TiO_2/C纳米复合气凝胶的制备及光催化性能研究
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摘要
TiO_2是一种性能优异的材料，在诸如颜料助剂、传感器、光电池等领域都得到了广泛应用，尤其作为光催化剂应用更为广泛。它的光催化活性主要由其形态、晶型、结晶程度及比表面积决定。如何获得一种理想的光催化剂并使这些性能最优化日益成为科研工作者的研究热点。迄今为止，合成方法有溶胶凝胶法、微胶囊法、水热法、气相沉积法及电化学方法等。而溶胶凝胶法由于成本低、操作简单、环境友好等特性而被广泛用于制备TiO_2基的复合材料。
本文使用一步溶胶-凝胶法制备了TiO_2/C复合气凝胶，并采用XRD、SEM、TEM、UV-Vis、拉曼光谱、N_2吸附等温线、XPS、原位红外、压汞实验等测试手段对样品微观形貌、晶型、微介孔全孔结构分布、样品表面元素价态等物理性能进行全面表征，将该材料应用于光催化降解亚甲基蓝，并探讨了其光催化降解机理。本课题主要从钛源前驱体、TiO_2设计质量、络合剂含量、稀土元素Ce的掺杂等几个方面展开了相关研究。
一、钛源前驱体对TiO_2/C复合气凝胶性能的影响研究
以钛酸四丁酯和四氯化钛为钛源前驱体制备不同样品，考察不同钛源对TiO_2/C复合气凝胶性能的影响。结果表明：相比于钛酸四丁酯，以四氯化钛为钛源前驱体制备的样品具有更大的比表面积、更高的吸附容量、TiO_2纳米粒子在无定型炭中的分布更加均匀、锐钛矿型TiO_2晶化程度高等特性；光催化降解实验结果表明后者具有更高的紫外光和可见光催化降解亚甲基蓝的效率。
二、TiO_2设计质量对TiO_2/C复合气凝胶性能的影响研究
研究了以四氯化钛为钛源前驱体，以TiO_2计的质量分别为2.65、3.03、3.80、4.91、5.31g制备五组样品，对比研究了样品对亚甲基蓝的紫外光和可见光催化降解亚甲基蓝的活性。结果表明：通过N_2吸附脱附等温线可知，TiO_2设计质量为3.80g时制备的样品具有最优的物理和化学性能，其比表面积为204.0m~2/g，孔容为0.34cm~3/g；通过透射电子显微镜及光电子能谱可知，样品中TiO_2纳米粒子镶嵌在无定型炭中，样品主要由C、Ti、O三种元素组成；通过XPS表征得知，样品中Ti主要以Ti~(4+)存在，结合XRD表征可知其以TiO_2形式存在；通过UV-vis分析可知，样品在可见光波段有较强的吸收；样品对亚甲基蓝溶液紫外和可见光催化降解实验可知，TiO_2设计质量为3.80g时制备的样品在紫外光下具有最佳的光催化活性，而TiO_2设计质量为5.31g时制备的样品在可见光下具有最佳的光催化活性。
三、络合剂含量对TiO_2/C复合气凝胶性能的影响
以TiO_2设计质量为3.80g，乙酰乙酸乙酯与钛的摩尔比分别为0.1、0.3、0.5、0.7和0.9制备五组样品，进行全面表征和光催化活性研究。结果表明：随着乙酰乙酸乙酯与钛的摩尔比的增加，样品中TiO_2的晶粒生长得到抑制；N_2吸附脱附结果表明，当乙酰乙酸乙酯与钛的摩尔比为0.5时其相对压力较高段的吸附容量最大，其比表面积达到298.9m~2/g，介孔孔容为0.87cm~3/g；拉曼光谱分析可知样品中的炭以无定型形式存在；UV-vis测试结果表明样品相对于P25而言其吸收带有不同程度的红移，表明其在可见光波段有较好的吸收；通过研究样品的投加量不同对亚甲基蓝紫外光催化降解，表明样品投加量增多对亚甲基蓝的紫外光催化降解效率没有显著提高。
四、稀土元素Ce的掺杂对TiO_2/C复合气凝胶性能的影响研究
研究了稀土元素Ce的掺杂及掺杂量对TiO_2/C复合气凝胶性能的影响。结果表明：当硝酸铈占TiO_2的质量百分比为3时，样品的比表面积为348.7m~2/g，总孔体积为1.43ml/g，平均孔直径为16.4nm；UV-vis测试表明，掺铈的样品在紫外光波段和可见光波段的吸收强度均高于未掺铈的样品；TEM和EDS测试表明样品由C、Ti、O、Ce四种元素组成，Ce元素的原子百分比为0.14-0.24；考察不同样品添加量对不同浓度亚甲基蓝的紫外光催化降解表明随着铈投加量的增加，其紫外光催化降解效率也增大，其中硝酸铈掺入量占TiO_2百分比为3%时的样品紫外光催化降解性能最好。
五、TiO_2/C复合气凝胶光催化降解亚甲基蓝机理研究
对TiO_2/C复合气凝胶对亚甲基蓝的紫外和可见光催化降解亚甲基蓝的机理进行了全面探讨，结果表明具有光催化活性的TiO_2纳米粒子和具有丰富孔结构的无定型炭的协同作用，可显著提高TiO_2/C复合气凝胶对亚甲基蓝的光催化性能，同时具有导电性能的碳可及时将光生电子传输，阻碍了光生电子和空穴的复合，因而有效提高了其光催化性能。
