Journal

ofNuclear
Materials
103& 104(1981)621-632 621
North-HollandPubtishingCompany

CORROSION AND COMPATIBILI~ CONSIDE~TIONS OF LIQUID METALS FOR

FUSION REACTOR APPLICATIONS1

P. F, Tortorelli
Oak Ridge National Laboratory
Oak Ridge, Tennessee 37830

and

0. K. Chopra
Argonne National Laboratory
Argonne, Illinois 60439

The current understanding of corrosion and environmentaleffects on the integrity and

mechanical properties of structural materials used with liquid metals in fusion reae-
tors is reviewed. Corrosion processes in liquid lithium systems are examined and
their influence on material degradation is discussed. Compatibilityconsiderations
that might arise from use of molten lead, bismuth, lead-bismuth,or lead-lithiumare
reviewed relative to the possible use of these liquids in fusion reactors.

1. INTRODUCTION of the structural material result in mass trans-

Liquid metals have several possible applications
in fusion energy systems [If. Alkali.metals,
such as sodium and lithium, are efficient heat
transfer media because of their high thermal
conductivities,high heat capacities, and exten-
sive liquid temperature ranges. Also, the
production of tritium by reactions of both iso-
topes of lithium with fusion-producedneutrons
requires the use of some form of this alkali
metal in fusion reactors operating on the D-T
cycle. Lithium could therefore serve the dual
role of reactor coolant and tritium breeder.
Molten lithium-containingalloys, such as Pb-Li
or Li-Bi-Pb, can provide adequate tritium
breeding with a reduced lithium inventory since
the lead and/or bismuth would serve as neutron
multipliers. Finally, relatively low-melting
heavier metals, such as pure lead or bismuth,
may be used for neutron rmltiplicationin con-
junction with solid lithium compounds for
tritium breeding to assure an acceptable tritium
yield.
If liquid metals are used in fusion reactors,
compatibilitywith the containment alloy(s) will
be of prime concern. The structural material
must maintain its integrity under large tem-
perature gradients, severe thermal cycling, and
intense irradiation. In liquid-metalheat
transport systems, dissolution and redeposition
lResearch sponsored by the Office of Fusion
Energy, U.S. Department of Energy under
contract W-7405-eng-26 with the Union Carbide
Corporation and contract W-31-109-eng-38with
Argonne Universities Association and the
University of Chicago.
fer heat exchanger fouling, flow restrictions,
transfer of radioactive material, and related
problems. The compositionaland microstructural
changes due to selective dissolution and inter-
granular corrosion can lead to material failures.
This paper reviews the current understanding of
the corrosion and environmentaleffects on
fusion reactor structural materials associated
with the use of liquid metals and is primarily
concerned with chemical compatibilityand
influence on mechanical properties. Corrosion
processes in liquid lithium systems are
examined, and their influence on material degra-
dation is discussed. Compatibilityconcerns
arising from use of lead, bismuth, or lead-
lithium are also reviewed relative to fusion
applications.
2. CORROSION AND MASS TRANSFER
2.1 Background
The corrosion and mass transfer of containment
material can be deleterious in any application
of circulating liquid metals. Corrosion in the
form of dissolution, intergranularpenetration,
and interstitial transfer to and/or from the
liquid metal can result in significant wall
thinning and/or loss of mechanical integrity.
Just as important, the deposition of corrosion
products in cooler areas of a circuit may lead
to severe flow restrictionsand concentrated
radionuclide accumulation outside the reactor
core structure. The former consequence would
increase pumping power requirements and decrease
the energy conversion efficiency, and the latter
phenomenon would complicate maintaining the
system and would require extra shielding in the
deposition areas.

