trends are apparent.
5. Postweld annealing for 8 hr at 1600°F had little effect on the
postirradiation properties.
At 1600°F, Fig. 5 shows the following trends.
1. The fracture strains were drastically lower for welds than for
base metal. Welds 3 and 8 had properties superior to those of the other
welds. DPostweld heat treating had a beneficial effect on the ductility.
2. Irradiation reduced the fracture strain to about 2% independent
of whether the test sample was base metal or a transverse weld.
All of the postirradiation results presented thus far have been
for materials irradiated at less than 300°F. We have irradiated several
samples of these heats and others at 1200 to 1400°F and find that there
are at least two significant differences in the results obtained. The
displacement damage anneals at these irradiation temperatures and the
tensile properties up to about 1000°F are the same for irradiated and
unirradiated materials. At higher test temperatures the fracture strain
is reduced even Turther if the irradiation temperature is in the range
of 1200 to 1400°F. For example, heat 5065 was found to have a fracture
strain of 11.3% (irradiated at 1200°F) at 1200°F compared with the
value of 22.2% (irradiated at less than 300°F) shown in Fig. 5. Weld 7
was observed to have fracture strains at 1200°F of 7.2 and 10.8% after
14
irradiation at 1200°F and less than 300°F, respectively. Thus, the
trends shown in Fig. 5 for samples irradiated at 300°F seem to hold for
irradiation temperatures in the 1200 to 1400°F range, although the actual
fracture strains may be lower for the higher irradiation temperature.
Creep-Rupture Properties*
The stress-rupture properties at 1200°F of several heats of base
metal are shown in Fig. 6. The data are described reasonably well by
a single line, although both air- and vacuum-melted materials are
involved. The line for the base materials is shown in Fig. 7 where a
comparison is made between the stress-rupture properties of the base
metal and the various welds involved in this study. All of the welds
had lower creep-rupture strength in the as-welded condition than the
base metal. Weld 3, which involved only vacuum-melted materials, had
significantly higher strength than the other welds. Welds 7 and 8, which
involved A1,0; and WC additions, also showed notably better performance
than welds 1, 4, and 6. The rupture lives of the welds approached those
of the base metal as the stress level was reduced; this is likely due to
thermal recovery of the weld metal during the long time at 1200°F. The
strength was improved greatly by a postweld anneal of 8 hr at 1600°F.
The fracture strains of the welds and several heats of base metal
are compared in Fig. 8. The fracture strain of the base metal was about
25% for short rupture lives of a few hours and decreased to values of
10 to 15% when the rupture life was 1000 hr. There is no appreciable
difference between air- and vacuum-melted alloys. The welds had fracture
*See Tables A-3 and A-4, Appendix, for the tabulated creep-rupture
data.
15
ORNL-CWG 68-12879