纳米结构ZnO在TiO_2薄膜上的电化学沉积及其光电性能
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摘要
本文采用电化学沉积技术以ITO/TiO2纳米薄膜为基底,以硝酸锌水溶液为电解液,实现了纳米结构ZnO在TiO2纳米薄膜上的生长,并通过XRD、SEM、EDS、Raman和PL光谱等方法对样品进行测试和表征。重点研究了电解液浓度、沉积时间、六次甲基四胺(HMT)的引入以及TiO2基底薄膜的微观结构等对纳米结构ZnO的生长及其光学性质的影响,并结合循环伏安等电化学测试探讨了过程机制。
采用溶胶-水热法合成TiO2膏体,通过浸渍提拉-旋涂过程制备了ITO/TiO2纳米薄膜,其具有规则均一的微观结构,粒径约为10 nm。以所合成的ITO/TiO2纳米薄膜为基底,采用0.03 mol/L的硝酸锌溶液为电解液和锌源,在-0.75 V的恒电压下,沉积得到纳米结构ZnO薄膜。ZnO具有六方相的晶体结构,并且沿着(002)晶面(c-轴)方向表现出明显的择优化生长,以至于形成了垂直于基底的ZnO纳米棒阵列。没有经过热处理,ZnO的结晶度依然很高。通过改变沉积时间、电解液浓度、TiO2基底薄膜的微观结构和引入功能分子等条件,可以方便地调控ZnO薄膜的结晶度以及表面形貌。结果表明,延长沉积时间、增加电解液浓度和引入一定量的HMT等均对ZnO薄膜的生长有促进作用,使得纳米棒的结晶度和取向更好,这与电化学沉积过程中沉淀剂OHˉ浓度的增加有关。与ITO玻璃基底相比,ZnO更易于在纳米结构TiO2薄膜上实现电化学沉积,并且基底薄膜的微观结构对ZnO生长有着较大的影响。
在325 nm波长光的激发下,所获得的ITO/TiO2/ZnO薄膜分别约在375 nm和520 nm处表现出窄的紫外光发射峰和宽的绿光发射带,这主要是ZnO发光所导致的。紫外光发射是近带边激子的辐射复合产生的,而绿光发射则通常被认为与ZnO薄膜的内部本征缺陷有关。通过调控ZnO的结晶度及其阵列的微观结构,可以改变复合薄膜的发光性能。
In this paper, well-aligned ZnO nanorod arrays have been successfully fabricated directly on anatase TiO2 nanoparticle films through a simple electrochemical deposition (ECD) method in the zinc nitrate solution. The samples were characterized by the methods of XRD, SEM, EDS, Raman and PL. The effects of the reactant concentration, deposition time, HMT additive and the microstructure of TiO2 film on the growth and the optical capability of the nanostructured ZnO obtained were studied in detail. The mechanism of ECD process was investigated by electrochemical methods such as cyclic voltammogram.
Nanosized anatase TiO2 film on the ITO glass has been fabricated via spin coat process, with TiO2 nanoparticles, which were synthesized by a sol–hydrothermal method. It had uniform structure, composed of spherical nanoparticles with 10 nm in diameter. With ITO/TiO2 film as substrate, 0.03 mol/L Zn(NO3)2 solution acted as electrolyte and Zn sources, we could obtain nanostructured ZnO film when deposition potential was -0.75 V. ZnO crystal prepared by electrodeposition was hexagonal phase and grew along [002] direction (c-axis) with obvious preferential orientation, so as to form ZnO nanorod arrays vertically on the substrate. Although ZnO crystals were not passed through thermal treatment, its crystallinity was still quite high.
Through altering deposition time, reactant concentration, microstructure of TiO2 film and adding functional molecule, we could regulate the crystallinity and surface morphology of ZnO film conveniently. The results showed that prolonging the deposition time, increasing the reactant concentration and adding a certain amount of HMT could promote the growth of ZnO film and increase crystallinity and orientation of nanorods, which is close related to the increase of depositon reagent OHˉconcentration in the ECD process. Compared with ITO glass substrate, ZnO could be more easily deposited on the TiO2 film, and the microstructure of film substrate had a great effect on the growth of ZnO.
