微波辅助N、S共掺杂纳米TiO_2制备、表征及光催化性能研究
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摘要
在全球性环境污染和能源危机日趋严重的今天,如何有效利用太阳能来治理污染已引起世界各国的广泛关注。半导体氧化物多相光催化技术,因具有能广泛地利用太阳能,并且能耗低、反应条件温和、操作简便、无二次污染、特别对生物难降解有机污染物具有很好的氧化降解作用等突出特点,已成为环境污染控制和治理方面的研究热点。在众多的半导体氧化物中,TiO_2因其良好的光电特性,光照射下能够被光子激活,在表面发生很强的氧化(或还原)作用,将绝大多数有机污染物降解并最终完全矿化为CO_2、H_2O和其他一些无机小分子物质而消除对环境的污染,以及化学性质稳定、安全无毒、来源丰富等特点,使之成为目前最为广泛和成熟的半导体氧化物材料之一。然而, TiO_2的禁带宽度较大(锐钛矿型TiO_2的Eg≈3.2eV),光催化仅限于紫外光区,而太阳光中紫外光(300nm～400nm)的含量只占3%～4%,太阳能利用率低;并且量子产率同样较低。因此,本文拟采取掺杂的方式制备高性能的TiO_2催化材料,以提高其光催化效率。
本文首先简要介绍了半导体光催化的基本原理,在总结和评述了提高半导体光催化总量子效率和太阳能利用率的各种方法及其研究进展和面临的主要问题的基础上,采用廉价易得的无机盐TiCl_4为钛源,硫脲为均相沉淀剂并提供硫元素,在微波辐照下合成了S掺杂的纳米TiO_2前驱体,然后在NH3/N2气氛中经程序升温的煅烧处理得到N、S共掺杂纳米TiO_2光催化剂。以纳米TiO_2的平均晶粒度、晶相结构和光催化活性为指标,考察了TiCl_4初始浓度、微波作用功率、微波作用时间、微波作用温度以及NH_3/N_2气氛中氮化温度等因素对制备的光催化剂性能的影响,得到N、S共掺杂纳米TiO_2制备的最佳工艺条件:初始c(Ti4+)为0.9 mol·L-1,微波作用功率900W,微波作用时间0.5h,微波作用温度95℃,NH2/N2气氛中高温氮化温度500℃。
采用XRD、UV-Vis/DRS、FT-IR、XPS、TG-DTA和TEM等现代分析测试手段对所制备的N、S共掺杂纳米TiO_2结构和性能进行表征。结果表明,所制备的N、S共掺杂可见光响应纳米TiO_2光催化剂为锐钛矿型和金红石型的混晶,晶粒基本呈球形或类球形,平均晶粒度在15～20nm之间;N元素以两种掺杂态存在:一种是以N_3-替位取代O_2-进入TiO_2晶格形成Ti-N-Ti联接的掺杂态,另一种是通过化学吸附NH_3或NH_4~+进入晶格原子间隙产生的掺杂态;S元素掺杂以S~(6+)取代Ti~(4+)进入TiO_2晶格,使晶格局部畸变,导致TiO_2的带隙变窄;而N、S共掺杂纳米TiO_2具有可见光催化活性是因为N、S元素的掺杂在禁带形成了新的杂质能级,使光催化剂的吸收边带红移至500～550nm处。
掺杂N、S元素的纳米TiO_2具有较强的光催化活性,光催化剂对甲基橙的可见光催化降解满足准一级动力学模型,且N、S元素的共掺杂对光催化剂的可见光催化活性具有协同作用。
同时,离子液体的添加对光催化剂的晶相组成有很大影响,并且有助于N、S元素的掺杂;添加阴离子为[BF_4]~-的离子液体可以引起F~-吸附在TiO_2表面的F元素掺杂;可见光降解甲基橙表明,添加离子液体后催化剂可见光活性得到提高。最后,初步探讨了其提高可见光活性机理。
Environment pollution and energy resource crisis are the hot topics today and, effective utilization of solar energy to solve pollution problems attains much attention now. With outstandingly characteristics in widely utilization of solar energy, low energy consumption, moderate reaction condition, convenient operation, no secondary pollution, and good oxidation degradation for bio-refractory organic pollutants, the semiconductor oxide heterogeneous photocatalytic technology is a hot research topic in environment science. Among those semiconductor oxides, TiO_2 has excellent photoelectric properties, which can activate photoelectron, occuring redox reaction on surface, decomposing most organic pollutants and mineralizing them into CO2, H2O and other small inorganic molecules completely under light irradiation. TiO_2 is also chemical stable, safe and imnoxious, abundant source. However, the energy band-gap of TiO_2 in the anatase crystalline is wide (Eg≈3.2eV) and it can only catalyze the degradation of persistent organic pollutants under ultraviolet light (300nm～400nm) irradiation, which accounts for only a small part (3%～5%) of solar energy with low quantun yield. The present work is focused on preparation of doped TiO_2 to get good photocatalytic performance catalyst.
