空心微球光催化材料的制备与光催化性能研究
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摘要
半导体光催化技术在能源利用和环境净化方面有着广泛的应用前景。光催化剂的光催化活性往往与其形貌紧密相关,其中空心结构的光催化剂由于具有较大的比表面积,较低的密度,以及良好的光催化活性而引起了人们越来越多的重视。各种各样的光催化剂中,TiO2因其良好的氧化能力、无毒、化学稳定性等优点而广为关注,所以二氧化钛空心球已成为材料科学、化学和环境科学等领域的研究热点。但是TiO2有着较大的禁带宽度,仅能利用太阳光中的部分紫外光辐照产生光催化作用,这就严重阻碍了它的广泛应用。半导体光催化剂钒酸铋因为可以实现可见光下降解有机物而成为当前研究的一个新的热点。单斜相钒酸铋的空心结构在可见光光催化领域展现了广阔的应用前景。本文主要是围绕二氧化钛空心球和钒酸铋空心球的合成、表征和性能等方面开展了如下研究：
以硫酸钛为钛源,在硫酸,水和三氟乙酸(TFA)的混合溶液中通过一步无模板的水热法制备出三氟乙酸改性的具有高活性的二氧化钛空心球。通过X射线衍射、X射线光电子能谱、N2吸附-脱附等温线、红外光谱、扫描电子显微镜和透射电子显微镜对所制备的样品进行了表征分析。在紫外灯照射下,二氧化钛表面产生的羟基自由基以对苯二甲酸为分子探针通过荧光技术进行了检测。二氧化钛的光催化活性是通过在紫外光照射下光催化氧化降解空气中的丙酮来检测的。三氟乙酸不仅诱导了空心球的形成,也促进了样品的晶化。三氟乙酸和硫酸钛的摩尔比对光催化活性有显著的影响。当摩尔比在0.5-5之间时,二氧化钛样品的活性都高于P25。在摩尔比等于2时,样品的活性达到最高,超出P25两倍多。这主要是由于空心结构和双峰介孔的球壳促进了光的吸收并加强了反应分子和产物分子的转移和输送。同时,表面吸附的三氟乙酸分子也减少了光生电子和空穴的复合。
在无模板添加剂的情况下,通过在硝酸铋,钒酸铵和水的混合溶液中添加尿素一步无模板水热法制备出单斜相钒酸铋空心球。通过X射线衍射、紫外可见吸收光谱、红外光谱和扫描电子显微镜对所制备的样品进行了表征分析。结果发现,尿素的加入量对钒酸铋的空心球的形成起了关键的作用。所有的样品都是单斜相,并且只有在添加尿素的情况下才有空心球的产生。钒酸铋空心球的形成是基于化学诱导自转变机理。此外,具有较薄球壳的钒酸铋空心球具有最好的光催化活性,这是归因于空心结构的形成。羟基自由基未在反应系统中检测到,说明羟基自由基不是主要的反应活性分子,而是空穴直接氧化。
Semiconductor photocatalysis is a popular technique that has great potential in environmental protection and energy utilization. The photocatalytic activity of photocatalysts always correlates with the morphology of photocatalysts. The photocatalysts with hollow structure have been widely and intensively investigated due to large specific surface area, low density and excellent photocatalytic activity. Among various oxide semiconductors, TiO2 has been proved to be the most suitable photocatalyst for its strong oxidizing power, nontoxicity and long-term stability against photo and chemical corrosion. TiO2 hollow structure has become a hot research covering materials science, chemistry and environmental science. However, because it has large band gap, TiO2 is effective only under ultraviolet irradiation, which restricts its practical application. Semiconductor BiVO4 has received great interest due the photodegradation of organic pollutants under visible light irradiation. Monoclinic-phase BiVO4 hollow structure provides the commercial application. In this dissertation, valuable explorations have been carried out on the synthesis of TiO2 and BiVO4 hollow microspheres, and study of their properties. The main points could be summarized as follows:
Trifluoroacetic acid (TFA) modified TiO2 (TFA-TiO2) hollow microspheres were prepared by one-pot hydrothermal treatment of Ti(SO4)2 in the presence of TFA at 180℃for 12 h. The prepared samples were characterized by X-ray diffraction, scanning and transmission electron microscopy, X-ray photoelectron spectroscopy, N2 adsorption-desorption isotherms and fourier transform infrared. The production rates of·OH on the surface of UV-illuminated TiO2 were detected by a photoluminescence (PL) method using terephthalic acid (TA) as probe molecule. The photocatalytic activity was evaluated by the photocatalytic decomposition of acetone in air under UV light illumination. The results show that TFA not only induces the formation of hollow microspheres, but also enhance their crystallization. The molar ratios of TFA to Ti(SO4)2 (R) have a great influence on photocatalytic activity. When R is in the