Materials Science & Engineering A 603 (2014) 104–113

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Materials Science & Engineering A

journal homepage: www.elsevier.com/locate/msea

The role of deformation temperature and strain on grain boundary

engineering of Inconel 600
B. Li, Sammy Tin n
Illinois Institute of Technology, Department of Mechanical, Materials and Aerospace Engineering, Chicago, IL 60616, USA

art ic l e i nf o a b s t r a c t

Article history: The present study investigates the effect of deformation temperature and strain on the formation of twin
Received 24 December 2013 boundaries in Inconel 600. With a constant strain rate of 0.003/s, deformation temperatures were varied
Received in revised form between 25 1C and 982 1C while strains varied between 11% and 80%. The resulting microstructures were
21 February 2014
characterized using electron back scatter diffraction both immediately following deformation and after
Accepted 24 February 2014
Available online 4 March 2014
an annealing cycle at 1025 1C. Comparison of the grain boundary characters associated with the samples
enabled correlation of the processing parameters to the formation of desirable coherent twin boundaries
Keywords: and the identification of a deformation mechanism map. Processing parameters associated with strain
Grain boundary engineering annealing and dynamic recovery were found to promote the formation and retention of twin boundaries,
Thermo-mechanical processing
while statically and dynamically recrystallized microstructures tend to contain large proportions of
Coincident site lattice
random grain boundaries that mitigate the effects of grain boundary engineering.
& 2014 Elsevier B.V. All rights reserved.

1. Introduction desirable ones to have distributed within the random boundary

Inconel 600 is a commercially available Ni–Cr–Fe alloy that
exhibits a good combination of strength, formability and environ-
mental resistance at elevated temperatures. This combination of
properties makes these materials ideally suited for use as structural
components in chemical processing equipment, nuclear reactors
and aerospace applications [1–4]. To improve the overall efficiency
and performance of many of these applications, advanced design
concepts require many of these structures to operate under higher
loads and temperatures. These continuous changes serve as the
primary motivation for the development of innovative new materi-
als, alloys and manufacturing processes. Pertaining to some of the
recent advances in processing, grain boundary engineering (GBE)
has been used to enhance the mechanical and environmental
resistance of polycrystalline engineering alloys [5–11]. Property
improvements associated with GBE have been attributed to the
increase in the overall proportion of “special boundaries” that
possess a large number of coincident lattice sites along grain
boundaries. Grain boundaries in polycrystalline alloys can be
classified on the basis of these coincident site lattices (CSL) and
the reciprocal density of the coinciding sites can be designated as Σ.
From this description, “special boundaries” are typically defined as
those with Σo29, with the Σ3 twin boundaries being the most
n
Correspondence to: Illinois Institute of Technology, MMAE Department E1-243,
Chicago, IL 60616, USA.
E-mail address: tin@iit.edu (S. Tin).
network. Polycrystalline alloys that contain a sufficiently high
fraction of these special CSL boundaries that break up the inter-
connectivity of the pre-existing random grain boundary network
[12–14] exhibit improved strength [15], creep performance [16]
resistance to intergranular fracture [9–11], stress corrosion cracking
[11–17] and fatigue crack propagation [18–19].
Recent advances in the development of electron back-scatter
diffraction (EBSD) characterization tools have enabled materials scien-
tists and engineers to develop a significantly better understanding of
the role of crystallographic texture and grain boundary character on
the properties of virtually all classes of materials. Despite some
successes in achieving significantly improved properties via GBE, these
advances have not yet been fully realized in the production of
physically large bulk structures. This can largely be attributed to the
existing practices for GBE that utilizes multiple iterations of cold
rolling to 5–20% strain at room temperature followed by short
annealing cycles of a few minutes after each deformation step. Since
each iteration of deformation and annealing imparts only a modest
increase in the fraction of twin and special grain boundaries, multiple
iterations are required to achieve a sufficiently high fraction (
50–
60%) of “special grain boundaries” that result in the improved proper-
ties. From a commercial manufacturing perspective, room temperature
deformation of high strength Ni-base superalloys of interest is
impractical as these materials can withstand only limited deformation
without cracking, forging die materials cannot withstand the forging
stresses required, and forging equipment would limit the size and
complexity of potential component configurations. Moreover, the
short annealing times employed to limit recrystallization and grain

