硫化铁系光电材料的绿色合成工艺及应用研究
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摘要
硫化铁系化合物是一类重要的半导体材料,具有优异的光电性能,因而在电池领域备受关注。纯相硫化铁系半导体纳米晶缺乏简单、精确可控、易复制和绿色环保的合成工艺,限制了它的规模化生产和商业应用。本文基于溶剂热和水热法开发了一步合成工艺,实现了高质量硫化铁系纳米材料的快速合成。首先以黄铁矿FeS2为研究对象,基于溶剂热法考察了反应原料、溶剂、温度、时间及添加剂等动力学参数对纳米晶的纯度和形貌的影响,将此工艺扩展到FeSe2、NiSx和NiSex的可控合成。进一步开发了纯相FeS2纳米晶(粒径5nm)的水热合成工艺路线,并进行表面改性,提高了纳米晶在大气环境下的稳定性。实现了FeS2的多形貌可控合成。最后,基于三正辛基氧膦(TOPO)修饰的FeS2纳米晶进行薄膜制备及电池组装。论文主要获得以下主要研究成果：
(1)黄铁矿FeS2的绿色合成工艺
开发了油酸-油胺双配体反应体系,以十六烷基三甲基溴化铵为表面活性剂,成功制备了纯相FeS2黄铁矿；通过拉曼光谱测试,进一步证明了所得样品的相结构；基于吸收光谱的测试,计算得到禁带宽度约为1.05eV(与硅禁带宽度接近,Eg=1.1eV)。通过优化溶剂和添加剂,获得了更小尺寸的类球形FeS2纳米晶(30nm),将反应时间缩短15min,同时降低了合成成本。
(2)花状和片状FeSe2的形貌可控合成
为了进一步拓宽FeS2的工艺应用范围,进行了花状和片状FeSe2晶体的合成工艺考察,在较宽的温度区间(200℃-300℃)实现了花状FeSe2样品的可控合成。伴随着温度的升高,形貌从花状向枝状结构转变。将铁源换为硝酸铁时,可在较宽的温度范围(180℃-300℃)获得FeSe2晶体,得到了类球状、絮状、片状及米状四种形貌的产物。基于反应过程的考察,推断其合成机理为：自由的三价铁离子与油胺(OLA)先结合形成相对稳定的"Fe-OLA"前驱体,当系统能量大于能量势垒时,硒源直接与铁前驱体反应形成FeSe2核,随后继续生长。OLA在形核过程起主要作用,而反应温度主要决定生长过程。
(3)多组分镍硫(硒)化合物的可控合成工艺
基于FeS2的合成工艺研究了镍硫(硒)化合物的工艺路线,采用一步法成功制备了四种镍硫(硒)化合物,并分别考察了反应温度和摩尔比对晶体相结构和形貌的影响。研究发现,镍硫化合物的合成温度范围较窄(在260℃左右),而镍硒化合物的合成范围,可从180℃-280℃变化。增加硫含量,产物依次出现Ni7S6正交相、Ni3S2三方相、NiS六方相和NiS2立方相,同时形貌从类球状向四方状变化。通过考察反应动力学参数,得到镍硫化合物形成机理为：Ni离子和S离子与OLA先结合形成相对稳定的“Ni-S-OLA"前驱体,紧接着随着反应能量的增加进而分解形成镍硫化合物核。当Ni/Se摩尔比为2：1时,延长反应时间,NiSe六方相逐渐向Ni3Se2菱形相转变；保持Ni/Se摩尔比为1：1时,通过改变反应温度(180℃-260℃),Ni1-xSe中的x值从0.15到0变化；当保持Ni/Se摩尔比为1：2时,随着反应温度升高,由NiSe2正交相向立方相转变,同时,样品形貌从星状向四方状改变。
(4)黄铁矿FeS2水热合成工艺路线
为了能获得更小尺寸的纳米晶,开发了一步合成FeS2纳米晶的水热合成路线,在140℃-220℃的温度范围内均可获得纯相FeS2,所得样品纯度高、结晶性好、颗粒小合成温度低且污染小。考察了反应时间、摩尔比及浓度对纳米晶的影响；采用TOPO表面处理后提高了FeS2产物的大气稳定性,6个月未出现氧化现象。另外,为了进一步实现FeS2晶体的形貌可控合成,以硝酸铁和半胱氨酸为原料,当溶剂为纯水时,可得到中空球状的白铁矿；且随着反应时间的增加,逐渐发生向黄铁矿相的转变,形貌转变为许多颗粒堆积而成的短棒状结构。当加入乙醇胺为溶剂时,获得立方体、片状、两种十四面体等形貌结构。
(5)FeS2薄膜制备及太阳能电池组装
基于TOPO表面修饰的FeS2纳米晶采用旋涂工艺进行薄膜制备。通过将FeS2分散在聚苯乙烯-甲苯胶体中,获得了均匀性较好的薄膜,但较大的厚度和较高的孔隙率阻碍薄膜的吸光率和造成层间的相互渗透,降低电池的光电响应并易引起短路现象；以氯仿为分散剂可提高薄膜的平整性和透明度,适宜的厚度也有利于光信号的传输。组装成Schottky电池和纳米晶／聚合物复合两类太阳能电池,产生了明显的光电响应信号。
Iron sulfide series have been extensively studied for their potential applications in solar cells. However, the lack of controllable and simple synthetic process of pure iron sulfide series limited their large-scale production and wide application. Based on solvothermal and hydrothermal method, one-step and facile synthetic route was developed to prepare high-quality iron sulfide series materials. In atmosphere, the synthetic process of sulfur group semiconductor, such as pyrite FeS2, FeSe2, NiSx, and NiSex were investigated. Meantime, the synthetic route of FeS2nanocrystals (NCs) was developed via hydrothermal method, and it was modified by trioctylphosphine oxide (TOPO), which could improve stability. Pyrite FeS2with various nanostructures had been prepared in an ethanolamine (ETA)/water binary solution. Finally, the film and solar cell were fabricated based on the FeS2NCs modified by TOPO. The achieved results are stated as follows:
