CN106083056A - 无压烧结制备碳化硅/二硅化钼复合陶瓷的方法 - Google Patents

无压烧结制备碳化硅/二硅化钼复合陶瓷的方法 Download PDF

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CN106083056A
CN106083056A CN201610406720.7A CN201610406720A CN106083056A CN 106083056 A CN106083056 A CN 106083056A CN 201610406720 A CN201610406720 A CN 201610406720A CN 106083056 A CN106083056 A CN 106083056A
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郭兴忠
杨辉
郑浦
高黎华
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Zhejiang Xinxin Mstar Technology Ltd
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Abstract

本发明公开了一种无压烧结制备碳化硅/二硅化钼复合陶瓷的方法，包括以下步骤：A、配制主原料：主原料由以下重量含量的成分组成：75％～85％的SiC、5％～15％的二硅化钼、10％的钇铝石榴石；B、将主原料均匀混合后，加入作为粘结剂的聚乙烯醇和作为分散剂的四甲基氢氧化铵，机械球磨制备成碳化硅复合粉体；聚乙烯醇占主原料总重的3.0％，四甲基氢氧化铵占主原料总重的2.0％；C、将造粒粉置于模具中采用干压一次成型，获得碳化硅坯体；D、将上述碳化硅坯体进行无压液相烧结，温度为1850℃～1950℃，保温4～6小时；得到碳化硅/二硅化钼复合陶瓷。

Description

无压烧结制备碳化硅/二硅化钼复合陶瓷的方法
技术领域
本发明涉及一种碳化硅/二硅化钼复合陶瓷的制造方法。
背景技术
碳化硅(SiC)陶瓷是一种典型的共价键结合的陶瓷材料，具有高温强度大、高温蠕变小、硬度高，耐磨、耐腐蚀、抗氧化、高热导率和高电导率以及热稳定性好，在机械、化工、能源、军工等高技术领域得到了大量的应用。例如，可用作高温、耐磨、耐腐蚀机械密封部件，各种砂轮和模具。但与一些氧化物结构陶瓷相比，碳化硅陶瓷的抗氧化性能不佳，在高温下表面会氧化形成二氧化硅薄膜，并可能析出方石英晶体，晶型转变导致薄膜开裂，使氧化速度加剧，对碳化硅陶瓷力学性能和使用性能产生很大的影响。
通过添加一些抗氧化性能优越的陶瓷材料，改善碳化硅陶瓷的抗氧化性能。二硅化钼是一种抗氧化性优越的结构陶瓷，广泛应用于高温抗氧化涂层材料、电加热元件、集成电极薄膜、结构材料、复合材料的增强剂、耐磨材料、结构陶瓷的连接材料等领域。将二硅化钼与碳化硅陶瓷进行复合，有望进一步改善碳化硅陶瓷的抗氧化性能。
已有碳化硅与二硅化钼的相关专利文献的报道。公开号CN105198480A公开了一种二硅化钼/碳化硅复合多孔陶瓷的制备方法。该方法使用Mo、Si、C、SiC及B元素粉模压成型，通过调整真空度并熔渗Si进行烧结，获得MoSi2/SiC复合多孔陶瓷，所得材料孔隙率稳定保持在50％或以上。该方法主要目的是制备更高使用温度和抗氧化性能环境下使用的多孔陶瓷品种。湖南大学高朋召课题组研究了梯度功能化MoSi2-RSiC复相陶瓷的制备及性能研究MoSi2-RSiC复合陶瓷的制备研究，主要以重结晶SiC为骨架材料、MoSi2为抗氧化调控材料，通过直接添加法或高温熔渗复合工艺制备高温抗氧化和力学性能优异、电热性能可调控的梯度功能化MoSi2-RSiC复相陶瓷。也有相关文献报道了采用碳化硅颗粒增强二硅化钼陶瓷的研究。上述研究并没有从碳化硅陶瓷自身抗氧化性的角度出发进行研究。
发明内容
本发明要解决的技术问题是提供一种无压烧结制备碳化硅/二硅化钼复合陶瓷的方法，采用本发明方法的所得材料不仅具有优越的抗氧化性，而且还具有良好的电热性能和力学性能，拓展了碳化硅陶瓷的应用领域。
为了解决上述技术问题，本发明提供一种无压烧结制备碳化硅/二硅化钼复合陶瓷的方法，包括以下步骤：
A、配制主原料：
主原料由以下重量含量的成分组成：75％～85％的SiC、5％～15％的二硅化钼、10％的钇铝石榴石；
B、将主原料均匀混合后，加入作为粘结剂的聚乙烯醇和作为分散剂的四甲基氢氧化铵，机械球磨制备成碳化硅复合粉体(能100目的筛)；
聚乙烯醇占主原料总重的3.0％，四甲基氢氧化铵占主原料总重的2.0％；
C、将造粒粉置于模具中采用干压一次成型，获得碳化硅坯体；
D、将上述碳化硅坯体进行无压液相烧结，温度为1850℃～1950℃，保温4～6小时；得到碳化硅/二硅化钼复合陶瓷。
作为本发明的无压烧结制备碳化硅/二硅化钼复合陶瓷的方法的改进：
所述步骤C的干压一次成型的压力为50～60Mpa。
本发明在碳化硅颗粒中加入抗氧化性优越、电热性好的二硅化钼，从而改善了碳化硅陶瓷的抗氧化性。本发明在优化配方的基础上采用无压液相烧结制得所需的材料。该方法制作的陶瓷既能保证力学性能又具有良好的抗氧化性能。
综上所述，本发明将碳化硅陶瓷高强耐磨、高温力学性能、抗蠕变等特性与二硅化钼高抗氧化性、高导热、高导电性能相结合，从而制备出优越力学性能和抗氧化性能的复合陶瓷，拓展其在高温热源结构领域的应用。
具体实施方式
下面结合具体实施例对本发明进行进一步描述，但本发明的保护范围并不仅限于此。
下述份均指重量份。
实施例1、一种无压烧结制备碳化硅/二硅化钼复合陶瓷的方法，依次进行以下步骤：
A、配制主原料：
将75份碳化硅粉末、15份二硅化钼、10份钇铝石榴石混合作为主原料；
B、将主原料均匀混合后，加入3份作为粘结剂的聚乙烯醇和2份作为分散剂的四甲基氢氧化铵，机械球磨制备成碳化硅复合粉体(能100目的筛)；
即，聚乙烯醇占主原料总重的3.0％，四甲基氢氧化铵占主原料总重的2.0％；
C、将造粒粉置于模具中采用干压一次成型(压力为50～60Mpa)，获得碳化硅坯体；
D、将上述碳化硅坯体进行无压液相烧结，温度为1900℃～1950℃，保温6小时；得到抗氧化性良好的碳化硅/二硅化钼复合陶瓷。
该碳化硅/二硅化钼复合陶瓷的体积密度3.3～3.4g/cm3，抗压强度大于1200MPa，抗折强度大于300MPa，弹性模量300GPa以上，抗氧化性在1600℃以上。
实施例2、一种无压烧结制备碳化硅/二硅化钼复合陶瓷的方法
将80份碳化硅粉末、10份二硅化钼、10份钇铝石榴石混合作为主原料，其余等同于实施例1。得到抗氧化性良好的碳化硅/二硅化钼复合陶瓷。
该碳化硅/二硅化钼复合陶瓷的体积密度3.2～3.3g/cm3，抗压强度大于1400MPa，抗折强度大于350MPa，弹性模量350GPa以上，抗氧化性在1570℃以上。
实施例3、一种无压烧结制备碳化硅/二硅化钼复合陶瓷的方法
将85份碳化硅粉末、5份二硅化钼、10份钇铝石榴石混合作为主原料，其余等同于实施例1。得到抗氧化性良好的碳化硅/二硅化钼复合陶瓷。
该碳化硅/二硅化钼复合陶瓷的体积密度3.1～3.2g/cm3，抗压强度大于1600MPa，抗折强度大于400MPa，弹性模量400GPa以上，抗氧化性在1500℃以上。
最后，还需要注意的是，以上列举的仅是本发明的若干个具体实施例。显然，本发明不限于以上实施例，还可以有许多变形。本领域的普通技术人员能从本发明公开的内容直接导出或联想到的所有变形，均应认为是本发明的保护范围。

