CN105866184B - 一种对二氧化碳敏感的镧-二氧化锡纳米纤维膜 - Google Patents
一种对二氧化碳敏感的镧-二氧化锡纳米纤维膜 Download PDFInfo
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Abstract
本发明提供了一种可用于检测CO2的La‑SnO2传感器膜的制备方法，属于气敏传感器技术领域。我们将二水氯化亚锡与氯化镧混合，通过静电纺丝法制备了La‑SnO2材料，再通过丝网印刷法制备成膜，该样品可检测大范围浓度的CO2，在空气气氛下对1000ppm CO2的灵敏值高达3.4。此方法制备简单，原料成本低，可重复性好，材料膜性能优异，具有很好的应用价值和前景。
Description
技术领域
本发明属于气敏传感器技术领域，具体涉及一种镧-二氧化锡(La-SnO2)纳米纤维膜的制备及其对二氧化碳的气敏性能研究。
背景技术
近年来，二氧化碳(CO2)产生的温室效应使气候变化异常、自然灾害频发和疾病增多等已引起世界各国的普遍关注，对CO2浓度进行快速准确的检测和监控尤为重要。此外，在室内空气质量监测、农业生产、清洁能源技术、化学化工等领域，也需要对CO2浓度进行严格控制。因此，研制性能优异的CO2传感器已成为目前国内外研究热点。
当前，检测CO2的手段主要包括红外、电化学和金属氧化物半导体(MOS)传感器检测法。其中，采用红外法检测CO2所需成本太高，电化学传感器又存在易漏电、寿命短等问题。而MOS传感器由于具有体积小、操作方便、成本低廉、响应时间和恢复时间短等优点，其产品发展迅速，目前已成为世界上产量最大、应用最广的传感器之一。然而，CO2是一种化学性质非常稳定的气体，用纯MOS材料检测CO2灵敏度非常低。为了提高MOS材料的敏感性能，人们尝试了多种方法，其中，二氧化锡(SnO2)表面修饰稀土元素的方法采用的较多。早在1993年，Mizuno等就研究了La-SnO2对CO2的灵敏性能(Sens.Actuators B,1993,13,473)，但其工作温度高达673K，高温测试增加了设备投入，因而应用上具有较大的局限。
迄今为止，文献中报道的MOS气敏传感器几乎都是在空气中使用。然而，很少有人研究背景气氛中氧浓度大小对CO2传感器检测性能的影响，而弄清楚这点能帮助我们更好地研究材料对CO2的敏感机制。Kim等人分别研究了在纯氮气、合成空气和纯氧背景气氛下，采用微滴注法制备的La-SnO2对2000ppm CO2的检测，发现材料在纯氧气氛下灵敏值最大，为1.59，在氮气气氛下对CO2几乎无响应(Sens.Actuators B,2000,62,61)。Zhou等人对比了氮气气氛和空气气氛下，还原氧化石墨烯对5000ppm CO2的检测，发现材料在空气气氛下灵敏值较大，约为1.1，在氮气气氛下约为1.01(Sens.Actuators B,2014,203,135)。显然，背景气氛中氧含量确实很大程度地影响着材料对CO2的检测。
为系统研究背景气氛中氧浓度对气敏性能的影响，我们以锡的无机盐为原料，采用静电纺丝法制备了La-SnO2纳米纤维，通过丝网印刷法制备成膜，然后进行性能测试。该方法制备简单，原料成本低，可重复性好，对CO2灵敏度高，具有很好的应用价值和前景。
发明内容
本发明的目的是提供一种检测CO2的传感器膜的制备方法。通过静电纺丝法制备La-SnO2纳米纤维，再通过丝网印刷法制备成膜。该制备方法具有成本低廉、操作方便、简单快捷等特点。
下面以二水氯化亚锡(SnCl2.2H2O)为例简要说明本发明的实现过程。首先采用静电纺丝法制备La-SnO2纳米纤维，将适量的纳米纤维和有机浆料混合均匀后涂覆在叉指电极上，涂层干燥后即为一层均匀膜。将上述覆有膜的叉指电极置于马弗炉中，分别在350℃和550℃下处理2小时后取出，得到测试基片，将测试基片放入洁净环境中保存，等待后续电学性质测试。该La-SnO2纤维膜可通过以下具体步骤实现：
(1)将0.6克二水氯化亚锡和氯化镧混合，其中镧元素与锡元素的摩尔比为8:100，然后分别加入4.42克二甲基甲酰胺和4.42克无水乙醇，将混合液搅拌30分钟；
(2)待上述二水氯化亚锡和氯化镧完全溶解后加入0.8克聚乙烯吡咯烷酮，搅拌12小时得到澄清透明的电纺前驱溶液；
(3)用注射器量取一定量的电纺前驱液进行纺丝，设置注射泵速度为1毫升/小时，直流高压电源正向供电电压为20千伏，负向供电电压为1千伏，纺丝喷头和收集板距离为15厘米；
(4)电纺得到的纤维在60℃下干燥24小时后置于管式炉中600℃处理2小时后得到样品，管式炉升温速率为1℃/分钟；
(5)取适量上述样品和有机浆料混合均匀，然后丝网印刷到印有铂电极的陶瓷片上，得到一层均匀的膜；
(6)将上述覆有膜的陶瓷片置于马弗炉中，分别在350℃和550℃下处理2小时后取出，得到测试基片，将测试基片放入洁净环境中保存，等待后续电学性质测试。
由上述过程可获得不同比例镧掺杂的SnO2纳米纤维膜(记作La-SnO2)。当背景气氛中氧浓度分别为0、50、500ppm时，16at.％掺杂的材料对CO2的灵敏度最高，当背景气氛中氧浓度为21％(合成空气)和100％时，8at.％掺杂的材料对CO2的灵敏度最高。且对于同种材料，随着背景气氛中氧浓度增加，材料对CO2的灵敏度增加。
