Mn，N掺杂纳米二氧化钛的制备及其光催化性能研究
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摘要
纳米TiO_2具有高的氧化还原能力、化学性质稳定、对人体无毒和成本低等优点,在利用太阳能的半导体中受到重视。近来TiO_2被广泛应用到空气净化(例如NOx及VOCs的降解)、杀菌以及水质净化方面,并可以将大多数有机污染物最终降解成为CO2、H2O以及其它无机小分子物质。但TiO_2禁带宽度大(3.2 eV),只能利用太阳光中的紫外线部分(仅占太阳光能3~5%),此外,光生电子与空穴的高复合几率还会降低光量子产率,这使TiO_2作为光催化剂在实际应用中难以大规模推广。考虑到以上因素,本研究使用锰、氮共掺杂TiO_2 ,对其进行改性研究,以期使TiO_2的吸收波长向可见光方向移动,并使TiO_2的光催化活性得到提高。
分别以MnSO4·H2 O和MnC2 O4·4H2O为锰源,采用水热法制备了锰掺杂的Mn-TiO_2光催化剂,并采用X-射线衍射、紫外-可见光漫反射光谱等技术对样品进行了表征。以罗丹明B的光催化降解为模型反应,考察了不同锰源、锰掺杂量对催化剂光催化性能的影响。结果表明,所有制备的Mn-TiO_2均表现为锐钛矿相,Mn的掺杂抑制了TiO_2晶粒生长,且以MnSO4·H2 O为锰源制备的Mn-TiO_2粒径略小于以MnC2 O4·4H2O为锰源制备的样品,所有Mn-TiO_2催化剂的光响应范围拓宽至可见光区域,对罗丹明B具有明显的可见光降解效果,并且以MnSO4·H2 O为锰源的催化剂具有较高的光催化活性。
采用溶胶-凝胶法成功合成了具有可见光响应的不同锰掺杂量的Mn-TiO_2和Mn-N-TiO_2光催化剂,并采用XRD、UV-vis、XPS、ESR等技术考察了锰掺杂量、多元掺杂、煅烧温度等因素对催化剂结构性质的影响。结果表明在400℃热处理的Mn-TiO_2和Mn-N-TiO_2样品均表现为锐钛矿晶型,Mn、N掺杂对TiO_2由锐钛矿相向金红石相的转变有明显抑制作用,其光响应范围拓宽至可见光区域。400℃热处理的Mn-N-TiO_2-400的XPS图谱表明N原子取代TiO_2中O形成Ti-N结构,同时发现加入了少量的Mn后,促进N元素在TiO_2的有效掺杂。以罗丹明B的光催化降解为模型反应表明,掺杂N、Mn元素后,催化剂对罗丹明B具有明显的可见光降解效果,并且Mn-N-TiO_2的可见光光催化活性优于TiO_2 ,N-TiO_2及Mn-TiO_2。
Photocatalysis based on powdered semiconductors has received much attention for the effective utilization of solar energy. Among all semiconductors, TiO_2 is the most widely studied photocatalyst, due to its strong redox ability, chemical stability, non-toxicity, and cheapness. Recently, TiO_2 is extensively applied to the purification of air such as De-NOx, De-VOCs, the bactericidal action, and degradation of organic pollutant compounds in wastewater. It can decompose most organic pollutants into CO2 , H2O, and other small inorganic molecules under UV light irradiation. However, TiO_2 absorbs only the very small ultraviolet part (3~5%) of solar light due to its wide band-gap (3.2 eV for anatase form). In addition, easy recombination of photo-induced electrons and holes makes the efficiency of photoquantum lower. These unfavorable factors make the large scale application of TiO_2 as mutual photocatalyst hampered. Considering the above factors, manganese and nitrogen was doped into TiO_2 to make its absorbing wavelength move to the visible light region and improve its photocatalytic performance.
Mn-doped TiO_2 nanocrystal photocatalysts, named Mn-TiO_2-S and Mn-TiO_2-C samples, were synthesized by a simple hydrothermal synthesis method using MnSO4·H2O and MnC2 O4·4H2O as manganese source, respectively. The samples were characterized by X-ray diffraction and UV-vis diffuse reflectance spectroscopy. The photocatalytic activity for the degradation of rhodamine B was evaluated, and the effects of the manganese source and Mn doping amount were investigated. The results showed that all of the Mn-TiO_2 had an anatase crystallite structure and the Mn doping inhibited the growth of the TiO_2 particles. The particle size of Mn-TiO_2 -S was smaller than that of Mn-TiO_2-C. The absorption edge of Mn-TiO_2 shifted to the visible light region. The Mn-TiO_2 showed obvious photocatalytic activity for the degradation of rhodamine B under visible light irradiation, and Mn-TiO_2-S samples showed higher photocatalytic activity than undoped TiO_2 and Mn-TiO_2-C samples.
Mn-doped and Mn-N-codeped TiO_2 nanocrystal photocatalysts were synthesized by sol-gel method. XRD, UV-vis, XPS, ESR were employed to characterize the structure of undoped TiO_2 and doped TiO_2 powders, and the effects of the Mn-N-codoping, Mn doping amount and heat treatment temperature were investigated. The results showed that all of the Mn-TiO_2 and Mn-N-TiO_2 had an anatase crystallite structure and Mn-N-codoping promote the phase transition from anatase phase to rutile phase. The absorption edge of Mn-TiO_2 and Mn-N-TiO_2 shifted to the visible light region. The XPS survey spectrum of Mn-N-TiO_2-400 sample calcined at 400℃suggsted that some N atoms substitute O atoms in TiO_2 lattice, and the introduction of a small amount of Mn facilitates further N uptake. N-TiO_2, Mn-TiO_2 and Mn-N-TiO_2 samples showed obvious photocatalytic activity for the degradation of rhodamine B under visible light irradiation, and Mn-N-TiO_2 samples showed higher photocatalytic activity than undoped TiO_2 , N-TiO_2 and Mn-TiO_2 samples.
