基于天然纤维素物质的含钛无机纳米功能材料的制备及性质研究
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摘要
世界经济的快速发展给社会带来了巨大的物质财富。但是,人们在享受经济发展及科技进步的同时,也不可避免的面临着环境污染及能源枯竭问题。能源短缺及能源的过度使用造成的环境问题正威胁着人类的生存与发展,成为人类面临的两大难题。纳米材料的迅猛发展极大的促进了科学技术的进步,有望在环境污染治理及新能源开发方面提供新的技术力量。二氧化钛纳米材料由于具有化学性质稳定、催化性能高、无毒无污染、价廉易得等诸多优点而成为半导体领域研究的热点。在纳米二氧化钛材料的合成及制备方法中,生物模板法由于具有制备方法简单、得到的纳米材料具有形貌及尺寸可控等优点而引起了人们的广泛兴趣。其中,天然纤维素材料来源广泛、无毒无污染、可降解且具有复杂的多层分级结构,是设计及合成各种功能纳米材料的理想模板。
本文以天然纤维素材料(定量滤纸)作为模板及构筑复合纳米材料的支架,通过表面溶胶-凝胶法在纤维素表面沉积二氧化钛超薄膜,之后通过惰性氛围碳化或是空气中煅烧的方法,制备得到了二氧化钛/碳纳米纤维复合材料或是二氧化钛纳米管材料。这些材料可作为金属纳米颗粒沉积的载体,来制备具有特定功能的复合纳米材料,主要结论如下：
(1)二氧化钛包裹的碳纳米纤维材料。以实验室常用的滤纸为模板,以钛酸四丁酯为前体物,通过表面溶胶-凝胶法,把二氧化钛超薄膜沉积到滤纸纤维素的表面。之后将二氧化钛超薄膜沉积的滤纸复合材料置于管式炉中,氮气氛围中碳化,纤维素转变为无定形碳纤维,同时,二氧化钛凝胶层超薄膜转变为锐钛矿型二氧化钛。SEM及TEM观察发现,该材料在微观上复制了滤纸纤维素材料复杂的多层分级结构及形貌特征,二氧化钛超薄膜(-12nm)均匀的包裹在碳纳米纤维上,且由颗粒尺寸均一的二氧化钛纳米颗粒组成。由于二氧化钛薄膜的包裹,纤维素纤维在碳化的过程中避免了高温烧结与聚集,因此具有较大的比表面积(404m2/g)。光催化实验结果表明,该材料在紫外光及太阳光的照射下,对水体中的染料具有良好的降解效果。我们对光催化降解染料的机理也做了一些研究,结果表明,在光照的作用下,二氧化钛包裹的碳纳米纤维材料会产生·OH自由基及·O2-,从而对染料具有极强的降解效果。光催化循环利用实验表明,经过3次循环之后,样品在180min内,仍然可以降解81%的亚甲基蓝染料。
(2)银纳米颗粒负载的二氧化钛包裹的碳纳米纤维材料。以钛酸四丁酯为前体物,通过表面溶胶-凝胶法在滤纸纤维素表面沉积二氧化钛超薄膜,通过氮气氛围中碳化的方法,将滤纸纤维素转变为碳纳米纤维,得到二氧化钛包裹的碳纳米纤维材料。将该材料浸泡在硝酸银溶液中,通过光照还原的方法,将Ag+转变为银纳米颗粒,得到银纳米颗粒负载的二氧化钛包裹的碳纳米纤维材料。通过SEM和TEM观察可以看到,该材料复制了滤纸纤维素的多层分级结构和形貌特征,二氧化钛超薄膜均匀的包裹在碳纳米纤维上,上面负载的银纳米颗粒分布均匀,颗粒尺寸均一且粒径较小,平均直径仅有5nm。因为多孔碳纳米纤维的存在,银纳米颗粒在二氧化钛包裹的碳纤维材料中的负载量也相对较高,可达9.5wt.%左右。抗菌实验结果表明,该材料对革兰氏阴性菌(大肠杆菌)及革兰氏阳性菌(金黄色葡萄球菌)均具有良好的抗菌效果,抗菌率分别为99.7%和72.1%。
(3)氮化钛纳米管材料。首先以钛酸四丁酯为前体物,通过溶胶-凝胶法,将二氧化钛凝胶层沉积到滤纸纤维素表面,在空气中煅烧除掉滤纸,得到锐钛矿型二氧化钛纳米管材料；然后将二氧化钛纳米管材料和镁粉以2.5：1的比例置于反应釜中,通入氮气,1200℃发生高温镁热还原反应,生成氮化钛纳米管材料。通过SEM和TEM观察可以发现,氮化钛纳米管材料在复制了滤纸纤维素的微观形貌和结构特征,氮化钛纳米管的管壁均匀,平均厚度为46nm。氮气吸附-脱附曲线表明,氮化钛纳米管材料具有相对较大的比表面积,为31.4m2/g。我们对氮化钛纳米管材料的电化学性质做了测试,结果表明,氮化钛纳米管材料具有典型双层超级电容器的特性,当放电电流为0.16A/g时,比电容可达74.2F/g。
(4)铂纳米颗粒负载的二氧化钛纳米管材料。以钛酸四丁酯为前体物,通过表面溶胶-凝胶法,在滤纸纤维素的表面沉积二氧化钛超薄膜,然后在空气中高温煅烧除掉滤纸模板,得到锐钛矿型二氧化钛纳米管材料。将二氧化钛纳米管材料浸渍在不同浓度的水合六氯铂酸溶液中,通过光照还原的方法,产生铂纳米颗粒,得到了铂纳米颗粒负载的二氧化钛纳米管材料。SEM和TEM观察发现,该材料在微观上复制了滤纸纤维素的多层分级结构和形貌特征,铂纳米颗粒分布均匀,大小尺寸在2-4nm之间。光催化产氢实验结果表明,当铂纳米颗粒的负载量为1wt.%左右时,其光催化产氢的活性最高,平均产氢速率为164.4μmol/h。我们对铂纳米颗粒负载的二氧化钛纳米管材料光催化产氢的性能做了循环利用,发现在5次循环利用之后,样品仍具有较高的光催化产氢性能。对其光催化产氢的机理研究表明,在二氧化钛纳米管材料中负载铂纳米颗粒之后,光照产生的·OH自由基显著增多。
The rapid progress in global economy has not only brought us fabulous wealth but also environmental problems.Energy exhaustion and environment pollution has become global problems faced today.Thus,providing abundant, clean, and secure renewable energy sources is one of the key technological challenges facing mankind. Nanomaterial possesses unique physical and chemical properties and an