0022-3115/81/0000-0000/$02.75
0 1981North-Holland
622 p. I:. Tortorelli, 0. K. Cltopra
This section reviews our current understanding
of corrosion and mass transfer by liquid metals.
The principal processes that contribute to the
corrosion of materials by liquid metals are
dissolution, alloying, intergranular penetration,
impurity transfer from or to the liquid metal,
and thermal- and concentration-gradient mass
transfer. Given this variety of possible corro-
sion phenomena, we find that liquid metal corro-
sion depends on many variables. These include
the melt itself; its impurity content; the
composition, impurity content, and microstruc-
ture of the containment material; temperature;
exposure time; and, in flowing systems, flow
velocity, AT (difference in temperature across a
circuit), and temperature profile. Some of
these variables are more important in certain
combinations of containment material and liquid
metal than in others, and these distinctions
will be discussed.
This section emphasizes lithium because it is
the only low-melting metal that has been studied
in any detail. for fusion applications. Much of
the early lithium work, however, was done in
support of other programs and can be generally
characterized by high exposure temperatures,
variable impurity concentrations in the lithium,
and a greater variety of structural materials
(see, for example, the review by DeVan et al.
[21). In more recent years, lithium compati-
bility research has been focused to a greater
extent on steels and exposure temperatures
relevant to fusion program requirements.
2.2 Lithium
2.2.1 Corrosion in static systems
Corrosion tests in static lithium provide a
simple method for determining the basic interac-
tions between lithium and structural materials.
Recently, such experiments have defined the
influence of various impurities in lithium on
its compatibility with several steels.
Specifically, the corrosion of austenitic
stainless steels in static lithium is sensitive
to the nitrogen concentration of the lithium
1351. High nitrogen levels in lithium lead to
rapid general dissolution and intergranular
penetration. Furthermore, the nitrogen con-
centration may have a threshold value at which
the corrosion mechanism changes significantly,
leading to significantly increased corrosive
effects on steels f51.
Static tests have also been used in studying the
compatibility of ferritic (Fe-Cr-Mo) steels with
pure lithium. Recent studies 16-81 have shown
that the resistance of 2 l/4 Cr-1 MO steel to
attack and decarburization by lithium depends on
the steel's initial microstructure. A the grain boundary penetration of pure iron
2 l/4 Q-1 MO steel that contains relatively
unstable carbides (with respect to Li2C2), such
as Fe3C and s-carbide, was attacked by lithium
[71. However, when normalized and tempered to
produce more stable carbide phases, this alloy
/ Liquid metals fbr fkim reactor appkations
resisted corrosion by static lithium and it
decarburized significantly less 181. Carbon
loss to the lithium may be further reduced by
use of alloying additions to stabilize the car-
bide microstructure or by increasing the chro-
mium content of the steel. A 12 Cr-1 MO (wt %)
steel (HT9) resisted decarburization by static
lithium at 500°C [81.
The problem of interstitial transfer between
lithium and the containment material is per-
tinent to refractory and reactive metals as well
as to steels. Refractory metals and titanium
are attractive for fusion applications because
they have very low solubilities in lithium and
the former can be used at higher temperatures
than most metals and alloys. However, their
properties are very nmch affected by their
interstitial content, and the transfer of
interstitial impurities to or from these metals
when in contact with lithium is of concern.
Static tests can play an important role in con-
firming predictions of the thermodynamic
equilibrium partitioning of these interstitials.
Such calculations have been based on the known
free energies of formation of the respective
compounds and the solubilities of oxygen,
nitrogen, carbon, and hydrogen in lithium and in
the refractory and reactive metals [9,10].
Redistribution of oxygen from niobium, tantalum,
and vanadium is predicted in this way and has
been observed [ll-151. Recent measurements [16]
agreed well with predictions of nitrogen
transfer from lithium to vanadium at 6OO*C.
Experiments in static lithium have clearly
defined the importance of oxygen in the attack
of niobium by lithium [11,12]. In this case,
the concentration of oxygen and its disposition
in the refractory metal determine the severity
of the attack. As such, the corrosion mechanism
is similar to the abovementioned attack of
2 i/4 Cr-1 MO steel because in both cases
penetration is accompanied by the rapid transfer
of an interstitial (oxygen in the niobium, carbon
in the steel) to the lithium. Other experiments
have shown that oxygen in tantalum has a similar
effect on the attack of tantalum by molten
lithium [11--131. Small additions of zirconium
to niobium and of hafnium to tantalum have
suppressed the effect of interstitial oxygen on
lithium attack of the respective refractory
metals.
Static lithium studies have been used to deter-
mine possible effects of stress on corrosion.
The rate of grain boundary penetration of
austenitic stainless steel exposed to molten
lithium of unspecified purity increased when the
steel was stressed in tension during
exposure [171. Other work [18,19] showed that
exposed to static high-nitrogen 03000 wt ppmf
lithium increased with increasing stress and
that the creep rate of the iron probably con-
trolled the penetration rate. Stress effects on
corrosion of austenitic stainless steel were
 P.E. Tortorelli, 0. K. Chopra / Liquid metals for fusion reactor applications
greater in flowing than in static lithium [17].
Although the effect of stress on the corrosion
of structural materials in impure lithium is
well-documented, stress effects in "pure"
lithium are not yet resolved. Recent results
[20] have indicated no effect of stress (103 to
945 K?a) on corrosion of HT9 exposed to flowing
pure lithium (100-200 wt ppm N) for 1000 h at
482oc.
2.2.2 Mass transfer in circulating lithium
systems
Although corrosion tests in static lithium serve
an important purpose in identifying and charac-
terizing the various reactions between lithium
and containment materials, an understanding of
the corrosion and mass transfer of structural
alloys in flowing lithium is our ultimate goal.
Thermal-gradientmass transfer occurs in non-
isothermal systems because of the temperature
dependence of solubility. Therefore, the AZ'of
a system is very important in determining the
corrosion rate in a liquid metal. In general,
the mass transfer rate of element i, Ri, at a
particular temperature can be described as
R< = k(C, - Ci) , (1)
where
k = the rate constant of the rate-
controlling dissolution or deposi-
tion step,
c, = the solubility of element i in the
liquid metal, and
Ci = the actual concentration of i in the
liquid metal stream.
Generally Ci is relatively constant around the
liquid metal circuit, but Cs depends exponen-
tially on temperature. The relative magnitude
of C'sand Ci determines whether R; is positive
