CN114229885A - CdO/SnO2复合纳米立方体气敏材料、制备方法及其在氢气检测中的应用 - Google Patents
CdO/SnO2复合纳米立方体气敏材料、制备方法及其在氢气检测中的应用 Download PDFInfo
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Abstract
一种CdO/SnO2复合纳米立方体气敏材料、制备方法及其在氢气检测中的应用,属于气敏材料技术领域。本发明以四氯化锡水合物和二氯化镉水合物为原料,以氢氧化钠和碳酸钠混合溶液为沉淀剂,采用共沉淀合成法制备出一系列具有不同摩尔比的CdO/SnO2复合纳米立方体气敏材料。其中,以摩尔比为1:1的CdO/SnO2复合纳米立方体气敏材料制作的气体传感器表现出优异的氢气检测性能。在较低的工作温度(220℃)下,对氢气的响应表现出高灵敏度、高选择性,极短的响应‑恢复时间等优点,这十分有利于氢气泄露的早期预警。本发明所述气敏材料的制备方法,制备条件简单、合成周期短,原料成本低,易于实现规模化生产。
Description
技术领域
本发明属于气敏材料技术领域,具体涉及一种CdO/SnO2复合纳米立方体气敏材料、制备方法及其在氢气检测中的应用。
背景技术
作为一种清洁的能源载体,氢气被广泛用于氢燃料电池、新能源汽车、石油化工、冶金工业、航天航空、食品加工及电子等行业。绿色氢能源的快速发展也有助于“碳达峰”、“碳中和”的加速实现。但是,氢气无色无嗅,不易被人察觉,且氢气在空气中的***下限仅为4%,只需不到0.02毫焦的能量即可将其引燃。这意味着,氢气一旦出现泄露,极有可能造成重大的安全事故。然而,由于氢气分子体积小,在氢气的制备、储存、运输及使用的每一阶段都有发生泄露的可能,因此,开发高灵敏度、低检测限、响应-恢复快的氢气传感器对于氢气泄露的早期预警具有极为重要的意义。
SnO2是经典的气敏材料之一,但它的氢气传感性能尚不能满足氢气检测的要求。而构建SnO2和其他金属氧化物的异质结构,通过费米能级控制效应和不同组分间的协同作用有可能提高其传感性能。利用纳米颗粒的表面特性以及小尺寸效应,也可以有效改善传感材料的选择性、稳定性、灵敏度,减少响应-恢复时间。
共沉淀法是制备小尺寸纳米粉体材料的常用方法之一,该方法具有操作简单、条件温和、合成周期短以及适合批量生产的特点。目前,工业上仍然主要采用该方法合成小尺寸纳米粉体材料。因此,采用共沉淀法制备纳米尺度SnO2基异质结构的氢气传感材料具有重要的实际应用价值和现实意义。
在本发明中,我们制备了一种CdO/SnO2复合纳米立方体气敏材料。该材料不但制备工艺简单,易于大规模生产,还表现出优异的传感灵敏度、选择性和快速响应等特性,可以用于低浓度氢气的快速检测。
发明内容
本发明旨在提供一种CdO/SnO2复合纳米立方体气敏材料、制备方法及其在氢气检测中的应用。本发明以四氯化锡水合物和二氯化镉水合物作为金属原料,以氢氧化钠和碳酸钠混合溶液为沉淀剂,制备出一系列不同摩尔比的CdO/SnO2复合纳米立方体(80~100nm)气敏材料。该系列材料在检测氢气方面,具有检测限低、灵敏度高、选择性好以及响应-恢复时间短等优势,可用于氢气泄露的监测预警,并且具有合成条件简单、制备周期短、原料成本低以及易实现规模化生产等优点。
本发明所述的一种CdO/SnO2复合纳米立方体气敏材料的制备方法,其步骤如下:
(1)沉淀剂溶液的配制:将摩尔比为(0.25~1):1的碳酸钠(Na2CO3)和氢氧化钠(NaOH)加入到去离子水中溶解;
(2)金属盐混合溶液的配制:将摩尔比为1:(0.25~4)的四氯化锡(SnCl4·5H2O)和氯化镉(CdCl2·2.5H2O)加入到去离子水中溶解,室温搅拌至均匀;
(3)向步骤(2)配置的溶液中逐滴、缓慢加入步骤(1)配置的沉淀剂,待pH值为6~12时停止滴加,继续搅拌;
(4)待步骤(3)沉淀完全后,对反应产物进行离心分离、水洗3~5次,干燥后得到前驱体;
(5)将步骤(4)得到的前驱体置于马弗炉中烧结,即可得到本发明所述CdO/SnO2复合纳米立方体气敏材料。
上述方法中,步骤(1)去离子水中,氢氧化钠(NaOH)的浓度为0.5~2mol/L;
上述方法中,步骤(2)去离子水中,四氯化锡(SnCl4·5H2O)的浓度为0.005~0.05mol/L;
上述方法中,步骤(3)的继续搅拌时间为1~10小时。