exponential growth of research activities has been seen in nanoscience and nanotechnology in the past decades. As one of the most promising photocatalysts, titania has attracted much attention due to its chemical stability, high phocatalytic activity, nontoxicity and low cost. Amongst various preparation methods, biotemplate synthesis is one of the most attractive production methods for its effectiveness and easy control of nanostructure and morphology. Particularly, natural cellulose substance is an ideal biotemplate due to its unique structures and properties.
Herein, titania thin film was first deposited on natural cellulose substance (filter paper) by the surface sol-gel method using titanium(Ⅳ)n-butoxide as precursor. Subsequently, the titania/filter paper nanocomposite was carbonized in nitrogen or calcined in air to obtain titania coated carbon nanofibrous material or titania nanotubular material.Metal nanoparticles such as Ag or Pt nanoparticles can be deposited on the titania coated carbon nanofibrous material or titania nanotubular material to obtain composite material with tailored properties.
(1)Titania coated carbon nanofibrous material. Ultrathin titania films were firstly deposited by the surface sol-gel process to coat each nanofiber in the filter paper, and successive calcination treatment under nitrogen atmosphere yielded the titania-carbon composite possessing the hierarchical morphologies and structures of the initial paper. The ultrathin titania coating hindered the coalescence effect of the carbon species that formed during the carbonization process of cellulose, and the original cellulose nanofibers were converted into porous carbon nanofibers (diameters from tens to hundreds of nanometers, with3-6nm pores) that coated with uniform anatase titania thin films (thickness-12nm, composed of anatase nanocrystals with sizes of～4.5 nm). This titania-coated nanofibrous carbon material possesses specific surface area of404m2/g, which is two orders of magnitude higher than the titania/cellulose hybrid prepared by atomic layer deposition of titania on the cellulose fibers of filter paper. The photocatalytic activity of the titania-carbon composite was evaluated by the improved photodegradation efficiency of different dyes in aqueous solutions under high-pressure fluorescent mercury lamp irradiation, as well as the effective photoreduction performance of silver cations to silver nanoparticles with ultraviolet irradiation. Experimental results showed that·OH radicals were detected under UV irradiation.
