Grain refinement mechanism of Fe–32Ni alloys

during multiaxial forging

B. J. Han* and Z. Xu
Warm deformation of Fe–32Ni alloy was studied in connection with microstructure developments
in multiple axial forging at a temperature of 823 K (y0.5Tm) and a strain rate of 1023 s21. The
microstructure evolution of the deformed alloys was investigated using EBSD and TEM. The
structural changes are characterised by the evolution of many mutually crossing sub-boundaries
at low to moderate strains, finally followed by the development of very fine grains with medium to
large angle boundaries at large strains. These new grains are concluded to be evolved by a kind
of continuous reaction, that is continuous dynamic recrystallisation; this process is that sub-
boundaries crossing each other subdivide an austenite grain into several subgrains and these
subgrains are gradually reoriented to new independent grains with their boundaries being
transformed into large angle boundaries in subsequent deformation.
Keywords: Grain refinement, Electron backscatter diffraction, Continuous dynamic recrystallisation, Fe–32Ni alloy

Introduction of such structure evolution is still not very clear.

Very fine grained metallic materials have some advan-
tages because of improved mechanical properties, i.e.
increasing workability and strengthening at elevated and
ambient temperatures.1,2 The grain refinement in single
phase metals and alloys without solid state phase
transformation can be achieved by any thermomecha-
nical processing, based on cold working followed by
annealing at elevated temperatures. This is a method of
static recrystallisation, which has been studied and
applied to many conventional materials. However, it is
generally agreed that there is a limitation for grain
refinement by such processing because of rapid grain
growth taking place in the surrounding highly deformed
matrix. This limit can be overcome by the application of
dynamic recrystallisation (DRX), which allows the fine
grained structures to be formed directly during deforma-
tion and to remain stable after working.3–5
It is well known that the dynamic grain size may be
considerably reduced by decreasing the deformation
temperature.3–7 On the other hand, the strains required
for the development of DRX increase with decreasing
temperature and thus the studies of grain refinement by
DRX are complicated by the need to apply severe high
deformation. Several specific techniques such as equal
channel angular extrusion (ECAE), accumulative roll
bonding (ARB) and torsion under high pressure had
been proposed.6–15 It has been shown that the submetre
grain structure resulted from a kind of continuous
dynamic recrystallisation.6–10 However, the mechanism
Key Laboratory for High Temperature Materials and Tests of Ministry of
Education, Shanghai Jiao Tong University, Shanghai 200030, China
*Corresponding author, email Hanbaojun80@tom.com
Therefore, study on the microstructure evolution
mechanism under severe plastic deformation is of great
value in theory.
The aim of the present work is to study the grain
refinement phenomena of Fe–32Ni alloy under warm
severe plastic deformation by multiaxial forging. The
microstructure evolution mechanism is discussed in detail.
Experimental procedure
A Fe–32Ni alloy (Fe–0.007C–0.01Si–0.04Mn–0.005P–
0.0006S–32.4Ni–0.022Al–0.00074N–0.020O) was used
as the experiment material because it is fully in austenite
state at ambient temperature fitting for the observation
and investigation of deformed microstructure.
The samples were machined into cubic shape with
starting dimensions of 14614614 mm3. These samples
were annealed at 1473 K for 60 min, giving an initially
austenite grain size of y100 mm. The samples were
preheated at 823 K for 600 s before they were alter-
nately forged with loading direction changed through
90u (i.e. x–y–z–x) using graphite as lubricant; the
forgings were carried out at 823 K and a strain rate of
1023 s21. The strain achieved in each stage of forging
was y0.5. The samples were taken out quickly and
quenched into cold water after the deformation.
The metallographic analysis was carried out using
optical microscope, electron backscattered diffraction
(EBSD) and JEM-2100F transmission electron micro-
scope. Microstructure observations were carried out on
sections with their normal verticals to the compression
axis. All the clearly defined grain boundaries were taken
into account to determine the grain boundary misor-
ientations. Misorientations of the grain boundaries were
analysed using the conventional Kikuchi line technique.

