CN109507242B - 多孔结构c@三氧化二铁复合纳米材料的制备方法及其产品和应用 - Google Patents
多孔结构c@三氧化二铁复合纳米材料的制备方法及其产品和应用 Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 29
- 239000002086 nanomaterial Substances 0.000 title claims abstract description 28
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 title claims abstract description 14
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 229910003145 α-Fe2O3 Inorganic materials 0.000 claims abstract description 5
- 238000001514 detection method Methods 0.000 claims abstract description 4
- 239000000243 solution Substances 0.000 claims description 60
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 42
- 238000003756 stirring Methods 0.000 claims description 34
- QCVGEOXPDFCNHA-UHFFFAOYSA-N 5,5-dimethyl-2,4-dioxo-1,3-oxazolidine-3-carboxamide Chemical compound CC1(C)OC(=O)N(C(N)=O)C1=O QCVGEOXPDFCNHA-UHFFFAOYSA-N 0.000 claims description 31
- 102000002322 Egg Proteins Human genes 0.000 claims description 31
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- 239000008367 deionised water Substances 0.000 claims description 14
- 229910021641 deionized water Inorganic materials 0.000 claims description 14
- 238000002156 mixing Methods 0.000 claims description 14
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims description 13
- 239000007789 gas Substances 0.000 claims description 12
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- 238000004108 freeze drying Methods 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 7
- 238000001914 filtration Methods 0.000 claims description 7
- 238000000227 grinding Methods 0.000 claims description 7
- 239000011261 inert gas Substances 0.000 claims description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- 239000007864 aqueous solution Substances 0.000 claims description 6
- 229910006540 α-FeOOH Inorganic materials 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 229910052786 argon Inorganic materials 0.000 claims description 3
- 239000000463 material Substances 0.000 abstract description 15
- 239000002341 toxic gas Substances 0.000 abstract description 2
- 230000035945 sensitivity Effects 0.000 description 8
- 229910044991 metal oxide Inorganic materials 0.000 description 3