Under the excitation wavelength of 325 nm, the as-prepared compound semiconductor film exhibited a strong and narrow near-ultraviolet PL peak located at about 375 nm and a weak and broad green emission band centered at 520 nm around, mainly assigned to the photoluminescence of ZnO. Ultraviolet emission peak is attributed to the exciton-related emission near the band-edge and green emission band is attributed to the intrinsic defects of ZnO generally. Through adjusting and controlling the crystallinity of ZnO and the microstructure of ZnO nanorods array, the photoluminescence performance of the composite film could be changed.
采用溶胶-水热法合成TiO2膏体,通过浸渍提拉-旋涂过程制备了ITO/TiO2纳米薄膜,其具有规则均一的微观结构,粒径约为10 nm。以所合成的ITO/TiO2纳米薄膜为基底,采用0.03 mol/L的硝酸锌溶液为电解液和锌源,在-0.75 V的恒电压下,沉积得到纳米结构ZnO薄膜。ZnO具有六方相的晶体结构,并且沿着(002)晶面(c-轴)方向表现出明显的择优化生长,以至于形成了垂直于基底的ZnO纳米棒阵列。没有经过热处理,ZnO的结晶度依然很高。通过改变沉积时间、电解液浓度、TiO2基底薄膜的微观结构和引入功能分子等条件,可以方便地调控ZnO薄膜的结晶度以及表面形貌。结果表明,延长沉积时间、增加电解液浓度和引入一定量的HMT等均对ZnO薄膜的生长有促进作用,使得纳米棒的结晶度和取向更好,这与电化学沉积过程中沉淀剂OHˉ浓度的增加有关。与ITO玻璃基底相比,ZnO更易于在纳米结构TiO2薄膜上实现电化学沉积,并且基底薄膜的微观结构对ZnO生长有着较大的影响。
在325 nm波长光的激发下,所获得的ITO/TiO2/ZnO薄膜分别约在375 nm和520 nm处表现出窄的紫外光发射峰和宽的绿光发射带,这主要是ZnO发光所导致的。紫外光发射是近带边激子的辐射复合产生的,而绿光发射则通常被认为与ZnO薄膜的内部本征缺陷有关。通过调控ZnO的结晶度及其阵列的微观结构,可以改变复合薄膜的发光性能。
In this paper, well-aligned ZnO nanorod arrays have been successfully fabricated directly on anatase TiO2 nanoparticle films through a simple electrochemical deposition (ECD) method in the zinc nitrate solution. The samples were characterized by the methods of XRD, SEM, EDS, Raman and PL. The effects of the reactant concentration, deposition time, HMT additive and the microstructure of TiO2 film on the growth and the optical capability of the nanostructured ZnO obtained were studied in detail. The mechanism of ECD process was investigated by electrochemical methods such as cyclic voltammogram.
Nanosized anatase TiO2 film on the ITO glass has been fabricated via spin coat process, with TiO2 nanoparticles, which were synthesized by a sol–hydrothermal method. It had uniform structure, composed of spherical nanoparticles with 10 nm in diameter. With ITO/TiO2 film as substrate, 0.03 mol/L Zn(NO3)2 solution acted as electrolyte and Zn sources, we could obtain nanostructured ZnO film when deposition potential was -0.75 V. ZnO crystal prepared by electrodeposition was hexagonal phase and grew along [002] direction (c-axis) with obvious preferential orientation, so as to form ZnO nanorod arrays vertically on the substrate. Although ZnO crystals were not passed through thermal treatment, its crystallinity was still quite high.
Through altering deposition time, reactant concentration, microstructure of TiO2 film and adding functional molecule, we could regulate the crystallinity and surface morphology of ZnO film conveniently. The results showed that prolonging the deposition time, increasing the reactant concentration and adding a certain amount of HMT could promote the growth of ZnO film and increase crystallinity and orientation of nanorods, which is close related to the increase of depositon reagent OHˉconcentration in the ECD process. Compared with ITO glass substrate, ZnO could be more easily deposited on the TiO2 film, and the microstructure of film substrate had a great effect on the growth of ZnO.
Under the excitation wavelength of 325 nm, the as-prepared compound semiconductor film exhibited a strong and narrow near-ultraviolet PL peak located at about 375 nm and a weak and broad green emission band centered at 520 nm around, mainly assigned to the photoluminescence of ZnO. Ultraviolet emission peak is attributed to the exciton-related emission near the band-edge and green emission band is attributed to the intrinsic defects of ZnO generally. Through adjusting and controlling the crystallinity of ZnO and the microstructure of ZnO nanorods array, the photoluminescence performance of the composite film could be changed.
引文
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