CN108455659B - 一种纳米棒状氧化铟气敏材料的制备方法 - Google Patents
一种纳米棒状氧化铟气敏材料的制备方法 Download PDFInfo
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Abstract
本发明涉及一种纳米棒状结构的氧化铟(In2O3)气敏材料的制备方法，属于无机纳米功能材料制备技术领域。本发明以四水合三氯化铟为铟源，采用十六烷基三甲基溴化铵为表面活性剂，在氢氧化钠碱性条件下水热反应制备氢氧化铟，最后进行热焙烧处理得到纳米棒状结构的氧化铟气敏材料。最终制备的氧化铟为立方相In2O3纳米棒状结构，对二氧化氮气体和硫化氢气体都具有很好的传感检测性能，而且对其他气体(一氧化碳、乙醇、氨气、氢气、甲醛等)不敏感；并且工作温度低、响应恢复迅速、灵敏度很高、检测限极低、选择性高、稳定性高。此外，这种氧化铟气敏材料还可以用于催化剂、电池材料、光电材料等领域。
Description
技术领域
本发明涉及一种纳米棒状结构的氧化铟(In2O3)气敏材料的制备方法，属于无机纳米功能材料制备技术领域。
背景技术
目前环境污染越来越受到人们的重视，特别是有毒有害的污染气体，对人们的健康带来极大的危害。其中二氧化氮(NO2)和硫化氢(H2S)是环境污染气体中危害性非常强的气体，在极低的浓度(ppm级)下，即可对人体健康造成很大的伤害，甚至在短时间内造成死亡。因此制造具有高灵敏度和低检测限的二氧化氮和硫化氢快速气敏传感器是非常重要的。
氧化铟是应用于半导体气敏传感器的一种重要的气敏材料，广泛应用于检测各种有毒有害气体方面的研究，例如二氧化氮、硫化氢、氢气、乙醇、一氧化碳、甲醛等，特别是对二氧化氮气体或者硫化氢气体具有很好的传感检测性能。但是目前研究报道的各种氧化铟气敏材料只是对二氧化氮或硫化氢中的一种气体具有高效的传感检测功能，既能够迅速高效的检测二氧化氮气体，又可以检测硫化氢气体的双功能氧化铟气敏材料目前还没有报道。
氧化铟的形貌和尺寸是其气敏性能和应用的重要因素，不同的形貌会有不同的晶体暴露面，晶体材料的各向异性决定了不同晶面具有不同的表面能和催化活性，控制晶体沿特定的晶向生长可以使活性较高的晶面暴露在材料表面参与气敏反应，而且即使形貌相似的氧化铟材料，其制备工艺不同，导致其表面活性不同，目标气体与氧化铟材料表面的化学吸附氧发生反应的速率不同，具体表现为气敏性能的很大差别，因此形貌和尺寸的调控一直是氧化铟材料的研究重点。因此具有工作温度低、响应恢复迅速、灵敏度高、检测限低、稳定性高等优点的氧化铟气敏材料，具有重要的意义。
发明内容
针对上述存在问题或不足，为解决现有氧化铟气敏材料无法同时检测二氧化氮气体和硫化氢气体的问题，本发明提供了一种纳米棒状结构氧化铟气敏材料的制备方法。
具体步骤如下：
步骤1、配置反应溶液
在乙醇中加入四水合三氯化铟，搅拌至完全溶解，得澄清三氯化铟溶液，其中四水合三氯化铟的浓度为：0.01mol/L～0.1mol/L。然后在搅拌下加入氢氧化钠水溶液(0.1～2mol/L)，搅拌5～30分钟，再加入十六烷基三甲基溴化铵(CTAB)，搅拌10～60分钟得到溶胶，CTAB和四水合三氯化铟的摩尔比为1:10至1:1。
步骤2、水热反应生成纳米棒状氢氧化铟
将步骤1制备的溶胶转移到聚四氟乙烯内衬的水热釜中，在120～200℃下水热反应5～24h。将水热反应后的产物过滤，用去离子水和乙醇的混合溶液洗涤，60～110℃烘干，得到白色氢氧化铟粉末。
步骤3、焙烧得到纳米棒状氧化铟
将步骤2制备的白色氢氧化铟粉末在350～600℃焙烧0.5～5小时，直至完成晶型转化，得纳米棒状氧化铟粉末。
将上述方法制备的纳米棒状结构氧化铟气敏材料应用于对二氧化氮气体和硫化氢气体的传感检测。
本发明以四水合三氯化铟为铟源，采用十六烷基三甲基溴化铵为表面活性剂，在氢氧化钠碱性条件下水热反应制备氢氧化铟，最后进行热焙烧处理得到纳米棒状结构的氧化铟气敏材料。
最终制备的氧化铟为立方相In2O3纳米棒状结构，直径15～40纳米之间，长度为50～300纳米，是一种优秀的气敏材料，对二氧化氮气体和硫化氢气体都具有很好的传感检测性能。对二氧化氮和硫化氢气体的传感检测性能优点表现为：工作温度低(对二氧化氮气体工作温度25℃至100℃；对硫化氢气体工作温度为25℃)、响应恢复迅速、检测限极低(0.001ppm的二氧化氮，0.005ppm的硫化氢)、灵敏度很高、稳定性高等。并且此氧化铟气敏材料对二氧化氮气体的传感检测表现为电阻的升高，对硫化氢气体表现为电阻的降低，而且对其他气体(一氧化碳、乙醇、氨气、氢气、甲醛等)不敏感，没有响应，因此这种氧化铟气敏材料可以对二氧化氮和硫化氢进行选择性检测。同时，此氧化铟材料还可以用于催化剂、电池材料、光电材料等领域。
