Niobium Additions in HP Heat-Resistant Cast

Stainless Steels
Gloria Dulce de Almeida Soares,* Luiz Henrique de Almeida,*
Tito Luiz da Silveira, *t and Iain Le May *~
*COPPE/UFRJ, P.O. Box 68505, 21945 Rio de Janeiro, RJ, Brazil; *Faculdade de Engenharia
Souza Marques, Rio de Janeiro, Brazil; and ~:Metallurgical Consulting Services Ltd., Saskatoon,
Canada

The microstructures of HP-type heat-resistant cast steels, having niobium additions up

to 2 wt.%, were examined in the as-cast condition and after artificial aging at 700, 900,
and ll00°C. Microstructural studies were conducted using scanning transmission electron
microscopy and x-ray diffraction. Instability of NbC between 700 and 1000°C occurs in
these alloys, with partial tranformation to a nickel-niobium silicide, G phase. A time-
temperature-transformation diagram has been constructed for the 1.97% Nb alloy. Creep
tests were made on the as-cast and aged material. Niobium containing alloys aged at 700
and 900°C display superior creep properties to those of the as-cast material or material
aged at 1100°C. The results of the creep tests have been related to the microstructuraI
changes taking place upon aging.

INTRODUCTION [4]. Moreover, there has not been a sys-

Improvements in the performance of heat-
resistant centrifugally cast stainless steels
have been made primarily through the ad-
dition of carbide-forming elements and
from the analysis of their creep behavior.
The new generation of this type of steel,
used as radiant tubes in pyrolysis and re-
former furnaces, shows improved creep
behavior in comparison with that of the
traditional steels [1-3]. However, the char-
acterization of the microstructure of such
steels and the relationship between mi-
crostructure and mechanical properties are
still not completely understood. Little has
been published concerning the balance of
the basic composition, e.g., the effect of
excess chromium in solid solution caused
by the consumption of carbon by the
stronger carbide formers has not been dis-
cussed extensively, although some effects
have been reported by the present authors
387
tematic study of phase characterization
and of the stability of phases over temper-
ature ranges for material in the aged con-
dition. Only recently, the Ni-Nb-Si inter-
metallic G phase was reported in a heat-
resistant cast steel exposed to long-term
service at high temperature [5].
In this study, the structural stability of
niobium-alloyed HP cast steel has been in-
vestigated. The alloys were produced in a
vacuum induction furnace, and the level
of total chromium was decreased as the
niobium content was increased. The
changes in microstructure as a result of
aging at different temperatures have been
examined, and the effect of niobium ad-
ditions on the microstructural changes has
been studied. Creep tests have been con-
ducted and the results interpreted :aking
the observed microstructures into consid-
eration. Initial observations of the micro-
structures of as-cast steel and of steel aged

