脉冲磁场对取向硅钢初次再结晶组织织构的影响
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摘要
磁场作为一种重要的物理场在调控材料组织结构领域得到了日益广泛的应用。将磁场与传统生产工艺相结合，可以制备新材料、开发新工艺从而得到性能更优的产品。其中，磁场热处理是前沿热点问题之一，具有广阔的创新空间。由于稳恒强磁场设备复杂、维护运行成本高，难以在工业生产中广泛应用，而脉冲磁场装备简单、能量密度大、运行成本低廉，具有广泛的工业应用前景。取向硅钢是一种重要的软磁功能材料，主要用于制作各种变压器铁芯，在电力电子、国防、民生等领域具有重要地位。再结晶微观组织、织构的控制是取向硅钢生产的核心技术，值得深入探索和研究。
本文选用商业生产普通取向硅钢(CGO钢)及高磁感取向硅钢（Hi-B钢）冷轧钢板为实验原料，利用课题组现有高压脉冲磁场设备及自研热处理装置进行不同热处理工艺下的非磁场与脉冲磁场热处理对比实验，借助电子背散射衍射(EBSD)技术对取向硅钢初次再结晶微观组织、晶体学取向以及晶界结构进行分析，研究了在不同热处理条件下，脉冲磁场对不同种类取向硅钢冷轧板初次再结晶组织及织构的影响规律。不同工艺条件下的热处理实验结果表明，脉冲磁场能够影响取向硅钢初次再结晶晶粒尺寸及分布、织构、晶界结构，磁场作用特点在不同热处理工艺中有所不同。本文通过磁有序作用及硅钢晶粒的磁自由能各向异性原理提出磁场作用机理假设，与实验结果能够较好地吻合。
Hi-B钢730℃等温退火过程中沿轧向施加1T脉冲磁场，退火时间少于80min时磁场使晶粒尺寸增加，退火时间大于80min时磁场使晶粒尺寸减小。磁有序抑制形核作用使磁场退火样品晶粒尺寸分布不均匀，出现混晶。磁场退火对{111}<110>、{001}<110>织构起抑制作用，对{111}<112>、{001}<120>织构起促进作用。脉冲磁场减少小角度晶界、增加高能晶界，在较短的退火时间效果更加明显。磁场减少整体CSL晶界，减少Goss晶粒周围小角晶界，增加其高能晶界，可能使Goss晶粒具备快速长大的潜力，为二次再结晶晶粒异常长大做组织准备。
CGO钢等时变温退火实验中沿轧向施加1T脉冲磁场，使平均晶粒尺寸增加，退火温度越高效果越弱。磁场退火样品晶粒尺寸分布不均匀，出现混晶。磁场抑制{111}<110>取向，增强{111}<112>取向；强烈抑制{001}<110>取向。高温磁场退火明显增加{001}<120>取向的体积含量。磁场减少整体小角度晶界、CSL晶界，增加高能晶界，较低退火温度下效果更加明显。磁场减少Goss晶粒周围小角晶界，增加高能晶界，增加CSL晶界，能使Goss晶粒在二次再结晶中获得快速长大的优势。
CGO钢连续退火实验中沿轧向施加2T脉冲磁场，使样品平均晶粒尺寸增加，增加幅度随退火温度和时间的增加而增加，760℃与780℃磁场促进晶粒长大作用最明显。磁场退火样品晶粒尺寸分布不均匀，出现混晶。随着退火温度和退火时间的增加，磁场抑制{111}<110>取向、{001}<110>取向，促进{111}<112>取向、{001}<120>取向、{110}<001>取向。对{111}<112>取向促进作用较为稳定，对{111}<110>取向抑制作用不稳定。磁场减少小角度晶界、增加高能晶界，760℃、780℃作用效果最明显。磁场在较低温度下减少整体CSL晶界，较高温度下增加整体CSL晶界。磁场减少Goss取向周围小角晶界，增加高能晶界，作用效果不如CGO钢等时变温退火明显。
CGO钢退火过程中施加不同方向脉冲磁场，将改变磁场方向与主要织构晶向的相对位置，即改变了主要织构在磁场中的自由能状态，从而对硅钢再结晶织构产生不同的影响。轧向磁场对Goss取向促进作用最强，相对促进{001}<120>取向形核生长，其次促进{111}<112>取向，相对抑制{111}<110>取向、{001}<110>取向。横向磁场相对促进{001}<120>取向形核生长，其次将促进{111}<110>取向形核生长，相对而言抑制{111}<112>取向、{001}<110>取向、Goss{110}<001>取向形核生长。法向磁场显著抑制γ织构，同时促进{001}<110>取向、{001}<120>取向、{001}<100>取向。2T磁场比1T磁场作用效果更加明显。
Magnetic field, as a significant physical field, has been widely applied to controlmaterial structure increasingly. Combined with the traditional process, it can be usedto prepare advanced material and develop new technology, manufacturebetter-performing products consequently. Magnetic heating treatment is one of thefrontier hotspots which has broad space and excellent prospect in innovation andapplication. The wide application of steady high-intensity magnetic field in industrycannot be realized because of its complicated infrastructure and high maintenancecosts, while the pulsed magnetic field used in this article has a prospect of wideindustry application because of its simple equipment, high-energy density andlow-running