(2) Titania-carbon composite material deposited with silver nanoparticles.Titania ultrathin film was first deposited on natural cellulose substance by means of a surface sol-gel method using titanium (Ⅳ) n-butoxide as precursor. Subsequently, the titania/filter paper composite material was carbonized in nitrogen atmosphere to obtanin titania coated carbon nanofibrous material. Sliver nanoparticles were then deposited on the titania-carbon composite to achieve titania-carbon nanofibrous material by photoreduction method. ICP-MS analysis showed that the content of deposited silver nanoparticles is as high as (9.5±0.1) wt.%, and TEM observation revealed that the deposited silver nanoparticles are uniform with small sizes (-5nm). The antibacterial activity of the hierarchical nanofibrous titania-carbon composite material deposited with silver nanoparticles was tested against both Gram-positive and Gram-negative bacteria and the material exhibited high inactivation of bacteria due to the synergistic effect of porous carbon nanofibres, anatase titania ultrathin film coating and high loading content of silver nanoparticles with small sizes.
(3) Hierarchical nanotubular titanium nitride material. Titania film was first deposited on natural cellulose substance by sol-gel method and titania replicas of filter paper was obtained after removal of filter paper by calcination in air at600℃for5h.Subsequently, magnesiothermic reduction of the prepared titania replicas of filter paper mentioned above was carried out in a homemade stainless steel autoclave. The titania replicas of filter paper and magnesium granules were separately spread evenly within two different steel boats and placed in the autoclave.The molar ratio of magnesium granules and titania replicas of filter paper was2.5:1. After filled with nitrogen gas, the autoclave was sealed into a vertical tube furnace and heated to1200℃for3h and allowed to cool to room temperature in the flowing N2atmosphere to avoid oxidation. The raw product was then collected and treated with2.0M HC1aqueous solution for6h to selectively dissolve the by-product magnesia. Electron micrographs of the material showed that the hierarchical nanotubular material replicated the hierarchical structure of the original filter paper and the wall of the nanotube was uniform with thickness of ca.46nm. The hierarchical titanium nitride material possessed high specific surface of31.4m2/g. Electrochemical measurements of the hierarchical nanotubular titanium nitride shows that the specific capacitance of the material was74.2F/g at current density of0.16A/g, which can be a used as potential electrode material.
(4) Hierarchical nanotubular titania material deposited with platinum nanoparticles. Titania ultrathin film was first deposited on natural cellulose substance by means of a surface sol-gel method using titanium (Ⅳ) n-butoxide as precursor and titania nanotubular material was obtained after removal of filter paper. Different mass ratio of platinum nanoparticles were subsequently deposited on the nanotubular titania material by photoreduction method. Electron micrograph of the material showed that platinum nanoparticles distributed on the nanotubular titania material uniformly with particle size of2-4nm. Photocatalytic hydrogen production catalyzed by the titania nanotubular material was conducted and results revealed that the highest photocatalytic activity was obtained when the mass ratio of the deposited platinum nanoparticles was1wt.%. Study on the mechanism of the photocatalytic hydrogen production showed that more·OH radicals were produced by deposition of platinum nanoparticles compared with bulk titania.
