有机酸解胶法制备的锐钛矿相TiO_2超细晶粒的自组装薄膜及其光电化学性能
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摘要
纳米二氧化钛溶胶由于具备了粉体与薄膜等固态材料不可比拟的亲和性及相容性,而成为了一种具有广阔应用前景的无机纳米材料。对于溶胶来说,稳定性和分散性是评价其性能好坏的重要指标,同时还会影响其在实际中的应用效果,因此,如何获得稳定高分散的溶胶仍是二氧化钛溶胶制备及应用过程中的核心问题。本论文采用沉淀-解胶法结合水热处理合成了锐钛矿相二氧化钛溶胶,同时,通过“自下而上”的方法,将二氧化钛溶胶作为基元,自组装制备了纳米二氧化钛薄膜,并对其在化学需氧量(chemical oxygen demand,COD)的检测以及染料敏化太阳能电池(Dye-sensitized solar cells,DSSCs)等方面的应用进行了研究。
以湿化学法得到的水合二氧化钛为原料,采用三氟乙酸作为解胶剂,通过沉淀-解胶法制备了锐钛矿相的二氧化钛纳米溶胶,结合水热处理进一步调控了溶胶中二氧化钛晶粒的尺寸。所获得的二氧化钛溶胶表现出了优异的分散性和稳定性。将干燥后的溶胶经煅烧处理获得二氧化钛粉体,通过苯酚的光催化降解实验研究了粉体的光催化活性,其中从溶胶Ti/8TFA-2中所获得的二氧化钛粉体表现出了优于商业纳米二氧化钛的光催化效果。
将导电玻璃分别交替浸泡在胶核带正电的TiO2溶胶和阴离子聚电解质聚苯乙烯磺酸钠(poly(styrene sulfonic acid) sodium salt,PSS)中,通过层层自组装技术制备了不同层数的TiO2/PSS薄膜,经500℃煅烧后,获得了致密的纳米TiO2薄膜,并在三电极体系的电化学池中研究了薄膜的光电催化性能。其中,层数为15层的薄膜电极表现出了最佳的光电催化活性。将其作为传感器用于COD的检测,最终获得的COD检测范围为0-130mg·L-1,最低检测限为1.0mg·L-1。由此可见,将层层自组装纳米TiO2薄膜电极用于COD的检测切实可行。
利用二氧化钛溶胶晶粒的高烧结活性,先将干燥后的溶胶进行低温煅烧(300℃,1h),煅烧后二氧化钛的比表面积从224.7m2/g降低到了94.9m2/g,适用于DSSC光阳极的制备,结合层层自组装法制备的阻挡层(预处理),通过丝网印刷法最终获得具有一定光学梯度的DSSC光阳极。经预处理后,DSSC的性能明显提高。为了进一步提高其光电性能,又将经预处理的DSSC光阳极进行了后处理,通过溶胶的内渗透改性后,DSSC的光电转换效率最终效率达到了7.87%。同时与传统的TiCl4处理的改性工艺相比,利用溶胶对光阳极进行预处理及后处理表现出了更好的改性效果。因此,对于DSSC来说,溶胶改性光阳极的方法可以有效代替传统的TiCl4处理工艺而被广泛应用。
由于柔性透明聚合物基底不能耐受高温,传统的制膜方法不再适用于在柔性基底上制备光阳极,为了解决这个问题,引入了全新的全纳米颗粒自组装的概念,利用层层自组装技术,以高结晶度的纳米二氧化钛溶胶与商业二氧化钛P25为原料,在柔性基底上制备了一系列全纳米二氧化钛颗粒自组装薄膜。为了进一步研究纳米二氧化钛薄膜的光电性能,将其分别用于水体中有机物的检测以及染料敏化太阳能电池光阳极的制备。全纳米二氧化钛颗粒自组装薄膜表现出了较高的光电催化活性,可有效检测出水体中有机物的含量。而以其作为光阳极所组装电池的性能还较低,实验中柔性DSSC的最高光电转换效率为1.09%。但这一定程度上证明了该方法可用于柔性DSSC光阳极的制备,并为在柔性透明导电基底上制备无机半导体薄膜提供了一个新的研究方向。
TiO2sols have been seen as one of the most useful inorganic materials since they can be more conveniently used than the solid TiO2nano-materials, such as TiO2nanoparticles and TiO2thin films. The stability and dispersity are always used to estimate the characteristics of the sols, which will affect their prosperities in the application. Therefore, the researches about TiO2sols still focus on the preparation of the highly dispersed TiO2sols. In this study, the anatase TiO2sols were synthesized by a peptization-hydrothermal process. Moreover, the TiO2thin films were prepared by self assembly technique through the "bottom-up" method. The applications of TiO2thin films in the fields about the determination of chemical oxygen demand (COD) and the fabrication of dye-sensitized solar cells (DSSCs) were systematically investigated as well.
