锗酸盐纳米结构的制备及其CO_2光催化还原的研究
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摘要
利用光催化还原将温室气体CO2转换成有用的碳氢燃料是解决能源危机和环境污染最有前途的方法之一。锗酸盐光催化剂导带弥散,电子迁移速率高,具有良好的光催化分解H2O和有机污染物降解性能。而光催化剂的尺寸、维度、暴露晶面、表面结构等对其光催化性能有着直接影响。本文采用溶剂热法,以乙二胺和水为混合溶剂合成了一批锗酸盐纳米结构,并将此体系扩展到镓酸盐纳米结构的制备,探讨了产物的形成机理,并研究了其光催化CO2还原性能。主要研究内容如下：
(1)调节乙二胺和水的比例,合成了“稻草”束状Zn2GeO4低维纳米结构。通过控制各反应条件研究了其生长机理,发现这种由1D纳米单元组成的束状结构的生成主要基于晶体的劈裂生长机制,类似于自然界中的一些矿石。通过负载不同的助催化剂,Zn2GeO4在氙灯全幅光照射下具有较好的光催化CO2还原成CH4活性。而且,将这种束状Zn2GeO4超结构在氮气气氛下氮化处理能够得到黄色的Zn1.7GeN1.8O固溶体,基本保留了前驱物的束状结构,该固溶体在可见光下具有较好的光催化CO2还原活性。
(2)在此溶剂体系中,合成了长度达数百微米,厚度约为7nm(相当于5个晶胞的厚度)和长径比高达10000的单晶Zn2GeO4纳米带。纳米带长度为[001]方向,宽度为[100]方向,纳米带上下两大暴露面为{0l0}面。纳米带的生成基于配位溶剂分子模板机制(SCMT),乙二胺吸附在固体表面,并选择性地吸附到到某些特定的面上从而控制晶体的生长方向和速度。Zn2GeO4(?)内米带超长和超薄的几何形状大大提高了其光催化还原CO2为甲烷的活性。
(3)在乙二胺(En)和水的体系中,以醋酸制为源,合成了直径约为2-3nm,长度达数百个纳米的In2Ge2O7(En)有机无机杂化超细纳米线。与纯无机In2Ge2O7纳米线和纳米管相比,这种杂化超细纳米线的发光光谱蓝移了近100nm。使用该超细纳米线光催化还原C02,以水蒸汽作为还原剂,结果表明光催化生成的产物为CO,不同于Zn2GeO4光催化剂。这些研究结果表明,温室气体CO2可以通过不同的锗酸盐催化剂选择性地还原成所需要的可再生燃料。
(4)将此溶剂体系扩展到镓酸盐纳米结构的制备中,以硝酸镓为镓源,合成了形貌规整大小均,具有3D分级结构的ZnGa2O4微米花,这些微米花是由{110}面暴露比例高达99.6%的超薄纳米片自组装而成。光催化CO2还原实验结果表明,{1110}面暴露的ZnGa2O4纳米片的光催化转换效率是{100}面暴露的立方体纳米晶和{111}面暴露的八面体纳米晶的4倍之多。对这三个表面进行DFT理计计算,发现ZnGa2O4{110}面阳离子密度高有利于CO2吸附,功函低CO2容易活化,从而增强了其CO2还原光催化性能。除此之外,ZnGa2O4微米花独特的3D分级结构也增强了其光催化性能,3D结构使得催化剂具有较大的比表面积,而纳米片的超薄结构也有利于载流子快速从内部迁移到表门面参与光催化反应。
Reduction of CO2to valuable hydrocarbons using solar energy is one of the best solutions to both the global warming and the energy shortage problems. The unique multi-dimensional channel structures of Metal germinates photocatalysts facilitates the separation of photogenerated charge carriers with good photocatalytic performance. The photocatalytic activity of photocatalysts is highly dictated by their sizes, shapes and crystal facets. In this dissertation, some germanate compounds nanomaterials were synthesized in a binary ethylenediamine (En)/water solvent system using a solvothermal route. The formation mechanism and photocatalytic activity of CO2reduction of these nanomaterials were studied. The details are summarized as follows:
(1) Sheaf-like, hyperbranched Zn2GeO4nanoarchitectures were successfully synthesized in this mixed-solvent system. These structures may be assigned to the splitting crystal growth mechanism, resembling some minerals observed in nature. Addition of increasing amounts of En was found to enhance the degree of crystal splitting. Nitridation of the resulting Zn2GeO4superstructures under NH3flow produced yellow Zn1.7GeN1.8O solid solution, which allows photocatalytically converse CO2into CH4in the presence of H2O at ambient conditions under visible light irradiation.
