改性TiO_2纳米管阵列的制备及光电性能研究
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摘要
阳极氧化法制备的TiO_2纳米管阵列因其具有高度整齐的一维排列结构、高的电子传输速率和电子寿命，在染料敏化太阳能电池中展现出诱人的应用前景。但又因结构易坍塌和染料吸附量低等问题，难以充分发挥一维TiO_2纳米管阵列的结构优势。本文针对阳极氧化法合成TiO_2纳米管阵列的制备条件选择和改善太阳能电池光电转化性能等问题进行了研究。选择不同的电解液体系，研究TiO_2纳米管阵列的结构及其影响因素；采用表面处理、ZnO及Sm_2O_3改性，使制得的TiO_2纳米管阵列获得了较高的光电转化效率。
在H_3PO_4/NH_4F无机电解液体系中采用阳极氧化法制得了TiO_2纳米管阵列，通过FESEM系统地考察了搅拌速率、煅烧温度、H_3PO_4添加量、F-浓度、氧化电压、氧化时间对纳米管阵列表面形貌、管径及管长的影响。结果发现，搅拌速率、H_3PO_4与F-浓度、氧化电压对形貌和孔径有较大的影响，氧化反应时间对管长的影响较为显著。根据单因素影响条件，选择其中影响较为显著的三个因素，采用Box-Behnken Design方法设计实验，通过软件模拟得到排列紧密的TiO_2纳米管阵列的最佳制备条件为：氧化时间为240min，氧化电压为15.39V，NH_4F的浓度为0.5mol/L，经由软件模拟得到TiO_2纳米管阵列管内径为33nm，管长为1.43μm。通过XRD和UV-vis表征手段分析了不同煅烧温度和煅烧时间对TiO_2纳米管阵列晶体结构和光电性质的影响，得到最佳的煅烧条件为500℃煅烧2h。并通过实时的电流监控探讨TiO_2纳米管阵列的生长机理。
以乙二醇有机体系为电解液，采用阳极氧化法制得了TiO_2纳米管阵列，分析了F-浓度、水添加量、氧化电压及反应温度对TiO_2纳米管阵列形貌、管径及管长的影响，发现水添加量是能否形成TiO_2纳米管阵列的关键因素，在40V的氧化电压，0.3wt%的NH_4F浓度，2vol%的水添加量及25℃的反应温度下得到的TiO_2纳米管阵列的管径光滑，且高度有序的排列。同时以乙二醇制备的TiO_2纳米管阵列为染料敏化太阳能电池的光阳极，采用四异丙氧基钛(TnB)和氧电浆联合处理其表面，结果表明：TiO_2纳米管阵列结构仍然存在，在纳米管阵列表面及侧壁出现了TiO_2纳米粒子，提高了表面粗糙度和亲水性，增加了染料的吸附量，相对于纯TiO_2纳米管阵列，染料敏化太阳能电池的光电转化效率从1.89%提高至3.68%。
采用阴极电沉积方法制备了异质结型ZnO/TiO_2纳米管阵列。研究了ZnO/TiO_2复合电极的表面形貌、晶形及光吸收性能，结果表明：阴极电沉积法制备的ZnO/TiO_2复合电极表面出现致密的ZnO粒子，表面粗糙度提高、禁带宽度变小、染料吸附量大、电子寿命长。以ZnO/TiO_2纳米管阵列为光阳极组装的染料敏化太阳能电池，相对于纯TiO_2纳米管阵列，60min电沉积的ZnO/TiO_2复合光阳极的光电转化效率可从1.71%提高至3.76%。
采用水热法制备了Sm_2O_3改性TiO_2纳米管阵列，研究了Sm_2O_3/TiO_2纳米管阵列表面形貌、晶形、光吸收和荧光发光性能，发现Sm_2O_3改性后TiO_2纳米管阵列的晶粒尺寸变小，禁带宽度变低；可一定程度地吸收紫外光，并通过荧光性质以可见光发射。将Sm_2O_3/TiO_2复合电极作为染料敏化太阳能电池的光阳极，发现通过Sm3+的下转换荧光性质，可提高太阳能电池中的短路电流。相对于纯TiO_2纳米管阵列，0.02mol/L Sm_2O_3/TiO_2复合光阳极的光电转化效率从1.86%提高至3.22%。这些改性研究为进一步探讨TiO_2纳米管阵列对染料敏化太阳能电池光电转化效率的提高提供了理论及实验参考。
TiO_2nanotubes arrays fabricated by anodization method have highly orderedone-dimensional structure, higher electron transport and electron lifetime, which havea better application prospect in dye-sensitized solar cells(DSSCs). However, becauseof the problems of collapose structure in synthetic process and low dye adsorption,the one-dimensional structure didn’t show advantages. This study carried out researchfor the problem of synthesized TiO_2nanotube arrays and how to improve thephotoelectric conversion efficiency of DSSCs. The structures and influence factorswere investigated by using different electrolytes. The photoelectric conversionefficiencies were improved through using surface modification, ZnO and Sm_2O_3modified TiO_2nanotubes.
