Journal of Magnetism and Magnetic Materials 507 (2020) 166849

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Journal of Magnetism and Magnetic Materials

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Primary recrystallization characteristics and magnetic properties T

improvement of high permeability grain-oriented silicon steel by trace Cr
addition
⁎
Yang Gaoa,b, Guang Xua,c, Xiaolong Guob, Guangqiang Lia,d, , Yong Wanga,d
a
State Key Laboratory of Refractories and Metallurgy, Wuhan University of Science and Technology, Wuhan, Hubei 430081 China
b
National Engineering Research Center for Silicon Steel, Wuhan, Hubei 430080, China
c
Center for Advanced Steels, International Research Institute for Steel Technology, Wuhan University of Science and Technology, Wuhan, Hubei 430081 China
d
Key Laboratory for Ferrous Metallurgy and Resources Utilization of Ministry of Education, Wuhan University of Science and Technology, Wuhan, Hubei 430081 China

A R T I C LE I N FO A B S T R A C T

Keywords: The effect of adding of 0.13 wt% Cr on the primary recrystallization and magnetic properties of high perme-
Grain-oriented silicon steel ability grain oriented silicon steel was studied. The results show that trace Cr refined both primary and sec-
Cr ondary grains. The reduction of final grain size resulted in decrease of 5.1%, 4.0% and 3.6% in the average of
Iron loss iron loss during magnetization at 50 Hz, 100 Hz and 200 Hz, respectively. Besides the conventional precipitates,
Primary recrystallization
there were two kinds of Cr-containing nitrides, i.e., the amorphous (Si, Cr) N formed in the matrix, and the
crystalline fcc-CrN formed at grain boundary. These precipitates acted as inhibitors to refine and homogenize
primary grains in the thickness direction. The beneficial {1 1 1} 〈1 1 2〉 texture component increased, while the
components that cannot form high-energy grain boundaries with Goss grains, such as {0 0 1} 〈1 1 0〉 and {1 1 2}
〈1 1 0〉 at different thickness layers decreased after primary recrystallization.

1. Introduction steel [2,3]. Therefore, it is very difficult to further improve the mag-
netic induction of products. On the other hand, researchers and man-
Reducing energy consumption of transformer is crucial to establish ufacturers have also been working on development of techniques for
clean and efficient power grid. Since the energy consumption of thin gauge and ultra-thin gauge less than 0.15 mm [4], high silicon steel
transformer is mainly composed of iron loss of core and copper loss of [2,5,6], optimal texture and morphology of final grains, insulating
coil, the magnetic properties of grain-oriented silicon steel as an im- coating with strong tensile and domain refinement to reduce iron loss.
portant raw material for core making, affects iron loss and energy ef- So in the process of improving product performance, both aspects
ficiency of transformer directly. So transformer manufacturers have should be taken into account.
been working for the grain-oriented silicon steel with excellent mag- The inhibition of normal growth of primary grains results in the
netic properties to meet the requirement of high energy efficiency desirable abnormal growth of Goss grains during secondary re-
transformers. crystallization, leading to the highest magnetic flux density [6]. Mi-
High permeability and low iron loss are two significant specifica- croalloying is an effective method to increase solute elements in silicon
tions of grain-oriented silicon steel with excellent magnetic properties. steel and increase the inhibition of normal grain growth. Therefore,
On the one hand, high permeability grain-oriented silicon steel can magnetic properties in grain-oriented silicon steels can be improved by
improve the design value of transformer flux and reduce the weight of means of microalloying. The mechanisms of its influence on improve-
core. High permeability grain-oriented silicon steel, known as Orient- ment of magnetic properties are in the following aspects: some micro-
core Hi-B developed by Nippon Steel Corporation (NSC) in 1968 and alloying elements can inhibit the normal growth of grains by segrega-
RG-H by Kawasaki steel in 1973 [1], have been produced since the last tion at boundaries, such as Sn [7] and Bi [8]. Some can improve the
century. At present, the magnetic induction B800 of products on the distribution of precipitates by segregation around or precipitating with
market is greater than 1.9 T, which is very close to the saturation traditional AlN and MnS, so that the development of secondary re-
magnetic induction intensity (Bs) of Fe-3% Si grain-oriented electrical crystallization is improved by a better state of inhibitors, such as Sn [9],

