Grain-oriented silicon steels were prepared at different heating rates during high temperature annealing,in which the evolution of magnetic properties,grain orientations and precipitates were studied.To illustrate the...Grain-oriented silicon steels were prepared at different heating rates during high temperature annealing,in which the evolution of magnetic properties,grain orientations and precipitates were studied.To illustrate the Zener factor,the diameter and number density of precipitates of interrupted testing samples were statistically calculated.The effect of precipitate ripening on the Goss texture and magnetic property was investigated.Data indicated that the trend of Zener factor was similar under different heating rates,first increasing and then decreasing,and that the precipitate maturing was greatly inhibited as the heating rate increased.Secondary recrystallization was developed at the temperature of 1010℃when a heating rate of 5℃/h was used,resulting in Goss,Brass and{110}<227>oriented grains growing abnormally and a magnetic induction intensity of 1.90T.Furthermore,increasing the heating rate to 20℃/h would inhibit the development of undesirable oriented grains and obtain a sharp Goss texture.However,when the heating rate was extremely fast,such as 40℃/h,poor secondary recrystallization was developed with many island grains,corresponding to a decrease in magnetic induction intensity to 1.87 T.At a suitable heating rate of 20℃/h,the sharpest Goss texture and the highest magnetic induction of 1.94 T with an onset secondary recrystallization temperature of 1020℃were found among the experimental variables in this study.The heating rate affected the initial temperature of secondary recrystallization by controlling the maturation of precipitates,leading to the deviation and dispersion of Goss texture,thereby reducing the magnetic properties.展开更多
The behaviors of different inhibitors including their composition, size, distribution, coalescence and coarsening were experimen-tally studied. It was observed that during secondary recrystallization of the tested ste...The behaviors of different inhibitors including their composition, size, distribution, coalescence and coarsening were experimen-tally studied. It was observed that during secondary recrystallization of the tested steel, the key inhibition effect was produced by Cu2S and AlN, but not MnS. With the increase of temperature, the size distributions of AlN and Cu2S were changed to some extent. However, signifi-cant changes in particle size were not observed. The initial temperature of abnormal growth was determined by measuring the evolution of particle sizes and their distribution density during heat treatment. AlN and Cu2S are the dominant inhibitors and both are necessary, which is verified by calculating the Zener factor.展开更多
Piezoelectric semiconductors bear the bifunctional photocatalysis and piezocatalysis,while the absent or weak internal charge driving force severely restricts its catalytic activity.Developing polarization strategy is...Piezoelectric semiconductors bear the bifunctional photocatalysis and piezocatalysis,while the absent or weak internal charge driving force severely restricts its catalytic activity.Developing polarization strategy is desirable,and particularly understanding its mechanism from a microscopic perspective remains scanty.Herein,we report a secondary recrystallization approach to achieving the simultaneous micro-and macroscopic polarization enhancement on Bi2WO6 nanosheets for boosting piezo-photocatalytic oxygen activation,and unravel the mechanism at an atom-level.The secondary recrystallization process not only results in a strengthened distortion of[WO6]octahedra with distortion index enhancement by~20%for a single octahedron,but also enables lateral crystal growth of nanosheets along the ab plane(av.50 to 180 nm),which separately allows the rise in dipole moment of unit cell(e.g.,1.63 D increase along a axis)and the stacking of the distorted[WO6]octahedron to accumulate the unit cell dipole,collectively contributing to the considerably strengthened spontaneous polarization and piezoelectricity.Besides,exposure of large-area{001}front facet enables more efficient capture and conversion of stress into piezo-potential.Therefore,the well-recrystallized Bi2WO6 nanosheets exhibit considerably promoted piezo-photocatalytic reactive oxygen species generation,given the decreased specific surface area.This work presents a feasible methodology to regulate inside-out polarization for guiding carriers transfer behavior,and may advance the solid understanding on the intrinsic mechanism.展开更多
