CN109280873A - 一种气敏涂层材料及其制备方法 - Google Patents
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Abstract
本发明涉及一种气敏涂层材料及其制备方法，属于半导体涂层材料领域。采用等离子喷涂技术，在金属氧化物半导体材料表面喷涂覆盖气敏涂层，通过机械手在材料表面一次形成多孔涂层。制备出的多孔涂层的孔状结构增加了金属氧化物半导体的比表面积，对气体的灵敏度增加，同时改善基体材料的稳定性、导电性、选择性，提高载体材料的响应速度，降低响应恢复时间。
Description
技术领域
本发明涉及一种气敏涂层材料及其制备方法，属于半导体涂层材料领域。
背景技术
氧化物半导体气敏传感器因具有灵敏度高，制造成本低和信号测量手段简单等特性而受到重点关注，但是单一组分的金属氧化物半导体材料气敏材料往往因为灵敏度低，选择性差，稳定性差和抗环境干扰能力差等缺点难以满足实际应用，将不同材料复合化是当代材料发展的方向。复合材料中由于强的界面相互作用使各个组分不仅能够保持各自的独立性，同时具备各个组分间协同作用而产生的单一材料并不具备的综合物理化学性能 ，进而弥补了上述单一材料的缺点。
纳米复合材料或材料表面改性应用在气体传感器上，能够提升敏感度，改善传感器选择性，降低工作温度等。但传统的表面方法存在有不足之处，如溅射法只能在金属氧化物半导体气敏材料溅射单一的某种贵金属（Au/Pt/Pd），且贵金属成本较高，浸渍法/水热法/微波辐射法存在表面改性的物质和金属氧化物半导体气敏材料之间粘结性不好，容易脱落，影响气敏材料的使用性能。所以，利用传统的改性方法仍然不能得到性能优异，且优异的持续时间长的金属氧化物半导体气敏改性材料。
发明内容
本发明的目的在于提供一种气敏涂层材料，具体为：在金属氧化物半导体材料表面喷涂覆盖气敏涂层，所述涂层由以下原料制备得到，各原料及其重量份数为：原料A为40-50重量份，原料B为20-30重量份，原料C为5-10重量份，原料D为10-35重量份；
所述原料A为氧化铜、氧化锌、氧化镍中的一种；
所述原料B为氧化锆、纳米氧化铟、氧化钛中的一种；
所述原料C为砷化镓、纳米氧化锡、硅中的一种；
所述原料D为二氧化锰、锑中的一种。
优选的，本发明所述纳米氧化铟的粒度为25~35nm，纳米氧化锡的粒度为20~30nm。
本发明的另一目的在于提供所述气敏涂层材料的制备方法，具体包括以下步骤:
（1）称取各原料进行烧结、破碎后得到混合粉末；
（2）对待喷涂的基材金属氧化物半导体材料进行喷砂粗糙处理；
（3）将步骤（1）得到的干燥粉末送入热喷涂系统的送粉器内；
（4）设置热喷涂技术工艺参数，启动热喷涂系统和机械手，在金属氧化物半导体材料表面喷涂覆盖一次后得到多孔涂层。
优选的，本发明步骤（4）中的所述热喷涂技术工艺参数为：氩气的气流量为90-130L/min，氮气的气流量为5-30L/min，工作电流为350-450A，工作电压为120-150V。
本发明所述步骤（4）中的热喷涂技术除普通气稳等离子喷涂技术外，还包括超音速火焰喷涂技术以及水稳等离子喷涂技术等。
本发明的有益效果：
（1）由于改性涂层粉末成分和比例合适，采用的等离子喷涂设备电流稳定，制备出的多孔改性涂层的孔状结构增加了金属氧化物半导体的比表面积，对气体的灵敏度增加，响应速度提高，且气敏材料的选择性、导电性都得到改善。
（2）本发明采用热喷涂技术在金属氧化物半导体气敏材料表面上一次喷涂，制备多孔涂层，降低制造成本，简单的工艺。
具体实施方式
以下为本发明的具体实施例，对本发明的技术方案做进一步详细描述，但是本发明的保护范围并不限于这些实施例，凡是不背离本发明构思的改变或等同替代均包括在本发明的保护范围之内。
实施例1
（1）取氧化铜400g、氧化锆200 g、砷化镓50 g、氧化锰350g进行烧结（烧结温度为1000℃，烧结时间为30min），然后破碎获得混合粉末，将干燥的粉末送入等离子喷涂设备；