⁎
Corresponding author at: P. O. Box 185, Wuhan University of Science and Technology, No. 947, Heping Avenue, Qingshan District, Wuhan City, China.
E-mail address: [email protected] (G. Li).

https://doi.org/10.1016/j.jmmm.2020.166849
Received 23 January 2020; Received in revised form 29 March 2020; Accepted 30 March 2020
Available online 31 March 2020
0304-8853/ © 2020 Elsevier B.V. All rights reserved.
Y. Gao, et al. Journal of Magnetism and Magnetic Materials 507 (2020) 166849

Cr [10,11], and Nb [12]. Techniques of improving magnetic properties crystal nucleus of Goss ({1 1 0} 〈0 0 1〉) grain originates in the sub-
by adding trace Cr to grain-oriented silicon steel have also been dis- surface layer about 1/4 of thickness [15], and at the same time in order
closed by NSC and POSCO. Cr was added to refine the primary grain to compare the difference between the subsurface layer and the middle
and increase the dispersion of precipitations. However, because Cr af- layer, the texture in the 1/4-layer and in the 1/2-layer across thickness
fects the efficiency of decarburization, its contents were not more than were both investigated. The samples were polished to the aim thick-
0.20 wt% by NSC [13] and 0.16 wt% by POSCO [14], respectively, and nesses by mechanical polishing. Textures at different layers were de-
finally the iron loss was reduced and magnetic properties were im- termined by a Rigaku-Dmax-2500 PC X-ray diffractometer. The primary
proved. Usually, according to the slab reheating temperature of before grains were observed by optical microscopy. Furthermore, the average
hot rolling slab, depending on the inhibitor selected such as MnS, AlN, sizes of primary grains in the area of surface to 1/4-layer and in the area
etc., the manufacturing technology of grain-oriented silicon steel can of 1/4-layer to 1/2-layer across thickness were calculated. In order to
divide into three categories, namely the high-temperature slab re- study the characteristics of inhibitors in primary recrystallization, the
heating method (over 1574 K), low-temperature slab reheating method precipitates after nitriding were observed and analyzed by a JEM-
(1374 K to 1474 K) and medium-temperature method (1474 K to 2100F trans-mission electron microscope (TEM), the compositions were
1574 K). In this study, the cold-rolled samples were prepared from hot- analyzed by EDS and the structures were analyzed by electron diffrac-
rolled plates produced by low-temperature slab reheating technology. tion.
However, there are still very limited studies on the effect of trace Cr on In order to study macrostructure and magnetic properties of the
characteristic of primary recrystallization structure and magnetic final products, the samples were treated by high-temperature annealing
properties of low-temperature reheating high permeability grain-or- to develop abnormal growth of secondary recrystallized grains. High-
iented silicon steel so far. Therefore, the objective of the present study is temperature annealing was conducted at 1463 K at pure H2 atmo-
to investigate the results of primary recrystallization characteristics and sphere. Finally, N and S in grain-oriented silicon steel which are very
magnetic properties improvement of low-temperature reheating high harmful to magnetic properties were removed and their contents were
permeability grain-oriented silicon steel by 0.13 wt% Cr addition. both less than 10 ppm. After the insulation coating was applied, the
samples were cut into 30 mm × 300 mm (Parallel to the rolling di-
rection) and annealed at 973℃ for stress-relief under the pure N2. B800
2. Experimental procedures
as an important evaluation standard for magnetic flux density of grain-
oriented silicon steel was measured under magnetic field of 800 A/m.
In order to study the effect of trace Cr on primary recrystallization
Iron loss (P), which is used as the evaluation standard of brand grade
of grain-oriented silicon steel, two kinds of industrial cold-rolled sheets
was also measured during the magnetization at 50 Hz, 100 Hz and
were adopted as the raw materials. The manufacturing process of grain-
200 Hz. In addition, macrostructures of grains in final products were
oriented silicon steel included steelmaking, casting, hot rolling, nor-
observed after removing the insulation coating by acid corrosion.
