CN106747666A - 一种耐高温涂层的制备方法 - Google Patents

一种耐高温涂层的制备方法 Download PDF

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CN106747666A
CN106747666A CN201611179890.2A CN201611179890A CN106747666A CN 106747666 A CN106747666 A CN 106747666A CN 201611179890 A CN201611179890 A CN 201611179890A CN 106747666 A CN106747666 A CN 106747666A
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袁振洲
刘欣宇
何丽娟
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Century Goldray Semiconductor Co Ltd
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Abstract

本发明公开了一种耐高温涂层的制备方法，所述方法为：首先对基体进行预处理，然后采用碳化物、烧结助剂、粘接剂与溶剂配置悬浊液，将悬浊液均匀喷涂或刷涂于所述基体表面，最后将喷好或刷好涂层的基体进行预温与烧结处理，即可在基体上得到一层厚度均匀、结构致密的耐高温涂层。本发明提供的耐高温涂层，耐温度高达3500℃，可用于材料生产用装置或部件的高温涂层的制备。本发明工艺过程成本低、简单易操作，重复性好，直接在材料表面形成致密、无裂纹的涂层。

Description

一种耐高温涂层的制备方法
技术领域
本发明涉及晶体、半导体材料生产制备领域，具体涉及一种耐高温涂层的制备方法。
背景技术
第三代半导体的晶体生长需要很高的温度(＞2100℃)，并且物理气相传输(PVT)生长晶体过程中，升华的源粉体(硅、铝)有较高的反应活性，侵蚀传统的基体材料制备的各部件，使基体表面腐蚀，腐蚀掉的颗粒进入晶体中造成晶体缺陷，进而对半导体的性能和品质产生重大的影响。直接使用耐高温碳化物(如碳化物)部件，成本增加数十倍甚至上百倍，若能采用耐高温涂层抑制腐蚀的发生和减少腐蚀产物的形成，提高材料的质量，将节省大笔成本。
碳化物熔点高(最高达3880℃)，在还原气氛下能耐受包括王水在内酸、碱、盐几乎所有物质的侵蚀(仅HF+HNO3复合酸除外)，高温化学稳定性和耐腐蚀性远高，且与石墨等基体具有良好的化学相容性，因而，碳化物是性能优异的涂层材料。
发明内容
针对现有技术中存在的问题，本发明的目的在于提供一种耐高温涂层的制备方法，其工艺过程成本低、简单易操作，重复性好，直接在材料表面形成致密、无裂纹的涂层。
为实现上述目的，本发明采用以下技术方案：
一种耐高温涂层的制备方法，所述方法为：首先对基体进行预处理，然后采用碳化物、烧结助剂、粘接剂与溶剂配置悬浊液，将悬浊液均匀喷涂或刷涂于所述基体表面，最后将喷好或刷好涂层的基体进行预温与烧结处理，即可在基体上得到一层厚度均匀、结构致密的耐高温涂层。
进一步，所述预处理为用高纯酒精或丙酮对所述基体表面进行清洗若干次；所述基体的材料为石英、石墨、Al2O3、SiC或MgO；所述碳化物的粒度为1-20 μm。
进一步，采用碳化物、烧结助剂、粘接剂与溶剂配置悬浊液具体为：称量适量的碳化物粉、烧结助剂，其中烧结助剂占涂层用粉末的1～35wt.％；然后取适量的溶剂，采用球磨机在玛瑙球磨罐中球磨或用玛瑙研钵手动研磨2～24h；取出，加入粘接剂搅拌，其中粘接剂质量百分比为溶剂的1％～10％，并且粘接剂与试剂混合液与碳化物粉质量比为0.3～1.0；得到碳化物涂层的悬浊液，静置待用。
进一步，所述碳化物包括WC、ZrC、TiC、NbC、B4C、NiC、CrC、Al4C3中的一种或两种。
进一步，所述烧结助剂包括Ti、Zr、Ta、Nb、W中的一种或两种金属单质以及碳粉，金属单质与碳粉的摩尔比为1:1。