http://dx.doi.org/10.1016/j.msea.2014.02.078
0921-5093 & 2014 Elsevier B.V. All rights reserved.
 B. Li, S. Tin / Materials Science & Engineering A 603 (2014) 104–113
growth are not compatible with the large thermal inertia inherent in
large complex structures. Moreover, the multiple deformation and
thermal processing cycles would add manufacturing lead time and
cost even if the aforementioned limitations could be overcome. As
such, the current approaches used for GBE are not ideally suited for
the fabrication of physically large, complex components for propulsion
and power generation applications.
In polycrystalline materials, the character of the grain boundaries is
extremely important and greatly influences both the physical and
mechanical properties of the material, particularly at elevated tem-
peratures [20–22]. In recent years, ultra-fine grain processing techni-
ques have been developed to produce bulk metallic materials with
sub-micron grain sizes [23–27]. At relatively low temperatures, the
high densities of grain boundaries serve as obstacles to restrict
dislocation activity and resist fatigue crack propagation. In these
instances, the Hall–Petch relationship is valid for numerous material
systems and relates changes in the yield strength to grain boundary
density or grain size. However, for structural materials intended for
use at elevated temperatures, fine grain sizes and high densities of
grain boundary area are not necessarily beneficial as grain boundary
sliding and the accumulation of cavitation damage contribute to the
degradation of creep properties. The random grain orientations that
exist in isotropic polycrystalline materials lead to the formation of a
random grain boundary network consisting of a statistical distribution
of grain boundary orientations. Depending on the relative orientations,
the coherency of the individual grains with their neighbors or CSL at
the boundary may vary significantly. CSL boundaries, with Σ429,
tend to contain large concentrations of crystalline defects and vacan-
cies that serve to both weaken the interface and promote diffusive
mechanisms at elevated temperatures. Under these conditions, grain
boundary diffusion and sliding are accelerated along these boundaries.
This leads to environmental degradation and poor resistance to creep
deformation. On the other hand, adjacent or neighboring grains that
exhibit CSL boundaries, with Σo29, have relatively coherent interfaces
that contain few crystalline defects that would serve to weaken the
boundaries. In this regard, coherent twin boundaries with Σ¼ 3 are
highly desirable features in grain boundary engineered materials since
they possess some of the lowest grain boundary energies [5–16,28,29].
Moreover, since there are comparatively fewer vacancies and defects
along low Σ interfaces, the mechanisms by which diffusion and mass
transport occurs along the interfaces are also more sluggish. Thus,
polycrystalline materials containing high proportions of special CSL
boundaries are desirable for use at elevated temperatures. In order to
induce the formation of sufficiently large fractions of special grain
boundaries, strain energy in the form of dislocations first needs to be
stored in the material. Upon subsequent annealing, the supplied
thermal energy enables the system to effectively utilize the stored
strain energy to form twins and other special CSL boundaries. It is still
not entirely clear whether the underlying mechanisms responsible can
be attributed to dislocation recovery or grain boundary migration
induced by the differences in strain energy. In this paper, the effect of
various hot deformation processing parameters on the formation of Σ3
boundaries in IN600 was investigated.
2. Procedure
Fully recrystallized hot rolled bars of IN600 with a composition
listed in Table 1, were machined into cylindrical compression
Table 1
Nominal composition of Inconel 600 (wt%).
Ni Cr Fe C Mn Si Cu
Bal. 15.5 8.0 0.15 1.0 0.50 0.50
105
specimens with a diameter of 10 mm and a height of 15 mm. Using
an MTS servo-hydraulic testing system equipped with a resistance
furnace, a total of 16 samples were compressed at a strain rate of
0.003/s to true strains of 11%, 28%, 51% and 80% at temperatures of
25 1C, 538 1C, 760 1C and 982 1C. Strains were measured using a
MTS high temperature extensometer with alumina extension arms
while temperatures were measured by averaging the values
obtained from three thermocouples attached directly to the sur-
face of the sample. For tests conducted at elevated temperatures,
the samples were immediately quenched in water following
deformation in order to preserve representative microstructures.
The compressed samples were sectioned longitudinally along their
centers using a low speed diamond saw. For each deformation
temperature and strain level, one half of the sample was subjected
to an annealing treatment that consisted of heating the sample
from room temperature to 1025 1C at a rate of 23.8 1C/min and an
18 min isothermal hold at 1025 1C. To investigate the effect of
annealing time on the formation of Σ3 boundaries, multiple
samples were deformed to 25% strain at 25 1C and sectioned.
These samples were placed directly into a furnace set at 1025 1C
and annealed for 5, 18, 38 and 60 min followed by a water quench.
Following deformation and/or heat treatment, all of the sam-
ples were prepared using standard metallographic procedures that
incorporated a final polish using 0.05 μm colloidal silica. A JEOL
5900 equipped with an Oxford Instruments Nordlys Nano EBSD
system was used to measure the character of the grain boundaries
and quantify the average intragranular misorientations. Multiple
EBSD scans were taken from each sample to produce statistically
significant results and provide quantitative information at differ-
ent length scales. High magnification scans were taken over an
area spanning 40  40 μm2 using a 0.1 μm step size. These EBSD
scans were used to produce inverse pole figures showing the
individual grain orientations and the magnitude of the intragra-
