二氧化钛光催化性能研究及纳米复合材料的制备
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摘要
二氧化钛半导体材料由于其强氧化性、化学性质稳定、无毒和价格低廉等优点而被广泛应用于气体传感器、太阳能电池、污水处理和空气净化等领域。然而由于二氧化钛的禁带宽度较大(锐钛型及金红石型二氧化钛的禁带宽度分别为3.2eV和3.0eV),只能吸收紫外光,而紫外光仅占太阳光的5%左右,对太阳能的利用率低。因此使二氧化钛对可见光产生响应从而提高二氧化钛半导体材料的太阳光利用效率是目前的研究热点。不同形态结构的二氧化钛半导体材料由于其独特的性能在不同的领域有各自潜在的应用。一维纳米结构材料(纳米线、纳米棒、纳米管、纳米棒)由于其独特的几何结构及新奇的物理化学性能而在纳米器件、药物释放、微电子和纳米传感器等领域具有潜在的应用。静电纺丝技术是制备一维二氧化钛纳米材料相对简单通用的方法。本论文采用简单可行的非水溶胶-凝胶法,以四氯化钛为前驱体,以乙醇为溶剂,不需要添加任何稳定剂即可成功制备带有醇盐结构的二氧化钛纳米粉体,然后利用二氧化钛纳米粉体制备了锐钛型二氧化钛水溶胶、DMF溶胶和碳掺杂二氧化钛纳米粉体。并利用锐钛型二氧化钛水溶胶的光催化聚合反应制备了PMMA／二氧化钛纳米杂化材料；以锐钛型二氧化钛DMF溶胶及PMMA聚合物为纺丝液,利用静电纺丝技术制备PMMA／锐钛型二氧化钛复合纤维,经过高温处理得到了具有可见光响应碳掺杂二氧化钛纳米纤维,并以亚甲基蓝为降解模型考察了碳掺杂二氧化钛纳米纤维的光催化降解活性；利用碳掺杂的二氧化钛纳米粉体在可见光下催化聚合制备PMMA聚合物,并对聚合产物进行了一系列的表征。本论文的主要研究工作和结果如下：
(1)利用非水溶胶-凝胶法简单方便的合成了结晶二氧化钛纳米粉体,把制备得到的二氧化钛纳米粉体分散到水中即可得到不同质量浓度的二氧化钛水溶胶。同时将二氧化钛纳米粉体分散到DMF溶剂中得到了不同质量浓度的二氧化钛DMF溶胶。当二氧化钛含量较低时,两种溶胶均保持较好的光学透明性和存放稳定性。XRD测试表明制备得到的二氧化钛水溶胶及DMF溶胶中的二氧化钛纳米颗粒保持了初始纳米粒子的锐钛型结晶结构,且结晶度较高。DLS测试显示随着二氧化钛质量浓度的增加,溶胶中的二氧化钛颗粒的尺寸也逐渐增大。
(2)不同含量的MAA偶联剂对二氧化钛水溶胶进行了表面改性,FT-IR分析证明MAA对二氧化钛的改性是有效的。利用改性后的二氧化钛水溶胶对MMA单体进行光催化聚合制备了PMMA二氧化钛杂化材料。结果显示MAA的引入有助于二氧化钛纳米粒子在PMMA聚合物基体中的均匀分散,从而有助于提高杂化材料的玻璃化温度、热稳定性和光学透明性。
(3)利用静电纺丝技术,以PMMA聚合物和锐钛型二氧化钛DMF溶胶为纺丝液制备了PMMA／结晶二氧化钛杂化纤维。再经高温处理得到具有可见光响应的锐钛型碳掺杂二氧化钛纳米纤维。XRD分析证明PMMA/二氧化钛杂化纤维中的无机组分仍保留了锐钛型二氧化钛的晶型。XPS结果表明可以通过对PMMA/二氧化钛杂化纤维的高温处理得到了碳掺杂二氧化钛纳米纤维。相对于PMMA/二氧化钛杂化纤维而言,碳掺杂二氧化钛纳米纤维表现出更高的可见光催化活性。具有可见光吸收的碳掺杂二氧化钛纳米纤维在污水处理及空气净化领域具有潜在的应用。
(4)利用制备得到的二氧化钛纳米粉体,经过热处理得到了碳掺杂二氧化钛纳米粉末。XRD分析表明碳掺杂的二氧化钛纳米粉体具有完美的锐钛型结晶相。根据XPS分析可知,制备得到的碳掺杂的二氧化钛纳米粉体具有两种掺杂形式碳原子。UV-Vis测试表明碳掺杂二氧化钛纳米粉体除了在紫外区域具有强的吸收之外,对可见光也具有很好的响应。利用碳掺杂二氧化钛纳米粉体在可见光条件下成功合成了PMMA聚合物。聚合物的数均分子量为1.28×106g／mol,分散系数为3.0。聚合物的玻璃化转变温度为127℃左右。碳掺杂的二氧化钛纳米颗粒有助于在光催化过程中更好的利用太阳光。
Titania has been widely used as gas sensors, solar-energy conversion and a promising photocatalyst for water and air purification because of its high oxidative power, chemical stability, low cost and nontoxicity. Unfortunately, one severe disadvantage of the titania semiconductor material is the large band gap of 3.0 or 3.2 eV in the rutile or anatase crystalline phase respectively and only absorbs the UV light which accounts for merely-5% of the solar spectrum.Therefore, there have been many efforts to extend activity of titania into the visible region to improve utilize efficiency of titania. Titania materials with different morphology and structure have applications in different fields. For their distinctive geometries, novel physical and chemical properties and potential applications in nanodevices, drug delivery, nanosensors and microelectronics,one-dimensional(1D)chemical nanostructures such as nanorods, nanowires, nanotubes, and nanobelts have attracted a great attention. Titania nanofibers and nanotubes had been successfully prepared by the electrospinning technique because it is a relatively simple and versatile method for fabricating ultrafine fibers. Herein, we used a convenient controlled nonhydrolytic sol-gel method to prepare alkoxide-bonded titania