malizing annealing and cold rolling. The control of alloy content was
Moreover, the magnetic domain structures were observed by powder-
carried out in the secondary refining after steelmaking in basic oxygen
pattern method. In this method, the silicon steel sheet was placed in the
furnace (BOF). For the molten steel with the same composition, Cr was
DC electric field to make the magnetic induction about 0.1 T, and a
added into the experimental batches to reach the target content during
container containing a water-based magnetic fluid was placed on the
the secondary refining. After continuous casting, slabs were reheated
surface of sheets, then the distribution patterns of the magnetic domain
below 1474 K and then hot rolled into the plates of 2.3 mm. Then the
under this condition were observed directly.
hot-rolled plates were treated by two-stage normalizing, that is the
plates were heated up to 1373 K and then air-cooled to 1173 K. After
3. Results and discussions
normalizing, one step cold rolling was conducted and 0.23 mm sheets
were obtained. The chemical compositions of two kinds of cool rolled
3.1. Macrostructure and magnetic properties
sheets are shown in Table 1. Trace Cr was added to sample A and the
comparison sample B was without Cr addition.
After high-temperature annealing and insulation coating treatment,
The cold-rolled sheets were treated by continuous decarburization
B800 of samples A and sample B was 1.905 T and 1.913 T respectively.
and nitriding, high-temperature annealing and insulation coating.
Although B800 has reached the magnetic standard of high permeability
Decarburization annealing was conducted at 1103 K for 250 s.
grain-oriented silicon steel, it seems that the magnetic flux density is
Decarburization atmosphere was a humidified mixture which consisted
slightly weakened by adding of 0.13 wt% Cr. In order to compare the
of 40% N2 and 60% H2, and the partial pressure ratio of H2O:H2 was
iron losses of different samples, Table 2 shows the changes in iron loss
0.30. Subsequently the samples were nitrided at 1023 K for 60 s, under
values during magnetization at 50 Hz, 100 Hz and 200 Hz, and the
the atmosphere of a dry mixture containing 75% H2 and 25% N2 with
results indicate that by adding 0.13 wt% Cr, iron losses were reduced by
NH3 injection. After continuous decarburization and nitriding, the
5.1%, 4.0% and 3.6% respectively. It also means that the effect of Cr on
contents of carbon in sample A and B were both less than 50 ppm, and
reducing iron loss is weaker at high frequency. Fig. 1a and c are the
the total contents of nitrogen were 217 ppm and 197 ppm respectively.
macrostructures of the samples after removing the insulation coating on
The recrystallization of low-temperature reheated grain-oriented silicon
the surface, and Fig. 1b and d show the domain pattern in the same
steel after continuous decarburization and nitriding annealing is termed
grain region. The microstructures in Fig. 1a and c indicate that addition
as primary recrystallization. The texture and inhibitors of the primary
of Cr effectively decreases grain size and improves homogeneity of
recrystallization status have important effects on the grain structure
secondary grains. The mean diameters of final grains were about 13 mm
and magnetic properties of final products. Therefore, it is necessary to
and 17 mm for samples A and B, respectively. The smaller grains in Cr
investigate the texture and precipitates of these two kinds of samples
added sample A mean that there are more grain boundaries, which is
after primary recrystallization. Some studies have confirmed that
harmful to magnetic induction. This is one reason for low magnetic flux
density B800 of Cr-added sample. On the other hand, the reduction of
Table 1
grain size decreases induction and the width of main domains, thus the
Chemical compositions of the raw materials (wt%).
energy loss can be reduced during magnetization. According to the
Samples C Si Al N Mn S Ti Cr Fe static magnetic domains observed by powder-pattern method from
Fig. 1b and 1d, it is easier to form a narrower main domain distribution
A 0.05 3.1 0.03 0.008 0.10 0.005 0.002 0.13 balance
B 0.05 3.1 0.03 0.008 0.10 0.005 0.002 — balance in the region with smaller grains. These well explain why the decrease
of grain size leads to the decrease in magnetic flux intensity and iron

