粉末冶金法制备高硅硅钢片的轧制和热处理工艺研究
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摘要
硅含量在6.5%左右的高硅硅钢片具有十分优异的磁性能：磁导率高、铁损低、磁致伸缩小,可以实现低能耗、低噪声,是一类节能环保的软磁材料。但是6.5%硅钢是一种脆性材料,不可轧制加工,因此不能用传统轧制的工艺来制备。目前只有日本采用CVD法实现了工业化生产,但其成本高昂。近十几年来,由于粉末冶金法成本低,成为人们制备高硅硅钢片的又一途径。
本文采用不同粉体原料,分别采用粉末轧制法和块体轧制法,探索了用粉末冶金法制备高硅硅钢片的工艺条件,研究了影响轧制工艺和硅钢磁性能的因素,得出了比较适宜的制备工艺,制得了性能较好的高硅硅钢片。
首先,以铁粉为对象,采用有限元法对粉体轧制过程进行了模拟和实验。模拟和实验结果表明,采用粉体轧制时,上下表面由于受力情况与内部不同,多呈现疏松的结构。粉体轧制时,粉体的流动性和辊缝是影响轧制带材的重要因素。辊缝是影响带材密度的主要因素,高流动性的粉体轧制得到的带材较为致密。当原料中存在流动性差的另一硅相时,流动性差的硅相易损失,使带材元素含量偏离配比。
纯铁在1400℃以下时难以烧结致密化。铁硅之间的扩散反应与粉体粒度和温度密切相关,从而影响烧结体的轧制能力,最终影响硅钢的性能。当硅粉粒度适当时,经初次热处理后,得到既无单质Si,又具有较好变形能力时,经二次轧制和高温热处理可以得到密度较高、性能较好的硅钢片。
加入少量的Sn可以提高Si与Fe的反应能力,从而在低温短时间内实现Si与Fe的反应。Sn的加入还可改善Fe的烧结,容易得到大晶粒的Fe。含H2的气氛对烧结硅钢不利,易造成硅的氧化。比较适宜的烧结气氛为Ar。
采用超细硅粉和铁粉混合后,经500-1000℃SPS处理后得到的块体材料具有变形能力,可以通过轧制得到厚度为0.3-0.4mmm的片材,但是经高温热处理得到的硅钢片材氧化严重,带材致密度不高,材料的磁性能比粉末轧制法制备的材料差。
以Fe和FeSi为原料经SPS烧结可制备出具有轧制能力的硅钢锭。FeSi原料的颗粒粒度、SPS温度、压力对Fe和FeSi颗粒之间的扩散反应有影响,从而影响最终产物的物相显微结构。由粗颗粒原料烧结的块体具有良好的延展性,表现为韧性断裂；随粒度的减小、烧结温度的升高,烧结试样延展性变差,逐渐变成脆性断裂。制备致密且具有良好延展性的硅钢锭的适宜工艺条件为：粗FeSi颗粒在1100℃以下温度烧结、烧结压力50MPa。
以具有可轧能力且密度高的硅钢块体为原料,经轧制减薄和退火处理,可以制备出性能较好的高硅硅钢片。其磁性能为饱和磁化强度17740Gs,矫顽力3.670e。其饱和磁化强度与由Fe和Si混合后再轧制烧结制备的硅钢相当,但矫顽力约降低9倍。
The high silicon steels with the silicon content of about 6.5% are energy-saving and environment-protected soft magnetic material with low-energy as well as low noise due to the excellent magnetic properties such as high magnetic permeability, low core loss, and low magnetostriction. However, the silicon steels with 6.5% silicon are too brittle to be rolled thus cannot be fabricated with the traditional rolling process. Up to now, only the Japanese have achieved industrialized production by CVD method with high cost. During recent decades, powder metallurgy, with low cost, has become another approach for the fabrication of the high silicon steels.
In this paper, powder rolling and bulk rolling were applied with different raw powder materials to explore the process conditions of high silicon steels fabrication by powder metallurgy. The factors affecting the rolling process and magnetic properties of silicon steels were investigated. The suitable fabrication process as well as silicon steels with good properties were obtained.