nanoparticles. The whole reaction procedure between TiCl4 and ethanol is simple without using any additional peptizing agent. Anatase titania hydrosol, anatase titania DMF sol and carbon-doped titania nanoparticles were prepared using the as-synthesized alkoxide-bonded titania nanoparticles. Then the PMMA/titania hybrid materials were prepared by the photocatalytic polymerization of the anatase titania hydrosol under the Xe light. The PMMA/titania hybrid nanofibers were prepared via the electrospinning method using the PMMA solution containing an anatase titania nonaqueous sol.After the calcination, the carbon-doped anatase titania nanofibers responded to the visible light were obtained. The PMMA polymer was also synthesized by the photocatalytic polymerization of the carbon-doped titania nanoparticles under visible light illumination. The main research content and results are as follows.
(1)The anatase titania nanoparticles prepared by a facile nonhydrolytic sol-gel reaction. Then the anatase titania nanoparticles were dispersed into water to form stale hydrosol.The titania DMF sol were also obtained by dispersing the anatase titania nanoparticles into DMF solvent. The two kinds of titania sols were stale and kept good transparency when the concentration of titania was low. The XRD patterns showed that the crystals of the titania in titania sols still retained the anatase phase and high crystalline. The DLS results exhibited the size of titania nanoparticles in the two kind sols gradually became large with increasing titania concentration.
(2) The surface modification of the titania nanoparticles was achieved by the formation of the bidentate coordination between titania and methacrylic acid molecules. The photocatalytic polymerization of methyl methacrylate was initiated by surface modified anatase titania nanoparticles under Xe lamp irradiation. The transparency of PMMA hybrid films was maintained because the modified titania nanoparticles were well dispersed in the polymer matrix.The glass transition temperatures and the thermal stabilities of PMMA nanocomposites prepared via photocatalytic polymerization were greatly improved compared with pure polymer.
(3) The PMMA/anatase titania hybrid nanofibers were prepared via electrospinning technique using the PMMA solution containing an anatase titania DMF sol. The carbon-doped titania nanofibers were also obtained by calcining the hybrid nanofibers. The XRD results showed that the anatase phase in the PMMA/titania hybrid nanofibers was preserved during the spinning. The XPS results demonstrated that the carbon doping into titania nanofibers was achieved via the calcination at 400℃. Compared with hybrid nanofibers, the carbon-doped titania nanofibers had higher photocatalytic activities toward the degradation of methylene blue under visible light irradiation. Therefore, the carbon-doped titania nanofibers showed promising applications in water cleaning and air purification.