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Y. Gao, et al. Journal of Magnetism and Magnetic Materials 507 (2020) 166849

Table 2
Iron loss (P, W/kg) during magnetization at different frequencies.
Magnetic induction (B), T P at 50 Hz P at 100 Hz P at 200 Hz

Sample A Sample B Reduction rate,% Sample A Sample B Reduction rate,% Sample A Sample B Reduction rate,%

0.20 0.012 0.013 5.6 0.039 0.041 6.7 0.125 0.136 7.9
0.40 0.047 0.049 5.4 0.148 0.157 6.2 0.461 0.495 6.8
0.60 0.105 0.109 4.3 0.318 0.328 3.0 0.996 1.039 4.2
0.80 0.183 0.191 4.4 0.561 0.588 4.6 1.693 1.761 3.9
1.00 0.283 0.299 5.2 0.850 0.875 2.9 2.575 2.651 2.9
1.20 0.398 0.420 5.1 1.179 1.216 3.0 3.542 3.645 2.8
1.40 0.536 0.568 5.7 1.569 1.633 3.9 4.733 4.840 2.2
1.60 0.710 0.744 4.6 2.046 2.113 3.2 6.125 6.282 2.5
1.70 0.828 0.874 5.2 2.361 2.429 2.8 6.961 7.137 2.5
1.80 1.067 1.125 5.2 2.886 2.985 3.3 8.187 8.321 1.6
Average 5.1 4.0 3.7

Fig. 1. Macrostructures of secondary recrystallization and patterns of static domain (a) Macrostructure and (b) static domain pattern of sample A, and (c) macro-
structure and (d) static domain pattern of sample B.

Fig. 2. Morphology and distribution of precipitates after nitriding. (a) and (b), precipitates in the matrix of Sample A and B respectively. (c), irregular precipitates
near grain boundaries in Sample A.

loss. Moreover, when magnetized at higher frequencies, the barrier of the magnetostatic energy of spontaneous magnetization by forming
grain boundaries to domain movement increases, and the effect of re- domains in the inner region of grain. The process of technical magne-
ducing iron loss by decreasing grain size is weakened. tization is the movement and change of domain. Due to the high per-
Magnetic domain refers to the region where the atomic magnetic meability of material in the rolling direction, even under a low mag-
moment aligned in a certain direction, and its width determines the netic field, domains with similar direction to the magnetic field moves
energy loss during the magnetization. Ferromagnetic materials reduce and increases in volume rapidly, forms the patterns of domains with

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Y. Gao, et al. Journal of Magnetism and Magnetic Materials 507 (2020) 166849

Fig. 3. TEM micrograph of conventional crystalline fcc-AlN in sample B: (a) bright-field image and EDS result, (b) dark-field image, (c) electron diffraction pattern,
(d) Calibration results of electron diffraction pattern (PDF-#800010) and (e) EDS result.

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Y. Gao, et al. Journal of Magnetism and Magnetic Materials 507 (2020) 166849

Fig. 4. TEM micrograph of amorphous (Si, Cr)N in sample A: (a) bright-field image, (b) dark-field image, (c) electron diffraction pattern and (d) EDS results.

different widths as shown in Fig. 1b and d. characteristics of high permeability grain-oriented silicon steel manu-
The formation of domains keeps materials in its lowest energy state. factured by low-temperature slab reheating, the amount of inherent
Smaller grains lead to the increase of crystal defects and internal stress, inhibitors AlN in primary recrystallization is small. Most precipitates in
which increase the magnetostatic energy of the material. In order to the matrix of two samples are rectangular in shape and less than
minimize energy, width of domains in oriented silicon steel with 200 nm in size (Fig. 2a and 2b). Apart from their similar shape, the
smaller grains becomes narrower. Moreover, according to [16], the main components of precipitates in two samples after nitriding are
relationship between the domain width D and grain size Gs is give by slightly different. The EDS results in Fig. 4d and 5d indicate that pre-
the formula (1) as follow: cipitates are mainly composed of Si and N, not as the conventional
precipitates AlN. Moreover, the precipitates in Sample A contain Cr, as
γGs shown in Fig. 4d. The microstructures of precipitates formed after ni-
D=
βμ0 Ms2 (1) triding were analyzed in Fig. 4c (amorphous (Si, Cr) N) and Fig. 5c
(amorphous Si3N4), and results of electron diffraction pattern show that
where γ is domain wall energy per unity volume, β is a non-dimensional
both two kinds of precipitates are amorphous. However, the size of
constant, Ms is the saturation magnetization, μ0 is the permeability of
amorphous (Si, Cr) N in sample A is smaller and the quantity is more.
vacuum.
The evolution of precipitates after nitriding can be explained by re-
This formula indicates that the domain width D is proportional to
ference [20], thus the nitrides were Si3N4 after nitrogen injection
the grain size Gs. Therefore, Sample A with small grain size has nar-
treatment. These precipitates were unstable and would dissolved and
rower domain width under low magnetic field conditions.
then precipitated as (Al, Si) N in the temperature range from 1023 K
to1173 K. At the temperature range of 973 K to 1073 K, it would take
3.2. Characteristics of precipitates in primary recrystallization four hours for Si3N4 to be fully converted into (Al, Si) N. According to
the research of nitriding in Fe-2 at.% Si alloy [21], the interface be-
Fig. 2 shows the morphology and distribution of precipitates in tween amorphous silicon-nitride and ferrite-martix has a lower inter-
surface area after nitriding. It is observed that the precipitates distribute facial energy than that between crystalline silicon-nitride and ferrite-
not only in matrix but also at grain boundaries. A smaller number of martix. In addition, Wu et al. pointed out that amorphous Si3N4 con-
crystalline precipitates are observed and confirmed to be conventional tains a large number of suspended bonds, which are easy to combine
crystal fcc-AlN precipitates in both samples A and B. For example in with other elements in silicon steel [22]. So a large number of solute
Fig. 3, the sizes of these precipitates are below 150 nm, which were element Cr can combine with the suspended bonds of amorphous Si3N4
formed after the normalizing annealing and acted as conventional in- and precipitated. Therefore, at the experimental nitriding temperature
herent inhibitors [17–19]. However, due to the composition