The TiO_2nanotube arrays were fabricated in H_3PO_4/NH_4F electrolyte by anodicoxidation method, in which the effects of stirring rates, calcination temperatures,H_3PO_4ammounts, F-concentrations, oxidic voltages and reaction times on surfacemorphology, tube length and tube diameter were investigated using FESEM analysis.The results show that stirring rates, F-concentrations and voltages have importanteffects on the morphology and pore diameter, whereas anodization times affect thelength of the TiO_2nanotube arrays. Based on the influencing conditions of singlefactor, we selected three important factors. The optimum experimental conditionswere obtained by using Box-Behnken Design. The optimal factor conditions wereobtained as follows: anodization time of240min, anodization voltage of15.39V,and NH_4F concentration of0.50mol/L. The results of software simulation using theoptimized conditions were as follows: TiO_2nanotube arrays were obtained with anaverage tube length of1.43μm and average tube diameter of33nm. Moreover, theeffects of calcining temperatures and calcining times on the phase transformation andphoto-electrical properties of TiO_2nanotubes were analyzed by XRD and UV-vis.The optimum calcination conditions were obtained at500℃for2h. The mechanismof fabrication of TiO_2nanotube arrays was investigated using real time-currentanalysis.
The TiO_2nanotube arrays were constructed in ethylene glycol electrolyte byanodic oxidation method. The effects of F-concentrations, oxidic voltages, amount ofH2O and reaction temperatures were investigated. The results show that the H2Oamount is a key factor to controlling the formation TiO_2nanotube arrays. TiO_2nanotube arrays have smooth tube wall and the most ordered structure obtained in anelectrolyte mixture of ethylene glycol,2vol%H2O and0.3wt%NH_4F at40V with 25℃reaction temperature. The surface of the TiO_2nanotube arrays were treatedwith titanium (IV) n-butoxide using a hydrothermal method in combination with anoxygen-plasma treatment. Comparative studies show that the roughness,hydrophilicity and the dye adsorption are increased. The TiO_2nanotube arrays treatedby the combined methods under optimum conditions exhibited a conversionefficiency is increased from1.89%to3.68%.
ZnO/TiO_2nanotube arrays were prepared by a convenient electro-depositiontechnique. The morphology, structure and electrochemical properties wereinvestigated. It is found that ZnO/TiO_2nanotube arrays possess higher roughness,higher dye adsorption, lower band gap energy and longer electron lifetime. Comparedwith that of bare TiO_2nanotube arrays, the photoelectrical performance of thedye-sensitized solar cells is increased from1.71%to3.76%with deposition for60min. This improvement comes from the synergetic effect between ZnO and TiO_2.
The highly ordered TiO_2nanotubes grown on Ti substrate were modifiedconveniently with samarium (Sm) by hydrothermal method for use in backilluminated dye-sensitized solar cells. The morphology, crystal phase, fluorescenceand electrochemical properties were investigated. It is found that Sm_2O_3/TiO_2nanotubes can decrease grain size and band gap energy, and transfer ultraviolet lightto visible light. As a down-conversion luminescence material, samarium oxideimproves the UV radiation harvesting. The result shows that Sm_2O_3modified TiO_2nanotubes can increase short-circuit current and photoelectrical properties ofdye-sensitized solar cells. When TiO_2nanotubes are modified using0.02mol/LSm_2O_3, the efficiency is improved from1.86%to3.22%compared to the bare TiO_2nanotubes. These modifications provide the theoretical and experimental referencefor improving photoelectrical conversion efficiency of dye-sensitized solar cells infuture explorations.
