CN113092544B - 级次结构氧化铋材料在气体检测中的应用 - Google Patents
级次结构氧化铋材料在气体检测中的应用 Download PDFInfo
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Abstract
本发明属于纳米材料应用技术领域,具体涉及一种级次结构氧化铋材料在气体检测中的应用,用于检测环境中的低浓度氨气的含量;所述级次结构氧化铋材料的整体呈现微球形貌,微球直径为1~3μm,由厚度为10~80nm的片层结构单元自组装而成;将氧化铋材料制成气体传感器敏感元件,在室温条件下对氨气具有高的灵敏度和选择性,适用于检测环境中微量有害气体;氧化铋作为气敏材料制成的气体传感器在使用时无需加热,省去了常规的气体传感器加热步骤,可直接放置在常温环境下操作;其应用方法简单,易操作,效率高,应用前景广阔。
Description
技术领域:
本发明属于纳米材料应用技术领域,具体涉及一种级次结构氧化铋材料在气体检测中的应用,将氧化铋用作半导体气体传感器的敏感材料,实现了环境中低浓度氨气的高灵敏度和高选择性检测。
背景技术:
氧化铋是一种重要的金属氧化物,其禁带宽度为2.85eV,具有较高的光导性和热导性,被广泛应用于光电器件、高温超导、催化剂和电子陶瓷等领域。近年来,人们对纳米氧化铋进行了广泛的研究,并取得了一些重要进展。例如,中国专利CN201510477953.1公开了一种微纳结构氧化铋材料及其制备方法,方法为将可溶性铋盐溶于乙醇/乙二醇溶剂中,得到可溶性铋盐溶液,之后将可溶性铋盐溶液密闭反应,再对反应液依次进行固液分离、洗涤和干燥处理,制得目的产物;得到的材料具有非化学计量,分子式为Bi2O2.33,非化学计量氧化铋纳米片的片厚为5~10nm,比表面积≥26.6m2/g;这种非化学计量Bi2O2.33对I-和IO3-离子均有吸附能力,可广泛地应用于对水环境中放射性碘的高效能吸附;中国专利申请CN202010381159.8公开了一种掺杂氧化铋颗粒的制备方法,包括如下步骤:按照Bi和A的摩尔比为5:1~2,将可溶性铋盐和可溶性A盐溶解在pH为1~6的酸性液体中,得到混合溶液;将所述混合溶液搅拌至所述混合溶液形成溶胶,接着加热使得所述溶胶转化为凝胶,并且将所述凝胶烘干得到前体;将所述前体在300℃~800℃的温度下烧结,得到所需的掺杂氧化铋颗粒,制得的掺杂氧化铋颗粒的一致性好,并且掺杂氧化铋颗粒中的α-Bi2O3转化为δ-Bi2O3,从而具有较佳的电学性能。
在半导体传感器中,金属氧化物的表面电导率通过其表面吸附还原性或氧化性气体而改变,从而实现对气体的检测。常见的金属氧化物气敏材料有二氧化锡、氧化锌和三氧化钨等,具有高的电子迁移率。而氧化铋电子迁移率较低,使得其在气体传感器领域受到了很大的局限。目前尚未有将氧化铋材料用于低功耗气体检测的报道。
发明内容:
本发明的目的在于克服现有技术的缺点,提供一种级次结构氧化铋材料在气体检测中的应用,将级次结构氧化铋材料用作半导体气体传感器的敏感元件,检测环境中氨气的含量。
为了达到上述目的,本发明提供了一种级次结构氧化铋材料在气体检测中的应用,采用级次结构氧化铋作为气体传感器的敏感材料,用于检测氨气。
进一步的,能够在常温环境下进行低浓度氨气的快速检测。
进一步的,所述气体传感器,能够在弯曲状态下操作。
进一步的,采用级次结构氧化铋制成的柔性气体传感器,在室温操作温度下对20ppm氨气的灵敏度最高达到1296。
进一步的,所述级次结构氧化铋材料由简单水热法制备而成,材料整体呈现微球形貌,微球直径为1~3μm,由厚度为10~80nm的片层结构单元组装而成。
本发明与现有技术相比,首次发现了氧化铋能够应用于环境中有害气体的检测,将氧化铋材料制成气体传感器敏感元件,在室温条件下对氨气具有高的灵敏度和选择性,适用于检测环境中微量有害气体;氧化铋作为气敏材料制成的传感器在使用时无需加热,省去了常规的气体传感器加热步骤,可直接放置在常温环境下操作;其应用方法简单,易操作,效率高,应用前景广阔。
附图说明:
图1为本发明涉及的实施例1制备的级次结构氧化铋材料的低倍SEM图。
图2为本发明涉及的实施例1制备的级次结构氧化铋材料的高倍SEM图。
图3为本发明涉及的实施例3焙烧后的氧化铋粉体的XRD谱图。
图4为本发明涉及的实施例3制备的气体传感器对20ppm氨气的响应恢复曲线。
图5为本发明涉及的实施例3制备的气体传感器对20ppm不同挥发性有机物的灵敏度数据分析图。
图6为本发明涉及的实施例3制备的气体传感器在不同弯曲角度下对20ppm氨气的灵敏度数据分析图。
图7为本发明涉及的实施例3制备的气体传感器在不同湿度下对20ppm氨气的灵敏度数据分析图。
图8为本发明涉及的实施例3制备的气体传感器响应与氨气浓度之间的关系图。
图9为本发明涉及的实施例3制备的柔性气体传感器的整体结构示意图。
具体实施方式:
下面通过具体实施例并结合附图对本发明作进一步说明。
实施例1:
本实施例涉及级次结构氧化铋材料的制备方法,具体步骤如下:
将34mL乙醇(C2H6O)与17mL乙二醇(C2H6O2)混合,然后加入0.97g五水合硝酸铋(Bi(NO3)3·5H2O),室温搅拌混合60min,然后将溶液转移到聚四氟乙烯内衬的不锈钢高压釜中,在160℃下反应5小时;反应结束后,离心,收集白色沉淀,将沉淀用乙醇洗涤,60℃干燥24h,得到氧化铋粉体。
对得到的产物进行如下表征:
用扫描电子显微镜(SEM)观察合成氧化铋的表面形貌,如图1和图2,由图可见,得到的产物是由厚度为10~80nm的片层结构单元自组装而成的直径为1~3μm的氧化铋微球。
用X-射线粉末衍射(XRD)表征合成氧化铋的物相结构和晶型,结果见图3,各特征峰与粉末衍射标准联合委员会标准卡片PDF#71-2274基本一致,其主要晶面间距d值(单位:埃)3.4564、3.3112、3.2532、3.1830、2.7097、2.6918分别对应于单斜氧化铋的(002)、(111)、(012)、(202)、(121)、(200)晶面,从图3中没有观察到杂质峰,证明得到的产物为结晶度高的单斜氧化铋。
实施例2:
本实施例涉及级次结构氧化铋材料的制备方法,具体步骤如下:
将0.5g五水合硝酸铋(Bi(NO3)3·5H2O)溶解在10mL乙二醇中,得到透明溶液,然后滴加20mL无水乙醇,室温搅拌混合60min。然后将溶液转移到聚四氟乙烯内衬的不锈钢高压釜中,在150℃下反应8小时。反应结束后,将离心收集所得的白色沉淀用乙醇洗涤,60℃干燥,得到氧化铋粉体。
实施例3:
本实施例为级次结构氧化铋材料在气体检测中的应用试验,将氧化铋作为气敏层制作气体传感器后置于气敏测试系统中进行气体灵敏度和选择性的检测,具体步骤为:
1、制备气体传感器:气体传感器由基底层1、电极层2、气敏层3和封装层4构成,所述基底层1为陶瓷片、无纺布或纸片;电极层2为叉指电极或横向结构电极;所述气敏层3为简单水热法制备的级次结构氧化铋,组成级次氧化铋微球的片层厚度在10~80nm之间;所述封装层4为沸石多孔膜;气体传感器的制备步骤为:在纸片基底上通过丝网印刷方法制作叉指电极,得纸基叉指电极;然后通过刮涂、旋涂或丝网印刷的方法涂覆气敏材料,具体为将实施例1或实施例2制得的氧化铋粉末置于马弗炉中,以5~10℃/min速度升温,在200~500℃下保持1~2h,得到焙烧后的氧化铋粉体,与松油醇充分混合后旋涂在纸基叉指电极上,烘干1~6h;之后涂覆沸石多孔膜,老化24h,得到柔性气体传感器。
2、气体检测:将制作好的气体传感器置于气敏测试系统中,通入空气或待测气体,恒定工作电压3V,工作温度22~30℃。分别测其在空气中和待测气体中的电流值,经过计算得到灵敏度。由图4可见,氧化铋粉体制成的柔性气体传感器敏感元件,在室温操作温度下对20ppm氨气的灵敏度最高达到1296,响应时间为20秒,恢复时间为7秒。同时测得该气体传感器对相同浓度甲苯、甲醇、乙醇、异丙醇、丙酮、三乙胺的灵敏度均低于11(图5),说明该气敏元件对环境中其他挥发性有机物的抗干扰能力强,有较好的选择性,适于检测环境中的氨气。这是由于级次结构氧化铋微球具有独特的多孔结构,提供了大量的气体通道,有利于氨气在材料表面的吸附,提高了检测灵敏度,有利于在室温下进行。由图6可见,该气体传感器在弯曲状态下的灵敏度变化很小,说明该方法可以进行柔性场景下的室温气体检测。由图7可见,该气体传感器的灵敏度随湿度增加小幅下降,下降趋势呈现线性关系,表明湿度对传感器的影响较小,而且可以通过线性校正加以补偿调节。如图8所示,在5ppm到100ppm测试范围内,该气体传感器的灵敏度与氨气浓度的变化呈线性关系。根据公式:
计算得到传感器的检测下限可达1.6ppm。
Claims (5)
1.一种级次结构氧化铋材料在气体检测中的应用,其特征在于:采用级次结构氧化铋作为气体传感器的敏感材料,用于检测氨气;所述级次结构氧化铋材料整体呈现微球形貌,由片层结构单元组装而成。
2.根据权利要求1所述的级次结构氧化铋材料在气体检测中的应用,其特征在于:能够在常温环境下对浓度1~100ppm的氨气进行快速检测。
3.根据权利要求1所述的级次结构氧化铋材料在气体检测中的应用,其特征在于:所述气体传感器,能够在弯曲状态下操作。
4.根据权利要求1所述的级次结构氧化铋材料在气体检测中的应用,其特征在于:采用级次结构氧化铋制成的柔性气体传感器,在室温操作温度下对20ppm氨气的灵敏度最高达到1296。
5.根据权利要求1所述的级次结构氧化铋材料在气体检测中的应用,其特征在于:所述级次结构氧化铋材料由简单水热法制备而成,所述微球直径为1~3μm,由厚度为10~80nm的片层结构单元组装而成。
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