In this dissertation, the basic principle about semiconductor photocatalysis was reviewed briefly at first. The methods, research progress and main problems about improving the total quantum-efficiency and utilization effeiciency of solar energy for semiconductor photocatalysis have been summarized. Then, the more available and cheaper inorganic TiCl_4 was used as raw material, and thiourea was used as the precipitator, as well as supply sulfur, S-doped nanosize TiO_2 precursors were prepared by homogeneous precipitation via microwave irradiation. And then N, S-codoped nanosize TiO_2 were prepared with temperature-programmed calcinations in NH_3/N_2 atmosphere. With the indexes of the average grain size, crystal composition, and photo catalytic activity of nanosize TiO_2, the initial TiCl_4 concentration, microwave power, microwave reaction time, microwave reaction temperature and calcinations temperature in NH_3/N_2 atmosphere on photocatalyst were studied. And process parameters were optimized also. The results showed N, S-codoped nanosize TiO_2 photocatalytic activity is upmost under the follow conditions: initial TiCl4 concentration, 0.9 mol·L~(-1); microwave power, 900W; microwave reaction time, 0.5h; microwave reaction temperature, 95℃; calcinations temperature in NH_3/N_2 atmosphere, 500℃.
The crystal structure and properties of N, S-codoped nanosize TiO_2 were characterized by XRD, UV-Vis/DRS, FT-IR, XPS and TEM. The results showed that the catalyst has mixed phase structure of anatase and rutile. The nanoparticle were spherical or spherical-like, and the particle size in the range of 15～20nm; Nitrogen was existed in two doping states: one is substitutional N impurity, which formated joint of Ti-N-Ti doping state, another is interstitial impurity by chemical-adsorption of NH_3 or NH4+; Sulfur ions (S6+) substituted partially for the lattice titanium ions (Ti~(4+)), which resulted in the localized crystal deformation of TiO_2 and the bandgap between valence band and conduction band narrowed. Visible-light photocatalytic activity obtained by N, S-codoped nanosize TiO_2, was because of formation of a new impurity level, which led it’s absorption spectrum red-shft to 500～550nm.
N, S-codoped nanosize TiO_2 has higher photocatalytic activity, and the degradation of MO in visible-light irradiation was proved fitted the pesudo-first-order model. The higher photocatalytic activity also attributed to the synergetic of N, S-codoped.
Besides, the crystal phase composition of photocatalysts were effected by ionic liquid addition, and it could also assisted to nitrogen and sulfur doping. Ionic liquid with anion of [BF_4]~- could cause F-doping which F~- absorbed on N, S-codoped nanosize TiO_2. The degradation of MO showed that the visible-light activity was improved by adding ionic liquid. The mechanism of visible-light improved with ionic liquid addition has been also discussed in the wnd.
本文首先简要介绍了半导体光催化的基本原理,在总结和评述了提高半导体光催化总量子效率和太阳能利用率的各种方法及其研究进展和面临的主要问题的基础上,采用廉价易得的无机盐TiCl_4为钛源,硫脲为均相沉淀剂并提供硫元素,在微波辐照下合成了S掺杂的纳米TiO_2前驱体,然后在NH3/N2气氛中经程序升温的煅烧处理得到N、S共掺杂纳米TiO_2光催化剂。以纳米TiO_2的平均晶粒度、晶相结构和光催化活性为指标,考察了TiCl_4初始浓度、微波作用功率、微波作用时间、微波作用温度以及NH_3/N_2气氛中氮化温度等因素对制备的光催化剂性能的影响,得到N、S共掺杂纳米TiO_2制备的最佳工艺条件:初始c(Ti4+)为0.9 mol·L-1,微波作用功率900W,微波作用时间0.5h,微波作用温度95℃,NH2/N2气氛中高温氮化温度500℃。
采用XRD、UV-Vis/DRS、FT-IR、XPS、TG-DTA和TEM等现代分析测试手段对所制备的N、S共掺杂纳米TiO_2结构和性能进行表征。结果表明,所制备的N、S共掺杂可见光响应纳米TiO_2光催化剂为锐钛矿型和金红石型的混晶,晶粒基本呈球形或类球形,平均晶粒度在15～20nm之间;N元素以两种掺杂态存在:一种是以N_3-替位取代O_2-进入TiO_2晶格形成Ti-N-Ti联接的掺杂态,另一种是通过化学吸附NH_3或NH_4~+进入晶格原子间隙产生的掺杂态;S元素掺杂以S~(6+)取代Ti~(4+)进入TiO_2晶格,使晶格局部畸变,导致TiO_2的带隙变窄;而N、S共掺杂纳米TiO_2具有可见光催化活性是因为N、S元素的掺杂在禁带形成了新的杂质能级,使光催化剂的吸收边带红移至500～550nm处。
掺杂N、S元素的纳米TiO_2具有较强的光催化活性,光催化剂对甲基橙的可见光催化降解满足准一级动力学模型,且N、S元素的共掺杂对光催化剂的可见光催化活性具有协同作用。
同时,离子液体的添加对光催化剂的晶相组成有很大影响,并且有助于N、S元素的掺杂;添加阴离子为[BF_4]~-的离子液体可以引起F~-吸附在TiO_2表面的F元素掺杂;可见光降解甲基橙表明,添加离子液体后催化剂可见光活性得到提高。最后,初步探讨了其提高可见光活性机理。