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分别以MnSO4·H2 O和MnC2 O4·4H2O为锰源,采用水热法制备了锰掺杂的Mn-TiO_2光催化剂,并采用X-射线衍射、紫外-可见光漫反射光谱等技术对样品进行了表征。以罗丹明B的光催化降解为模型反应,考察了不同锰源、锰掺杂量对催化剂光催化性能的影响。结果表明,所有制备的Mn-TiO_2均表现为锐钛矿相,Mn的掺杂抑制了TiO_2晶粒生长,且以MnSO4·H2 O为锰源制备的Mn-TiO_2粒径略小于以MnC2 O4·4H2O为锰源制备的样品,所有Mn-TiO_2催化剂的光响应范围拓宽至可见光区域,对罗丹明B具有明显的可见光降解效果,并且以MnSO4·H2 O为锰源的催化剂具有较高的光催化活性。
采用溶胶-凝胶法成功合成了具有可见光响应的不同锰掺杂量的Mn-TiO_2和Mn-N-TiO_2光催化剂,并采用XRD、UV-vis、XPS、ESR等技术考察了锰掺杂量、多元掺杂、煅烧温度等因素对催化剂结构性质的影响。结果表明在400℃热处理的Mn-TiO_2和Mn-N-TiO_2样品均表现为锐钛矿晶型,Mn、N掺杂对TiO_2由锐钛矿相向金红石相的转变有明显抑制作用,其光响应范围拓宽至可见光区域。400℃热处理的Mn-N-TiO_2-400的XPS图谱表明N原子取代TiO_2中O形成Ti-N结构,同时发现加入了少量的Mn后,促进N元素在TiO_2的有效掺杂。以罗丹明B的光催化降解为模型反应表明,掺杂N、Mn元素后,催化剂对罗丹明B具有明显的可见光降解效果,并且Mn-N-TiO_2的可见光光催化活性优于TiO_2 ,N-TiO_2及Mn-TiO_2。
Photocatalysis based on powdered semiconductors has received much attention for the effective utilization of solar energy. Among all semiconductors, TiO_2 is the most widely studied photocatalyst, due to its strong redox ability, chemical stability, non-toxicity, and cheapness. Recently, TiO_2 is extensively applied to the purification of air such as De-NOx, De-VOCs, the bactericidal action, and degradation of organic pollutant compounds in wastewater. It can decompose most organic pollutants into CO2 , H2O, and other small inorganic molecules under UV light irradiation. However, TiO_2 absorbs only the very small ultraviolet part (3~5%) of solar light due to its wide band-gap (3.2 eV for anatase form). In addition, easy recombination of photo-induced electrons and holes makes the efficiency of photoquantum lower. These unfavorable factors make the large scale application of TiO_2 as mutual photocatalyst hampered. Considering the above factors, manganese and nitrogen was doped into TiO_2 to make its absorbing wavelength move to the visible light region and improve its photocatalytic performance.
Mn-doped TiO_2 nanocrystal photocatalysts, named Mn-TiO_2-S and Mn-TiO_2-C samples, were synthesized by a simple hydrothermal synthesis method using MnSO4·H2O and MnC2 O4·4H2O as manganese source, respectively. The samples were characterized by X-ray diffraction and UV-vis diffuse reflectance spectroscopy. The photocatalytic activity for the degradation of rhodamine B was evaluated, and the effects of the manganese source and Mn doping amount were investigated. The results showed that all of the Mn-TiO_2 had an anatase crystallite structure and the Mn doping inhibited the growth of the TiO_2 particles. The particle size of Mn-TiO_2 -S was smaller than that of Mn-TiO_2-C. The absorption edge of Mn-TiO_2 shifted to the visible light region. The Mn-TiO_2 showed obvious photocatalytic activity for the degradation of rhodamine B under visible light irradiation, and Mn-TiO_2-S samples showed higher photocatalytic activity than undoped TiO_2 and Mn-TiO_2-C samples.
Mn-doped and Mn-N-codeped TiO_2 nanocrystal photocatalysts were synthesized by sol-gel method. XRD, UV-vis, XPS, ESR were employed to characterize the structure of undoped TiO_2 and doped TiO_2 powders, and the effects of the Mn-N-codoping, Mn doping amount and heat treatment temperature were investigated. The results showed that all of the Mn-TiO_2 and Mn-N-TiO_2 had an anatase crystallite structure and Mn-N-codoping promote the phase transition from anatase phase to rutile phase. The absorption edge of Mn-TiO_2 and Mn-N-TiO_2 shifted to the visible light region. The XPS survey spectrum of Mn-N-TiO_2-400 sample calcined at 400℃suggsted that some N atoms substitute O atoms in TiO_2 lattice, and the introduction of a small amount of Mn facilitates further N uptake. N-TiO_2, Mn-TiO_2 and Mn-N-TiO_2 samples showed obvious photocatalytic activity for the degradation of rhodamine B under visible light irradiation, and Mn-N-TiO_2 samples showed higher photocatalytic activity than undoped TiO_2 , N-TiO_2 and Mn-TiO_2 samples.
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引文
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