钨酸盐微/纳米材料的控制合成及性能研究
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摘要
本论文旨在研究金属钨酸盐微／纳米材料的控制合成、机理及性质。分别以KN03溶液和蒸馏水为溶剂用水热法成功制备了3D分级结构Bi2WO6微球和八面体Bi2WO6,探讨了3D分级结构Bi2WO6微球的形成机理；利用简单的水热法制备了新颖复合体系ZnWO4-Cu和ZnWO4-Cu2O,探讨了Cu在光催化与类芬顿协同效应中的作用；利用水热法在较为温和的条件下制备了介稳结构的立方ZrW2O8,分析了不同反应条件对产物的影响,并通过掺杂少量的钼,合成在室温条件下具有高温立方β相结构的ZrMoxW2-xO8材料。
论文主要内容概述如下：
1、3D分级结构Bi2WO6微球的控制合成及光催化性质
分别以KN03溶液和蒸馏水为溶剂,利用水热法制备了3D分级结构Bi2WO6微球和八面体Bi2WO6。通过X射线粉末衍射(XRD)、扫描电镜(SEM)、紫外一可见漫反射光谱(DRS)、比表面(BET)对产物进行表征。实验表明,KN03在控制合成3D分级结构Bi2WO6微球的过程中起到重要的作用。通过调节KN03溶液的浓度,我们推测Bi2WO6的3D微球是由晶核向外有取向生长而成,而不是由纳米片自组装形成的。以光催化降解亚甲基蓝为模型,研究了合成产物的光催化性能。结果表明八面体钨酸铋和钨酸铋微球对亚甲基蓝的脱色率分别达33.56%和99.17%,主要是因为Bi2WO6微球具有大的比表面积和特殊的分级结构。比表面积较大,电子空穴对的分离效率高；特殊的分级结构和孔结构不仅能提供丰富的有机小分子通道,还能提高光的利用率。进一步以吡啶为探针分子,通过吸附毗啶红外光谱探讨了Bi2WO6的表面酸性与光催化之间的关系。研究显示,Bi2WO6具有较强的表面酸性,增强了Bi2WO6与RhB分子之问吸附作用,有利于染料分子上的电子跃迁至催化剂上,易于发生光敏化和光催化反应。
2、新颖复合体系ZnWO4-Cu的制备及光催化.类芬顿协同效应
采用水热法成功合成了新颖的复合体系ZnWO4-Cu,合成方法简单,绿色环保。利用XRD、TEM和XPS对产物进行了详细的表征。以亚甲基蓝为模型污染物,在紫外光下研究了产物的光催化性能。结果表明：由于光催化和类芬顿协同作用的影响,ZnWO4-Cu的光催化活性明显优于纯ZnWO4,且Cu和ZnWO4摩尔比是0.2的样品光催化活性最高。在光催化降解MB的过程中,Cu起到了非常重要的作用。一方面Cu与H2O2反应产生羟基自由基进而氧化MB；另一方面Cu+和Cu2+作为电子捕获剂,捕获ZnWO4在紫外光照射下产生的电子,降低光生电子和空穴对的复合率,从而提高产物光催化活性。此外,详细的讨论了Cu的复合量对ZnWO4光催化活性的影响,当复合过量的Cu时,ZnWO4-Cu的光催化活性明显降低,原因在于金属Cu表面形成的钝化层不能够及时的捕获光生电子还原成Cu,使Cu+/Cu2+成为光生电子和空穴的再复合中心,降低催化剂的光催化活性。进一步提出可能的光催化降解机理。本文还采用水热法制备了复合体系ZnWO4-Cu2O,以亚甲基蓝为模型污染物,在太阳光下研究了产物的光催化性能。对于样品ZnC-0、 ZnC-0.1、ZnC-0.2和ZnC-0.3, MB的脱色率分别为46.54%、78.5%、88.34%和76.53%,并探讨了Cu20复合量对产物光催化活性的影响。
3、负热膨胀材料ZrW2O8和ZrW1.4Mo0.6O8的水热合成
作为一种性能优异的各向同性负热膨胀材料,立方相ZrW2O8备受世人关注。但ZrW2O8处于介稳态,热稳定范围很窄,合成较为困难。本文采用水热法在较温和的条件下制备了介稳的立方ZrW2O8。利用XRD、SEM、FT-IR等手段对产物进行表征。分析了不同反应条件对产物的影响,并对合成条件作出了优化。通过掺杂少量的钼,合成在室温条件就具有高温立方p相结构的ZrMoxW2-xO8材料。
In this thesis, the Synthesis, Mechanism and Properties of Micro-/Nano-Materials of Tungstate were investigated. Three-dimensional (3D) hierarchical Bi2WO6microsphere and octahedral Bi2WO6have been synthesized by a facile hydrothermal method using KNO3solution and distill water as solvent, respectively. A possible mechanism on the formation of Bi2WO6microsphere was proposed; A novel coupled system of ZnWO4-Cu and ZnWO4-Cu2O were successfully synthesized by the hydrothermal method. The effects of the amount of Cu on the photocatalytic performance of ZnWO4-Cu were investigated in detail. The cubic ZrW2O8was successfully synthesized by hydrothermal method with mild conditions, and the influence of synthetic conditions on the outcome was discussed. ZrMoxW2-xO8this had the cubic β-ZrW2O8structure at room temperature was successfully synthesized by doping a certain proportion of Mo.