nular misorientations. Lower magnification scans over an area of
350  350 μm2 using 0.7 μm step size were used to generate
datasets that contained statistically significant numbers of grains
for determination of the grain boundary characters. Data from
samples in the as-deformed condition were compared to those
following annealing.
3. Results
In the as-received or hot rolled condition, the IN600 sample
contained equiaxed grains with an average grain size of approxi-
mately 7.7 μm, Fig. 1a. Twin or Σ3 boundaries were observed in
this initial condition and EBSD analyses revealed that their length
fraction (total Σ3 length/total length of all boundaries) was 36%.
The grain orientation map for hot rolled IN600, shown in Fig. 1b,
also reveals that there were no measurable changes in the
intragranular misorientations that correspond to plastic deforma-
tion or the presence of pre-existing dislocation networks and is
consistent with a fully recrystallized microstructure.
Cylindrical compression samples were deformed to various
strain levels at different temperatures. Depending on the deforma-
tion temperature, the samples exhibited characteristic flow beha-
viors, Fig. 2. The peak flow stresses were observed to decrease
dramatically as a function of temperature and ranged from
143 MPa at 25 1C to 16 MPa at 982 1C. Additionally, the degree or
magnitude of strain hardening was also observed to decrease as
deformation temperatures increased. Only a modest amount of
strain hardening was evident at 760 1C and no strain hardening
was observed during deformation at 982 1C. As samples were
deformed to various levels of true strain at these temperatures, the
corresponding changes in the microstructure were characterized.
In the as-deformed condition, the magnitude of the intragranular
106 B. Li, S. Tin / Materials Science & Engineering A 603 (2014) 104–113
Fig. 1. (a) Band contrast image showing the distribution of Σ3 boundaries and
(b) an inverse pole figure showing the individual grain orientations in the initial
microstructure of a hot rolled IN600 bar.
Fig. 2. Flow stresses of Inconel 600 during deformation at different temperatures.
Samples were deformed to true strains of 11%, 28%, 51% and 80%.
misorientations averaged over the whole sample were observed
to increase as a function of strain, but decreased as deforma-
tion temperatures increased, Table 2. Comparing the results for
Table 2
Average internal misorientation of as-deformed samples (deg).
11% 28% 51% 80%
25 1C 0.423 0.776 – –
538 1C 0.339 0.587 – –
760 1C 0.249 0.433 0.461 0.640
982 1C 0.168 0.207 0.265 0.397
samples deformed to true strains of 11%, deformation at tempera-
tures of 25 1C and 982 1C resulted in internal misorientations of
0.4231 and 0.1681, respectively. The samples deformed at inter-
mediate temperatures exhibited misorientation values that were
in-between these values. As the true strain was increased from 11%
to 80% in the samples deformed at 982 1C, the misorientation
values increased accordingly from 0.1681 to 0.3971. Microstructu-
rally, the underlying grain structures of these samples were also
observed to change as a function of temperature and strain.
As deformation occurred in the IN600 samples tested at 25 1C
and 538 1C, the macroscopic strains were accommodated via
plastic flow and the originally equiaxed grains became compressed
and elongated in the direction perpendicular to the applied stress.
This led to increasingly higher magnitudes of intragranular mis-
orientation that affected the ability to index and generate statis-
tically significant EBSD maps of samples deformed to 51% and 80%
strain at 25 1C and 538 1C.
For the IN600 samples deformed at 760 1C, however, dynamic
recrystallization was observed to occur following deformation to
28% strain and the fraction recrystallized increased progressively
as a function of strain, Fig. 3a–d. Consistent with the absence of
strain hardening, dynamic recrystallization resulted in only a
modest increase in the average intragranular misorientation
within this set of samples. Following deformation to 80% strain
at 760 1C, the microstructure consisted entirely of equiaxed grains
as the structure had completely undergone dynamic recrystalliza-
tion. Increasing the deformation temperature from 538 1C to
760 1C initiated dynamic recrystallization, but increasing the
deformation temperature to 982 1C was found to suppress
dynamic recrystallization as mechanisms responsible for dynamic
recovery dominated. No evidence of grain refinement via dynamic
recrystallization was observed in samples deformed at 982 1C,
Fig. 3e–h. Prior to annealing, a substantial amount of grain growth
had already occurred as the average size of the grains following
deformation at 982 1C is 14.5 μm, which is significantly larger than
the 7.7 μm grain size measured in the starting condition. The
kinetics of dynamic recovery at this temperature allowed for
accelerated annihilation of dislocations as no strain hardening
and only a modest increase in intragranular misorientation was
observed.
Following annealing of the as-deformed samples at 1025 1C, the
microstructures of the samples were once again characterized
using EBSD techniques. Band contrast maps of the annealed
samples are presented in Fig. 4 and the Σ3 boundaries are high-
lighted. Depending on the deformation temperature and strain,
drastic differences in the microstructure of the IN600 samples
were observed. For the samples deformed at 25 1C, static recrys-
tallization was noted following annealing of samples deformed to
strain levels greater than 11%, Fig. 4b and c. A bi-modal grain size
distribution was observed in these samples and the fraction
recrystallized increased as a function of the overall strain. No
recrystallization was observed in the 25 1C sample deformed to
11% strain as the microstructure was observed to consist of
equiaxed grains measuring approximately 17.2 μm.
The IN600 samples deformed at 538 1C exhibited microstruc-
tures that were similar to the samples deformed at 25 1C following
 B. Li, S. Tin / Materials Science & Engineering A 603 (2014) 104–113 107

