有序介孔二氧化钛—碳复合材料的制备及其光电化学性能
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摘要
本论文主要针对甲醇燃料电池（DMFC）催化剂二氧化钛材料导电性差、热稳定性弱以及禁带宽等问题，探索具有新型结构和优异性能的催化剂载体的制备方法。采用低聚合度高分子材料为碳源，三嵌段表面活性剂为结构导向剂，通过三元共组装法制备有序介孔二氧化钛-碳复合材料，并在其中复合碳纳米管、氧化石墨烯及氧化钨等组分，提高二氧化钛介孔有序结构的热稳定性、改善导电性能、降低禁带宽度，进一步增强负载催化剂后的光电化学活性。主要研究内容包括：
1、提出在有序介孔二氧化钛上用脉冲电位阶跃法负载金属Pt，利用二氧化钛光催化与Pt电催化的协同作用，在紫外光照下研究甲醇的光电化学催化氧化行为，改善燃料电池催化剂载体的性能，为形成甲醇燃料电池/光电电池联合能量转换系统提供新思路。
2、设计一种新颖结构的催化剂载体，是以钛酸四丁酯为前驱体，低聚合度的酚醛树脂为碳源，F127为结构导向剂，通过三元共组装法制备了介孔结构有序的二氧化钛-碳复合材料。研究发现这种复合材料在600℃仍能保持介孔结构的有序性，有序介孔结构的热稳定性得到明显提升。实验结果表明碳组分包覆在二氧化钛晶粒的外表，限制了热处理过程中晶粒的长大，又起到“粘结”晶粒的作用，从而阻碍了二氧化钛有序介孔结构的热收缩。
3、为增强有序介孔二氧化钛的导电性，采用聚苯乙烯磺酸钠（PSS）活化修饰碳纳米管，制备有序介孔二氧化钛-碳-碳纳米管复合材料。研究表明随着碳纳米管的加入，有序介孔结构的热稳定性提高至700℃，复合材料的导电能力获得了进一步改善。且由于纳米碳管的良好导电性以及电子定向传输作用，使二氧化钛的导电能力增强，量子转化效率提高，光响应电流由0.4μA升高至7μA，光电化学催化电流峰值提高2倍。
4、采用改进后的HUMMERS法制备氧化石墨，经超声剥离、高温热解还原，制备有序介孔二氧化钛-碳-氧化石墨烯复合材料。该复合材料有序介孔结构的热稳定性可达900℃，光吸收波长出现红移现象，当氧化石墨烯添加量为8%时，未沉积铂时的光响应电流为13.2μA，沉积铂后可达32.4μA。结果表明，氧化石墨烯的高导电能力促进了空穴/电子对的分离，有利于铂位点甲醇氧化反应的去极化，从而获得较高的光响应电流。
5、以钛酸四丁酯为钛源、三嵌段共聚物F127为模板剂、低分子量的酚醛树脂为碳源、硅钨酸为钨源，经高温热解制备了具有较好光电催化活性的介孔二氧化钛-碳-氧化钨复合材料。研究表明，氧化钨的掺杂使材料的禁带宽度从3.2eV降低为2.7eV，提高了该复合材料在可见光区的转换率。电化学负载Pt后，复合材料的光电催化电流峰值达7μA。另外，氧化钨含量为8%时，经波长256nm紫外光50秒辐照后，在非光照状况下复合材料出现电流长时间缓慢下降现象，去除可能的电化学因素，推测认为这种现象是复合材料中氧化钨具有电子储存的能力所致。
6、把n-型半导体有序介孔二氧化钛与p-型半导体氢氧化镍通过电沉积进行复合。在波长256nm紫外光的照射下，复合材料中空穴在两种半导体中扩散使Ni(II)氧化为Ni(III)，从而实现光电效应的氧化能在氢氧化镍中存储。研究表明，光照充电后放电时间随沉积电流的增加而增加，。而2.0mA的试样放电时间反而较小，原因可能是过高的电流使氢氧化镍沉积过多、氢氧化镍颗粒太大，堵塞了二氧化钛的光电传输通道而影响储能效果。
TiO2materials are expected to play an important role in solving many serious challenges due toits good characteries of powerful oxidation strength, high chemical stability.But in the practicalapplication, there existed many problems such as poor electrical conductivity, weak thermal stabilityand wider band gap. In order to solve these issues, this work carried out the basic and applied researchto explore the preparation of the new structure of the catalyst support and resolve the mechanism ofthe how to improve the activity and the stability of the catalyst.In this work, we prepared orderedmesoporous titanium dioxide-carbon composites by organic-inorganic self-assembly method aspolymer materials as the carbon source, Trebloc surfactant as a structure directing agent. To enhancetheir photoelectrochemical activity, highly graphitized carbon material such as carbon nanotubes,Graphene oxide is introduced into the composites.Meanwhile, tungsten oxide is also added todecrease the band gap of the composite.The main contents include:
At first, we have designed a novel catalyst with highly ordered mesoporous structure. A highlyordered mesoporous titanium oxide-carbon composite material is synthesized by organic-inorganicself-assembly with tetrabutyl titanate as precursor, phenolic resin as a polymer source, F127as thestructure directing agent. The introducing of the carbon as a "binder" to "bond" together prevented thetitanium oxide grain growth during the heat treatment. This combined the carbon with strong thermalstability and titanium oxide with the highly photocatalysic performance, preventing the collapse of themesoporous skeleton structure of Titania, effectively improving the oxidation of methanol.Meanwhile, combined the electro-catalytic performance of platinum and the photocatalytic activity oftitanium oxide, to research its behavior of methanol oxidation to joint the DMFC/photovoltaic cellssystem.Platinum is deposited on the surface of the electrode, which can improve the electricalconductivity, increase the active points of the electrodes and separate the electron and hole.