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Y. Gao, et al. Journal of Magnetism and Magnetic Materials 507 (2020) 166849

Fig. 5. TEM micrograph of amorphous Si3N4 in sample B: (a) bright-field image, (b) dark-field image, (c) electron diffraction pattern and (d) EDS result.

of 1023 K for 40 s, the composite amorphous nitrides (Si, Cr) N were boundary. PD represents the driving force causing by interface energy.
found in the samples containing 0.13 wt% Cr. Pz represents the Zener resistance causing by inhibitors. α is the shape
In addition, irregular morphology precipitates with Cr and Si were factor. R and r are the average radii of grains and inhibitors, respec-
found at the grain boundaries, according to the result of EDS in tively. f is the volume fraction of inhibitors. And γs is the specific grain
Fig. 6(e). Unlike the amorphous precipitates after nitriding, this type of boundary energy.
precipitates is crystalline nitride. The analysis of electron diffraction Without considering the grain boundary energy of the specific grain,
pattern in Fig. 6c and d indicates that the precipitates are fcc-CrN. the effect of inhibitors on primary recrystallization was evaluated by
According to the microstructure in dark field image in Fig. 6b, the macroscopic analysis according to formula (2). Under the condition of
crystalline CrN is oval shape and smaller than 50 nm, which is sur- chemical composition in this experiment, the content of inhibitor
rounded by the amorphous Si3N4 according to the diffraction pattern. forming element Cr in sample A is larger compared with sample B. Cr-
This phenomenon indicates that the crystalline CrN precipitates earlier containing inhibitors have been found at grain boundaries and in the
and becomes the nucleus of the later ones, and the space around the matrix after nitriding in sample A. The combination of Cr and N results
precipitates promotes the precipitation of amorphous Si3N4. These fine in more small nitrides after nitriding. Therefore, compared with sample
dispersed precipitates are a good type of inhibitor for grain-oriented B, more and smaller amorphous nitrides were formed in sample A. In
silicon steel. addition, the size of crystalline CrN formed at grain boundaries was
Primary recrystallization is formed during decarburization and ni- fine, which enhanced the pinning ability to inhibit grain growth in
triding. Decarburization occurs in the first 100 s of decarburization, and primary crystallization. As a result of the increased precipitation of
the content of carbon can be reduced to less than 100 ppm. [23] small inhibitors, Pz would increase in sample A, which has an excellent
Thereafter the primary recrystallization is almost pure ferrite and grain effect on inhibiting primary recrystallization before the abnormal
growth occurs. During the process of primary grain growth, inhibitors growth of secondary recrystallization. The size of primary grains is
can inhibit grain growth by hindering the migration of grain bound- shown in Section 3.3.
aries, which can be explained by the following formula (2) [24].
aγs γ
P = PD − PZ = − 3f s 3.3. Texture of primary recrystallization
R 2r (2)
where P represents the driving force for the migration of grain Optical microstructure of primary recrystallization after nitriding is

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Y. Gao, et al. Journal of Magnetism and Magnetic Materials 507 (2020) 166849

Fig. 6. TEM micrograph of crystalline fcc-CrN in sample A: (a) bright-field image and EDS spectroscopy, (b) dark-field image, (c) electron diffraction pattern, (d)
Calibration results of electron diffraction pattern (PDF-#110065) and (e) EDS result.