Fig. 3. Orientation images from as deformed samples of IN600 at (a) 760 1C/11% strain, (b) 760 1C/28% strain, (c) 760 1C/51% strain, (d) 760 1C/80% strain, (e) 982 1C/11% strain,
(f) 982 1C/28% strain, (g) 982 1C/51% strain, (h) 982 1C/80% strain.
108 B. Li, S. Tin / Materials Science & Engineering A 603 (2014) 104–113

Fig. 4. Band contrast maps showing the grain structure and density of Σ3 boundaries following a one hour anneal at 1025 1C of the IN600 samples deformed at (a) 25 1C/11%
strain, (b) 25 1C/28% strain, (c) 25 1C/80% strain, (d) 538 1C/11% strain, (e) 538 1C/28% strain, (f) 538 1C/80% strain, (g) 760 1C/11% strain, (h) 760 1C/28% strain, (i) 760 1C/80%
strain, (j) 982 1C/11% strain, (k) 982 1C/28% strain and (l) 982 1C/80% strain.

Table 3
Grain boundary character of samples deformed at different temperatures and strain
followed by a one hour anneal at 1025 1C.

Deformation Average Σ3 Twin Length of Length of

temperature/ grain size, fraction twins, μm random
strain μm (%) boundaries, μm

As-received 7.7 36 13,211 23,314

25 1C/11% 17.2 64 13,769 7757
25 1C/28% 12.2 48 13,747 14,915
25 1C/51% 11.6 46 11,802 13,783
25 1C/80% 13.2 48 9312 10,096
538 1C/11% 25.3 69 14,141 6403
538 1C/28% 12.5 49 11,502 11,927
538 1C/51% 12.4 50 11,005 12,937
538 1C/80% 16.0 55 10,977 8833
760 1C/11% 35.0 73 13,704 5023
760 1C/28% 11.1 47 13,676 15,312
760 1C/51% 13.9 49 10,417 11,056
760 1C/80% 17.6 59 10,585 7502
Fig. 5. Surface plot showing the measured Σ3 boundary length following a one
982 1C/11% 52.2 81 10,406 2402
hour anneal at 1025 1C of the IN600 samples deformed to various strains at
982 1C/28% 25.8 59 10,727 7417
different temperatures.
982 1C/51% 22.2 59 10,025 6904
982 1C/80% 24.8 64 10,973 6172

