CN111094212A - 渗硅处理炉用耐火物 - Google Patents
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Abstract
本发明的目的在于提供一种变质、脆化少,寿命长的渗硅处理炉用耐火物。所述渗硅处理炉用耐火物含有合计35质量%以上的选自硅的氧化物、硅的氮化物和硅的氧氮化物中的1种或2种以上和合计0.05质量%以下的碱金属,并且,气孔率为25体积%以下,压缩强度为5MPa以上。
Description
技术领域
本发明涉及一种在如钢带的连续渗硅处理炉那样的使用氯化硅气体的炉中使用的耐火物。
背景技术
硅钢板具有优异的软磁特性,因此作为变压器、马达的铁芯材料广泛使用。已知硅钢板显示出如下优异的磁特性,即Si含量越多铁损越少,Si约为6.5wt%时磁致伸缩为0,最大透磁率成为峰值等。作为工业上制造这样的高硅钢板的方法,例如已知有如专利文献1所示的利用气体渗硅法的制造方法。该制造方法能够通过将如下的一系列工序作为连续生产线而高效地制造高硅钢带,即,通过加热Si含量比较低的钢带并在含有氯化硅气体(SiCl4)的非氧化性气体气氛中进行渗硅处理,从而使Si渗透,接着实施使Si向板厚方向扩散的扩散热处理,冷却后卷绕成钢圈状。
进行上述渗硅处理的连续渗硅处理炉在1200℃以上的炉内温度下长时间运转,并且,气氛气体中含有的氯化硅气体(SiCl4)是反应性非常高、腐蚀性强的气体。因此存在如下问题:在高温的炉内活性化的氯化硅气体与作为连续渗硅处理炉的炉材料的耐火物发生反应,使耐火物劣化。
作为连续渗硅处理炉用的耐火物,例如已知应用专利文献2、3中记载的耐火物。
现有技术文献
专利文献
专利文献1:日本特开昭62-227078号公报
专利文献2:日本特开平10-147856号公报
专利文献3:日本特开平08-169750号公报
发明内容
另一方面,存在如下问题:在高硅钢板的制造中途作为副产物产生的氯化铁(气体)渗透到炉内的耐火物中,在炉壁或炉床附近的温度降低部分发生凝聚或凝固。该凝聚·凝固的氯化铁堆积在耐火物内而与耐火物中的氧化物进行还原反应,促进耐火物的变质、脆化。
另外,在炉内的耐火物因修补等原因暴露于大气中的情况下,堆积在耐火物中的氯化铁吸收大气中的水分而膨胀。其结果,耐火物本身的体积增加而膨胀,因此炉壁、炉床的耐火物从炉内侧溢出,在耐火物产生龟裂而破裂。因此,存在耐火物的寿命短,更新周期变短的问题。
已知使用专利文献2、3中记载的耐火物时,能够抑制因氯化硅气体导致的耐火物的变质·脆化,但是难以抑制由氯化铁导致的耐火物的变质·脆化的促进。
本发明是鉴于上述实际情况而完成的,目的在于提供一种变质、脆化少,寿命长的渗硅处理炉用耐火物。
本发明人等进行了反复深入的研究,其结果获得如下见解:通过使用具有规定的成分组成且气孔率低的耐火物,从而能够提高耐火物的寿命,延长更新周期。
本发明是基于这样的见解而完成的,具有以下的宗旨。
[1]一种渗硅处理炉用耐火物,含有合计35质量%以上的选自硅的氧化物、硅的氮化物和硅的氧氮化物中的1种或2种以上和合计0.05质量%以下的碱金属,并且,气孔率为25体积%以下,压缩强度为5MPa以上。
[2]根据[1]所述的渗硅处理炉用耐火物,其中,还含有合计1.0质量%以下的Mg、Ca、Ti、Fe、Cr和Zr的各氧化物。