shown in Fig. 7, where RD means rolling direction and ND represents subsurface region and the center region is smaller than that in sample B.
transverse direction. The sizes of primary grains in the area of surface to In sample B, the grains growth in the center region is obvious. Some
1/4-layer and in the area of 1/4-layer to 1/2-layer were estimated, the grains have been coarsened to over 50 μm. The size of the primary grain
division of the areas is shown in Fig. 8 and the results are listed in is consistent with the previous analysis of inhibitors in Section 3.2.
Table 3. The results in Table 3 show that the size of primary grain in Coarsened primary grains are not conducive to be absorbed by Goss
sample A is smaller and its dimensional variation between the grains during secondary recrystallization, thus hindering the

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Y. Gao, et al. Journal of Magnetism and Magnetic Materials 507 (2020) 166849

Fig. 7. Optical microstructure of primary recrystallization after nitriding. (a), sample A. (b), sample B.

Fig. 8. Texture of cold rolled sheets at different layers across thickness of sample A and B.

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Y. Gao, et al. Journal of Magnetism and Magnetic Materials 507 (2020) 166849

Table 3 of (1 1 1) < uvw > components recrystallize and grow to make the γ-
Sizes of primary grains in the different area across thickness, μm. fiber the strongest component. However, the grain boundaries between
Samples surface to 1/4-layer 1/4-layer to 1/2-layer {1 1 1} 〈1 1 2〉 and {0 0 1} 〈1 1 0〉 or {1 1 2} 〈1 1 0〉 are the high-angle
grain boundaries which can migrate quickly, the primary re-
A 16.2 17.5 crystallization finally would have a strong γ-fiber dominated by {1 1 1}
B 17.1 19.2
〈1 1 2〉. In order to compare the change of the strength of important
texture components in primary recrystallization, the orientation dis-
tribution intensities of α-fiber and γ-fiber at different layers are shown
development of perfect Goss texture and being harmful to magnetic
in Fig. 10. From Fig. 10, it shows that α-fiber dominated by {0 0 1}
properties. Therefore, it is a key technology to control primary grains in
〈1 1 0〉 are still very strong in the 1/4 thickness layer and center layer
a uniform and suitable size range by using inhibitors and segregation
of sample B. While in sample A, the strength of {0 0 1} 〈1 1 0〉 de-
elements.
creased obviously, especially in the center layer. According to the or-
The textures of primary grains are equally important, so the texture
ientation densities of γ-fiber, the strength of {1 1 1} 〈1 1 0〉 varies little,
of cold-rolled sheets and nitrided samples at different layers were
meaning that this component changes little during the primary re-
measured. The ODF results of cold-rolled sheet at different layers are
crystallization. The strength of {1 1 1} 〈1 1 2〉 in different layers of
shown in Fig. 8. It can be seen that the texture types of different samples
sample A is significantly stronger than that in sample B. As mentioned
are basically the same. The textures of the two kinds of cold-rolled
earlier, the growth of recrystallization is also affected by inhibitors.
samples all contain strong α-fiber and weak γ-fiber. Moreover, the
According to formula (1), under the action of inhibitor pinning, grains
texture strength around {0 0 1} 〈1 1 0〉 is much higher on the sub-
with high boundary energy (γs ) can move faster. Because there are large
surface layer of cold-rolled samples than that of the center layer. This is
angle boundaries between {1 1 1} 〈1 1 2〉 and other components, the
because grain-oriented silicon steel belongs to low-carbon steel, which
migration rates of these boundaries are greater. The movement of grain
is easy to form strong {0 0 1} 〈1 1 0〉 and {1 1 1} 〈1 1 0〉 after cold
boundaries with low migration rate was inhibited due to the strong
rolling with a large reduction ratio [25]. The ODF results of sheets after
inhibition ability in sample A, so grains with {1 1 1} 〈1 1 2〉 are easier
nitriding at different layers are shown in Fig. 9. This result indicates
to recrystallize and the intensity of {1 1 1} 〈1 1 2〉 becomes stronger.
that after decarburization and nitriding, the texture has changed from
On the contrary, other types of grains would grow easily in the con-
strong α-fiber which is dominated by {0 0 1} 〈1 1 0〉 to {3 1 1} 〈1 3 6〉
dition that the inhibitor is weak, finally the γ-fiber is relatively weaker.
and γ-fiber which are dominated by {1 1 1} 〈1 1 2〉. This kind texture is
The type of texture has a decisive effect on secondary re-
the typical type of primary recrystallization in grain-oriented silicon
crystallization of Goss texture. Early studies have shown that nuclei of
steel with a large reduction ratio cold-rolling. The strain energy storage
Goss grains in primary recrystallization would be distributed around
of grains in different orientation is different in cold rolling deformation
the deformation band with the texture of {1 1 1} 〈1 1 2〉 and form ∑9
matrix and the order of energy storage on different crystal faces is as
boundary, which is beneficial to the growth of secondary re-
follow, (1 1 0) > (1 1 1) > (1 1 2) > (0 0 1) [26]. Because the (1 1 0)
crystallization [27]. Moreover, from the perspective of high-energy
[uvw] components in cold-rolled sheets are very small, a large number