上述方法中,步骤(4)的干燥温度为60~80℃,干燥时间为5~12小时。
上述方法中,步骤(5)的烧结温度为300~500℃,升温速率为2~5℃/min,烧结时间为1~3小时。
气体传感器由外表面带有两条平行、环状且彼此分立金电极的Al2O3陶瓷管、涂覆在Al2O3陶瓷管外表面和金电极上的CdO/SnO2复合纳米立方体气敏材料(气敏材料的厚度为20μm)、置于Al2O3陶瓷管内的镍铬加热线圈(阻值30Ω)组成;在每条金电极上引出两条铂丝,在镍铬加热线圈的两端引出两条铂丝,镍铬合金加热丝作为发热体以控制传感器工作温度,Al2O3陶瓷管通过六条铂丝焊接在六角形底座上。
本发明的优点如下:
1、本发明所述一种CdO/SnO2复合纳米立方体气敏材料,制备方法简单、合成条件易实现、合成周期短、原料成本低,并且易于实现规模化生产。
2、本发明所述一种CdO/SnO2复合纳米立方体气敏材料,利用了纳米粒子的特性,从尺寸效应出发提高了氢气检测的传感性能。
3、本发明所述一种CdO/SnO2复合纳米立方体气敏材料,通过构建异质结构,实现对电子结构的调节,以提高氢气检测的传感性能。
4、本发明所述一种CdO/SnO2复合纳米立方体气敏材料在检测氢气方面,具有检测灵敏度高、响应-恢复速度快等优点。这极大有助于对氢气的快速检测和及时预警,为氢气的安全使用提供了保证。
附图说明
图1:一系列不同摩尔比的CdO/SnO2复合纳米立方体气敏材料以及CdO、SnO2纯相的粉末X射线衍射(XRD)图谱及其标准XRD卡片。
图2:实施例1所得CdO/SnO2(摩尔比1:1)复合纳米立方体气敏材料的扫描电子显微镜(SEM)照片,颗粒尺寸在80~100nm。
图3:实施例2所得CdO/SnO2(摩尔比2:1)复合纳米立方体气敏材料的扫描电子显微镜(SEM)照片,颗粒尺寸在80~100nm。
图4:实施例3所得CdO/SnO2(摩尔比1:2)复合纳米立方体气敏材料的扫描电子显微镜(SEM)照片,颗粒尺寸在80~100nm。
图5(A):实施例1所得CdO/SnO2复合纳米立方体气敏材料对500ppm氢气的响应-恢复曲线。在220℃的工作温度下,响应值为19,响应、恢复时间均小于5s。
图5(B):实施例1所得CdO/SnO2复合纳米立方体气敏材料对10ppm氢气的响应-恢复曲线。在220℃的工作温度下,响应值为2.6,这说明其检测下限较低,可有效监测氢气的泄露。响应值为气体传感器在空气气氛下的两金电极间电阻(Ra)和待测气氛下两金电极间电阻(Rg)之比(S=Ra/Rg)。
图6:实施例1所得CdO/SnO2复合纳米立方体气敏材料对500ppm不同气体的响应值柱状图。在220℃的工作温度下,该材料对一氧化碳、二氧化碳、甲烷、乙烷、丙烷、乙烯等气体基本不响应,说明它对氢气具有优异的专一性响应。
具体实施方式
下面通过实施例对本发明作进一步说明,但本发明的保护范围不限于下述实施例。本领域技术人员清楚,在不偏离本发明主旨和范围的情况下可以对本发明做出变化或调整,这些变化或调整也纳入本发明的保护范围内。
实施例1:摩尔比为1:1的CdO/SnO2复合纳米立方体气敏材料的制备。
(1)称取4g氢氧化钠(NaOH)和5.3g碳酸钠(Na2CO3),摩尔比为2:1,溶解于100mL去离子水中,配置成氢氧化钠(NaOH)浓度为1mol/L,碳酸钠(Na2CO3)浓度为0.5mol/L混合溶液,作为沉淀剂;
(2)称取0.1461g五水合四氯化锡(SnCl4·5H2O)和0.0951g二点五水合氯化镉(CdCl2·2.5H2O),摩尔比为1:1,溶解于50mL去离子水中,配置成五水合四氯化锡(SnCl4·5H2O)浓度为0.0167mol/L,二点五水合氯化镉(CdCl2·2.5H2O)浓度为0.0167mol/L混合溶液,室温搅拌至均匀;
(3)向步骤(2)配置的溶液中逐滴、缓慢加入步骤(1)所配置的沉淀剂,待pH值为11时停止滴加,继续搅拌5小时;
(4)待沉淀完全后,对反应产物进行离心分离、水洗三次,然后将反应产物置于80℃干燥箱中干燥12小时;
(5)将步骤(4)干燥后得到的前驱体置于马弗炉中,以3℃/min的速率升温至400℃烧结2小时,最终得到本发明所述的一种用于快速检测氢气的气敏材料,该材料为摩尔比为1:1的CdO/SnO2复合纳米立方体。
实施例2:摩尔比为2:1的CdO/SnO2复合纳米立方体气敏材料的制备。