(dissolution)or negative (deposition). While
solubility is important in determining mass
transfer'rates (211, it alone is not sufficient
since the kinetics of the dissolution and depo-
sition reactions [as represented by k in
Eq. (l)] can profoundly influence the overall
rate of transfer [221.
The flow velocity of lithium or any other liquid
metal used in fusion applicationswill be deter-
mined by the metal's use in the reactor. A
fluid used solely for tritium breeding could be
semistagnant, but the use of a liquid metal as a
coolant requires high flow velocities. Since we
would expect that corrosion rates will increase
with velocity over a definite velocity range,
the magnitude and possibly the mechanism of mass
transfer will depend on the particular fusion
reactor design. Thermal-convectionloops (TCLs),
in which the temperature gradient induces flow
around a circuit, are appropriate for mass
623
transfer studies at low flow velocities typical
of semistagnant tritium-breedingblankets 1231.
Experiments at higher velocities require the use
of forced-convection(pumped) loops (FCLs),
which also allow the flow velocity to be varied
over a much wider range than possible with
TCLs [24].
Recent lithium TCL studies [23,25,261have
defined the mass transfer of type 316 stainless
steel as a function of exposure time and
temperature. Material is dissolved in the
hotter region of a loop and is subsequently
deposited in its cooler areas. Figure 1 shows a
characteristicmass transfer profile for type
316 stainless steel in flowing lithium [23].
The weight changes around such loops have been
studied as a function of time, and both dissolu-
tion and deposition rates reached steady-state
(that is, time-independent)values after an ini-
tial period (150~3000 h) characterized by
higher, rapidly changing rates (23,261. This
type of dependence is shown in Fig. 2. Since
the slope at any point along the curve in Fig. 2
is the instantaneousdissolution rate, this rate
eventually becomes constant with time. After
several thousand hours of exposure to flowing
lithium, the composition and structure of the
near-surface region of type 316 stainless steel
are quite different from those of the initial
alloy (see Fig. 3). The stainless steel surface
is preferentiallydepleted of nickel and, to a
lesser extent, chromium. The loss of nickel
destabilized the austenite and led to formation
of a ferrite layer. Experiments in nonisothermal
higher velocity lithium (FCLs) showed similar
dissolution behavior. Steady-state corrosion
rates were reached (241 after about 1000 h at
440 and 490°C, and loop specimens were depleted
in nickel and chromium after being exposed to
high-velocity lithium [24,27,29].-
80
I I I
. a
40 - l -
.
.
. l
.
600°C 525°C 1°C
4!50
1
-120/- l I
I 0
, :
I I
-160 1
0 0.50 1.00 1.50 2.00
DISTANCE FROM BOTTOMOF HOT LEC Iml
Figure 1 : Typical weight change profile for
type 316 stainless steel exposed to purified
lithium for 9000 h in a thermal-convectionloop.
From Ref. [23].
624 P.F. Tortorelli, 0. K. Chopra / Liquid metals for fusion reactor applicatims
120 /-
600°C /’
,’
co /’
/’
Figure 2 : Weight loss versus time at 600°C for
type 316 stainless steel in a pure lithium
thermal-convection loop.
Figure 3 : Type 316 stainless steel exposed
purified lithium for 8000 h in a thermal-
convection loop. From Ref. 1231.
The influence of nitrogen on corrosion by
flowing lithium has not been as well-
characterized as has its effect under static
conditions (see above). However, some evidence
shows that nitrogen can have a detrimental
effect. Results 1301 from a TCL that circulated
lithium between 593 and 871°C showed that an
increase in the nitrogen content of the lithium
from 125 to 370 wt ppm increased the rate of
mass transfer by 42%. Another study [31] indi-
cated that the overall mass transfer rate of
type 304 stainless steel was significantly
greater in air-contaminated lithium than in pure
lithium and that the contaminated lithium caused
preferential leaching of the chromium from the
steel [possibly due to Cr-Li3N reactions [32]
reducing Ci -see Eq. (l)l. This latter obser-
vation is consistent with the results from other
work [33], in which chromium was preferentially
leached from austenitic stainless steel in
unpurified lithium with unknown impurity
concentrations. Also, in this study type 316
stainless steel at 600°C dissolved about twice
as fast as reported [23] for measurements in
pure lithium. More recent experiments [29] have
shown a definite effect of nitrogen on the
dissolution rates of austenitic stainless steel
at 400°C, and, as described below in the mechan-
ical properties section, on corrosive penetration
of HT9 (12 wt % Cr-1 wt % MO steel) [34]. In
contrast, no effect of a higher initial nitrogen
concentration in lithium (500 wt ppm) was
observed in a type 316 stainless steel TCL
operating between 400 and 6OO'C [25].
The inconsistency of nitrogen effects reported
for flowing lithium compared with those for
static lithium could indicate that mass transfer
of chromium and nickel complicates the nitrogen
effects. More work is obviously required to
completely characterize the effect of high
nitrogen levels in flowing lithium on corrosion
and mass transfer.
As discussed above, the low solubilities of
refractory metals and titanium in lithium make
them attractive for use in flowing lithium.
With sufficiently low impurity levels in the
lithium and refractory metal, very little corro-
sion has been reported (16,351 for Nb, Ta, V, W,
Mo-C.5 wt % Ti, and V-15 wt % Cr in flowing
lithium at temperatures greater than those
usually considered for fusion applications. If
the oxygen concentration of the niobium is
allowed to rise above a threshold concentration
(-200 wt ppm), then severe attack of the
niobium, such as occurs in static lithium
tests [11,12], is observed in flowing lithium
systems [351. This problem may be eliminated by
assuring a consistently low concentration of
oxygen in the metal or by adding zirconium to
the niobium [11,35]. When the niobium-zirconium
to alloy is properly heat-treated, the zirconium
acts as an "internal getter" and raises the
effective threshold oxygen concentration for the
onset of attack. Experiments [35,36] with
lithium loops of niobium alloyed with 1 to
5 wt % Zr have shown that these alloys are com-
patible with flowing lithium, although some mass
transfer of zirconium has been observed at 1000°C
and above [36].
Although deposition of corrosion products is an
important consideration in assessing the use-
fulness of any liquid metal circuit, it has not
been studied in as arch detail as dissolution.
Deposition in lithium-type 316 stainless steel
TCLs was time-dependent [261. As with
dissolution [231, the deposition rate decreased
with time until a steady state was reached. The
composition of the TCL mass transfer deposits
also varied with operating time [26]. The
deposits were initially pure chromium but
gradually incorporated significant concentrations
of iron and nickel. Somewhat different behavior
has been reported for FCL systems. Iron
crystals with a few chromium-rich deposits were
reported for one FCL experiment [29], whereas
 P. F. Tortorelli, 0. K. Chopra / Liquid metals for fusion reactor applications 625

