Materials Transactions, Vol. 53, No. 4 (2012) pp.

658 to 661
2012 The Japan Institute of Metals

Irregular or Smooth Grain Boundaries Evolved

after Secondary Recyrstallization of Fe3%Si Steel
Hyung-Ki Park1,2, Chang-Soo Park1, Tae-Wook Na1, Chan-Hee Han2 and Nong-Moon Hwang1,+
1

Department of Materials Science and Engineering, Seoul National University, Seoul 151-742, Korea
POSCO Technical Research Laboratories, POSCO, Pohang, Korea

Irregular or smooth grain boundaries after secondary recrystallization are formed depending on whether interpass aging is adopted or not
during cold rolling of Fe3%Si steel. Interpass aging induces the primary texture of high intensity of {111}112 and {411}148 orientations,
which have a 9 relation with respect to the Goss orientation and therefore are favorable for Goss grains to grow by solid-state wetting. Under
this condition Goss grains come in contact with each other by wetting without leaving any small grains in between, resulting in irregular
boundaries. [doi:10.2320/matertrans.M2011268]
(Received August 30, 2011; Accepted December 27, 2011; Published February 15, 2012)
Keywords: abnormal grain growth, secondary recrystallization, grain boundary wetting, interpass aging

1.

Introduction

Abnormal grain growth (AGG), which is also referred to as

secondary recrystallization, often occurs in polycrystalline
metals. During AGG only a few grains grow abnormally
consuming the neighboring matrix grains. This phenomenon
is particularly famous in Fe3%Si alloy because the core loss
of Fe3%Si can be minimized by properly controlling AGG.
Since the rst report of the selective AGG of Goss grains in
Fe3%Si alloy by Goss in 1935,1) many efforts have been
made to understand the mechanism because of its technological importance and scientic interest. In spite of intensive
efforts, however, the underlying principle has not yet been
claried.
The selective AGG of Goss grains has been approached
mainly based on the high mobility of grain boundaries
shared by Goss grains with other matrix grains.24) However,
misorientation analyses between Goss grains and matrix
grains do not support this assumption.5,6) On the other hand,
Hwang et al.710) has suggested the sub-boundary enhanced
solid-state wetting for selective AGG of Goss grains, where
the growth advantage of abnormally-growing grains is
approached in terms of grain boundary energy. According
to this mechanism, if a grain has sub-boundaries of very low
energy, the probability of solid-state wetting becomes so high
that the grain containing sub-boundaries undergo selective
AGG. In relation to this possibility, Park et al.11) observed
that sub-boundaries exist exclusively in abnormally-growing
Goss grains using transmission electron microscopy. Also,
Dorner et al.12) conrmed the existence of sub-boundaries
exclusively within Goss grains after primary recrystallization
of a sheet sample reduced 89% by cold rolling of a single
crystal of Goss orientation. The solid-state wetting mechanism could successfully explain many puzzling structures
such as the formation of island and peninsular grains at the
growth front7,13) and the pancake-shaped growth of Goss
grains in highly grain-oriented electrical steel of Fe3%Si.14)
Normally smooth grain boundaries are evolved after
secondary recrystallization of Fe3%Si steel, whereas highly
+

Corresponding author, E-mail: nmhwang@snu.ac.kr

irregular grain boundaries are evolved if interpass aging is

adopted during cold rolling. Interpass aging, which refers to
short time aging treatments at 150300C between passes
of the single stage cold rolling has been reported to improve
the magnetic properties of highly grain-oriented electrical
steel.1517) Interpass aging has been studied extensively but
its effect is not clearly understood. Quite different microstructures are evolved after secondary recrystallization,
depending on whether interpass aging is adopted or not:
highly irregular grain boundaries are produced with interpass
aging whereas smooth grain boundaries are produced
without interpass aging. The purpose of this work is to
study why irregular grain boundaries are evolved after
secondary recrystallization in the Fe3%Si sheet specimens
undergoing interpass aging. Rather than studying the benecial effect of the interpass aging, our study is limited to the
mechanism as to the different morphology evolution of grain
boundaries between the two processes with and without
interpass aging.
2.