Low-temperature slab-reheated grain-oriented silicon steel is characterized by a sharp {411}〈148〉 primary recrystallization texture. To date, the influence of this texture on secondary recrystallization is not clear...Low-temperature slab-reheated grain-oriented silicon steel is characterized by a sharp {411}〈148〉 primary recrystallization texture. To date, the influence of this texture on secondary recrystallization is not clear. Microtextures in primary and secondary reerystallized sheets of low-temperature reheated grain-oriented silicon steel were examined using electron backscatter diffraction. By comparing the textures and microstructures of specific primary reerystallized grains neighboring secondary grains with those of other primary grains, the influences of primary re- crystallization textures and microstructures on the orientations of secondary grains were investigated. Results show that for low-temperature reheated graiworiented silicon steel, the primary recrystallization sheet comprises { 411 } 〈148〉, {111}〈112〉, and {001}〈120〉 texture componems. During secondary recrystallization, the {111}〈112〉 primary recrystallized grains were easily consumed by abnormally grown Goss, deviated Goss, Brass, or {210}〈001〉grains ;the { 411 }〈148〉 primary recrystallized grains were more resistant to being swallowed; and the {001} 〈120 grains were the most resistant to being consumed. For a particular primary grain, the distribution of its surrounding grain boundaries determined how easily it is consumed during secondary recrystallization. Primary grains surrounded by 20°- 45° grain boundaries were consumed much earlier than those having grain boundaries above 45°, which is in accordance with high-energy grain boundary theory. In addition, special ∑9 boundaries between {411}〈148〉 and Goss grains move more slowly than ∑9 boundaries between {111 }〈112〉 and Goss grains, which is attributed to the different positions of 〈110〉 rotation axis with respect to the normals of grain boundaries.展开更多
To avoid the unfavorable effect of precipitates on magnetic properties,low addition of 0.16 wt%NbC was employed in Fe_(82.5)Ga_(17.5)alloy,and 0.27 mm sheets were successfully prepared by a rolling process.Strong Goss...To avoid the unfavorable effect of precipitates on magnetic properties,low addition of 0.16 wt%NbC was employed in Fe_(82.5)Ga_(17.5)alloy,and 0.27 mm sheets were successfully prepared by a rolling process.Strong Goss texture was obtained in Fe-Ga sheets by two-stage annealing process.The sulfur annealing in quartz ampoules was made to produce the preferred growth of Goss texture,with a 51%increase in the observed saturation magnetostriction,from 87×10^(-6)in the Ar-annealed sheets to 132×10^(-6)in the S-annealed sheets.However,large amounts of S-rich and Nb-rich precipitates were formed in the S-annealed sheets.High-temperature annealing of the S-annealed sheets at 1,200℃under a flow hydrogenargon atmosphere could effectively eliminate the precipitates and promote the selective growth of(110)grains due to the low surface energy.Large grains(~2 cm)of secondary recrystallization were achieved in the final annealed sheets,with the maximum average saturation magnetostriction of 180×10^(-6).展开更多
The slab low-temperature reheating grain-oriented silicon steel was prepared in the laboratory,and the high-temperature annealing interruption tests were carried out.The effects of aluminum(which meant acid-soluble al...The slab low-temperature reheating grain-oriented silicon steel was prepared in the laboratory,and the high-temperature annealing interruption tests were carried out.The effects of aluminum(which meant acid-soluble aluminum)on the grain size texture,precipitate,magnetic properties and their correlations were studied.The results showed that with the increase in aluminum element,the grain size decreased,while the intensity of{114}<481>and{111}<112>textures increased in the primary recrystallization structure.Meanwhile,the pinning force during the secondary recrystallization and the onset secondary recrystallization temperature were increased.The precipitates were concluded to have a more important role on determining the onset secondary recrystallization temperature than the primary grain size.The higher onset temperature resulted in sharper Goss texture and the better magnetic properties,but when the aluminum content came up to a certain extent,a fine-grain structure was developed.The most suitable aluminum content for present study was 0.025 wt.%,while the onset secondary recrystallization temperature and the primary texture were considered to be conducive to the sharpness of Goss texture.展开更多