进一步，所述粘接剂为聚乙烯醇、聚乙烯醇缩醛类、聚乙烯吡咯烷酮、环氧树脂、酚醛树脂或石墨胶的任一种。
进一步，所述溶剂为去离子水、高纯度酒精其中的一种。
进一步，所述耐高温涂层的厚度为50um～500um。
进一步，所述预温的温度为100℃～400℃。
进一步，所述烧结温度为1600℃～2500℃，压强为8×104Pa～1×105Pa，保护气氛为氩气、氦气、氢气中的一种。
本发明具有以下有益技术效果：
本发明的工艺制备的耐高温涂层的粘连性较大，不至于脱落；烧结助剂有效降低TaC涂层的烧结温度，并能增加烧结产物的致密度，有效提高烧结产物的物理性能；TaC悬浊液有利于喷/刷涂较为轻薄的涂层，保证避免透气性的同时，有效减少了厚度过后造成的开裂问题。
综上，本发明的方法简单，能制备一种厚度致密、粘连性大、结构致密的TaC涂层，实现了涂层的不脱落、无裂纹，从而达到将基体有效隔离的目的。
具体实施方式
下面，结合实施例，对本发明进行更全面的说明。然而，本发明可以体现为多种不同形式，并不应理解为局限于这里叙述的示例性实施例。而是，提供这些实施例，从而使本发明全面和完整，并将本发明的范围完全地传达给本领域的普通技术人员。
本发明提供了一种耐高温涂层的制备方法，该方法为：首先对基体进行预处理，然后采用碳化物、烧结助剂、粘接剂与溶剂配置悬浊液，将悬浊液均匀喷涂或刷涂于基体表面，最后将喷好或刷好涂层的基体进行预温与烧结处理，即可在基体上得到一层厚度均匀、结构致密的耐高温涂层。
其中，预处理为用高纯酒精或丙酮对所述基体表面进行清洗若干次；基体的材料为石英、石墨、Al2O3、SiC或MgO；碳化物的粒度为1-20μm。
采用碳化物、烧结助剂、粘接剂与溶剂配置悬浊液具体为：称量适量的碳化物粉、烧结助剂，其中烧结助剂占涂层用粉末的1～35wt.％；然后取适量的溶剂，采用球磨机在玛瑙球磨罐中球磨或用玛瑙研钵手动研磨2～24h；取出，加入粘接剂搅拌，其中粘接剂质量百分比为溶剂的1％～10％，并且粘接剂与试剂混合液与碳化物粉质量比为0.3～1.0；得到碳化物涂层的悬浊液，静置待用。
碳化物包括WC、ZrC、TiC、NbC、B4C、NiC、CrC、Al4C3中的一种或两种。烧结助剂包括Ti、Zr、Ta、Nb、W中的一种或两种金属单质以及碳粉，金属单质与碳粉的摩尔比为1:1。粘接剂为聚乙烯醇、聚乙烯醇缩醛类、聚乙烯吡咯烷酮、环氧树脂、酚醛树脂或石墨胶的任一种。溶剂为去离子水、高纯度酒精其中的一种。耐高温涂层的厚度为50um～500um。预温的温度为100℃～400℃。烧结温度为1600℃～2500℃，压强为8×104Pa～1×105Pa，保护气氛为氩气、氦气、氢气中的一种。
实施例一：
1)选用石墨基体，并用高纯酒精进行清洗2次，避免表面污染物；
2)称量适量19.6g的WC粉、0.35g的Zr粉、0.05的C粉；量取20ml的去离子水，采用球磨机在玛瑙球磨罐中球磨2h。取出，加入0.2g聚乙烯醇搅拌；得到碳化物涂层的悬浊液，静置待用；
3)采用画刷，将WC涂层的悬浊液均匀地刷涂在石墨基体表面；
4)将有涂层的石墨基体，置于加热炉中，通保护气体氩气，预烧温度为200℃，时间0.5h；
5)将有涂层的石墨基体，置于加热炉中，通保护气体氩气，压强为9×104Pa，7h升至2300℃，保持2h；随炉缓冷到室温即可开炉使用。
实施例二：
1)选用石英基体，并用高纯酒精进行清洗3次，避免表面污染物；
2)称量适量16g的WC粉、3.75g的Ta粉、0.25g的C粉；量取10ml的去离子水，采用球磨机在玛瑙球磨罐中球磨20h。取出，加入1.6g聚乙烯吡咯烷酮搅拌，得到碳化物涂层的悬浊液，静置待用；
3)采用喷枪，将碳化物涂层的悬浊液均匀地刷涂在石墨基体表面；
4)将有涂层的石英基体，置于真空干燥炉中，抽真空，预烧温度为100℃，时间1h；
5)将有涂层的石英基体，置于加热炉中，通保护气体氢气，压强为8×104Pa，5h升至1600℃，保持4h；随炉缓冷到室温即可开炉使用。
本发明制备碳化物涂层经实例检验技术稳定，工艺简单，涂层性能好，能耗小，成本低，周期短，生产效率较高。
上面所述只是为了说明本发明，应该理解为本发明并不局限于以上实施例，符合本发明思想的各种变通形式均在本发明的保护范围之内。