- 150000004706 metal oxides Chemical class 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 238000005979 thermal decomposition reaction Methods 0.000 description 2
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 2
- -1 Fe2O3 Chemical class 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
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Abstract
本发明公开了一种C@三氧化二铁复合纳米材料的制备方法及其产品和应用,该方法利用蛋清作为生物模板,在生物模板表面生长α‑FeOOH,利用冷冻干燥技术干燥,可确保蛋清保持其生物结构,然后在惰性气体氛围中高温处理,使蛋清碳化并且α‑FeOOH热分解得到C@α‑Fe2O3复合纳米结构。以C@α‑Fe2O3复合纳米结构制备的元件,可利用C材料优异的导电性,从而提升其电学性能,该复合材料可用于有毒气体的检测、超级电容器等领域。
Description
技术领域
本发明涉及气敏材料技术领域,具体是指一种C@三氧化二铁复合纳米材料的制备方法及其产品和应用。
背景技术
金属氧化物如Fe2O3、ZnO、SnO2、WO3等由于具有性能优异、环境友善、资源丰富、价格低廉等优点,是研究较为广泛的气敏材料。通过金属氧化物表面修饰、金属/贵金属掺杂等工艺可提升材料的气敏性能,在气敏传感器领域有非常广泛的应用。
决定半导体气敏材料灵敏度的关键因素包括材料表面与待测气体的反应以及材料的导电性,其中前者决定敏感材料的响应灵敏度,后者可决定材料的能耗。Fe2O3作为气体敏感材料一直受到科研界和产业界的关注,但是半导体金属氧化物的导电性能较差,通过与碳材料符合可提升其导电性能,进而提升材料的气体灵敏性。
发明内容
为克服现有技术的不足,本发明的目的在于提供一种C@三氧化二铁复合纳米材料的制备方法。
本发明的再一目的在于:提供一种上述方法制备的C@三氧化二铁复合纳米材料产品。
本发明的又一目的在于:提供一种上述产品的应用。
本发明目的通过下述方案实现:一种多孔结构C@三氧化二铁复合纳米材料的制备方法,利用蛋清作为生物模板,在生物模板表面生长α-FeOOH,利用冷冻干燥技术干燥,可确保蛋清保持其生物结构,然后在惰性气体氛围中高温热处理,使蛋清碳化并且α-FeOOH热分解得到C@α-Fe2O3复合纳米结构,包括如下步骤:
步骤一:取10g蛋清与去离子水混合搅拌,蛋清的浓度为10~40wt%,过滤除去蛋清溶液中的白色絮状物,得到溶液A;
步骤二:按摩尔浓度0.05~0.2mol/L配FeSO4·7H2O的水溶液,搅拌30min后,向上述溶液中加入乙二醇,乙二醇与去离子水的体积比为1:1~3,搅拌10min,得到溶液B;
步骤三:将步骤一所得溶液A和步骤二所得溶液B按体积比为1~3:1混合,搅拌30min后将溶液在搅拌状态下加热至40~60 ℃,保持5~10h后将溶液降至室温,将所得产物于-80℃冷冻干燥;将干燥好的样品置于管式炉中,在惰性气体氛围下热处理,研磨得到C@Fe2O3复合纳米材料。
步骤三所述的惰性气体为高纯的氮或氩。
步骤三所述的热处理温度为300~350℃保持1.5~2h,450~600℃保持2~3h,升温速度均为1~3℃/min。
本发明还提供了一种多孔结构C@三氧化二铁复合纳米材料,根据上述任一所述方法制备得到。
另外,本发明也提供了上述一种多孔结构C@三氧化二铁复合纳米材料在丙酮气体检测中的应用。
本发明一种简单可行的制备C@Fe2O3纳米材料的方法,该方法利用蛋清作为生物模板,在生物模板表面生长α-FeOOH,利用冷冻干燥技术干燥,可确保蛋清保持其生物结构,然后在惰性气体氛围中高温处理,使蛋清碳化并且α-FeOOH热分解得到C@α-Fe2O3复合纳米结构。以C@α-Fe2O3复合纳米结构制备的元件,可利用C材料优异的导电性,从而提升其电学性能,该复合材料可用于有毒气体的检测、超级电容器等领域
本发明提供一种简单的制备多孔结构C@Fe2O3的方法,可增加材料表面的比表面积及活性位点,大幅提高纳米材料的气敏性能,且制备工艺简单,制备的成本低,对进一步推进半导体气敏器件的发展具有实际应用价值。
附图说明
图1为本发明实施例1制得的多孔结构C@Fe2O3对丙酮的响应图。
具体实施方式
实施例1:
取10g蛋清与去离子水混合搅拌,蛋清的浓度为30wt%,过滤除去蛋清溶液中的白色絮状物,得到溶液A;
按摩尔浓度0.05mol/L配FeSO4·7H2O的水溶液,搅拌30min后,向上述溶液中加入乙二醇,乙二醇与去离子水的体积比为1:1,搅拌10min,得到溶液B;
将溶液A和溶液B混合,溶液A和溶液B的体积比为1~3;搅拌30min后将溶液在搅拌状态下加热至60 ℃,保持8h后将溶液降至室温,将所得产物于-80℃冷冻干燥;将干燥好的样品置于管式炉中,在高纯氮气体氛围下热处理,热处理温度为300℃保持2h,500℃保持2.5h,升温速度均为2℃/min,研磨得到C@Fe2O3复合纳米材料。