As shown in Fig. 3, deformation at 760 1C and 982 1C resulted in

annealing, Fig. 4d–f. With an average grain size of 25.3 μm, grain
growth occurred in the sample deformed to 11% strain at 538 1C
and annealed. Higher levels of strain again resulted in static
recrystallization and refinement of the underlying grain structure.
Fig. 4e shows the partially recrystallized microstructure of the
sample deformed to 28% at 538 1C after annealing. Straining the
sample to 80% at 538 1C accelerates the rate of recrystallization
during annealing and a coarser, more uniform grain structure was
observed, Fig. 4f.
dynamic recrystallization at strain levels above 11%. Annealing of
these samples at 1025 1C induced grain growth of the dynamically
recrystallized grains and promoted recovery or further recrystalli-
zation to alleviate any residual strain within the microstructure,
Fig. 4h–i, k–l. The samples deformed to 11% strain at 760 1C and
982 1C did not appear to recrystallize as grain growth increased
the average grain size of these samples to 35.0 μm and 55.2 μm,
respectively, following annealing, Fig. 4g and j. Interestingly, these
two samples also contained significantly high fractions of internal
 B. Li, S. Tin / Materials Science & Engineering A 603 (2014) 104–113
Fig. 6. Surface plot showing the measured random boundary length following a
one hour anneal at 1025 1C of the IN600 samples deformed to various strains at
different temperatures.
Fig. 7. Surface plot showing the variation in grain size following a one hour anneal
at 1025 1C of the IN600 samples deformed to various strains at different
temperatures.
Fig. 8. Surface plot showing the length fraction of Σ3 boundaries following a one
hour anneal at 1025 1C of the IN600 samples deformed to various strains at
different temperatures.
twin boundaries. In the other samples, the majority of twin
boundaries were observed to either bisect the grain or originate
from grain boundaries.
Results from the assessment of the character of the grain bound-
aries in the various samples are summarized in Table 3 and Figs. 5–8.
Over a constant scan area of 350 μm  350 μm, the total Σ3 boundary
109
length in each of the samples was averaged and plotted in the form of
a surface plot as a function of both strain and deformation tempera-
ture, Fig. 5. Characterization of the as-deformed samples revealed that
in all instances, the overall length of the Σ3 boundaries decreased
modestly when compared to the total length of Σ3 boundaries in the
as-received IN600 material prior to deformation (13,211 μm). Follow-
ing annealing, however, Σ3 boundaries were created and the mea-
sured length of Σ3 boundaries in samples deformed at 25 1C/11%
strain, 538 1C/11% strain, 760 1C/11% strain, 25 1C/28% strain, 760 1C/
28% strain increased modestly to length values greater than 13,211 μm.
The Σ3 boundary lengths in all other samples were measured to be
less than 13,211 μm, with the sample deformed at 25 1C/80% strain to
have the lowest Σ3 boundary length of 9312 μm.
The length of the random boundaries for all of the annealed IN600
samples was also averaged and plotted in the form of surface plot,
Fig. 6. As the initial grain size of the as-received material was 7.7 μm,
the overall grain length of random grain boundaries over a
350 μm  350 μm scan area was 23,314 μm. Grain growth occurred
in all of the deformed IN600 samples following annealing and this led
to an overall reduction in the length of the random grain boundaries.
Since samples deformed to strains of 28% and 51% at deformation
temperatures of 25 1C, 538 1C and 760 1C were observed to recrystal-
lize either partially or fully, the resulting grain refinement served to
create random grain boundaries and counteract the reduction attrib-
uted to grain growth. This is reflected in by the bulge in the center of
the surface plot in Fig. 5. Overall, the average length of the random
grain boundaries was observed to be inversely proportional to the
average grain sizes measured for the specimens, Fig. 6. Large grain
sizes correspond to relatively low values of the random grain
boundary length while the fine grains were associated with the higher
values. The average grain size was observed to increase as a function of
temperature, but decrease as a function of increasing strain.
With quantification of the average lengths associated with
random and Σ3 boundaries in the various samples, the length
fraction ratio (total Σ3 boundary length/total length of all bound-
aries) was plotted, Fig. 7. By comparing the length fraction ratio,
samples containing large Σ3 boundary lengths and relatively small
random boundary lengths were readily revealed. Irrespective of
the deformation temperature, the samples deformed to 11% all
exhibited relatively large grain sizes and Σ3 lengths after anneal-
ing. This resulted in the Σ3 length fractions ranging between 64%
and 81% for samples deformed at 25 1C to 982 1C, respectively.
These values are significantly higher than the Σ3 length fraction of
36% measured in samples of IN600 in the as-received or hot rolled
condition. With recrystallization and grain refinement occurring
during deformation or following annealing in the samples
deformed to strains of 28% and 51% at temperatures of 25 1C,
538 1C and 760 1C, the resulting increase in the random grain
boundary length was responsible for a decrease in the Σ3 length
fractions. The microstructures of samples deformed to 80% strain
at 25 1C, 538 1C and 760 1C followed by the 1025 1C anneal were
fully recrystallized and experienced some grain growth. Under
these conditions, the Σ3 length fractions were observed to increase
modestly. As shown in Fig. 2e–h, no evidence of dynamic recrys-
tallization was observed following deformation to the various
strain levels at 982 1C. The samples deformed at 982 1C exhibited
the largest average grain sizes, Fig. 6, and the highest Σ3 length
fractions, Fig. 7, following annealing. Although grain sizes of the
samples deformed at 982 1C are significantly larger than those
deformed at lower temperatures, they are still smaller when
compared to the average grain size observed in undeformed
samples of IN600 that were subjected to the identical annealing
heat treatment at 1025 1C. Fig. 9 shows the electron band contrast
