WO2023060742A1 - 支化纳米线结构的气敏纳米材料、制备方法及其应用 - Google Patents

支化纳米线结构的气敏纳米材料、制备方法及其应用 Download PDF

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WO2023060742A1
WO2023060742A1 PCT/CN2021/137495 CN2021137495W WO2023060742A1 WO 2023060742 A1 WO2023060742 A1 WO 2023060742A1 CN 2021137495 W CN2021137495 W CN 2021137495W WO 2023060742 A1 WO2023060742 A1 WO 2023060742A1
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nanowires
gas
branched
niobium
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卢红亮
吴滔滔
朱立远
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光华临港工程应用技术研发(上海)有限公司
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
    • G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
    • G01N27/12—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of a solid body in dependence upon absorption of a fluid; of a solid body in dependence upon reaction with a fluid, for detecting components in the fluid
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    • G01N27/127—Composition of the body, e.g. the composition of its sensitive layer comprising nanoparticles

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  • the invention relates to the technical field of semiconductor nanomaterial preparation, in particular to a gas-sensitive nanomaterial with a branched nanowire structure, a preparation method and an application thereof.
  • resistive gas sensors based on semiconductor nanomaterials have received great attention and have been widely used in various fields such as gas leak alarm, environmental gas monitoring, and industrial gas analysis.
  • the development of various new gas sensors based on metal oxide semiconductor materials with high specific surface area, excellent gas adsorption capacity and high carrier mobility has become a current research hotspot.
  • the technical problem to be solved by the present invention is to provide a gas-sensing nanomaterial with a branched nanowire structure with better gas adsorption capacity and high carrier mobility, a preparation method and its application.
  • the present invention provides a method for preparing a gas-sensitive nanomaterial with a branched nanowire structure, which includes the following steps: providing a solution of NH 4 F; placing metal niobium sheets in the solution to grow nanowires, and Nb 2 O 5 nanowires are grown on the surface of niobium sheets; ZnO shell film is prepared on the surface of niobium sheets with Nb 2 O 5 nanowires grown by atomic layer deposition technology; Zn(NO 3 ) 2 of 6.25 ⁇ 25mM and 6.25 ⁇ A mixed solution of 25mM HMT; the niobium sheets coated with ZnO and Nb 2 O 5 nanowires on the surface were placed in the mixed solution, and ZnO branched nanowires were grown on the surface; branched Nb 2 O 5 -ZnO Transfer and disperse the nanowires from the niobium sheet substrate to deionized water to obtain Nb 2 O 5 -ZnO branched nanowire
  • the invention provides a gas-sensing nano material based on the Nb 2 O 5 -ZnO core-shell branched nano wire structure prepared by the above preparation method.
  • the present invention provides an application of the gas-sensing nano-material based on the Nb 2 O 5 -ZnO core-shell branched nano-wire structure in detecting hydrogen sulfide gas.
  • niobium pentoxide (Nb 2 O 5 ) is an important n-type oxide wide bandgap (about 3.4eV) semiconductor with good conductivity and high concentration of oxygen Vacancies are good for trapping electrons, so excellent sensors based on Nb 2 O 5 are worthy of research.
  • Gas sensors based on a single niobium oxide material have relatively poor gas sensing performance.
  • the preparation of composite structural materials has attracted extensive research interest and is generally considered to be an effective approach to improve the performance of gas sensors.
  • Constructing a core-shell heterostructure composed of two or more semiconductor materials can not only produce a synergistic effect of various properties of various materials, but also increase the additional consumption due to the electron trapping of interface states and the formation of heterojunctions. Variations in width and interfacial barrier, resulting in a larger sensor response than pristine nanostructures.
  • the construction of hierarchical structures, such as branched nanowires is conducive to the increase of specific surface area and the formation of more heterojunctions or homojunctions at the interface between multilevel nanostructures, further enhancing the sensor response.