Environment pollution and energy resource crisis are the hot topics today and, effective utilization of solar energy to solve pollution problems attains much attention now. With outstandingly characteristics in widely utilization of solar energy, low energy consumption, moderate reaction condition, convenient operation, no secondary pollution, and good oxidation degradation for bio-refractory organic pollutants, the semiconductor oxide heterogeneous photocatalytic technology is a hot research topic in environment science. Among those semiconductor oxides, TiO_2 has excellent photoelectric properties, which can activate photoelectron, occuring redox reaction on surface, decomposing most organic pollutants and mineralizing them into CO2, H2O and other small inorganic molecules completely under light irradiation. TiO_2 is also chemical stable, safe and imnoxious, abundant source. However, the energy band-gap of TiO_2 in the anatase crystalline is wide (Eg≈3.2eV) and it can only catalyze the degradation of persistent organic pollutants under ultraviolet light (300nm～400nm) irradiation, which accounts for only a small part (3%～5%) of solar energy with low quantun yield. The present work is focused on preparation of doped TiO_2 to get good photocatalytic performance catalyst.
In this dissertation, the basic principle about semiconductor photocatalysis was reviewed briefly at first. The methods, research progress and main problems about improving the total quantum-efficiency and utilization effeiciency of solar energy for semiconductor photocatalysis have been summarized. Then, the more available and cheaper inorganic TiCl_4 was used as raw material, and thiourea was used as the precipitator, as well as supply sulfur, S-doped nanosize TiO_2 precursors were prepared by homogeneous precipitation via microwave irradiation. And then N, S-codoped nanosize TiO_2 were prepared with temperature-programmed calcinations in NH_3/N_2 atmosphere. With the indexes of the average grain size, crystal composition, and photo catalytic activity of nanosize TiO_2, the initial TiCl_4 concentration, microwave power, microwave reaction time, microwave reaction temperature and calcinations temperature in NH_3/N_2 atmosphere on photocatalyst were studied. And process parameters were optimized also. The results showed N, S-codoped nanosize TiO_2 photocatalytic activity is upmost under the follow conditions: initial TiCl4 concentration, 0.9 mol·L~(-1); microwave power, 900W; microwave reaction time, 0.5h; microwave reaction temperature, 95℃; calcinations temperature in NH_3/N_2 atmosphere, 500℃.
The crystal structure and properties of N, S-codoped nanosize TiO_2 were characterized by XRD, UV-Vis/DRS, FT-IR, XPS and TEM. The results showed that the catalyst has mixed phase structure of anatase and rutile. The nanoparticle were spherical or spherical-like, and the particle size in the range of 15～20nm; Nitrogen was existed in two doping states: one is substitutional N impurity, which formated joint of Ti-N-Ti doping state, another is interstitial impurity by chemical-adsorption of NH_3 or NH4+; Sulfur ions (S6+) substituted partially for the lattice titanium ions (Ti~(4+)), which resulted in the localized crystal deformation of TiO_2 and the bandgap between valence band and conduction band narrowed. Visible-light photocatalytic activity obtained by N, S-codoped nanosize TiO_2, was because of formation of a new impurity level, which led it’s absorption spectrum red-shft to 500～550nm.
N, S-codoped nanosize TiO_2 has higher photocatalytic activity, and the degradation of MO in visible-light irradiation was proved fitted the pesudo-first-order model. The higher photocatalytic activity also attributed to the synergetic of N, S-codoped.
Besides, the crystal phase composition of photocatalysts were effected by ionic liquid addition, and it could also assisted to nitrogen and sulfur doping. Ionic liquid with anion of [BF_4]~- could cause F-doping which F~- absorbed on N, S-codoped nanosize TiO_2. The degradation of MO showed that the visible-light activity was improved by adding ionic liquid. The mechanism of visible-light improved with ionic liquid addition has been also discussed in the wnd.
引文
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