image of an undeformed sample of IN600 annealed at 1025 1C for
one hour. The average grain size was found to increase from 7.7 μm
to 69.9 μm as a result of the annealing treatment only.
110 B. Li, S. Tin / Materials Science & Engineering A 603 (2014) 104–113
Fig. 9. Electron band contrast image of an undeformed sample of IN600 annealed
at 1025 1C for one hour.
Fig. 10. Changes in grain size and the character of the grain boundaries of IN600
deformed at 25 1C to 25% strain as a function of annealing time.
The effect of annealing time on the grain boundary character of
IN600 was also investigated as part of this study, Fig. 10. Using
samples deformed to 28% strain at 25 1C, annealing times at
1025 1C were varied from 5 min to 60 min. Starting with the an
average grain size of 7.7 μm, annealing of the deformed sample for
5 min resulted primarily in grain growth as the average grain size
increased to 10 μm. As the grain size increased, there was a
corresponding decrease in both the length of Σ3 boundaries and
the length of random grain boundaries. The average length of the
random grain boundaries was observed to decrease significantly
from 23,314 μm to 14,110 μm while the average length of Σ3
boundaries decreased slightly from 13,211 μm to 12,242 μm.
Extending the annealing time to 18 and 38 min induced recrys-
tallization as the average grain size decreased to 8.6 μm and
9.1 μm, respectively. The formation of new grains during recrys-
tallization also creates random grain boundaries and increases
their overall length. Partial recrystallization was observed follow-
ing the 18 min anneal and nearly full recrystallization occurred
after 38 min. In the partially recrystallized structure associated
with the 18 min annealed sample, a bi-modal grain size distribu-
tion exists in which relatively fine recrystallized grains coexist
with some of the original grains that were able to undergo grain
growth. Growth of the original grains contributes to the formation
and lengthening of Σ3 boundaries, while the formation of recrys-
tallized grains extends the length of random grain boundaries.
As recrystallization progresses, the original grains that have grown
slightly and contain high proportions of Σ3 boundaries are replaced
by newly formed recrystallized grains. This results in the simulta-
neous decrease in Σ3 boundary length and increase in random
boundary length seen in the sample annealed for 38 min at 1025 1C.
Annealing these samples for 60 min resulted in complete or full
recrystallization and growth of the recrystallized grains. As the
recrystallized grains grow, the grain size increases and annealing
twins form. This results in a decrease in the random boundary
length and an increase in the Σ3 boundary length.
4. Discussion
Controlling the character or grain boundaries in polycrystalline
materials, or grain boundary engineering, has been demonstrated
to enhance the physical and mechanical properties of a wide
variety of low stacking fault energy materials. Populating the grain
boundary network with a high proportion of low energy Σ3
boundaries and breaking up the connectivity of the random grain
boundary network has been key to achieving these improved
properties [11–19]. Conventional approaches for grain boundary
engineering rely on multiple iterations of cold work followed
by annealing to exploit strain annealing mechanisms for both
the formation of Σ3 boundaries and their migration into the
random boundary network. Although effective, these conventional
approaches are somewhat limited and not economically viable for
the production of physically large and complex shaped compo-
nents. Using IN600 as a model alloy system, this study was aimed
at better understanding the effects of deformation temperature
and strain on the formation of Σ3 boundaries following annealing.
4.1. Strain annealing
Deformation of the samples to 11% strain followed by annealing
at 1025 1C did not result in any recrystallization phenomena and
strain annealing was responsible for a significant increase in both
the Σ3 length fraction and grain size, Figs. 6 and 7. Although
increasing deformation temperature did result in an increase in
the average grain size following annealing, Fig. 4a, d, g and j, the
extent of grain growth in the deformed and annealed samples was
significantly smaller when compared to an as-received, unde-
formed sample of IN600 that was subjected to a nominally
identical annealing treatment, Fig. 8. As the deformation tempera-
tures increased, increasing levels of dislocation recovery occurred
and led to smaller degrees of intragranular misorientation occur-
ring within the microstructures of the samples. Both grain growth
and the degree of dislocation recovery were found to effect the
formation of S3 boundaries in this set of samples. Compared to the
average total length of Σ3 boundaries measured in the as-received
or undeformed samples, a modest increase in the overall length of
Σ3 boundaries was measured following annealing of the samples
deformed to 11% strain at 25 1C, 538 1C and 760 1C. Since char-
acterization of the as-deformed specimens showed a reduction in
the length of Σ3 boundaries, these results clearly indicate that the
majority of Σ3 boundaries observed within the microstructures
formed during the annealing process. Σ3 boundaries have been
reported to form as a result of dislocation interactions between the
induced plastic strain and the grain boundaries. Varying the
deformation temperature from 25 1C to 982 1C likely affected
the nature of the dislocation substructure. Consistent with the
hardening behavior observed in the flow stress curves in
Fig. 2, deformation at 25 1C and 538 1C to a strain of 11% most
likely involves predominately planar slip as dislocations are
 B. Li, S. Tin / Materials Science & Engineering A 603 (2014) 104–113
predominately confined to their slip planes. As temperatures
increase to 760 1C and 982 1C, thermal activation enables disloca-
tion climb and the formation of low energy sub-grain networks.
Interestingly, the overall length of Σ3 boundaries in samples
deformed to 11% at 25 1C, 538 1C and 760 1C were nearly equiva-
lent, but their grain sizes and corresponding length of random
boundaries in these samples varied. Among these samples, the