iron and iron-manganese deposits have been found

in other FCLs [37,38]. The reason for the
differences in the nature of the deposits is
unknown, although the iron deposits were found
in experiments using lithium with somewhat
higher nitrogen concentrations. Also, FCLs may
provide magnetic traps for dissolved iron and

I
manganese; preferential deposition has been *(0.02) (2.21,
observed in electromagnetic pump ducts [37,38]
and magnetic flowmeter tubing [37]. Therefore, (i.811
TCL experiments, which are free from the effects \
O(O.02) (0.5)
of magnetic fields, appear to yield different
deposition results. (0.21A -

Because of the many variables - temperature,

nitrogen concentration of the lithium, AT, etc. l(+.o)
- it is difficult to compile a definitive data (4$
set of measured corrosion rates in lithium for a

particular fusion application. The most
complete data for any alloy, under relevant
conditions, are the measurements for type 316
stainless steel, but any data correlation suf-
fers from the varied conditions of the different
experiments. Under the semistagnant condition
typical of TCLs, dissolution rates from 10 to
30 mg/(m"h) have recently been reported for
6OO'C exposures [23,33]. The data from FCL
tests vary over a broader range. Figure 4 is a
compilation of applicable data and shows this
scatter. (The plot and the slope of the
arbitrarily drawn line are based on the assump-
tion of an Arrhenius temperature dependence for
the dissolution rate [23]). As indicated in
Fig. 4, some of the variance in the data can be
related to the respective nitrogen concentrations
of the lithium. Ihe inverse temperature depend-
ence found in one study [24] was attributed to
the sluggishness of the austenite-ferrite trans-
formation at the lower temperature. The data in
Fig. 4 and additional results from FCL studies
[24,27,29] show a definite dependence of the
corrosion rate on flow velocity. In particular,
measurements of corrosion rates as a function of
velocity t241 indicated that fluid mechanics
played a major role in determining the corrosion
rate of type 316 stainless steel by lithium.
Additionally, a TCL study [231 yielded an acti-
vation energy for dissolution that was indicative
of rate control by liquid-phase diffusion, which
would be consistent with a velocity-dependent
corrosion rate. Magnetohydrodynamic effects
arising from lithium flowing in the magnetic
fields of a fusion reactor currently constitute
an unknown factor but may influence corrosion.
Such possibilities have recently been
discussed [39].
Even less corrosion data relevant to fusion con-
ditions are available for other alloys and
metals in lithium. However, from our present
understanding of lithium corrosion, we can spec-
ulate on the relative resistance of various
materials to mass transfer in lithium. The
preferential depletion of nickel from austenitic
stainless steel exposed to flowing lithium
strongly indicates that reducing the nickel con-
centration of an alloy would improve corrosion
1
-1
\
,001 I I
4.o i.2 4.4 1.6
l/T (A0-3 K)
Figure 4 : Arrhenius plot of corrosion rate
data for type 316 stainless steel exposed to
flowing lithium. Numbers in parentheses repre-
sent flow velocities in m/s. Open symbols are
data from thermal-convection loops; rest of data
is from forced-convection loops.
resistance. Indeed, a recent study using
TCLs (401 showed that the mass transfer rate at
500°C was proportional to the initial nickel
concentration for alloys containing between 10
and 30 wt % Ni. Other work [41] in flowing
lithium indicated that although higher nickel
(40 and 52 wt %) alloys are corroded more than
type 316 stainless steel, the degradation is not
a simple function of the nickel content at these
concentrations. These results would lead us to
expect that an Fe-Cr-Mo alloy such as
2 l/4 Cr-1 MO steel or HT9 [12 Cr-1 MO (wt %)I
would have better resistance to corrosion by
lithium than an austenitic stainless steel.
However, after a transient period, the steady-
state dissolution rates of austenitic and
ferritic steels should be approximately equal
since, as described above, a nickel-depleted
ferritic surface forms on the austenitic steel
and at steady state would be similar in surface
composition to that of Fe-Cr-Mo alloys similarly
exposed. The total amount of material removed
will still be greater for the austenitic steel
because of its higher initial corrosion rate,
and this could lead to earlier flow restriction
by mass transfer deposits.
Currently available data indicate that corrosion
rates of austenitic and ferritic steels would
probably be acceptable (<15 pm/year) for service
below 45O-500°C in pure lithium, particularly at
low flow velocities. The higher strength, higher
626 RF. Tortorelli, 0. K. Chopra / Liquid metals for fusion reactor uppliratiws
nickel alloys are more corroded in lithium and
thus are unacceptable for use in lithium at such
temperatures unless an effective corrosion inhi-
bition technique could be employed (see below).
If impurity levels are controlled, the refractory