(1)称取4g氢氧化钠(NaOH)和5.3g碳酸钠(Na2CO3),摩尔比为2:1,溶解于100mL去离子水中,配置成氢氧化钠(NaOH)浓度为1mol/L,碳酸钠(Na2CO3)浓度为0.5mol/L混合溶液,作为沉淀剂;
(2)称取0.1268g二点五水合氯化镉(CdCl2·2.5H2O)和0.0974g五水合四氯化锡(SnCl4·5H2O),摩尔比为2:1,溶解于50mL去离子水中,配置成五水合四氯化锡(SnCl4·5H2O)浓度为0.0056mol/L,二点五水合氯化镉(CdCl2·2.5H2O)浓度为0.0111mol/L混合溶液,室温搅拌至均匀;
(3)向步骤(2)配置的溶液中逐滴、缓慢加入步骤(1)所配置的沉淀剂,待pH值为11时停止滴加,继续搅拌5小时;
(4)待沉淀完全后,对反应产物进行离心分离、水洗三次,然后将反应产物置于80℃干燥箱中干燥12小时;
(5)将步骤(4)干燥后得到的前驱体置于马弗炉中,以3℃/min的速率升温至400℃烧结2小时,最终得到本发明所述的一种用于快速检测氢气的气敏材料,该材料为摩尔比为2:1的CdO/SnO2复合纳米立方体。
实施例3:摩尔比为1:2的CdO/SnO2复合纳米立方体气敏材料的制备。
(1)称取4g氢氧化钠(NaOH)和5.3g碳酸钠(Na2CO3),摩尔比为2:1,溶解于100mL去离子水中,配置成氢氧化钠(NaOH)浓度为1mol/L,碳酸钠(Na2CO3)浓度为0.5mol/L混合溶液,作为沉淀剂;
(2)称取0.0634g二点五水合氯化镉(CdCl2·2.5H2O)和0.1948g五水合四氯化锡(SnCl4·5H2O),摩尔比为1:2,溶解于50mL去离子水中,配置成五水合四氯化锡(SnCl4·5H2O)浓度为0.0111mol/L,二点五水合氯化镉(CdCl2·2.5H2O)浓度为0.0056mol/L混合溶液,室温搅拌至均匀;
(3)向步骤(2)配置的溶液中逐滴、缓慢加入步骤(1)所配置的沉淀剂,待pH值为11时停止滴加,继续搅拌5小时;
(4)待沉淀完全后,对反应产物进行离心分离、水洗三次,然后将反应产物置于80℃干燥箱中干燥12小时;
(5)将步骤(4)干燥后得到的前驱体置于马弗炉中,以3℃/min的速率升温至400℃烧结2小时,最终得到本发明所述的一种用于快速检测氢气的气敏材料,该材料为摩尔比为1:2的CdO/SnO2复合纳米立方体。
Claims (8)
1.一种CdO/SnO2复合纳米立方体气敏材料的制备方法,其步骤如下:
(1)沉淀剂溶液的配制:将摩尔比为(0.25~1):1的碳酸钠和氢氧化钠加入到去离子水中溶解;
(2)金属盐混合溶液的配制:将摩尔比为1:(0.25~4)的四氯化锡和氯化镉加入到去离子水中溶解,室温搅拌至均匀;
(3)向步骤(2)配置的溶液中逐滴、缓慢加入步骤(1)配置的沉淀剂,待pH值为6~12时停止滴加,继续搅拌;
(4)待步骤(3)沉淀完全后,对反应产物进行离心分离、水洗3~5次,干燥后得到前驱体;
(5)将步骤(4)得到的前驱体进行烧结,即得到CdO/SnO2复合纳米立方体气敏材料。
2.如权利要求1所述的一种CdO/SnO2复合纳米立方体气敏材料的制备方法,其特征在于:步骤(1)去离子水中,氢氧化钠的浓度为0.5~2mol/L。
3.如权利要求1所述的一种CdO/SnO2复合纳米立方体气敏材料的制备方法,其特征在于:步骤(2)去离子水中,四氯化锡的浓度为0.005~0.05mol/L。
4.如权利要求1所述的一种CdO/SnO2复合纳米立方体气敏材料的制备方法,其特征在于:步骤(3)的继续搅拌时间为1~10小时。
5.如权利要求1所述的一种CdO/SnO2复合纳米立方体气敏材料的制备方法,其特征在于:步骤(4)的干燥温度为60~80℃,干燥时间为5~12小时。
6.如权利要求1所述的一种CdO/SnO2复合纳米立方体气敏材料的制备方法,其特征在于:步骤(5)的烧结温度为300~500℃,升温速率为2~5℃/min,烧结时间为1~3小时。
7.一种CdO/SnO2复合纳米立方体气敏材料,其特征在于:是由权利要求1~6任何一项所述的方法制备得到。
8.权利要求7所述的一种CdO/SnO2复合纳米立方体气敏材料在氢气检测中的应用。
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