Claims (10)

1.一种耐高温涂层的制备方法，其特征在于，所述方法为：首先对基体进行预处理，然后采用碳化物、烧结助剂、粘接剂与溶剂配置悬浊液，将悬浊液均匀喷涂或刷涂于所述基体表面，最后将喷好或刷好涂层的基体进行预温与烧结处理，即可在基体上得到一层厚度均匀、结构致密的耐高温涂层。
2.根据权利要求1所述的耐高温涂层的制备方法，其特征在于，所述预处理为用高纯酒精或丙酮对所述基体表面进行清洗若干次；所述基体的材料为石英、石墨、Al2O3、SiC或MgO；所述碳化物的粒度为1-20μm。
3.根据权利要求1所述的耐高温涂层的制备方法，其特征在于，采用碳化物、烧结助剂、粘接剂与溶剂配置悬浊液具体为：称量适量的碳化物粉、烧结助剂，其中烧结助剂占涂层用粉末的1～35wt.％；然后取适量的溶剂，采用球磨机在玛瑙球磨罐中球磨或用玛瑙研钵手动研磨2～24h；取出，加入粘接剂搅拌，其中粘接剂质量百分比为溶剂的1％～10％，并且粘接剂与试剂混合液与碳化物粉质量比为0.3～1.0；得到碳化物涂层的悬浊液，静置待用。
4.根据权利要求1所述的耐高温涂层的制备方法，其特征在于，所述碳化物包括WC、ZrC、TiC、NbC、B4C、NiC、CrC、Al4C3中的一种或两种。
5.根据权利要求1所述的耐高温涂层的制备方法，其特征在于，所述烧结助剂包括Ti、Zr、Ta、Nb、W中的一种或两种金属单质以及碳粉，金属单质与碳粉的摩尔比为1:1。
6.根据权利要求1所述的耐高温涂层的制备方法，其特征在于，所述粘接剂为聚乙烯醇、聚乙烯醇缩醛类、聚乙烯吡咯烷酮、环氧树脂、酚醛树脂或石墨胶的任一种。
7.根据权利要求1所述的耐高温涂层的制备方法，其特征在于，所述溶剂为去离子水、高纯度酒精其中的一种。
8.根据权利要求1所述的耐高温涂层的制备方法，其特征在于，所述耐高温涂层的厚度为50um～500um。
9.根据权利要求1所述的耐高温涂层的制备方法，其特征在于，所述预温的温度为100℃～400℃。
10.根据权利要求1所述的耐高温涂层的制备方法，其特征在于，所述烧结温度为1600℃～2500℃，压强为8×104Pa～1×105Pa，保护气氛为氩气、氦气、氢气中的一种。
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