(1) Process optimization of the synthesis of pyrite FeS2via solvothermal method
The coligand (oleic acid (OA)-oleylamine (OLA)) system was developed to prepare pure pyrite FeS2. The phase structure was proved by Raman measurement. The absorption peaks of FeS2samples were at1185nm corresponding to a band gap of1.05eV, which was close to that of silicon (Eg=1.1eV). Meantime, the FeS2sample with smaller particle size was obtained through the optimization of solvents and additives, besides the reaction time was decreased to15min and the cost was greatly reduced.
(2) Controllable synthesis of flower-like and flake-like FeSe2via solvothermal method
In order to extend the process route of FeS2, the synthesis of flower-like and flake-like FeSe2crystals were investigated. The flower-like FeSe2crystals could be got from200℃to300℃with the morphologies changed from flower-like to stick-like structure. When the iron source was replaced by ferric nitrate, four morphologies of the FeSe2samples, including globular, flocculent, flake-like, and rice-like, were obtained in a wide temperature range (180℃-300℃). Based on the reaction dynamics, the mechanism was considered that OLA reacted with free Fe3+to form relatively stable Fe-OLA complex, and then combined with selenium powder to form the FeSe2nuclei. Moreover, the OLA dominated the nucleation process and reaction temperature dominated the growth process.
(3) Controllable synthesis of nickel sulfide (selenide) series via solvothermal method
Based on the process route of the FeS2crystal, the nickel sulfide (selenide) compounds were oriented to synthesize through one-step approach, and the influence of phase structures and morphologies by the reaction temperature and molar ratio were investigated. With increasing of the sulfur content, the products with four kinds of morphologies were obtained in sequence, which were trigonal Ni3S2, rthorhombic Ni7S6, hexagonal NiS and cubic NiS2-Based on the kinetic parameters, the mechanism was found as Ni2+and S powder combined with OLA to form to Ni-S-OLA precursor, and then decomposed to nickel sulfide series. When the molar ratio of Ni/Se was2:1, hexagonal NiSe gradually transformed into rhombohedral Ni3Se2with the extension of the reaction time. The x value of Ni1-xSe could be adjusted from0to0.15with the reaction temperatures from180℃to260℃, and the star-like orthorhombic NiSe2converted to square cubic NiSe2with the increase of temperature at a certain Ni/Se ratio of1:2.
