胶溶法制备TiO_2纳米晶溶胶及其应用研究
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摘要
TiO_2作为一种半导体光催化材料,具有效率高、能耗低、无毒、稳定性好等优点,在环境污染治理方面应用前景广阔。其中,TiO_2薄膜由于能通过在多种基材上的负载应用,克服粉体型TiO_2易聚集、难回收等问题,受到了广泛关注。近年来,随着TiO_2薄膜在工程塑料,有机涂层等不耐热或大面积难以加热材料表面应用需求的增加,其低温制备成为该领域研究的热点。
本文对TiO_2薄膜的低温制备及应用进行了研究,提出利用以TiO_2纳米晶溶胶为主要成分的有机/无机复合涂膜液,低温负载制备TiO_2薄膜的研究课题。论文以价格低廉的TiOSO_4无机盐为前驱体,采用胶溶法制备TiO_2纳米晶溶胶,并设计TiO_2纳米晶溶胶/醋丙乳液、TiO_2纳米晶溶胶/有机硅溶胶复合体系,解决单一TiO_2纳米晶溶胶涂膜不均匀、薄膜附着力欠佳等应用问题。主要研究工作包括以下几个方面:
(1)TiO_2纳米晶溶胶的制备及优化研究
以价格低廉的TiOSO_4为原料,采用沉淀-胶溶工艺,研究了酸性和中性两类TiO_2纳米晶溶胶的制备方法,重点考察了溶胶制备条件对TiO_2结晶度、粒径大小以及溶胶光催化活性的影响。优化的酸性TiO_2溶胶制备条件为:水浴胶溶温度60℃,水浴胶溶时间6h,HNO_3的添加量H~+:Ti~(4+)=4。优化的中性TiO_2溶胶制备条件为:pH=7～8,水浴温度65℃,水浴时间4h,H_2O_2的添加量为H_2O_2:Ti~(4+)=16。酸性和中性两类TiO_2纳米晶溶胶的对比研究表明,酸性TiO_2溶胶在溶胶稳定性及光催化活性方面均优于中性TiO_2溶胶。
(2)TiO_2/醋丙复合薄膜制备及性能研究
选择醋丙乳液与TiO_2纳米晶溶胶复合,着重考察了复合体系中TiO_2用量对薄膜结构与性能的影响。结果表明:TiO_2纳米晶溶胶/醋丙乳液复合体系具有较高的稳定性和良好的成膜特性;涂膜后,随TiO_2含量的增大,薄膜表面的TiO_2粒子增多,薄膜粗糙度增大;当复合薄膜中添加的TiO_2溶胶浓度由0.1 mol/L提高到0.3mol/L时,紫外光激发下复合薄膜对罗丹明B的分解率由53.8%提高到了78.8%,对水的接触角由66°降低到50°。
(3)TiO_2/有机硅复合薄膜制备及性能研究
采用胶溶法制备以醇为主要溶剂的TiO_2纳米晶溶胶,并与有机硅溶胶进行复合。在此基础上,开展复合溶胶在聚碳酸酯板(PC板)表面的涂膜研究,主要考察了TiO_2溶胶添加量、TiO_2溶胶浓度以及涂膜层数对复合薄膜结构与性能的影响。结果表明:TiO_2溶胶添加量为40wt%时,复合溶胶的成膜性较好;添加的TiO_2溶胶浓度为0.3mol/L时,获得的复合薄膜具有良好的光催化性能,对罗丹明B的降解率达到74.4%;当涂膜层数为2层时,在保证复合薄膜中TiO_2负载量的同时,薄膜均匀、无开裂现象,并且具有较好的光透过率。
TiO_2 is a kind of semiconductor photocatalysts with excellent properties such as high efficiency,low energy consumption,innocuity,good stability,which makes it have important applications in renewable energy and environment fields.TiO_2 thin films is researched widely as it can overcome the shortcomings of TiO_2 powder that is easy to agglomerate and difficult to recycle when being applied on a variety of substrate,.In recent years,with the increasing demand of application in surfaces of materials which do not resist heat or the surface area is too large to heat,such as engineering plastics,organic coatings and so on,It is becoming hot to prepare TiO_2 thin film at low temperature.
