以TiO_2光催化剂为基的过渡金属氧化物结构和性能的研究
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摘要
本论文的主要工作是基于探索在异相催化反应中,尤其是在目前比较热门的光催化反应研究领域中,催化剂的结构和其催化性能之间的相互关系。半导体材料Ti02具有廉价,无毒,化学性质稳定,降解有机物彻底等优点,被广泛地应用于光催化领域。本论文即以不同的制备方法,合成具备一定功能的TiO2光催化剂,并将其应用于吸附,酸催化以及光催化反应,研究经不同制备方法合成的具有特殊结构的Ti02光催化剂,其吸附、催化性能与其结构之间的相互关系,探讨催化学科中构效关系这一基础问题。主要结果如下：
1.利用溶胶凝胶法制备了不同Ce含量的CeO2-TiO2过渡金属复合氧化物,研究了此种复合氧化物界面和表面的结构,以及这种特殊结构对于有机染料甲基橙的吸附性能影响。通过XRD、可见光激发Raman和紫外光激发Raman、XPS、SEM等常规表征,以及同步辐射XAFS表征,我们发现此复合氧化物系列有如下特征：Ce未进入Ti02晶格,当Ce含量较低时,Ce会在Ti02内部氧缺陷成核,并随Ce含量增加形成Ce02萤石结构,Ce在界面上会首先形成Ce-O-Ti结构,并且少量Ce的加入对TiO2的局域结构和锐钛矿相的相稳定即可起很大的作用。CeO2-TiO2复合氧化物中Ti02是表面富集的,Ce02则分布在相对较内层,这种体相-表面组成分布的不均匀不仅可以由上述表征手段,如XRD、紫外拉曼和可见拉曼、XPS综合得出,也可由此复合氧化物在不同Ce含量时,对于甲基橙的化学选择吸附的差异而看出。藉由纯Ti02和纯CeO2对有机染料甲基橙吸附性能的巨大差异,我们发现了一种简单的化学选择性吸附方法,通过对比不同Ce含量的复合氧化物对甲基橙吸附的特点,来确定复合氧化物的表面组成。并且我们已经将这种方法成功的应用到了几个其他相似的体系,包括CeO2-Fe2O3, CeO2-ZrO2等。我们希望通过这种简单的方法可以有效的确定复杂的复合氧化物体系的表面组成。
2.利用共沉淀法制备了不同Ce含量的CeO2-TiO2过渡金属复合氧化物,通过XRD、EXAFS等研究方法表征了其体相、表面和界面结构,发现一定的Ce/Ti比可形成固溶体结构,如Ceo.3Ti0.7O2这种特殊的单斜晶体固溶体结构。复合氧化物随着Ce含量的增加,由于固溶体生成,其结构表现出更加复杂的变化趋势。由H2-TPR和CO-TPR结果表明,固溶体样品的氧化还原性由于其结构的特殊关系并不同于其他复合氧化物样品,复合氧化物和固溶体样品的储氧能力均大于纯的Ce02样品。CO-TPR中发现了水汽变换现象,这可能与样品表面的羟基浓度有关。此种方法制备的复合氧化物,对甲基橙的吸附能力随着Ce含量的增加而增大。各复合氧化物对甲基橙的吸附主要是依靠Ce02的吸附作用,因此,表面组成的变化是影响复合氧化物和固溶体吸附性能的主要因素。化学选择吸附方法也可用于这个体系的样品表面组成测定。
CeO2-TiO2复合氧化物体系均未表现出好的光降解甲基橙的催化活性,这可能与样品制备方法,反应体系的选择,反应装置的效率都有关系。
3.低温下,以[TiO(C2O4)2]2-为反应物,经氨水沉淀后得前驱体,不同温度焙烧后得到掺杂N元素的Ti02光催化剂。结果表明：制得的Ti02光催化剂都是锐钛矿相样品,且N元素在Ti02晶格间隙位掺杂,由于掺杂导致的光照响应波长范围已经明显进入了可见光区域。经程序升温反应实验,我们发现400℃焙烧样品表面有共价草酸基团,存在Bronsted酸性位。各样品对甲基橙的光催化降解都有比较好的活性,而且400℃焙烧的样品因为其酸性,对甲基橙有较好的吸附作用,是一种具有酸催化和光催化的双功能催化剂。
4.以硫酸氧钛铵为前躯体,通过不同温度焙烧一步法合成了掺杂N,S非金属元素的Ti02光催化剂。800℃焙烧样品仍能保持锐钛矿相结构,有较好的晶体稳定性。XPS结果表明样品均为四价S阳离子掺杂,且600℃焙烧样品为N、S双掺,且N处于Ti02晶格间隙位。这种N、S的掺杂并未明显减小样品的禁带宽度。通过NH3-TPD和1H固体核磁共振谱表征,600℃焙烧样品表面有较多的磺酸酸性基团构成的Bronsted酸性位。通过光降解有机染料甲基橙和光解水制氢来检测各个光催化剂的催化活性。不同温度焙烧的样品在全波长光下均对甲基橙降解有比较好的催化活性,其中600℃焙烧样品活性最优,好于商品化的P25。可见光下,由于掺杂的原因,各样品均对甲基橙有光降解作用。在担载Pt之后,催化剂全波长光照下光解水产氢活性有了明显提高。而由于担载Pt和N、S元素掺杂的共同作用,可以一定程度上提高Ti02可见光下产氢活性。600℃焙烧样品为N、S双掺,表面又有磺酸酸性基团构成的Bronsted酸性位,因此其是同时具有酸催化和光催化性质的双功能催化剂。其在酯化反应中对乙酸乙酯的生成有很好的催化作用,而在可见光下对降解甲基橙以及光解水制氢也有很好的活性,是一种很具应用前景的双功能催化剂。
The major work in this dissertation is focused on the study of the relationships between the structures and the catalytical properties of the catalysts in the heterogeneous catalysis, especially in photocatalysis, which is one of the hot research fields these years. Semiconductor material TiO2 is low-cost, non-toxic, chemically stable, and it can photodegrade the organic pollutants completely. So it has been widely used in photocatalysis. In this dissertation, We have prepared the TiO2 photocatalyst with certain functions by different methods, and it has been utilized in adsorption, acid-catalysis and photocatalysis. We have investigated the adsorption, catalytical properties of these TiO2 photocatalysts, and the relationships between the structures and the properties of these catalysts.
