染料敏化太阳能电池光阳极的制备、性质和光电转换机理研究
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摘要
染料敏化TiO_2太阳能电池具有可见光响应强、光电转换效率高、环境友好和成本低等优点，对于新能源开发应用具有广阔的发展前景。但是，在光电转换的过程中，光生电子将通过染料敏化TiO_2太阳能电池的光阳极中的表面、界面缺陷，如，表面氧空位能级等与价带的光生空穴复合，从而降低了太阳能电池的光电转换效率。本论文针对上述难题，设计和制备了一系列新型染料敏化TiO_2太阳能电池的光阳极，详细研究了光阳极的物理化学性质，测定了染料敏化太阳能电池的光电转换效率，并讨论其光电转换机理。主要研究内容如下：
1、采用改性的TiCl4水解法制备出TiO_2-5、TiO_2-10和TiO_2-20三种不同表面性质的样品。利用Rup2P（(1,10-邻菲咯啉)2-2-(2-吡啶基)苯咪唑钌混配配合物）作为敏化剂，制备出Rup2P/TiO_2-5/ITO、Rup2P/TiO_2-10/ITO和Rup2P/TiO_2-20/ITO表面敏化薄膜电极。测试结果表明三种薄膜电极的光电转换效率为Rup2P/TiO_2-10/ITO最高，Rup2P/TiO_2-20/ITO次之，Rup2P/TiO_2-5/ITO最低。利用吸收光谱(DRS)、表面光电压谱(SPS)、荧光光谱(PL)和表面光电流作用谱等分析了Rup2P和三种TiO_2的能带结构和表面性质；利用光致循环伏安和表面光电流作用谱研究了三种薄膜电极的光致界面电荷转移过程。结果证明，在光致界面电荷转移过程中，TiO_2层表面氧空位对Rup2P/TiO_2-X/ITO薄膜电极光致电荷转移产生重要影响，并进一步讨论了Rup2P/TiO_2-X/ITO薄膜电极的光电流产生机理。
2、采用溶胶-凝胶法制备出In表面修饰的TiO_2(TiO_2-Inx%)纳米粒子。利用N719（二(四丁基铵)顺式-双(异硫氰基)双(2,2'-联吡啶-4,4'-二羧酸)钌(II)）作为敏化剂，制备出N719/TiO_2/FTO和N719/TiO_2-Inx%/FTO染料敏化薄膜电极。光电转换效率实验表明，N719/TiO_2-Inx%/FTO薄膜电极的光电转换效率均高于N719/TiO_2/FTO，其中N719/TiO_2-In0.1%/FTO的光电转换效率比N719/TiO_2/FTO提高了20%。利用X射线衍射谱(XRD)、X射线光电子能谱(XPS)、漫反射吸收光谱(DRS)、荧光光谱(PL)和表面光电流作用谱确定了TiO_2-Inx%样品中In离子的存在方式和能带结构；利用表面光电流作用谱研究了N719/TiO_2-Inx%/FTO薄膜电极的光致界面电荷转移过程。结果表明，In离子在TiO_2表面形成O-In-Cln（n=1或2）物种，该物种的表面态能级在导带下0.3eV；在光电流产生过程中，O-In-Cl（nn=1或2）表面态能级有效地抑制了光生载流子在TiO_2-Inx%层的复合，促进了阳极光电流的增加，从而导致N719/TiO_2-Inx%/FTO薄膜电极的光电转化效率高于N719/TiO_2/FTO，并进一步讨论了光致界面电荷转移的机理。
3、采用溶胶-凝胶法制备出Sn掺杂的TiO_2(TiO_2-Snx%)纳米粒子。利用N719作为敏化剂，制备出N719/TiO_2/FTO和N719/TiO_2-Snx%/FTO染料敏化薄膜电极。利用X射线衍射谱(XRD)、X射线光电子能谱(XPS)、漫反射吸收光谱(DRS)、荧光光谱(PL)和表面光电流作用谱确定了TiO_2-Snx%样品中Sn离子的存在方式和能带结构。研究结果表明，Sn离子以取代式掺杂方式进入TiO_2晶格，在TiO_2下方0.1eV处形成掺杂能级；在光电流产生过程中，掺杂能级有效地抑制了光生载流子在TiO_2-Snx%层的复合，促进了阳极光电流的增加。光电转换效率实验表明，N719/TiO_2-Snx%/FTO薄膜电极的光电转换效率均高于N719/TiO_2/FTO，其中N719/TiO_2-In0.2%/FTO的光电转换效率比N719/TiO_2/FTO提高了46%。同时，利用表面光电流作用谱研究了N719/TiO_2-Snx%/FTO薄膜电极的光致界面电荷转移过程，并进一步讨论了光致界面电荷转移的机理。
