TiO_2基可见光响应纳米光催化剂的制备、表征分析及性能研究
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摘要
目前,稀土元素掺杂改性TiO_2光催化剂已成为国内、外光催化领域研究热点,且已有众多学者探讨过稀土元素自身性质与稀土元素掺杂改性后的TiO_2光催化活性之间的关系。但对于稀土元素性质对稀土元素掺杂改性TiO_2光催化机理及掺杂机理尚存在较多争议。本研究通过溶胶—凝胶法制备稀土元素(RE)(La、Ce、Gd、Er、Yb、Y)改性TiO_2纳米光催化剂粉体,以草酸和偶氮染料为降解目标物检验其光催化活性,用XRD、TEM、BET、DRS及XPS对其晶体结构及形貌、光谱效应和化学组态进行分析。对掺杂量和煅烧温度对其光催化剂活性、晶体结构及形貌、光谱效应和化学组态的影响,以及在不同波长光的激发下的光催化活性进行了探讨,并对各稀土元素固有性质对于稀土掺杂改性TiO_2的掺杂机理和催化降解有机污染物的光催化活性的影响机理做了深入分析。
以TiCl_4为TiO_2的前驱体,通过水热合成法制备了N掺杂改性的TiO_2纳米光催化剂,所制备的纳米粉体为黄色。其光催化剂的活性以KI溶液和草酸溶液为目标物、在不同激发波长光源激发下测定。由XRD和BET表征分析可知,所制备的N掺杂改性的TiO_2光催化剂样品的晶型为锐钛矿、和少量板钛矿组成,且其粒径分布在7nm到10nm范围内,比表面积分布于71.24m2·g~(-1)到170.38m2·g~(-1)范围内。由DRS表征分析可知,所制备的纳米粉体光催化剂的吸收光谱明显红移,且禁带宽度最小可被减小至2.80eV,可充分利用可见光。由XPS表征分析去化学组态可知,Ti-N键和NOx为所掺杂N的主要存在形式。Raman表征分析进一步验证了N-TiO_2键的存在。
在本研究提出了以Ce和N为目标掺杂物,通过改进的溶胶—凝胶工艺合成可见光响应TiO_2光催化剂纳米粉体。并通过XRD,BET,DRS,Raman和XPS对其晶体结果及化学组态进行表征分析。其中,引入的N有效减小其禁带宽度而使受激发所需能量降低,即2.40eV(铈掺杂改性)降低到2.21eV(铈、氮共掺杂改性);XPS表征分析确定了Ce3+/Ce4+,NOx和Ti-O-N和Ti-O-Ce的存在。其光催化剂机理通过在不同激发波长光源(λ>365nm,λ>420nm,λ>500nm,λ>550nm,λ>600nm)下光催化降解亚甲基蓝(MB)进行研究。在本文的研究范围内确定了最佳掺杂比例为0.70 at.% Ce和0.70 at.% N。本研究系统的讨论了影响光催化反应过程的主要参数,即所掺杂的N与Ce的原子百分比和激发波长,以及反应过程的一级动力学。光催化活性的提高应归因于在反应过程中所大量形成的·OH自由基,且光生电子空—穴对的复合是影响MB光催化降解的关键因素。本研究用改性半导体(晶体结构和化学组态改性)薄膜材料替代纯TiO_2薄膜,即N掺杂改性的TiO_2(N-TiO_2)薄膜,增强其表面与染料(N719)的键合强度、染料在其表面的吸附量及稳定性,提高太阳能电池的光电转化效率和使用寿命。提高太阳能的利用率的同时,延长光生电子寿命和提高光生电子密度,进而揭示DSSCs光电转化效率的提高与光生电子之间的关系,并对N-TiO_2薄膜为光阳极的DSSCs内的光生电子寿命、光生电子密度及扩散系数与N-TiO_2晶体结构及个元素的化学组态间的关系做了深入、系统研究。
Rear earth (RE) doped TiO_2 nano-photocatalyst attracted the increasing attentions, and many attempts have been made to explore the relationship between the properties of rear earth elements itself and the photocatalytic activities of as-prepared photocatalyst. However, up to now, the effects of the properties of rear earth elements itself on the mechanism of doping process and activity still kept unclear. The RE (La, Ce, Gd, Er, Yb, Y) doped TiO_2 nano-photocatalyst was synthesized using modified sol-gel technique, and the activities were evaluated using oza dye solution and oxalic acid solution as the model reactant under different light source. The as-prepared particles were characterized using XRD, TEM, BET, DRS and XPS. The effects of doping amount and sintering temperature on the crystal morphology, crystal structure and the chemical component were carried out in this study. Further, the process of photodegradation and the mechanism of photocatalyst have been studied well.