[3]根据[1]或[2]所述的渗硅处理炉用耐火物,其中,含有合计90质量%以上的选自硅的氧化物、硅的氮化物和硅的氧氮化物中的1种或2种以上。
根据本发明,能够提供一种变质、脆化少,寿命长的渗硅处理炉用耐火物。因此,如果应用本发明的耐火物作为使用氯化硅气体的连续渗硅处理炉的耐火物,则长时间不发生变质、脆化,显示优异的耐久性。因此,在利用气体渗硅法的高硅钢板的连续生产线中,不产生耐火物的劣化等,能够进行长期间稳定的作业。
附图说明
图1是制造高硅钢板的连续渗硅处理设备的示意图。
具体实施方式
制作由各种材质构成的耐火物。将这些耐火物置于含有氯化硅气体的气氛(SiCl4:约15vol%,炉内温度:约1200℃)的炉内3个月时间,检测各耐火物的外观、重量、体积等的变化。其结果可知大量含有硅的氧化物(二氧化硅)、硅的氮化物(氮化硅)和硅的氧氮化物(氧氮化硅)中的任1种或2种以上的耐火物对氯化硅气体的损伤最少。与此相对,发现由硅的碳化物构成的耐火物的损伤程度大。
接下来,作为耐火物对氯化硅气体的耐损伤性的评价,对耐火物表面的变质状况、脆化状况进行了检测,研究了变质状况、脆化状况与硅的氧化物、硅的氮化物、硅的氧氮化物的合计含量之间的关系。
其结果是选自硅的氧化物、硅的氮化物、硅的氧氮化物中的1种或2种以上的合计含量小于35质量%的耐火物成为表面变质、脆化而存在缺损的状态或产生了发丝状裂纹的状态,并且龟裂、剥落的产生也显著。相对于此,选自硅的氧化物、硅的氮化物、硅的氧氮化物中的1种或2种以上的合计含量为35质量%以上的耐火物虽然看到一部分产生了龟裂,但不是导致炉材表层部的脱落这样的变质、脆化,可以判断该耐火物基本可以继续使用。
由此,本发明中,将耐火物中含有的硅的氧化物、硅的氮化物、硅的氧氮化物的含量规定为合计35质量%以上的选自硅的氧化物、硅的氮化物、硅的氧氮化物中的1种或2种以上。优选含有合计90质量%以上的选自硅的氧化物、硅的氮化物、硅的氧氮化物中的1种或2种以上。通过设为90质量%以上,变质·脆化显著减少,也不产生龟裂的产生,得到良好的结果。
本发明中,作为耐火物中含有的硅的氧化物、硅的氮化物、硅的氧氮化物,优选为氮化硅、熔融二氧化硅,特别优选为熔融二氧化硅。
本发明中,将耐火物中含有的碱金属的含量规定为合计0.05质量%以下。耐火物中含有的碱金属有助于与氯化硅气体的反应性。如果碱金属的含量超过0.05质量%则进行耐火物与氯化硅气体的反应,有可能在耐火物表面产生龟裂或出现缺损。
本发明中,优选将耐火物中含有的Mg、Ca、Ti、Fe、Cr和Zr的各氧化物的含量的合计设为1.0质量%以下。耐火物中含有的Mg、Ca等的氧化物,也有助于与氯化硅气体的反应性。如果Mg、Ca等的氧化物的含量超过1.0质量%则进行耐火物与氯化硅气体的反应,有可能在耐火物表面产生龟裂或出现缺损。
作为耐火物的上述物质以外的剩余部分,为Al2O3、杂质,作为杂质可以含有上述物质以外的金属氧化物等。
还存在如下问题:在高硅钢板的制造中途作为副产物产生的氯化铁(气体)渗透到炉内的耐火物中,在炉壁、炉床附近的温度降低部分发生凝聚或凝固。该凝聚或凝固的氯化铁堆积在耐火物内,从而进行与耐火物中的氧化物的还原反应,促进耐火物的变质、脆化。另外,在炉内的耐火物因修补等原因暴露于大气中的情况下,堆积在耐火物中的氯化铁吸收大气中的水分而膨胀。其结果,耐火物本身的体积增加而膨胀,因此炉壁、炉床的耐火物向炉内侧溢出,或在耐火物产生龟裂而发生破裂。因此,存在耐火物的寿命短,更新周期短的问题。