4、采用溶胶-凝胶法制备出B掺杂的TiO_2(TiO_2-Bx%)纳米粒子。利用N719作为敏化剂，制备出N719/TiO_2/FTO和N719/TiO_2-Bx%/FTO染料敏化薄膜电极。利用X射线衍射谱(XRD)、X射线光电子能谱(XPS)、漫反射吸收光谱(DRS)、荧光光谱(PL)和表面光电流作用谱确定了TiO_2-Bx%样品中B离子的存在方式和能带结构。结果表明，B离子以间隙式掺杂方式进入TiO_2晶格，掺杂能级的位置在TiO_2价带上方0.1eV。在光电流产生过程中，B掺杂有效地抑制了光生载流子在TiO_2-Bx%层的复合，促进了阳极光电流的增加。光电转换效率实验表明，N719/TiO_2-Bx%/FTO薄膜电极的光电转换效率高于N719/TiO_2/FTO，其中N719/TiO_2-B0.05%/FTO的光电转换效率比N719/TiO_2/FTO提高了15.8%。利用表面光电流作用谱研究了N719/TiO_2-Bx%/FTO薄膜电极的光致界面电荷转移过程，并进一步讨论了光致界面电荷转移的机理。
Dye-sensitized TiO_2solar cells with strong visible light response, highphotoelectric conversion efficiency, environment-friendly and low cost, and hasbroad prospects for development in the new energy development. However, in theprocess of the photoelectric conversion, photo-generated electrons will compositewith photo-generated holes of the valence band by the surface of the photoanode andinterface defects, such as surface oxygen vacancies energy levels, which wouldreducing the photoelectric conversion efficiency. In response to these problems, inthis paper we designed and prepared a series of new nano-titanium dioxide electrode,a detailed study of the physical and chemical properties of the thin-film electrode,photoelectric conversion efficiency of dye-sensitized solar cell and discuss itsphotoelectric conversion mechanism. The main points could be summarized asfollows:
1、TiO_2-5, TiO_2-10and TiO_2-20samples prepared by modified TiCl4hydrolyzed,have different properties on surface. Then they were further surface-sensitized withthe Rup2P（Ru(phen)2(PIBH) complex）for surface sensitization film electrode ofRup2P/TiO_2-5/ITO, Rup2P/TiO_2-10/ITO and Rup2P/TiO_2-20/ITO. The measuredresults of photovoltaic properties of the three films revealed that Rup2P/TiO_2-10/ITOis best and the Rup2P/TiO_2-5/ITO is worst. We analyzed the energy band structures,properties on surface of Rup2P and the three TiO_2samples using DRS, SPS, PL andphotocurrent action spectrum; studied the photo-induced charge transfer process withcyclic voltammograms under irradiation and photocurrent action spectra. The resultsrevealed the oxygen vacancy at the TiO_2surface was very important for thephoto-induced charge transfer process of Rup2P/TiO_2-X/ITO, and further more wediscussed the photocurrent mechanism of Rup2P/TiO_2-X/ITO.
