Journal of Nuclear Materials 83 (1979) 305-312

0 Norm-Hound Publishing Company

LOW-TEMPERGTUREDU~ILITYOFANELECTRON-BEAM-WELDEDMOLYBDENUMSHEET
PREDOPEDWITHASMALLAMOUNTOFCARBON

Yutaka HIRAOKA, Masatoshi OKADA and Ryoji WATANABE

National Research Institute for Metals, 2-3-12, Nakameguro, Meguro-ku, Tokyo 153, Japan

Received 5 December 1978

The mechanical properties of unwelded and electron-beam-welded sintered molybdenum sheets, in which carbon was
doped or not, were examined by means of a tensile test at tempemtures from -100 to 80C. Scanning electron microscopy
was applied to determine the fracture mode of the specimen and to observe the distribution of precipitates over grain boun-
daries. The results indicated that a small amount of predoped carbon was effective on the improvement in the low-temper-
ature ductility of the welded specimen as well as that of the unwelded one. Such effects are reasonably explained in terms
of the enhancement of the crack propagation stress in the fused zone of the weldment.

1. Introduction There are several reports about the effects of

Electron-beam welding can produce joints of
higher quality in molybdenum or molybdenum-base
alloys than any other fusion-welding method at the
present time. This technique has several advantages
[ 1 ] : exceptionally high power densities and low heat
input that result in narrow fused zone and heat-
affected zone, small grain size in the fused or the heat-
affected zone and little contamination by the weld-
ing atmosphere. On the other hand, the fact that
electron-beam welding is a fusion-welding process is
probably its greatest disadvantage [ 11. Recrystalli-
zation and grain growth cannot be avoided during
fusion welding, and these structures will induce a loss
in ductility, i.e., an increase in ductile-brittle transi-
tion temperature (DBTT).
In our previous report [2], the ductility of a rela-
tively fine-grained sintered molybdenum sheet was
examined by means of a bend test at low temperatures.
It was concluded that a small amount of additional
carbon remarkably improved the ductility of molyb-
denum and changed the fracture mode from an inter-
granular type to a mixed one. These results were
reasonably interpreted mainly by the e~ancement of
the crack propagation stress, which was attributed
to the increase of carbon concentration on grain
boundaries.
carbon on the ductility of welded molybdenum, but
their results significantly differ even in arc-cast
molybdenum of about the same carbon content.
Platte (31 indicated that the ductility of the weld-
ment increased with increasing the carbon content
from 0.02 to 0.06%. Monroe et al. [4] found that
ductility increased ;vith decreasing the carbon content
from commercially fabricated molybdenum having
0.015 to 0.042% carbon. Such a disa~eement seems to
be related to some effect of sheet fabrication history OII
the ducility of the weldment [5].
The purpose of the present report is to measure
the mechanical properties of the unwelded and the
electron-beam-welded sintered molybdenum sheets
by means of tensile test. The effects of a small amount
of additional carbon on the ductile-brittle transi-
tion behavior of the weldment or on the low-temper-
ature ductility of fused zone, heat-affected zone and
base-metal zone were investigated in detail.
2. Experimental procedures
Materials with different carbon contents were
used for our investigation. One was an as-received
commercial sintered molybdenum sheet (1 mm thick)
and the other was a carbon-doped one by the car-