<~Elsevier Science Publishing Co., Inc., 1992 MAFERIALS CHARACI ERIZA l'lOX 2Y:Bg7 3o6 (19~)E)
t~55 A v e n u e of the Americas, New York, NY 10010 1044 5~03 92 S5 (10
388
at 900°C have been presented previously
by the authors [4].
BIBLIOGRAPHIC REVIEW
The development of improved heat-resis-
tant cast austenitic steels has been accom-
plished by the addition of stronger carbide
formers such as niobium and titanium.
This is the case for modified HK and mod-
ified HP steels, which have been used in
petrochemical furnaces, mainly in the form
of centrifugally cast tubes.
The basic HP composition, without niob-
ium or titanium additions, exhibits the typ-
ical microstructure of an as-cast heat-resis-
tant steel, consisting of an austenite matrix
surrounded by carbides, mainly in inter-
dendritic orientation. In this alloy the pri-
mary carbides have been identified as
chromium carbides of Cr7C3 type [4]. The
stronger carbide-forming elements pro-
duce microstructural modifications other
than the partial replacement of the chro-
mium carbide. A characteristic feature
caused by addition of niobium is fragmen-
tation of the primary carbide network, the
effect increasing with increase in niobium
content. This fragmentation is reported to
be responsible for minimizing creep crack
growth at the carbide/matrix interfaces [1,
5]. In as-cast steel, the niobium additions
also cause modification of the stoichiom-
etry of the chromium carbides, these pass-
ing from M7C3 tO M23C6 type, as the quan-
tity of niobium increases.
Exposure of such heat-resistant cast
steels to high temperature leads to second-
ary precipitation, and the addition of niob-
ium delays the coarsening of the secondary
precipitation, the precipitates remaining
finer and less coalesced when compared
with those of the basic HP steel [4].
Transformation of NbC to a nickel-niob-
ium silicide has been reported in wrought
low-carbon stainless steel [6, 7] and in
heat-resistant centrifugally cast steel [5].
This silicide, usually of composition
Ni16Nb6Si7 (G phase), was detected in as-
sociation with chromium carbide particles,
G. D. de Almeida Soares et al.
which are thought to precipitate as a result
of carbon expelled by the NbC ~ G trans-
formation [5, 6]. The G phase does not ap-
pear to be detrimental to the mechanical
properties of the steel, and some authors
report that it is more deformable than is
niobium carbide [7]. Many particles of the
complex nickel-niobium silicide were iden-
tified in an HK niobium-modified cast tube
that had operated for more than 60,000
hours at a temperature of 900°C, strength-
ening the idea that such precipitates are
not necessary deleterious [5].
MATERIALS A N D EXPERIMENTAL
PROCEDURE
Table 1 shows the chemical composition of
the four experimental heats. Control of the
content of gases and residual elements was
also conducted, and their levels are shown
in Table 2: their concentrations are well
below the requirements of the project. The
chemical balance used to define the alloys'
composition has been described by Bar-
babela [8].
The alloys were subjected to exposure
for 1000 hours at temperatures of 700, 900,
and 1100°C. These values were chosen be-
cause they are, respectively, close to the
temperature of the cold region, the service
temperature, and the maximum tempera-
ture in petrochemical furnaces of the type
in which they would be used.
The phases precipitated after aging were
identified using scanning transmission
electron microscopy, energy dispersive x-
Table 1 Chemical Composition of
Experimental Alloys
Composition (wt. %)
Alloy C Ni Cr Mn Si Nb
A 0.43 32.6 26.0 0.92 1.81 - -
B 0.43 33.8 24.3 1.11 1 . 7 1 0.69
C 0.39 33.4 22.3 1.11 1 . 8 0 1.23
D 0.39 32.6 20.4 0.97 1 . 6 3 1.97
Niobium Additions in HP Steels
Table 2 Concentration of Gases and Residual
Elements in the Experimental Alloys
(Mean Values)
Element ppm
H 4
O 245
N 115
S 40
P <20
Pb 100
Bi <10
Cu 22
Cd 3 ture. On the other hand, the niobium car-
Sn <10
Sb <10
ray (EDX) analysis, and x-ray diffraction of
extracted residues. Thin foils were pre-
pared in a jet polishing unit using a 10%
HC1-H20 solution. The final polish was
made using electrolytic polishing with a
perchloric/glycerol/ethanol solution (10/20/
70) at 16V d.c. and 10°C. The residues ex-
tracted using Berzelius' solution were
mounted on a copper grid covered with a
Formvar film for examination by scanning
transmission electron microscopy.
Creep tests were made on the as-cast al-
loys and on material aged for 1000 hours.
Tests were run at 925°C at a stress of 45
MPa.
Additional aging treatments were made
on Alloy D (1.97% Nb) to define the NbC
G phase transformation curve over the
temperature range 700-1100°C, for a range
of times. The transformations were moni-
tored by means of x-ray diffraction of ex-
tracted residues, the 0.198nm interplanar
spacing on the spectra being used to char-
acterize the presence of G phase.
RESULTS
MICROSTRUCTURAL ANALYSIS
During aging, the primary precipitates in
the as-cast structure (M7C3, M23C6, and
389