(2) Single-crystalline Zn2GeO4nanobelts with thickness as thin as～7nm (corresponding to five repeating cell units) and aspect ratio up to10,000has been synthesized using this solvothermal route. En can adsorb on solid surfaces and selectively bind to some specific panels to control the velocity and direction of crystal growth, which was termed as the solvent-coordination molecular-template mechanism. The ultralong and ultra-thin geometry of the Zn2GeO4nanoribbon proves to improve the photocatalytic activity toward reduction of CO2in the presence of water vapor into CH4.
(3)A novel, highly crystalline indium germinate hybrid subnanowire, which we denote as In2Ge2O7(En), with general diameters of2-3nm and lengths up to hundreds of nanometres was synthesized in this En/water solvent system. The hybrid ultrathin nanowire exhibits an ultraviolet photoluminescence emission, a dramatic blue shift by more than100nm relative to pure inorganic In2Ge2O7nanowire andmicrotubes. The In2Ge2O7(En) ultrathin nanowire performs selectively the photocatalytic reduction of CO2into CO in the presence of water vapor. With reference to our Zn2GeO4nanoribbon photocatalyst, which was recently used to produce CH4under the same photocatalytic conditions, this work is a significant sign that the greenhouse gas, CO2, can be ameliorated into desirable kinds of renewable fuels using different germinate catalysts.
(4) Well-defined,3D hierarchical microcrystals united with ultrathin ZnGa2O4nanosheets with over99.6%exposed{110} facets with highly active surfaces were deposited in this (En)/water solvent system. The{110}-dominant ZnGa2O4nanosheets proves4-time conversion efficiency of CO2reduction higher than cubic nanocrystals with{100} and octahedral nanocrystals with{111} surfaces. The enhancement of the photocatalytic efficiency is strongly associated with inherent catalytic behavior of {110} surface with high density of cations for CO2absorption and low work function for enhanced CO2activation. In addition, the unique3D hierarchical architecture also promotes the photocatalytic performance through high surface area, ultrathin thickness which allows charge carriers to move rapidly from the interior to the surface to participate in the photoreduction reaction, and improvement of light scattering to be in favor of enhancing the light absorption.
(1)调节乙二胺和水的比例,合成了“稻草”束状Zn2GeO4低维纳米结构。通过控制各反应条件研究了其生长机理,发现这种由1D纳米单元组成的束状结构的生成主要基于晶体的劈裂生长机制,类似于自然界中的一些矿石。通过负载不同的助催化剂,Zn2GeO4在氙灯全幅光照射下具有较好的光催化CO2还原成CH4活性。而且,将这种束状Zn2GeO4超结构在氮气气氛下氮化处理能够得到黄色的Zn1.7GeN1.8O固溶体,基本保留了前驱物的束状结构,该固溶体在可见光下具有较好的光催化CO2还原活性。
(2)在此溶剂体系中,合成了长度达数百微米,厚度约为7nm(相当于5个晶胞的厚度)和长径比高达10000的单晶Zn2GeO4纳米带。纳米带长度为[001]方向,宽度为[100]方向,纳米带上下两大暴露面为{0l0}面。纳米带的生成基于配位溶剂分子模板机制(SCMT),乙二胺吸附在固体表面,并选择性地吸附到到某些特定的面上从而控制晶体的生长方向和速度。Zn2GeO4(?)内米带超长和超薄的几何形状大大提高了其光催化还原CO2为甲烷的活性。
(3)在乙二胺(En)和水的体系中,以醋酸制为源,合成了直径约为2-3nm,长度达数百个纳米的In2Ge2O7(En)有机无机杂化超细纳米线。与纯无机In2Ge2O7纳米线和纳米管相比,这种杂化超细纳米线的发光光谱蓝移了近100nm。使用该超细纳米线光催化还原C02,以水蒸汽作为还原剂,结果表明光催化生成的产物为CO,不同于Zn2GeO4光催化剂。这些研究结果表明,温室气体CO2可以通过不同的锗酸盐催化剂选择性地还原成所需要的可再生燃料。
(4)将此溶剂体系扩展到镓酸盐纳米结构的制备中,以硝酸镓为镓源,合成了形貌规整大小均,具有3D分级结构的ZnGa2O4微米花,这些微米花是由{110}面暴露比例高达99.6%的超薄纳米片自组装而成。光催化CO2还原实验结果表明,{1110}面暴露的ZnGa2O4纳米片的光催化转换效率是{100}面暴露的立方体纳米晶和{111}面暴露的八面体纳米晶的4倍之多。对这三个表面进行DFT理计计算,发现ZnGa2O4{110}面阳离子密度高有利于CO2吸附,功函低CO2容易活化,从而增强了其CO2还原光催化性能。除此之外,ZnGa2O4微米花独特的3D分级结构也增强了其光催化性能,3D结构使得催化剂具有较大的比表面积,而纳米片的超薄结构也有利于载流子快速从内部迁移到表门面参与光催化反应。
