ZnO/Ag纳米复合材料的金属、非金属掺杂及其光催化性能研究
摘要
本文研究了ZnO/Ag纳米复合材料的金属掺杂和非金属掺杂工艺及其掺杂后的光催化性能。研制出光催化性能较好的铁掺杂ZnO/Ag、镉掺杂ZnO/Ag、氮掺杂ZnO/Ag纳米复合材料。
1.以Zn(SO4)2、NH4HCO3、AgNO3、Fe2(SO4)3等为原料,采用两步液相沉淀法对ZnO/Ag纳米复合材料进行过渡金属铁掺杂。考察铁的掺杂比和掺铁反应物浓度对ZnO/Ag纳米复合材料光催化性能的影响规律。采用TEM、XRD等测试方法对铁掺杂ZnO/Ag纳米复合材料的微观形貌和物相结构进行表征。通过观察甲基橙溶液宏观颜色变化及采用UV-vis对铁掺杂ZnO/Ag纳米复合材料光催化降解甲基橙溶液的结果进行表征。
结果表明:铁掺杂可以改善ZnO/Ag纳米复合材料的光催化性能。铁掺杂ZnO/Ag纳米复合材料粒径较小、分散好、团聚程度小。掺铁反应物浓度为0.134 mol?L-1、铁的掺杂比为5 %时甲基橙的降解速率最高,3 h后对甲基橙溶液的降解率达到97.2 %。
2.以Zn(NO3)2、(NH4)2CO3、AgNO3、Cd(NO3)2、NH3·H2O等为原料,采用配位均匀共沉淀法对ZnO/Ag纳米复合材料进行过渡金属镉掺杂。考察镉的掺杂比和掺镉反应物浓度对ZnO/Ag纳米复合材料的光催化性能的影响规律。采用TEM、XRD、FT-IR、ICP等测试方法对掺杂材料的微观形貌、物相结构、组成、组分含量进行表征。通过观察甲基橙溶液宏观颜色变化及采用UV-vis对镉掺杂ZnO/Ag纳米复合材料光催化降解甲基橙溶液的结果进行表征。
结果表明:镉掺杂可以改善ZnO/Ag纳米复合材料的光催化性能。镉掺杂ZnO/Ag纳米复合材料分散性较好,粒径在20 nm左右。掺镉反应物浓度0.084 mol?L-1、掺杂比1:12时镉掺杂ZnO/Ag纳米复合材料的光催化性能最好,3 h后对甲基橙溶液的降解率达到97.9 %,此组掺杂材料中Cd、Zn、Ag的质量比为5:33:3。
3.以Zn(SO4)2、NH4HCO3、AgNO3、N2、H2等为原料,采用等离子法对ZnO/Ag纳米复合材料进行非金属氮掺杂。考察渗氮时间对ZnO/Ag纳米复合材料的光催化性能的影响规律。采用TEM、XRD、元素分析等测试方法对掺杂材料的微观形貌、物相结构、氮含量进行表征。通过观察甲基橙溶液的宏观颜色变化及采用UV-vis对氮掺杂ZnO/Ag纳米复合材料光催化降解甲基橙溶液的结果进行表征。
结果表明:等离子法氮掺杂可以明显改善ZnO/Ag纳米复合材料的光催化性能。氮掺杂ZnO/Ag纳米复合材料分散性较好,粒径在20 nm左右。渗氮时间30 min对应的氮掺杂ZnO/Ag纳米复合材料的光催化性能最好。2h后对甲基橙溶液的降解率达到99.7 %。
4.以Zn(SO4)2、NH4HCO3、AgNO3、C3N3H6等为原料,用气相法对ZnO/Ag纳米复合材料进行非金属氮掺杂。通过正交实验考察渗氮温度、掺杂比、保温时间对ZnO/Ag纳米复合材料光催化性能的影响规律。采用TEM、XRD、ICP、元素分析等测试方法对掺杂材料的微观形貌、物相结构、氮含量进行表征。通过观察甲基橙溶液宏观颜色变化及采用UV-vis对氮掺杂ZnO/Ag纳米复合材料光催化降解甲基橙溶液的结果进行表征。
结果表明:气相法氮掺杂可以明显改善ZnO/Ag纳米复合材料的光催化性能。氮掺杂ZnO/Ag纳米复合材料分散性较好,粒径在20 nm左右。渗氮温度、掺杂比和保温时间均对ZnO/Ag纳米复合材料的光催化性能有影响,其中掺杂比对ZnO/Ag纳米复合材料的光催化性能影响最大。降解30 min后,渗氮温度380℃、掺杂比1、保温时间2.5 h的氮掺杂ZnO/Ag纳米复合材料对甲基橙溶液的降解率达到94 %,此组纳米复合材料中含氮量为2.564 %。
In this paper, ZnO/Ag nanocomposites doped by Fe, Cd and N were prepared for improving photocatalytic properties of nanocomposites.