costs. Grain-oriented silicon steel is an important soft magnetic materialmainly be used in production of various kinds of iron core. Silicon steel plays a veryimportant role in power electronics, national defense and livelihoods. The control ofrecrystallization microstructure and texture, as core technology of oriented siliconsteel production, deserves our in-depth exploration and researching.
Cold plates for commercial common grain-oriented silicon steel (CGO) and highmagnetic-induction grain-oriented silicon steel (Hi-B) were chosen as experimentalmaterial. The existing high-voltage pulsed magnetic field device and self-madeheating treatment furnace were used to carry out comparative experiments with andwithout pulsed magnetic field in different heating treatment conditions.Microstructure, crystal orientation and grain boundary structure of silicon steel wereanalyzed using electron back scattering diffraction (EBSD). The effect of pulsedmagnetic field on primary recrystallization microstructure and texture of orientedsilicon steel in different heating treatment conditions was studied. Experimentalresults show that pulsed magnetic field annealing can affect the primary recrystallization grain size and distribution, texture and grain boundary structure. Themagnetic field effects is different under different conditions. Based on the magneticorder and anisotropy energy of silicon steel grain during magnetic annealing, ahypothesis about magnetic field action mechanism is proposed, which is fairlysupported by almost all of the experimental results in this work.
When cold rolled Hi-B specimens were annealed at730℃for different timewithout and with1T magnetic field parallel to rolling direction of specimens, grainsize of magnetic annealing specimens is bigger than that of the non-magneticannealing for the annealing time less than80min, while a opposite result is obtainedwhen the annealing time more than80min. The magnetic annealing specimens havemischcrystal structure because of magnetic ordering in nucleation. Magneticannealing inhibits {111}<110>,{001}<110> texture and facilitates {111}<112>,{001}<120> texture. Magnetic annealing reduces low-angle grain boundary and CSLgrain boundary and, at the same time increases high-energy grain boundary in all ofthe grains,especially in the case of shorter time annealing. Magnetic annealingreduces low-angle grain boundary and increases high-energy grain boundary aroundGoss texture, which might possess the Goss grains a priority in grain growth duringsecondary recrystallization.