305
306 Y.Hiraoka et at. f Ductility of eIect~o~-beam-welled MOsheet

burizing treatment. The details of the process were 3. Results

given in our previous report [2]. The homogenizing
condition was at 1500C for 20 min in vacuum. The The mechanical properties of the unwelded and
contents of carbon, oxygen and nitrogen in each mater- welded specimens were determined by the tensile test
ial were chemically analyzed. The as-received material at temperatures from -100 to 8OC.
contained about 7 wtppm carbon and the carbon- Yield strength (uv) and fracture strength (ar) and
doped one about 24 w&pm. Oyxgen and nitrogen total elongation (er) of the unwelded specimens, in
contents were about 10 wtppm and <5 wtppm, which carbon was doped (C-DOPES-SNEAKED)
respectively for both materials. or not (AS ANNEALED), are listed in table 1. A
These two materials were electron-beam welded, sm& amount of additional carbon induces a large
where the welding direction was perpendi~~ar to increase in the fracture streng~ at low temperature,
the rolling direction. The welding conditions were as while it induces a slight increase in the yield strength.
follows: a voltage of 50 kV in conjunction with a These results are consistent with those of our pre-
current of 50 mA and a welding speed of about 30 vious work [2]. The total elongation decreases rapidly
mm/s. After welding the surface of the wel~ent with tempemture around 30C for AS ANNEALED
was mechanically polished to eliminate several defects and -40C for C-DOPED-ANNEALED. The elonga-
such as spatter holes. tion of the latter specimen nearly equals that of the
The material which was carbon-doped only in the former at high temperature (above SOOC),but exceeds
fused zone and the heat-affected zone after welding it at low tem~rature.
was prepared as follows. At first the base-metal zone Fig. 1. shows the yield strength and the fracture
of the undoped welded material was covered with thin strength of the electron-beam-welded (EBW) speci-
aluminium foil and then carbon was deposited by the mens, in which carbon was pre-doped (C-DOPED-
vacuum vaporizing method on both surfaces of the ~BW-ANNEALED~ or not ~BW-ANNEALED~.
sample. This sample was homogenized for 20 min at EBW-C-DOPED (FZ, HAZ)-ANNEALED shows a
1500C in vacuum. Lastly the homogenized one was specimen which was carbon-doped only in FZ and
mechanically polished in order to remove the surface HAZ after welding. It is shown that pre-doped carbon
layer. also induces a large increase in ur at low temperature,
Tensile-test specimens with a gage section: 14 mm while it induces a slight increase in u,, in the same as
long and 4 mm wide were cut out from these unwelded
and welded sheets, in which carbon was doped or not.
All these specimens were anneated at 1500C for 60 Table 1
Tensile data for the unwelded specimens
min in vacuum before testing. The welded specimens
were etched, and the length of the fused zone (FZ), Sample T
heat-affected zone (HAZ) and base-metal zone (BMZ) CC> ;rly08
Pa) ;IfOa Pa) &
was measured by means of a magnifying microscope
AS ANNEALED 80 1.89 4.17 42.5
before and after the test. The length of FZ and HAZ
50 2.56 4.53 40.9
before testing were about 1.26 and 1.94 mm, respec- 20 3.37 4.73 7.1
tively. The microstructure of BMZ of the welded -20 4.81 1.6
specimen was just the same as that of the unwelded -SO 4$3 4.69 0
one. The microstructure of HAZ was nearly equal to C-DOPED- 80 2.50 4.63 52.1
that of BMZ. The tensile-test specimens were pulled ANNEALED 50 3.28 4.78 45.3
to fracture at a crosshead speed of 1 mm/min over 20 3.80 5.69 46.1
temperature ranges from -100 to 80C. -20 5.15 6.20 39.4
-50 5.98 7.71 14.8
Scanning electron microscopy @EM) was applied
-60 6.76 8.08 11.3
to determine the fracture mode of the specimen, -70 7.01 8.11 5.2
which was broken in the tensile test. Precipitates over -100 af 7.81 0
the grain boundary fracture surfaces were also ob-
served. a) Fractured within elastic limit.
 Y. H&a&z et al. /Lhrctility of ele~t~n-~ea~welded MO sheet 307

of EBW-ANNEALED is relatively small and is no

more than 10% even at 80C. In contrast C-DOPED-
EBW-ANNEALED shows a large increase in the elon-
gation compared with EBW-A~EALED. EBW-C-
DOPED (FZ, HAZ)-ANNEALED shows as small an
elongation as EBW-ANNEALED below 2OC, but it
shows as large a elongation as ~-DOPED-EBW-~-
NEALED above 50C.
Figs. 3 a-c show the elongation in FZ(e&,
HAZ(eHAz) and BMZ(en& as a function of tem-
perature. eFZ, eHAz and enMz are calculated by the
0. EBW-ANNEALED following equation
A. C.DOPED-EBW-ANNEALED