1. The preparation of CeO2-TiO2 transition metal composite oxides with different Ce contents via sol-gel-method. We investigated the interfacial/surface structures of the composites, and the adsorption ability toward methyl orange based on the unique structure. Based on the results of XRD, UV-Raman and Visible-Raman, XPS, XAFS, we found that:Ce do not enter the TiO2 lattice, Ce first nucleated at the defects in the bulk of TiO2, as the Ce content increased, it formed the CeO2 fluorite structure. On the interface, Ce-O-Ti bond formed, a few amount of Ce can stabilize the local structure and anatase phase of TiO2. In CeO2-TiO2 composite oxides, TiO2 is rich in surface, and CeO2 is distributed in inner layer. It was concluded not only from these characterization techniques above, but also from the selective chemisorption toward methyl orange by the composite oxides. Based on the distinguished differences of the adsorption ability toward methyl orange between CeO2 and TiO2, we developed a facile method to identify the surface composition of the CeO2-TiO2 composite oxides, and we have broaden the application to other composite oxides, like CeO2-Fe2O3, CeO2-ZrO2 et al. We hope that the surface composition of complex composite oxides can easily identified by this method.
2. The preparation of CeO2-TiO2 transition metal composite oxides with different Ce via co-precipitation method. We have investigated the bulk, surface and interface structures of the composite oxides by XRD, XAFS et al. the solid solution could formed, like the Ce/Ti ratio 3:7, Ce0.3Ti0.7O2 is a monoclinic solid solution. As the Ce content increased, because of the formation of the solid solution, the structure evolution of the composite oxides is more complicated. The results of H2-TPR and CO-TPR show that the redox properties of solid solution are different with other composite oxides based on the unique structure. The oxygen storage ability of composite oxides and solid solution is better than CeO2. We found water-gas reaction in CO-TPR, it is related to the concentration of the hydroxyl groups on the surface of the composite oxides. The adsorption ability toward methyl orange by the composite oxides become stronger as the increasing of the Ce content. CeO2 is the main component that adsorbed methyl orange, thus the evolution of the surface components is the main point that effect the adsorption properties of the composite oxides.
