CN108439991A - 一种应用于超高温感应加热的发热材料及其制备方法 - Google Patents
一种应用于超高温感应加热的发热材料及其制备方法 Download PDFInfo
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Abstract
本发明涉及一种应用于超高温感应加热的发热材料及其制备方法，属于发热材料领域。本发明的发热材料，各组分质量百分比为：二硅化钼粉20～85％；二硼化锆粉5～70％；碳化硅粉2～20％；粘结剂1～10％；增塑剂1～10％；润滑剂1～10％；水5～20％。本发明发热材料的制备方法为，将二硅化钼粉、二硼化锆粉、碳化硅粉和粘结剂加入球磨机中，与无水乙醇共混；将共混后的泥浆经干燥得到粉料过筛；增塑剂和润滑剂与水混合后加入过筛后的粉料中，再用练泥机练泥成泥料；泥料经陈腐后采用真空挤出工艺成型；挤出成型的生坯经干燥、脱脂处理后，在1600～1900℃条件下烧结1～3小时，得到目标产品。本发明制得的超高温感应发热材料在氧化性气氛中的最高使用温度可高达1800～1900℃。
Description
技术领域
本发明涉及一种应用于超高温感应加热的发热材料及其制备方法，属于发热材料领域。
背景技术
感应炉是利用物料的感应电热效应而使物料加热或熔化的电炉，包括感应熔炼炉和感应加热炉。感应熔炼炉主要用于物料(一般为金属)的熔炼，感应加热炉主要用于物料的加热，包括物料的整体均匀加热、表面加热或局部加热等。感应炉具有加热速度快、电热效率高、氧化脱炭少、加热均匀、无污染、占地面积小、低能耗和温控精度高等传统加热设备不可比拟的优点，被广泛应用于炼钢、铸铁生产、机械零件加工、粉末冶金等领域。
目前在感应加热设备中应用较多的发热材料主要有贵金属、金属合金和石墨，理论上石墨的发热温度可高达3000℃左右，然而众所周知，石墨在高温下极易被氧化，从而制约其在超高温氧化性环境中的应用，贵金属和金属合金材料由于发热温度较低、成本较高、耐腐蚀性差等缺点而不能被普遍应用于发热材料领域中，因此研制一种低成本且在氧化性环境中能长期循环使用的感应发热材料是将感应加热设备普遍应用的关键。
陶瓷及陶瓷基复合材料具有熔点高、抗热震性好、生产成本低、耐腐蚀性和抗氧化性优异等特点，近年来受到了本领域研究人员的普遍关注，其中MoSi2陶瓷材料由于具有升温速率快、发热量大、电导率稳定、热膨胀系数低、高温下表面生成致密的保护膜而具有优异的高温抗氧化性等特点，被广泛应用于电加热设备的发热材料中，是目前高温加热领域中最具发展前景的陶瓷发热材料之一，然而当其在超高温(>1800℃)氧化性环境中使用时，由于表面氧化膜的破裂、脱落和快速分解导致其使用寿命大大缩短，且MoSi2陶瓷材料还存在高温环境(1350℃以上)强度低、中温环境(1000℃以下)韧性差、低温环境(400-600℃)氧化快等缺点。当前国内外材料科学工作者开展了大量改善MoSi2陶瓷材料力学性能的研究工作，并取得了令人满意的结果，大大扩展了MoSi2陶瓷材料在高温结构材料领域的应用空间。但若将其应用于超高温发热材料领域，优异的超高温抗氧化性无疑是其最为重要的性能之一，以牺牲其高温抗氧化性而换来力学性能的改善不能满足其在超高温极端环境中的使用要求。因此，在当前改善MoSi2陶瓷材料力学性能的研究基础上提高其在超高温环境中的抗氧化性是提高MoSi2陶瓷材料使用温度与使用寿命的关键，对扩展MoSi2陶瓷材料在高温加热材料领域的应用空间具有重要意义。