Experimental Procedure

An ingot of Fe3%Si, which employed AlN as an inhibitor

of grain growth to produce the highly grain-oriented
electrical steel, was used as a starting material. The steel
ingot was hot rolled to 2.3 mm and the thickness was further
reduced to 0.3 mm by one stage cold rolling method, which
is equivalent to a total engineering thickness reduction of
= 87%. To investigate the effect of interpass aging during
cold rolling on the microstructure evolution after secondary
recrystallization, specimens with and without interpass aging
were prepared during cold rolling. The specimen with
interpass aging was given four separate treatments for
5 min at 250C at intermediate thicknesses of 1.5, 0.95,
0.62, and 0.43 mm. Hereafter, these two specimens with and
without interpass aging will be referred to as A and B,
respectively.
Precipitates play a critical role in inducing AGG. In highly
grain-oriented electrical steel, precipitates such as AlN serve
as a grain growth inhibitor at low temperature and AGG
occurs when precipitates start to dissolve or coarsen at high

Irregular or Smooth Grain Boundaries Evolved after Secondary Recyrstallization of Fe3%Si Steel

Fig. 1

The microstructures after secondary recrystallization (a) with and (b) without interpass aging during cold rolling.

temperatures. The effect of AlN on secondary recrystallization would not be changed by such a low temperature heat
treatment by interpass aging, and therefore would be the
same in both specimens. The two specimens were annealed at
850C for 150 s for decarburization and primary recrystallization. These specimens underwent a stepwise heat treatment
at 15C/h up to 1200C and held for 10 h for secondary
recrystallization. The sheet specimens were etched with
50% water50% HCl at 80C to identify the grain boundaries of abnormally-grown grains.
To investigate the texture after primary recrystallization at
the surface layer, where Goss nuclei for AGG were
distributed, the two specimens after primary recrystallization
with a thickness of 0.3 mm were polished down to a thickness
of 0.26 mm. The macrotextures were examined by a
conventional X-ray texture goniometer (D8 Advance,
Bruker) using Co K radiation. From three incomplete pole
gures, the three-dimensional orientation distribution function (ODF) was calculated by the series expansion method
and presented in the orientation space dened by the Euler
angles (1, , 2).18) To determine the orientation relationships of individual grains relative to the Goss orientation,
{110}001, the specimens after primary recrystallization
were analyzed by electron backscattered diffractometer
(EBSD) attached to a eld-emission scanning electron
microscope (JSM-6500F, JEOL). EDAX/TSL software was
used to analyze the orientation.
3.

659

Results and Discussion

Figures 1(a) and 1(b) are the microstructures of A and

B, respectively, after secondary recrystallization and its
corresponding (100) and (110) pole gures are shown on the
right inset of each gure. The pole gures indicate that
abnormally-grown grains in both specimens had a Goss

orientation. Figure 1(a) for A with interpass aging shows

highly irregular grain boundaries whereas Fig. 1(b) for B
without interpass aging shows smooth grain boundaries. This
different grain boundary morphology would come from the
different surroundings of Goss grains in the texture after
primary recrystallization, which affects the growth rate of the
Goss grains during secondary recrystallization. Indeed,
Homma and Hutchinson19) reported the effect of the texture
after primary recrystallization on the growth rate of the Goss
grains. Also, in the viewpoint of solid-state wetting
mechanism, the primary texture affects the growth rate of
the Goss grains because it determines the distribution of
the orientation relation between the Goss grains and matrix
grains.14) Therefore, to clarify the different grain boundary
morphology between the A and B, the textures after
primary recrystallization were compared by X-ray diffraction.
Figures 2(a) and 2(b) show ODFs of A and B after
primary recrystallization, respectively. Mainly evolved orientations were the same between the two specimens.
However, the texture of B was more broadly distributed
than that of A. In both specimens, {111}112 and
{411}148 orientations developed during primary recrystallization. Heavily cold rolled body-centered cubic steel,
consisting of -ber (RD // 110) and -ber (ND //
111) textures, is known to have a tendency to generate
{111}112 and {411}148 orientations after primary
recrystallization.20) The stored energy of the grains developed
after cold rolling is maximal in the {111}112 orientation,
resulting in preferred nucleation of this orientation.21) The
{411}148 orientation was experimentally shown to nucleate in the deformed -ber texture.20,22) Although the
development of the {411}148 texture is well established,
its formation mechanism has not been understood clearly.23)
To clarify the difference of the texture in more detail, the
ODF sections at 2 = 45 of the specimen with and without

660

H.-K. Park, C.-S. Park, T.-W. Na, C.-H. Han and N.-M. Hwang

Fig. 2 ODFs of the specimens (a) with and (b) without interpass aging after primary recyrstallization. To clarify the difference of the
texture in more detail, ODF sections at 2 = 45 of the specimen (c) with and (d) without interpass aging were magnied.