(4) Controllable synthesis of pyrite FeS2via hydrothermal method
To obtian the smaller size of FeS2NCs, the hydrothermal method was developed to prepare FeS2NCs. The obtianed FeS2NCs were of pure phase, high crystallization, stable surface, and small size. The FeS2NCs modified by TOPO showed excellent air stability over six months. Meantime, pyrite FeS2with various novel nanostructures had been prepared on a large scale in an ETA/water binary solution. When only pure water was used as solvents, hollow sphere of marcasite FeS2sample were achieved, and it would transform into rod-like structure been piled up with nanoparticles. When ETA was added into the solvent, cubic, flake-like, and two kinds of tetrakaidecahedron shape of pyrite pure FeS2crystals were obtained by adjsuting the volume ratio of ETA and H2O.
(5) Film preparation and solar cell assembly of FeS2NCs
The film was prepared by spin-coating method with the FeS2NCs modified by TOPO. The FeS2NCs dispersed in the colloid of polystyrene and toluene showed uniform and smooth property of the prepared film, while its large thickness and high porosity hindered the absorbance of light and led to the permeation of the film, decreasing photoeclectric response and causing the short circuit. After dispersing the FeS2NCs into chloroform, the obtained film displayed good smoothness and transparency with suitable transmission of optical signals. Finally, the Schottky and nanocrystalline/polymer composite solar cell were assembled, and produced a clear signal of photoelectric response.
(1)黄铁矿FeS2的绿色合成工艺
开发了油酸-油胺双配体反应体系,以十六烷基三甲基溴化铵为表面活性剂,成功制备了纯相FeS2黄铁矿；通过拉曼光谱测试,进一步证明了所得样品的相结构；基于吸收光谱的测试,计算得到禁带宽度约为1.05eV(与硅禁带宽度接近,Eg=1.1eV)。通过优化溶剂和添加剂,获得了更小尺寸的类球形FeS2纳米晶(30nm),将反应时间缩短15min,同时降低了合成成本。
(2)花状和片状FeSe2的形貌可控合成
为了进一步拓宽FeS2的工艺应用范围,进行了花状和片状FeSe2晶体的合成工艺考察,在较宽的温度区间(200℃-300℃)实现了花状FeSe2样品的可控合成。伴随着温度的升高,形貌从花状向枝状结构转变。将铁源换为硝酸铁时,可在较宽的温度范围(180℃-300℃)获得FeSe2晶体,得到了类球状、絮状、片状及米状四种形貌的产物。基于反应过程的考察,推断其合成机理为：自由的三价铁离子与油胺(OLA)先结合形成相对稳定的"Fe-OLA"前驱体,当系统能量大于能量势垒时,硒源直接与铁前驱体反应形成FeSe2核,随后继续生长。OLA在形核过程起主要作用,而反应温度主要决定生长过程。
(3)多组分镍硫(硒)化合物的可控合成工艺
基于FeS2的合成工艺研究了镍硫(硒)化合物的工艺路线,采用一步法成功制备了四种镍硫(硒)化合物,并分别考察了反应温度和摩尔比对晶体相结构和形貌的影响。研究发现,镍硫化合物的合成温度范围较窄(在260℃左右),而镍硒化合物的合成范围,可从180℃-280℃变化。增加硫含量,产物依次出现Ni7S6正交相、Ni3S2三方相、NiS六方相和NiS2立方相,同时形貌从类球状向四方状变化。通过考察反应动力学参数,得到镍硫化合物形成机理为：Ni离子和S离子与OLA先结合形成相对稳定的“Ni-S-OLA"前驱体,紧接着随着反应能量的增加进而分解形成镍硫化合物核。当Ni/Se摩尔比为2：1时,延长反应时间,NiSe六方相逐渐向Ni3Se2菱形相转变；保持Ni/Se摩尔比为1：1时,通过改变反应温度(180℃-260℃),Ni1-xSe中的x值从0.15到0变化；当保持Ni/Se摩尔比为1：2时,随着反应温度升高,由NiSe2正交相向立方相转变,同时,样品形貌从星状向四方状改变。
(4)黄铁矿FeS2水热合成工艺路线
为了能获得更小尺寸的纳米晶,开发了一步合成FeS2纳米晶的水热合成路线,在140℃-220℃的温度范围内均可获得纯相FeS2,所得样品纯度高、结晶性好、颗粒小合成温度低且污染小。考察了反应时间、摩尔比及浓度对纳米晶的影响；采用TOPO表面处理后提高了FeS2产物的大气稳定性,6个月未出现氧化现象。另外,为了进一步实现FeS2晶体的形貌可控合成,以硝酸铁和半胱氨酸为原料,当溶剂为纯水时,可得到中空球状的白铁矿；且随着反应时间的增加,逐渐发生向黄铁矿相的转变,形貌转变为许多颗粒堆积而成的短棒状结构。当加入乙醇胺为溶剂时,获得立方体、片状、两种十四面体等形貌结构。
(5)FeS2薄膜制备及太阳能电池组装
基于TOPO表面修饰的FeS2纳米晶采用旋涂工艺进行薄膜制备。通过将FeS2分散在聚苯乙烯-甲苯胶体中,获得了均匀性较好的薄膜,但较大的厚度和较高的孔隙率阻碍薄膜的吸光率和造成层间的相互渗透,降低电池的光电响应并易引起短路现象；以氯仿为分散剂可提高薄膜的平整性和透明度,适宜的厚度也有利于光信号的传输。组装成Schottky电池和纳米晶／聚合物复合两类太阳能电池,产生了明显的光电响应信号。