综上所述，本发明制备的氧化铟气敏材料可同时检测二氧化氮气体和硫化氢气体，且测试灵敏度高，响应恢复迅速，检测限低。
附图说明
图1为实施例1制备的纳米棒状氧化铟材料的扫描电镜照片；
图2为实施例1制备的纳米棒状氧化铟材料的X射线衍射谱图；
图3为实施例1制备的纳米棒状氧化铟材料的对二氧化氮气体的气敏响应恢复曲线；
图4为实施例1制备的纳米棒状氧化铟材料的对硫化氢气体的气敏响应恢复曲线。
具体实施方式
下面结合实施例和附图对本发明做进一步的详细说明。
实施例1
取1.10g四水合三氯化铟加入到50ml无水乙醇中配制成0.075mol/L的三氯化铟乙醇溶液。取1.50g氢氧化钠加入到50ml去离子水中配置成0.75mol/L NaOH水溶液。
分别取20mL的上述三氯化铟乙醇溶液和20mL的上述NaOH水溶液混合，加入0.27g十六烷基三甲基溴化铵(CTAB)(摩尔比InCl3·4H2O:CTAB＝5:1)，搅拌1小时。
将前述制得溶液放入50mL反应釜中，然后放入鼓风干燥箱，设置温度为180℃，反应12小时。反应结束后，将所得白色沉淀产物用去离子水和乙醇的混合溶液洗涤，在干燥箱中60℃干燥6小时得白色的氢氧化铟粉末。将这种氢氧化铟粉末在马弗炉中500℃煅烧2小时，得到黄色的氧化铟粉末。
纳米棒状氧化铟材料的扫描电镜图片如图1所示，显示了制备的氧化铟的纳米棒结构，平均直径22纳米，平均长度为210纳米，比表面积为18.9m2/g。XRD测量结果如图2所示表明其为具有立方晶相的氧化铟；图3可以看出基于氧化铟纳米棒的传感器在100℃对二氧化氮检测显示出快速响应/恢复时间，高灵敏度和低至0.001ppm的检测限。图4所示基于氧化铟纳米棒的传感器在25℃对硫化氢检测显示出快速响应/恢复时间，高灵敏度和低至0.005ppm的检测限。说明作为气敏材料，它对二氧化氮气体和硫化氢气体具有很好的气敏性能。
实施例2
取3.30g四水合三氯化铟加入到50ml无水乙醇中配制成0.225mol/L的三氯化铟乙醇溶液。取3.0g氢氧化钠加入到50ml去离子水中配置成1.50mol/L NaOH水溶液。
分别取20mL的上述三氯化铟乙醇溶液和20mL的上述NaOH水溶液混合，加入0.60g十六烷基三甲基溴化铵(CTAB)，搅拌1小时。
将前述制得溶液放入50mL反应釜中，然后放入鼓风干燥箱，设置温度为150℃，反应24小时。反应结束后，将所得白色沉淀产物用去离子水和乙醇的混合溶液洗涤，在干燥箱中100℃干燥2小时得白色的氢氧化铟粉末。将这种氢氧化铟粉末在马弗炉中400℃煅烧3小时，得到黄色的氧化铟粉末。
电子显微镜下观察氧化铟为纳米棒状，平均直径32纳米，平均长度为430纳米，比表面积为11.8m2/g。XRD测量结果表明其为具有立方晶相的氧化铟。作为气敏材料，测试发现它对二氧化氮气体和硫化氢气体具有很好的气敏性能。
Claims (2)
1.一种纳米棒状结构氧化铟气敏材料的制备方法，具体步骤如下：
步骤1、配置反应溶液
在乙醇中加入四水合三氯化铟，搅拌至完全溶解，得澄清三氯化铟溶液，其中四水合三氯化铟的浓度为：0.01mol/L～0.1mol/L；然后在搅拌下加入0.1～2mol/L的氢氧化钠水溶液，搅拌5～30分钟；再加入十六烷基三甲基溴化铵CTAB，搅拌10～60分钟得到溶胶，CTAB和四水合三氯化铟的摩尔比为1:10至1:1；
步骤2、水热反应生成纳米棒状氢氧化铟
将步骤1制备的溶胶转移到聚四氟乙烯内衬的水热釜中，在150～200℃下水热反应12～24h；将水热反应后的产物过滤，用去离子水和乙醇的混合溶液洗涤，60～110℃烘干，得到白色氢氧化铟粉末；
步骤3、焙烧得到纳米棒状氧化铟
将步骤2制备的白色氢氧化铟粉末在350～600℃焙烧0.5～5小时，直至完成晶型转化，得纳米棒状氧化铟粉末。
2.将权利要求1制备的纳米棒状结构氧化铟气敏材料应用于对二氧化氮气体和硫化氢气体的传感检测。
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