在H_3PO_4/NH_4F无机电解液体系中采用阳极氧化法制得了TiO_2纳米管阵列，通过FESEM系统地考察了搅拌速率、煅烧温度、H_3PO_4添加量、F-浓度、氧化电压、氧化时间对纳米管阵列表面形貌、管径及管长的影响。结果发现，搅拌速率、H_3PO_4与F-浓度、氧化电压对形貌和孔径有较大的影响，氧化反应时间对管长的影响较为显著。根据单因素影响条件，选择其中影响较为显著的三个因素，采用Box-Behnken Design方法设计实验，通过软件模拟得到排列紧密的TiO_2纳米管阵列的最佳制备条件为：氧化时间为240min，氧化电压为15.39V，NH_4F的浓度为0.5mol/L，经由软件模拟得到TiO_2纳米管阵列管内径为33nm，管长为1.43μm。通过XRD和UV-vis表征手段分析了不同煅烧温度和煅烧时间对TiO_2纳米管阵列晶体结构和光电性质的影响，得到最佳的煅烧条件为500℃煅烧2h。并通过实时的电流监控探讨TiO_2纳米管阵列的生长机理。
以乙二醇有机体系为电解液，采用阳极氧化法制得了TiO_2纳米管阵列，分析了F-浓度、水添加量、氧化电压及反应温度对TiO_2纳米管阵列形貌、管径及管长的影响，发现水添加量是能否形成TiO_2纳米管阵列的关键因素，在40V的氧化电压，0.3wt%的NH_4F浓度，2vol%的水添加量及25℃的反应温度下得到的TiO_2纳米管阵列的管径光滑，且高度有序的排列。同时以乙二醇制备的TiO_2纳米管阵列为染料敏化太阳能电池的光阳极，采用四异丙氧基钛(TnB)和氧电浆联合处理其表面，结果表明：TiO_2纳米管阵列结构仍然存在，在纳米管阵列表面及侧壁出现了TiO_2纳米粒子，提高了表面粗糙度和亲水性，增加了染料的吸附量，相对于纯TiO_2纳米管阵列，染料敏化太阳能电池的光电转化效率从1.89%提高至3.68%。
采用阴极电沉积方法制备了异质结型ZnO/TiO_2纳米管阵列。研究了ZnO/TiO_2复合电极的表面形貌、晶形及光吸收性能，结果表明：阴极电沉积法制备的ZnO/TiO_2复合电极表面出现致密的ZnO粒子，表面粗糙度提高、禁带宽度变小、染料吸附量大、电子寿命长。以ZnO/TiO_2纳米管阵列为光阳极组装的染料敏化太阳能电池，相对于纯TiO_2纳米管阵列，60min电沉积的ZnO/TiO_2复合光阳极的光电转化效率可从1.71%提高至3.76%。
采用水热法制备了Sm_2O_3改性TiO_2纳米管阵列，研究了Sm_2O_3/TiO_2纳米管阵列表面形貌、晶形、光吸收和荧光发光性能，发现Sm_2O_3改性后TiO_2纳米管阵列的晶粒尺寸变小，禁带宽度变低；可一定程度地吸收紫外光，并通过荧光性质以可见光发射。将Sm_2O_3/TiO_2复合电极作为染料敏化太阳能电池的光阳极，发现通过Sm3+的下转换荧光性质，可提高太阳能电池中的短路电流。相对于纯TiO_2纳米管阵列，0.02mol/L Sm_2O_3/TiO_2复合光阳极的光电转化效率从1.86%提高至3.22%。这些改性研究为进一步探讨TiO_2纳米管阵列对染料敏化太阳能电池光电转化效率的提高提供了理论及实验参考。
TiO_2nanotubes arrays fabricated by anodization method have highly orderedone-dimensional structure, higher electron transport and electron lifetime, which havea better application prospect in dye-sensitized solar cells(DSSCs). However, becauseof the problems of collapose structure in synthetic process and low dye adsorption,the one-dimensional structure didn’t show advantages. This study carried out researchfor the problem of synthesized TiO_2nanotube arrays and how to improve thephotoelectric conversion efficiency of DSSCs. The structures and influence factorswere investigated by using different electrolytes. The photoelectric conversionefficiencies were improved through using surface modification, ZnO and Sm_2O_3modified TiO_2nanotubes.