range of 0.5-5, the photocatalytic activity of the samples is higher than that of commercial Degussa P25 TiO2 powders (P25) and pure TiO2 samples. At R=2, the photocatalytic activity of the sample reaches the highest and exceeds that of P25 by a factor of more than two times. This is ascribed to the fact that the former has hollow interior and bimodal mesoporous shells enhancing harvesting of light and the transfer and transport of reactant and product molecules, also, the surface adsorbed TFA can reduce the recombination of photo-generated electrons and holes.
Monoclinic-phase BiVO4 hollow microspheres have been successfully fabricated in a large scale by one-pot hydrothermal template-free route. X-ray diffraction, scanning electron microscopy, UV/Vis diffuse reflectance spectroscopy, Fourier transform infrared spectrometry, and photoluminescence were used to characterize the products. The results show that the amount of urea added in the hydrothermal reaction and hydrothermal time have been shown to play key roles in the formation of BiVO4 hollow microspheres. all the samples posses the monoclinic phase, and hollow microspheres appear in the presence of urea. Chemically induced self-transformation mechanism for the formation of the BiVO4 hollow spherical structure has been proposed in the observation of hydrothermal time. In addition, BiVO4 hollow microspheres with the thin shell exhibit the higher visible-light photocatalytic activity than other samples due to the formation of hollow structure. Hydroxyl radicals (·OH) were not detected on the surface of BiVO4 under visible-light irradiation by the photoluminescence technique, which indicates that·OH is not the dominant photo-oxidant and a photogenerated hole could instead directly participate in the photocatalytic reaction.
以硫酸钛为钛源,在硫酸,水和三氟乙酸(TFA)的混合溶液中通过一步无模板的水热法制备出三氟乙酸改性的具有高活性的二氧化钛空心球。通过X射线衍射、X射线光电子能谱、N2吸附-脱附等温线、红外光谱、扫描电子显微镜和透射电子显微镜对所制备的样品进行了表征分析。在紫外灯照射下,二氧化钛表面产生的羟基自由基以对苯二甲酸为分子探针通过荧光技术进行了检测。二氧化钛的光催化活性是通过在紫外光照射下光催化氧化降解空气中的丙酮来检测的。三氟乙酸不仅诱导了空心球的形成,也促进了样品的晶化。三氟乙酸和硫酸钛的摩尔比对光催化活性有显著的影响。当摩尔比在0.5-5之间时,二氧化钛样品的活性都高于P25。在摩尔比等于2时,样品的活性达到最高,超出P25两倍多。这主要是由于空心结构和双峰介孔的球壳促进了光的吸收并加强了反应分子和产物分子的转移和输送。同时,表面吸附的三氟乙酸分子也减少了光生电子和空穴的复合。
在无模板添加剂的情况下,通过在硝酸铋,钒酸铵和水的混合溶液中添加尿素一步无模板水热法制备出单斜相钒酸铋空心球。通过X射线衍射、紫外可见吸收光谱、红外光谱和扫描电子显微镜对所制备的样品进行了表征分析。结果发现,尿素的加入量对钒酸铋的空心球的形成起了关键的作用。所有的样品都是单斜相,并且只有在添加尿素的情况下才有空心球的产生。钒酸铋空心球的形成是基于化学诱导自转变机理。此外,具有较薄球壳的钒酸铋空心球具有最好的光催化活性,这是归因于空心结构的形成。羟基自由基未在反应系统中检测到,说明羟基自由基不是主要的反应活性分子,而是空穴直接氧化。
Semiconductor photocatalysis is a popular technique that has great potential in environmental protection and energy utilization. The photocatalytic activity of photocatalysts always correlates with the morphology of photocatalysts. The photocatalysts with hollow structure have been widely and intensively investigated due to large specific surface area, low density and excellent photocatalytic activity. Among various oxide semiconductors, TiO2 has been proved to be the most suitable photocatalyst for its strong oxidizing power, nontoxicity and long-term stability against photo and chemical corrosion. TiO2 hollow structure has become a hot research covering materials science, chemistry and environmental science. However, because it has large band gap, TiO2 is effective only under ultraviolet irradiation, which restricts its practical application. Semiconductor BiVO4 has received great interest due the photodegradation of organic pollutants under visible light irradiation. Monoclinic-phase BiVO4 hollow structure provides the commercial application. In this dissertation, valuable explorations have been carried out on the synthesis of TiO2 and BiVO4 hollow microspheres, and study of their properties. The main points could be summarized as follows:
Trifluoroacetic acid (TFA) modified TiO2 (TFA-TiO2) hollow microspheres were prepared by one-pot hydrothermal treatment of Ti(SO4)2 in the presence of TFA at 180℃for 12 h. The prepared samples were characterized by X-ray diffraction, scanning and transmission electron microscopy, X-ray photoelectron spectroscopy, N2 adsorption-desorption isotherms and fourier transform infrared. The production rates of·OH on the surface of UV-illuminated TiO2 were detected by a photoluminescence (PL) method using terephthalic acid (TA) as probe molecule. The photocatalytic activity was evaluated by the photocatalytic decomposition of acetone in air under UV light illumination. The results show that TFA not only induces the formation of hollow microspheres, but also enhance their crystallization. The molar ratios of TFA to Ti(SO4)2 (R) have a great influence on photocatalytic activity. When R is in the range of 0.5-5, the photocatalytic activity of the samples is higher than that of commercial Degussa P25 TiO2 powders (P25) and pure TiO2 samples. At R=2, the photocatalytic activity of the sample reaches the highest and exceeds that of P25 by a factor of more than two times. This is ascribed to the fact that the former has hollow interior and bimodal mesoporous shells enhancing harvesting of light and the transfer and transport of reactant and product molecules, also, the surface adsorbed TFA can reduce the recombination of photo-generated electrons and holes.
Monoclinic-phase BiVO4 hollow microspheres have been successfully fabricated in a large scale by one-pot hydrothermal template-free route. X-ray diffraction, scanning electron microscopy, UV/Vis diffuse reflectance spectroscopy, Fourier transform infrared spectrometry, and photoluminescence were used to characterize the products. The results show that the amount of urea added in the hydrothermal reaction and hydrothermal time have been shown to play key roles in the formation of BiVO4 hollow microspheres. all the samples posses the monoclinic phase, and hollow microspheres appear in the presence of urea. Chemically induced self-transformation mechanism for the formation of the BiVO4 hollow spherical structure has been proposed in the observation of hydrothermal time. In addition, BiVO4 hollow microspheres with the thin shell exhibit the higher visible-light photocatalytic activity than other samples due to the formation of hollow structure. Hydroxyl radicals (·OH) were not detected on the surface of BiVO4 under visible-light irradiation by the photoluminescence technique, which indicates that·OH is not the dominant photo-oxidant and a photogenerated hole could instead directly participate in the photocatalytic reaction.
引文
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