发明内容
本发明的目的是为了解决目前感应加热设备中发热材料在超高温氧化性环境中使用受到限制的问题，而提供一种在超高温氧化性环境中能长期循环使用的感应发热材料。
本发明的目的是通过以下技术方案实现的：
本发明的一种应用于超高温感应加热的发热材料，该材料配方中各组分的质量百分比如下：
所述的粘结剂为：环氧树脂、甲基纤维素、羟甲基纤维素、羟丙基纤维素、羟甲基丙基纤维素、木质素磺酸钠、聚乙烯醇、明胶、硅酸乙酯、大米淀粉、高岭土、膨润土中的一种；
所述增塑剂为：氧化钙、氧化镁、氧化钾、氧化钠、邻苯二甲酸二甲酯、脂肪醇二元酸酯、甲基纤维素、聚乙二醇、木质磺酸钠、木质磺酸钾、微生物多糖中的一种；
所述润滑剂为：硬脂酸乙二酯、双硬脂酸乙二醇酯、甘油、矿物油、石蜡、液体石蜡、乳化石蜡、聚乙烯蜡、氧化聚乙烯蜡、硬脂酸锌、油酸、聚四氟乙烯、硬脂酰胺中的一种。
本发明的一种应用于超高温感应加热的发热材料的制备方法，具体制备步骤如下：
1)按配方总质量100份计算，将20～85份的二硅化钼粉、5～70份的二硼化锆粉、2～20份的碳化硅粉和1～10份的粘结剂加入球磨机中，按料/球质量比为1：(1～4)、200～600rpm转速下与无水乙醇共混1～10小时，得到混合均匀的泥浆；
2)将步骤1)得到的泥浆于20～100℃条件下干燥1～10小时，得到混合均匀的粉料，并过60～300目筛；
3)按配方总质量100份计算，将1～10份的增塑剂和1～10份的润滑剂同时加到5～20份的水中配制成型剂溶液；
4)将步骤3)配制好的成型剂溶液加入步骤2)过筛后的混合粉料中，用练泥机练泥1～8小时，练泥机的转速为10～40r/min；然后将练泥后的泥料放置在室温环境中陈腐12～48小时；再将陈腐后的泥料采用真空陶瓷挤出机挤出成型，真空陶瓷挤出机的真空度为-0.05～-0.1Mpa，挤出压力为15～25Mpa，挤出速度为1～3m/min；挤出成型的生坯于25～100℃环境中干燥12～48小时，得到发热材料半成品；
5)将步骤4)制得的发热材料半成品于200～600℃条件下脱脂处理，然后在真空烧结炉中1600～1900℃条件下烧结1～3小时，得到超高温感应的发热材料成品。
所述的粘结剂为：环氧树脂、甲基纤维素、羟甲基纤维素、羟丙基纤维素、羟甲基丙基纤维素、木质素磺酸钠、聚乙烯醇、明胶、硅酸乙酯、大米淀粉、高岭土、膨润土中的一种；
所述增塑剂为：氧化钙、氧化镁、氧化钾、氧化钠、邻苯二甲酸二甲酯、脂肪醇二元酸酯、甲基纤维素、聚乙二醇、木质磺酸钠、木质磺酸钾、微生物多糖中的一种；
所述润滑剂为：硬脂酸乙二酯、双硬脂酸乙二醇酯、甘油、矿物油、石蜡、液体石蜡、乳化石蜡、聚乙烯蜡、氧化聚乙烯蜡、硬脂酸锌、油酸、聚四氟乙烯、硬脂酰胺中的一种。
有益效果：
本发明提出的成型方法易操作、成本低、生产周期短，可通过简单的工艺过程批量制备能在氧化性环境中、1800℃以上的温度范围使用的感应发热材料。本发明所提出的感应发热材料体系由二硅化钼、二硼化锆和碳化硅三相组成，不但弥补了单一二硅化钼低温环境氧化快、中温环境韧性差和高温环境强度低的缺陷，而且在保持二硅化钼本身优异电学性能的同时提高了二硅化钼的超高温抗氧化性，所制备的感应发热材料在1800℃以上的氧化性环境中能长期循环使用，解决了当前感应加热设备在超高温氧化性环境中使用受到限制的问题。