(4) Carbon-doped titania nanoparticles in a pure anatase phase colored dark brown were successfully prepared using a convenient controlled nonhydrolytic sol-gel method followed by annealing at 400℃. The XPS indicated that substitutional and interstitial carbon atoms coexist in the lattice of titania. The UV-Vis spectrum showed that these carbon-doped titania nanoparticles exhibit significant photo response from UV to near infrared region in excess of 950 nm. The PMMA polymer was prepared by photocatalytic polymerization of the carbon-doped titania nanoparticles under the visible light illumination. The Mn of the purified PMMA was～1.28×106 g/mol and its polydispersity was 3.0. The glass transition temperature of obtained PMMA was about 127℃. This carbon-doped titania would be benefit to allow the more efficient use of sunlight in photocatalysis and photochemistry.
(1)利用非水溶胶-凝胶法简单方便的合成了结晶二氧化钛纳米粉体,把制备得到的二氧化钛纳米粉体分散到水中即可得到不同质量浓度的二氧化钛水溶胶。同时将二氧化钛纳米粉体分散到DMF溶剂中得到了不同质量浓度的二氧化钛DMF溶胶。当二氧化钛含量较低时,两种溶胶均保持较好的光学透明性和存放稳定性。XRD测试表明制备得到的二氧化钛水溶胶及DMF溶胶中的二氧化钛纳米颗粒保持了初始纳米粒子的锐钛型结晶结构,且结晶度较高。DLS测试显示随着二氧化钛质量浓度的增加,溶胶中的二氧化钛颗粒的尺寸也逐渐增大。
(2)不同含量的MAA偶联剂对二氧化钛水溶胶进行了表面改性,FT-IR分析证明MAA对二氧化钛的改性是有效的。利用改性后的二氧化钛水溶胶对MMA单体进行光催化聚合制备了PMMA二氧化钛杂化材料。结果显示MAA的引入有助于二氧化钛纳米粒子在PMMA聚合物基体中的均匀分散,从而有助于提高杂化材料的玻璃化温度、热稳定性和光学透明性。
(3)利用静电纺丝技术,以PMMA聚合物和锐钛型二氧化钛DMF溶胶为纺丝液制备了PMMA／结晶二氧化钛杂化纤维。再经高温处理得到具有可见光响应的锐钛型碳掺杂二氧化钛纳米纤维。XRD分析证明PMMA/二氧化钛杂化纤维中的无机组分仍保留了锐钛型二氧化钛的晶型。XPS结果表明可以通过对PMMA/二氧化钛杂化纤维的高温处理得到了碳掺杂二氧化钛纳米纤维。相对于PMMA/二氧化钛杂化纤维而言,碳掺杂二氧化钛纳米纤维表现出更高的可见光催化活性。具有可见光吸收的碳掺杂二氧化钛纳米纤维在污水处理及空气净化领域具有潜在的应用。
(4)利用制备得到的二氧化钛纳米粉体,经过热处理得到了碳掺杂二氧化钛纳米粉末。XRD分析表明碳掺杂的二氧化钛纳米粉体具有完美的锐钛型结晶相。根据XPS分析可知,制备得到的碳掺杂的二氧化钛纳米粉体具有两种掺杂形式碳原子。UV-Vis测试表明碳掺杂二氧化钛纳米粉体除了在紫外区域具有强的吸收之外,对可见光也具有很好的响应。利用碳掺杂二氧化钛纳米粉体在可见光条件下成功合成了PMMA聚合物。聚合物的数均分子量为1.28×106g／mol,分散系数为3.0。聚合物的玻璃化转变温度为127℃左右。碳掺杂的二氧化钛纳米颗粒有助于在光催化过程中更好的利用太阳光。
Titania has been widely used as gas sensors, solar-energy conversion and a promising photocatalyst for water and air purification because of its high oxidative power, chemical stability, low cost and nontoxicity. Unfortunately, one severe disadvantage of the titania semiconductor material is the large band gap of 3.0 or 3.2 eV in the rutile or anatase crystalline phase respectively and only absorbs the UV light which accounts for merely-5% of the solar spectrum.Therefore, there have been many efforts to extend activity of titania into the visible region to improve utilize efficiency of titania. Titania materials with different morphology and structure have applications in different fields. For their distinctive geometries, novel physical and chemical properties and potential applications in nanodevices, drug delivery, nanosensors and microelectronics,one-dimensional(1D)chemical nanostructures such as nanorods, nanowires, nanotubes, and nanobelts have attracted a great attention. Titania nanofibers and nanotubes had been successfully prepared by the electrospinning technique because it is a relatively simple and versatile method for fabricating ultrafine fibers. Herein, we used a convenient controlled nonhydrolytic sol-gel method to prepare alkoxide-bonded titania nanoparticles. The whole reaction procedure between TiCl4 and ethanol is simple without using any additional peptizing agent. Anatase titania hydrosol, anatase titania DMF sol and carbon-doped titania nanoparticles were prepared using the as-synthesized alkoxide-bonded titania nanoparticles. Then the PMMA/titania hybrid materials were prepared by the photocatalytic polymerization of the anatase titania hydrosol under the Xe light. The PMMA/titania hybrid nanofibers were prepared via the electrospinning method using the PMMA solution containing an anatase titania nonaqueous sol.After the calcination, the carbon-doped anatase titania nanofibers responded to the visible light were obtained. The PMMA polymer was also synthesized by the photocatalytic polymerization of the carbon-doped titania nanoparticles under visible light illumination. The main research content and results are as follows.