By rolling and nitriding processes, 0.23- to 0.3-mm-thick grain-oriented 6.5 wt% silicon steel sheets were produced. The core losses of grain-oriented 6.5 wt% silicon steel at frequencies ranging from 400 Hz to 20 kHz...By rolling and nitriding processes, 0.23- to 0.3-mm-thick grain-oriented 6.5 wt% silicon steel sheets were produced. The core losses of grain-oriented 6.5 wt% silicon steel at frequencies ranging from 400 Hz to 20 kHz were lower than that of the grain-oriented 3 wt% silicon steel with the same thickness by 16.6-35.8%. The secondary recrystallization behavior was investigated by scanning electron microscopy, energy-dispersive spectroscopy, and electron backscattered diffraction. The results show that the secondary recrystallization in high-silicon steel sheets develops more completely as the nitrogen content increases after nitriding, secondary recrystallized grain sizes become larger, and the sharpness of Goss texture increases. Because more { 110} (116) grains in the subsurface and the central layer of the sheets have a lot of 20°-45° high-energy boundaries in addition to Goss grains, {110} (116) can be the main component through selective growth during secondary recrystallization when the inhibitor quantity is not enough and inhibitor intensity is weaker. The increases in nitrogen content can increase the inhibitor intensity and hinder abnormal growth of a mount of {110} (116) grains and therefore enhance the sharpness of Goss texture.展开更多
On the basis of statistical data of MnS in the conventional 3% Si steel sheeets after various annealing processes,the critical inclusion factor has been evaluated to be 20 mm^(-1).The inhi- bition of MnS to grain grow...On the basis of statistical data of MnS in the conventional 3% Si steel sheeets after various annealing processes,the critical inclusion factor has been evaluated to be 20 mm^(-1).The inhi- bition of MnS to grain growth has been exactly described.展开更多
When Sn segregated at grain boundaries of high induction oriented silicon steel,no remarka- ble interaction between Sn and other elements was observed.At the starting temperature of secondary recrystallization,950℃,a...When Sn segregated at grain boundaries of high induction oriented silicon steel,no remarka- ble interaction between Sn and other elements was observed.At the starting temperature of secondary recrystallization,950℃,a certain Sn still segregates at grain boundaries.Sn seems to act as a supplemental inhibitor through grain boundary segregation.According to theoreti- cal analysis,an addition of Sn may decrease the secondary recrystallization temperature of high induction oriented silicon steel,and it is in agreement with the experimental result.展开更多
In this study, high- and low-grade grain-oriented electrical steels were used as the initial materials to produce 0.08-mm-thick sheet with one-step cold-rolling method. Electron backscattering diffraction analysis tec...In this study, high- and low-grade grain-oriented electrical steels were used as the initial materials to produce 0.08-mm-thick sheet with one-step cold-rolling method. Electron backscattering diffraction analysis technique and X-ray diffraction texture analysis technique were adopted to investigate the effect of initial Goss texture sharpness on texture evolution and magnetic properties of ultra-thin grain-oriented electrical steel. The results showed that primary recrystal- lization and secondary recrystallization were the main processes that occurred during annealing. The induced factors for secondary recrystallization of two grades samples were not Consistent. The high-grade samples presented texture induction mechanism, while the low-grade samples revealed strong surface-energy induction mechanism. The initial Goss texture sharpness had a great impact on texture evolution and magnetic properties of ultra-thin grain-oriented electrical steel. The Goss texture component formed after primary recrystallization was stronger, and better magnetic properties were obtained at low frequencies. For low-grade samples, secondary recrystallization enhanced the intensity of Goss texture, and both grain size and texture contributed to better high-frequency magnetic properties after secondary recrystallization. By controlling the annealing process, the magnetic properties of low-grade products could be significantly improved, thus achieving conversion from low-grade to high-grade products.展开更多
High energy synchrotron diffraction offers great potential to study the recrystallization kinetics of metallic materials. To study the formation of Goss texture ({ [10}(001)) of grain oriented (GO) silicon steel...High energy synchrotron diffraction offers great potential to study the recrystallization kinetics of metallic materials. To study the formation of Goss texture ({ [10}(001)) of grain oriented (GO) silicon steel during secondary recrystallization process, an in situ experiment using hi gh energy X-ray diffraction was designed. The results showed that the secondary recrystallization began when the heating temperature was 1,494 K, and the grains grew rapidly above this temperature. With an increase in annealing temperature, the large grains with 7 orientation [〈111〉//normal direction] formed and gradually occupied the dominant position. As the annealing temperature increased even further, the grains with Goss orientation to a very large size by devouring the 7 orientation grains that formed in the early annealing stage. A single crystal with a Goss orientation was observed in the GO silicon steel when the annealing temperature was 1,540 K.展开更多
