CN110357143B - 用于Hg(0)传感器的敏感材料MoS2-Ag2S - Google Patents
用于Hg(0)传感器的敏感材料MoS2-Ag2S Download PDFInfo
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Abstract
一种用于Hg(0)传感器的敏感材料MoS2‑Ag2S，属于半导体传感器技术领域。本发明的目的是以硫化物半导体为模板的MoS2‑Ag2S电阻型传感器用于检测Hg(0)的用于Hg(0)传感器的敏感材料MoS2‑Ag2S。本发明取去离子水；称取硝酸银，钼酸铵，六次甲基四安，硫化钠；在搅拌状态下分别将称量的药品逐一溶解；在完全溶解后搅拌10 min，然后移入反应釜中，水热200℃，保持12h；将反应釜在高压状态下自然冷却至室温，然后将黑色产物分别用去离子水和乙醇离心洗涤3次；将洗涤后收集的黑色产物在真空干燥箱中干燥24h，真空干燥箱温度设为60℃。本发明对Hg(0)有良好的气敏性能。最终能对Hg(0)的含量进行检测，使得检测下限可达0.001mg/m3。
Description
技术领域
本发明属于半导体传感器技术领域。
背景技术
汞作为剧毒金属物质之一，对生物和环境造成严重危害。由于它具有迁移性、生物累积性和持久性，使得高级生物比低级生物更易累积，对高级生物造成的伤害更加明显。其中人为排放量中比例占较大的为燃煤排放，因此联合国在2010年制定燃煤排放的相关措施。目前采用的检测方法主要基于冷原子吸收光谱法，冷原子荧光光谱法原理。基于此原理的设备比较复杂且人工误差大等缺点，无法快速有效的检测气态元素汞含量。
近些年由于半导体材料的兴起，由半导体制作的传感器具有良好的灵敏度，选择性，响应恢复时间短，稳定性好等特点。因此开发一款远程快速实时监测的汞传感器已成为汞检测的趋势。
发明内容
本发明的目的是以硫化物半导体为模板的MoS2-Ag2S电阻型传感器用于检测Hg(0)的用于Hg(0)传感器的敏感材料MoS2-Ag2S。
本发明取70 mL去离子水；准确称取4mmol硝酸银，1mmol钼酸铵，4mmol六次甲基四安，9mmol硫化钠；在搅拌状态下分别将称量的药品逐一溶解；在完全溶解后搅拌10 min，然后移入100 mL反应釜中，水热200℃，保持12h；将反应釜在高压状态下自然冷却至室温，然后将黑色产物分别用去离子水和乙醇离心洗涤3次；将洗涤后收集的黑色产物在真空干燥箱中干燥24h，真空干燥箱温度设为60℃。
本发明用上述敏感材料MoS2-Ag2S制作的气体传感器，其步骤是：
①以Al2O3陶瓷管为衬底，陶瓷管两段各有一个圆环状的金电极，每个金电极均有两根铂丝做引线；
②将一制得的MoS2-Ag2S层状纳米花材料用玛瑙研钵研细，滴入几滴去离子水调成糊状,然后用细毛刷涂抹在陶瓷管的外表面,涂层厚度尽量均匀,除引线外，陶瓷管的外表面及环状金电极完全被MoS2-Ag2S层状纳米花材料覆盖；
③陶瓷管自然或在红外灯下阴干,把镍铬合金加热丝从陶瓷管内部穿入,最后将引脚焊接在器件管座上，得到Hg(0)传感器。
本发明的MoS2-Ag2S层状纳米花材料，由纳米片团簇成纳米花，纳米花大小分布均一。由于硫键和银的汞齐的使得气敏半导体气敏性能增加。从而对Hg(0)有良好的气敏性能。最终能对Hg(0)的含量进行检测，使得检测下限可达0.001mg/m3。
附图说明
图1是 (a)SEM在500nm视野下的照片 (b)SEM在200nm视野下的照片 (c)TEM在200nm视野下的照片 (d)材料的XRD谱图；
图2：材料的元素分布图；
图3：(a)传感器件示意图，(b)传感器实际图像；
图4：实例1中传感器在不同Hg(0)浓度下的响应曲线；
图5：实例1中传感器在最佳响应恢复曲线；
图6：实例1中传感器对不同干扰气体的选择性；
图7：实例1中Hg(0)气体传感器对不同干扰气体的选择性。
具体实施方式