Titanium dioxide (TiO_2) is one of the most materials, and plays an important rolein many applications such as paints, pigment, additive, gas sensors, photovoltaic cell,and especially acting as photocatalyst. Its photocatalytic activity generally depends onits morphology, crystal composition, crystallinity, and surface area. How to optimizethem is a long-term topic of obtaining an ideal catalyst. Up to now, many variousmethods, including sol-gel, micelle, hydrothermal, vapor deposition methods, as wellas electrochemical approaches, have been introduced to solve these issues. Inparticular, sol-gel, with its low cost, simple operation, friendly environment, has beenextensively used to prepare TiO_2-based nanomaterials.
In this paper, TiO_2/C nano-composite aerogels were prepared by one-pot sol-gelapproach. The crystalline phase and micromechanism of the samples weresystematically characterized by XRD, SEM, TEM, UV-Vis, Raman spectrum,nitrogen adsorption, XPS, IR spectroscopy, etc. The mechanisms of degradation tomethylene blue chloride with the TiO_2/C nano-composite aerogels were discussed. Inthis work, effect of the precursor of TiO_2, content of TiO_2, content of complexingagent, content of Ce on their catalytic activity were investigated.
1. The effect of the precursor of TiO_2on structure and performance asphotocatalysts
Different samples were prepared by using tetrabutyl titanate and titaniumtetrachloride as the titanium precursor. The performance from different precursors ofTiO_2was studied. Results showed that the samples from titanium tetrachloride hadlarger specific surface area, higher adsorption capacity, more uniform distribution ofTiO_2nanoparticles in the amorphous carbon structure and sharper characteristic peakof anatase TiO_2grain than that with tetrabutyl titanate as the titanium source. Theresults also showed that the samples from titanium tetrachloride had higher efficiencyphotocatalytic degradation on methylene blue than that of tetrabutyl titanate.