metals and titanium (t5OO"C) would be the best
materials in terms of corrosion resistance to
lithium.
2.2.3 Corrosion inhibition in lithium systems
The development of techniques to inhibit corro-
sion by lithium may help to reduce the extent of
mass transfer and possibly allow the use of an
alloy that would otherwise be unsuitable for
lithium service. Aluminized layers formed by
additions of aluminum to lithium have been
found [42] to reduce corrosion of alloy 600
176 ~i-8 Fe-16 Cr (wt %>] in static lithium and
to decrease the mass transfer of type 316
stainless steel in flowing lithium by a factor
of 5. Work with preformed commercially prepared
aluminide diffusion surface coatings 1411 showed
that such coatings reduced the attack of high-
nickel alloys by flowing lithium at 400°C. At
this low temperature,however, no real benefit
of the aluminide coatings was found for type 316
stainless and ferritic steels [41]. In fact,
aluminization of ferritic steels may adversely
affect their mechanical properties during expo-
sure to lithium 18,411. Nickel-bearingalloys
with adherent coatings of MO, Mo-Ti, and Al
(applied from a molten sodium solution) were
resistant to corrosive attack by flowing lithium
at temperatures up to 900°C 1431. Furthermore,
the addition of aluminum to static nitrogen-
contaminated lithium decreased the corrosive-
nesa [44]. Therefore, effective corrosion
inhibition in lithium systems can be realized
from using mechanically stable surfaces composed
of elements or intermetalliccompounds that
resist solution in lithium.
2.3 Bismuth and Lead
As noted above, molten bismuth, lead, or lead-
bismuth may be used for neutron multiplication
in conjunction with a solid tritium-breeding
material. Such liquid metals might be used in a
semistagnant condition, with flow simply arising
from relatively small temperature gradients
across the melts. Much of the experimentalwork
on corrosion by these liquid metals is over 20
years old and is not directly relevant to fusion
applications. This review will therefore
address the general materials considerationsfor
corrosion by bismuth, lead, and lead-bismuth.
Bismuth is very aggressive toward iron-base
alloys 145-691. Measurements of corrosion rates
of selected iron-base alloys in bismuth TCLs f47]
are shown in Table 1. These rates are much
greater than those that would be measured in
pure lithium under similar conditions. For
example, although the dissolution rate of
18 Cr-8 Ni fwt X) stainless steel in a bismuth
TCL with a maxirmm temperature of 700°C was
reported [47] as 25 x lo3 mg/(m2'h), the rate
for a similar steel in a lithium TCL with a
maximum temperature of 650°C was 17 mg/(m2'h)
]25]. In general, increasing the nickel and/or
manganese contents of containment alloys results
in significant increases in their corrosion
rates in bismuth [47]. For ferritic steels,
corrosion increased with an increase in chromium
content but was reduced by increased carbon
concentrations [4+47]. As with other liquid
metals, corrosion by bismuth was accelerated by
increases in maximum loop temperature and the
temperature differential of the loop [45,46].
Certain refractory metals were corrosion-
resistant to bismuth at temperatures up to 7OO'C
(with a AZ' of lOO*C): MO, Ta-8 wt % W-2 wt % hf,
and Ta-lo wt % W [47,49]. Niobium, on the other
hand, was not compatible with bismuth at the
temperatures investigated (27OO'C) ]49,50].
The unacceptably high corrosion rates of iron-
base alloys in bismuth can be reduced by
inhibitor techniques. The most effective method
is the addition of zirconium 0100 ppm) to the
bismuth [45-481, which results in substantially
lower mass transfer rates (see Table 1). The
zirconium in the bismuth inhibits the corrosion
of steels by surface reaction with nitrogen and,
possibly, carbon to form inert surface layers of
ZrN and ZrC 145,461. Factors influencing the
nitrogen and carbon activities and distributions
affect the inhibition and, therefore, the corro-
sion resistance of steel in bismuth ]45]. The
ZrN may spa11 [45,48], but increasing the nitro-
gen concentration in the steel can possibly
reduce spallation 146,481.
Table 1. Corrosion rate of steels in
in Bismutha
Corrosion Rate (g/m2*h)
Tmax = 700°C, AT = 50°C
Steel
Bi+MgC Bi f Mgc + Zr
Mild steel 12.1 <O.l
2 l/4 Cr-1 MO 16.5 1.9
13 Cr 17.7 5.2
18 Cr-8 Ni 24.8 5.2
aFrom Ref. [47].
&ajor alloy additions are listed
(nominal wt 4).
OMg is added to control the oxygen
activity in the Bi.
Although lead can also be quite corrosive
[46,47,51-531, it is not as aggressive as pure
bismuth [46,471. Corrosion experiments with
lead [52] have indicated a qualitative rela-
tionship between the solubility of the alloy in
the lead and the attack by lead. Because of the
large solubility of nickel in lead [54], nickel
and some nickel-rich alloys are readily corroded
[51,521. However, intermetallic compound for-
mation in some of these alloys can give a con-
 P. F. Tortorelli, 0. K. Chopra /Liquid
metals offer excellent corrosion resistance [Sl].
