析出相质点对取向硅钢二次再结晶的影响

基于Humphreys回复、再结晶和晶粒长大统一理论,研究了析出相质点的Zenner钉扎对Fe-3%Si取向硅钢二次再结晶的影响.比较了一般取向硅钢(CGO)和高磁感取向硅钢(HGO)的晶粒尺寸、晶界参数以及析出相质点的Zenner钉扎因子.结果表明,高斯晶粒与普通晶粒相比没有明显的尺寸优势,具有强烈高斯织构的HGO在晶界能和晶界活动性上与CGO的差异非常小,二者具有相近的临界Zenner因子;但HGO中析出相质点更为细小和弥散,其Zenner因子是CGO的2.8～5.0倍,因此HGO中Zenner因子更大,其高斯晶粒更容易率先达到临界条件而发生二次再结晶,从而在二次再结晶后具有更强的高斯织构.     

CGO硅钢各阶段织构遗传继承性的EBSD分析

利用EBSD技术对CGO硅钢热轧、中间退火、脱碳退火及二次再结晶退火组织及织构进行分析,研究了CGO硅钢各阶段加工制备过程中高斯{110}001晶粒的形状、尺寸及分布特点,分析了高斯取向晶粒在各工序过程中的遗传继承性特点。结果表明,CGO硅钢热轧板的次表层存在Goss取向晶粒,历经一次冷轧及中间退火后Goss取向晶粒基本消失,一次再结晶之后Goss织构仍不是主要织构,主要织构为{111}110和{111}112,说明Goss取向晶粒在二次再结晶退火前数量及尺寸上并不占优势,二次再结晶过程中Goss取向晶粒异常长大形成锋锐Goss织构。{111}110和{111}112织构组分的强度在一次冷轧中不断增加,{111}112织构组分的强度在二次冷轧后达到最大而{111}110织构组分是在初次再结晶后变强。     

湿H2气氛下CGO硅钢初次再结晶织构演变行为

通过对湿H2气氛下,相同退火温度、不同退火时间的CGO硅钢初次再结晶样品进行金相组织观察,并进行了EBSD微观织构分析,研究了CGO硅钢初次再结晶过程中的组织及再结晶织构演变行为。结果表明,在湿H2气氛下,820℃保温,CGO硅钢初次再结晶过程约在120 s时完成。随着退火时间的延长,γ面上{111}<112>织构含量逐渐减少,{111}<110>织构先减少后增多,随着再结晶的完成,部分{111}<112>取向晶粒向高斯{110}<001>取向转化的同时,也向{111}<110>取向转化,高斯{110}<001>织构含量逐渐增多。高斯取向晶粒较多是由{111}<112>取向晶粒转化而来,同时也证明了CGO硅钢高斯取向晶粒的二次再结晶异常长大生长机制为择优形核。     

常化温度对无抑制剂取向硅钢性能影响

在实验室中采用无抑制剂法制备取向硅钢,对无抑制剂取向硅钢的热轧和常化工艺进行了研究。结果表明,850℃常化的取向硅钢组织中具有更多的{111}面组分,有助于晶界迁移发生二次再结晶而形成单一Goss织构;而900℃、950℃常化后的取向硅钢中晶粒尺寸过大,晶界数量减少,不利于二次再结晶的发展。随常化温度升高;磁感应强度降低;铁损值增高。     

脉冲磁场对Hi-B钢初次再结晶织构的影响

采用原位连续检测的方法研究了脉冲磁场对高磁感取向硅钢(Hi-B钢)初次再结晶晶粒尺寸和织构的影响。结果表明,冷轧Hi-B钢760℃退火过程中,施加1.5 T脉冲磁场在一定程度上促进了晶粒再结晶长大过程,再结晶平均晶粒尺寸增长速率大于普通退火试样;脉冲磁场的施加不改变主要织构类型,退火后主要织构依然为γ织构;脉冲磁场使织构强度降低,且抑制γ织构的发展,促进Goss织构和{001}110织构的发展。     