（2）对待喷涂的金属氧化物半导体气敏材料Ge表面进行20目白刚玉喷砂粗糙处理，然后利用干燥空气对喷砂后的材料表面进行洁净处理；
（3）启动喷涂系统和机械手进行等离子喷涂，工艺参数为：主气为 Ar和N2， 氩气的气流量为90L/min，氮气的气流量为15L/min；工作电流为350A，工作电压为 110V；送粉器送粉气体为Ar，气体流量为 45L/min；喷嘴距离金属氧化物半导体气敏材料距离为9cm，喷嘴的移动速度为0.05m/s。得到的多孔涂层检测气体的浓度≥30ppm，响应时间为10s；对H2S、CO2、乙醇三种气体的敏感性良好；导电性是原来的1倍。
实施例2
（1）取氧化锌460g、25nm的氧化铟250 g、30nm的氧化锡80 g、氧化锰210 g进行烧结（烧结温度为1000℃，烧结时间为30min），然后破碎获得混合粉末，将干燥的粉末送入等离子喷涂设备；
（2）对待喷涂的金属氧化物半导体气敏材料Ge表面进行20目白刚玉喷砂粗糙处理（使用的沙粒材料为白刚玉，沙粒的粒度为18μm），然后利用干燥空气对喷砂后的材料表面进行洁净处理；
（3）启动喷涂系统和机械手进行等离子喷涂，工艺参数为：主气为 Ar和N2， 氩气的气流量为130L/min，氮气的气流量为30L/min；工作电流为450A，工作电压为 150V；送粉器送粉气体为Ar，气体流量为 45L/min；喷嘴距离金属氧化物半导体气敏材料距离为9cm，喷嘴的移动速度为0.05m/s。得到的多孔涂层检测的气体浓度≥45ppm，响应时间为15s；对NO2、SO2、NH3、丙酮、乙醇五种气体的敏感性良好；导电性是原来的1.6倍
实施例3
（1）取氧化镍500g、氧化钛300 g、硅100 g、锑100 g进行烧结（烧结温度为1000℃，烧结时间为30min），然后破碎获得混合粉末，将干燥的粉末送入等离子喷涂设备；
（2）对待喷涂的金属氧化物半导体气敏材料Ge表面进行20目白刚玉喷砂粗糙处理（使用的沙粒材料为白刚玉，沙粒的粒度为18μm），然后利用干燥空气对喷砂后的材料表面进行洁净处理；
（3）启动喷涂系统和机械手进行等离子喷涂，工艺参数为：主气为Ar和N2， 氩气的气流量为90L/min，氮气的气流量为15L/min；工作电流为350A，工作电压为 110V；送粉器送粉气体为Ar，气体流量为 45L/min；喷嘴距离金属氧化物半导体气敏材料距离为9cm，喷嘴的移动速度为0.05m/s。得到的多孔涂层检测的气体浓度≥70ppm，响应时间为30s；对NO2、SO2、NH3、H2S、CO2、CH4、丙酮、乙醇八种气体的敏感性良好；导电性是原来的2.1倍。
Claims (4)
1.一种气敏涂层材料，其特征在于：在金属氧化物半导体材料表面喷涂覆盖气敏涂层，所述涂层由以下原料制备得到，各原料及其重量份数为：原料A为40-50重量份，原料B为20-30重量份，原料C为5-10重量份，原料D为10-35重量份；
所述原料A为氧化铜、氧化锌、氧化镍中的一种；
所述原料B为氧化锆、纳米氧化铟、氧化钛中的一种；
所述原料C为砷化镓、纳米氧化锡、硅中的一种；
所述原料D为二氧化锰、锑中的一种。
2.根据权利要求1中所述气敏涂层材料，其特征在于：纳米氧化铟的粒度为25~35nm，纳米氧化锡的粒度为20~30nm。
3.权利要求1中所述气敏涂层材料的制备方法，其特征在于，具体包括以下步骤:
（1）称取各原料进行烧结、破碎得到混合粉末；
（2）对待喷涂的基材金属氧化物半导体材料进行喷砂粗糙处理；
（3）将步骤（1）得到的干燥粉末送入热喷涂系统的送粉器内；
（4）设置热喷涂技术工艺参数，启动热喷涂系统和机械手，在金属氧化物半导体材料表面喷涂覆盖一次后得到多孔涂层。
4.根据权利要求1所述表面改性的气敏涂层材料的制备方法，其特征在于：步骤（4）中的所述热喷涂技术工艺参数为：氩气的气流量为90-130L/min，氮气的气流量为5-30L/min，工作电流为350-450A，工作电压为120-150V。
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