Fig. 9. Texture of sheets after nitriding at different layers across thickness of sample A and B.

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Y. Gao, et al. Journal of Magnetism and Magnetic Materials 507 (2020) 166849

Fig. 10. Orientation densities of (a) α-fiber, (b) γ-fiber at different layers after nitriding.

Table 4 (1) With the addition of 0.13 wt% Cr, the average value of iron loss
The quantitative analysis of major texture in primary recrystallization and their during magnetization reduced by 5.1% at 50 Hz, 4.0% at 100 Hz
relationships with Goss texture {1 1 0} 〈0 0 1〉. and 3.6% at 200 Hz respectively. The reduction of the final grain
Major texture, Samples Layer, Volume Grain- Axis size resulted in the narrowing of the domain width, but the increase
deviation fraction of fraction, boundary orientation of grain boundary was not good for improving magnetic induction.
angle ≤ 12° thickness % angle,° (2) Besides the traditional precipitates, there were two kinds of Cr-
containing nitrides when 0.13 wt% Cr was added. One kind was a
{1 1 1} 〈1 1 2〉 A 1/4 5.31 35.3 [−1 0 1]
1/2 4.78 large amount of amorphous (Si, Cr) N formed in the matrix. Another
B 1/4 4.84 was crystalline fcc-CrN, whose size was smaller than 50 nm and
1/2 3.87 would enhance the pinning effect in primary crystallization.
{1 1 1} 〈1 1 0〉 A 1/4 2.82 46.0 [0 1 5] (3) By adding 0.13 wt% Cr, the primary grain size was more uniform in
1/2 2.91
B 1/4 2.42
thickness direction and more beneficial textures such as {1 1 1}
1/2 2.61 〈1 1 2〉 were obtained. Meanwhile, the {0 0 1} 〈1 1 0〉 and {1 1 2}
{0 0 1} 〈1 1 0〉 A 1/4 1.59 62.8 [-1–2 2] 〈1 1 0〉 texture components which cannot form HEGB with Goss
1/2 2.05 grains at different thickness are fewer.
B 1/4 2.25
1/2 2.42
{1 1 2} 〈1 1 0〉 A 1/4 2.54 46.0 [0 –1 5] Credit authorship contribution statement
1/2 2.81
B 1/4 3.18 Yang Gao: Writing - original draft, Investigation, Data curation.
1/2 2.91 Guang Xu: Methodology, Writing - review & editing. Xiaolong Guo:
Methodology, Resources. Guangqiang Li: Methodology, Resources,
Writing - review & editing. Yong Wang: Investigation, Writing - ori-
grain boundary theory (HEGB), the grain boundary with a mis-
ginal draft.
orientation from 20° to 45° around Goss nuclei could get rid of pinning
effects and move at first [28]. The quantitative analysis results of major
Declaration of Competing Interest
texture types and the relationship between other main texture and Goss
are shown in Table 4. According to the results in Table 4, there are more
benefiting texture {1 1 1} 〈1 1 2〉 in sample A. On the other hand, the The authors declare that they have no known competing financial
primary grains with {0 0 1} 〈1 1 0〉 and {1 1 2} 〈1 1 0〉 which can not interests or personal relationships that could have appeared to influ-
form HEGB with Goss grains are fewer in sample A. Therefore, due to ence the work reported in this paper.
the smaller size of primary grains and more benefiting texture, more
Goss nuclei can grow in the secondary recrystallization in sample A, Acknowledgement
which leads to the more and smaller final grains than that of sample B.
This work was supported by National Key R&D Program of China
(Grant No. 2016YFB0300302). The authors acknowledge the National
4. Conclusions Key R&D Program of China.

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