具体实施方式
下面结合实施例对本发明的内容作进一步描述。
实施例1
一种应用于超高温感应加热的发热材料的制备方法，具体制备步骤如下：
1)将820g的二硅化钼粉、159g的二硼化锆粉、21g的碳化硅粉和25g的羟甲基丙基纤维素加入球磨机中，按料球质量比为1：3、于500rpm转速下与无水乙醇共混5小时，得到混合均匀的泥浆；
2)将步骤1)得到的泥浆于85℃条件下干燥2小时得到混合均匀的粉料并过60目筛；
3)将10g的聚乙二醇和25g的油酸同时加到130g的水中配制成型剂溶液；
4)将步骤3)配制好的成型剂溶液加入步骤2)过筛后的混合粉料中，采用练泥机练泥2小时，练泥机的转速为30r/min，然后将练泥后的泥料放置在室温环境中陈腐24小时，再将陈腐后的泥料采用真空陶瓷挤出机挤出成型，真空陶瓷挤出机的真空度为-0.095Mpa，挤出压力为20Mpa，挤出速度为1m/min；挤出成型的生坯于90℃环境中干燥24小时，得到发热材料半成品；
5)将步骤4)制得的发热材料半成品于600℃条件下脱脂处理，然后在真空烧结炉中1800℃条件下烧结1小时，得到超高温感应的发热材料成品。所制备的超高温感应的发热材料成品导电性良好，表面氧化膜连续且致密，弯曲强度是纯MoSi2发热材料弯曲强度的1.27倍，耐热温度为1900℃。
实施例2
一种应用于超高温感应加热的发热材料的制备方法，具体制备步骤如下：
1)将631g的二硅化钼粉、326g的二硼化锆粉、43g的碳化硅粉和50g的聚乙烯醇(PVA)加入球磨机中，按料球质量比为1：1、于400rpm转速下与无水乙醇共混3小时得到混合均匀的泥浆；
2)将步骤1)得到的泥浆于80℃条件下干燥1小时得到混合均匀的粉料并过60目筛；
3)将10g的邻苯二甲酸二甲酯和20g的甘油同时加到110g的水中配制成型剂溶液；
4)将步骤3)配制好的成型剂溶液加入步骤2)过筛后的混合粉料中，采用练泥机练泥2小时，练泥机的转速为15r/min，然后将泥料放置在室温环境中陈腐24小时，再将陈腐后的泥料采用真空陶瓷挤出机挤出成型，真空陶瓷挤出机的真空度为-0.09Mpa，挤出压力为15Mpa，挤出速度为2m/min；挤出成型的生坯于85℃环境中干燥24小时，得到发热材料半成品；
5)将步骤4)制得的发热材料半成品于400℃条件下脱脂处理，然后在真空烧结炉中1850℃条件下烧结1小时，得到超高温感应发热材料成品。所制备的超高温感应发热材料导电性良好，表面氧化膜中分布有少量氧化锆颗粒，弯曲强度与纯MoSi2发热材料的弯曲强度相当，耐热温度为1850℃。
实施例3
一种应用于超高温感应加热的发热材料的制备方法，具体制备步骤如下：
1)将432g的二硅化钼粉、502g的二硼化锆粉、66g的碳化硅粉和30g的甲基纤维素加入球磨机中，按料球质量比为1：2、于400rpm转速下与无水乙醇共混4小时得到混合均匀的泥浆；
2)将步骤1)得到的泥浆于85℃条件下干燥2小时得到混合均匀的粉料并过60目筛；
3)将15g的脂肪醇二元酸酯和25g的油酸同时加到150g的水中配制成型剂溶液；
4)将步骤3)配制好的成型剂溶液加入步骤2)过筛后的混合粉料中，采用练泥机练泥2小时，练泥机的转速为20r/min，然后将泥料放置在室温环境中陈腐24小时，再将陈腐后的泥料采用真空陶瓷挤出机挤出成型，真空陶瓷挤出机的真空度为-0.095Mpa，挤出压力为20Mpa，挤出速度为2m/min；挤出成型的生坯于90℃环境中干燥24小时，得到发热材料半成品；