interpass aging, which include orientations mainly evolved in

body-centered cubic iron, were magnied as shown in
Figs. 2(c) and 2(d), respectively. The drastic difference in
the texture intensity between the two specimens is revealed.
Compared with the main texture after primary recrystallization of B, that of A has a signicantly high intensity of
orientations near {111}112 and {411}148, which have a
9 relationship with respect to the Goss orientation. Indeed,
the changes of texture after primary recrystallization by
interpass aging were reported.1517) In relation to this change
of texture, Matsuo et al.15) reported that interpass aging
during cold rolling causes free carbon to pin dislocations,
which inhibits a complex slip such as cross-slip, and
promotes the deformation by a single slip. Therefore,
interpass aging would affect the deformation behavior during
cold rolling, which might again affect the change of the
texture after primary recyrstallization.
The difference of the texture determines a percentage of
low energy boundaries relative to the Goss orientation, which
affects the growth rate of Goss grains during secondary
recrystallization. In the mechanism of secondary recrystallization by solid-state wetting, the high growth rate corresponds to the high probability of wetting, which would
depend on the texture after primary recrystallization.14) For

example, if the texture produces a higher percentage of low

energy grain boundaries with respect to the Goss orientation,
the wetting probability of Goss grains increases.7,10) For this,
the percentage of coincidence site lattice (CSL) boundaries,
which would be considered as low energy boundaries,24,25)
relative to the Goss orientation was calculated using EBSD.
In fact, the crystallographic relationship as well as the
boundary plane should be considered to determine the
boundary energy.26) However, the data for the boundary
plane are not available; we had to assume that the boundaries
with CSL relationship have low energy.
Figure 3 shows the percentage of CSL boundaries relative
to the Goss orientation in the specimens after primary
recrystallization. values were calculated up to 29b using
Brandons criteria.27) In order to get statistically reliable data,
a sufciently large number of grains were examined: 9105
and 8926 grains in the A and B, respectively. The black
and gray colored bars indicate the percentage of the matrix
grains with the CSL relationship in the A and B,
respectively. The specimen with interpass aging had a higher
percentage of CSL boundaries, especially low index (3
9), than that without pass aging. The higher percentage of
9 boundary can be understood by the primary texture of
the specimen with interpass aging which had a high intensity

Irregular or Smooth Grain Boundaries Evolved after Secondary Recyrstallization of Fe3%Si Steel

4.

661

Conclusion

In conclusion, the Fe3%Si sheet steel, which underwent

interpass aging during cold rolling, shows highly irregular
grain boundaries after secondary recrystallization. This aspect
is attributed to the high growth rate of Goss grains by solidstate wetting, which is again attributed to a higher percentage
of low energy boundaries relative to the Goss orientation
resulted from interpass aging.
Acknowledgements

Fig. 3 The percentage of the matrix grains with the CSL relation with the
Goss grain calculated using Brandons criteria. The black color indicates a
CSL percentage of the specimen with interpass aging and the gray one
indicates that without interpass aging.

of the {111}112 and {411}148 orientations having 9

relation with the Goss orientation.
If 19 boundaries in Fig. 3 are assumed to have low
energy enough for the Goss grains to undergo solid-state
wetting, the difference in their percentage between A and
B is worth noticing. The percentage of 19 boundaries
in Fig. 3 is 8.62% in A and 6.9% in B, which suggests that
the wetting probability in A should be higher than that in
B. This means that the growth rate of Goss grains by solidstate wetting in A would be higher than that in B due to its
higher percentage of low energy boundaries. Therefore, the
rate of secondary recrystallization in A would be higher
than that in B.
In the case of A, an abnormally-growing Goss grain
comes in contact with another abnormally-growing Goss
grain by solid-state wetting without leaving any small grains
in between, before the appreciable normal grain growth
(NGG) occurs among matrix grains. It should be noted that
the growth front of Goss grains growing by solid-state
wetting is highly irregular as featured by very high frequency
of peninsular grains.7,13) As a result, the grain boundaries of
A, whose growth front proceeds by solid-state wetting,
would be highly irregular as shown in Fig. 1(a).
In the case of B, however, the rate of secondary
recrystallization is relatively low and some NGG of matrix
grains would occur before abnormally-growing Goss grains
meet each other during secondary recrystallization. When
NGG occurs, high energy boundaries between the matrix
grains are replaced by low energy boundaries. If the matrix
grain boundaries have predominantly low energy, solid-state
wetting is not favored.8) In this condition, the abnormallygrowing Goss grains undergo further growth not by solidstate wetting but by the non-wetting mode, where the
boundary migrates by the difference in the grain boundary
curvature. Therefore, the microstructure after secondary
recrystallization is similar to that of NGG with smooth grain
boundaries as shown in Fig. 1(b).

This work was nancially supported by POSCO Technical

Research Laboratories.
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