基于汞齐相互作用，研究开发了以金材料为模板的传感器。如开发了金薄膜电阻型传感器，金材料声表面传感器，金纳米棒光纤渐逝波传感器，金材料的波长检测型表面等离子体共振传感器，金纳米颗粒复合碳纳米管电阻型传感器。金传感器响应恢复时间过长，检测范围窄，稳定性差等特点。MoS2-PANI电阻型传感器，响应和恢复时间快，分别在8-10min，15-20min，并且具有良好的选择性，较宽的检测范围从0.55-452.51mg/m3。PANI-TiO2电阻型传感器，AgCl-H2Ti2O5电阻型传感器。检测范围比之前硫化物半导体窄，响应时间也大于20min。因此本发明是基于硫化物半导体为模板的MoS2-Ag2S电阻型传感器用于检测Hg(0)。
本发明本发明所述的MoS2-Ag2S层状纳米花材料，由纳米花团簇成花状的纳米材料。纳米花大小分布均一。
本发明首先以硝酸银、钼酸铵、六次甲基四胺、硫化钠为原料，在200℃下水热12h，成功制备了MoS2-Ag2S层状纳米花复合材料；最后将材料构筑成Hg(0)传感器。本发明所述的MoS2-Ag2S层状纳米花材料的具体制备方法如下：
1.MoS2-Ag2S层状纳米花材料的制备
所用药品均为实验纯，使用前未做提纯处理。取70 mL去离子水。准确称取4mmol硝酸银，1mmol钼酸铵，4mmol六次甲基四安，9mmol硫化钠。在搅拌状态下分别将称量的药品逐一溶解。在完全溶解后搅拌10 min，然后移入100 mL反应釜中，水热200℃，保持12h。将反应釜在高压状态下自然冷却至室温，然后将黑色产物分别用去离子水和乙醇离心洗涤3次。将洗涤后收集的黑色产物在真空干燥箱中干燥24h，真空干燥箱温度设为60℃。
2.气体传感器的制作：
①以Al2O3陶瓷管为衬底，陶瓷管两段各有一个圆环状的金电极，每个金电极均有两根铂丝做引线。
②将一制得的MoS2-Ag2S层状纳米花材料用玛瑙研钵研细，滴入几滴去离子水调成糊状,然后用细毛刷涂抹在陶瓷管的外表面,涂层厚度尽量均匀,除引线外，陶瓷管的外表面及环状金电极完全被MoS2-Ag2S层状纳米花材料覆盖
③陶瓷管自然或在红外灯下阴干,把镍铬合金加热丝从陶瓷管内部穿入,最后将引脚焊接在器件管座上，得到Hg(0)传感器。
在这里，传感器的灵敏度定义为S=(Rg-R0)/R0式中：Rg为元件在被测气体中的稳定电阻，R0为元件在空气中的稳定电阻；响应时间被定义为在被测气体中传感器输出变化达到稳定值的90%的时间，恢复时间被定义为传感器在气体被移除后（在空气中）达到初始稳定值的10%所需的时间。本发明所述的MoS2-Ag2S层状纳米花材料在气敏测试时采用的是静态配气法。
如图1所示：实例1中由图(d)可观察到的XRD图所对应的标准卡片是Ag2S，。由(a)SEM在500nm视野下的照片可以看到该纳米复合材料是由小薄片团簇在一起形成花状的形貌，形貌大小分布均一。图(b)SEM在200nm视野下的照片的可以看到复合材料是由纳米小薄片通过弯曲团聚在一起，中间的褶皱增大了材料的比表面积，更加有利于对目标气体的吸附。由(c)TEM在200nm视野下的照片可以得到，该材料形成的花状外貌，是自内向外伸展，所以TEM表现出花状内部较暗外部较明的特点。
如图2所示，由于通过XRD不能判断MoS2的存在，对材料做了mapping，从元素分布图和能谱图中可以看出，材料Ag、Mo、S是存在的，可以证明MoS2的存在。
如图3所示，从图1和2不能判断出材料是层状结构，通过图3高倍TEM，可以看出它是由MoS2和Ag2S相互穿插的层状结构。
如图4所示：实例1中的由Hg(0)气体传感器由气敏元件和基座两部分构成，其中气敏元件由Al2O3衬底、MoS2-Ag2S层状纳米花材料、环状Au电极、Pt线和镍铬合金电阻丝5部分构成。
由图5可知：实例1中Hg(0)气体传感器对不同Hg(0)浓度的响应灵敏度曲线，从中可以看出浓度在452mg/m3时对Hg(0)的响应最优，响应检测下限可达0.001mg/m3。
由图6可知：实例1中Hg(0)气体传感器最佳响应曲线。从中可以看到响应和恢复时间均在10S左右。
由图7可知：实例1中Hg(0)气体传感器对不同干扰气体的选择性。对乙醇、H2S、NO2、NH3等干扰气体具有良好的选择性。
实例1:
基于MoS2-Ag2S层状纳米花材料的Hg(0)气体传感器，其制备方法如下：