In order to enhance the photoelectric-chemical performance, sodium polystyrene sulfonate (PSS)modified carbon nanotube was chosen to order mesoporous Titanium dioxide-carbon-carbonnanotube composite material. The experiments showed that with the content of carbon nanotubes andincrease of the temperature, existed the “mixed crystal effect”, enhance the thermal stability (700degree) and photocatalytic performance of the material due to higher crystallization degree, transmission of the electronic and sharper electron-hole separation, thereby increasing the overallphoto-response current from0.4μA to7μA..
To further improve the electrical conductivity, we synthesis the highly orderly mesoporoustitanium dioxide-carbon-graphite oxide composite materials by organic-inorganic self-assemblymethods, with the graphite oxide as raw material.By appropriate methods to effectively improve thedispersion of graphite oxide to find the right TiO2modification process. Tests show that orderedmesoporous titanium-carbon-graphite oxide composite material better methanol oxidationperformance after the irradiation of ultraviolet light excitation, wherein, the doping amount of thegraphite oxide with8%and the calcining temperature with900℃is chosen as the best modifiedconditions, photocurrent increased to13.2μA.
Silicotungstic acid is doped in the mesoporous titanium dioxide-carbon material to furtherimprove the photoelectrochemical properties of titanium dioxide material,. XRD and TEMcharacterization of the phase structure showed that the composite material has high orderedmesoporous structure.Current-time measures displayed that the materials has the optical and electricalproperties when WO3doping amount is8%.More important, in the Current-time measures process, itwas observed that the current value of the samples calcined under air atmosphere is no suddentransitions to the minimum value but after a period of decreased slowly when the removal of theultraviolet light irradiation, WO3electronic storage capacity is taken into account the energy storageconcept
We deposited nickel hydroxide material by galvanostatic deposition in TiO2electrode materialsto research energy storage properties of TiO2-Ni (OH)2composite materials,. the charge and dischargecurves show that the explode with1.5mA current deposition of nickel hydroxide displayed the bestdioxide material storage performance, Charge and discharge curves proved that TiO2-Ni (OH)2composite materials has the energy storage performance, layed the foundation for further study of thetitanium dioxide material in the dark environment.
1、提出在有序介孔二氧化钛上用脉冲电位阶跃法负载金属Pt，利用二氧化钛光催化与Pt电催化的协同作用，在紫外光照下研究甲醇的光电化学催化氧化行为，改善燃料电池催化剂载体的性能，为形成甲醇燃料电池/光电电池联合能量转换系统提供新思路。
2、设计一种新颖结构的催化剂载体，是以钛酸四丁酯为前驱体，低聚合度的酚醛树脂为碳源，F127为结构导向剂，通过三元共组装法制备了介孔结构有序的二氧化钛-碳复合材料。研究发现这种复合材料在600℃仍能保持介孔结构的有序性，有序介孔结构的热稳定性得到明显提升。实验结果表明碳组分包覆在二氧化钛晶粒的外表，限制了热处理过程中晶粒的长大，又起到“粘结”晶粒的作用，从而阻碍了二氧化钛有序介孔结构的热收缩。
3、为增强有序介孔二氧化钛的导电性，采用聚苯乙烯磺酸钠（PSS）活化修饰碳纳米管，制备有序介孔二氧化钛-碳-碳纳米管复合材料。研究表明随着碳纳米管的加入，有序介孔结构的热稳定性提高至700℃，复合材料的导电能力获得了进一步改善。且由于纳米碳管的良好导电性以及电子定向传输作用，使二氧化钛的导电能力增强，量子转化效率提高，光响应电流由0.4μA升高至7μA，光电化学催化电流峰值提高2倍。
4、采用改进后的HUMMERS法制备氧化石墨，经超声剥离、高温热解还原，制备有序介孔二氧化钛-碳-氧化石墨烯复合材料。该复合材料有序介孔结构的热稳定性可达900℃，光吸收波长出现红移现象，当氧化石墨烯添加量为8%时，未沉积铂时的光响应电流为13.2μA，沉积铂后可达32.4μA。结果表明，氧化石墨烯的高导电能力促进了空穴/电子对的分离，有利于铂位点甲醇氧化反应的去极化，从而获得较高的光响应电流。
5、以钛酸四丁酯为钛源、三嵌段共聚物F127为模板剂、低分子量的酚醛树脂为碳源、硅钨酸为钨源，经高温热解制备了具有较好光电催化活性的介孔二氧化钛-碳-氧化钨复合材料。研究表明，氧化钨的掺杂使材料的禁带宽度从3.2eV降低为2.7eV，提高了该复合材料在可见光区的转换率。电化学负载Pt后，复合材料的光电催化电流峰值达7μA。另外，氧化钨含量为8%时，经波长256nm紫外光50秒辐照后，在非光照状况下复合材料出现电流长时间缓慢下降现象，去除可能的电化学因素，推测认为这种现象是复合材料中氧化钨具有电子储存的能力所致。
6、把n-型半导体有序介孔二氧化钛与p-型半导体氢氧化镍通过电沉积进行复合。在波长256nm紫外光的照射下，复合材料中空穴在两种半导体中扩散使Ni(II)氧化为Ni(III)，从而实现光电效应的氧化能在氢氧化镍中存储。研究表明，光照充电后放电时间随沉积电流的增加而增加，。而2.0mA的试样放电时间反而较小，原因可能是过高的电流使氢氧化镍沉积过多、氢氧化镍颗粒太大，堵塞了二氧化钛的光电传输通道而影响储能效果。