The TiO_2nanotube arrays were fabricated in H_3PO_4/NH_4F electrolyte by anodicoxidation method, in which the effects of stirring rates, calcination temperatures,H_3PO_4ammounts, F-concentrations, oxidic voltages and reaction times on surfacemorphology, tube length and tube diameter were investigated using FESEM analysis.The results show that stirring rates, F-concentrations and voltages have importanteffects on the morphology and pore diameter, whereas anodization times affect thelength of the TiO_2nanotube arrays. Based on the influencing conditions of singlefactor, we selected three important factors. The optimum experimental conditionswere obtained by using Box-Behnken Design. The optimal factor conditions wereobtained as follows: anodization time of240min, anodization voltage of15.39V,and NH_4F concentration of0.50mol/L. The results of software simulation using theoptimized conditions were as follows: TiO_2nanotube arrays were obtained with anaverage tube length of1.43μm and average tube diameter of33nm. Moreover, theeffects of calcining temperatures and calcining times on the phase transformation andphoto-electrical properties of TiO_2nanotubes were analyzed by XRD and UV-vis.The optimum calcination conditions were obtained at500℃for2h. The mechanismof fabrication of TiO_2nanotube arrays was investigated using real time-currentanalysis.
The TiO_2nanotube arrays were constructed in ethylene glycol electrolyte byanodic oxidation method. The effects of F-concentrations, oxidic voltages, amount ofH2O and reaction temperatures were investigated. The results show that the H2Oamount is a key factor to controlling the formation TiO_2nanotube arrays. TiO_2nanotube arrays have smooth tube wall and the most ordered structure obtained in anelectrolyte mixture of ethylene glycol,2vol%H2O and0.3wt%NH_4F at40V with 25℃reaction temperature. The surface of the TiO_2nanotube arrays were treatedwith titanium (IV) n-butoxide using a hydrothermal method in combination with anoxygen-plasma treatment. Comparative studies show that the roughness,hydrophilicity and the dye adsorption are increased. The TiO_2nanotube arrays treatedby the combined methods under optimum conditions exhibited a conversionefficiency is increased from1.89%to3.68%.
ZnO/TiO_2nanotube arrays were prepared by a convenient electro-depositiontechnique. The morphology, structure and electrochemical properties wereinvestigated. It is found that ZnO/TiO_2nanotube arrays possess higher roughness,higher dye adsorption, lower band gap energy and longer electron lifetime. Comparedwith that of bare TiO_2nanotube arrays, the photoelectrical performance of thedye-sensitized solar cells is increased from1.71%to3.76%with deposition for60min. This improvement comes from the synergetic effect between ZnO and TiO_2.
The highly ordered TiO_2nanotubes grown on Ti substrate were modifiedconveniently with samarium (Sm) by hydrothermal method for use in backilluminated dye-sensitized solar cells. The morphology, crystal phase, fluorescenceand electrochemical properties were investigated. It is found that Sm_2O_3/TiO_2nanotubes can decrease grain size and band gap energy, and transfer ultraviolet lightto visible light. As a down-conversion luminescence material, samarium oxideimproves the UV radiation harvesting. The result shows that Sm_2O_3modified TiO_2nanotubes can increase short-circuit current and photoelectrical properties ofdye-sensitized solar cells. When TiO_2nanotubes are modified using0.02mol/LSm_2O_3, the efficiency is improved from1.86%to3.22%compared to the bare TiO_2nanotubes. These modifications provide the theoretical and experimental referencefor improving photoelectrical conversion efficiency of dye-sensitized solar cells infuture explorations.
引文
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