2、We prepared surface-modified TiO_2nanoparticle (TiO_2-Inx%) by using sol-gelmethod. By using N719（[NaRu(4,40-bis-(5-(hexylthio)thiophen-2-yl)-2,20-bipyridine)(4-carboxylicacid-40-carboxylate-2,20-bipyridine)(NCS)2]） as thesensitizing agent, the N719/TiO_2/FTO and N719/TiO_2-Inx%/FTO film electrodes were prepared. Under the solar cell structure of the thin film electrodes, thephotoelectric conversion efficiency of all the N719/TiO_2-Inx%/FTO film electrodeswere higher than that of N719/TiO_2/FTO, and the photoelectric conversion efficiencyof the N719/TiO_2-In0.1%/FTO was enhanced by20%than that of N719/TiO_2/FTO.We analyzed the band structure and presence of In ion in TiO_2-Inx%samples usingXRD, XPS, DRS, PL spectra and surface photocurrent action spectra. Thephoto-induced charge transfer process of the N719/TiO_2-Inx%/FTO film electrodeswere studied by surface photocurrent action spectra. The results show that the speciesO-In-Cl（nn=1or2）are formed at the TiO_2surface, and the surface state energy levelsof the species locates at0.3eV below the conduction band of TiO_2. The surface stateenergy levels of the species can effectively inhibit the recombination ofphoto-generated carrier in the process of photocurrent generation, increase the anodicphotocurrent, and improve the photoelectric conversion efficiency ofN719/TiO_2-Inx%/FTO thin film electrode significantly. And the charge transfermechanism in the light-induced interfacial is further discussed.
3、We prepared Sn ions doped TiO_2nanoparticle (TiO_2-Snx%) by using sol-gelmethod. By using N719as the sensitizing agent, the N719/TiO_2/FTO andN719/TiO_2-Snx%/FTO film electrodes were prepared. We analyzed the bandstructure and presence of Sn ion in TiO_2-Snx%samples using XRD, XPS, DRS, PLspectra and surface photocurrent action spectra. The results show that the Sn ionssubstituted the lattice titanium ions in TiO_2lattice. And thus, the doping energy levelwas located at0.1eV below the conduction band of TiO_2; The energy levels of thespecies can effectively inhibit the recombination of photo-generated carrier in theprocess of photocurrent generation, increase the anodic photocurrent. Under the solarcell structure of the thin film electrodes, the photoelectric conversion efficiency of allthe N719/TiO_2-Snx%/FTO film electrodes were higher than that of N719/TiO_2/FTO,and the photoelectric conversion efficiency of the N719/TiO_2-Sn0.2%/FTO wasenhanced by46%than that of N719/TiO_2/FTO. The photo-induced charge transferprocess of the N719/TiO_2-Snx%/FTO film electrodes were studied by surfacephotocurrent action spectra. And the charge transfer mechanism in the light-inducedinterfacial is further discussed.
4、We prepared B ions doped TiO_2nanoparticle (TiO_2-Bx%) by using sol-gelmethod. By using N719as the sensitizing agent, the N719/TiO_2/FTO andN719/TiO_2-Bx%/FTO film electrodes were prepared. We analyzed the band structureand presence of Sn ion in TiO_2-Bx%samples using XRD, XPS, DRS, PL spectra andsurface photocurrent action spectra. The results show that the B ions gap-type dopinginto the TiO_2lattice; the doping energy level was located at0.1eV on the valenceband of TiO_2. The B doped TiO_2can effectively inhibit the recombination ofphoto-generated carrier in the process of photocurrent generation, increase the anodicphotocurrent. Under the solar cell structure of the thin film electrodes, thephotoelectric conversion efficiency of the N719/TiO_2-Bx%/FTO film electrodes werehigher than that of N719/TiO_2/FTO, and the photoelectric conversion efficiency ofthe N719/TiO_2-B0.05%/FTO was enhanced by15.8%than that of N719/TiO_2/FTO.The photo-induced charge transfer process of the N719/TiO_2-Bx%/FTO filmelectrodes were studied by surface photocurrent action spectra., and the chargetransfer mechanism in the light-induced interfacial is further discussed.