本发明人等对这样的由氯化铁引起的耐火物的变质、脆化进行了反复深入的研究。其结果发现通过将耐火物的气孔率设为25体积%以下,能够抑制耐火物的变质、脆化。
堆积在耐火物中的氯化铁(固体)越是耐火物中的气孔增多越容易堆积到耐火物中。堆积在耐火物中的氯化铁因与大气接触而膨胀,从内侧向耐火物赋予压力,因此成为使耐火物劣化的原因。由此,优选耐火物中的气孔少,通过使气孔率为25体积%以下,能够抑制氯化铁在耐火物中的堆积,能够防止耐火物的劣化。因此,本发明中,通过将气孔率设为25体积%以下,能够抑制耐火物的变质、脆化。其结果,能够实现高硅钢板的连续生产线上的长期稳定作业。
另外,准备各种成分组成一定但压缩强度不同的耐火物。将这些耐火物置于含有氯化铁气体的气氛(FeCl2浓度:约15vol%,炉内温度:约1200℃)的炉内1周时间后,暴露于大气中2个月时间,其后检测膨胀状态的变化。其结果发行压缩强度与由氯化铁导致的膨胀状态之间存在紧密的关系,如果压缩强度小于5MPa则膨胀状态增加,发生破裂。因此,本发明中,将耐火物的压缩强度设为5MPa以上。压缩强度小于5MPa时,作为副产物的氯化铁气体渗透到耐火物中导致耐火物膨胀,耐火物破裂,对表面外观带来影响。优选压缩强度为20~200MPa。应予说明,压缩强度优选为200MPa以下。
另外,本发明中,气孔率和压缩强度的测定方法没有特别限制,根据常规方法求得即可。另外,也可以使用气孔率为25体积%以下、压缩强度为5MPa以上的耐火物。
实施例1
制作具有各种成分组成的耐火物(50mm×50mm×50mm),将这些设置在图1所示的高硅钢板的连续生产线的渗硅处理炉内。将渗硅处理炉的气氛设为SiCl4浓度:15vol%、炉内温度:1200℃连续运转3个月时间后,对各耐火物的损伤状况进行检测。将各耐火物的成分组成、气孔率、压缩强度和损伤状况的结果示于表1。
作为损伤状况,根据表面观察和反应性进行判断。表面观察是通过观察耐火物的外观,根据劣化状况以存在缺损>存在龟裂>变色>无变化这四个阶段进行评价。另外,关于反应性,根据劣化状况以◎◎、◎、○、×这4个阶段(◎◎:不反应,◎:几乎不反应,○:反应少(虽然观察到耐火物劣化,但可继续使用的等级),×:反应显著)进行评价。表面观察中,将无变色、变化作为合格,反应性中将◎◎、◎和○作为合格。
根据表1的结果,本发明例均为良好的结果。
实施例2
对于实施例1中显示良好的结果的No.10、19、31,对用作渗硅处理炉的耐火物时的更新周期进行了检测。其结果是,在使用No.10、19的情况下,将现有的耐火物(专利文献3的耐火物)的更新周期设为1时,更新周期能够延长到1.5倍。另外,使用No.31时,能够将更新周期延长到现有的耐火物的3倍。
Claims (3)
1.一种渗硅处理炉用耐火物,含有合计35质量%以上的选自硅的氧化物、硅的氮化物和硅的氧氮化物中的1种或2种以上,和合计0.05质量%以下的碱金属,
并且,气孔率为25体积%以下,压缩强度为5MPa以上。
2.根据权利要求1所述的渗硅处理炉用耐火物,其中,还含有合计1.0质量%以下的Mg、Ca、Ti、Fe、Cr和Zr的各氧化物。
3.根据权利要求1或2所述的渗硅处理炉用耐火物,其中,含有合计90质量%以上的选自硅的氧化物、硅的氮化物和硅的氧氮化物中的1种或2种以上。
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