observed increases in the Σ3 length fractions can be largely
attributed to reductions in the length of the random boundaries
as opposed to increases in Σ3 length. Additionally high relative
proportions of internal twins, or self-contained twins that are
present within the grains, were observed in samples deformed at
760 1C and 982 1C. These observations were consistent with low
mobilities associated with Σ3 boundaries during grain growth.
As expected, strain annealing mechanisms were responsible for
increasing the overall length and length fraction of Σ3 boundaries
in the samples deformed to 11% strain, but increases in grain size
due to elevated deformation temperatures also contributed to
increasing the Σ3 length fractions.
4.2. Static recrystallization
Recrystallization events are typically avoided during grain
boundary engineering as the nucleation and growth of recrystal-
lized grains tends to populate the microstructure with high
fractions of high angle or random grain boundaries [6,8]. Σ3
boundaries may form in recrystallized microstructures, but will
likely occur naturally as annealing twins induced during growth of
the recrystallized grains. The proportion of Σ3 annealing twin
boundaries will scale proportionally as a function of grain size and
forming high proportions of them in fine grained microstructures
will be limited as dislocation – grain boundary interaction events
are absent in recrystallized microstructures. A bi-modal grain size
distribution characteristic of partial recrystallization was observed
to occur during annealing of samples deformed to 28% and 51%
strain at 25 1C and 538 1C, Fig. 4b and e. Due to the relatively small
size and lack of Σ3 boundaries in the newly recrystallized grains,
the fraction of random grain boundaries increased, Fig. 6, while
the grain size decreased, Fig. 7. Since the recrystallized grains are
also replacing the original grain structure that contained moderate
fractions of Σ3 boundaries, the overall length of the Σ3 boundaries
in the partially recrystallized specimens also decreased, Fig. 5.
Increasing the deformation strain to 80% produced fully recrystal-
lized microstructures after annealing, Fig. 4c and f. Once fully
recrystallized, the new strain free grains do grow during annealing
and some Σ3 annealing twins form. Compared to the samples
deformed to 11% at 25 1C and 538 1C, grain refinement does occur
following annealing of the 80% deformed samples, Fig. 7. As there
was no residual strain or significant dislocation density within the
grains to stimulate the formation of Σ3 boundaries during anneal-
ing the average overall Σ3 length and Σ3 length fraction are
relatively low in these fully recrystallized samples, Figs. 5 and 8.
4.3. Dynamic recrystallization
During static recrystallization, dislocation recovery and recrystalli-
zation are limited to occurring following deformation and during the
subsequent heat treatment [30–35]. In these instances, the stored
strain energy serves as the driving force for the nucleation and growth
of strain free grains. Dynamic recrystallization, however, occurs when
the deformation temperatures and strain rates enable recovery and
recrystallization events to occur while strain is being accumulated. In
these instances, newly recrystallized grains form during deformation.
As they form and grow, these initially strain free grains are also able to
accommodate additional straining. Unlike statically recrystallized grain
structures, dynamically recrystallized grains may contain significant
111
dislocation densities following deformation. These residual dislocation
densities in dynamically recrystallized grain structures were found to
affect the resulting grain boundary character and formation of Σ3
boundaries following annealing. As seen in Fig. 3a–d, deformation of
IN600 at 760 1C resulted in dynamic recrystallization. The fraction of
the microstructure that had dynamically recrystallized was propor-
tional to the strain and the microstructure has completely recrystal-
lized as the sample was being strained to 80%. Consistent with the
intragranular misorientations measured in these samples, Table 2,
remnant plastic deformation was stored within the microstructure.
Annealing of these samples resulted in strain induced growth of the
dynamically recrystallized grains, Fig. 4h and i. Unlike the highly
strained samples deformed at 25 1C and 538 1C where static recrys-
tallization results in a strain or dislocation free microstructure where
the reduction in surface or interfacial energies drive grain growth,
dynamic recrystallization produced a refined grain structure contain-
ing a sufficiently high strain level or dislocation density that was able
to enhance the formation of Σ3 boundaries during annealing.
Although the overall length of the Σ3 boundaries measured in the
sample deformed to 80% at 982 1C was nominally identical to that
measured in the same sample following annealing, the average grain
size increased from 14.5 μm to 24.8 μm as a result of the annealing,
Fig. 7. The larger grain size also corresponds to a significant reduction
in the overall length of random grain boundaries and results in a net
overall increase in the length ratio of Σ3 boundaries, Fig. 8. Hence,
strain-annealing and dislocation grain boundary interactions that
occur within fully, dynamically recrystallized microstructures do
appear to increase the overall length ratio of Σ3 boundaries at large
magnitudes of strain.
4.4. Dynamic recovery
A deformation temperature of 982 1C corresponds to a homo-
logous temperature, Tm, of 0.77 for IN600. Considering that the
microstructure of IN600 consists of a solid solution strengthened,
single phase austenitic structure, dynamic recovery mechanisms
can dominate and accommodate high levels of strain during high
temperature deformation [36,37]. Since there was no evidence of
grain refinement in the microstructures immediately following
deformation at 982 1C, Fig. 3e–h, dynamic recovery was likely the
dominant mechanism responsible for accommodating the
imposed strain. The lack of hardening observed in the flow stress
curves, Fig. 2, and the relatively low magnitude of the average
intragranular misorientations measured in the as-deformed
microstructures, Table 2, were all consistent with dynamic recov-