2. The effect of the content of TiO_2on their structure and photocatalyticperformance
The samples were prepared from titanium tetrachloride as titanium source, inwhich the amounts of TiO_2converted from the precursor were2.65,3.03,3.80,4.91,5.31g respectively. The experimental photocatalytic degradation on methylene wasdone, and it was showed that the sample had the optimal physical and chemical performance through N_2adsorption when the TiO_2amount was3.80g, and its surfacearea was204m~2/g, and pore volume was0.34cm~3/g. The results from thetransmission electron microscopy and photoelectron spectroscopy showed that TiO_2nanoparticles embedded in the amorphous carbon in the samples which mainlyconsisted of three elements of C, Ti, O, in which element Ti existed as Ti~(4+)throughXPS analysis. It was showed that the samples had strong absorption in the visibleband through UV-vis analysis, which indicated that they had excellent visible lightcatalytic activity. The sample when the amount of TiO_2was3.80g had the bestphotocatalytic activity under UV light, and that when the amount of TiO_2was5.31gTiO_2had the best photocatalytic activity under visible light.
3. The effect of the content of complexing agent on their structure andphotocatalytic performance
The samples were prepared from different contents of complexing agent, inwhich mole fraction of ethyl acetoacetate to Ti was0.1to0.9. The results showed thatthe growth of TiO_2was restrained with the molar ration of ethyl acetoacetate to Tiincreasing. The sample of the ratio0.5had the largest adsorption capacity in the highrelative pressure through N_2adsorption, with surface area of298.9m~2/g and mesporevolume of0.87cm~3/g. The carbon of the samples existed as amorphous form byRaman spectroscopy. They had diverse redshift compared to P25by UV-vis diffusereflection, which manifested its good absorption in the visible region. It was showedthat the degradation ability did not increase with the increasing amount of complexingagent.
4. The effect of Ce content on their structure and photocatalytic performance
The doping of rare earth element Ce and its content were studied to investigateits effect on the properties of TiO_2/C composite aerogels. The results showed that thesample of Ce%-3had348.7m~2/g of surface area,1.43cm~3/g of pore volume and16.4nm of average pore diameter. The samples doped with Ce had a higher lightadsorption than that without Ce though UV-vis. The samples were consisted of C, Ti,O and Ce, in which the atomic percentage of Ce was0.14-0.24through TEM andEDS. The sample of Ce%-3had best UV and visible light catalytic degradationefficiency.
5. The degradation mechanism of the TiO_2/C composite aerogels