本文以天然纤维素材料(定量滤纸)作为模板及构筑复合纳米材料的支架,通过表面溶胶-凝胶法在纤维素表面沉积二氧化钛超薄膜,之后通过惰性氛围碳化或是空气中煅烧的方法,制备得到了二氧化钛/碳纳米纤维复合材料或是二氧化钛纳米管材料。这些材料可作为金属纳米颗粒沉积的载体,来制备具有特定功能的复合纳米材料,主要结论如下：
(1)二氧化钛包裹的碳纳米纤维材料。以实验室常用的滤纸为模板,以钛酸四丁酯为前体物,通过表面溶胶-凝胶法,把二氧化钛超薄膜沉积到滤纸纤维素的表面。之后将二氧化钛超薄膜沉积的滤纸复合材料置于管式炉中,氮气氛围中碳化,纤维素转变为无定形碳纤维,同时,二氧化钛凝胶层超薄膜转变为锐钛矿型二氧化钛。SEM及TEM观察发现,该材料在微观上复制了滤纸纤维素材料复杂的多层分级结构及形貌特征,二氧化钛超薄膜(-12nm)均匀的包裹在碳纳米纤维上,且由颗粒尺寸均一的二氧化钛纳米颗粒组成。由于二氧化钛薄膜的包裹,纤维素纤维在碳化的过程中避免了高温烧结与聚集,因此具有较大的比表面积(404m2/g)。光催化实验结果表明,该材料在紫外光及太阳光的照射下,对水体中的染料具有良好的降解效果。我们对光催化降解染料的机理也做了一些研究,结果表明,在光照的作用下,二氧化钛包裹的碳纳米纤维材料会产生·OH自由基及·O2-,从而对染料具有极强的降解效果。光催化循环利用实验表明,经过3次循环之后,样品在180min内,仍然可以降解81%的亚甲基蓝染料。
(2)银纳米颗粒负载的二氧化钛包裹的碳纳米纤维材料。以钛酸四丁酯为前体物,通过表面溶胶-凝胶法在滤纸纤维素表面沉积二氧化钛超薄膜,通过氮气氛围中碳化的方法,将滤纸纤维素转变为碳纳米纤维,得到二氧化钛包裹的碳纳米纤维材料。将该材料浸泡在硝酸银溶液中,通过光照还原的方法,将Ag+转变为银纳米颗粒,得到银纳米颗粒负载的二氧化钛包裹的碳纳米纤维材料。通过SEM和TEM观察可以看到,该材料复制了滤纸纤维素的多层分级结构和形貌特征,二氧化钛超薄膜均匀的包裹在碳纳米纤维上,上面负载的银纳米颗粒分布均匀,颗粒尺寸均一且粒径较小,平均直径仅有5nm。因为多孔碳纳米纤维的存在,银纳米颗粒在二氧化钛包裹的碳纤维材料中的负载量也相对较高,可达9.5wt.%左右。抗菌实验结果表明,该材料对革兰氏阴性菌(大肠杆菌)及革兰氏阳性菌(金黄色葡萄球菌)均具有良好的抗菌效果,抗菌率分别为99.7%和72.1%。
(3)氮化钛纳米管材料。首先以钛酸四丁酯为前体物,通过溶胶-凝胶法,将二氧化钛凝胶层沉积到滤纸纤维素表面,在空气中煅烧除掉滤纸,得到锐钛矿型二氧化钛纳米管材料；然后将二氧化钛纳米管材料和镁粉以2.5：1的比例置于反应釜中,通入氮气,1200℃发生高温镁热还原反应,生成氮化钛纳米管材料。通过SEM和TEM观察可以发现,氮化钛纳米管材料在复制了滤纸纤维素的微观形貌和结构特征,氮化钛纳米管的管壁均匀,平均厚度为46nm。氮气吸附-脱附曲线表明,氮化钛纳米管材料具有相对较大的比表面积,为31.4m2/g。我们对氮化钛纳米管材料的电化学性质做了测试,结果表明,氮化钛纳米管材料具有典型双层超级电容器的特性,当放电电流为0.16A/g时,比电容可达74.2F/g。
(4)铂纳米颗粒负载的二氧化钛纳米管材料。以钛酸四丁酯为前体物,通过表面溶胶-凝胶法,在滤纸纤维素的表面沉积二氧化钛超薄膜,然后在空气中高温煅烧除掉滤纸模板,得到锐钛矿型二氧化钛纳米管材料。将二氧化钛纳米管材料浸渍在不同浓度的水合六氯铂酸溶液中,通过光照还原的方法,产生铂纳米颗粒,得到了铂纳米颗粒负载的二氧化钛纳米管材料。SEM和TEM观察发现,该材料在微观上复制了滤纸纤维素的多层分级结构和形貌特征,铂纳米颗粒分布均匀,大小尺寸在2-4nm之间。光催化产氢实验结果表明,当铂纳米颗粒的负载量为1wt.%左右时,其光催化产氢的活性最高,平均产氢速率为164.4μmol/h。我们对铂纳米颗粒负载的二氧化钛纳米管材料光催化产氢的性能做了循环利用,发现在5次循环利用之后,样品仍具有较高的光催化产氢性能。对其光催化产氢的机理研究表明,在二氧化钛纳米管材料中负载铂纳米颗粒之后,光照产生的·OH自由基显著增多。
The rapid progress in global economy has not only brought us fabulous wealth but also environmental problems.Energy exhaustion and environment pollution has become global problems faced today.Thus,providing abundant, clean, and secure renewable energy sources is one of the key technological challenges facing mankind. Nanomaterial possesses unique physical and chemical properties and an exponential growth of research activities has been seen in nanoscience and nanotechnology in the past decades. As one of the most promising photocatalysts, titania has attracted much attention due to its chemical stability, high phocatalytic activity, nontoxicity and low cost. Amongst various preparation methods, biotemplate synthesis is one of the most attractive production methods for its effectiveness and easy control of nanostructure and morphology. Particularly, natural cellulose substance is an ideal biotemplate due to its unique structures and properties.
Herein, titania thin film was first deposited on natural cellulose substance (filter paper) by the surface sol-gel method using titanium(Ⅳ)n-butoxide as precursor. Subsequently, the titania/filter paper nanocomposite was carbonized in nitrogen or calcined in air to obtain titania coated carbon nanofibrous material or titania nanotubular material.Metal nanoparticles such as Ag or Pt nanoparticles can be deposited on the titania coated carbon nanofibrous material or titania nanotubular material to obtain composite material with tailored properties.