Reduction of CO2to valuable hydrocarbons using solar energy is one of the best solutions to both the global warming and the energy shortage problems. The unique multi-dimensional channel structures of Metal germinates photocatalysts facilitates the separation of photogenerated charge carriers with good photocatalytic performance. The photocatalytic activity of photocatalysts is highly dictated by their sizes, shapes and crystal facets. In this dissertation, some germanate compounds nanomaterials were synthesized in a binary ethylenediamine (En)/water solvent system using a solvothermal route. The formation mechanism and photocatalytic activity of CO2reduction of these nanomaterials were studied. The details are summarized as follows:
(1) Sheaf-like, hyperbranched Zn2GeO4nanoarchitectures were successfully synthesized in this mixed-solvent system. These structures may be assigned to the splitting crystal growth mechanism, resembling some minerals observed in nature. Addition of increasing amounts of En was found to enhance the degree of crystal splitting. Nitridation of the resulting Zn2GeO4superstructures under NH3flow produced yellow Zn1.7GeN1.8O solid solution, which allows photocatalytically converse CO2into CH4in the presence of H2O at ambient conditions under visible light irradiation.
(2) Single-crystalline Zn2GeO4nanobelts with thickness as thin as～7nm (corresponding to five repeating cell units) and aspect ratio up to10,000has been synthesized using this solvothermal route. En can adsorb on solid surfaces and selectively bind to some specific panels to control the velocity and direction of crystal growth, which was termed as the solvent-coordination molecular-template mechanism. The ultralong and ultra-thin geometry of the Zn2GeO4nanoribbon proves to improve the photocatalytic activity toward reduction of CO2in the presence of water vapor into CH4.
(3)A novel, highly crystalline indium germinate hybrid subnanowire, which we denote as In2Ge2O7(En), with general diameters of2-3nm and lengths up to hundreds of nanometres was synthesized in this En/water solvent system. The hybrid ultrathin nanowire exhibits an ultraviolet photoluminescence emission, a dramatic blue shift by more than100nm relative to pure inorganic In2Ge2O7nanowire andmicrotubes. The In2Ge2O7(En) ultrathin nanowire performs selectively the photocatalytic reduction of CO2into CO in the presence of water vapor. With reference to our Zn2GeO4nanoribbon photocatalyst, which was recently used to produce CH4under the same photocatalytic conditions, this work is a significant sign that the greenhouse gas, CO2, can be ameliorated into desirable kinds of renewable fuels using different germinate catalysts.
(4) Well-defined,3D hierarchical microcrystals united with ultrathin ZnGa2O4nanosheets with over99.6%exposed{110} facets with highly active surfaces were deposited in this (En)/water solvent system. The{110}-dominant ZnGa2O4nanosheets proves4-time conversion efficiency of CO2reduction higher than cubic nanocrystals with{100} and octahedral nanocrystals with{111} surfaces. The enhancement of the photocatalytic efficiency is strongly associated with inherent catalytic behavior of {110} surface with high density of cations for CO2absorption and low work function for enhanced CO2activation. In addition, the unique3D hierarchical architecture also promotes the photocatalytic performance through high surface area, ultrathin thickness which allows charge carriers to move rapidly from the interior to the surface to participate in the photoreduction reaction, and improvement of light scattering to be in favor of enhancing the light absorption.
引文
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