I
Pi = -Ii - lie x 100 , i = FZ, HAZ or BMZ , (11
01 f I
3 4 5 6 fl0
1/T tl?K)
where ei is the elongation in zone i, and Zioand li are
Fig. 1. Yieldstrength(ov) and fracture strength(of) VS. lengths of zone i before and after testing, respectively.
reciprocalof absolutetemperaturefor the weldedspecimens; In the case of EBW-ANNEALED (ftg_ 3a) eFZ, +A2
(01,(~1,(0) apply to uy and (01,(9, (~1to of. and enMZ are small and nearly of the same order. The
values of C-DOPED-EBW-ANNEALED (tig. 3b)
for the unwelded specimens. However, absolute values are nearly of the same order one another below -50%
of the strength of the welded specimens are smaller but eFz is larger than eHAz or enMZ above -20C.
than those of the unwelded ones. Locations of The absolute values of ei are much larger for this
fracture were at the center of FZ in the case of EBW- specimen than those for EBW-ANNEALED at any
ANNEALED and C-SPED-EBW-ANNEALED. On temperature. The results of EBW-C-DOPED (FZ,
rare occasions the former specimen fractured at the HAZ)-ANNEALED are a little different from above
boundary between FZ and HAZ. In the case of EBW- two specimens (see fig. 3c). eFz, eHA2 and enMz are
C-DOPED (FZ, HAZ)-ANNEALED locations of of the same order and are as small as those of EBW-
fracture were at BMZ below 20% while at the center ANNEALED below 20C. Above 50% however, these
of FZ above 50C. values rapidly increase and become comparable with
Total elongation of the welded specimens are those of C-DOPED-EBW-ANNEALED. This ten-
plotted against temperature in fig. 2. The elongation dency is in a manner similar to that of the total elon-
gation (see fig. 2).
eHAz and enMz are of the same order for each
specimen at any temperature. This result and the
microstructure of HAZ and BMZ shown in fig. 4 sug-
gests that HAZ and BMZ are almost equivalent both
mechanically and metallographically. And changes in
eHAZ or enM2 correspond well to those in eT*
Scanning electron micrographs of the welded
specimens, which were tested at -SOC, are shown in
fig. 5. EBW-ANNEALED shows a typical inter-
granular fracture mode and no precipitates are visible,
while C-DOPED-EBW-ANNEALED shows an almost
TEST TEMPEt7.4TURE ("9 cleavage fracture mode and fine carbide particles
Fig. 2. Total elongation(eT) vs. test temperature for the are recognized over grain boundary fracture surfaces.
weldedspecimens. EBW-C-DOPED (FZ, HAZ)-ANNEALED showed an
308 Y. Hiraoka et al. f Ductility of elec~on-berm-welded MO sheet

(a) E BW -ANNEALED
10

0
400 -50 0 50 100
TEST TEMPERATURE (C)

a (b)
I I I

7o _ C-DOPED -EBW-ANNEALED

0 FZ
60 - fi HA2
q BMZ
50-
2 //:
-._ 40 /

o,30 ._
(I,

20

10

0
-100 -50 0 50 100
TEST TEMPERATURE (*Cl TEST TEMPERATURE fc)

Fig. 3. Elongation in FZ (eFZ), HAZ &AZ) and BMZ (eg& for the welded specimens as a function of temperature; (a) EBW-
ANNEALED, (b) C-DOPED-EBW-ANNEALED, (c) EBW-C-DOPED (FZ, HAZ)-ANNEALED.

Fig. 4. Microstructure of the welded specimen (EBW-ANNEALED) illustrated on the photomicrograph.

