CN105461308A - 一种用可塑法制备再结晶碳化硅制品的方法 - Google Patents

一种用可塑法制备再结晶碳化硅制品的方法 Download PDF

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CN105461308A
CN105461308A CN201610018879.1A CN201610018879A CN105461308A CN 105461308 A CN105461308 A CN 105461308A CN 201610018879 A CN201610018879 A CN 201610018879A CN 105461308 A CN105461308 A CN 105461308A
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肖汉宁
刘寒
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Abstract

本发明公开了一种用可塑法制备再结晶碳化硅制品的方法，其原料由质量份数为60~70份碳化硅粗粉、30~40份碳化硅细粉、1~3份增塑剂和1~3份润滑剂组成，碳化硅粗粉的粒径为20~150微米；碳化硅细粉的粒径为0.2~2微米；该方法包括以下步骤：将碳化硅粗粉用球磨整形得整形碳化硅粗粉；将碳化硅细粉用聚乙二胺溶液进行包覆处理得改性碳化硅细粉；将改性碳化硅细粉与增塑剂混匀，加入整形碳化硅粗粉、水和润滑剂，捏炼成可塑碳化硅泥料；将可塑碳化硅泥料挤制得湿坯，再干燥得生坯；将生坯烧结，出炉得再结晶碳化硅制品。该再结晶碳化硅制品的体积密度为2.5~2.65g/cm3，室温抗弯强度为80~110MPa；与注浆法比，生产效率高、周期短、成本低、产品的均匀性好和可靠性高。