The details are summarized as follows:
1. Controlled Synthesis of Three-Dimensional Hierarchical Bi2WO6Microspheres with Optimum Photocatalytic Activity
Three-dimensional (3D) hierarchical Bi2WO6microsphere and octahedral Bi2WO6have been synthesized by a facile hydrothermal method using KNO3solution and distill water as solvent, respectively. The obtained products were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), N2adsorption/desorption (BET), and UV-vis diffuse reflectance spectroscopy (DRS) in detail. The concentrated KNO3played a key role for the formation of3D Bi2WO6hierarchical microspheres. By changing the concentration of KNO3solution, we deduced that3D hierarchical Bi2WO6microsphere was produced through crystal plane-selective growth starting from cores, not through aggregation of rectangular platelets which were produced independently. The photocatalytic activity of the as-synthesized products was evaluated by monitoring the degradation of MB solution. The decoloration ratio of MB was33.56%and99.17%respectively for the octahedral Bi2WO6and Bi2WO6microsphere, which was attributed to the larger surface area and special hierarchical structure of Bi2WO6microsphere. For large surface area, the ratio of the surface charge carrier transfer rate to the electron-hole recombination rate could be greatly improved. The hierarchical architecture with large surface area and pore system not only improved the molecular transport of reactants, but also allowed more efficient light harvesting. By pyridine adsorption, the surface acidity of catalyst Bi2WO6was measured using infrared spectroscopy. The relationship between surface acidity of Bi2WO6and photocatalytic degradation of RhB was explored. It was found that the more surface acid sites of Bi2WO6, the stronger adsorption between with RhB and Bi2WO6. Consequently, the photogenerated electrons on the dye could more easily transfer to the photocatalyst, leading to the photosensitization and photocatalysis.
2. ZnWO4-Cu System with Enhanced Photocatalytic Activity by Photo-Fenton-Like Synergistic Reaction
A novel coupled system of ZnWO4-Cu was successfully synthesized by the hydrothermal method. The synthesis was simple and green. The as-synthesized samples were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM) and X-ray photoelectron spectroscopy (XPS). The photocatalytic activity was evaluated by monitoring the degradation of MB solution under UV light irradiation. The catalytic activity of ZnWO4-Cu was much higher than that of bare ZnWO4and the photocatalytic activity of the ZC-0.2was best, which was attributed to the synergistic effect between photocatalysis and Fenton-like process. Cu played a key role in the process of photocatalytic degradation of MB. The copper reagent not only served as a heterogeneous catalyst for the decomposition of H2O2so as to generate hydroxyl radicals to attack the contaminants, but also acted as an electron shuttle that promoted the separation of the photogenerated carriers. Furthermore, the effects of the amount of Cu on the photocatalytic performance of ZnWO4-Cu were investigated in detail. The photocatalytic degradation ratio of MB decreased when too much Cu was introduced which was attributed to the passivation layer on the Cu surface could not be reduced timely by the photogenerated electron. The redundant Cu+/Cu2+may react with both photogenerated electrons and holes as recombination center, thereby make the photocatalytic activity of ZnWO4decreased.The possible mechanism of the synergistic system was proposed. A coupled system of ZnWO4-Cu2O was synthesized by the hydrothermal method. The photocatalytic activity was evaluated by monitoring the degradation of MB solution under sunlight irradiation. The degradation ratio of MB was46.54%、78.5%、88.34%and76.53%respectively for ZnC-0, ZnC-0.1, ZC-0.2and ZC-0.3. The effects of the amount of Cu2O on the photocatalytic performance of ZnWO4-Cu2O were investigated.
