中间退火温度对Fe-3wt%Si取向硅钢抑制剂演变的影响

在实验室模拟CSP工艺采用二次冷轧制备了Fe-3wt%Si取向硅钢,研究了取向硅钢制备过程中,中间退火温度对抑制剂演变的影响。结果表明,中间退火温度为940 ℃时,中间退火和脱碳退火后试验钢中析出抑制剂尺寸更加细小,分布更加弥散,数量更多;高温退火后,抑制剂析出明显减少,只有少量粗大未熔析出,析出物大多为不规则的(Al,Si)N及(Cu,Mn)S复合析出。     

取向硅钢低温板坯加热高温二次再结晶退火中抑制剂的析出特点

利用透射电镜研究了采用"固有抑制剂法"低温板坯加热试制普通取向硅钢冷轧板,高温二次再结晶退火过程中抑制剂的析出行为,分析了各种抑制剂对初次再结晶的抑制作用。结果表明:除常规AlN和AlN+Cu2S析出物之外,还有少量短棒状MnSiN2析出相(正交结构);AlN相具有强烈的抑制效果,起到了主抑制剂作用;少量的MnSiN2相具有辅助抑制作用,同时在高温二次再结晶退火条件下,部分MnSiN2分解并与基体中的Al作用生成AlN,加强了AlN的抑制作用。     

取向硅钢退火新工艺

取向硅钢退火新工艺传统的晶粒取向硅钢要求板坯高温（１３５０ｏＣ）均热，以获得抑制剂析出物（ＭｎＳ或ＡＩＮ）的最佳弥散，同时也要求高温（１２００℃）箱式退火，以实现二次再结晶后钢的净化。这些高温处理能耗大且设备投资高。为此提出制造取向硅钢的新工艺，它要...     

含锡取向硅钢高温二次再结晶退火过程中抑制剂的析出特点

采用透射电镜研究了含锡取向硅钢高温二次再结晶退火过程中抑制剂的析出行为,分析了抑制剂对初次再结晶的抑制作用。结果表明,析出物除了常规的AlN和MnS外,还有少量Sn单质;其中AlN和MnS相是主要抑制剂,具有强烈的抑制作用;少量Sn相起辅助抑制作用,控制析出物AlN的尺寸和数量,有助于主抑制剂的弥散分布。抑制剂在600~700 ℃时开始析出长大,900 ℃显著长大,1020 ℃平均尺寸达到最大值;抑制剂的尺寸随退火温度升高而增大,体积分数、分布密度则先增大后减少。当退火温度达到1000 ℃时,析出物平均粒径约50.3 nm,体积分数最大约3.81%,分布密度约5.9×10¹⁴ 个/cm³。根据试验和Zener因子综合判定抑制力,Zener因子随退火温度升高而增加,在900 ℃达到最大139,析出物分布密度达到最大8.9×10¹⁴个/cm³;在1020 ℃时,Zener因子几乎为零,完成二次再结晶过程。     

不同厚度的取向硅钢片组织和磁性能研究

对不同厚度的取向硅钢进行了不同工艺的退火处理,利用金相、TEM、磁性能检测对其进行了分析。结果表明:厚0.15、0.08mm的成品磁性较差,组织以变形带为主,未完成再结晶;厚0.08mm试样比厚0.15mm试样有更多的再结晶晶粒;550℃退火时析出的抑制剂较多,抑制剂可促进高斯织构的形成,尤其是Al N;再结晶程度越好,高斯取向织构数量越多,成品的磁性能越好。     

Nb对取向硅钢热轧板中抑制剂析出行为的影响

采用金相显微镜(OM)和透射电镜(TEM)研究了Nb对取向硅钢中抑制剂析出行为的影响。结果表明,取向硅钢中的抑制剂不仅有Al N和MnS的细小析出物,还有大量细小的Nb(C,N)析出颗粒,0.050%Nb硅钢热轧板中的析出物的面积密度较大、平均晶粒尺寸较小,且0.050%Nb试样热轧组织中再结晶分数较低,回复和变形组织较多。采用Thermal-Calc软件验证了中温加热的可行性,表明在取向硅钢中加入适当的Nb可降低取向硅钢的加热温度。     

含稀土取向硅钢高温铁素体区的再结晶及抑制剂析出行为

利用Gleeble 1500D、SEM、TEM、ICP等研究手段,分析了含稀土取向硅钢在1200℃铁素体区热轧变形30%、保温不同时间后水冷的再结晶及抑制剂析出行为。结果表明,含稀土取向硅钢高温铁素体区热轧后仅发生动态回复,未发生动态再结晶,析出相的数量没有明显增加;热轧后保温20 s左右开始发生静态再结晶,抑制剂析出相开始析出并且长大,再结晶发生率越高,析出相体积分数增长越快。变形结束后析出相中Cu₂S和MnS数量相差不多,再结晶发生率为64%时,MnS增长约7.4%,Cu₂S增长约19.34%。析出相大多于晶内析出,随保温时间延长部分抑制剂逐渐在晶界处形核并长大。     