1、采用改性的TiCl4水解法制备出TiO_2-5、TiO_2-10和TiO_2-20三种不同表面性质的样品。利用Rup2P（(1,10-邻菲咯啉)2-2-(2-吡啶基)苯咪唑钌混配配合物）作为敏化剂，制备出Rup2P/TiO_2-5/ITO、Rup2P/TiO_2-10/ITO和Rup2P/TiO_2-20/ITO表面敏化薄膜电极。测试结果表明三种薄膜电极的光电转换效率为Rup2P/TiO_2-10/ITO最高，Rup2P/TiO_2-20/ITO次之，Rup2P/TiO_2-5/ITO最低。利用吸收光谱(DRS)、表面光电压谱(SPS)、荧光光谱(PL)和表面光电流作用谱等分析了Rup2P和三种TiO_2的能带结构和表面性质；利用光致循环伏安和表面光电流作用谱研究了三种薄膜电极的光致界面电荷转移过程。结果证明，在光致界面电荷转移过程中，TiO_2层表面氧空位对Rup2P/TiO_2-X/ITO薄膜电极光致电荷转移产生重要影响，并进一步讨论了Rup2P/TiO_2-X/ITO薄膜电极的光电流产生机理。
2、采用溶胶-凝胶法制备出In表面修饰的TiO_2(TiO_2-Inx%)纳米粒子。利用N719（二(四丁基铵)顺式-双(异硫氰基)双(2,2'-联吡啶-4,4'-二羧酸)钌(II)）作为敏化剂，制备出N719/TiO_2/FTO和N719/TiO_2-Inx%/FTO染料敏化薄膜电极。光电转换效率实验表明，N719/TiO_2-Inx%/FTO薄膜电极的光电转换效率均高于N719/TiO_2/FTO，其中N719/TiO_2-In0.1%/FTO的光电转换效率比N719/TiO_2/FTO提高了20%。利用X射线衍射谱(XRD)、X射线光电子能谱(XPS)、漫反射吸收光谱(DRS)、荧光光谱(PL)和表面光电流作用谱确定了TiO_2-Inx%样品中In离子的存在方式和能带结构；利用表面光电流作用谱研究了N719/TiO_2-Inx%/FTO薄膜电极的光致界面电荷转移过程。结果表明，In离子在TiO_2表面形成O-In-Cln（n=1或2）物种，该物种的表面态能级在导带下0.3eV；在光电流产生过程中，O-In-Cl（nn=1或2）表面态能级有效地抑制了光生载流子在TiO_2-Inx%层的复合，促进了阳极光电流的增加，从而导致N719/TiO_2-Inx%/FTO薄膜电极的光电转化效率高于N719/TiO_2/FTO，并进一步讨论了光致界面电荷转移的机理。
3、采用溶胶-凝胶法制备出Sn掺杂的TiO_2(TiO_2-Snx%)纳米粒子。利用N719作为敏化剂，制备出N719/TiO_2/FTO和N719/TiO_2-Snx%/FTO染料敏化薄膜电极。利用X射线衍射谱(XRD)、X射线光电子能谱(XPS)、漫反射吸收光谱(DRS)、荧光光谱(PL)和表面光电流作用谱确定了TiO_2-Snx%样品中Sn离子的存在方式和能带结构。研究结果表明，Sn离子以取代式掺杂方式进入TiO_2晶格，在TiO_2下方0.1eV处形成掺杂能级；在光电流产生过程中，掺杂能级有效地抑制了光生载流子在TiO_2-Snx%层的复合，促进了阳极光电流的增加。光电转换效率实验表明，N719/TiO_2-Snx%/FTO薄膜电极的光电转换效率均高于N719/TiO_2/FTO，其中N719/TiO_2-In0.2%/FTO的光电转换效率比N719/TiO_2/FTO提高了46%。同时，利用表面光电流作用谱研究了N719/TiO_2-Snx%/FTO薄膜电极的光致界面电荷转移过程，并进一步讨论了光致界面电荷转移的机理。
4、采用溶胶-凝胶法制备出B掺杂的TiO_2(TiO_2-Bx%)纳米粒子。利用N719作为敏化剂，制备出N719/TiO_2/FTO和N719/TiO_2-Bx%/FTO染料敏化薄膜电极。利用X射线衍射谱(XRD)、X射线光电子能谱(XPS)、漫反射吸收光谱(DRS)、荧光光谱(PL)和表面光电流作用谱确定了TiO_2-Bx%样品中B离子的存在方式和能带结构。结果表明，B离子以间隙式掺杂方式进入TiO_2晶格，掺杂能级的位置在TiO_2价带上方0.1eV。在光电流产生过程中，B掺杂有效地抑制了光生载流子在TiO_2-Bx%层的复合，促进了阳极光电流的增加。光电转换效率实验表明，N719/TiO_2-Bx%/FTO薄膜电极的光电转换效率高于N719/TiO_2/FTO，其中N719/TiO_2-B0.05%/FTO的光电转换效率比N719/TiO_2/FTO提高了15.8%。利用表面光电流作用谱研究了N719/TiO_2-Bx%/FTO薄膜电极的光致界面电荷转移过程，并进一步讨论了光致界面电荷转移的机理。
Dye-sensitized TiO_2solar cells with strong visible light response, highphotoelectric conversion efficiency, environment-friendly and low cost, and hasbroad prospects for development in the new energy development. However, in theprocess of the photoelectric conversion, photo-generated electrons will compositewith photo-generated holes of the valence band by the surface of the photoanode andinterface defects, such as surface oxygen vacancies energy levels, which wouldreducing the photoelectric conversion efficiency. In response to these problems, inthis paper we designed and prepared a series of new nano-titanium dioxide electrode,a detailed study of the physical and chemical properties of the thin-film electrode,photoelectric conversion efficiency of dye-sensitized solar cell and discuss itsphotoelectric conversion mechanism. The main points could be summarized asfollows:
1、TiO_2-5, TiO_2-10and TiO_2-20samples prepared by modified TiCl4hydrolyzed,have different properties on surface. Then they were further surface-sensitized withthe Rup2P（Ru(phen)2(PIBH) complex）for surface sensitization film electrode ofRup2P/TiO_2-5/ITO, Rup2P/TiO_2-10/ITO and Rup2P/TiO_2-20/ITO. The measuredresults of photovoltaic properties of the three films revealed that Rup2P/TiO_2-10/ITOis best and the Rup2P/TiO_2-5/ITO is worst. We analyzed the energy band structures,properties on surface of Rup2P and the three TiO_2samples using DRS, SPS, PL andphotocurrent action spectrum; studied the photo-induced charge transfer process withcyclic voltammograms under irradiation and photocurrent action spectra. The resultsrevealed the oxygen vacancy at the TiO_2surface was very important for thephoto-induced charge transfer process of Rup2P/TiO_2-X/ITO, and further more wediscussed the photocurrent mechanism of Rup2P/TiO_2-X/ITO.
2、We prepared surface-modified TiO_2nanoparticle (TiO_2-Inx%) by using sol-gelmethod. By using N719（[NaRu(4,40-bis-(5-(hexylthio)thiophen-2-yl)-2,20-bipyridine)(4-carboxylicacid-40-carboxylate-2,20-bipyridine)(NCS)2]） as thesensitizing agent, the N719/TiO_2/FTO and N719/TiO_2-Inx%/FTO film electrodes were prepared. Under the solar cell structure of the thin film electrodes, thephotoelectric conversion efficiency of all the N719/TiO_2-Inx%/FTO film electrodeswere higher than that of N719/TiO_2/FTO, and the photoelectric conversion efficiencyof the N719/TiO_2-In0.1%/FTO was enhanced by20%than that of N719/TiO_2/FTO.We analyzed the band structure and presence of In ion in TiO_2-Inx%samples usingXRD, XPS, DRS, PL spectra and surface photocurrent action spectra. Thephoto-induced charge transfer process of the N719/TiO_2-Inx%/FTO film electrodeswere studied by surface photocurrent action spectra. The results show that the speciesO-In-Cl（nn=1or2）are formed at the TiO_2surface, and the surface state energy levelsof the species locates at0.3eV below the conduction band of TiO_2. The surface stateenergy levels of the species can effectively inhibit the recombination ofphoto-generated carrier in the process of photocurrent generation, increase the anodicphotocurrent, and improve the photoelectric conversion efficiency ofN719/TiO_2-Inx%/FTO thin film electrode significantly. And the charge transfermechanism in the light-induced interfacial is further discussed.