 Y. Hiraoka et al /Ductility of electron-beam-weldedMOsheet 309

Fig. 5. Scanning electron micro~aphs of the welded specimen which is tested at -50C; (Ieft) EBW-ANNEALED, {right)
C-DOPED-EBW-ANNEALED.

~tergr~ul~ fracture mode similar to AS A~EALED,
although its micrograph is not shown here.
4. Discussion
With respect to the ductile-brittle transition
behavior, a model proposed by Wronski et al. [6] can
be adequately employed in the present work. This is
shown as follows:
T>T,, ON (-y) <UP > (2)
T<T,, oN>nP,
T=Tc, t&J(=$)=@3~C,
where uv is the yield strength and ON,up, UCand Tc
are the crack nucleation stress, crack propagation
stress, critical stress and the critical temperature,
respectively. According to these relations two param-
eters UCand Tc can be estimated by using the tensile
data. Tc was considered to be an expression of DBTT
in the present discussion.
In fig. 6 critical stress (UC)is plotted against reci-
procal of the absolute critical temperature (Tc) for the
unwelded and the welded specimens. The following
two suggestions can be reasonably accepted. One is
that the parameters uc and Tc for the welded speci-
men are characteristic values of FZ in the case of
EBW-ANNEALED or C-DOPED-EBW-ANNEALED,
and those of BMZ in the case of EBW-C-DOPED
(FZ, HAZ)-ANNEALED, considering the locations
(3) of fracture in these specimens at low temperature.
The other is that uc means up, the stress that propaga-
(4)
tes microcracks through grain boundaries and/or
matrices, at and around T = Tc, since the tempera-
ture dependence of up is relatively small at low tem-
perature from our previous work [2].
On the basis of these suggestions, the following
310 Y. Hiraoka et al. /Ductility
Tc (Cl
P--++?
l EBW-ANNEALED
10 - A C4OPED-EBW-ANNEALED
n EBW-~:;~~~~-ANNEALED
A The embrittlement of materials after welding
i
3 5-
b
b b
0 AS ANNFALEO
A C-DOPED -ANNt4LED
-3 4 5
l/Tc (dd)
Fig. 6. Critical stress (a~) vs. reciprocal of absolute critical
temperatureIT& for the unwelded and the welded speci-
mens.
conclusions are drawn from fig. 6. For the unwelded
specimens UC,i.e. up increases and Tc decreases, that
is, low-temperature ductility of the specimen is lm-
proved by a small amount of additional carbon. These
results are in good agreement with those of the bend
test [2]. For the welded specimens it is shown that a
small amount of pre-doped carbon also remains
effective on the improvement in the low-tempera-
ture ductility after welding and induces an enhance-
ment of up of FZ (comparing C-DOPED-EBW-
ANNEALED with EBW-~NEALED), This effect
seems to be associated with the increase of carbon
concentration on grain boundaries in a manner simi-
lar to for the unwelded specimens. UCand Tc of EBW-
C-DOPED (FZ, Hi)-~NEALED are just equal
to those of AS ANNEALED. This result is reason-
able, considering that uc and Tc show characteristic
values of BMZ whose microstructure is entirely the
same as that of AS ~NEALED.
The brittle fracture mode change from intergra-
nular to cleavage by a small amount of pre-doped
carbon can be explained by means of the enhance-
ment of up. For EBW-ANNEALED the inter~an~ar
crack propagation stress is much less than the trans-
granular one, i.e. cleavage fracture stress, thus crack
propagates mainly through~grain boundaries when
the applied stress reaches the fracture stress. For
C-DOPED-EBW-ANNEALED the intergranular
crack propagation stress increases and becomes com-
of Electra-beam-welded Mo sheet
parable with or larger than the cleavage fracture stress,
thus cracks propagate mainly through matrices. The
cleavage fracture stress is inherent and not so much
affected by the existence of in&tsions or precipitates
-
[73.
compared with the unwelded ones seems to result
from the directional coarse grain of FZ (see fig. 4).
Correlations between DBTT and grain size have been
investigated by several workers. A generally accepted
idea is that an increase of the grain size induces an
increase of DBTT f&9]. In contrast ThomIey et al.
6 [lo] suggested that DBTT did not change with
increasing grain size from 22-24 to 30&m, either by
~cre~g armealing temperature or by strain anneal-
ing. In the latter case, however, not only the change
in the grain size but also the different distribution of
carbon, oxygen or nitrogen atoms at grain boundaries
and in matrices followed by the heat treatment should
be considered. The effect of the directional grain of
FZ on UCor up is not certain in the present step.
The temperature dependences of ei (i = FZ, HAZ
or BMZ) and er can be interpreted by considering
the deformation behavior of the welded specimen as
follows. Figs. 7a rind 7b show eFz, eHAz and f?uMzaS
a function of elongation corresponding to the points
A, B, C or D in the nominal stress * -elongation
curves obtained for C-DOPED-EBW-ANNEALED
at -50C and 20C. It is shown that in the case where
the specimen is brittle (see fig. 7a), FZ, HAZ and BMZ
deform together until the applied nominal stress
reaches the maximum nominal stress (ah) and then
the specimen fractures at FZ. On the other hand, in
the case where the specimen is ductile (see fig. 7b),
FZ, HAZ and BMZ deform in the same way until the
applied normal stress reaches u& but after that FZ
only deforms, reduces in area and then fractures. The
m~um norn~~ stress (oh) was defined to be the
nominal stress corresponding to the fracture strength
in the former case and to the nominal stress corre-
* Nominal stress (CT+)is calculated by F/A0 (F is applied load
and A0 is primary cross-section area of the specimen). The
reason why not a true stress but a nominal stress is us& in
the present discussion is that the relation, which holds during
the deformation of a specimen composed of three zones f,2
and3,iso= UT = uf = us. u+ is the applied nominal stress
and ut (i = 1,2 or 3) is the nominal stress applied to zone i.
 I: Hiraok et al. /Ductility ~~eIect~~-cam-welded MO sheet 311