The photocatalytic activity of the CeO2-TiO2 composite oxides for the photodegradation of methyl orange is low. It could be the preparation method, the type of the photocatalytic reaction, or the efficiency of the experiment's equipment that needed the further study.
3. The N-doped TiO2 photocatalysts have been prepared by clacination of the precusors at different temperature, which was synthesized via the precipitation of [TiO(C2O4)2]2-by ammonium hydroxide at low temperature. The results shows that all the photocatalysts are anatase phase, N is doped at the interstitial sites in TiO2 lattice, and because of this N doping, the light response of these photocatalysts is moved into the visible light region. Based on the TPRS results, we found that the photocatalyst calcined at 400℃is covalently bonded with oxalate groups on the surface to form Bronsted acid sites. All photocatalysts are performed well in the photocatalytic reaction for the degradation of methyl orange. The photocatalyst calcined at 400℃could adsorb methyl orange effectively because of the acidity, and it is an acid-catalysis and photocatalysis bi-funcitional catalyst.
4. We developed an one-step method to prepare N,S co-doped TiO2 photocatalyst via the controlled thermal decomposition of ammonium titanyl sulfate. the photocatalyst calcined at 800 C is still anatase, shows the phase stabilization ability. The results of XPS show that the photocatalysts are all S(IV) cation doping, the photocatalyst calcined at 600℃is co-doped with N,S and N is at the interstitial sites in TiO2 lattices. The band gap of TiO2 is not narrowed down by these doping. Based on the results of NH3-TPD and 1H soild-state MAS NMR, the photocatalyst calcined at 600 C is covalently bonded with the sulfate acid groups on the surface to form Bronsted acid sites. The evaluation of the photocatalytic activity is conducted by the photodegradation of methyl orange and photolysis of water for H2 production. Under all-wavelength light illumination, the photocatalytic activity of the photodegradation of methyl orange is well for all the photocatalysts, the photocatalyst calcined at 600℃is most active, better than the commercial P25. All the photocatalysts could degrade methyl orange under visible light illumination because of the N, S doping. After Pt loading, the H2 production under all-wavelength light illumination by the photocatalysts increased dramatically compared with the bare TiO2. Because of the synergy effect of Pt loading and the N, S co-doping, the 0.1Pt/TiO2 shows an improved photocatalytic activity for H2 production. the photocatalyst calcined at 600℃is both very active in the esterification for the ethyl acetate production and the photocatalytic reactions. So it is a acid-catalysis and photocatalysis bi-functional catalyst.