NbC) are partially transformed and sec-
ondary precipitation (M23C6, G-phase, and
NbC) occurs. The structural changes are
temperature and composition dependent.
With increase of niobium content, the ex-
tent of the secondary precipitation de-
creases, the fragmentation of the primary
carbide network is more marked, and the
coalescence of the precipitated phases is
reduced. The primary chromium carbides
are largely stable upon aging, although
transformation from M7C3 to M23C6 could
be detected after aging at high tempera-
bide is unstable under certain aging con-
ditions and can be transformed in situ to
a nickel-niobium silicide (G phase). These
microstructural observations are described
more fully as follows.
Chromium Carbides (M7C3, M23C6)
High aging temperatures promote a ten-
dency toward chromium enrichment in the
M7C3 primary carbide (as cast) that was
precipitated in all alloys except Alloy D
(1.97% Nb). In Alloy D, the primary chro-
mium carbide was identified as of M23C6
type because of carbon consumption aris-
ing from preferential precipitation of NbC.
Figure 1 is a bar diagram showing the
weight fraction of each carbide type pre-
cipitated in the as-cast state. This diagram
Phases(wr
100
80
60
40
20
/
0
(0%Nb) (o.e~Nb) O.~'Y*Nb) O.sw'/,a~)
As cast alloys
Fie. 1. Bar diagram showing the weight fraction of
each type of carbide identified by x-ray diffraction and
quantified by chemical analysis of extracted residues
from the as-cast alloys, considering stoichiometric
relationships.
390
was constructed through quantification of
the extracted residues, and it shows the
decreasing concentration of chromium car-
bides with increase in niobium content.
After aging at 700°C, the primary chro-
mium carbide maintained the M7C3 stoi-
chiometry, but at 900 and 1100°C, all par-
ticles had been transformed to M23C6. Be-
cause of the high degree of matrix
supersaturation, M23C6 was also present in
all alloys after aging, in the form of sec-
ondary carbides. The M23C6 precipitated
during aging had an orientation relation-
ship with the matrix defined as
[ll0]carbide I11110]~, as shown in Fig. 2. The
EDX analysis indicated that, like the Cr7C3,
the Cr23C6 carbide contained some dis-
solved iron and nickel; thus, it is referred
to as being M23C6. EDX analysis indicated
the composition of the precipitates as
(Cro.86Feo.1oNio.04)23C6 for Alloy B aged at
900°C for 1000 hours.
Several chromium carbide particles hav-
ing Widmanst~itten morphology (needle
FIc. 2. Secondary chromium carbides of M23C6type precipitated in Alloy B aged at 700°C for 1000 hours. (a)
Lowermagnification view, (b) higher magnification view showing [ll0]carbideII[1]-0]rnatrixorientation relationship.
G. D. de Almeida Soares et al.
shaped) were identified in the aged alloys,
particularly in Alloy B. This appears to be
related to an excess of chromium with re-
spect to the carbon in the solid solution,
although a satisfactory relationship be-
tween the chemical composition and the
volumetric fraction of needles could not be
obtained. (It may be noted that, when the
chemical balance used to define the alloys'
composition is considered, Alloy B has a
higher ratio of chromium to carbon in so-
lution than do Alloys C and D [8].) Figure
3 shows the appearance of these particles
in Alloy B aged at 700°C, where the diag-
onal [113] alignment of the small precipi-
tated carbides can be identified. Figure 4
shows small needle-shaped particles of
M23C6 in Alloy B after aging at 1100°C, al-
though at this temperature, optical mi-
croscopy shows a high degree of coales-
cence [8]. The EDX spectra also suggest
that the chromium carbide could exhibit
enrichment in niobium after long expo-
sure, as noted previously [4].
Niobium Additions in HP Steels
FIG. 3. Cuboid particles of secondary M23C6 carbides
with diagonal alignment in Alloy B aged at 700°C for
1000 hours (extracted residues on copper grid).
FIG. 4. Cuboid and Widmanst/itten particles of M23C6
carbide precipitated in Alloy B after 1000 hours aging
at 1100°C.
391
NbC Carbide
The face-centered cubic carbide, NbC, is
formed as a result of the addition of niob-
ium. Optical microscopy shows the pri-
mary carbide to exhibit a "Chinese-script"
morphology, which can also be seen at
high magnification from scanning trans-
mission electron microscopy in Fig. 5. The
calculated lattice parameter was 0.47nm.
After aging at 700 and 900°C, the niobium
carbide displayed instability with respect
to G phase. The quantity of NbC detected
by x-ray diffraction in Alloys B and C aged
at 900°C was very small. After aging at
1100°C, NbC was the only niobium-rich
phase detected by x-ray diffraction.
G Phase
This phase was detected in all niobium-
containing specimens aged at 700 and
900°C as a consequence of the high-tem-
perature instability of NbC. After aging at
700 and 900°C, some secondary particles
having a round shape were identified
FIG. 5. NbC primary carbide network exhibiting a
Chinese scriptlike morphology: Alloy B in the ds-cast
condition.
392 G. D. de Almeida Soares et al.