In addition, an oxide film on ferrous alloys can
give protection against lead attack [52,53] and
has been suggested [52] as a reason why some data
indicated lower than expected corrosion rates.
Alloys that form oxide films at low oxidizing
potentials (such as those containing aluminum)
are relatively more resistant to lead corrosion.
As with bismuth, an additive (titanium) to lead
has been effective in inhibiting corrosion
[47,48,52]. One study [47] indicated that the
corrosion rate of steel exposed to inhibited
lead is about that of steel in inhibited
bismuth. This would therefore suggest a similar
protective film of TIC or TIN [47]. The use of
coatings for lead corrosion protection has not
been very successful (because of adherence
problems) with the exception of plasma-sprayed
molybdenum on 2 l/4 Cr-1 Mo steel and aluminized
specimens of the same steel [52]. In the former
case, protection was afforded by the high corro-
sion resistance of molybdenum, and in the latter
it was probably provided by formation of protec-
tive oxide films as described above.
From corrosion considerations, lead would be
preferable to bismuth for a neutron multiplier.
Its use would probably be limited to relatively
low temperatures (350-4OO'C) in a nearly static
condition (small AT) with ferrous alloys of low
nickel and chromium activity. Inhibition tech-
niques (additions of about 500 ppm Ti to lead or
100 ppm Zr to bismuth) could be implemented to
raise the temperature limits. The limited
amount of work done on corrosion by lead-bismuth
alloys [46,551 indicates that the same con-
siderations apply to their use and that the
solvent properties are bewteen those of lead and
bismuth [46].
2.4 Lead-Lithium
Lead-lithium alloys are possible candidates for
the tritium-breeding, cooling, and/or neutron
multiplying functions in fusion reactors. Such
alloys are less reactive with water and air than
pure lithium and therefore present less risk
under accident conditions. Additionally, the
lead provides neutron multiplication that en-
hances the tritium yield from the reduced lithium
inventory. Relatively little work has been done
on its corrosivity, however. Recent experi-
ments [56] with static Pb-17 at. % Li (which is
the lowest melting composition) have shown that
type 316 stainless steel was dissolved at 500°C
at rates substantially greater than the negli-
gible rates measured for similar exposures to
pure lithium. In this sense, this lead-rich
solution acts like pure lead. Other work [7,57]
has shown that, as for pure lithium, the extent
of penetration of 2 l/4 Cr-1 MO steel exposed to
liquid lead-lithium depends on the steel's
microstructure for alloys containing up to
3.6 at. % Pb and that the presence of up to this
much lead did not nmrkedly affect the mechanism
by which liquid lithium attacks the steel. The
metals for fusion reactor applications 621
untempered bainitic microstructure of
2 l/4 Cr-1 Mo steel was highly susceptible to
intergranular penetration by solutions of up to
3.6 at. % Pb in lithium, but tempering the steel
effectively prevented significant attack.
However, a higher lead alloy, Pb-17 at. % Li,
did not penetrate 2 l/4 Cr-1 MO steel regardless
of its initial microstructure [571. Although
more work in this area is obviously required,
preliminary results indicate that corrosion of
structural materials exposed to lead-lithium
will be related to corrosive attack by lithium
when the melts are predominately lithium and to
pure lead corrosion when the ratio of lead to
lithium atoms is high.
3. ENVIRONMENTAL EFFECTS ON MECHANICAL
PROPERTIES
The corrosive action of liquid metals can
substantially degrade the mechanical properties
of structural materials. To understand the
influences of the liquid metal environment on
the mechanical behavior of materials, it is
important to examine the nature of the effects.
Environmental effects can be divided into two
classes: the influence of the environment
itself and the effects of microstructural and
compositional changes that occur in the material
during the long-term exposure to the environment.
Liquid metal environments can influence the pro-
cesses at a free surface and thereby affect the
surface-active properties of the material. For
example, processes such as liquid metal
embrittlement, oxidation, and carburization can
change the mode and rate of crack propagation
and change the ductility or fatigue life of the
material. On the other hand, long exposures of
the material to liquid metals change its bulk
properties. Processes such as substitutional or
interstitial element transfer, grain boundary
penetration, and thermal aging can weaken the
material and affect mechanical properties.
Factors that aggravate corrosion or aging pro-
cesses (for example, temperature, impurities in
the environment, and mass transfer) cause a
significant deterioration in the mechanical
properties of materials.
This section reviews the data on mechanical
properties of structural materials in liquid
metal environments that are of interest for