In this paper we researched the low temperature preparation and application of TiO_2 thin film,put forward the research programe of preparing TiO_2 thin film by nano-crystal TiO_2 sol,prepared TiO_2 sol with anatase using low-cost inorganic salts TiOSO_4 as precursors by colloidal chemical method,designed the composite system of nano-crystal TiO_2 sol/vinyl acetate-acrylate latex,nano-crystal TiO_2 sol/organosilicon sol,so as to solve practical application problem such as ununiformity and poor adhesion of film prepared by pure nano-crystal TiO_2 sol.Specific major tasks include the following aspects:
(1) Study on preparation and optimization of TiO_2 nanocrystalline sol
Using low-cost TiOSO_4 as precursors,preparation of acid and neutral TiO_2 sol were studied by peptizing method The impact of preparing conditions on crystallinity degree, particle size.photocatalytic efficiency of TiO_2 sol were emphatically investigated. Optimized preparing conditions of acid TiO_2 sol are as follows:peptizing temperature and time were 60℃and 6h separately,adding amount of HNO_3 was H~+:Ti~(4+)=4.Optimized preparation conditions of neutral TiO_2 sol are as follows:peptizing temperature and time were 65℃and 4h separately,adding amount of H_2O_2 was H~+:Ti~(4+)=16 By comparing acid and neutral TiO_2 sol,it is known that the stability and photocatalytic activity of acidic TiO_2 sol are better than that of neutral TiO_2 sol.
(2) Study on preparation and properties of vinyl acetate-acrylate/TiO_2 composite film The acid TiO_2 nanocrystalline sol was added into vinyl acetate-acrylate latex.The impact of TiO_2 content in the compound system on the structure and properties of the film were emphatically investigated.The results show that the composite coating solution has high stability and excellent film forming property.With the increase of TiO_2 sol addition,the amount of TiO_2 particles in the surface of the film increases,which leads to the increase of roughness of the film.When the concentration of the TiO_2 sol increases from 0.1 mol/L to 0.3mol/L,decomposition rate of the composite film to rhodamine B increases from 53.8%to 78.8%and the contact angle decreased from 66°to50°after the UV irradiation.
(3) Study on preparation and properties of organosilicon/TiO_2 composite film
Ethanol based acid TiO_2 nanocrystalline sol was prepared by colloidal chemical method and then added in organosilicon sol.On this basis,research on preparing films on the surface of polycarbonate sheet(PC sheet) by composite coating solution were carried out.The adding amount of TiO_2 sol,concentration of TiO_2 sol and coating layers of the composite fihn were mainly studied.The results show that when the adding amount of TiO_2 sol is 40wt%,fihn forming property of the composite coating solution is well.When the concentration of the TiO_2 sol is 0.3mol/L,photocatalytic performance of the composite film is the best,and decomposition rate of the composite film to rhodamine B was 74.4%.When the coating layer was two,it guarantees much TiO_2 particles on the PC sheet,and the film is uniformity,less crack and has sufficient light transmittance.
本文对TiO_2薄膜的低温制备及应用进行了研究,提出利用以TiO_2纳米晶溶胶为主要成分的有机/无机复合涂膜液,低温负载制备TiO_2薄膜的研究课题。论文以价格低廉的TiOSO_4无机盐为前驱体,采用胶溶法制备TiO_2纳米晶溶胶,并设计TiO_2纳米晶溶胶/醋丙乳液、TiO_2纳米晶溶胶/有机硅溶胶复合体系,解决单一TiO_2纳米晶溶胶涂膜不均匀、薄膜附着力欠佳等应用问题。主要研究工作包括以下几个方面:
(1)TiO_2纳米晶溶胶的制备及优化研究
以价格低廉的TiOSO_4为原料,采用沉淀-胶溶工艺,研究了酸性和中性两类TiO_2纳米晶溶胶的制备方法,重点考察了溶胶制备条件对TiO_2结晶度、粒径大小以及溶胶光催化活性的影响。优化的酸性TiO_2溶胶制备条件为:水浴胶溶温度60℃,水浴胶溶时间6h,HNO_3的添加量H~+:Ti~(4+)=4。优化的中性TiO_2溶胶制备条件为:pH=7～8,水浴温度65℃,水浴时间4h,H_2O_2的添加量为H_2O_2:Ti~(4+)=16。酸性和中性两类TiO_2纳米晶溶胶的对比研究表明,酸性TiO_2溶胶在溶胶稳定性及光催化活性方面均优于中性TiO_2溶胶。
(2)TiO_2/醋丙复合薄膜制备及性能研究
选择醋丙乳液与TiO_2纳米晶溶胶复合,着重考察了复合体系中TiO_2用量对薄膜结构与性能的影响。结果表明:TiO_2纳米晶溶胶/醋丙乳液复合体系具有较高的稳定性和良好的成膜特性;涂膜后,随TiO_2含量的增大,薄膜表面的TiO_2粒子增多,薄膜粗糙度增大;当复合薄膜中添加的TiO_2溶胶浓度由0.1 mol/L提高到0.3mol/L时,紫外光激发下复合薄膜对罗丹明B的分解率由53.8%提高到了78.8%,对水的接触角由66°降低到50°。
(3)TiO_2/有机硅复合薄膜制备及性能研究