(1)The anatase titania nanoparticles prepared by a facile nonhydrolytic sol-gel reaction. Then the anatase titania nanoparticles were dispersed into water to form stale hydrosol.The titania DMF sol were also obtained by dispersing the anatase titania nanoparticles into DMF solvent. The two kinds of titania sols were stale and kept good transparency when the concentration of titania was low. The XRD patterns showed that the crystals of the titania in titania sols still retained the anatase phase and high crystalline. The DLS results exhibited the size of titania nanoparticles in the two kind sols gradually became large with increasing titania concentration.
(2) The surface modification of the titania nanoparticles was achieved by the formation of the bidentate coordination between titania and methacrylic acid molecules. The photocatalytic polymerization of methyl methacrylate was initiated by surface modified anatase titania nanoparticles under Xe lamp irradiation. The transparency of PMMA hybrid films was maintained because the modified titania nanoparticles were well dispersed in the polymer matrix.The glass transition temperatures and the thermal stabilities of PMMA nanocomposites prepared via photocatalytic polymerization were greatly improved compared with pure polymer.
(3) The PMMA/anatase titania hybrid nanofibers were prepared via electrospinning technique using the PMMA solution containing an anatase titania DMF sol. The carbon-doped titania nanofibers were also obtained by calcining the hybrid nanofibers. The XRD results showed that the anatase phase in the PMMA/titania hybrid nanofibers was preserved during the spinning. The XPS results demonstrated that the carbon doping into titania nanofibers was achieved via the calcination at 400℃. Compared with hybrid nanofibers, the carbon-doped titania nanofibers had higher photocatalytic activities toward the degradation of methylene blue under visible light irradiation. Therefore, the carbon-doped titania nanofibers showed promising applications in water cleaning and air purification.
(4) Carbon-doped titania nanoparticles in a pure anatase phase colored dark brown were successfully prepared using a convenient controlled nonhydrolytic sol-gel method followed by annealing at 400℃. The XPS indicated that substitutional and interstitial carbon atoms coexist in the lattice of titania. The UV-Vis spectrum showed that these carbon-doped titania nanoparticles exhibit significant photo response from UV to near infrared region in excess of 950 nm. The PMMA polymer was prepared by photocatalytic polymerization of the carbon-doped titania nanoparticles under the visible light illumination. The Mn of the purified PMMA was～1.28×106 g/mol and its polydispersity was 3.0. The glass transition temperature of obtained PMMA was about 127℃. This carbon-doped titania would be benefit to allow the more efficient use of sunlight in photocatalysis and photochemistry.
引文
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