Whencold rolled CGO specimens were annealed at different temperature for60min without and with1T pulsed magnetic field in rolling direction, the averagegrain size of magnetic annealing specimens is bigger than non-magnetic annealingones, the effect is weakened with the annealing temperature rises. The magneticannealing specimens have mischcrystal structure. Magnetic annealing restrains{111}<110> texture and facilitates {111}<112> texture a little, meanwhile, restrains{001}<110> texture and facilitates {001}<120> texture strongly. Magnetic annealingreduces low-angle grain boundary and CSL grain boundary，meanwhile increaseshigh-energy grain boundary in all of the grains and the impact is more pronounced inlower annealing temperature. Magnetic annealing reduces low-angle grain boundarymeanwhile increases high-energy grain boundary and CSL grain boundary aroundGoss texture, making Goss texture has advantage in grain growth during secondaryrecrystallization.
When cold rolled CGO specimens were annealed at20℃/h from700℃to different temperature without and with2T rolling direction magnetic field, magneticannealing increases average grain size, and the grain size increases with the increasingannealing time and temperature. The most obvious effect of increasing grain sizeappears at760℃and780℃. The magnetic annealing specimens have mischcrystalstructure. Magnetic annealing restrains {111}<110> texture and {001}<110> texture,meanwhile facilitates {111}<112> texture and {001}<120> texture and Goss texturealong with the increasing annealing time and temperature. The magnetic promotioneffect of {111}<112> is stable and the magnetic inhibition effect of {111}<110> isunstable relatively. Magnetic annealing reduces low-angle grain boundary，meanwhileincreases high-energy grain boundary in all of grains and the impact is morepronounced at760℃and780℃. Magnetic annealing decreases CSL grain boundaryat lower temperature and increases CSL grain boundary at higher temperature in all ofgrains. Magnetic annealing reduces low-angle grain boundary and increaseshigh-energy grain boundary around Goss texture, but the effect is not obvious.
When CGO was annealed in magnetic field along different directions withrespect to the sample coordinate system, magnetic field has different effects onrecrystallization texture of silicon steel because it changes the free energy of maintextures. Magnetic field along rolling direction facilitates {001}<120> texture and{111}<112> nucleation and grain growth, meanwhile restrains {111}<110> textureand {001}<110> texture. Magnetic field along transverse direction facilitates{001}<120> texture and {111}<110> nucleation and grain growth, meanwhilerestrains {111}<112> texture,{001}<110> texture and Goss texture. Magnetic fieldalong normal direction facilitates {001}<120> texture,{001}<110> texture and{001}<100> texture, meanwhile restrains γ texture strongly. The2T magnetic field ismore efficient than1T magnetic field.
本文选用商业生产普通取向硅钢(CGO钢)及高磁感取向硅钢（Hi-B钢）冷轧钢板为实验原料，利用课题组现有高压脉冲磁场设备及自研热处理装置进行不同热处理工艺下的非磁场与脉冲磁场热处理对比实验，借助电子背散射衍射(EBSD)技术对取向硅钢初次再结晶微观组织、晶体学取向以及晶界结构进行分析，研究了在不同热处理条件下，脉冲磁场对不同种类取向硅钢冷轧板初次再结晶组织及织构的影响规律。不同工艺条件下的热处理实验结果表明，脉冲磁场能够影响取向硅钢初次再结晶晶粒尺寸及分布、织构、晶界结构，磁场作用特点在不同热处理工艺中有所不同。本文通过磁有序作用及硅钢晶粒的磁自由能各向异性原理提出磁场作用机理假设，与实验结果能够较好地吻合。