Nitrogen doped titanium dioxide nanoparticles were prepared by heating titanium hydroxide with urea. The yellow powders obtained after calcination at 450 oC 2 h in air. Photocatalysis the photoconversion KI and oxalic acid solution have been operated under different light source irradiation. X-Ray Diffraction (XRD) and surface area analysis show the presence of anatase/brookite TiO_2 nanoparticles with crystallite size ranging from 7nm to 10 nm and specific surface area ranging from 71.24 to 170.38 m2·g~(-1), depending on the amount of urea used. Diffuse Reflectance Spectroscopy (DRS) shows a shift in the range of 400~580nm and narrowing of the bandgap up to 2.80 eV, which can be attributed to the creation of visible light absorbing titanium oxynitride centres by the doping process. X-Ray Photoelectron Spectroscopy confirms the presence of Ti-N bond and oxynitride should be main doped nitrogen species due to new coming N-TiO_2 vibration at 550 cm~(-1) from Raman spectrum, XPS analysis.
Based on the above theorical analysis, cerium and nitrogen co-doped anatase TiO_2 nanoparticles were synthesized using a one-step technique via a modified sol-gel process and characterized by XRD, BET, DRS, Raman and XPS. The photocatalytic mechanism of the degradation of methylene blue (MB) under fluorescent light and visible light irradiation was studied. Co-doping cerium and nitrogen in the crystal lattice of TiO_2 narrowed the band gap from 2.40 eV (Ce-doped TiO_2) to 2.21 eV (Ce/N co-doped TiO_2). Ce~(4+)/Ce~(3+) pairs, oxynitride species and Ti-O-N and Ti-O-Ce bonds were determined by XPS. The recombination of photogenerated electron-hole pairs was inhibited due to the synergistic effect of doping with Ce~(4+)/ Ce~(3+) ions and N atoms. The optimal doping ratio was 0.70% Ce and 0.70% N using MB photocatalytic degradation under fluorescent light and visible light irradiation (λ>420 nm). The photocatalytic mechanism and was investigated through methylene blue (MB) photocatalytic degradation using various filtered wavelengths of light (λ>365nm,λ>420nm,λ>500nm,λ>550nm,λ>600nm) for a period. Two experimental parameters were studied systematically, namely the atomic ratio of doped N to Ce and the irradiation wavelength number. The photocatalytic degradation of MB over CNT NPs in aqueous suspension was found to follow approximately first-order kinetics according to the Langmuir-Hinshelwood model. The enhanced photocatalytic degradation was attributed to the increased number of photogenerated·OH radicals.The enhanced photocatalytic degradation under visible light irradiation was attributed to the increasing number of photogenerated·OH radicals. The recombination of photogenerated e--h+ was attributed to be the key factor for the decrease in the photocatalytic degradation efficiency of MB.
The targeted dye sensitized solar cells in this study were fabricated using the modified nano-photocatalyst (N doped TiO_2 nanoparticles) as the electrode and N719 as the dye sensitizer. By enforced the connections between the conductivity film and dye, the absorbance of amount, the enhanced efficiency and life time of solar cells have been found. Meanwhile, the properties of photo-generated electrons have been studied in detailed, such as the electron life time, the electron density, the diffusion coefficient. The relationship between the properties of photo-generated electrons, the crystal structure, and the chemical component of N doped TiO_2 nanoparticles was dicussed in this part.
以TiCl_4为TiO_2的前驱体,通过水热合成法制备了N掺杂改性的TiO_2纳米光催化剂,所制备的纳米粉体为黄色。其光催化剂的活性以KI溶液和草酸溶液为目标物、在不同激发波长光源激发下测定。由XRD和BET表征分析可知,所制备的N掺杂改性的TiO_2光催化剂样品的晶型为锐钛矿、和少量板钛矿组成,且其粒径分布在7nm到10nm范围内,比表面积分布于71.24m2·g~(-1)到170.38m2·g~(-1)范围内。由DRS表征分析可知,所制备的纳米粉体光催化剂的吸收光谱明显红移,且禁带宽度最小可被减小至2.80eV,可充分利用可见光。由XPS表征分析去化学组态可知,Ti-N键和NOx为所掺杂N的主要存在形式。Raman表征分析进一步验证了N-TiO_2键的存在。
在本研究提出了以Ce和N为目标掺杂物,通过改进的溶胶—凝胶工艺合成可见光响应TiO_2光催化剂纳米粉体。并通过XRD,BET,DRS,Raman和XPS对其晶体结果及化学组态进行表征分析。其中,引入的N有效减小其禁带宽度而使受激发所需能量降低,即2.40eV(铈掺杂改性)降低到2.21eV(铈、氮共掺杂改性);XPS表征分析确定了Ce3+/Ce4+,NOx和Ti-O-N和Ti-O-Ce的存在。其光催化剂机理通过在不同激发波长光源(λ>365nm,λ>420nm,λ>500nm,λ>550nm,λ>600nm)下光催化降解亚甲基蓝(MB)进行研究。在本文的研究范围内确定了最佳掺杂比例为0.70 at.% Ce和0.70 at.% N。本研究系统的讨论了影响光催化反应过程的主要参数,即所掺杂的N与Ce的原子百分比和激发波长,以及反应过程的一级动力学。光催化活性的提高应归因于在反应过程中所大量形成的·OH自由基,且光生电子空—穴对的复合是影响MB光催化降解的关键因素。本研究用改性半导体(晶体结构和化学组态改性)薄膜材料替代纯TiO_2薄膜,即N掺杂改性的TiO_2(N-TiO_2)薄膜,增强其表面与染料(N719)的键合强度、染料在其表面的吸附量及稳定性,提高太阳能电池的光电转化效率和使用寿命。提高太阳能的利用率的同时,延长光生电子寿命和提高光生电子密度,进而揭示DSSCs光电转化效率的提高与光生电子之间的关系,并对N-TiO_2薄膜为光阳极的DSSCs内的光生电子寿命、光生电子密度及扩散系数与N-TiO_2晶体结构及个元素的化学组态间的关系做了深入、系统研究。