钛微合金化无取向硅钢的再结晶行为

利用半小时等温法、光学显微镜、显微硬度计和透射电镜等研究了钛微合金化无取向硅钢和普通无取向硅钢的再结晶温度、硬度、显微组织和析出物分布。结果表明：钛微合金化无取向硅钢的再结晶温度比普通无取向硅钢的再结晶温度高55℃;两种钢的显微组织变化规律相同,随着退火温度升高再结晶晶粒开始出现,硬度降低,变形组织逐渐被取代;钛微合金化无取向硅钢中含有纳米级含钛析出物,分布在位错附近,在退火过程中会钉扎位错,阻碍晶界移动延缓再结晶。     

硅钢极薄带三次再结晶退火过程中的组织演化

采用异步轧制方法将成品工业取向硅钢板冷轧到0.10mm,然后在氢气热处理炉中进行三次再结晶高温退火,研究异步轧制硅钢极薄带退火过程中的再结晶过程.结果表明,硅钢极薄带在800℃退火时发生初次再结晶,晶粒取向主要为高斯取向,磁感低;900℃时初次再结晶中极少数晶粒突然长大而发生二次再结晶,对0.1mm的极薄带不能形成完善的高斯织构,磁性能下降;在1200℃时在合适的退火条件下可以发生三次再结晶,在极薄带中获得了取向集中的高斯织构和优异的磁性能.     

基于CSP工艺取向硅钢抑制剂析出及再结晶脱碳退火行为

利用SEM、EBSD和XRD等相关技术,研究了脱碳退火工艺对基于CSP工艺取向硅钢再结晶退火后的组织、晶界特征及析出相的影响。结果表明,脱碳退火5 min后,取向硅钢的再结晶晶粒尺寸较小,晶界特征理想,高能晶界Σ3和Σ9富集在{111}112、{112}1 10和{332}533等有利取向周围,促进了二次再结晶过程中高斯晶粒的形成;退火时间为7 min时,大角度晶界和{111}112、{112}1 10、{332}533等有利取向数量下降,不利于高斯晶粒的形核和长大;经不同脱碳退火工艺(3 min、5 min和7 min),析出相总体呈弥散状态分布,析出物在脱碳退火5 min的析出细小且分布均匀。     

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钢二次再结晶动力学及换气温度对磁性能的影响

采用＂中断法＂确定了Hi-B取向硅钢二次再结晶动力学,即二次再结晶的开始温度和温度区间,对比分析了Hi-B取向硅钢与CGO取向硅钢二次再结晶动力学的差异及原因;考察了不同换气温度对二次再结晶晶粒尺寸和磁性能的影响。结果表明,在氮氢混合气氛下,Hi-B硅钢二次再结晶过程比CGO硅钢滞后,发生在1040℃至1120℃之间,其动力学曲线近似为S型;二次再结晶退火时,随着换气温度的升高,最终晶粒尺寸增大,磁感和铁损增加。     

Experimental Studies and Numerical Simulation on the Nitriding Process of Grain-Oriented Silicon SteelEI北大核心CSCD

Grain-oriented silicon steel (GOSS) is an important functional material used as lamination cores in various transformers. Its magnetic properties are strongly dependent on the sharpness of Goss texture, which is developed during the secondary recrystallization annealing of product. In order to save energy and reduce cut-down operation costs, Nippon steel first lowered the slab-reheating temperature from 1350-1400 degrees C to 1150 degrees C and adopted the nitriding process to form nitride inhibitors before recrystallization annealing in 1970s. In this new process, nitriding is the critical process because it controls the size, distribution and volume fraction of nitride precipitates, which then determines the subsequent development of Goss texture. Although it is of great importance for good quality control of industrial GOSS product, unfortunately, a quantitative mathematic modeling on nitriding kinetics is still in lack. In this work, nitriding kinetics were both measured experimentally and simulated by modeling. The N contents after various nitriding periods and N concentration gradient across thickness were both measured. It has been found that the N content increases slowly at the beginning of 60 s and then much more rapidly during nitriding. There exists a sharp N concentration gradient within the depth of 0.03 mm to the steel sheet surface, which diminishes after about 0.04 mm depth. With the different assumptions on N-transfer coefficient from gas to the steel matrix, the first mathematic modeling on nitriding kinetics of GOSS has been successfully established and solved numerically. The simulation results suggest that only when the N-transfer coefficient, f, changes with time following the Avrami function, f=A(1-exp(-kt(n))), the calculated nitriding kinetics are consistent with the measurements. Such an Avrami-type dependence results from the reduction kinetics of oxide layer on the surface of silicon steel sheet during nitriding, in which both plate-like and spherical oxides were observed at the beginning but most of them became spherical after nitriding.     