取向硅钢二次再结晶过程中的取向选择行为

采用实验和计算的方法研究了取向硅钢二次再结晶织构的演变过程。发现取向硅钢通过二次再结晶过程中连续的取向选择,最终获得单一Goss ({110}001)织构。在二次再结晶动力学模型中引入依赖取向的相对晶界能系数,可定量描述不同偏差角Goss及非Goss取向晶粒的长大速率差异。通过分析初次再结晶晶粒尺寸分布、晶界特征和抑制力水平等因素对二次再结晶取向选择行为的耦合影响,提出增强Goss晶粒取向选择优势的多参数匹配方法。     

含Cu CGO硅钢高温退火过程的织构演变规律

对低温板坯加热工艺生产的以Cu2S为主要抑制剂的CGO硅钢的高温退火过程进行了试验,使用X射线衍射仪和电子背散射衍射技术对高温退火过程中不同阶段的织构演变规律进行了分析。结果表明：该工艺条件下CGO硅钢在700 ℃完成初次再结晶,1000 ℃时已经发生了二次再结晶,初次再结晶基体中以γ线织构和{112}<110>织构为主,Goss晶粒含量很少,平均位向偏差角为16°左右;二次再结晶发生后,Goss晶粒的位向偏差角降低到10°以下,随着退火温度的升高Goss晶粒的位向逐渐准确。     

含铜CGO硅钢高温退火过程中的织构演变规律

对低温板坯加热工艺生产的以Cu_2S为主要抑制剂的CGO硅钢的高温退火过程进行了试验,使用X射线衍射仪和电子背散射衍射技术对高温退火过程中不同阶段的织构演变规律进行了分析。结果表明,该工艺条件下CGO硅钢在700℃完成初次再结晶,1000℃时已经发生了二次再结晶,初次再结晶基体中以γ织构和{112}110织构为主,Goss晶粒含量很少,平均位向偏差角为16°左右;二次再结晶发生后,Goss晶粒的位向偏差角降低到10°以下,随着退火温度的升高Goss晶粒的位向逐渐准确。     

二次冷轧中间退火对基于CSP工艺的取向硅钢组织及织构的影响

在实验室模拟CSP工艺条件下制备了取向硅钢,研究了二次冷轧中间退火工艺对组织和织构的影响。结果表明,中间退火温度对取向硅钢脱碳,高温退火组织及织构均产生明显影响。经940 ℃中间退火后,取向硅钢脱碳再结晶晶粒较850 ℃中间退火的多,且再经高温退火处理后,晶粒粗化,最大晶粒尺寸达4.8 mm;高斯织构组分密度达27.00,较850 ℃中间退火试样高。     

渗氮及预处理对取向硅钢二次再结晶的影响

对硅钢进行离子渗氮,改变其表面氮浓度,可显著影响二次再结晶效果。结果表明,渗氮增量约为0.02wt%时最有利于Goss织构的形成。而影响取向硅钢二次晶粒平均尺寸的主要因素是初次晶粒尺寸和表面有效抑制剂数量密度。硅钢中氮含量的微小变化会极大地影响二次晶粒长大。氮含量0.0282wt%的硅钢样品经700℃×1 h预处理,其高温退火后的二次再结晶效果最好。     

日本高磁感取向硅钢最新进展(I)

收集整理日本2004年度硅钢专利文献152项,其中高磁感Hi-B取向硅钢专利文献34项.Hi-B钢最新技术涉及诸多方面,主要有：开发新型抑制剂和高磁场用钢、研究低温板坯加热工艺、改进脱碳退火工艺、改善薄膜外观质量,采取措施降低铁损等,本文仅对其中的部分进行分析、研究,以供借鉴.     

日本高磁感取向硅钢最新进展(Ⅱ)

收集整理日本2004年度硅钢专利文献152项,其中高磁感Hi—B取向硅钢专利文献34项。Hi—B钢最新技术涉及诸多方面,本文对开发高温退火隔离剂,改善最终高温退火工艺,无铬薄膜的形成方法,改善薄膜质量进行了分析、研究,以供借鉴。     

New process for production of ultra-thin grain oriented silicon steel

The Hi-B silicon steels were cold rolled by cross shear rolling (CSR) with different mismatch speed ratio(MSR)s and conventional rolling(CR) respectively, followed by primary recrystallization annealing. The effects of MSR and annealing temperature on magnetic properties of ultra-thin grain oriented silicon steel were analyzed. Experimental results show that, with the increase of MSR, the magnetic properties can be remarkably improved. The higher the annealing temperature is, the higher the magnetic induction and the lower the iron loss in ultra-thin silicon steel is.     