Claims (2)

1.无压烧结制备碳化硅/二硅化钼复合陶瓷的方法，其特征是包括以下步骤：
A、配制主原料：
主原料由以下重量含量的成分组成：75％～85％的SiC、5％～15％的二硅化钼、10％的钇铝石榴石；
B、将主原料均匀混合后，加入作为粘结剂的聚乙烯醇和作为分散剂的四甲基氢氧化铵，机械球磨制备成碳化硅复合粉体；
聚乙烯醇占主原料总重的3.0％，四甲基氢氧化铵占主原料总重的2.0％；
C、将造粒粉置于模具中采用干压一次成型，获得碳化硅坯体；
D、将上述碳化硅坯体进行无压液相烧结，温度为1850℃～1950℃，保温4～6小时；得到碳化硅/二硅化钼复合陶瓷。
2.根据权利要求1所述无压烧结制备碳化硅/二硅化钼复合陶瓷的方法，其特征是：
所述步骤C的干压一次成型的压力为50～60Mpa。
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CN107253862A (zh) * 2017-07-18 2017-10-17 深圳市千禾盛科技有限公司 一种玻璃热弯成型模具用陶瓷及其制备方法
CN107500771A (zh) * 2017-07-10 2017-12-22 深圳市千禾盛科技有限公司 玻璃热弯成型模具用陶瓷及其制备方法
CN108358643A (zh) * 2018-03-29 2018-08-03 中国科学院上海硅酸盐研究所 一种红外光源材料及其制备方法
CN109288140A (zh) * 2018-12-06 2019-02-01 广东国研新材料有限公司 一种电子烟用多孔陶瓷发热体及其制备方法
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CN107500771A (zh) * 2017-07-10 2017-12-22 深圳市千禾盛科技有限公司 玻璃热弯成型模具用陶瓷及其制备方法
CN107253862A (zh) * 2017-07-18 2017-10-17 深圳市千禾盛科技有限公司 一种玻璃热弯成型模具用陶瓷及其制备方法
CN108358643A (zh) * 2018-03-29 2018-08-03 中国科学院上海硅酸盐研究所 一种红外光源材料及其制备方法
CN108358643B (zh) * 2018-03-29 2020-12-11 中国科学院上海硅酸盐研究所 一种红外光源材料及其制备方法
CN109288140A (zh) * 2018-12-06 2019-02-01 广东国研新材料有限公司 一种电子烟用多孔陶瓷发热体及其制备方法
CN109288140B (zh) * 2018-12-06 2021-08-27 广东国研新材料有限公司 一种电子烟用多孔陶瓷发热体及其制备方法
CN111848172A (zh) * 2020-07-24 2020-10-30 厦门大学 二硅化钼/碳化硅三维聚合物先驱体陶瓷及其制备方法
CN111848172B (zh) * 2020-07-24 2021-09-28 厦门大学 二硅化钼/碳化硅三维聚合物先驱体陶瓷及其制备方法

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