5)将步骤4)制得的发热材料半成品于600℃条件下脱脂处理，然后在真空烧结炉中1900℃条件下烧结1小时，得到超高温感应发热材料成品。所制备的超高温感应发热材料导电性良好，表面氧化膜中分布有大量氧化锆颗粒，弯曲强度与纯MoSi2发热材料的弯曲强度相当，耐热温度为1800℃。
Claims (5)
1.一种应用于超高温感应加热的发热材料，其特征是：该材料配方中各组分的质量百分比如下：
所述的粘结剂为：环氧树脂、甲基纤维素、羟甲基纤维素、羟丙基纤维素、羟甲基丙基纤维素、木质素磺酸钠、聚乙烯醇、明胶、硅酸乙酯、大米淀粉、高岭土、膨润土中的一种；
所述增塑剂为：氧化钙、氧化镁、氧化钾、氧化钠、邻苯二甲酸二甲酯、脂肪醇二元酸酯、甲基纤维素、聚乙二醇、木质磺酸钠、木质磺酸钾、微生物多糖中的一种；
所述润滑剂为：硬脂酸乙二酯、双硬脂酸乙二醇酯、甘油、矿物油、石蜡、液体石蜡、乳化石蜡、聚乙烯蜡、氧化聚乙烯蜡、硬脂酸锌、油酸、聚四氟乙烯、硬脂酰胺中的一种。
2.一种应用于超高温感应加热的发热材料的制备方法，其特征是具体制备步骤如下：
1)按配方总质量100份计算，将20～85份的二硅化钼粉、5～70份的二硼化锆粉、2～20份的碳化硅粉和1～10份的粘结剂加入球磨机中，与无水乙醇共混1～10小时，得到混合均匀的泥浆；
2)将步骤1)得到的泥浆于20～100℃条件下干燥1～10小时，得到混合均匀的粉料，并过60～300目筛；
3)按配方总质量100份计算，将1～10份的增塑剂和1～10份的润滑剂同时加到5～20份的水中配制成型剂溶液；
4)将步骤3)配制好的成型剂溶液加入步骤2)过筛后的混合粉料中，用练泥机练泥成泥料；然后将练泥后的泥料放置在室温环境中陈腐12～48小时；再将陈腐后的泥料采用真空挤出工艺成型；挤出成型的生坯于25～100℃环境中干燥12～48小时，得到发热材料半成品；
5)将步骤4)制得的发热材料半成品于200～600℃条件下脱脂处理，然后在真空烧结炉中1600～1900℃条件下烧结1～3小时，得到超高温感应的发热材料成品；
所述的粘结剂为：环氧树脂、甲基纤维素、羟甲基纤维素、羟丙基纤维素、羟甲基丙基纤维素、木质素磺酸钠、聚乙烯醇、明胶、硅酸乙酯、大米淀粉、高岭土、膨润土中的一种；
所述增塑剂为：氧化钙、氧化镁、氧化钾、氧化钠、邻苯二甲酸二甲酯、脂肪醇二元酸酯、甲基纤维素、聚乙二醇、木质磺酸钠、木质磺酸钾、微生物多糖中的一种；
所述润滑剂为：硬脂酸乙二酯、双硬脂酸乙二醇酯、甘油、矿物油、石蜡、液体石蜡、乳化石蜡、聚乙烯蜡、氧化聚乙烯蜡、硬脂酸锌、油酸、聚四氟乙烯、硬脂酰胺中的一种。
3.如权利要求2所述的制备方法，其特征是：所述步骤1)中球磨时的料/球质量比为1：(1～4)；球磨时的转速为200～600。
4.如权利要求2所述的制备方法，其特征是：所述步骤4)中练泥工艺采用的转速为10～40r/min，练泥时间1～8小时。
5.如权利要求2所述的制备方法，其特征是：所述的真空挤出工艺采用真空陶瓷挤出机，真空陶瓷挤出机的真空度为-0.05～-0.1Mpa，挤出压力为15～25Mpa，挤出速度为1～3m/min。
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