1. Fe-doped ZnO/Ag nanocomposites were prepared by dual-step liquid deposition approach with ZnSO4, NH4HCO3, AgNO3, Fe2(SO4)3 as raw materials. The influences of iron-doped concentration and iron-doped ratio on photocatalytic properties of ZnO/Ag nanocomposites were systemically studied. The micromorphology, microstructures were characterized by transmission electron microcopy, X-ray diffraction. The photocatalytic properties of Fe doped-ZnO/Ag nanocomposites were analyzed quantitatively by UV-vis and macroscopic color change of methyl orange solutions.
The results show that: doping iron could improve the photocatalytic properties of ZnO/Ag nanocomposites. Fe-doped ZnO/Ag nanocomposite was well-dispersed with small particle size between 15-20 nm. The photocatalytic properties of Fe-doped ZnO/Ag nanocomposites with doping concentration of 0.134 mol?L-1 and doping ratio of 5 % were best, and the degradation ratio of methyl orange solutions was 97.2 % after 3 h.
2. Cd-doped ZnO/Ag nanocomposites were prepared by coordination homogeneous precipitation approach with Zn(NO3)2, (NH4)2CO3, AgNO3, Cd(NO3)2, NH3·H2O as raw materials. The influences of cadmium-doped concentration and cadmium-doped ratio on photocatalytic properties of ZnO/Ag nanocomposites were systemically studied. The micromorphology, microstructures, components, contents of components were characterized by transmission electron microcopy, X-ray diffraction, Fourier transform infrared spectroscopy and inductively coupled plasma emission spectrometer. The photocatalytic properties of Cd doped-ZnO/Ag nanocomposites were analyzed quantitatively by UV-vis and macroscopic color change of methyl orange solutions.
The results show that: doping cadmium could improve the photocatalytic properties of ZnO/Ag nanocomposites. Cd-doped ZnO/Ag nanocomposite was well-dispersed with small particle size about 20 nm. The optimization cadmium-doping conditions are shown as follows: the reactant concentration 0.084 mol/L, the doping ratio 1:12, and the degradation ratio of methyl orange solutions was 97.9 % after 3 h. The mass rate of Cd, Zn and Ag of this Cd-doped ZnO/Ag nanocomposite is 5:33:3.
3. N-doped ZnO/Ag nanocomposites were prepared by a combination of liquid deposition approach and subsequent plasma nitriding with Zn(SO4)2, NH4HCO3, AgNO3, N2, H2 as raw materials. The influences of nitriding time on photocatalytic properties of ZnO/Ag nanocomposites were systemically studied. The micromorphology, microstructures, contents of components were characterized by transmission electron microcopy, X-ray diffraction, elemental analyzer. The photocatalytic properties of N doped-ZnO/Ag nanocomposites were analyzed quantitatively by UV-vis and macroscopic color change of methyl orange solutions.
The results show that: doping nitrogen could improve the photocatalytic properties of ZnO/Ag nanocomposites. N-doped ZnO/Ag nanocomposite was well-dispersed with small particle size between 15-20 nm. The photocatalytic properties of N-doped ZnO/Ag nanocomposites with nitriding time 30 min were best, and the degradation ratio of methyl orange solutions was 99.7 % after 2 h.
4. N-doped ZnO/Ag nanocomposites were prepared by a combination of liquid deposition approach and atmosphere nitriding with Zn(SO4)2, NH4HCO3, AgNO3, C3N3H6 as raw materials. The influences of nitriding time, nitrogen-doped ratio, holding time on photocatalytic properties of ZnO/Ag nanocomposites were systemically studied. The micromorphology, microstructures, contents of components were characterized by transmission electron microcopy, X-ray diffraction, inductively coupled plasma emission spectrometer and elemental analyzer. The photocatalytic properties of N doped-ZnO/Ag nanocomposites were analyzed quantitatively by UV-vis and macroscopic color change of methyl orange solutions.
The results show that: doping nitrogen could improve the photocatalytic properties of ZnO/Ag nanocomposites. N-doped ZnO/Ag nanocomposite was well-dispersed with small particle size between 15-20 nm. The nitriding time, nitrogen-doped ratio and holding time affected the photocatalytic properties of ZnO/Ag nanocomposites, and the maximum impact factor was doping ratio. When nitriding parameter was 380℃, 1, 2.5 h, the degradation rate of methyl orange was the best and was 94 % after 30 min, and N wt. % was 2.564 %.