ery occurring during deformation. As the samples were being
deformed at 982 1C, the macroscopic strains were accommodated
by dislocations rearranging themselves into low energy configura-
tions or three dimensional subgrain networks. The enhanced
mobility of dislocations at 982 1C enabled dislocation climb and
annihilation events to occur within the subgrain walls and sup-
press strain hardening and dynamic recrystallization. Interestingly,
deformation at 982 1C did not result in a significant overall
reduction in the measured length of the Σ3 boundaries, although
some grain growth did occur during deformation at 982 1C as the
average grain size increased from an initial size of 7.7 μm to
14.7 μm immediately following deformation to a true strain of
80%. By preserving much of the original Σ3 boundary length while
simultaneously reducing the length of random grain boundaries
via grain growth during deformation, the length fraction of Σ3
boundaries could be increased. The subsequent annealing of the
specimens deformed at 982 1C was found to induce some addi-
tional grain growth and result in a corresponding reduction of the
random grain boundary length, but did not serve to generate
additional Σ3 boundary length. Based on these observations, it
appears that under deformation conditions where dynamic
112 B. Li, S. Tin / Materials Science & Engineering A 603 (2014) 104–113
Fig. 11. Contour map showing the length fraction of Σ3 boundaries as a function of
deformation temperature and strain. Depending on the processing parameters,
different mechanisms may dominate and effect the development of microstructure
and grain boundary character.
recovery dominates, Σ3 boundaries are neither created nor
destroyed. This permits samples deformed at 982 1C to 11% strain
followed by an annealing cycle to exhibit a Σ3 length fraction of
81% at a grain size of 52.2 μm. When compared to the grain
boundary character of undeformed samples of IN600 that were
annealed using the same thermal cycle, Fig. 8 (79% Σ3 length
fraction with a grain size of 69.9 μm), mechanisms associated with
dynamic recovery at 982 1C were responsible for increasing the Σ3
length fractions while maintaining a modestly reduced grain size.
The formation of denser subgrain networks and following defor-
mation at strains between 25% and 80% further restricts the grain
boundary mobilities during annealing as the average grain sizes in
these samples are on the order of 22.2–25.8 μm. Despite the
smaller average grain sizes, Σ3 length fractions between 59% and
63% were obtained in these samples.
To summarize, a preliminary process map spanning a broad range
of temperatures and strains for grain boundary engineering of IN600
was created, Fig. 11. Although the benefits associated with grain
boundary engineering are substantial, process routes that rely on
strain annealing mechanisms that are enabled via multiple iterations
of cold deformation followed by annealing are not commercially viable
and only utilized in a limited number of applications. The present
investigation was aimed at quantifying the effects of different strain
accommodation mechanisms on the formation of Σ3 boundaries.
Consistent with other published studies, strain annealing or deforma-
tion to relatively low levels of strain (11%) followed by annealing was
noted to significantly increase the population of Σ3 or twin bound-
aries. Here, the effect of increasing deformation temperature largely
contributed to accelerate the grain growth kinetics and coarser grained
structures were found to possess higher Σ3 length fractions. Increasing
the strain above 11% while maintaining deformation temperatures
between 25 1C and 538 1C led to static recrystallization of the grain
structure during annealing. Processing parameters that result in static
recrystallization or the formation of new grains that increase the
overall random boundary length need to be avoided as this contributes
to a reduction of the Σ3 length ratio. Consistent with other reported
studies [38], continuous dynamic recrystallization mechanisms
become operative at strains 411% and may potentially be utilized
for increasing the length fraction of Σ3 boundaries following complete
recrystallization at high strains. The Σ3 length fractions in partially
recrystallized microstructures tend to be comparatively low as the
presence of small, recrystallized grains contributes primarily to
increasing the length of the random grain boundaries. Continuous
dynamic recrystallization involves the formation of subgrain structures
and the rotation of the subgrain structures to form discrete recrys-
tallized grains. However, unlike the grain refinement mechanisms
associated with static recrystallization that minimize all of the
dislocations and stored strain energy within the microstructure upon
recrystallization, grains formed via continuous dynamic recrystalliza-
tion may still contain some residual dislocations that dissociate and
interact with grain boundaries to induce the formation of Σ3 twin
boundaries during annealing. This was observed during annealing of
the sample deformed at 760 1C to 80% strain as the overall Σ3 length
fraction increased once the microstructure was fully recrystallized.
Processing parameters conducive for dynamic recovery also appear to
be capable of increasing the proportion and length fraction of Σ3
boundaries. No grain refinement occurs under these conditions and
the majority of the Σ3 boundaries are preserved during deformation.
Mechanisms associated with dynamic recovery also reduce the grain
boundary mobilities and restrict the extent of grain growth that occurs
during the annealing cycle. Based on these findings, both dynamic
recrystallization and dynamic recovery mechanisms may potentially
be exploited to develop commercially viable processes for grain
boundary engineering of high performance alloys. As an outlook in
order to utilize the benefits associated with grain boundary engineer-
ing, Σ3 boundaries need to be migrated into the random grain
boundary network in order to break up their connectivity.
To accomplish this, an additional deformation anneal iteration would
likely need to be employed and such investigations are currently on-
going.
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