Anatase TiO2sols with high dispersity and stability were prepared by the peptization of amorphous precipitates in trifluoroactic acid (TFA) solution. The crystallite size of TiO2in the sols was tuned by the subsequently hydrothermal treatment. In order to investigate the photocataltic activities of the TiO2in sol and remove affection of the organics on the surface of the TiO2in photocatalysis. The dried TiO2sols were calcined at500℃for2h, and the degradation of phenol proved that the photocatalytic activities of the obtained TiO2nanoparticles. The nanoparticles obtained from the sample Ti/8TFA-2had shown a better photocatalytic activity than that of the commercial TiO2nanoparticles.
The positive charged nanoparticles in the sol Ti/8TFA-2and the poly(styrene sulfonic acid) sodium salt (PSS) solution were used to prepare TiO2/PSS thin films by a layer-by-layer (LBL) self-assembly technique, and the compact TiO2thin films were obtained after calcination at500℃.The TiO2LBL thin films were introduced to be working electrodes in three-electrode photoelectrochemical cells. The15-layer TiO2thin film electrode showed the highest photoelectrochemical property and it was employed as a sensor for the chemical oxygen demand. The detection limit of1.0mg-L"1with a working range of0-130mg-L"1was achieved. The results demonstrated the practicability of the photoelectrocatalysis for COD determination through the LBL TiO2thin film electrodes.
Since the TiO2nanocrystals in the sol were easy to sinter, the dried sol was calcined at300℃for1h to eliminate the organics over the surface of TiO2and increase the crystallite size of the TiO2nanocrystals (the special surface area of the calcined TiO2decreased from224.7m2/g to94.9m2/g) to prepare the paste for the porous layer of DSSCs. The compact layer was prepared by the diluted sol through the layer-by-layer self assembly technique to control its thickness. Compared with the DSSCs without the compact layer, the cells with the LBL compact layers showed improved photovoltaic properties. In order to further enhance the photovoltatic properties of the DSSCs, the photoanodes with compact films were also modified by the TiO2sol through the post treatment, and finally the photoelectron conversion efficiency of the modified DSSC had increased to7.87%. The treatment with the TiO2sol was a better way for the modification of DSSC photoanodes than the traditional treatment through a TiCl4solution, which also showed the great potential in the application of the preparation and modification for the DSSC photoanodes.
The flexible transparent conductive oxide (TCO) substrates are always with a low thermal stability at high temperature, and the thin films can not prepared on them through the traditional methods.The all-nanoparticle self-assembly technique was used in this study to solve this problem. The all-nanoparticle TiO2thin film was prepared by the crystallized TiO2nanoparticles in sol and the commercial TiO2(P25) through the layer-by-layer self assembly method. The TiO2films were applied in water quality assessment and the fabrication of DSSC photoanodes. They had showed the high photocatalytic properties in water quality assessment, but the photoelectron conversion efficiencies of DSSCs with the all-nanoparticle TiO2thin film photoanodes were low. The highest photoelectron conversion efficiency of flexible DSSC with the all-nanoparticle TiO2thin film photoanode just arrived to1.09%. Moreover, the results demonstrated the practicability of the all-nanoparticle assembly technique in DSSC and presented a brand new way to fabricate the TiO2films on flexible TCO substrates.
以湿化学法得到的水合二氧化钛为原料,采用三氟乙酸作为解胶剂,通过沉淀-解胶法制备了锐钛矿相的二氧化钛纳米溶胶,结合水热处理进一步调控了溶胶中二氧化钛晶粒的尺寸。所获得的二氧化钛溶胶表现出了优异的分散性和稳定性。将干燥后的溶胶经煅烧处理获得二氧化钛粉体,通过苯酚的光催化降解实验研究了粉体的光催化活性,其中从溶胶Ti/8TFA-2中所获得的二氧化钛粉体表现出了优于商业纳米二氧化钛的光催化效果。
将导电玻璃分别交替浸泡在胶核带正电的TiO2溶胶和阴离子聚电解质聚苯乙烯磺酸钠(poly(styrene sulfonic acid) sodium salt,PSS)中,通过层层自组装技术制备了不同层数的TiO2/PSS薄膜,经500℃煅烧后,获得了致密的纳米TiO2薄膜,并在三电极体系的电化学池中研究了薄膜的光电催化性能。其中,层数为15层的薄膜电极表现出了最佳的光电催化活性。将其作为传感器用于COD的检测,最终获得的COD检测范围为0-130mg·L-1,最低检测限为1.0mg·L-1。由此可见,将层层自组装纳米TiO2薄膜电极用于COD的检测切实可行。
利用二氧化钛溶胶晶粒的高烧结活性,先将干燥后的溶胶进行低温煅烧(300℃,1h),煅烧后二氧化钛的比表面积从224.7m2/g降低到了94.9m2/g,适用于DSSC光阳极的制备,结合层层自组装法制备的阻挡层(预处理),通过丝网印刷法最终获得具有一定光学梯度的DSSC光阳极。经预处理后,DSSC的性能明显提高。为了进一步提高其光电性能,又将经预处理的DSSC光阳极进行了后处理,通过溶胶的内渗透改性后,DSSC的光电转换效率最终效率达到了7.87%。同时与传统的TiCl4处理的改性工艺相比,利用溶胶对光阳极进行预处理及后处理表现出了更好的改性效果。因此,对于DSSC来说,溶胶改性光阳极的方法可以有效代替传统的TiCl4处理工艺而被广泛应用。
由于柔性透明聚合物基底不能耐受高温,传统的制膜方法不再适用于在柔性基底上制备光阳极,为了解决这个问题,引入了全新的全纳米颗粒自组装的概念,利用层层自组装技术,以高结晶度的纳米二氧化钛溶胶与商业二氧化钛P25为原料,在柔性基底上制备了一系列全纳米二氧化钛颗粒自组装薄膜。为了进一步研究纳米二氧化钛薄膜的光电性能,将其分别用于水体中有机物的检测以及染料敏化太阳能电池光阳极的制备。全纳米二氧化钛颗粒自组装薄膜表现出了较高的光电催化活性,可有效检测出水体中有机物的含量。而以其作为光阳极所组装电池的性能还较低,实验中柔性DSSC的最高光电转换效率为1.09%。但这一定程度上证明了该方法可用于柔性DSSC光阳极的制备,并为在柔性透明导电基底上制备无机半导体薄膜提供了一个新的研究方向。