At the beginning, the simulation and experiment was carried out based on the finite element method, with iron as the objection. The loose structure was more likely to appear due to different load-carrying conditions between the inner and the out surface during powder rolling. The strip quality was greatly influenced by the roll gap and the powder flow ability since the gap was the main factor contributing to the strip density and dense strip could be attained with high flow ability powder. When another poor flow ability silicon phase existed in the raw material, the content of the strip could drift due to easy loss of such silicon phase.
Pure iron is difficult to densify during sintering below 1400℃. The diffusion reaction between iron and silicon is closely related to the powder granularity and temperature, thus affecting the rolling ability as well as the final properties. With the proper silicon powder granularity, the green strip, having a good deformation ability and no elemental Si after the first heat treatment, could transform to high density silicon steels after the second rolling and heat treatment.
The reaction between Si and Fe could be stimulated by small introduction of Sn thus being achieved in low temperature and short time, which also improved the sintering of Fe with a large crystal grain. The atmosphere with H2 deteriorated the sintering of silicon steel and resulted in the oxidation of Si while Ar atmosphere is better.
The bulk material, with the blend of ultra-fine Si and Fe powder, had the deformation ability after 500-1000℃SPS treatment, which can transform to strip with the thickness of 0.3-0.4mm by rolling. They were severely oxidized after high temperature heat treatment with lower density and magnetic properties compared to materials by powder rolling.
The silicon steel ingots can be fabricated by SPS technique with Fe and FeSi as the raw materials. The powder granularity as well as SPS temperature and pressure can affect the diffusion reaction between Fe and FeSi particles, hence influencing the microstructure of the final products. The bulk material with coarse powder had good ductility and performed ductile failure. With the decreasing granularity and the increasing temperature, the ductility degraded and brittle failure gradually took place. The proper processing condition for dense and ductile silicon steels should be:the coarse FeSi particles with the sintering temperature below 1100℃and the pressure 50MPa.
The high silicon steels can be produced by roll-thinning and annealing with the highly dense silicon steel bulk as the raw materials. The saturated magnetization was 17740Gs and coercive force was 3.67Oe. The saturated magnetization is equivalent to that silicon steel blended by Fe and Si, but the coercive force reduced 9 times.
本文采用不同粉体原料,分别采用粉末轧制法和块体轧制法,探索了用粉末冶金法制备高硅硅钢片的工艺条件,研究了影响轧制工艺和硅钢磁性能的因素,得出了比较适宜的制备工艺,制得了性能较好的高硅硅钢片。
首先,以铁粉为对象,采用有限元法对粉体轧制过程进行了模拟和实验。模拟和实验结果表明,采用粉体轧制时,上下表面由于受力情况与内部不同,多呈现疏松的结构。粉体轧制时,粉体的流动性和辊缝是影响轧制带材的重要因素。辊缝是影响带材密度的主要因素,高流动性的粉体轧制得到的带材较为致密。当原料中存在流动性差的另一硅相时,流动性差的硅相易损失,使带材元素含量偏离配比。
纯铁在1400℃以下时难以烧结致密化。铁硅之间的扩散反应与粉体粒度和温度密切相关,从而影响烧结体的轧制能力,最终影响硅钢的性能。当硅粉粒度适当时,经初次热处理后,得到既无单质Si,又具有较好变形能力时,经二次轧制和高温热处理可以得到密度较高、性能较好的硅钢片。
加入少量的Sn可以提高Si与Fe的反应能力,从而在低温短时间内实现Si与Fe的反应。Sn的加入还可改善Fe的烧结,容易得到大晶粒的Fe。含H2的气氛对烧结硅钢不利,易造成硅的氧化。比较适宜的烧结气氛为Ar。
采用超细硅粉和铁粉混合后,经500-1000℃SPS处理后得到的块体材料具有变形能力,可以通过轧制得到厚度为0.3-0.4mmm的片材,但是经高温热处理得到的硅钢片材氧化严重,带材致密度不高,材料的磁性能比粉末轧制法制备的材料差。
以Fe和FeSi为原料经SPS烧结可制备出具有轧制能力的硅钢锭。FeSi原料的颗粒粒度、SPS温度、压力对Fe和FeSi颗粒之间的扩散反应有影响,从而影响最终产物的物相显微结构。由粗颗粒原料烧结的块体具有良好的延展性,表现为韧性断裂；随粒度的减小、烧结温度的升高,烧结试样延展性变差,逐渐变成脆性断裂。制备致密且具有良好延展性的硅钢锭的适宜工艺条件为：粗FeSi颗粒在1100℃以下温度烧结、烧结压力50MPa。
以具有可轧能力且密度高的硅钢块体为原料,经轧制减薄和退火处理,可以制备出性能较好的高硅硅钢片。其磁性能为饱和磁化强度17740Gs,矫顽力3.670e。其饱和磁化强度与由Fe和Si混合后再轧制烧结制备的硅钢相当,但矫顽力约降低9倍。