fusion reactor applications (specifically,
lithium, bismuth, lead, and lead-bismuth). The
significance of various test and environmental
parameters is discussed.
3.1 Lithium Environment
Information on the effect of a lithium environ-
ment on the mechanical properties of materials
is limited. Most of the data on environmental
effects in lithium have been obtained by con-
ducting tensile tests in argon on tube specimens
filled with lithium [17,58]. Control tests were
performed either in vacuum or in argon. The
effects of lithium on the ultimate tensile
628 P E Tortorelli, 0. K. Clropra / Liquid metals fbr fusion reactor upplicatiom
strength (UTS) and ductility of the material
have been determined as a function of temper-
ature, strain rate, and purity of lithium.
Between 200 and 800°C, the strength and, most
particularly, the ductility of Armco iron in
lithium were considerably lower than in vacuum
[581. Test specimens showed evidence of grain
boundary penetration. The degree of weakening
of the grain boundaries depended on temperature
and strain rate. The tensile strength of
Fe-18 Cr-10 Ni (wt. %) stainless steel tested at
200 to 1000°C was not significantly affected by
lithium [17]. The effect of lithium on ductility
depended on strain rate and temperature. The
effect is negligible at a strain rate of
2.7 X 1(r3/s, but at 4 X 1e5/s the elongation
is noticeably reduced above 300°C.
The influence of lithium exposure on room-
temperature tensile properties of stainless and
low-alloy steels depends primarily on the extent
of the various corrosion phenomena, such as
selective leaching of substitutional elements,
interstitial element transfer, and grain bound-
ary penetration [8,17,59]. Factors that
increase corrosion significantly reduce tensile
strength. For example, preexposure of HT9 to
static lithium at 500°C had no significant
effect on tensile strength, but that of low-alloy
2 l/4 Cr-1 MO steel exposed to lithium at 500 to
600°C was reduced because of decarburization
181. Tensile properties of Fe-18 Cr-9 Ni (wt %)
steel exposed to stagnant lithium did not change
significantly, but specimens exposed to flowing
lithium suffered sharp reductions in tensile
strength [17].
The creep strength also was affected by lithium
exposure [17,58]. The time to rupture of Armco
iron in 400°C lithium was five to six orders of
magnitude smaller than that in argon. The
CYCLES TO FAILURE.N(
effect of lithium was greatly reduced at higher
temperatures. The creep strength of austenitic
stainless steel tested at 700°C in a flowing
lithium TCL was significantly lower than that in
static lithium or in argon [17]. The long-term
creep strength of austenitic stainless steel at
7OO'C in filtered lithium or lithium contaminated
with 1 wt % N or 0 was not significantly dif-
ferent from that in argon. These results are
surprising in that nitrogen can increase corro-
sion of stainless steels (see above). However,
the concentration of nitrogen in the filtered
lithium samples was not specified for these
tests. It could have been sufficiently high
that further addition of 1% N had no effect.
The significance of corrosion processes on the
degradation of mechanical properties of materials
has been demonstrated by use of a diffusion
coating on the metal surface to eliminate direct
metal-lithium contact and thereby inhibit corro-
sion and its effect on strength [43,601.
The influence of a lithium environment on the
fatigue properties has recently been investi-
gated in an FCL with lithium of controlled
purity [341. The low-cycle fatigue properties
of HT9 alloy and type 304 stainless steel were
strongly influenced by the concentration of
nitrogen in the lithium. Fatigue-life data for
HT9 tested at 482°C in lithium containing dif-
ferent levels of nitrogen are shown in Fig. 5.
The fatigue life of HT9 alloy in lithium con-
taining 1000 to 1500 wt ppm N was a factor of 2
to 5 lower than that in lithium with 100 to 200
wt ppm N. The fatigue life in low-nitrogen
lithium was not significantly different from
that in sodium. Increased corrosion due to high
nitrogen content in lithium was reflected in the
fracture mode; specimens tested in high-nitrogen
lithium showed intergranular fracture and grain-
boundary cracks on the surface [34].
 P.F. Tortorelli, 0. K. Chopra / Liquid metals for fusion reactor applications
The effects of corrosion on fatigue crack growth
rates of steels in a static lithium environment
have also been studied. At high nitrogen con-
centrations in the lithium, over the frequency
range of 0.067 to 20 Hz, the fatigue crack
growth rates of prenotched samples of type 304L
stainless steel at 7OO“C and 2 l/4 Cr-1 MO steel
at 5OO'C were greater than those in argon
[61-631. For 2 l/4 Cr-1 Mo steel, the crack
propagation rate was greater at higher fre-
quencies. The effect of this type of lithium
environment was reflected in the observed
intergranular fracture at all frequencies for
type 304L stainless steel and at low frequencies
for 2 l/4 Cr-1 MO steel. At higher frequencies