Fie. 6. G phase particles with round shape, precipi- FIG. 8. G phase particles identified by nickel line scan
tated at chromium carbide-matrix interface: Alloy B in Alloy B aged at 900°C, resulting from in situ trans-
aged at 700°C for 1000 hours. formation of primary niobium carbides.

along the interfaces between the matrix
and the primary chromium carbides, as
shown in Fig. 6. Upon exposure at 900°C,
the intensity of the NbC peaks shown on
the x-ray spectra decreased substantially
from that for as-cast material (Fig. 7). Con-
firming the observations of the x-ray data,
several G phase particles, the products of
in situ transformation of niobium carbides,
were identified by electron microscopy in
all niobium alloyed specimens; this is il-
lustrated in Fig. 8. The in situ transformed

I I

5(3 50

40 40

30 30

20 20

10 10

600 50° 40° 3( 60 o 50° 40° 3 0°

FIG. 7. X-ray diffraction spectra for Alloy C, showing intensity versus diffraction angle. (a) In the as-cast con-
dition, and (b) after 1000 hours at 900°C, showing a marked decrease in the intensity of the NbC peaks as a
consequence of NbC---*G phase transformation.
 Niobium Additions in HP Steels 393

precipitates maintain the m o r p h o l o g y of

1,200 I Alloy D 1.97 Nb
the primary carbides.
1,100 :3
M e a s u r e m e n t of the lattice p a r a m e t e r for
the face-centered cubic n i c k e l - n i o b i u m sil- 1.000 2 ~lb
icide indicates a value of 1.13nm. All peaks
of the x-ray spectra agree with the data for
E M~C8 G Phase + NbC
silicide of the type Ni16Nb7Si6 [9], although
the semi-quantitative EDX analysis of
these particles indicated a composition 700 ~ I
Ni6Nbs.sSi4.3. The EDX analysis also indi-
cated that iron and c h r o m i u m can be dis-
3 10 30 1(30 3OO 1,000
solved in this silicide. Time (h)
Because no G phase was detected by
FIG. 9. Time-temperature-precipitation curves deter-
x-ray or electron microscopy in any spec- m i n e d from x-ray diffraction data for Alloy D (1.97%
imen aged at 1100°C, the range of stability Nb), s h o w i n g the stability range for G phase. The
of NbC was d e t e r m i n e d by m e a n s of ad- solid circles represent conditions w h e r e M2~C~, G
ditional aging tests. The time-temperature- phase and NbC coexist. In some cases (at longer
precipitation curves s h o w n in Fig. 9 define times) the NbC was ve D, little, but was detectable.
the NbC transformation of Alloy D (1.97%
Nb). The solid circles r e p r e s e n t identifi-
cation of G phase on the x-ray spectra,
based on an interplanar spacing of in all aging conditions, an arrow indicating
0.198nm, c o r r e s p o n d i n g to {440} planes. an increasing v o l u m e fraction of M23C~, or
The nose of the curve is at 950°C, G phase relates to precipitation associated
approximately. with the n e t w o r k of primary carbides and
Table 3 illustrates the phases detected at also with secondary precipitation in the
the different aging conditions for each austenite matrix. Table 3 shows the
alloy. The arrows indicate if the v o l u m e changes in each phase for each aging con-
fraction of a particular phase is increasing dition with respect to the original as-cast
or decreasing d u r i n g aging. For all alloys condition.