文摘Grain-oriented silicon steels were prepared at different heating rates during high temperature annealing,in which the evolution of magnetic properties,grain orientations and precipitates were studied.To illustrate the Zener factor,the diameter and number density of precipitates of interrupted testing samples were statistically calculated.The effect of precipitate ripening on the Goss texture and magnetic property was investigated.Data indicated that the trend of Zener factor was similar under different heating rates,first increasing and then decreasing,and that the precipitate maturing was greatly inhibited as the heating rate increased.Secondary recrystallization was developed at the temperature of 1010℃when a heating rate of 5℃/h was used,resulting in Goss,Brass and{110}<227>oriented grains growing abnormally and a magnetic induction intensity of 1.90T.Furthermore,increasing the heating rate to 20℃/h would inhibit the development of undesirable oriented grains and obtain a sharp Goss texture.However,when the heating rate was extremely fast,such as 40℃/h,poor secondary recrystallization was developed with many island grains,corresponding to a decrease in magnetic induction intensity to 1.87 T.At a suitable heating rate of 20℃/h,the sharpest Goss texture and the highest magnetic induction of 1.94 T with an onset secondary recrystallization temperature of 1020℃were found among the experimental variables in this study.The heating rate affected the initial temperature of secondary recrystallization by controlling the maturation of precipitates,leading to the deviation and dispersion of Goss texture,thereby reducing the magnetic properties.
基金supported by the National Natural Science Foundation of China (No.50871015)
文摘The behaviors of different inhibitors including their composition, size, distribution, coalescence and coarsening were experimen-tally studied. It was observed that during secondary recrystallization of the tested steel, the key inhibition effect was produced by Cu2S and AlN, but not MnS. With the increase of temperature, the size distributions of AlN and Cu2S were changed to some extent. However, signifi-cant changes in particle size were not observed. The initial temperature of abnormal growth was determined by measuring the evolution of particle sizes and their distribution density during heat treatment. AlN and Cu2S are the dominant inhibitors and both are necessary, which is verified by calculating the Zener factor.
基金the National Key Research and Development Program of China(No.2022YFB3803600)the National Natural Science Foundation of China(Nos.52272244 and 51972288)+1 种基金the Fundamental Research Funds for the Central Universities(No.2652022202)2021 Graduate Innovation Fund Project of China University of Geosciences,Beijing(No.ZY2021YC006).
文摘Piezoelectric semiconductors bear the bifunctional photocatalysis and piezocatalysis,while the absent or weak internal charge driving force severely restricts its catalytic activity.Developing polarization strategy is desirable,and particularly understanding its mechanism from a microscopic perspective remains scanty.Herein,we report a secondary recrystallization approach to achieving the simultaneous micro-and macroscopic polarization enhancement on Bi2WO6 nanosheets for boosting piezo-photocatalytic oxygen activation,and unravel the mechanism at an atom-level.The secondary recrystallization process not only results in a strengthened distortion of[WO6]octahedra with distortion index enhancement by~20%for a single octahedron,but also enables lateral crystal growth of nanosheets along the ab plane(av.50 to 180 nm),which separately allows the rise in dipole moment of unit cell(e.g.,1.63 D increase along a axis)and the stacking of the distorted[WO6]octahedron to accumulate the unit cell dipole,collectively contributing to the considerably strengthened spontaneous polarization and piezoelectricity.Besides,exposure of large-area{001}front facet enables more efficient capture and conversion of stress into piezo-potential.Therefore,the well-recrystallized Bi2WO6 nanosheets exhibit considerably promoted piezo-photocatalytic reactive oxygen species generation,given the decreased specific surface area.This work presents a feasible methodology to regulate inside-out polarization for guiding carriers transfer behavior,and may advance the solid understanding on the intrinsic mechanism.