ß 2006 Institute of Materials, Minerals and Mining

Published by Maney on behalf of the Institute
Received 5 March 2006; accepted 20 April 2006
DOI 10.1179/174328406X131037 Materials Science and Technology 2006 VOL 22 NO 11 1359
Han and Xu Grain refinement mechanism of Fe–32Ni alloys during multiaxial forging

1023 s21 are shown in Fig. 1. It is clearly seen that the

features of microstructure evolved are sensitively chan-
ged by strain. Early deformation brings about the
evolution of elongated subgrains (Fig. 1b), the size of
which rapidly decreases. Upon further multiple strain-
ing, the grains become more equiaxed and fine grains in
sizes of y1 mm are developed at last when the
cumulative strain is y5.6 (Fig. 1c).
Typical TEM microstructures that evolved during
multiple axial forging are shown in Fig. 2. It can be seen
that the early multiple deformations brought about the
evolution of high dislocations density roughly homo-
geneously arranged in parallel dislocations rich layers
that were crossed by dense dislocation walls. A typical
example of such substructure at a strain of 1.5 is
presented in Fig. 2a. Upon further multiple deformation
to high cumulative strain, the volume fraction of the
highly misoriented substructures increased substantially,
leading to the full development of well defined fine
grains throughout. The sub-boundaries became sharp
and narrow accompanied as the dislocation densities in
grain interiors decrease in average. A typical micro-
structure evolved by severe deformation to total strains
of 9.6 is presented in Fig. 2b.
Typical EBSD maps of the microstructures that
evolved during multiple axial forging are shown in
Fig. 3. It can be found that after early deformation, the
elongated subgrains formed. Upon further deformation,
more equiaxed fine grains were obtained.

Misorientations of strain induced grain

1 Typical optical micrographs of Fe–32Ni deformed with
strains of a 0, b 1.5 and c 5.6 at 823 K and strain rate
of 1023 s21
Results and discussion
Microstructure evolution
Typical optical microstructures that evolved during
multiple axial forging at 823 K and a strain rate of
boundaries
Since the grain refinement under severe plastic deforma-
tion can result from a kind of continuous DRX, i.e. a
gradual transformation of strain induced subgrains into
fine grains,16–18 the grain boundaries misorientations
can be used as a parameter that allows following the
development process of ultrafine grains. The grain
boundary misorientations that developed under differ-
ent strain levels are shown in Fig. 4. It can be seen that
distribution of grain boundary misorientations that
evolved in the sample with strain about 1.5 is
characterised by a small fraction of high angle bound-
aries. For simplicity, a critical separating misorientation
between low and high angle boundaries is selected
around 15u, which is approximately where it is not
longer possible to discern well separated dislocations
forming the boundaries. It can be found that the average