低温取向硅钢高温退火抑制剂的演化

取向硅钢利用析出物作为抑制剂,抑制初次再结晶晶粒的长大,抑制剂是取向硅钢发生二次再结晶的基本条件之一。文中通过低温板坯加热技术制备取向硅钢,采用透射电镜（TEM）观察并研究了高温退火阶段抑制剂的演化过程。结果表明,渗氮后形成的非晶态Si3N4析出物不稳定,在700～750℃退火升温阶段转化为（Al,Si）N;（Al,Si）N颗粒在800℃发生团聚,随后长大并粗化;（Al,Si）N是低温取向硅钢主要抑制剂,随退火温度的升高,（Al,Si）N抑制力大幅下降。     

Effect of Initial Goss Texture Sharpness on Texture Evolution and Magnetic Properties of Ultra-thin Grain-oriented Electrical Steel

In this study, high-and low-grade grain-oriented electrical steels were used as the initial materials to produce0.08-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 recrystallization 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.     

电工钢中黄铜织构行为及其对Goss织构的影响

本文通过EBSD取向成像技术检测追踪了取向硅钢热轧、脱碳退火及二次再结晶过程中黄铜取向晶粒的形成规律.结果表明,黄铜取向的形成是热轧时Goss取向在剪切力作用下向铜型取向转动受阻而绕法向转动的结果.与Goss晶粒和{111}〈112〉取向晶粒类似,黄铜取向和{111}〈110〉取向晶粒之间存在形变与再结晶相互转化的密切关系;二次再结晶时若抑制剂钉扎控制不当,在次表层的Goss晶粒快速长入中心层之前,黄铜取向晶粒已长成大尺寸并接触样品表面,随后的Goss大晶粒就很难吞并黄铜取向晶粒.     

Secondary Recrystallization Behaviors of Grain-Oriented 6.5 wt% Silicon Steel Sheets Produced by Rolling and Nitriding Processes

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 k Hz 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.     

Hi-B钢二次再结晶退火过程中未异常长大Goss晶粒晶界特征

采用中断法并结合电子背散射衍射(EBSD)技术,研究了Hi-B钢二次再结晶退火过程中大量未异常长大Goss取向晶粒的晶界特征。结果表明:未异常长大Goss取向晶粒的晶粒尺寸相较于基体晶粒和相邻晶粒并没有明显的差异性。同时未异常长大Goss取向晶粒与异常长大Goss取向晶粒周围的HE晶界和CSL晶界比例也没有明显的差异。在二次再结晶退火过程中,尺寸优势、HE晶界、CSL晶界和Goss取向偏离度都不能保证Goss取向晶粒发生异常长大。而随着退火温度的升高,Goss取向晶粒有逐渐向标准Goss晶粒取向靠拢的趋势。     

取向电工钢中MnS析出粒子在冷变形过程中的行为

利用场发射扫描电子显微镜观察了试验材料Fe-3.12%Si-0.11%Mn-0.021%S中MnS析出粒子在变形量为0%～68%的冷压缩加工过程中的分布状态,统计了MnS粒子的总面密度及不同尺寸范围粒子的面密度,分析了冷压缩加工过程中MnS粒子的变化规律。结果表明,冷变形过程造成了几十纳米尺寸MnS粒子的碎化和10 nm以下粒子的少量回溶行为;但未能造成尺寸过于粗大粒子的细化。分析认为,MnS粒子与基体的界面能和塑性变形造成位错密度的明显升高构成了细小粒子回溶的驱动力。MnS粒子在冷轧过程中的细化,有利于防止初次再结晶晶粒粗化,促进取向电工钢二次再结晶过程的顺利进行及锋锐Goss织构的生成。     

Control of recrystallization during high-temperature hot-rolling of grain-oriented silicon steel

Recrystallization kinetics of 3 % Si steel after hot rolling in the temperatures between 1373 and 1573 K, which is quite important to obtain uniform magnetic properties, was studied. Recrystallization rate after hot rolling was relatively slow because of low dislocation density, which resulted from rapid recovery, and its behavior was strongly influenced by the initial grain size and coexistence of the γphase. Based on these Findings, controlling technology of recrystallization during hot rolling of grain-oriented Si steels is discussed.