Description

一种用可塑法制备再结晶碳化硅制品的方法
技术领域
本发明涉及一种用可塑法制备再结晶碳化硅制品的方法，属于碳化硅材料技术领域。
背景技术
再结晶碳化硅制品因其高温强度高、抗氧化和耐腐蚀性好、在使用过程中不变形等优点而成为重要的高温结构材料，在新材料、电子技术、航天航空、化工、冶金等领域获得越来越广泛的应用。
与其他陶瓷在烧结过程中产生收缩而致密化的机理不同，再结晶碳化硅的烧结机理是蒸发—凝聚，在烧结过程中没有收缩，因而最终制品的密度取决于烧结前生坯的颗粒堆积密度。为了最大限度地获得高的生坯密度，前人已对碳化硅原料的颗粒级配进行了大量研究，如通过合理的粗细颗粒配比和粒径分布来增加颗粒间的填充密度。此外，采用注浆工艺成型再结晶碳化硅制品也是提高生坯密度的重要手段，因碳化硅颗粒在浆料中可通过流动调整角度，从而获得最大的堆积密度。因此，目前再结晶碳化硅制品的成型主要采用注浆工艺。但注浆工艺的生产效率低，占用场地大，生产周期长，导致生产规模受限，制备成本高，也影响到再结晶碳化硅制品的进一步推广应用。
发明内容
本发明要解决的技术问题是，针对现有再结晶碳化硅制品注浆工艺生产效率低、周期长、成本高等不足，开发出一种用可塑法真空挤制工艺高效率制备再结晶碳化硅制品的方法，并解决碳化硅原料同时具有良好可塑性和高的颗粒堆积密度等技术难题。
本发明的技术方案是，提供一种用可塑法制备再结晶碳化硅制品的方法，其原料由质量份数为60~70份碳化硅粗粉、30~40份碳化硅细粉、1~3份增塑剂和1~3份润滑剂组成，所述碳化硅粗粉的粒径为20~150微米；所述碳化硅细粉的粒径为0.2~2微米；该方法包括以下步骤：
（1）将碳化硅粗粉用球磨进行整形处理，去除颗粒的尖角和棱角，过筛后得整形碳化硅粗粉；将碳化硅细粉用浓度为2~15%的聚乙二胺溶液进行包覆处理，得改性碳化硅细粉；
（2）将改性碳化硅细粉与增塑剂混合均匀，然后加入整形碳化硅粗粉，混合均匀后，再加入水和润滑剂，在捏炼机中捏炼成含水量为8~15%的可塑碳化硅泥料；
（3）将可塑碳化硅泥料在真空挤出机中挤制为所需形状的湿坯，经干燥后得生坯；
（4）将生坯在保护气体下烧结，出炉后得再结晶碳化硅制品。
进一步地，所述增塑剂为羧甲基纤维素、羟丙基甲基纤维素和聚乙烯醇中的一种或多种。
进一步地，所述保护气体为氩气。
进一步地，所述润滑剂为桐油和改性植物油的一种或多种。
进一步地，所述步骤（4）中，将生坯在真空电阻炉或感应加热炉中烧结，烧结的温度为2100~2400℃。
进一步地，所述步骤（3）中，所述干燥为微波干燥。
以下对本发明做出进一步说明。
本发明首先对粒径为20~150微米的碳化硅粗粉进行整形处理，去除颗粒的尖角和棱角，得到近球形的颗粒；然后对粒径为0.2~2微米的碳化硅细粉用一定浓度的聚乙二胺溶液进行包覆处理，其作用是通过聚乙二胺的空间位阻作用提高细粉的可分散性和流动性，从而使碳化硅细粉能更好地填充到碳化硅粗粉的间隙中，同时降低形成可塑泥料时的需水量。此外，还对形成碳化硅可塑泥料的增塑剂和润滑剂进行了科学选择和配比优化。
本发明的技术贡献是：（1）将碳化硅粗粉进行整形处理，去除颗粒的尖角和棱角，有效降低了挤出时的摩擦阻力，减少了对模具的磨损，同时也有利于提高泥料的固相含量。（2）将碳化硅细粉用一定浓度的聚乙二胺溶液进行包覆处理，其作用是通过聚乙二胺的空间位阻作用提高细粉的可分散性和流动性，从而使碳化硅细粉能更好地填充到碳化硅粗粉的间隙中，同时降低可塑碳化硅泥料的含水量。（3）加入润滑剂有效降低了碳化硅颗粒之间的摩擦系数，减少了挤出阻力，并通过真空挤出时推力的作用实现颗粒间的紧密堆积，有利于提高生坯密度和强度。（4）将可塑法真空挤出与微波干燥技术相结合，大幅提高了再结晶碳化硅制品的成型效率，缩短了干燥时间，并有效减少了制品的干燥变形和开裂。
本发明的有益效果是，用本发明制备的再结晶碳化硅制品与用注浆法制备的再结晶碳化硅制品相比，具有以下优势：（1）成型及干燥时间由注浆法的3天以上缩短到1小时左右，大幅提高了生产效率，降低了生产成本；（2）制品的规整度好，生坯强度高；（3）材料的组成和结构均匀，制品的可靠性好。
具体实施方式
实施例1：本实施例提供一种用可塑法制备再结晶碳化硅制品的方法，其原料由质量份数为68份碳化硅粗粉、32份碳化硅细粉、1.5份增塑剂和1.5份润滑剂组成，具体工艺步骤为：
（1）将碳化硅粗粉用球磨6小时进行整形处理，去除颗粒的尖角和棱角，过200目筛后取筛上物为整形碳化硅粗粉；将碳化硅细粉用浓度为5%的聚乙二胺溶液进行包覆处理，得改性碳化硅细粉；
（2）将改性碳化硅细粉与增塑剂混合均匀，然后加入整形碳化硅粗粉，混合均匀后，再缓慢加入水和润滑剂，在捏炼机中捏炼成含水量8%的可塑碳化硅泥料；
（3）将可塑碳化硅泥料在真空挤出机中挤制（挤出压力6MPa，真空度大于95%）为所需形状的湿坯，经微波干燥18分钟后得生坯；
（4）将生坯在真空电阻炉中于2300℃烧结3.5小时，用氩气作为保护气体，出炉后得再结晶碳化硅制品。
所述碳化硅粗粉的平均粒径为80微米；所述碳化硅细粉的平均粒径为0.5微米；所述增塑剂为1份羟丙基甲基纤维素和0.5份聚乙烯醇的混合物；所述润滑剂为桐油。
用上述方案制备的再结晶碳化硅制品的体积密度在2.55g/cm3，抗弯强度达到90MPa。
实施例2：本实施例提供一种用可塑法制备再结晶碳化硅制品的方法，其原料由质量份数为65份碳化硅粗粉、35份碳化硅细粉、2份增塑剂和2份润滑剂组成，具体工艺步骤为：
（1）将碳化硅粗粉球磨5小时进行整形处理，去除颗粒的尖角和棱角，过150目筛后取筛上物为整形碳化硅粗粉；将碳化硅细粉用浓度为10%的聚乙二胺溶液进行包覆处理，得改性碳化硅细粉；
（2）将改性碳化硅细粉与增塑剂混合均匀，然后加入整形碳化硅粗粉，混合均匀后，再缓慢加入水和润滑剂，在捏炼机中捏炼成含水量10%的可塑碳化硅泥料；
（3）将可塑碳化硅泥料在真空挤出机中挤制（挤出压力5MPa，真空度大于95%）为所需形状的湿坯，经微波干燥15分钟后得生坯；
（4）将生坯在真空电阻炉中于2350℃烧结3小时，用氩气作为保护气体，出炉后得再结晶碳化硅制品。所述碳化硅粗粉的平均粒径为100微米；所述碳化硅细粉的平均粒径为1微米；所述增塑剂为1.5份羟丙基甲基纤维素和0.5份聚乙烯醇的混合物；所述润滑剂为改性植物油。
用上述方案制备的再结晶碳化硅制品的体积密度为2.6g/cm3，抗弯强度达到100MPa。
实施例3：本实施例提供一种用可塑法制备再结晶碳化硅制品的方法，其原料由质量份数为62份碳化硅粗粉、38份碳化硅细粉、2.5份增塑剂和1份润滑剂组成，具体工艺步骤为：
（1）将碳化硅粗粉用球磨4小时进行整形处理，去除颗粒的尖角和棱角，过250目筛后取筛上物为整形碳化硅粗粉；将碳化硅细粉用浓度为15%的聚乙二胺溶液进行包覆处理，得改性碳化硅细粉；
（2）将改性碳化硅细粉与增塑剂混合均匀，然后加入整形碳化硅粗粉，混合均匀后，再缓慢加入水和润滑剂，在捏炼机中捏炼成含水量12%的可塑碳化硅泥料；
（3）将可塑碳化硅泥料在真空挤出机中挤制（挤出压力7MPa，真空度大于95%）为所需形状管状的湿坯，经微波干燥20min后得生坯；
（4）将生坯在真空电阻炉中于2300℃烧结2.5小时，用氩气作为保护气体，出炉后得再结晶碳化硅制品。
所述碳化硅粗粉的平均粒径为60微米；所述碳化硅细粉的平均粒径为0.48微米；所述增塑剂为2份羟丙基甲基纤维素和0.5份聚乙烯醇的混合物；所述润滑剂为桐油。
用上述方案制备的再结晶碳化硅制品的体积密度为2.5g/cm3，抗弯强度80MPa。