The degradation mechanism to methylene blue of TiO_2/C composite aerogelsunder UV and visible light was systematically discussed in this paper. It was showedthat the best photocatalytic performance of the materials was ascribed to the activity of TiO_2and abundant pore structure and amorphous carbon, which could facilitateelectron transfer and prevent recombination of e/h pair.
本文使用一步溶胶-凝胶法制备了TiO_2/C复合气凝胶，并采用XRD、SEM、TEM、UV-Vis、拉曼光谱、N_2吸附等温线、XPS、原位红外、压汞实验等测试手段对样品微观形貌、晶型、微介孔全孔结构分布、样品表面元素价态等物理性能进行全面表征，将该材料应用于光催化降解亚甲基蓝，并探讨了其光催化降解机理。本课题主要从钛源前驱体、TiO_2设计质量、络合剂含量、稀土元素Ce的掺杂等几个方面展开了相关研究。
一、钛源前驱体对TiO_2/C复合气凝胶性能的影响研究
以钛酸四丁酯和四氯化钛为钛源前驱体制备不同样品，考察不同钛源对TiO_2/C复合气凝胶性能的影响。结果表明：相比于钛酸四丁酯，以四氯化钛为钛源前驱体制备的样品具有更大的比表面积、更高的吸附容量、TiO_2纳米粒子在无定型炭中的分布更加均匀、锐钛矿型TiO_2晶化程度高等特性；光催化降解实验结果表明后者具有更高的紫外光和可见光催化降解亚甲基蓝的效率。
二、TiO_2设计质量对TiO_2/C复合气凝胶性能的影响研究
研究了以四氯化钛为钛源前驱体，以TiO_2计的质量分别为2.65、3.03、3.80、4.91、5.31g制备五组样品，对比研究了样品对亚甲基蓝的紫外光和可见光催化降解亚甲基蓝的活性。结果表明：通过N_2吸附脱附等温线可知，TiO_2设计质量为3.80g时制备的样品具有最优的物理和化学性能，其比表面积为204.0m~2/g，孔容为0.34cm~3/g；通过透射电子显微镜及光电子能谱可知，样品中TiO_2纳米粒子镶嵌在无定型炭中，样品主要由C、Ti、O三种元素组成；通过XPS表征得知，样品中Ti主要以Ti~(4+)存在，结合XRD表征可知其以TiO_2形式存在；通过UV-vis分析可知，样品在可见光波段有较强的吸收；样品对亚甲基蓝溶液紫外和可见光催化降解实验可知，TiO_2设计质量为3.80g时制备的样品在紫外光下具有最佳的光催化活性，而TiO_2设计质量为5.31g时制备的样品在可见光下具有最佳的光催化活性。
三、络合剂含量对TiO_2/C复合气凝胶性能的影响
以TiO_2设计质量为3.80g，乙酰乙酸乙酯与钛的摩尔比分别为0.1、0.3、0.5、0.7和0.9制备五组样品，进行全面表征和光催化活性研究。结果表明：随着乙酰乙酸乙酯与钛的摩尔比的增加，样品中TiO_2的晶粒生长得到抑制；N_2吸附脱附结果表明，当乙酰乙酸乙酯与钛的摩尔比为0.5时其相对压力较高段的吸附容量最大，其比表面积达到298.9m~2/g，介孔孔容为0.87cm~3/g；拉曼光谱分析可知样品中的炭以无定型形式存在；UV-vis测试结果表明样品相对于P25而言其吸收带有不同程度的红移，表明其在可见光波段有较好的吸收；通过研究样品的投加量不同对亚甲基蓝紫外光催化降解，表明样品投加量增多对亚甲基蓝的紫外光催化降解效率没有显著提高。
四、稀土元素Ce的掺杂对TiO_2/C复合气凝胶性能的影响研究
研究了稀土元素Ce的掺杂及掺杂量对TiO_2/C复合气凝胶性能的影响。结果表明：当硝酸铈占TiO_2的质量百分比为3时，样品的比表面积为348.7m~2/g，总孔体积为1.43ml/g，平均孔直径为16.4nm；UV-vis测试表明，掺铈的样品在紫外光波段和可见光波段的吸收强度均高于未掺铈的样品；TEM和EDS测试表明样品由C、Ti、O、Ce四种元素组成，Ce元素的原子百分比为0.14-0.24；考察不同样品添加量对不同浓度亚甲基蓝的紫外光催化降解表明随着铈投加量的增加，其紫外光催化降解效率也增大，其中硝酸铈掺入量占TiO_2百分比为3%时的样品紫外光催化降解性能最好。
五、TiO_2/C复合气凝胶光催化降解亚甲基蓝机理研究
对TiO_2/C复合气凝胶对亚甲基蓝的紫外和可见光催化降解亚甲基蓝的机理进行了全面探讨，结果表明具有光催化活性的TiO_2纳米粒子和具有丰富孔结构的无定型炭的协同作用，可显著提高TiO_2/C复合气凝胶对亚甲基蓝的光催化性能，同时具有导电性能的碳可及时将光生电子传输，阻碍了光生电子和空穴的复合，因而有效提高了其光催化性能。
Titanium dioxide (TiO_2) is one of the most materials, and plays an important rolein many applications such as paints, pigment, additive, gas sensors, photovoltaic cell,and especially acting as photocatalyst. Its photocatalytic activity generally depends onits morphology, crystal composition, crystallinity, and surface area. How to optimizethem is a long-term topic of obtaining an ideal catalyst. Up to now, many variousmethods, including sol-gel, micelle, hydrothermal, vapor deposition methods, as wellas electrochemical approaches, have been introduced to solve these issues. Inparticular, sol-gel, with its low cost, simple operation, friendly environment, has beenextensively used to prepare TiO_2-based nanomaterials.