1.利用溶胶凝胶法制备了不同Ce含量的CeO2-TiO2过渡金属复合氧化物,研究了此种复合氧化物界面和表面的结构,以及这种特殊结构对于有机染料甲基橙的吸附性能影响。通过XRD、可见光激发Raman和紫外光激发Raman、XPS、SEM等常规表征,以及同步辐射XAFS表征,我们发现此复合氧化物系列有如下特征：Ce未进入Ti02晶格,当Ce含量较低时,Ce会在Ti02内部氧缺陷成核,并随Ce含量增加形成Ce02萤石结构,Ce在界面上会首先形成Ce-O-Ti结构,并且少量Ce的加入对TiO2的局域结构和锐钛矿相的相稳定即可起很大的作用。CeO2-TiO2复合氧化物中Ti02是表面富集的,Ce02则分布在相对较内层,这种体相-表面组成分布的不均匀不仅可以由上述表征手段,如XRD、紫外拉曼和可见拉曼、XPS综合得出,也可由此复合氧化物在不同Ce含量时,对于甲基橙的化学选择吸附的差异而看出。藉由纯Ti02和纯CeO2对有机染料甲基橙吸附性能的巨大差异,我们发现了一种简单的化学选择性吸附方法,通过对比不同Ce含量的复合氧化物对甲基橙吸附的特点,来确定复合氧化物的表面组成。并且我们已经将这种方法成功的应用到了几个其他相似的体系,包括CeO2-Fe2O3, CeO2-ZrO2等。我们希望通过这种简单的方法可以有效的确定复杂的复合氧化物体系的表面组成。
2.利用共沉淀法制备了不同Ce含量的CeO2-TiO2过渡金属复合氧化物,通过XRD、EXAFS等研究方法表征了其体相、表面和界面结构,发现一定的Ce/Ti比可形成固溶体结构,如Ceo.3Ti0.7O2这种特殊的单斜晶体固溶体结构。复合氧化物随着Ce含量的增加,由于固溶体生成,其结构表现出更加复杂的变化趋势。由H2-TPR和CO-TPR结果表明,固溶体样品的氧化还原性由于其结构的特殊关系并不同于其他复合氧化物样品,复合氧化物和固溶体样品的储氧能力均大于纯的Ce02样品。CO-TPR中发现了水汽变换现象,这可能与样品表面的羟基浓度有关。此种方法制备的复合氧化物,对甲基橙的吸附能力随着Ce含量的增加而增大。各复合氧化物对甲基橙的吸附主要是依靠Ce02的吸附作用,因此,表面组成的变化是影响复合氧化物和固溶体吸附性能的主要因素。化学选择吸附方法也可用于这个体系的样品表面组成测定。
CeO2-TiO2复合氧化物体系均未表现出好的光降解甲基橙的催化活性,这可能与样品制备方法,反应体系的选择,反应装置的效率都有关系。
3.低温下,以[TiO(C2O4)2]2-为反应物,经氨水沉淀后得前驱体,不同温度焙烧后得到掺杂N元素的Ti02光催化剂。结果表明：制得的Ti02光催化剂都是锐钛矿相样品,且N元素在Ti02晶格间隙位掺杂,由于掺杂导致的光照响应波长范围已经明显进入了可见光区域。经程序升温反应实验,我们发现400℃焙烧样品表面有共价草酸基团,存在Bronsted酸性位。各样品对甲基橙的光催化降解都有比较好的活性,而且400℃焙烧的样品因为其酸性,对甲基橙有较好的吸附作用,是一种具有酸催化和光催化的双功能催化剂。
4.以硫酸氧钛铵为前躯体,通过不同温度焙烧一步法合成了掺杂N,S非金属元素的Ti02光催化剂。800℃焙烧样品仍能保持锐钛矿相结构,有较好的晶体稳定性。XPS结果表明样品均为四价S阳离子掺杂,且600℃焙烧样品为N、S双掺,且N处于Ti02晶格间隙位。这种N、S的掺杂并未明显减小样品的禁带宽度。通过NH3-TPD和1H固体核磁共振谱表征,600℃焙烧样品表面有较多的磺酸酸性基团构成的Bronsted酸性位。通过光降解有机染料甲基橙和光解水制氢来检测各个光催化剂的催化活性。不同温度焙烧的样品在全波长光下均对甲基橙降解有比较好的催化活性,其中600℃焙烧样品活性最优,好于商品化的P25。可见光下,由于掺杂的原因,各样品均对甲基橙有光降解作用。在担载Pt之后,催化剂全波长光照下光解水产氢活性有了明显提高。而由于担载Pt和N、S元素掺杂的共同作用,可以一定程度上提高Ti02可见光下产氢活性。600℃焙烧样品为N、S双掺,表面又有磺酸酸性基团构成的Bronsted酸性位,因此其是同时具有酸催化和光催化性质的双功能催化剂。其在酯化反应中对乙酸乙酯的生成有很好的催化作用,而在可见光下对降解甲基橙以及光解水制氢也有很好的活性,是一种很具应用前景的双功能催化剂。
The major work in this dissertation is focused on the study of the relationships between the structures and the catalytical properties of the catalysts in the heterogeneous catalysis, especially in photocatalysis, which is one of the hot research fields these years. Semiconductor material TiO2 is low-cost, non-toxic, chemically stable, and it can photodegrade the organic pollutants completely. So it has been widely used in photocatalysis. In this dissertation, We have prepared the TiO2 photocatalyst with certain functions by different methods, and it has been utilized in adsorption, acid-catalysis and photocatalysis. We have investigated the adsorption, catalytical properties of these TiO2 photocatalysts, and the relationships between the structures and the properties of these catalysts.