采用胶溶法制备以醇为主要溶剂的TiO_2纳米晶溶胶,并与有机硅溶胶进行复合。在此基础上,开展复合溶胶在聚碳酸酯板(PC板)表面的涂膜研究,主要考察了TiO_2溶胶添加量、TiO_2溶胶浓度以及涂膜层数对复合薄膜结构与性能的影响。结果表明:TiO_2溶胶添加量为40wt%时,复合溶胶的成膜性较好;添加的TiO_2溶胶浓度为0.3mol/L时,获得的复合薄膜具有良好的光催化性能,对罗丹明B的降解率达到74.4%;当涂膜层数为2层时,在保证复合薄膜中TiO_2负载量的同时,薄膜均匀、无开裂现象,并且具有较好的光透过率。
TiO_2 is a kind of semiconductor photocatalysts with excellent properties such as high efficiency,low energy consumption,innocuity,good stability,which makes it have important applications in renewable energy and environment fields.TiO_2 thin films is researched widely as it can overcome the shortcomings of TiO_2 powder that is easy to agglomerate and difficult to recycle when being applied on a variety of substrate,.In recent years,with the increasing demand of application in surfaces of materials which do not resist heat or the surface area is too large to heat,such as engineering plastics,organic coatings and so on,It is becoming hot to prepare TiO_2 thin film at low temperature.
In this paper we researched the low temperature preparation and application of TiO_2 thin film,put forward the research programe of preparing TiO_2 thin film by nano-crystal TiO_2 sol,prepared TiO_2 sol with anatase using low-cost inorganic salts TiOSO_4 as precursors by colloidal chemical method,designed the composite system of nano-crystal TiO_2 sol/vinyl acetate-acrylate latex,nano-crystal TiO_2 sol/organosilicon sol,so as to solve practical application problem such as ununiformity and poor adhesion of film prepared by pure nano-crystal TiO_2 sol.Specific major tasks include the following aspects:
(1) Study on preparation and optimization of TiO_2 nanocrystalline sol
Using low-cost TiOSO_4 as precursors,preparation of acid and neutral TiO_2 sol were studied by peptizing method The impact of preparing conditions on crystallinity degree, particle size.photocatalytic efficiency of TiO_2 sol were emphatically investigated. Optimized preparing conditions of acid TiO_2 sol are as follows:peptizing temperature and time were 60℃and 6h separately,adding amount of HNO_3 was H~+:Ti~(4+)=4.Optimized preparation conditions of neutral TiO_2 sol are as follows:peptizing temperature and time were 65℃and 4h separately,adding amount of H_2O_2 was H~+:Ti~(4+)=16 By comparing acid and neutral TiO_2 sol,it is known that the stability and photocatalytic activity of acidic TiO_2 sol are better than that of neutral TiO_2 sol.
(2) Study on preparation and properties of vinyl acetate-acrylate/TiO_2 composite film The acid TiO_2 nanocrystalline sol was added into vinyl acetate-acrylate latex.The impact of TiO_2 content in the compound system on the structure and properties of the film were emphatically investigated.The results show that the composite coating solution has high stability and excellent film forming property.With the increase of TiO_2 sol addition,the amount of TiO_2 particles in the surface of the film increases,which leads to the increase of roughness of the film.When the concentration of the TiO_2 sol increases from 0.1 mol/L to 0.3mol/L,decomposition rate of the composite film to rhodamine B increases from 53.8%to 78.8%and the contact angle decreased from 66°to50°after the UV irradiation.
(3) Study on preparation and properties of organosilicon/TiO_2 composite film
Ethanol based acid TiO_2 nanocrystalline sol was prepared by colloidal chemical method and then added in organosilicon sol.On this basis,research on preparing films on the surface of polycarbonate sheet(PC sheet) by composite coating solution were carried out.The adding amount of TiO_2 sol,concentration of TiO_2 sol and coating layers of the composite fihn were mainly studied.The results show that when the adding amount of TiO_2 sol is 40wt%,fihn forming property of the composite coating solution is well.When the concentration of the TiO_2 sol is 0.3mol/L,photocatalytic performance of the composite film is the best,and decomposition rate of the composite film to rhodamine B was 74.4%.When the coating layer was two,it guarantees much TiO_2 particles on the PC sheet,and the film is uniformity,less crack and has sufficient light transmittance.
引文
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