TiO2sols have been seen as one of the most useful inorganic materials since they can be more conveniently used than the solid TiO2nano-materials, such as TiO2nanoparticles and TiO2thin films. The stability and dispersity are always used to estimate the characteristics of the sols, which will affect their prosperities in the application. Therefore, the researches about TiO2sols still focus on the preparation of the highly dispersed TiO2sols. In this study, the anatase TiO2sols were synthesized by a peptization-hydrothermal process. Moreover, the TiO2thin films were prepared by self assembly technique through the "bottom-up" method. The applications of TiO2thin films in the fields about the determination of chemical oxygen demand (COD) and the fabrication of dye-sensitized solar cells (DSSCs) were systematically investigated as well.
Anatase TiO2sols with high dispersity and stability were prepared by the peptization of amorphous precipitates in trifluoroactic acid (TFA) solution. The crystallite size of TiO2in the sols was tuned by the subsequently hydrothermal treatment. In order to investigate the photocataltic activities of the TiO2in sol and remove affection of the organics on the surface of the TiO2in photocatalysis. The dried TiO2sols were calcined at500℃for2h, and the degradation of phenol proved that the photocatalytic activities of the obtained TiO2nanoparticles. The nanoparticles obtained from the sample Ti/8TFA-2had shown a better photocatalytic activity than that of the commercial TiO2nanoparticles.
The positive charged nanoparticles in the sol Ti/8TFA-2and the poly(styrene sulfonic acid) sodium salt (PSS) solution were used to prepare TiO2/PSS thin films by a layer-by-layer (LBL) self-assembly technique, and the compact TiO2thin films were obtained after calcination at500℃.The TiO2LBL thin films were introduced to be working electrodes in three-electrode photoelectrochemical cells. The15-layer TiO2thin film electrode showed the highest photoelectrochemical property and it was employed as a sensor for the chemical oxygen demand. The detection limit of1.0mg-L"1with a working range of0-130mg-L"1was achieved. The results demonstrated the practicability of the photoelectrocatalysis for COD determination through the LBL TiO2thin film electrodes.
Since the TiO2nanocrystals in the sol were easy to sinter, the dried sol was calcined at300℃for1h to eliminate the organics over the surface of TiO2and increase the crystallite size of the TiO2nanocrystals (the special surface area of the calcined TiO2decreased from224.7m2/g to94.9m2/g) to prepare the paste for the porous layer of DSSCs. The compact layer was prepared by the diluted sol through the layer-by-layer self assembly technique to control its thickness. Compared with the DSSCs without the compact layer, the cells with the LBL compact layers showed improved photovoltaic properties. In order to further enhance the photovoltatic properties of the DSSCs, the photoanodes with compact films were also modified by the TiO2sol through the post treatment, and finally the photoelectron conversion efficiency of the modified DSSC had increased to7.87%. The treatment with the TiO2sol was a better way for the modification of DSSC photoanodes than the traditional treatment through a TiCl4solution, which also showed the great potential in the application of the preparation and modification for the DSSC photoanodes.
The flexible transparent conductive oxide (TCO) substrates are always with a low thermal stability at high temperature, and the thin films can not prepared on them through the traditional methods.The all-nanoparticle self-assembly technique was used in this study to solve this problem. The all-nanoparticle TiO2thin film was prepared by the crystallized TiO2nanoparticles in sol and the commercial TiO2(P25) through the layer-by-layer self assembly method. The TiO2films were applied in water quality assessment and the fabrication of DSSC photoanodes. They had showed the high photocatalytic properties in water quality assessment, but the photoelectron conversion efficiencies of DSSCs with the all-nanoparticle TiO2thin film photoanodes were low. The highest photoelectron conversion efficiency of flexible DSSC with the all-nanoparticle TiO2thin film photoanode just arrived to1.09%. Moreover, the results demonstrated the practicability of the all-nanoparticle assembly technique in DSSC and presented a brand new way to fabricate the TiO2films on flexible TCO substrates.
引文
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