TiO2materials are expected to play an important role in solving many serious challenges due toits good characteries of powerful oxidation strength, high chemical stability.But in the practicalapplication, there existed many problems such as poor electrical conductivity, weak thermal stabilityand wider band gap. In order to solve these issues, this work carried out the basic and applied researchto explore the preparation of the new structure of the catalyst support and resolve the mechanism ofthe how to improve the activity and the stability of the catalyst.In this work, we prepared orderedmesoporous titanium dioxide-carbon composites by organic-inorganic self-assembly method aspolymer materials as the carbon source, Trebloc surfactant as a structure directing agent. To enhancetheir photoelectrochemical activity, highly graphitized carbon material such as carbon nanotubes,Graphene oxide is introduced into the composites.Meanwhile, tungsten oxide is also added todecrease the band gap of the composite.The main contents include:
At first, we have designed a novel catalyst with highly ordered mesoporous structure. A highlyordered mesoporous titanium oxide-carbon composite material is synthesized by organic-inorganicself-assembly with tetrabutyl titanate as precursor, phenolic resin as a polymer source, F127as thestructure directing agent. The introducing of the carbon as a "binder" to "bond" together prevented thetitanium oxide grain growth during the heat treatment. This combined the carbon with strong thermalstability and titanium oxide with the highly photocatalysic performance, preventing the collapse of themesoporous skeleton structure of Titania, effectively improving the oxidation of methanol.Meanwhile, combined the electro-catalytic performance of platinum and the photocatalytic activity oftitanium oxide, to research its behavior of methanol oxidation to joint the DMFC/photovoltaic cellssystem.Platinum is deposited on the surface of the electrode, which can improve the electricalconductivity, increase the active points of the electrodes and separate the electron and hole.
In order to enhance the photoelectric-chemical performance, sodium polystyrene sulfonate (PSS)modified carbon nanotube was chosen to order mesoporous Titanium dioxide-carbon-carbonnanotube composite material. The experiments showed that with the content of carbon nanotubes andincrease of the temperature, existed the “mixed crystal effect”, enhance the thermal stability (700degree) and photocatalytic performance of the material due to higher crystallization degree, transmission of the electronic and sharper electron-hole separation, thereby increasing the overallphoto-response current from0.4μA to7μA..
To further improve the electrical conductivity, we synthesis the highly orderly mesoporoustitanium dioxide-carbon-graphite oxide composite materials by organic-inorganic self-assemblymethods, with the graphite oxide as raw material.By appropriate methods to effectively improve thedispersion of graphite oxide to find the right TiO2modification process. Tests show that orderedmesoporous titanium-carbon-graphite oxide composite material better methanol oxidationperformance after the irradiation of ultraviolet light excitation, wherein, the doping amount of thegraphite oxide with8%and the calcining temperature with900℃is chosen as the best modifiedconditions, photocurrent increased to13.2μA.
Silicotungstic acid is doped in the mesoporous titanium dioxide-carbon material to furtherimprove the photoelectrochemical properties of titanium dioxide material,. XRD and TEMcharacterization of the phase structure showed that the composite material has high orderedmesoporous structure.Current-time measures displayed that the materials has the optical and electricalproperties when WO3doping amount is8%.More important, in the Current-time measures process, itwas observed that the current value of the samples calcined under air atmosphere is no suddentransitions to the minimum value but after a period of decreased slowly when the removal of theultraviolet light irradiation, WO3electronic storage capacity is taken into account the energy storageconcept
We deposited nickel hydroxide material by galvanostatic deposition in TiO2electrode materialsto research energy storage properties of TiO2-Ni (OH)2composite materials,. the charge and dischargecurves show that the explode with1.5mA current deposition of nickel hydroxide displayed the bestdioxide material storage performance, Charge and discharge curves proved that TiO2-Ni (OH)2composite materials has the energy storage performance, layed the foundation for further study of thetitanium dioxide material in the dark environment.
引文
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