1.以Zn(SO4)2、NH4HCO3、AgNO3、Fe2(SO4)3等为原料,采用两步液相沉淀法对ZnO/Ag纳米复合材料进行过渡金属铁掺杂。考察铁的掺杂比和掺铁反应物浓度对ZnO/Ag纳米复合材料光催化性能的影响规律。采用TEM、XRD等测试方法对铁掺杂ZnO/Ag纳米复合材料的微观形貌和物相结构进行表征。通过观察甲基橙溶液宏观颜色变化及采用UV-vis对铁掺杂ZnO/Ag纳米复合材料光催化降解甲基橙溶液的结果进行表征。
结果表明:铁掺杂可以改善ZnO/Ag纳米复合材料的光催化性能。铁掺杂ZnO/Ag纳米复合材料粒径较小、分散好、团聚程度小。掺铁反应物浓度为0.134 mol?L-1、铁的掺杂比为5 %时甲基橙的降解速率最高,3 h后对甲基橙溶液的降解率达到97.2 %。
2.以Zn(NO3)2、(NH4)2CO3、AgNO3、Cd(NO3)2、NH3·H2O等为原料,采用配位均匀共沉淀法对ZnO/Ag纳米复合材料进行过渡金属镉掺杂。考察镉的掺杂比和掺镉反应物浓度对ZnO/Ag纳米复合材料的光催化性能的影响规律。采用TEM、XRD、FT-IR、ICP等测试方法对掺杂材料的微观形貌、物相结构、组成、组分含量进行表征。通过观察甲基橙溶液宏观颜色变化及采用UV-vis对镉掺杂ZnO/Ag纳米复合材料光催化降解甲基橙溶液的结果进行表征。
结果表明:镉掺杂可以改善ZnO/Ag纳米复合材料的光催化性能。镉掺杂ZnO/Ag纳米复合材料分散性较好,粒径在20 nm左右。掺镉反应物浓度0.084 mol?L-1、掺杂比1:12时镉掺杂ZnO/Ag纳米复合材料的光催化性能最好,3 h后对甲基橙溶液的降解率达到97.9 %,此组掺杂材料中Cd、Zn、Ag的质量比为5:33:3。
3.以Zn(SO4)2、NH4HCO3、AgNO3、N2、H2等为原料,采用等离子法对ZnO/Ag纳米复合材料进行非金属氮掺杂。考察渗氮时间对ZnO/Ag纳米复合材料的光催化性能的影响规律。采用TEM、XRD、元素分析等测试方法对掺杂材料的微观形貌、物相结构、氮含量进行表征。通过观察甲基橙溶液的宏观颜色变化及采用UV-vis对氮掺杂ZnO/Ag纳米复合材料光催化降解甲基橙溶液的结果进行表征。
结果表明:等离子法氮掺杂可以明显改善ZnO/Ag纳米复合材料的光催化性能。氮掺杂ZnO/Ag纳米复合材料分散性较好,粒径在20 nm左右。渗氮时间30 min对应的氮掺杂ZnO/Ag纳米复合材料的光催化性能最好。2h后对甲基橙溶液的降解率达到99.7 %。
4.以Zn(SO4)2、NH4HCO3、AgNO3、C3N3H6等为原料,用气相法对ZnO/Ag纳米复合材料进行非金属氮掺杂。通过正交实验考察渗氮温度、掺杂比、保温时间对ZnO/Ag纳米复合材料光催化性能的影响规律。采用TEM、XRD、ICP、元素分析等测试方法对掺杂材料的微观形貌、物相结构、氮含量进行表征。通过观察甲基橙溶液宏观颜色变化及采用UV-vis对氮掺杂ZnO/Ag纳米复合材料光催化降解甲基橙溶液的结果进行表征。
结果表明:气相法氮掺杂可以明显改善ZnO/Ag纳米复合材料的光催化性能。氮掺杂ZnO/Ag纳米复合材料分散性较好,粒径在20 nm左右。渗氮温度、掺杂比和保温时间均对ZnO/Ag纳米复合材料的光催化性能有影响,其中掺杂比对ZnO/Ag纳米复合材料的光催化性能影响最大。降解30 min后,渗氮温度380℃、掺杂比1、保温时间2.5 h的氮掺杂ZnO/Ag纳米复合材料对甲基橙溶液的降解率达到94 %,此组纳米复合材料中含氮量为2.564 %。
In this paper, ZnO/Ag nanocomposites doped by Fe, Cd and N were prepared for improving photocatalytic properties of nanocomposites.