1. The preparation of CeO2-TiO2 transition metal composite oxides with different Ce contents via sol-gel-method. We investigated the interfacial/surface structures of the composites, and the adsorption ability toward methyl orange based on the unique structure. Based on the results of XRD, UV-Raman and Visible-Raman, XPS, XAFS, we found that:Ce do not enter the TiO2 lattice, Ce first nucleated at the defects in the bulk of TiO2, as the Ce content increased, it formed the CeO2 fluorite structure. On the interface, Ce-O-Ti bond formed, a few amount of Ce can stabilize the local structure and anatase phase of TiO2. In CeO2-TiO2 composite oxides, TiO2 is rich in surface, and CeO2 is distributed in inner layer. It was concluded not only from these characterization techniques above, but also from the selective chemisorption toward methyl orange by the composite oxides. Based on the distinguished differences of the adsorption ability toward methyl orange between CeO2 and TiO2, we developed a facile method to identify the surface composition of the CeO2-TiO2 composite oxides, and we have broaden the application to other composite oxides, like CeO2-Fe2O3, CeO2-ZrO2 et al. We hope that the surface composition of complex composite oxides can easily identified by this method.
2. The preparation of CeO2-TiO2 transition metal composite oxides with different Ce via co-precipitation method. We have investigated the bulk, surface and interface structures of the composite oxides by XRD, XAFS et al. the solid solution could formed, like the Ce/Ti ratio 3:7, Ce0.3Ti0.7O2 is a monoclinic solid solution. As the Ce content increased, because of the formation of the solid solution, the structure evolution of the composite oxides is more complicated. The results of H2-TPR and CO-TPR show that the redox properties of solid solution are different with other composite oxides based on the unique structure. The oxygen storage ability of composite oxides and solid solution is better than CeO2. We found water-gas reaction in CO-TPR, it is related to the concentration of the hydroxyl groups on the surface of the composite oxides. The adsorption ability toward methyl orange by the composite oxides become stronger as the increasing of the Ce content. CeO2 is the main component that adsorbed methyl orange, thus the evolution of the surface components is the main point that effect the adsorption properties of the composite oxides.
The photocatalytic activity of the CeO2-TiO2 composite oxides for the photodegradation of methyl orange is low. It could be the preparation method, the type of the photocatalytic reaction, or the efficiency of the experiment's equipment that needed the further study.
3. The N-doped TiO2 photocatalysts have been prepared by clacination of the precusors at different temperature, which was synthesized via the precipitation of [TiO(C2O4)2]2-by ammonium hydroxide at low temperature. The results shows that all the photocatalysts are anatase phase, N is doped at the interstitial sites in TiO2 lattice, and because of this N doping, the light response of these photocatalysts is moved into the visible light region. Based on the TPRS results, we found that the photocatalyst calcined at 400℃is covalently bonded with oxalate groups on the surface to form Bronsted acid sites. All photocatalysts are performed well in the photocatalytic reaction for the degradation of methyl orange. The photocatalyst calcined at 400℃could adsorb methyl orange effectively because of the acidity, and it is an acid-catalysis and photocatalysis bi-funcitional catalyst.
4. We developed an one-step method to prepare N,S co-doped TiO2 photocatalyst via the controlled thermal decomposition of ammonium titanyl sulfate. the photocatalyst calcined at 800 C is still anatase, shows the phase stabilization ability. The results of XPS show that the photocatalysts are all S(IV) cation doping, the photocatalyst calcined at 600℃is co-doped with N,S and N is at the interstitial sites in TiO2 lattices. The band gap of TiO2 is not narrowed down by these doping. Based on the results of NH3-TPD and 1H soild-state MAS NMR, the photocatalyst calcined at 600 C is covalently bonded with the sulfate acid groups on the surface to form Bronsted acid sites. The evaluation of the photocatalytic activity is conducted by the photodegradation of methyl orange and photolysis of water for H2 production. Under all-wavelength light illumination, the photocatalytic activity of the photodegradation of methyl orange is well for all the photocatalysts, the photocatalyst calcined at 600℃is most active, better than the commercial P25. All the photocatalysts could degrade methyl orange under visible light illumination because of the N, S doping. After Pt loading, the H2 production under all-wavelength light illumination by the photocatalysts increased dramatically compared with the bare TiO2. Because of the synergy effect of Pt loading and the N, S co-doping, the 0.1Pt/TiO2 shows an improved photocatalytic activity for H2 production. the photocatalyst calcined at 600℃is both very active in the esterification for the ethyl acetate production and the photocatalytic reactions. So it is a acid-catalysis and photocatalysis bi-functional catalyst.
引文
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