3、We prepared Sn ions doped TiO_2nanoparticle (TiO_2-Snx%) by using sol-gelmethod. By using N719as the sensitizing agent, the N719/TiO_2/FTO andN719/TiO_2-Snx%/FTO film electrodes were prepared. We analyzed the bandstructure and presence of Sn ion in TiO_2-Snx%samples using XRD, XPS, DRS, PLspectra and surface photocurrent action spectra. The results show that the Sn ionssubstituted the lattice titanium ions in TiO_2lattice. And thus, the doping energy levelwas located at0.1eV below the conduction band of TiO_2; The energy levels of thespecies can effectively inhibit the recombination of photo-generated carrier in theprocess of photocurrent generation, increase the anodic photocurrent. Under the solarcell structure of the thin film electrodes, the photoelectric conversion efficiency of allthe N719/TiO_2-Snx%/FTO film electrodes were higher than that of N719/TiO_2/FTO,and the photoelectric conversion efficiency of the N719/TiO_2-Sn0.2%/FTO wasenhanced by46%than that of N719/TiO_2/FTO. The photo-induced charge transferprocess of the N719/TiO_2-Snx%/FTO film electrodes were studied by surfacephotocurrent action spectra. And the charge transfer mechanism in the light-inducedinterfacial is further discussed.
4、We prepared B ions doped TiO_2nanoparticle (TiO_2-Bx%) by using sol-gelmethod. By using N719as the sensitizing agent, the N719/TiO_2/FTO andN719/TiO_2-Bx%/FTO film electrodes were prepared. We analyzed the band structureand presence of Sn ion in TiO_2-Bx%samples using XRD, XPS, DRS, PL spectra andsurface photocurrent action spectra. The results show that the B ions gap-type dopinginto the TiO_2lattice; the doping energy level was located at0.1eV on the valenceband of TiO_2. The B doped TiO_2can effectively inhibit the recombination ofphoto-generated carrier in the process of photocurrent generation, increase the anodicphotocurrent. Under the solar cell structure of the thin film electrodes, thephotoelectric conversion efficiency of the N719/TiO_2-Bx%/FTO film electrodes werehigher than that of N719/TiO_2/FTO, and the photoelectric conversion efficiency ofthe N719/TiO_2-B0.05%/FTO was enhanced by15.8%than that of N719/TiO_2/FTO.The photo-induced charge transfer process of the N719/TiO_2-Bx%/FTO filmelectrodes were studied by surface photocurrent action spectra., and the chargetransfer mechanism in the light-induced interfacial is further discussed.
引文
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[2] Nazeemuddin M K,Kay A,Rodicio I,et al.Conversion of light to electricity by cis-X2Bis(2,2'-bipyridyldicarboxylate)rutheniyum(II)charge-transfer sensitizers(X=Cl-, B-, I-, CN-,andSCN-) on nanocrystalline TiO2electrodes, J. Am. Chem. Soc.1993,115,6382-6390
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[9] Chiba, Y., Islam, A., Watanabe, Y. et al. Dye-Sensitized Solar Cells with ConversionEfficiency of11.1%.J. Appl. Phys.2006,45, L638.
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[22] Wang E J., Yang W S., Cao Y A. Unique Surface Chemical Species on Indium Doped TiO2and Their Effect on the Visible Light Photocatalytic Activity. J. Phys. Chem. C2009,113,20912.
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