  • step S10 providing a solution of NH 4 F
  • step S11 placing metal niobium sheets in the solution to grow nanowires, and growing nanowires on the surface of niobium sheets Nb 2 O 5 nanowires are grown
  • step S12 using atomic layer deposition technology to prepare a ZnO shell film on the surface of the niobium sheet with Nb 2 O 5 nanowires grown
  • Step S13 providing 6.25-25mM Zn(NO 3 ) 2 and a mixed solution of HMT of 6.25-25mM
  • step S14 placing the niobium sheet coated with ZnO and Nb2O5 nanowires on the surface in the mixed solution, and branching and growing ZnO branched nanowires on the surface
  • step S15 Transfer and disperse the Nb 2 O 5 -ZnO branched nanowires from the niobium substrate into deionized water to obtain
  • the concentration of NH 4 F in the NH 4 F solution is 0.03 ⁇ 0.06 mol/L.
  • the metal niobium sheets are multiple sheets, which are placed in parallel in the NH 4 F solution.
  • step S11 further include the step of cleaning the metal niobium sheet, specifically the step of cleaning with absolute ethanol and deionized water in sequence, after ultrasonic cleaning for 10-15 minutes, and drying with nitrogen.
  • the length of the Nb 2 O 5 nanowires is 700-1100 nm, and the diameter is 40-60 nm.
  • step S13 a mixed solution of 6.25-25 mM Zn(NO 3 ) 2 and 6.25-25 mM HMT is provided, and the mixing ratio is 1:1 by volume.
  • the ZnO branched nanowires are further ultrasonically separated from the niobium sheet substrate and uniformly dispersed in deionized water.
  • the ZnO branched nanowires have a length of 80-150nm and a diameter of 15-40nm.
  • the step of the gas-sensitive nanomaterial in step S16 is further to drop the obtained suspension with a mass volume ratio of 1 to 5 mg/ml on a standard cleaned quartz substrate, and place it in the air at a temperature of 50 to 80 ° C. Bake until completely dry; naturally cool to room temperature to obtain a niobium oxide/zinc oxide core-shell branched nanowire structure gas-sensing nanomaterial.
  • the Nb 2 O 5 -ZnO core-shell branched nanowire structure based on the above technical solution is a gas-sensitive nano-material, which has application properties in the detection of hydrogen sulfide gas.
  • a preparation process of a gas-sensitive nanomaterial based on an n-n junction niobium oxide/zinc oxide core-shell branched nanowire structure comprises the following steps:
  • a preparation process of a gas-sensitive nanomaterial based on an n-n junction niobium oxide/zinc oxide core-shell branched nanowire structure comprises the following steps:
  • the obtained niobium oxide/zinc oxide core-shell branched nanowires are used for gas sensing test of 10-4ppm hydrogen sulfide gas.
  • the sensitivity defined as responsivity-1
  • the sensitivity of Nb2O5 - ZnO (branched) nanowires is 1.25
  • that of pure Nb2O5 nanowires is 1.06
  • Nb2O5 -ZnO (unbranched) nanowires have a sensitivity of 1.19
  • the core-shell branched nanowire structure of the present invention increases the sensing sensitivity to 10ppm hydrogen sulfide gas by 18% compared with pure Nb 2 O 5 nanowires, which is comparable to Compared with Nb 2 O 5 -ZnO (unbranched) nanowires, the sensitivity is improved by 5%, and the sensitivity to hydrogen sulfide gas at other concentrations is also improved to varying degrees.
  • the comparison test results of the gas sensitivity is improved by 5%
  • niobium pentoxide (Nb 2 O 5 ) is an important n-type oxide wide bandgap (about 3.4eV) semiconductor with good The conductivity and high concentration of oxygen vacancies are beneficial to capture electrons, so excellent sensors based on Nb 2 O 5 are worthy of investigation.
  • Gas sensors based on a single niobium oxide material have relatively poor gas sensing performance.
  • the preparation of composite structural materials has attracted extensive research interest and is generally considered to be an effective approach to improve the performance of gas sensors.
  • Constructing a core-shell heterostructure composed of two or more semiconductor materials can not only produce a synergistic effect of various properties of various materials, but also increase the additional consumption due to the electron trapping of interface states and the formation of heterojunctions. Variations in width and interfacial barrier, resulting in a larger sensor response than pristine nanostructures.
  • the construction of hierarchical structures, such as branched nanowires is conducive to the increase of specific surface area and the formation of more heterojunctions or homojunctions at the interface between multilevel nanostructures, further enhancing the sensor response.