Table 3 Phases Detected in the Different Alloys and Aging Conditions

Alloy

A B C D
Alloy condition 0% Nb 0.69% Nb 1.23% Nb 1.97'~'~ Nb

As-cast M7C3 M7C3 M7C3 --

-- -- -- M2~C,
-- NbC NbC NbC
A g e d 700°C 1000 h M7C3 ,l, M7C3 ,~ M7C3 ~, --
M23C6 i' M23C~, T M23C, I' M2~C,, T
-- NbC ~ NbC ~ NbC
- - G1' Gi' GI"
Aged 900°C 1000 h M23C6 I' M23C~ T M23Ce, 1' M2~C(, T
-- NbC ~ NbC $ NbC
-- GT GJ' GI"
Aged 1100°C 1000 h M23C6 I' M23C~ 1' M23C, 1' M2~C, '~
-- NbC 1' NbC I' NbC 1'
The arrows indicate if the volume fraction of a particular phase is increasing ( ~' ) or decreasing ( ,~) with respect to the as-cast
data.
394 G. D. de Almeida Soares et al.

6OO
[] o% Nb DISCUSSION
• o.sg~ Nb
5OO
," • 1.2~,6 Nb Aging at 700°C is characterized by exten-
,:' • 1.9"t%Nb
sive secondary precipitation. The precipi-
tation was identified as chromium carbide
o f M23C6 type plus small particles of G
phase. Many particles'of this silicide were
m
observed at the interfaces between the ma-
1.. ~:i:iiiii ............. trix and primary chromium carbides. At
700°C the transformation of the primary
o ~ , , ........ , ......... , ......... , ......... , ......... , ........
As cast 700 800 go0 1,000 1,100 1,200 NbC to G is not as well defined as at 900°C,
Aging temperature
even using x-ray diffraction or transmis-
FIG. 10. Rupture time as a function of prior aging tem- sion electron microscopy.
perature for all alloys creep tested at 925°C and The increase in the rupture time shown
45MPa. by the alloys aged at 700°C may be a con-
sequence of the extensive fine secondary
precipitation and of the fragmentation of
MECHANICAL PROPERTIES
the primary carbides. The decrease in the
volumetric fraction of secondary precipi-
tation with increase in niobium content
Figures 10 and 11, respectively, show the
may explain the relatively lower rupture
variation in rupture life and minimum
time for Alloy D (1.97% Nb). However, it
creep rate as a function of aging temper-
is important that Alloy D still shows much
ature for creep tests at 925°C and 45MPa.
better creep properties when compared
The lower values of rupture time and high
with Alloy A without niobium.
values of minimum creep rate for Alloy A
The instability of the niobium carbide is
(0% Nb) may be seen, as well as similar
a distinct feature observed upon aging at
effects for all alloys after aging at 1100°C.
900°C, with extensive transformation of
Alloys B - D display improved creep prop-
the primary NbC to the nickel-niobium sil-
erties after aging at 700 and 900°C, al-
icide. For all Nb-alloyed steels, the amount
though the properties of Alloys B and C
of G phase after aging at 900°C for 1000
are not so much improved over the unaged
hours was nearly constant, this being es-
material when aged at 900°C.
timated from the intensity of the 0.198nm
peak on the x-ray diffraction spectra. On
the other hand, the secondary precipita-
0.001
c3 O~Nb
tion has coalesced to a considerable extent.
• o.e8% Nb
Hence, the creep behavior observed in
0.0001
Q 1 . 2 ~ Nb Figs. 10 and 11 is probably related to the
IE-(~
• 1.97~ Nb fragmentation of the primary carbides by
o
the addition of niobium, this being greater
~ IE4~ in Alloy D. The improved creep behavior
E
of Alloy D over that of Alloys B and C may
"E 1E4~7
also be associated with delay in the coa-
1E4~ lescence of the secondary precipitation
owing to the higher niobium concentra-
IE4~ r-~
Asca~
, ........
700
~.........
800 900
, ........
1,000
, ..... , ......... , ........
1,100 1,200
tion. The low rupture time shown by Alloy
Aging tern~ratLIre ~°C) B after aging at 900°C may also be related
FIG. 11. Minimum creep rate as a function of prior to the higher volume fraction of the needle-
aging temperature for all alloys creep tested at 925°C shaped chromium carbide caused by the
and 45MPa. higher Cr/C ratio of this alloy.