Rear earth (RE) doped TiO_2 nano-photocatalyst attracted the increasing attentions, and many attempts have been made to explore the relationship between the properties of rear earth elements itself and the photocatalytic activities of as-prepared photocatalyst. However, up to now, the effects of the properties of rear earth elements itself on the mechanism of doping process and activity still kept unclear. The RE (La, Ce, Gd, Er, Yb, Y) doped TiO_2 nano-photocatalyst was synthesized using modified sol-gel technique, and the activities were evaluated using oza dye solution and oxalic acid solution as the model reactant under different light source. The as-prepared particles were characterized using XRD, TEM, BET, DRS and XPS. The effects of doping amount and sintering temperature on the crystal morphology, crystal structure and the chemical component were carried out in this study. Further, the process of photodegradation and the mechanism of photocatalyst have been studied well.
Nitrogen doped titanium dioxide nanoparticles were prepared by heating titanium hydroxide with urea. The yellow powders obtained after calcination at 450 oC 2 h in air. Photocatalysis the photoconversion KI and oxalic acid solution have been operated under different light source irradiation. X-Ray Diffraction (XRD) and surface area analysis show the presence of anatase/brookite TiO_2 nanoparticles with crystallite size ranging from 7nm to 10 nm and specific surface area ranging from 71.24 to 170.38 m2·g~(-1), depending on the amount of urea used. Diffuse Reflectance Spectroscopy (DRS) shows a shift in the range of 400~580nm and narrowing of the bandgap up to 2.80 eV, which can be attributed to the creation of visible light absorbing titanium oxynitride centres by the doping process. X-Ray Photoelectron Spectroscopy confirms the presence of Ti-N bond and oxynitride should be main doped nitrogen species due to new coming N-TiO_2 vibration at 550 cm~(-1) from Raman spectrum, XPS analysis.
Based on the above theorical analysis, cerium and nitrogen co-doped anatase TiO_2 nanoparticles were synthesized using a one-step technique via a modified sol-gel process and characterized by XRD, BET, DRS, Raman and XPS. The photocatalytic mechanism of the degradation of methylene blue (MB) under fluorescent light and visible light irradiation was studied. Co-doping cerium and nitrogen in the crystal lattice of TiO_2 narrowed the band gap from 2.40 eV (Ce-doped TiO_2) to 2.21 eV (Ce/N co-doped TiO_2). Ce~(4+)/Ce~(3+) pairs, oxynitride species and Ti-O-N and Ti-O-Ce bonds were determined by XPS. The recombination of photogenerated electron-hole pairs was inhibited due to the synergistic effect of doping with Ce~(4+)/ Ce~(3+) ions and N atoms. The optimal doping ratio was 0.70% Ce and 0.70% N using MB photocatalytic degradation under fluorescent light and visible light irradiation (λ>420 nm). The photocatalytic mechanism and was investigated through methylene blue (MB) photocatalytic degradation using various filtered wavelengths of light (λ>365nm,λ>420nm,λ>500nm,λ>550nm,λ>600nm) for a period. Two experimental parameters were studied systematically, namely the atomic ratio of doped N to Ce and the irradiation wavelength number. The photocatalytic degradation of MB over CNT NPs in aqueous suspension was found to follow approximately first-order kinetics according to the Langmuir-Hinshelwood model. The enhanced photocatalytic degradation was attributed to the increased number of photogenerated·OH radicals.The enhanced photocatalytic degradation under visible light irradiation was attributed to the increasing number of photogenerated·OH radicals. The recombination of photogenerated e--h+ was attributed to be the key factor for the decrease in the photocatalytic degradation efficiency of MB.
The targeted dye sensitized solar cells in this study were fabricated using the modified nano-photocatalyst (N doped TiO_2 nanoparticles) as the electrode and N719 as the dye sensitizer. By enforced the connections between the conductivity film and dye, the absorbance of amount, the enhanced efficiency and life time of solar cells have been found. Meanwhile, the properties of photo-generated electrons have been studied in detailed, such as the electron life time, the electron density, the diffusion coefficient. The relationship between the properties of photo-generated electrons, the crystal structure, and the chemical component of N doped TiO_2 nanoparticles was dicussed in this part.
引文
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