2 Typical TEM microstructures of Fe–32Ni deformed with strains of a 1.5 and b 9.6 at 823 K and strain rate of 1023 s21

1360 Materials Science and Technology 2006 VOL 22 NO 11

 Han and Xu
3 Typical EBSD maps of Fe–32Ni deformed with strains
of a 1.5 and b 9.6 at 823 K and strain rate of 1023 s21
grain boundary misorientation is y10u and the fraction
of high angle boundaries does not exceed 40% after a
strain of 1.5. Both the average grain boundary
misorientations and the fraction of high angle bound-
aries increase with increasing strain. The corresponding
low angle grain boundaries seemingly fall and spread
towards high angle misorientations with decreasing
grain sizes. Figure 5 shows changing of the fraction
of high angle boundaries with the strain. It can be
found that at a low strain of 0.5, strain induced (sub)
structures comprise many low angle boundaries and the
fraction of high angle boundaries is y30%, whereas
further multiple deformation of these samples to a
total strain of y10 causes the fraction of high angle
4 Electron backscattered diffraction orientation distributions of grain boundaries with cumulative strains of a 1.5 and b
9.6
Grain refinement mechanism of Fe–32Ni alloys during multiaxial forging
5 Effect of cumulative strain on fraction of high angle
boundaries of Fe–32Ni alloy deformed at 823 K and
strain rate of 1023 s21
boundaries to increase to above 70% and corresponds to
an almost full development of the new ultrafine grained
microstructure.
Evolution mechanism of grain refinement
The average misorientation and the fraction of high
angle boundaries are frequently used to analyse the
progress in grain refinement during large deformation.19
The experimental results described above suggested that
the transformation of strain induced dislocation sub-
boundaries into conventional grain boundaries, in
general, is accompanied by the increase in their
misorientations and the fraction of high angle bound-
aries as well as the dislocation rearrangement inside sub-
boundaries, which had been found in many metals and
alloys.20,21 The result of the fraction of high angle
boundaries as a function of strain (Fig. 5) is similar to
that found in some other large strain deformation
techniques, such as ECAE by Harris et al.22,23 and ARB
by Saito et al.24,25 However, their development mechan-
isms are quite different. Generally speaking, the ECAE
and ARB are usually developed at intermediate or high
temperatures, and the high angle boundaries are formed
by a process named geometric dynamic recrystallisation
(GRX). This process is that at larger strains, high angle
boundaries are pushed together and the subgrain size
remains approximately constant during deformation;
eventually, the separation of high angle boundaries is
equal to the subgrain size, the high angle boundaries
Materials Science and Technology 2006 VOL 22 NO 11 1361
Han and Xu Grain refinement mechanism of Fe–32Ni alloys during multiaxial forging
a initial grain; b after first pass; c after second pass with deformation direction rotated 90u; d subgrains angled in subse-
quent passes
6 Evolution mechanism of continuous dynamic recrystallisation during multiaxial forging
impinge and a microstructure of small and almost
equiaxed grains are formed.26 In contrast, the develop-
ment of the fine grains in the present deformation
technique (multiaxial forging) was under relatively lower
temperature (y0.5Tm), which can be described as a
process of continuous rotation of subgrains during
severe plastic deformation, i.e. continuous dynamic
recrystallisation.16–18,27 The evolution of continuous
DRX during multiaxial forging can be summarised as
a process in Fig. 6. When initial grains are deformed in
some direction, deformed bands will be produced along
a certain direction in deformed grains by slip shear.
Once the deformation direction changes, other deformed
bands will also be formed along other directions; in this
way, deformed bands will cross each other, by which an
austenite grain can be subdivided into several subgrains.
Multiple axial forging promotes the rapid formation of
many intersecting dislocation boundaries in different
directions because of the variation in the slip systems
operating from pass to pass. Therefore, the subgrains
are formed continuously, they will be gradually reor-
iented by rotation to new independent grains and their
boundaries transformed into large angle boundaries in
subsequent passes. The deformation bands of Fe–32Ni
alloy formed in the process of deformation are shown in
Fig. 7. It can be found that the bands are crossing each
other.
7 Deformation band morphology crossing each other in
Fe–32Ni alloy at 823 K and strain rate of 1023 s21
1362 Materials Science and Technology 2006 VOL 22
Conclusions
Grain refinement behaviour of Fe–32Ni alloy under
severe plastic deformation was investigated in multiaxial
forging at 823 K and a strain rate of 1023 s21. The main
results can be summarised as follows: the Fe–32Ni alloy
austenite grains were greatly refined through multiaxial
forging. The grain refinement mechanism during multi-
axial forging can be summarised as such a process that
deformed bands crossing each other subdivide an
austenite grain into several subgrains and these sub-
grains are gradually reoriented to new independent
grains with their boundaries being transformed into
large angle boundaries in subsequent deformation.
Acknowledgements
The authors would like to acknowledge the financial
support of the National Natural Science Foundation of
China under granted number 50471017.
References
1. O. A. Kaibyshev: ‘Superplasticity of alloys, intermetallics and
ceramics’; 1992, Berlin, Springer.
2. F. J. Humphreys, P. B. Prangnell and J. R. Bowen: Trans. Roy.
Soc. Lond. A, 1999, 357A, 1663.
3. F. J. Humphreys and M. Hatherly: ‘Recrystallization and related
annealing phenomena’; 1996, Oxford, Pergamon Press.
4. T. Sakai and J. J. Jonas: Acta Metall., 1984, 132, 89.
5. T. Sakai: J. Mater: Process. Technol., 1995, 53, 349.
6. N. Tsuji: Tetsu-to-Hagane, 2002, 88, 359.
7. R. Z. Valiev, R. K. Isalamgliev and I. V. Alexadrov: Prog. Mater.
Sci., 2000, 45, 103.
8. N. Tsuji, Y. Saito, S. H. Lee and Y. Minamino: Sci. Technol. Adv.
Mater., 2003, 5, 338.
9. Y. Saito, N. Tsuji, H. Utsunomiya and T. Sakai: Acta Mater.,
1999, 47, 579.
10. H. Kitahara, N. Tsuji and Y. Minamino: Proc. Int. Conf. on
‘Martensitic transformations’, Shanghai, China, May 2005,
Shanghai Jiao Tong University, 52–53.
11. D. H. Shin, W. G. Kim, K.-T. Park, C. S. Lee and N. J. Kim: Proc.
Int. Conf. on ‘Martensitic transformations’, Shanghai, China, May
2005, Shanghai Jiao Tong University, 62.
12. D. H. Shin, R. Ueji, Y. Minamino and Y. Saito: Scr. Mater., 2002,
46, 305.
13. K. Tsuzaki: ISIJ Int., 2002, 42, 1325.
14. S. Takaki and T. Tsuchiyama: Proc. 2nd Int. Conf. on ‘Advanced
structural steels’, Shanghai, China, April 2004, The Chinese Society
for Metals, 106–113.
15. A. Belyakov, T. Sakai, H. Miura and R. Kaibyshev: Scr. Mater.,
2000, 42, 319.
16. A. Belyakov, W. Gao, H. Miura and T. Sakai: Metall. Mater.
Trans. A, 1998, 29A, 2957.
17. A. Belyakov, T. Sakai and H. Miura: Mater. Trans. JIM, 2000, 41,
476.
NO 11
 Han and Xu Grain refinement mechanism of Fe–32Ni alloys during multiaxial forging