基金Item Sponsored by National High Technology Research and Development Program of China(2012AA03A505)
文摘Low-temperature slab-reheated grain-oriented silicon steel is characterized by a sharp {411}〈148〉 primary recrystallization texture. To date, the influence of this texture on secondary recrystallization is not clear. Microtextures in primary and secondary reerystallized sheets of low-temperature reheated grain-oriented silicon steel were examined using electron backscatter diffraction. By comparing the textures and microstructures of specific primary reerystallized grains neighboring secondary grains with those of other primary grains, the influences of primary re- crystallization textures and microstructures on the orientations of secondary grains were investigated. Results show that for low-temperature reheated graiworiented silicon steel, the primary recrystallization sheet comprises { 411 } 〈148〉, {111}〈112〉, and {001}〈120〉 texture componems. During secondary recrystallization, the {111}〈112〉 primary recrystallized grains were easily consumed by abnormally grown Goss, deviated Goss, Brass, or {210}〈001〉grains ;the { 411 }〈148〉 primary recrystallized grains were more resistant to being swallowed; and the {001} 〈120 grains were the most resistant to being consumed. For a particular primary grain, the distribution of its surrounding grain boundaries determined how easily it is consumed during secondary recrystallization. Primary grains surrounded by 20°- 45° grain boundaries were consumed much earlier than those having grain boundaries above 45°, which is in accordance with high-energy grain boundary theory. In addition, special ∑9 boundaries between {411}〈148〉 and Goss grains move more slowly than ∑9 boundaries between {111 }〈112〉 and Goss grains, which is attributed to the different positions of 〈110〉 rotation axis with respect to the normals of grain boundaries.
基金the National Basic Research Program of China(No.2011CB606304)the National Natural Science Foundation of China(No.51271019)+1 种基金the Fundamental Research Funds for the Central Universities(No.FRFSD-12-025A)the National Natural Science Foundation for Postdoctoral Scientists of China(No.2011M500229)。
文摘To avoid the unfavorable effect of precipitates on magnetic properties,low addition of 0.16 wt%NbC was employed in Fe_(82.5)Ga_(17.5)alloy,and 0.27 mm sheets were successfully prepared by a rolling process.Strong Goss texture was obtained in Fe-Ga sheets by two-stage annealing process.The sulfur annealing in quartz ampoules was made to produce the preferred growth of Goss texture,with a 51%increase in the observed saturation magnetostriction,from 87×10^(-6)in the Ar-annealed sheets to 132×10^(-6)in the S-annealed sheets.However,large amounts of S-rich and Nb-rich precipitates were formed in the S-annealed sheets.High-temperature annealing of the S-annealed sheets at 1,200℃under a flow hydrogenargon atmosphere could effectively eliminate the precipitates and promote the selective growth of(110)grains due to the low surface energy.Large grains(~2 cm)of secondary recrystallization were achieved in the final annealed sheets,with the maximum average saturation magnetostriction of 180×10^(-6).
文摘The slab low-temperature reheating grain-oriented silicon steel was prepared in the laboratory,and the high-temperature annealing interruption tests were carried out.The effects of aluminum(which meant acid-soluble aluminum)on the grain size texture,precipitate,magnetic properties and their correlations were studied.The results showed that with the increase in aluminum element,the grain size decreased,while the intensity of{114}<481>and{111}<112>textures increased in the primary recrystallization structure.Meanwhile,the pinning force during the secondary recrystallization and the onset secondary recrystallization temperature were increased.The precipitates were concluded to have a more important role on determining the onset secondary recrystallization temperature than the primary grain size.The higher onset temperature resulted in sharper Goss texture and the better magnetic properties,but when the aluminum content came up to a certain extent,a fine-grain structure was developed.The most suitable aluminum content for present study was 0.025 wt.%,while the onset secondary recrystallization temperature and the primary texture were considered to be conducive to the sharpness of Goss texture.