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Abstract

一种支化纳米线结构的气敏纳米材料的制备方法，包括如下步骤：提供NH4F的溶液(S10)；将金属铌片置于溶液中进行纳米线生长，在铌片表面生长出Nb 2O 5纳米线(S11)；采用原子层沉积技术在生长有Nb 2O 5纳米线的铌片表面制备ZnO壳层薄膜(S12)；提供6.25～25mM的Zn(NO 3) 2和6.25～25mM的HMT的混合溶液(S13)；将表面包覆ZnO和Nb 2O 5纳米线的铌片放置于混合溶液中，在其表面支化生长出ZnO支化纳米线(S14)；将Nb 2O 5-ZnO支化纳米线从铌片衬底上转移分散至去离子水中，获得Nb 2O 5-ZnO支化纳米线悬浮液(S15)；再将得到的悬浮液滴石英片衬底上，干燥并冷却后得到Nb 2O 5-ZnO支化纳米线结构的气敏纳米材料(S16)。

Description

支化纳米线结构的气敏纳米材料、制备方法及其应用 技术领域
本发明涉及半导体纳米材料制备技术领域，尤其涉及一种支化纳米线结构的气敏纳米材料、制备方法及其应用。
背景技术
近年来，基于半导体纳米材料的电阻式气体传感器受到了极大的关注，已经广泛应用于气体泄漏警报、环境气体监测和工业气体分析等各个领域。研发各种拥有高比表面积、优异的气体吸附能力和高载流子迁移率的基于金属氧化物半导体材料的新型气体传感器已成为当前的研究热点。
发明内容
本发明所要解决的技术问题是，提供一种具有更好气体吸附能力和高载流子迁移率的支化纳米线结构的气敏纳米材料、制备方法及其应用。
为了解决上述问题，本发明提供了一种支化纳米线结构的气敏纳米材料的制备方法，包括如下步骤：提供NH 4F的溶液；将金属铌片置于溶液中进行纳米线生长，在铌片表面生长出Nb 2O 5纳米线；采用原子层沉积技术在生长有Nb 2O 5纳米线的铌片表面制备ZnO壳层薄膜；提供6.25～25mM的Zn(NO 3) 2和6.25～25mM的HMT的混合溶液；将表面包覆ZnO和Nb 2O 5纳米线的铌片放置于混合溶液中，在其表面支化生长出ZnO支化纳米线；将Nb 2O 5-ZnO支化纳米线从铌片衬底上转移分散至去离子水中，获得Nb 2O 5-ZnO支化纳米线悬浮液；再将得到的悬浮液滴石英片衬底上，干燥并冷却后得到Nb 2O 5-ZnO支化纳米线结构的气敏纳米材料。
本发明提供了一种上述的制备方法制得的基于Nb 2O 5-ZnO核壳支化纳米线结构的气敏纳米材料。
本发明提供了一种上述的基于Nb 2O 5-ZnO核壳支化纳米线结构的气敏纳米材料在检测硫化氢气体方面的应用。
在各种金属氧化物半导体材料中，五氧化二铌(Nb 2O 5)是一种重要的n型氧化物宽禁带(约为3.4eV)半导体，具有良好的导电性和高浓度的氧空位，利于捕获电子，因此基于Nb 2O 5的优良传感器是值得研究的。基于单一氧化铌材料的气体传感器其气敏性能相对较差。由此，复合结构材料的制备引起了广泛的研究兴趣，被普遍认为是一种提高气体传感器性能的有效方法。构建由两种或多种半导体材料组成的核壳异质结构，不仅能产生各种材料的多种特性的协同效应，而且由于界面态的电子俘获和异质结的形成，增加了额外的耗尽宽度和界面势垒的变化，由此带来比原始纳米结构更大的传感器响应。此外，层次结构的构建，如分枝状的纳米线，有利于比表面积的增加和在多级纳米结构之间的界面上形成更多的异质结或同质结，进一步提升传感器响应。
附图说明
附图1所示是本具体实施方式所述方法的实施步骤示意图。
附图2所示为实施例一中Nb 2O 5纳米线的扫描电镜形貌图。