Hi-B钢730℃等温退火过程中沿轧向施加1T脉冲磁场，退火时间少于80min时磁场使晶粒尺寸增加，退火时间大于80min时磁场使晶粒尺寸减小。磁有序抑制形核作用使磁场退火样品晶粒尺寸分布不均匀，出现混晶。磁场退火对{111}<110>、{001}<110>织构起抑制作用，对{111}<112>、{001}<120>织构起促进作用。脉冲磁场减少小角度晶界、增加高能晶界，在较短的退火时间效果更加明显。磁场减少整体CSL晶界，减少Goss晶粒周围小角晶界，增加其高能晶界，可能使Goss晶粒具备快速长大的潜力，为二次再结晶晶粒异常长大做组织准备。
CGO钢等时变温退火实验中沿轧向施加1T脉冲磁场，使平均晶粒尺寸增加，退火温度越高效果越弱。磁场退火样品晶粒尺寸分布不均匀，出现混晶。磁场抑制{111}<110>取向，增强{111}<112>取向；强烈抑制{001}<110>取向。高温磁场退火明显增加{001}<120>取向的体积含量。磁场减少整体小角度晶界、CSL晶界，增加高能晶界，较低退火温度下效果更加明显。磁场减少Goss晶粒周围小角晶界，增加高能晶界，增加CSL晶界，能使Goss晶粒在二次再结晶中获得快速长大的优势。
CGO钢连续退火实验中沿轧向施加2T脉冲磁场，使样品平均晶粒尺寸增加，增加幅度随退火温度和时间的增加而增加，760℃与780℃磁场促进晶粒长大作用最明显。磁场退火样品晶粒尺寸分布不均匀，出现混晶。随着退火温度和退火时间的增加，磁场抑制{111}<110>取向、{001}<110>取向，促进{111}<112>取向、{001}<120>取向、{110}<001>取向。对{111}<112>取向促进作用较为稳定，对{111}<110>取向抑制作用不稳定。磁场减少小角度晶界、增加高能晶界，760℃、780℃作用效果最明显。磁场在较低温度下减少整体CSL晶界，较高温度下增加整体CSL晶界。磁场减少Goss取向周围小角晶界，增加高能晶界，作用效果不如CGO钢等时变温退火明显。
CGO钢退火过程中施加不同方向脉冲磁场，将改变磁场方向与主要织构晶向的相对位置，即改变了主要织构在磁场中的自由能状态，从而对硅钢再结晶织构产生不同的影响。轧向磁场对Goss取向促进作用最强，相对促进{001}<120>取向形核生长，其次促进{111}<112>取向，相对抑制{111}<110>取向、{001}<110>取向。横向磁场相对促进{001}<120>取向形核生长，其次将促进{111}<110>取向形核生长，相对而言抑制{111}<112>取向、{001}<110>取向、Goss{110}<001>取向形核生长。法向磁场显著抑制γ织构，同时促进{001}<110>取向、{001}<120>取向、{001}<100>取向。2T磁场比1T磁场作用效果更加明显。
Magnetic field, as a significant physical field, has been widely applied to controlmaterial structure increasingly. Combined with the traditional process, it can be usedto prepare advanced material and develop new technology, manufacturebetter-performing products consequently. Magnetic heating treatment is one of thefrontier hotspots which has broad space and excellent prospect in innovation andapplication. The wide application of steady high-intensity magnetic field in industrycannot be realized because of its complicated infrastructure and high maintenancecosts, while the pulsed magnetic field used in this article has a prospect of wideindustry application because of its simple equipment, high-energy density andlow-running costs. Grain-oriented silicon steel is an important soft magnetic materialmainly be used in production of various kinds of iron core. Silicon steel plays a veryimportant role in power electronics, national defense and livelihoods. The control ofrecrystallization microstructure and texture, as core technology of oriented siliconsteel production, deserves our in-depth exploration and researching.
Cold plates for commercial common grain-oriented silicon steel (CGO) and highmagnetic-induction grain-oriented silicon steel (Hi-B) were chosen as experimentalmaterial. The existing high-voltage pulsed magnetic field device and self-madeheating treatment furnace were used to carry out comparative experiments with andwithout pulsed magnetic field in different heating treatment conditions.Microstructure, crystal orientation and grain boundary structure of silicon steel wereanalyzed using electron back scattering diffraction (EBSD). The effect of pulsedmagnetic field on primary recrystallization microstructure and texture of orientedsilicon steel in different heating treatment conditions was studied. Experimentalresults show that pulsed magnetic field annealing can affect the primary recrystallization grain size and distribution, texture and grain boundary structure. Themagnetic field effects is different under different conditions. Based on the magneticorder and anisotropy energy of silicon steel grain during magnetic annealing, ahypothesis about magnetic field action mechanism is proposed, which is fairlysupported by almost all of the experimental results in this work.