Niobium Additions in HP Steels
Based on t,he limited test time of 1000
hours, the m a x i m u m t e m p e r a t u r e for the
stability of G p h a s e is b e t w e e n 1000 a n d
1050°C, as indicated in Fig. 9. This value
is greater t h a n those d e t e r m i n e d b y Powell
et al. [6] a n d Ecob et al. [7]. In the p r e s e n t
case, the high n i o b i u m content p r o b a b l y
acts to extend the field of stability of the G
phase, as occurs with titanium in the
n i c k e l - t i t a n i u m - s i l i c o n s y s t e m [10]. More-
over, the higher nickel content in the pres-
ent alloys, as c o m p a r e d w i t h those studied
b y Powell et al. a n d Ecob et al., should as-
sist with d e c o m p o s i t i o n of the N b C by fa-
voring the nickel-rich phases. The role of
o x y g e n content on N b C d e c o m p o s i t i o n , as
p o s t u l a t e d by Ecob et al. [7], is still unclear.
The characteristic of aging at 1100°C is
the stability of NbC. R u p t u r e life of spec-
i m e n s aged at this t e m p e r a t u r e w a s almost
i n d e p e n d e n t of the n i o b i u m content, the
mechanical b e h a v i o r being inferior to that
of the a g e d alloys in w h i c h G p h a s e w a s
present. At this t e m p e r a t u r e , the contri-
bution of the s e c o n d a r y precipitation is not
c o n s i d e r e d to be significant. It is i m p o r t a n t
to note that the creep tests w e r e p e r f o r m e d
at 925°C, at w h i c h t e m p e r a t u r e the N b C ---*
G p h a s e t r a n s f o r m a t i o n can occur. The
short time of the creep tests of the speci-
m e n s a g e d at 1100°C w a s insufficient to
p r o d u c e extensive t r a n s f o r m a t i o n as com-
p a r e d to that occurring d u r i n g aging at 900
and 700°C. The results p r e s e n t e d in Figs.
10 a n d 11 indicate a greater contribution to
creep strength f r o m a f r a g m e n t e d n e t w o r k
of G phase.
CONCLUSIONS
In all the Nb-alloyed H P steels studied, the
p r i m a r y N b C exhibited a r a n g e of insta-
bility with t e m p e r a t u r e a n d time. U p o n
aging, the N b C can be t r a n s f o r m e d to
Ni16Nb6Si7, G phase. The extent of this
t r a n s f o r m a t i o n d e p e n d s on aging t e m p e r -
ature a n d n i o b i u m content, a n d can be al-
m o s t c o m p l e t e with an in situ transfor-
395
m a t i o n k e e p i n g the original Chinese script-
like m o r p h o l o g y .
Artificial aging p r o m o t e s c h r o m i u m en-
r i c h m e n t of the M7C3 c h r o m i u m carbide
a n d s e c o n d a r y precipitation of M23C6
s h o w i n g a [110] relationship with the aus-
tenite matrix. Alloys h a v i n g a higher ratio
of c h r o m i u m to carbon in solution s h o w a
diagonal a l i g n m e n t of M23C6 cuboids, re-
sulting in n e e d l e - s h a p e d precipitates that
can be d e t r i m e n t a l to the mechanical
properties.
C r e e p test results indicate the relevance
of the s e c o n d a r y precipitation and suggest
a greater contribution to creep strength of
a f r a g m e n t e d p r i m a r y microstructure con-
taining G p h a s e as c o m p a r e d with that
f r o m one containing NbC.
The authors thank M. C. S. Miranda for the
graphical work, and are grateful for financial
support received from CBMM--Companhia
Brasileira de Metalurgia e Minerafdo, FINEP/
CNP (Brazil), the International Development
Research Centre (IDRC), and the Natural Sci-
ences and Engineering Research Council (Can-
ada). Thanks are expressed to Professor D. Tro-
man and Mary Mager of the University of Brit-
ish Columbia for the use of the Hitachi STEM
and for helpful discussions. Thanks are also ex-
pressed to Sr. Luiz Rosa for the use of facilities.
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Received February 1992; accepted July 1992.