I I
(a) T = -50% (b) T: ZOC

0 FZ

.L.,L A
IO 0 5 lo 15
ELONG All0 N, e (1.)

Fig. 7. eFZ, effA~ and egMZ as a function of elongation corresponding to each point in the nominal stress-elongation curve for
C-DOPED-EBW-ANNEALED which is tested at (a) -50C and (b) at 20C.

sponding to the ultimate tensile strength in the latter from the enhancement of ok. These two effects are
case. At iow temperature c& corresponds to up. The both attributed to the enhancement of up of FZ.
values of u& for the unwelded and welded speci- The singular behavior in elongation for EBW-C-
mens are plotted against reciprocal of the absolute DOPED (FZ, HAZ)-ANNEALED is also interpreted
temperature in fig. 8. It is shown that u& for the by using fig. 8. At low temperature, the brittle frac-
welded specimen is smaller than that for the un-
welded one. A small amount of carbon induces a
remarkable increases in u&, particularIy at low tem-
perature for both unwelded and welded specimens.
In conclusion, total elongation of the welded speci-
men at a given temperature is determined by eFZ
before failure, and eH_&Zand eBMZcorresponding to
us of the welded specimen by the relation (I+= u& =
&AZ = uiMz. In table 2, the elongation in HAZ and
BMZ (eHAZ+BMz)estimated approximately in terms
of & of the welded specimen and the nominal stress-
elongation curve of the unwelded specimen, are
listed together with the experimental values of +AZ
0 AS ANNEALED
and +Mz. The estimated values are quantitatively a C-DOPED-ANNEALED
2-
in fairly good agreement with the experimental ones
* EBW-ANNEALEO
for EBW-ANNEALED or for C-DOPED-EBW-AN- l- . C-OOPEO-EBW-ANNEALED

NEALED. Thus the improvement in low-temperature

ductiiity of the welded specimen by a small amount
of pre-doped carbon can be explained by the follow-
ing two effects: one is the increase of eFz and the Fig. 8. Maximum nominal stress (oh) vs. temperature for the
other is the increase of e&+2 and eBMz that results unwelded and the welded specimens.
312 y. H&u&u et al. / hctility of e~e~t~n-beam-weided MO sheet

Table 2 following conclusions were drawn.