When cold rolled Hi-B specimens were annealed at730℃for different timewithout and with1T magnetic field parallel to rolling direction of specimens, grainsize of magnetic annealing specimens is bigger than that of the non-magneticannealing for the annealing time less than80min, while a opposite result is obtainedwhen the annealing time more than80min. The magnetic annealing specimens havemischcrystal structure because of magnetic ordering in nucleation. Magneticannealing inhibits {111}<110>,{001}<110> texture and facilitates {111}<112>,{001}<120> texture. Magnetic annealing reduces low-angle grain boundary and CSLgrain boundary and, at the same time increases high-energy grain boundary in all ofthe grains,especially in the case of shorter time annealing. Magnetic annealingreduces low-angle grain boundary and increases high-energy grain boundary aroundGoss texture, which might possess the Goss grains a priority in grain growth duringsecondary recrystallization.
Whencold rolled CGO specimens were annealed at different temperature for60min without and with1T pulsed magnetic field in rolling direction, the averagegrain size of magnetic annealing specimens is bigger than non-magnetic annealingones, the effect is weakened with the annealing temperature rises. The magneticannealing specimens have mischcrystal structure. Magnetic annealing restrains{111}<110> texture and facilitates {111}<112> texture a little, meanwhile, restrains{001}<110> texture and facilitates {001}<120> texture strongly. Magnetic annealingreduces low-angle grain boundary and CSL grain boundary，meanwhile increaseshigh-energy grain boundary in all of the grains and the impact is more pronounced inlower annealing temperature. Magnetic annealing reduces low-angle grain boundarymeanwhile increases high-energy grain boundary and CSL grain boundary aroundGoss texture, making Goss texture has advantage in grain growth during secondaryrecrystallization.
When cold rolled CGO specimens were annealed at20℃/h from700℃to different temperature without and with2T rolling direction magnetic field, magneticannealing increases average grain size, and the grain size increases with the increasingannealing time and temperature. The most obvious effect of increasing grain sizeappears at760℃and780℃. The magnetic annealing specimens have mischcrystalstructure. Magnetic annealing restrains {111}<110> texture and {001}<110> texture,meanwhile facilitates {111}<112> texture and {001}<120> texture and Goss texturealong with the increasing annealing time and temperature. The magnetic promotioneffect of {111}<112> is stable and the magnetic inhibition effect of {111}<110> isunstable relatively. Magnetic annealing reduces low-angle grain boundary，meanwhileincreases high-energy grain boundary in all of grains and the impact is morepronounced at760℃and780℃. Magnetic annealing decreases CSL grain boundaryat lower temperature and increases CSL grain boundary at higher temperature in all ofgrains. Magnetic annealing reduces low-angle grain boundary and increaseshigh-energy grain boundary around Goss texture, but the effect is not obvious.
When CGO was annealed in magnetic field along different directions withrespect to the sample coordinate system, magnetic field has different effects onrecrystallization texture of silicon steel because it changes the free energy of maintextures. Magnetic field along rolling direction facilitates {001}<120> texture and{111}<112> nucleation and grain growth, meanwhile restrains {111}<110> textureand {001}<110> texture. Magnetic field along transverse direction facilitates{001}<120> texture and {111}<110> nucleation and grain growth, meanwhilerestrains {111}<112> texture,{001}<110> texture and Goss texture. Magnetic fieldalong normal direction facilitates {001}<120> texture,{001}<110> texture and{001}<100> texture, meanwhile restrains γ texture strongly. The2T magnetic field ismore efficient than1T magnetic field.
引文
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