所制得的多孔结构C@Fe2O3对丙酮的响应图如图1所示,合成的多孔C@Fe2O3对1ppm丙酮的灵敏度为15.12,最佳工作温度为180℃。
实施例2
取10g蛋清与去离子水混合搅拌,蛋清的浓度为20wt%,过滤除去蛋清溶液中的白色絮状物,得到溶液A;
按摩尔浓度0.1mol/L配FeSO4·7H2O的水溶液,搅拌30min后,向上述溶液中加入乙二醇,乙二醇与去离子水的体积比为1:3,搅拌10min,得到溶液B;
将溶液A和溶液B混合,溶液A和溶液B的体积比为1~2;搅拌30min后将溶液在搅拌状态下加热至50 ℃,保持8h后将溶液降至室温,将所得产物于-80℃冷冻干燥;将干燥好的样品置于管式炉中,在高纯氮气体氛围下热处理,热处理温度为350℃保持2h,500℃保持3h,升温速度均为1.5℃/min,研磨得到C@Fe2O3复合纳米材料。
本实施例合成的多孔C@Fe2O3对1ppm丙酮的灵敏度为17.6,最佳工作温度为180℃。
实施例3
取10g蛋清与去离子水混合搅拌,蛋清的浓度为10wt%,过滤除去蛋清溶液中的白色絮状物,得到溶液A;
按摩尔浓度0.2mol/L配FeSO4·7H2O的水溶液,搅拌30min后,向上述溶液中加入乙二醇,乙二醇与去离子水的体积比为1:2,搅拌10min,得到溶液B;
将溶液A和溶液B混合,溶液A和溶液B的体积比为1~2;搅拌30min后将溶液在搅拌状态下加热至50 ℃,保持8h后将溶液降至室温,将所得产物于-80℃冷冻干燥;将干燥好的样品置于管式炉中,在高纯氮气体氛围下热处理,热处理温度为350℃保持2h,500℃保持3h,升温速度均为1.5℃/min,研磨得到C@Fe2O3复合纳米材料。
本实施例合成的多孔C@Fe2O3对1ppm丙酮的灵敏度为11.58,最佳工作温度为180℃。
实施例4
取10g蛋清与去离子水混合搅拌,蛋清的浓度为40wt%,过滤除去蛋清溶液中的白色絮状物,得到溶液A;
按摩尔浓度0.2mol/L配FeSO4·7H2O的水溶液,搅拌30min后,向上述溶液中加入乙二醇,乙二醇与去离子水的体积比为1:3,搅拌10min,得到溶液B;
将溶液A和溶液B混合,溶液A和溶液B的体积比为1:1;搅拌30min后将溶液在搅拌状态下加热至40 ℃,保持5h后将溶液降至室温,将所得产物于-80℃冷冻干燥;将干燥好的样品置于管式炉中,在高纯氩气体氛围下热处理,热处理温度为300℃保持2h,450℃保持3h,升温速度均为1℃/min,研磨得到C@Fe2O3复合纳米材料。
本实施例合成的多孔C@Fe2O3对1ppm丙酮的灵敏度为13.55,最佳工作温度为180℃。
实施例5
取10g蛋清与去离子水混合搅拌,蛋清的浓度为40wt%,过滤除去蛋清溶液中的白色絮状物,得到溶液A;
按摩尔浓度0.2mol/L配FeSO4·7H2O的水溶液,搅拌30min后,向上述溶液中加入乙二醇,乙二醇与去离子水的体积比为1:3,搅拌10min,得到溶液B;
将溶液A和溶液B混合,溶液A和溶液B的体积比为1:1;搅拌30min后将溶液在搅拌状态下加热至40 ℃,保持5h后将溶液降至室温,将所得产物于-80℃冷冻干燥;将干燥好的样品置于管式炉中,在空气气体氛围下热处理,热处理温度为300℃保持2h,450℃保持3h,升温速度均为1℃/min,研磨得到C@Fe2O3复合纳米材料。
本实施例在空气中热处理样品,合成的材料为多孔Fe2O3,其对1ppm丙酮的灵敏度为5.36,最佳工作温度为230℃。
Claims (4)
1.一种多孔结构C@三氧化二铁复合纳米材料的制备方法,其特征在于,利用蛋清作为生物模板,在生物模板表面生长α-FeOOH,利用冷冻干燥确保蛋清保持其生物结构,然后在惰性气体氛围中高温热处理,使蛋清碳化并且α-FeOOH热分解得到C@α-Fe2O3复合纳米结构,包括如下步骤:
步骤一:取10g蛋清与去离子水混合搅拌,蛋清的浓度为10~40wt%,过滤除去蛋清溶液中的白色絮状物,得到溶液A;
步骤二:按摩尔浓度0.05~0.2mol/L配FeSO4·7H2O的水溶液,搅拌30min后,加入乙二醇,乙二醇与去离子水的体积比为1:(1~3),搅拌10min,得到溶液B;
步骤三:将步骤一所得溶液A和步骤二所得溶液B按体积比为1~3:1混合,搅拌30min后将溶液在搅拌状态下加热至40~60℃,保持5~10h后将溶液降至室温,将所得产物于-80℃冷冻干燥;将干燥好的样品置于管式炉中,在惰性气体氛围高温下热处理,研磨得到C@Fe2O3复合纳米材料;其中,
步骤三热处理中,温度为300~350℃保持1.5~2h,450~600℃保持2~3h,升温速度均为1~3℃/min。
2.根据权利要求1所述多孔结构C@三氧化二铁复合纳米材料的制备方法,其特征在于:步骤三所述的惰性气体为高纯的氮或氩。
3.一种多孔结构C@三氧化二铁复合纳米材料,其特征在于根据权利要求1或2所述方法制备得到。
4.根据权利要求3所述多孔结构C@三氧化二铁复合纳米材料在丙酮气体检测中的应用。
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