The high silicon steels with the silicon content of about 6.5% are energy-saving and environment-protected soft magnetic material with low-energy as well as low noise due to the excellent magnetic properties such as high magnetic permeability, low core loss, and low magnetostriction. However, the silicon steels with 6.5% silicon are too brittle to be rolled thus cannot be fabricated with the traditional rolling process. Up to now, only the Japanese have achieved industrialized production by CVD method with high cost. During recent decades, powder metallurgy, with low cost, has become another approach for the fabrication of the high silicon steels.
In this paper, powder rolling and bulk rolling were applied with different raw powder materials to explore the process conditions of high silicon steels fabrication by powder metallurgy. The factors affecting the rolling process and magnetic properties of silicon steels were investigated. The suitable fabrication process as well as silicon steels with good properties were obtained.
At the beginning, the simulation and experiment was carried out based on the finite element method, with iron as the objection. The loose structure was more likely to appear due to different load-carrying conditions between the inner and the out surface during powder rolling. The strip quality was greatly influenced by the roll gap and the powder flow ability since the gap was the main factor contributing to the strip density and dense strip could be attained with high flow ability powder. When another poor flow ability silicon phase existed in the raw material, the content of the strip could drift due to easy loss of such silicon phase.
Pure iron is difficult to densify during sintering below 1400℃. The diffusion reaction between iron and silicon is closely related to the powder granularity and temperature, thus affecting the rolling ability as well as the final properties. With the proper silicon powder granularity, the green strip, having a good deformation ability and no elemental Si after the first heat treatment, could transform to high density silicon steels after the second rolling and heat treatment.
The reaction between Si and Fe could be stimulated by small introduction of Sn thus being achieved in low temperature and short time, which also improved the sintering of Fe with a large crystal grain. The atmosphere with H2 deteriorated the sintering of silicon steel and resulted in the oxidation of Si while Ar atmosphere is better.
The bulk material, with the blend of ultra-fine Si and Fe powder, had the deformation ability after 500-1000℃SPS treatment, which can transform to strip with the thickness of 0.3-0.4mm by rolling. They were severely oxidized after high temperature heat treatment with lower density and magnetic properties compared to materials by powder rolling.
The silicon steel ingots can be fabricated by SPS technique with Fe and FeSi as the raw materials. The powder granularity as well as SPS temperature and pressure can affect the diffusion reaction between Fe and FeSi particles, hence influencing the microstructure of the final products. The bulk material with coarse powder had good ductility and performed ductile failure. With the decreasing granularity and the increasing temperature, the ductility degraded and brittle failure gradually took place. The proper processing condition for dense and ductile silicon steels should be:the coarse FeSi particles with the sintering temperature below 1100℃and the pressure 50MPa.
The high silicon steels can be produced by roll-thinning and annealing with the highly dense silicon steel bulk as the raw materials. The saturated magnetization was 17740Gs and coercive force was 3.67Oe. The saturated magnetization is equivalent to that silicon steel blended by Fe and Si, but the coercive force reduced 9 times.
引文
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