附图3所示为实施例一中ZnO壳层薄膜的扫描电镜形貌图。
附图4所示为实施例一中ZnO纳米线的扫描电镜形貌图。
附图5所示为实施例二中ZnO纳米线的扫描电镜形貌图。
附图6所示为采用本具体实施方式所述技术方案进行不同材料的气体灵敏度的对比测试结果。
具体实施方式
下面结合附图对本发明提供的支化纳米线结构的气敏纳米材料、制备方法及其应用的具体实施方式做详细说明。
附图1所示是本具体实施方式所述方法的实施步骤示意图，包括：步骤S10，提供NH 4F的溶液；步骤S11，将金属铌片置于溶液中进行纳米线生长，在铌片表面生长出Nb 2O 5纳米线；步骤S12，采用原子层沉积技术在生长有Nb 2O 5纳米线的铌片表面制备ZnO壳层薄膜；步骤S13，提供6.25～25mM的Zn(NO 3) 2和6.25～25mM的HMT的混合溶液；步骤S14，将表面包覆ZnO和Nb 2O 5纳米线的铌片放置于混合溶液中，在其表面支化生长出ZnO支化纳米线；步骤S15，将Nb 2O 5-ZnO支化纳米线从铌片衬底上转移分散至去离子水中，获得Nb 2O 5-ZnO支化纳米线悬浮液；步骤S16，将得到的悬浮液滴石英片衬底上，干燥并冷却后得到Nb 2O 5-ZnO支化纳米线结构的气敏纳米材料。
具体的说，在上述步骤S10中，NH 4F的溶液中NH 4F的浓度为0.03～0.06mol/L。步骤S11中，所述金属铌片为多片，平行放置于NH 4F的溶液中。步骤S11之前，进一步包括清洗金属铌片的步骤，具体是依次用无水乙醇和去离子水清洗各超声清洗10～15min后，用氮气吹干的步骤。步骤S11中Nb 2O 5纳米线的长度为700～1100nm，直径为40～60nm。
在步骤S13中，提供6.25～25mM的Zn(NO 3) 2和6.25～25mM的HMT的混合溶液，其混合比例为体积比1：1。
步骤S15的获得悬浮液的步骤，进一步使将ZnO支化纳米线从铌片衬底上超声分离，均匀分散在去离子水中。ZnO支化纳米线的长度为80～150nm，直径为15～40nm。
步骤S16的所述气敏纳米材料的步骤，进一步是将得到的质量体积比为1～5mg/ml的悬浮液滴在标准清洗过的石英片衬底上，空气中50～80℃的温度下烘烤直至完全干燥；自然冷却至室温，得到氧化铌/氧化锌核壳支化纳米线结构的气敏纳米材料。
上述技术方案的到的基于Nb 2O 5-ZnO核壳支化纳米线结构是一种气敏纳米材料，具有在检测硫化氢气体方面的应用性质。
以下给出上述技术方案的两个实施例。
实施例1
一种基于n-n结氧化铌/氧化锌核壳支化纳米线结构的气敏纳米材料的制备工艺包括以下步骤：
(1)取一块大小为2.0cm×2.0cm的金属铌片作为衬底和源材料，依次浸泡于无水乙醇和去离子水中各超声清洗10min，室温下用高纯氮气吹干。
(2)配制NH 4F浓度为0.045mol/L的溶液作为反应液。
(3)将清洗干燥后的金属铌片作为衬底和源材料，平行放置于溶液中，在200℃下生长6h，生长结束后，取出铌片，去离子水清洗，室温下用高纯氮气吹干，铌片表面生长出平均长度为1μm，平均直径为50nm的Nb 2O 5纳米线(如图2所示为Nb 2O 5纳米线的扫描电镜形貌图)。
(4)将生长有Nb 2O 5纳米线的铌片放入BENEQ TFS-200ALD反应腔中，采用原子层沉积技术制备ZnO壳层薄膜，其中设定反应温度为200℃，选择(二乙基锌)DEZ作为锡源，去离子水作为氧源，不需加热，并设定生长循环数为100cycles，其中每个循环的生长过程包括0.2s DEZ脉冲，10s N 2(g)吹扫，0.2s去离子水脉冲和10s N 2(g)吹扫，制备得到ZnO壳层薄膜厚度为20nm(如图3所示为ZnO壳层薄膜的扫描电镜形貌图)。
