CN108572198A - 一氧化氮气敏材料及其在制备传感器上的应用 - Google Patents
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Abstract
本发明公开了一氧化氮气敏材料及其在制备传感器上的应用。该一氧化氮气敏材料由In2O3和Nb2O5的WO3混合而成。此一氧化氮气敏材料在制备传感器上的应用包括以下步骤:称量In2O3,Nb2O5和WO3,混合后加入乙醇搅拌均匀,投入球磨机中磨碎得混合粉末;将混合粉末烘干后,加入粘合剂造粒;将母粒通过压片处理后烧结得一氧化氮气敏材料,备用;清洗平面电极,将一氧化氮气敏材料作为靶托和清洗完的平面电极装入脉冲激光沉积设备腔体内,调节,沉积薄膜;待沉积结束后,取出样品封装处理,即可。利用本发明一氧化氮气敏材料制备的传感器可以在较低的温度下检测ppb级的一氧化氮,且半导体型NO传感器体积小,制造工艺简单。
Description
技术领域
本发明属于气体检测技术领域,具体涉及一氧化氮气敏材料及其在制备传感器上的应用。
背景技术
一氧化氮(NO)是汽车发动机排气和化石燃料发电厂产生的一种常见有毒气体,严重危害环境和人类健康。然而,NO不仅是化学工业中的重要中间体,还是人体中重要的信使分子和效应分子。此外,在一些生理和病理过程中作为一种生物标记气体,例如在肺病和哮喘的研究中,通常需要在家里或室外定时对病人进行监测。值得注意的是,这种类型的气体传感器通常需要有ppb级的NO分辨率。然而,在现有的快速诊断分析设备中,用于哮喘的传感器非常少,很多都还在试验阶段。所以,研发便携式、低成本、高灵敏度、高选择性的NO气体传感器迫在眉睫。
申请号2017112166961,名称为NO2化学电阻式气体传感器及其制备方法。该传感器包括自下而上依次设置的基底、绝缘层、表面修饰层、活性敏感层以及源漏电极,表面修饰层的材质为含端氨基的硅烷化合物,含端氨基的硅烷化合物的分子式为H2N-(CH2)n-SiCl3,H2N-(CH2)n-Si(OCH3)3或H2N-(CH2)n-Si(OC2H5)3,其中,n=3-18,活性敏感层的材质为有机半导体。本发明还提供了一种上述NO2化学电阻式气体传感器的制备方法:在基底表面形成平整的绝缘层,然后使含端氨基的硅烷化合物在绝缘层表面进行自组装,形成表面修饰层;在表面修饰层上沉积活性敏感层,在活性敏感层上沉积源漏电极,形成NO2化学电阻式气体传感器。虽然本发明是对NO2的检测,可应用于一氧化氮的检测,但最低检测限偏低,需要改进。
发明内容
本发明所要解决的技术问题在于克服现有一氧化氮传感器技术的不足,提供一氧化氮气敏材料及其在制备传感器上的应用,用一氧化氮气敏材料制备的传感器可以在较低的温度下检测ppb级别的一氧化氮,且半导体型NO传感器体积小,制造工艺简单。
为解决现有技术问题,本发明采取的技术方案为:
一氧化氮气敏材料,由In2O3和Nb2O5的WO3混合而成,所述In2O3和Nb2O5的WO3的质量比为1:1:98。
上述一氧化氮气敏材料在制备传感器上的应用。
作为改进的是,所述制备传感器步骤如下:
步骤1,按质量比为1:1:98称量In2O3,Nb2O5和WO3,混合后加入乙醇搅拌均匀,投入球磨机中磨碎得混合粉末;
步骤2,将混合粉末烘干后,加入粘合剂造粒;
步骤3,将母粒通过压片处理后,于600℃下烧结3小时,然后升温至900℃烧结6小时,得一氧化氮气敏材料,备用;
步骤4,清洗平面电极,将步骤3中一氧化氮气敏材料作为靶托和清洗完的平面电极装入脉冲激光沉积设备腔体内,调节,沉积薄膜,其中靶托与平面电极间距离为5.5cm;
步骤5,待沉积结束后,取出样品封装处理,即可。
作为改进的是,步骤1中加入乙醇量是10mL,球磨时间为24小时。
作为改进的是,步骤2中烘干温度为80℃,烘干时间4小时;粘合剂为质量分数为4%的聚乙烯醇,粘合剂的用量为0.5ml。
作为改进的是,步骤3中压片处理的压力为5Mpa,压制时间为5min,然后逐渐加压,在压力为10Mpa时压10min,压力为15Mpa时压10min,压力为20Mpa时压10min,最后压力为25Mpa时压30min成型。
作为改进的是,步骤3中升温速率为5℃/min。
作为改进的是,步骤4中清洗平面电极的步骤如下:用去离子水超声清洗5min;分别用丙酮和乙醇超声清洗10min;用去离子水超声清洗10min;洗完后用氮气枪吹干备用。
作为改进的是,步骤5中沉积过程中温度为250℃,氧压为10Pa,激光能量为400MJ,频率为10Hz,沉积时间为25min。
传感器工作原理如下:
当通入待测气体NO,会在气敏材料表面发生如下反应:
O2(ads) -+NO(g)→NO- (ads)+O2(g)
NO与WO3表面已吸附的氧离子接触,并与其发生氧化还原反应,导致其表面电子耗尽层厚度变化,使电导率发生变化。通过测定这时候的电阻Rg,然后与其在空气中的阻值Ra相比,即Rg/Ra。其比值就是响应。
有益效果:
与现有技术相比,本发明通过脉冲激光沉积制备的掺杂In2O3和Nb2O5的WO3一氧化氮气敏材料,且用此一氧化碳气敏材料制备的传感器可以在较低温度下检测ppb级别的NO,检测限在20ppb,并且具有较高的选择性。
附图说明
图1为本发明一氧化氮气敏材料制备的传感器在最佳工作温度70℃时对不同浓度NO的动态响应图;
图2为本发明一氧化氮气敏材料制备的传感器在最佳工作温度70℃时对各种气体的响应图。
具体实施方式
下面通过具体实施例对本发明作进一步详细介绍。
实施例1
一氧化氮气敏材料,由In2O3和Nb2O5的WO3混合而成,所述In2O3和Nb2O5的WO3的质量比为1:1:98,所述一氧化氮气敏材料通过脉冲激光沉积而成。
上述一氧化氮气敏材料在制备传感器上的应用。
上述应用,包括以下步骤:
步骤1,按质量比为1:1:98称量In2O3,Nb2O5和WO3,混合后加入10mL乙醇搅拌均匀,投入球磨机中球磨24小时得混合粉末;
步骤2,将混合粉末于80℃烘干4小时后,加入质量分数为4%的聚乙烯醇,粘合剂的用量为0.5ml造粒;
步骤3,将母粒通过压片处理后,在600℃煅烧3小时,升温至900℃烧结6小时,且升温效率为5℃/min,得一氧化氮气敏材料,备用,其中压片处理的压力为5Mpa,压制时间为5min,然后逐渐加压,在压力为10Mpa时压10min,压力为15Mpa时压10min,压力为20Mpa时压10min,最后压力为25Mpa时压30min成型;
步骤4,清洗平面电极,将步骤3中一氧化氮气敏材料作为靶托和清洗完的平面电极装入脉冲激光沉积设备腔体内,调节,沉积薄膜,其中靶托与平面电极间距离为5.5cm,清洗平面电极先用去离子水超声清洗5min;其次,用丙酮和乙醇超声清洗10min;第三,用去离子水超声清洗10min;最后用氮气枪吹干备用;
步骤5,待沉积结束后,取出样品封装处理得传感器,其中,沉积过程中温度为250℃,氧压为10Pa,激光能量为400MJ,频率为10Hz,沉积时间为25min。
将上述传感器在空气中240℃下老化7天,测试其性能。所得数据如图1-2所示图1为本发明制备的传感器在最佳工作温度70℃时对不同浓度NO的动态响应示意图,从图中可以看出该传感器可以分辨不同浓度的NO,且响应较好。
图2为是本发明制备的传感器在最佳工作温度70℃时对各种气体的响应结果图,从图中可以看出传感器对于100ppb的NO响应是56.1,测定浓度远小于除NO2外的其他气体,而响应却高了15倍以上,说明本发明的传感器有较好的选择性。
本发明通过脉冲激光沉积制备的掺杂In2O3和Nb2O5的WO3一氧化氮气敏材料,且用此一氧化碳气敏材料制备的传感器可以在较低温度下检测ppb级别的NO,检测限在20ppb,并且具有较高的选择性。
以上所述,仅为本发明较佳的具体实施方式,本发明的保护范围不限于此,任何熟悉本技术领域的技术人员在本发明披露的技术范围内,可显而易见地得到的技术方案的简单变化或等效替换均落入本发明的保护范围内。
Claims (9)
1.一氧化氮气敏材料,由In2O3和Nb2O5的WO3混合而成,所述In2O3和Nb2O5的WO3的质量比为1:1:98。
2.基于权利要求1所述的一氧化氮气敏材料在制备传感器上的应用。
3.根据权利要求2所述的应用,其特征在于,所述制备传感器的步骤如下:步骤1,按质量比为1:1:98称量In2O3,Nb2O5和WO3,混合后加入乙醇搅拌均匀,投入球磨机中磨碎得混合粉末;步骤2,将混合粉末烘干后,加入粘合剂造粒;步骤3,将母粒通过压片处理后,于600℃下烧结3小时,然后升温至900℃烧结6小时,得一氧化氮气敏材料,备用;步骤4,清洗平面电极,将步骤3中一氧化氮气敏材料作为靶托和清洗完的平面电极装入脉冲激光沉积设备腔体内,调节,沉积薄膜,其中靶托与平面电极间距离为5.5cm;步骤5,待沉积结束后,取出样品封装处理,即可。
4.根据权利要求3所述的应用,其特征在于,步骤1中加入乙醇量是10mL,球磨时间为24小时。
5.根据权利要求3所述的应用,其特征在于,步骤2中烘干温度为80℃,烘干时间4小时;粘合剂为质量分数为4%的聚乙烯醇,粘合剂的用量为0.5ml。
6.根据权利要求3所述的应用,其特征在于,步骤3中压片处理的压力为5Mpa,压制时间为5min,然后逐渐加压,在压力为10Mpa时压10min,压力为15Mpa时压10min, 压力为20Mpa时压10min,最后压力为25Mpa时压30min成型。
7.根据权利要求3所述的应用,其特征在于,步骤3中升温速率为5℃/min。
8.根据权利要求3所述的应用,其特征在于,步骤4中清洗平面电极的步骤如下:用去离子水超声清洗5min;分别用丙酮和乙醇超声清洗10min;用去离子水超声清洗10min;洗完后用氮气枪吹干备用。
9.根据权利要求3所述的应用,其特征在于,步骤5中沉积过程中温度为250℃,氧压为10Pa,激光能量为400MJ,频率为10Hz,沉积时间为25min。
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