①所用药品均为实验纯，使用前未做提纯处理。取70 mL去离子水。准确称取4mmol硝酸银，1mmol钼酸铵，4mmol六次甲基四安，9mmol硫化钠。在搅拌状态下分别将称量的药品逐一溶解。在完全溶解后搅拌10 min，然后移入100 mL反应釜中，水热200℃，保持12h。将反应釜在高压状态下自然冷却至室温，然后将黑色产物分别用去离子水和乙醇离心洗涤3次。将洗涤后收集的黑色产物在真空干燥箱中干燥24h，真空干燥箱温度设为60℃。
②以Al2O3陶瓷管为衬底，陶瓷管两段各有一个圆环状的金电极，每个金电极均有两根铂丝做引线。
③将一制得的MoS2-Ag2S层状纳米花材料用玛瑙研钵研细，滴入几滴去离子水调成糊状,然后用细毛刷涂抹在陶瓷管的外表面,涂层厚度尽量均匀,除引线外，陶瓷管的外表面及环状金电极完全被MoS2-Ag2S层状纳米花材料覆盖
④陶瓷管自然或在红外灯下阴干，自然冷却后,把镍铬合金加热丝从陶瓷管内部穿入,最后将引脚焊接在器件管座上，得到Hg(0)气体传感器。
实例2
基于MoS2-Ag2S层状纳米花材料的Hg(0)气体传感器，在不同浓度下对Hg(0)进行检测：
①打开精密数字多用表，可编程直流电源以及电脑。在电脑上打开软件“FLUCK”，设置1s检测一次。将制作的敏感元件插在测试插口上，可以立即在精密数字多用表的显示屏幕上看到敏感元件的即时电阻，并且在软件窗口上也可以看出电阻的变化曲线。记录下此时的电阻R0、加热电流和电压。
②在1L静态配气瓶中用注射器充入100 ml Hg(0)气体（用油浴锅对也太汞进行加热，加热温度为30℃，此时所配Hg(0)的浓度为3mg/m3），塞紧瓶塞。打开瓶塞，将Hg(0)气体传感器插入气瓶中，使Hg(0)气体传感器处于Hg(0)气体的氛围中。待电阻稳定之后，记录下此时的电阻Rg；将Hg(0)气体传感器取出，于原位置放置，使电阻恢复到稳定。一次检测完成
③改变汞浓度依次测量不同浓度下，该传感器对Hg(0)的响应。
实例3
基于MoS2-Ag2S层状纳米花材料的Hg(0)气体传感器，在不同Hg(0)浓度下的响应：
①打开精密数字多用表，可编程直流电源以及电脑。在电脑上打开软件“FLUCK”，设置1s检测一次。将制作的敏感元件插在测试插口上，可以立即在精密数字多用表的显示屏幕上看到敏感元件的即时电阻，并且在软件窗口上也可以看出电阻的变化曲线。记录下此时的电阻R0。
②在1L静态配气瓶中用注射器充入100 ml Hg(0)气体（用油浴锅对也太汞进行加热，加热温度为30℃，此时所配Hg(0)的浓度为3mg/m3），塞紧瓶塞。打开瓶塞，将Hg(0)气体传感器插入气瓶中，使Hg(0)气体传感器处于Hg(0)气体的氛围中。待电阻稳定之后，记录下此时的电阻Rg；将Hg(0)气体传感器取出，于原位置放置，使电阻恢复到稳定。一次检测完成
③依次改变注入的Hg(0)气体体积，使得Hg(0)浓度为0.001 mg/3、0.005 mg/m3、0.01 mg/m3、0.1 mg/m3、0.5mg/m3、1 mg/m3、5 mg/m3、10 mg/m3、20 mg/m3、30mg/m3等，对传感器进行测试。
Claims (1)
1.一种用于Hg(0)传感器的敏感材料MoS2-Ag2S，其特征在于：取70 mL去离子水；准确称取4mmol硝酸银，1mmol钼酸铵，4mmol六次甲基四胺，9mmol硫化钠；在搅拌状态下分别将称量的药品逐一溶解；在完全溶解后搅拌10 min，然后移入100 mL反应釜中，水热200℃，保持12h；将反应釜在高压状态下自然冷却至室温，然后将黑色产物分别用去离子水和乙醇离心洗涤3次；将洗涤后收集的黑色产物在真空干燥箱中干燥24h，真空干燥箱温度设为60℃，其中得到的MoS2-Ag2S为层状纳米花材料；
用上述敏感材料MoS2-Ag2S制作的气体传感器：
①以Al2O3陶瓷管为衬底，陶瓷管两段各有一个圆环状的金电极，每个金电极均有两根铂丝做引线；
②将一制得的MoS2-Ag2S层状纳米花材料用玛瑙研钵研细，滴入几滴去离子水调成糊状,然后用细毛刷涂抹在陶瓷管的外表面,涂层厚度尽量均匀,除引线外，陶瓷管的外表面及环状金电极完全被MoS2-Ag2S层状纳米花材料覆盖；
③陶瓷管自然或在红外灯下阴干,把镍铬合金加热丝从陶瓷管内部穿入,最后将引脚焊接在器件管座上，得到Hg(0)传感器。
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