3. Hydrothermal synthesis of negative thermal expansion ZrW2O8and ZrMoxW2-xO8
As an excellent kind of isotropic negative thermal expansion materials, cubic ZrW2O8is coming to be people's concern. But it is difficult to be synthesized because it is metastable and has narrow thermodynamic stability range.The cubic ZrW2O8was successfully synthesized by hydrothermal method with mild conditions. The obtained products were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) and Fourier transform infrared spectrometer (FT-IR). The influence of synthetic conditions on the outcome was discussed and made optimization in this passage. ZrMoxW2-xO8this had the cubic β-ZrW2O8structure at room temperature was successfully synthesized by doping a certain proportion of Mo.
论文主要内容概述如下：
1、3D分级结构Bi2WO6微球的控制合成及光催化性质
分别以KN03溶液和蒸馏水为溶剂,利用水热法制备了3D分级结构Bi2WO6微球和八面体Bi2WO6。通过X射线粉末衍射(XRD)、扫描电镜(SEM)、紫外一可见漫反射光谱(DRS)、比表面(BET)对产物进行表征。实验表明,KN03在控制合成3D分级结构Bi2WO6微球的过程中起到重要的作用。通过调节KN03溶液的浓度,我们推测Bi2WO6的3D微球是由晶核向外有取向生长而成,而不是由纳米片自组装形成的。以光催化降解亚甲基蓝为模型,研究了合成产物的光催化性能。结果表明八面体钨酸铋和钨酸铋微球对亚甲基蓝的脱色率分别达33.56%和99.17%,主要是因为Bi2WO6微球具有大的比表面积和特殊的分级结构。比表面积较大,电子空穴对的分离效率高；特殊的分级结构和孔结构不仅能提供丰富的有机小分子通道,还能提高光的利用率。进一步以吡啶为探针分子,通过吸附毗啶红外光谱探讨了Bi2WO6的表面酸性与光催化之间的关系。研究显示,Bi2WO6具有较强的表面酸性,增强了Bi2WO6与RhB分子之问吸附作用,有利于染料分子上的电子跃迁至催化剂上,易于发生光敏化和光催化反应。
2、新颖复合体系ZnWO4-Cu的制备及光催化.类芬顿协同效应
采用水热法成功合成了新颖的复合体系ZnWO4-Cu,合成方法简单,绿色环保。利用XRD、TEM和XPS对产物进行了详细的表征。以亚甲基蓝为模型污染物,在紫外光下研究了产物的光催化性能。结果表明：由于光催化和类芬顿协同作用的影响,ZnWO4-Cu的光催化活性明显优于纯ZnWO4,且Cu和ZnWO4摩尔比是0.2的样品光催化活性最高。在光催化降解MB的过程中,Cu起到了非常重要的作用。一方面Cu与H2O2反应产生羟基自由基进而氧化MB；另一方面Cu+和Cu2+作为电子捕获剂,捕获ZnWO4在紫外光照射下产生的电子,降低光生电子和空穴对的复合率,从而提高产物光催化活性。此外,详细的讨论了Cu的复合量对ZnWO4光催化活性的影响,当复合过量的Cu时,ZnWO4-Cu的光催化活性明显降低,原因在于金属Cu表面形成的钝化层不能够及时的捕获光生电子还原成Cu,使Cu+/Cu2+成为光生电子和空穴的再复合中心,降低催化剂的光催化活性。进一步提出可能的光催化降解机理。本文还采用水热法制备了复合体系ZnWO4-Cu2O,以亚甲基蓝为模型污染物,在太阳光下研究了产物的光催化性能。对于样品ZnC-0、 ZnC-0.1、ZnC-0.2和ZnC-0.3, MB的脱色率分别为46.54%、78.5%、88.34%和76.53%,并探讨了Cu20复合量对产物光催化活性的影响。
3、负热膨胀材料ZrW2O8和ZrW1.4Mo0.6O8的水热合成
作为一种性能优异的各向同性负热膨胀材料,立方相ZrW2O8备受世人关注。但ZrW2O8处于介稳态,热稳定范围很窄,合成较为困难。本文采用水热法在较温和的条件下制备了介稳的立方ZrW2O8。利用XRD、SEM、FT-IR等手段对产物进行表征。分析了不同反应条件对产物的影响,并对合成条件作出了优化。通过掺杂少量的钼,合成在室温条件就具有高温立方p相结构的ZrMoxW2-xO8材料。
In this thesis, the Synthesis, Mechanism and Properties of Micro-/Nano-Materials of Tungstate were investigated. Three-dimensional (3D) hierarchical Bi2WO6microsphere and octahedral Bi2WO6have been synthesized by a facile hydrothermal method using KNO3solution and distill water as solvent, respectively. A possible mechanism on the formation of Bi2WO6microsphere was proposed; A novel coupled system of ZnWO4-Cu and ZnWO4-Cu2O were successfully synthesized by the hydrothermal method. The effects of the amount of Cu on the photocatalytic performance of ZnWO4-Cu were investigated in detail. The cubic ZrW2O8was successfully synthesized by hydrothermal method with mild conditions, and the influence of synthetic conditions on the outcome was discussed. ZrMoxW2-xO8this had the cubic β-ZrW2O8structure at room temperature was successfully synthesized by doping a certain proportion of Mo.