In this paper, TiO_2/C nano-composite aerogels were prepared by one-pot sol-gelapproach. The crystalline phase and micromechanism of the samples weresystematically characterized by XRD, SEM, TEM, UV-Vis, Raman spectrum,nitrogen adsorption, XPS, IR spectroscopy, etc. The mechanisms of degradation tomethylene blue chloride with the TiO_2/C nano-composite aerogels were discussed. Inthis work, effect of the precursor of TiO_2, content of TiO_2, content of complexingagent, content of Ce on their catalytic activity were investigated.
1. The effect of the precursor of TiO_2on structure and performance asphotocatalysts
Different samples were prepared by using tetrabutyl titanate and titaniumtetrachloride as the titanium precursor. The performance from different precursors ofTiO_2was studied. Results showed that the samples from titanium tetrachloride hadlarger specific surface area, higher adsorption capacity, more uniform distribution ofTiO_2nanoparticles in the amorphous carbon structure and sharper characteristic peakof anatase TiO_2grain than that with tetrabutyl titanate as the titanium source. Theresults also showed that the samples from titanium tetrachloride had higher efficiencyphotocatalytic degradation on methylene blue than that of tetrabutyl titanate.
2. The effect of the content of TiO_2on their structure and photocatalyticperformance
The samples were prepared from titanium tetrachloride as titanium source, inwhich the amounts of TiO_2converted from the precursor were2.65,3.03,3.80,4.91,5.31g respectively. The experimental photocatalytic degradation on methylene wasdone, and it was showed that the sample had the optimal physical and chemical performance through N_2adsorption when the TiO_2amount was3.80g, and its surfacearea was204m~2/g, and pore volume was0.34cm~3/g. The results from thetransmission electron microscopy and photoelectron spectroscopy showed that TiO_2nanoparticles embedded in the amorphous carbon in the samples which mainlyconsisted of three elements of C, Ti, O, in which element Ti existed as Ti~(4+)throughXPS analysis. It was showed that the samples had strong absorption in the visibleband through UV-vis analysis, which indicated that they had excellent visible lightcatalytic activity. The sample when the amount of TiO_2was3.80g had the bestphotocatalytic activity under UV light, and that when the amount of TiO_2was5.31gTiO_2had the best photocatalytic activity under visible light.
3. The effect of the content of complexing agent on their structure andphotocatalytic performance
The samples were prepared from different contents of complexing agent, inwhich mole fraction of ethyl acetoacetate to Ti was0.1to0.9. The results showed thatthe growth of TiO_2was restrained with the molar ration of ethyl acetoacetate to Tiincreasing. The sample of the ratio0.5had the largest adsorption capacity in the highrelative pressure through N_2adsorption, with surface area of298.9m~2/g and mesporevolume of0.87cm~3/g. The carbon of the samples existed as amorphous form byRaman spectroscopy. They had diverse redshift compared to P25by UV-vis diffusereflection, which manifested its good absorption in the visible region. It was showedthat the degradation ability did not increase with the increasing amount of complexingagent.
4. The effect of Ce content on their structure and photocatalytic performance
The doping of rare earth element Ce and its content were studied to investigateits effect on the properties of TiO_2/C composite aerogels. The results showed that thesample of Ce%-3had348.7m~2/g of surface area,1.43cm~3/g of pore volume and16.4nm of average pore diameter. The samples doped with Ce had a higher lightadsorption than that without Ce though UV-vis. The samples were consisted of C, Ti,O and Ce, in which the atomic percentage of Ce was0.14-0.24through TEM andEDS. The sample of Ce%-3had best UV and visible light catalytic degradationefficiency.
5. The degradation mechanism of the TiO_2/C composite aerogels
The degradation mechanism to methylene blue of TiO_2/C composite aerogelsunder UV and visible light was systematically discussed in this paper. It was showedthat the best photocatalytic performance of the materials was ascribed to the activity of TiO_2and abundant pore structure and amorphous carbon, which could facilitateelectron transfer and prevent recombination of e/h pair.
引文
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