Claims (6)

1.一种用可塑法制备再结晶碳化硅制品的方法，其特征在于，其原料由质量份数为60~70份碳化硅粗粉、30~40份碳化硅细粉、1~3份增塑剂和1~3份润滑剂组成，所述碳化硅粗粉的粒径为20~150微米；所述碳化硅细粉的粒径为0.2~2微米；该方法包括以下步骤：
（1）将碳化硅粗粉用球磨进行整形处理，去除颗粒的尖角和棱角，过筛后得整形碳化硅粗粉；将碳化硅细粉用浓度为2~15%的聚乙二胺溶液进行包覆处理，得改性碳化硅细粉；
（2）将改性碳化硅细粉与增塑剂混合均匀，然后加入整形碳化硅粗粉，混合均匀后，再加入水和润滑剂，在捏炼机中捏炼成含水量为8~15%的可塑碳化硅泥料；
（3）将可塑碳化硅泥料在真空挤出机中挤制为所需形状的湿坯，经干燥后得生坯；
（4）将生坯在保护气体下烧结，出炉后得再结晶碳化硅制品。
2.如权利要求1所述的方法，其特征在于，所述增塑剂为羧甲基纤维素、羟丙基甲基纤维素和聚乙烯醇中的一种或多种。
3.如权利要求1所述的方法，其特征在于，所述保护气体为氩气。
4.如权利要求1所述的方法，其特征在于，所述润滑剂为桐油和改性植物油的一种或多种。
5.如权利要求1所述的方法，其特征在于，所述步骤（4）中，将生坯在真空电阻炉或感应加热炉中烧结，烧结的温度为2100~2400℃。
6.如权利要求1所述的方法，其特征在于，所述步骤（3）中，所述干燥为微波干燥。
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CN110655406A (zh) * 2019-09-30 2020-01-07 山东金鸿新材料股份有限公司 一种反应烧结碳化硅热交换器管及其制备方法
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CN115340385A (zh) * 2022-08-30 2022-11-15 武汉工程大学 一种孔径可控的微米孔径碳化硅多孔陶瓷及其制备方法

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