基金Financial support from the National HighTechnology Research and Development Program of China(No.2012AA03A505)
文摘By rolling and nitriding processes, 0.23- to 0.3-mm-thick grain-oriented 6.5 wt% silicon steel sheets were produced. The core losses of grain-oriented 6.5 wt% silicon steel at frequencies ranging from 400 Hz to 20 kHz were lower than that of the grain-oriented 3 wt% silicon steel with the same thickness by 16.6-35.8%. The secondary recrystallization behavior was investigated by scanning electron microscopy, energy-dispersive spectroscopy, and electron backscattered diffraction. The results show that the secondary recrystallization in high-silicon steel sheets develops more completely as the nitrogen content increases after nitriding, secondary recrystallized grain sizes become larger, and the sharpness of Goss texture increases. Because more { 110} (116) grains in the subsurface and the central layer of the sheets have a lot of 20°-45° high-energy boundaries in addition to Goss grains, {110} (116) can be the main component through selective growth during secondary recrystallization when the inhibitor quantity is not enough and inhibitor intensity is weaker. The increases in nitrogen content can increase the inhibitor intensity and hinder abnormal growth of a mount of {110} (116) grains and therefore enhance the sharpness of Goss texture.
文摘On the basis of statistical data of MnS in the conventional 3% Si steel sheeets after various annealing processes,the critical inclusion factor has been evaluated to be 20 mm^(-1).The inhi- bition of MnS to grain growth has been exactly described.
文摘When Sn segregated at grain boundaries of high induction oriented silicon steel,no remarka- ble interaction between Sn and other elements was observed.At the starting temperature of secondary recrystallization,950℃,a certain Sn still segregates at grain boundaries.Sn seems to act as a supplemental inhibitor through grain boundary segregation.According to theoreti- cal analysis,an addition of Sn may decrease the secondary recrystallization temperature of high induction oriented silicon steel,and it is in agreement with the experimental result.
基金financially supported by the National High Technology Research and Development Program of China(Grant No.2012AA03A505)
文摘In this study, high- and low-grade grain-oriented electrical steels were used as the initial materials to produce 0.08-mm-thick sheet with one-step cold-rolling method. Electron backscattering diffraction analysis technique and X-ray diffraction texture analysis technique were adopted to investigate the effect of initial Goss texture sharpness on texture evolution and magnetic properties of ultra-thin grain-oriented electrical steel. The results showed that primary recrystal- lization and secondary recrystallization were the main processes that occurred during annealing. The induced factors for secondary recrystallization of two grades samples were not Consistent. The high-grade samples presented texture induction mechanism, while the low-grade samples revealed strong surface-energy induction mechanism. The initial Goss texture sharpness had a great impact on texture evolution and magnetic properties of ultra-thin grain-oriented electrical steel. The Goss texture component formed after primary recrystallization was stronger, and better magnetic properties were obtained at low frequencies. For low-grade samples, secondary recrystallization enhanced the intensity of Goss texture, and both grain size and texture contributed to better high-frequency magnetic properties after secondary recrystallization. By controlling the annealing process, the magnetic properties of low-grade products could be significantly improved, thus achieving conversion from low-grade to high-grade products.
基金supported by the Key Projects of the National Science & Technology Pillar Program (No. 2011BAE13B03)the Fundamental Research Funds for the Central Universities (No. N110502001)
文摘High energy synchrotron diffraction offers great potential to study the recrystallization kinetics of metallic materials. To study the formation of Goss texture ({ [10}(001)) of grain oriented (GO) silicon steel during secondary recrystallization process, an in situ experiment using hi gh energy X-ray diffraction was designed. The results showed that the secondary recrystallization began when the heating temperature was 1,494 K, and the grains grew rapidly above this temperature. With an increase in annealing temperature, the large grains with 7 orientation [〈111〉//normal direction] formed and gradually occupied the dominant position. As the annealing temperature increased even further, the grains with Goss orientation to a very large size by devouring the 7 orientation grains that formed in the early annealing stage. A single crystal with a Goss orientation was observed in the GO silicon steel when the annealing temperature was 1,540 K.