Estimated elongation in HAZ and BMZ (eHAZ+BMZ) and (1) A small amount of additional carbon remark-
experimental values ofeHAZ and eBMZ for the welded ably improved the low-temperature ductility of the
specimens (EBW-ANNEALED and C-DOPED-EBW-AN-
NEALED)
unwelded specimens. This result is consistent with
that of the bend test.
Specimen T Estimated Experimental (%) (2) A small amount of pre-doped carbon remains
(c) eHAZ+BMZ eHAZ eBMZ effective on the improvement of the low-tempera-
ture ductility after welding and changes the fracture
EBW-ANNEALED 80 12.1 11.7 9.0
3.0 2.2
mode from an intergranular type to a cleavage type.
50 2.8
20 2.1 3.0 2.5 These results can be reasonably explained by the
-20 0 1.5 0.3 enhancement of the brittle fracture stress cp of FZ
-50 0 0 0 by the increase of carbon concentration on grain
C-DOPED-EBW- 80 13.3 14.8 12.4 boundaries.
ANNEALED 50 13.5 15.1 13.5
20 13.6 14.8 13.0
-20 12.4 11.2 10.8 Acknowledgement
-50 11.1 .9.3 8.3
-60 5.3 6.8 5.1
-70 0 1.0 0 The authors wish to express their thanks to Mr.
F. Morito for his valuable discussion. Also they are
indebted to Dr. T. Suzuki for the chemical analysis
of carbon, oxygen and nitrogen contents and to Mr:
ture stress (oh or op) of C-DOPED-EBW-~- H. Irie for the electron-beam welding of molybdenum.
NEALED is much greater than that of AS ANNEALED.
This suggests that up of the carbon-doped FZ is
much greater than that of the undoped BMZ, thus References
EBW-C-DOPED (FZ, HAZ)-ANNEALED should
fail in BMZ rather than in FZ and have a small elon- [I] E. Kalns, Climax Report L-216-12 (1977).
gation. At high temperature, the maximum nominal [ 21 Y. Hiraoka, F. Morito, M. Okada and R. Watanabe,
3. Nucl. Mater. 78 (1978) 192.
stress is similar for C-DOPED-EBW-~NEALED
[3] W.N. Platte, WADC Technical Report 57-309 (1957).
and AS ANNEALED, and the carbon-doped FZ and [4] R.E. Monroe, N.E. Weare and D.C. Martin, Weld. J.
the undoped BMZ are both fairly ductile, thus FZ of 35 (1956) 488-s.
this specimen is expected to deform in a manner [S] N.E. Weare, R.E. Monroe and D.C. Martin, Weld. J.
similar to C-DOPED-EBW-ANNEALED and have 36 (1957) 291-s.
[6] A.S. Wronski, A.C. Chilton and E.M. Capron, Acta
as large an elongation as the latter material. In this Met. 7 (1969) 751.
case the specimen failed in FZ. [7] C. Crussard, R. Borione, J. Plateau, Y. Morillon and F.
Maratray, J. Iron Steel Inst. 183 (1956) 146.
[S j A.G. Ingram, J.W. Spretnak and H.R. Ogden, Trans.
5. Conclusion AIME 230 (1964) 1345.
[9] N. Aritomi and K. Tsuya, J. Jap. Inst. Metals 35
(1971) 662.
Tensile test was performed at low temperatures [ 10 ] J.C!. Thornley and A.S. Wronski, 3. Less-Common
for the unwelded and the welded sintered-molyb- Metals 21 (1970) 205.
denum sheet, in which carbon was doped or not. The