(5)配制12.5mM的Zn(NO 3) 2和12.5mM的HMT的混合溶液，按1：1混合配制。
(6)将上述经原子层沉积制备得到的样品，即生长有已包覆ZnO的Nb 2O 5纳米线的铌片作为衬底，平行放置于溶液中，在80℃下生长5h，生长结束后，取出铌片，去离子水清洗，室温下用高纯氮气吹干。铌片表面支化生长出平均长度为130nm，平均直径为20nm的ZnO纳米线(如图4所示为ZnO纳米线的扫描电镜形貌图)；
将Nb 2O 5-ZnO支化纳米线从铌片衬底上超声分离，均匀分散在去离子水中，再将得到的悬浮液滴在标准清洗过的石英片衬底上，空气中50～80℃的温度下烘烤直至完全干燥；自然冷却至室温后，即得到白色的平均长度为400nm，平均直径为90nm(壳层厚度为20nm)的氧化铌/氧化锌核壳支化纳米线结构的气敏纳米材料。
实施例2
一种基于n-n结氧化铌/氧化锌核壳支化纳米线结构的气敏纳米材料的制备工艺包括以下步骤：
(1)取一块大小为2.0cm×2.0cm的金属铌片作为衬底和源材料，依次浸泡于无水乙醇和去离子水中各超声清洗10min，室温下用高纯氮气吹干。
(2)配制NH 4F浓度为0.045mol/L的溶液作为反应液。
(3)将清洗干燥后的金属铌片作为衬底和源材料，平行放置于溶液中，在200℃下生长6h，生长结束后，取出铌片，去离子水清洗，室温下用高纯氮气吹干，铌片表面生长出平均长度为900nm，平均直径为50nm的Nb 2O 5纳米线。
(4)将生长有Nb 2O 5纳米线的铌片放入BENEQ TFS-200ALD反应腔中，采用原子层沉积技术制备ZnO壳层薄膜，其中设定反应温度为200℃，选择(二乙基锌)DEZ作为锡源，去离子水作为氧源，不需加热，并设定生长循环数为100cycles，其中每个循环的生长过程包括0.2s DEZ脉冲，10s N 2(g)吹扫，0.2s去离子水脉冲和10s N 2(g)吹扫，制备得到ZnO壳层薄膜厚度为20nm。
(5)配制25mM的Zn(NO 3) 2和25mM的HMT的混合溶液，按1：1混合配制。
(7)将上述经原子层沉积制备得到的样品，即生长有已包覆ZnO的Nb 2O 5纳米线的铌片作为衬底，平行放置于溶液中，在80℃下生长3h，生长结束后，取出铌片，去离子水清洗，室温下用高纯氮气吹干。铌片表面支化生长出平均长度为200nm，平均直径为30nm的ZnO纳米线(如图5所示为ZnO纳米线的扫描电镜形貌图)；
将Nb 2O 5-ZnO支化纳米线从铌片衬底上超声分离，均匀分散在去离子水中，再将得到的悬浮液滴在标准清洗过的石英片衬底上，空气中50～80℃的温度下烘烤直至完全干燥；自然冷却至室温后，即得到白色的平均长度为350nm，平均直径为90nm(壳层厚度为20nm)的氧化铌/氧化锌核壳支化纳米线结构的气敏纳米材料。
利用得到的氧化铌/氧化锌核壳支化纳米线对10～4ppm的硫化氢气体进行气体传感测试。对10ppm的硫化氢气体，Nb 2O 5-ZnO(已支化)纳米线的灵敏度(定义为响应度-1)为1.25，而纯Nb 2O 5纳米线的灵敏度为1.06，Nb 2O 5-ZnO(未支化)纳米线的灵敏度为1.19，本发明的核壳支化纳米线结构将对10ppm硫化氢气体的传感灵敏度相较于纯Nb 2O 5纳米线提高了18％，相较于Nb 2O 5-ZnO(未支化)纳米线提高了5％，对其它浓度下的硫化氢气体其灵敏度也有不同程度的提升。如图6所示为不同材料的气体灵敏度的对比测试结果，显示上述技术方案提供的材料具有更为灵敏的气敏性能。