基于Stoney公式适用性分析——取向硅钢绝缘涂层张应力的计算

目的改善涂层张应力状态,进而提升取向硅钢的电磁性能。方法用扫描电镜、辉光光谱仪分析了添加磷酸盐的胶体二氧化硅绝缘涂层的厚度和微观结构,采用静态拉伸试验得到了取向硅钢沿不同位向的力学特性。在此基础上,根据取向硅钢各向异性的特点和绝缘涂层的实际状态,用Stoney公式对取向硅钢涂层应力的适用性进行了讨论。结果取向硅钢的各向异性不满足Stoney公式的适用条件,实际测试的取向硅钢的力学性能结果表明,取向硅钢符合正交对称各向异性材料的一般规律,据此给出了涂层对取向硅钢产生的张应力的计算公式,利用该公式对不同涂覆工艺条件下的胶体二氧化硅绝缘涂层的张应力进行了计算,涂层厚度在1～2μm范围内,双面张应力的计算值为4～11 MPa。结论文中张应力的计算公式不仅适用于取向硅钢,同样适用于其他基体为各向异性的类似情况。通过张应力的计算可知,涂层厚度与张应力呈正相关,张应力的增大将会促使取向硅钢的铁损降低。因此,开发大张力的绝缘涂层,是进一步改善取向硅钢磁性能的有效途径之一。     

Investigation of nitrogen mass transfer within an industrial plasma nitriding system I: The role of surface deposits

It has been proposed that in plasma nitriding, sputtering of material from biased components within the chamber assists in the nitrogen mass transfer process. Here, we investigate the effects of this sputter deposition process on the nitriding response of biased and unbiased AISI P20 steel samples mounted in a large-scale plasma nitriding system operated at 520 °C. Films with nanostructured morphologies resulting from Volmer-Weber film growth were observed on Si substrates placed adjacent to AISI P20 steel substrates after nitriding experiments. Auger depth profiling revealed that the films on the Si substrates had a stoichiometric ratio of 4:1 Fe:N. This suggested that the particles consisted largely of Fe₄N and it was concluded that they were formed from atoms and small clusters sputtered from biased components in the chamber. Despite the deposition of these films, no significant improvement in surface hardness was observed in the steel samples unless bias was applied to them. Furthermore, the maximum hardness achieved in biased P20 samples after the nitriding process occurred in the samples positioned adjacent to the Si samples supporting the thinnest deposited films. These findings do not support the proposition that in plasma nitriding, nitrogen mass transfer occurs predominantly by sputter deposition of iron nitride.     

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.     

晶粒取向硅钢微组织和微织构演变过程的研究

研究了晶粒取向硅钢微组织和微织构的演变过程，研究发现了大量的高斯取向与｛111｝〈112〉取向有关。此外，发现了单晶的2种高斯取向晶粒都出现在冷轧阶段，并具有不同的一次再结晶行为。本研究从单晶实验中得到的结果，有助于工业生产解决高斯织构异常生长的问题。     

取向硅钢韧脆转变温度及影响因素

以鞍钢0.27 mm规格高磁感取向硅钢板为研究对象,通过测量不同温度下常化样品的力学性能,结合微观组织和断口形貌观察,确定其韧脆转变温度及影响因素。结果表明:该取向硅钢临界断裂强度约为590 MPa,韧脆转变温度区间为60~80 ℃。在0~100 ℃测试温度范围内,随温度升高,磷元素偏聚浓度由90%左右降低至65%左右,相应平衡时间短,有利于提高晶界结合强度并弱化脆断倾向。此外,常化组织晶粒粗化和铁素体与珠光体不均匀变形产生的微裂纹是脆化的主要组织因素,不利于取向硅钢的冷轧加工。     

浇注成型Si_3N_4-SiC制品的研究

以经过颗粒整形的绿碳化硅及硅粉为原料,以阿拉伯树脂、硅酸钠等为添加剂,制做了氮化硅结合碳化硅制品。在对真空氮化烧结温度控制系统和烧成机理进行分析的基础上,开发制定了合理的氮化烧成工艺曲线。烧结出的浇注成型Si3N4-SiC烧嘴套经过多家公司应用验证,性能优良,可替代进口产品。提高了产品的成品率。