本发明所提供的制备La-SnO2纳米纤维膜的方法，可实现对大范围的CO2浓度检测。该方法制备简单，原料成本低，可重复性好，具有很好的应用价值和前景。
附图说明
图1为测试基片制备示意图。
图2为氮气气氛下，纯SnO2及4at.％、8at.％、12at.％、16at.％La-SnO2对1000ppmCO2的灵敏度随温度变化曲线图。
图3为不同氧浓度背景气氛，300℃下，16at.％La-SnO2的电阻随1000ppm CO2通断气变化曲线图。
图4为空气气氛，300℃下，纯SnO2及4at.％、8at.％、12at.％、16at.％La-SnO2的电阻随1000ppm CO2通断气变化曲线图。
图5为不同氧浓度背景气氛，300℃下，8at.％和16at.％La-SnO2对CO2的灵敏度随CO2浓度变化曲线图。
具体实施方式
下面结合附图和实施例来详细描述本发明。
实施例1，将0.6克二水氯化亚锡和氯化镧混合，其中镧元素与锡元素的摩尔比为8:100，然后分别加入4.42克二甲基甲酰胺和4.42克无水乙醇(共4个样)，将混合液搅拌30分钟至无机盐完全溶解，再加入0.8克聚乙烯吡咯烷酮，搅拌12小时得到澄清透明的电纺前驱溶液。用注射器量取一定量的电纺前驱液进行纺丝。设置注射泵速度为1毫升/小时，直流高压电源正向供电电压为20千伏，负向供电电压为1千伏，纺丝喷头和收集板距离为15厘米。将电纺得到的纤维在60℃下干燥24小时后置于管式炉中600℃处理2小时，管式炉升温速率为1℃/分钟。取70毫克上述样品和30毫克有机浆料混合均匀后丝网印刷到印有铂电极的陶瓷片上，得到一层均匀的膜。将上述覆有膜的陶瓷片置于马弗炉中，分别在350℃和550℃下处理2小时后取出，得到测试基片，其过程如图1所示。
图2给出了氮气气氛下，纯SnO2及4at.％、8at.％、12at.％、16at.％La-SnO2对1000ppm CO2的灵敏度随温度变化曲线图。从图中可知，在所测温度范围内，300℃下材料膜对1000CO2的灵敏度最高。从图中还可得知，在所掺杂浓度范围内，16at.％La-SnO2对CO2的灵敏度最高。
图3给出了不同氧浓度背景气氛，300℃下，16at.％La-SnO2的电阻随1000ppm CO2通断气变化曲线图。从图中可知，通CO2后材料电阻下降，停止通入CO2后材料能很快恢复到初始电阻。从图中还可得知，对于同种材料，随着背景气氛中氧浓度增加，材料对CO2的灵敏度增加，分别为2、2.4、3、3.4、3.6。
图4给出了空气气氛，300℃下，纯SnO2及4at.％、8at.％、12at.％、16at.％La-SnO2的电阻随1000ppm CO2通断气变化曲线图。从图中可知，在所掺杂浓度范围内，8at.％La-SnO2对CO2的灵敏度最高。
图5给出了不同氧浓度背景气氛，300℃下，8at.％和16at.％La-SnO2对CO2的灵敏度随CO2浓度变化曲线图。从图中可知，当背景气氛中氧浓度为0、50和500ppm时，材料在测高浓度CO2时出现饱和现象，而当背景气氛中氧浓度为21％(合成空气)和100％时，在所测CO2浓度范围100-1000000ppm内，材料没有出现饱和现象，且在这两种背景气氛下，8at.％La-SnO2对1000000ppm CO2的灵敏度分别高达393和607。
Claims (1)
1.一种对二氧化碳敏感的镧-二氧化锡纳米纤维膜的制备方法，其制备步骤包括：
(1)将0.6克二水氯化亚锡和氯化镧混合，其中镧元素与锡元素的摩尔比为8:100，然后分别加入4.42克二甲基甲酰胺和4.42克无水乙醇，将混合液搅拌30分钟；
(2)待上述二水氯化亚锡和氯化镧完全溶解后加入0.8克聚乙烯吡咯烷酮，搅拌12小时得到澄清透明的电纺前驱溶液；
(3)用注射器量取一定量的电纺前驱液进行纺丝，设置注射泵速度为1毫升/小时，直流高压电源正向供电电压为20千伏，负向供电电压为1千伏，纺丝喷头和收集板距离为15厘米；
(4)电纺得到的纤维在60℃下干燥24小时后置于管式炉中600℃处理2小时后得到样品，管式炉升温速率为1℃/分钟；
(5)取适量上述样品和有机浆料混合均匀，然后丝网印刷到印有铂电极的陶瓷片上，得到一层均匀的膜；
(6)将上述覆有膜的陶瓷片置于马弗炉中，分别在350℃和550℃下处理2小时后取出，得到测试基片，将测试基片放入洁净环境中保存，等待后续电学性质测试。
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| "CO2 Sensing Properties of La-loaded SnO2 Thin Films Prepared by Sputtering";Hiroshi Sakama等;《Chemistry Letters》;20041231;第33卷(第9期);第1080页左栏倒数第一段及右栏第一-二段 |
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| "PVP-assisted Sb-doped SnO2 nanofibers synthesized byelectrospinning process";Somtop Santibenchakul等;《Key Engineering Materials》;20160125;全文 |
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