The details are summarized as follows:
1. Controlled Synthesis of Three-Dimensional Hierarchical Bi2WO6Microspheres with Optimum Photocatalytic Activity
Three-dimensional (3D) hierarchical Bi2WO6microsphere and octahedral Bi2WO6have been synthesized by a facile hydrothermal method using KNO3solution and distill water as solvent, respectively. The obtained products were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), N2adsorption/desorption (BET), and UV-vis diffuse reflectance spectroscopy (DRS) in detail. The concentrated KNO3played a key role for the formation of3D Bi2WO6hierarchical microspheres. By changing the concentration of KNO3solution, we deduced that3D hierarchical Bi2WO6microsphere was produced through crystal plane-selective growth starting from cores, not through aggregation of rectangular platelets which were produced independently. The photocatalytic activity of the as-synthesized products was evaluated by monitoring the degradation of MB solution. The decoloration ratio of MB was33.56%and99.17%respectively for the octahedral Bi2WO6and Bi2WO6microsphere, which was attributed to the larger surface area and special hierarchical structure of Bi2WO6microsphere. For large surface area, the ratio of the surface charge carrier transfer rate to the electron-hole recombination rate could be greatly improved. The hierarchical architecture with large surface area and pore system not only improved the molecular transport of reactants, but also allowed more efficient light harvesting. By pyridine adsorption, the surface acidity of catalyst Bi2WO6was measured using infrared spectroscopy. The relationship between surface acidity of Bi2WO6and photocatalytic degradation of RhB was explored. It was found that the more surface acid sites of Bi2WO6, the stronger adsorption between with RhB and Bi2WO6. Consequently, the photogenerated electrons on the dye could more easily transfer to the photocatalyst, leading to the photosensitization and photocatalysis.
2. ZnWO4-Cu System with Enhanced Photocatalytic Activity by Photo-Fenton-Like Synergistic Reaction
A novel coupled system of ZnWO4-Cu was successfully synthesized by the hydrothermal method. The synthesis was simple and green. The as-synthesized samples were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM) and X-ray photoelectron spectroscopy (XPS). The photocatalytic activity was evaluated by monitoring the degradation of MB solution under UV light irradiation. The catalytic activity of ZnWO4-Cu was much higher than that of bare ZnWO4and the photocatalytic activity of the ZC-0.2was best, which was attributed to the synergistic effect between photocatalysis and Fenton-like process. Cu played a key role in the process of photocatalytic degradation of MB. The copper reagent not only served as a heterogeneous catalyst for the decomposition of H2O2so as to generate hydroxyl radicals to attack the contaminants, but also acted as an electron shuttle that promoted the separation of the photogenerated carriers. Furthermore, the effects of the amount of Cu on the photocatalytic performance of ZnWO4-Cu were investigated in detail. The photocatalytic degradation ratio of MB decreased when too much Cu was introduced which was attributed to the passivation layer on the Cu surface could not be reduced timely by the photogenerated electron. The redundant Cu+/Cu2+may react with both photogenerated electrons and holes as recombination center, thereby make the photocatalytic activity of ZnWO4decreased.The possible mechanism of the synergistic system was proposed. A coupled system of ZnWO4-Cu2O was synthesized by the hydrothermal method. The photocatalytic activity was evaluated by monitoring the degradation of MB solution under sunlight irradiation. The degradation ratio of MB was46.54%、78.5%、88.34%and76.53%respectively for ZnC-0, ZnC-0.1, ZC-0.2and ZC-0.3. The effects of the amount of Cu2O on the photocatalytic performance of ZnWO4-Cu2O were investigated.
3. Hydrothermal synthesis of negative thermal expansion ZrW2O8and ZrMoxW2-xO8
As an excellent kind of isotropic negative thermal expansion materials, cubic ZrW2O8is coming to be people's concern. But it is difficult to be synthesized because it is metastable and has narrow thermodynamic stability range.The cubic ZrW2O8was successfully synthesized by hydrothermal method with mild conditions. The obtained products were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) and Fourier transform infrared spectrometer (FT-IR). The influence of synthetic conditions on the outcome was discussed and made optimization in this passage. ZrMoxW2-xO8this had the cubic β-ZrW2O8structure at room temperature was successfully synthesized by doping a certain proportion of Mo.
引文
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