the fracture of the 2 l/4 Cr-1 MO steel was
transgranular with cleavage facets. These
results indicate that liquid lithium may cause
embrittlement under certain material and test
conditions, such as high nitrogen levels, high
cyclic frequencies, and stress risers. However,
these effects appear to be associated with
increased grain boundary corrosion or selective
attack along preferred crystallographic planes
rather than with surface-active processes
relating to classic liquid metal embrittlement.
3.2 Lead, Bismuth, and Lead-Bismuth Environments
The embrittlement of materials under the
influence of surface-active liquid metals has
been the subject of several investigations.
Armco iron and low-alloy steels wetted with
lead, bismuth, or lead-bismuth eutectic severely
lost ductility between 200 and 4OO'C [66-66].
The tensile strength also decreased continuously
and reached a minimum at 400°C. The largest
drop of ductility was observed at approximately
350°C. Specimens exposed to embrittling metals
failed as a result of the growth of a brittle
crack, whereas in an inert environment they
failed by ductile fracture. The temperature
range for embrittlement extends considerably
below the melting point of the melt and is
related to the temperature interval of reduced
plasticity or "blue brittleness" of specimens
tested in vacuum. Stress relaxation in this
temperature range is inhibited and thus promotes
strain hardening, which is more pronounced in
specimens deformed in liquid metals [64,67].
The influence of lead-bismuth eutectic environ-
ment on the fatigue strength of ferritic and
austenitic steels has been investigated at tem-
peratures between 300 and 600°C [68,69]. The
fatigue strength of various grades of steels
when wetted by molten lead-bismuth eutectic was
substantially reduced by penetration of the
liquid metal along the grain boundaries. The
deleterious effects of liquid lead-bismuth
eutectic can be prevented by the formation of an
oxide film on the steel surface, which, if
maintained, inhibits the wetting of the steel by
the liquid metal. 'Ihe weakening effect of lead-
bismuth eutectic can also be eliminated by
controlling the cyclic frequency. The fatigue
life of low-alloy steel tested in liquid lead-
bismuth at a strain rate of 8.0 X 10-6/s was
629
about the same as that in air, but a drastic
reduction in fatigue strength was observed at a
strain rate of 5.3 X 1(r3/s t70,711. The
reverse strain-rate effect in liquid metals is
explained by accelerated grain boundary dif-
fusion of liquid metal under high cyclic
stresses. The absence of the harmful effects at
slow strain rates is associated with the relax-
ation of local stresses such that conditions
conducive to grain-boundary diffusion by the
liquid metal cannot be produced.
4. SUMMARY
Materials compatibility considerations for the
uses of liquid metals in fusion reactors have
been reviewed. Most of the fusion-relevant com-
patibility research has been lithium-related, so
the effects of a lithium environment are
discussed in the most detail.
Corrosion by liquid lithium may take several
forms and may include dissolution, grain bound-
ary penetration, and interstitial and mass
transfer. These processes primarily involve
bulk phenomena. Sufficiently high nitrogen
levels in lithium will increase corrosivity to
ferrous alloys and have a deleterious effect on
fatigue resistance. Although more work is
required to define corrosion processes in
lithium, it appears that applications of ferrous
alloys exposed to pure lithium will probably be
limited to service temperatures of 450 to 500°C
by mass transfer and deposition effects.
Corrosion inhibition by aluminized layers can
reduce the corrosion of certain alloys by
lithium and raise the effective service tem-
perature limits. Most of the data on the
effects of a lithium environment on mechanical
properties have been obtained in static lithium.
Further mechanical tests in flowing lithium of
controlled purity are required to definitively
establish the influence of test and environ-
mental variables on mechanical properties.
Corrosion of ferrous alloys by heavier molten
metals (Pb, Bi, Pb-Bi, Pb-Li) can be severe,
although inhibition techniques are available.
Corrosion considerations would favor lead or
lead-bismuth over bismuth for use as a neutron
multiplier. The corrosivity of lead-lithium
depends on the relative amounts of lead and
lithium. Use of heavier metals may signifi-
cantly affect the mechanical properties of the
containment materials. Data on corrosion by
these liquid metals under fusion-related con-
ditions are needed.
In the absence of impurity effects, refractory
metals are, in most cases, the most resistant
materials to corrosion by liquid metals.
ACKNOWLEDGMENTS
The authors thank .I. H. DeVan and F. W. Wiffen
for reviewing the manuscript, S. Peterson for
editing, and K. L. Perry and A. J. Carter for
report preparation.
630 P.F.Tortorelli,
O.K.Chopra/ Liquidmetalsforfusion
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