18. A. Belyakov, T. Sakai, H. Miura and K. Tsuzaki: Philos. Mag. A,
2001, 81A, 2629.
19. A. Belyakov, K. Tsuzaki, H. Miura and T. Sakai: Acta Mater.,
2003, 51, 847–861.
20. D. Kuhlmann-Wilsdorf and N. Hansen: Scr. Metall. Mater. Trans.,
1991, 25, 1557.
21. D. A. Hughes and N. Hansen: Acta Mater., 1997, 45, 3871.
22. C. Harris, P. B. Prangnell and X. Duan: Proc. Conf. ICAA-6,
Toyohashi, Japan, July 1998, The Japan Institute of Light Metals,
Vol. 1, 583.
23. A. Gholinia, P. B. Prangnell and M. V. Markushev: Acta Mater.,
2000, 48, 1115.
24. Y. Saito, H. Utsunomiya and N. Tsuji: Acta Mater., 1999, 47, 579–
583.
25. N. Tsuji, Y. Saito and H. Utsunomiya: Scr. Mater., 1999, 40, 795–
800.
26. H. J. McQueen, O. Knustad and N. Ryum: Scr. Mater., 1985, 19,
73–78.
27. F. J. Humphreys and M. Hatherly: ‘Recrystallization and related
annealing phenomena’; 1995, Oxford, Pergamon Press.

Materials Science and Technology 2006 VOL 22 NO 11 1363