(1)Titania coated carbon nanofibrous material. Ultrathin titania films were firstly deposited by the surface sol-gel process to coat each nanofiber in the filter paper, and successive calcination treatment under nitrogen atmosphere yielded the titania-carbon composite possessing the hierarchical morphologies and structures of the initial paper. The ultrathin titania coating hindered the coalescence effect of the carbon species that formed during the carbonization process of cellulose, and the original cellulose nanofibers were converted into porous carbon nanofibers (diameters from tens to hundreds of nanometers, with3-6nm pores) that coated with uniform anatase titania thin films (thickness-12nm, composed of anatase nanocrystals with sizes of～4.5 nm). This titania-coated nanofibrous carbon material possesses specific surface area of404m2/g, which is two orders of magnitude higher than the titania/cellulose hybrid prepared by atomic layer deposition of titania on the cellulose fibers of filter paper. The photocatalytic activity of the titania-carbon composite was evaluated by the improved photodegradation efficiency of different dyes in aqueous solutions under high-pressure fluorescent mercury lamp irradiation, as well as the effective photoreduction performance of silver cations to silver nanoparticles with ultraviolet irradiation. Experimental results showed that·OH radicals were detected under UV irradiation.
(2) Titania-carbon composite material deposited with silver nanoparticles.Titania ultrathin film was first deposited on natural cellulose substance by means of a surface sol-gel method using titanium (Ⅳ) n-butoxide as precursor. Subsequently, the titania/filter paper composite material was carbonized in nitrogen atmosphere to obtanin titania coated carbon nanofibrous material. Sliver nanoparticles were then deposited on the titania-carbon composite to achieve titania-carbon nanofibrous material by photoreduction method. ICP-MS analysis showed that the content of deposited silver nanoparticles is as high as (9.5±0.1) wt.%, and TEM observation revealed that the deposited silver nanoparticles are uniform with small sizes (-5nm). The antibacterial activity of the hierarchical nanofibrous titania-carbon composite material deposited with silver nanoparticles was tested against both Gram-positive and Gram-negative bacteria and the material exhibited high inactivation of bacteria due to the synergistic effect of porous carbon nanofibres, anatase titania ultrathin film coating and high loading content of silver nanoparticles with small sizes.
(3) Hierarchical nanotubular titanium nitride material. Titania film was first deposited on natural cellulose substance by sol-gel method and titania replicas of filter paper was obtained after removal of filter paper by calcination in air at600℃for5h.Subsequently, magnesiothermic reduction of the prepared titania replicas of filter paper mentioned above was carried out in a homemade stainless steel autoclave. The titania replicas of filter paper and magnesium granules were separately spread evenly within two different steel boats and placed in the autoclave.The molar ratio of magnesium granules and titania replicas of filter paper was2.5:1. After filled with nitrogen gas, the autoclave was sealed into a vertical tube furnace and heated to1200℃for3h and allowed to cool to room temperature in the flowing N2atmosphere to avoid oxidation. The raw product was then collected and treated with2.0M HC1aqueous solution for6h to selectively dissolve the by-product magnesia. Electron micrographs of the material showed that the hierarchical nanotubular material replicated the hierarchical structure of the original filter paper and the wall of the nanotube was uniform with thickness of ca.46nm. The hierarchical titanium nitride material possessed high specific surface of31.4m2/g. Electrochemical measurements of the hierarchical nanotubular titanium nitride shows that the specific capacitance of the material was74.2F/g at current density of0.16A/g, which can be a used as potential electrode material.
(4) Hierarchical nanotubular titania material deposited with platinum nanoparticles. Titania ultrathin film was first deposited on natural cellulose substance by means of a surface sol-gel method using titanium (Ⅳ) n-butoxide as precursor and titania nanotubular material was obtained after removal of filter paper. Different mass ratio of platinum nanoparticles were subsequently deposited on the nanotubular titania material by photoreduction method. Electron micrograph of the material showed that platinum nanoparticles distributed on the nanotubular titania material uniformly with particle size of2-4nm. Photocatalytic hydrogen production catalyzed by the titania nanotubular material was conducted and results revealed that the highest photocatalytic activity was obtained when the mass ratio of the deposited platinum nanoparticles was1wt.%. Study on the mechanism of the photocatalytic hydrogen production showed that more·OH radicals were produced by deposition of platinum nanoparticles compared with bulk titania.
引文
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