1. Fe-doped ZnO/Ag nanocomposites were prepared by dual-step liquid deposition approach with ZnSO4, NH4HCO3, AgNO3, Fe2(SO4)3 as raw materials. The influences of iron-doped concentration and iron-doped ratio on photocatalytic properties of ZnO/Ag nanocomposites were systemically studied. The micromorphology, microstructures were characterized by transmission electron microcopy, X-ray diffraction. The photocatalytic properties of Fe doped-ZnO/Ag nanocomposites were analyzed quantitatively by UV-vis and macroscopic color change of methyl orange solutions.
The results show that: doping iron could improve the photocatalytic properties of ZnO/Ag nanocomposites. Fe-doped ZnO/Ag nanocomposite was well-dispersed with small particle size between 15-20 nm. The photocatalytic properties of Fe-doped ZnO/Ag nanocomposites with doping concentration of 0.134 mol?L-1 and doping ratio of 5 % were best, and the degradation ratio of methyl orange solutions was 97.2 % after 3 h.
2. Cd-doped ZnO/Ag nanocomposites were prepared by coordination homogeneous precipitation approach with Zn(NO3)2, (NH4)2CO3, AgNO3, Cd(NO3)2, NH3·H2O as raw materials. The influences of cadmium-doped concentration and cadmium-doped ratio on photocatalytic properties of ZnO/Ag nanocomposites were systemically studied. The micromorphology, microstructures, components, contents of components were characterized by transmission electron microcopy, X-ray diffraction, Fourier transform infrared spectroscopy and inductively coupled plasma emission spectrometer. The photocatalytic properties of Cd doped-ZnO/Ag nanocomposites were analyzed quantitatively by UV-vis and macroscopic color change of methyl orange solutions.
The results show that: doping cadmium could improve the photocatalytic properties of ZnO/Ag nanocomposites. Cd-doped ZnO/Ag nanocomposite was well-dispersed with small particle size about 20 nm. The optimization cadmium-doping conditions are shown as follows: the reactant concentration 0.084 mol/L, the doping ratio 1:12, and the degradation ratio of methyl orange solutions was 97.9 % after 3 h. The mass rate of Cd, Zn and Ag of this Cd-doped ZnO/Ag nanocomposite is 5:33:3.
3. N-doped ZnO/Ag nanocomposites were prepared by a combination of liquid deposition approach and subsequent plasma nitriding with Zn(SO4)2, NH4HCO3, AgNO3, N2, H2 as raw materials. The influences of nitriding time on photocatalytic properties of ZnO/Ag nanocomposites were systemically studied. The micromorphology, microstructures, contents of components were characterized by transmission electron microcopy, X-ray diffraction, elemental analyzer. The photocatalytic properties of N doped-ZnO/Ag nanocomposites were analyzed quantitatively by UV-vis and macroscopic color change of methyl orange solutions.
The results show that: doping nitrogen could improve the photocatalytic properties of ZnO/Ag nanocomposites. N-doped ZnO/Ag nanocomposite was well-dispersed with small particle size between 15-20 nm. The photocatalytic properties of N-doped ZnO/Ag nanocomposites with nitriding time 30 min were best, and the degradation ratio of methyl orange solutions was 99.7 % after 2 h.
4. N-doped ZnO/Ag nanocomposites were prepared by a combination of liquid deposition approach and atmosphere nitriding with Zn(SO4)2, NH4HCO3, AgNO3, C3N3H6 as raw materials. The influences of nitriding time, nitrogen-doped ratio, holding time on photocatalytic properties of ZnO/Ag nanocomposites were systemically studied. The micromorphology, microstructures, contents of components were characterized by transmission electron microcopy, X-ray diffraction, inductively coupled plasma emission spectrometer and elemental analyzer. The photocatalytic properties of N doped-ZnO/Ag nanocomposites were analyzed quantitatively by UV-vis and macroscopic color change of methyl orange solutions.
The results show that: doping nitrogen could improve the photocatalytic properties of ZnO/Ag nanocomposites. N-doped ZnO/Ag nanocomposite was well-dispersed with small particle size between 15-20 nm. The nitriding time, nitrogen-doped ratio and holding time affected the photocatalytic properties of ZnO/Ag nanocomposites, and the maximum impact factor was doping ratio. When nitriding parameter was 380℃, 1, 2.5 h, the degradation rate of methyl orange was the best and was 94 % after 30 min, and N wt. % was 2.564 %.
引文
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