从上述技术方案可以看出，在各种金属氧化物半导体材料中，五氧化二铌(Nb 2O 5)是一种重要的n型氧化物宽禁带(约为3.4eV)半导体，具有良好的导电性和高浓度的氧空位，利于捕获电子，因此基于Nb 2O 5的优良传感器是值得研究的。基于单一氧化铌材料的气体传感器其气敏性能相对较差。由此，复合结构材料的制备引起了广泛的研究兴趣，被普遍认为是一种提高气体传感器性能的有效方法。构建由两种或多种半导体材料组成的核壳异质结构，不仅能产生各种材料的多种特性的协同效应，而且由于界面态的电子俘获和异质结的形成，增加了额外的耗尽宽度和界面势垒的变化，由此带来比原始纳米结构更大的传感器响应。此外，层次结构的构建，如分枝状的纳米线，有利于比表面积的增加和在多级纳米结构之间的界面上形成更多的异质结或同质结，进一步提升传感器响应。
以上所述仅是本发明的优选实施方式，应当指出，对于本技术领域的普通技术人员，在不脱离本发明原理的前提下，还可以做出若干改进和润饰，这些改进和润饰也应视为本发明的保护范围。

Claims (11)

  1. 一种支化纳米线结构的气敏纳米材料的制备方法，其中，包括如下步骤：
    提供NH 4F的溶液；
    将金属铌片置于溶液中进行纳米线生长，在铌片表面生长出Nb 2O 5纳米线；
    采用原子层沉积技术在生长有Nb 2O 5纳米线的铌片表面制备ZnO壳层薄膜；
    提供6.25～25mM的Zn(NO 3) 2和6.25～25mM的HMT的混合溶液；
    将表面包覆ZnO和Nb 2O 5纳米线的铌片放置于混合溶液中，在其表面支化生长出ZnO支化纳米线；
    将Nb 2O 5-ZnO支化纳米线从铌片衬底上转移分散至去离子水中，获得Nb 2O 5-ZnO支化纳米线悬浮液；
    再将得到的悬浮液滴石英片衬底上，干燥并冷却后得到Nb 2O 5-ZnO支化纳米线结构的气敏纳米材料。
  2. 如权利要求1所述的方法，其中，NH 4F的溶液中NH 4F的浓度为0.03～0.06mol/L。
  3. 如权利要求1所述的方法，其中，所述金属铌片为多片，平行放置于NH 4F的溶液中。
  4. 如权利要求1所述的方法，其中，提供6.25～25mM的Zn(NO 3) 2和6.25～25mM的HMT的混合溶液的混合比例为体积比1：1。
  5. 如权利要求1所述的方法，其特征在于，所述获得悬浮液的步骤，进一步是将ZnO支化纳米线从铌片衬底上超声分离，均匀分散在去离子水中。
  6. 如权利要求1所述的方法，其中，所述得到气敏纳米材料的步骤，进一 步是将得到的质量体积比为1～5mg/ml的悬浮液滴在标准清洗过的石英片衬底上，空气中50～80℃的温度下烘烤直至完全干燥；自然冷却至室温，得到氧化铌/氧化锌核壳支化纳米线结构的气敏纳米材料。
  7. 如权利要求1所述的方法，其中，金属铌片置于溶液中进行纳米线生长的步骤前，进一步包括清洗金属铌片的步骤，具体是依次用无水乙醇和去离子水清洗各超声清洗10～15min后，用氮气吹干的步骤。
  8. 如权利要求1所述的方法，其中，Nb 2O 5纳米线的长度为700～1100nm，直径为40～60nm。
  9. 如权利要求1所述的方法，其中，ZnO支化纳米线的长度为80～150nm，直径为15～40nm。
  10. 一种如权利要求1所述的制备方法制得的基于Nb 2O 5-ZnO核壳支化纳米线结构的气敏纳米材料。
  11. 一种如权利要求10所述的基于Nb 2O 5-ZnO核壳支化纳米线结构的气敏纳米材料在检测硫化氢气体方面的应用。
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