Iron sulfide series have been extensively studied for their potential applications in solar cells. However, the lack of controllable and simple synthetic process of pure iron sulfide series limited their large-scale production and wide application. Based on solvothermal and hydrothermal method, one-step and facile synthetic route was developed to prepare high-quality iron sulfide series materials. In atmosphere, the synthetic process of sulfur group semiconductor, such as pyrite FeS2, FeSe2, NiSx, and NiSex were investigated. Meantime, the synthetic route of FeS2nanocrystals (NCs) was developed via hydrothermal method, and it was modified by trioctylphosphine oxide (TOPO), which could improve stability. Pyrite FeS2with various nanostructures had been prepared in an ethanolamine (ETA)/water binary solution. Finally, the film and solar cell were fabricated based on the FeS2NCs modified by TOPO. The achieved results are stated as follows:
(1) Process optimization of the synthesis of pyrite FeS2via solvothermal method
The coligand (oleic acid (OA)-oleylamine (OLA)) system was developed to prepare pure pyrite FeS2. The phase structure was proved by Raman measurement. The absorption peaks of FeS2samples were at1185nm corresponding to a band gap of1.05eV, which was close to that of silicon (Eg=1.1eV). Meantime, the FeS2sample with smaller particle size was obtained through the optimization of solvents and additives, besides the reaction time was decreased to15min and the cost was greatly reduced.
(2) Controllable synthesis of flower-like and flake-like FeSe2via solvothermal method
In order to extend the process route of FeS2, the synthesis of flower-like and flake-like FeSe2crystals were investigated. The flower-like FeSe2crystals could be got from200℃to300℃with the morphologies changed from flower-like to stick-like structure. When the iron source was replaced by ferric nitrate, four morphologies of the FeSe2samples, including globular, flocculent, flake-like, and rice-like, were obtained in a wide temperature range (180℃-300℃). Based on the reaction dynamics, the mechanism was considered that OLA reacted with free Fe3+to form relatively stable Fe-OLA complex, and then combined with selenium powder to form the FeSe2nuclei. Moreover, the OLA dominated the nucleation process and reaction temperature dominated the growth process.
(3) Controllable synthesis of nickel sulfide (selenide) series via solvothermal method
Based on the process route of the FeS2crystal, the nickel sulfide (selenide) compounds were oriented to synthesize through one-step approach, and the influence of phase structures and morphologies by the reaction temperature and molar ratio were investigated. With increasing of the sulfur content, the products with four kinds of morphologies were obtained in sequence, which were trigonal Ni3S2, rthorhombic Ni7S6, hexagonal NiS and cubic NiS2-Based on the kinetic parameters, the mechanism was found as Ni2+and S powder combined with OLA to form to Ni-S-OLA precursor, and then decomposed to nickel sulfide series. When the molar ratio of Ni/Se was2:1, hexagonal NiSe gradually transformed into rhombohedral Ni3Se2with the extension of the reaction time. The x value of Ni1-xSe could be adjusted from0to0.15with the reaction temperatures from180℃to260℃, and the star-like orthorhombic NiSe2converted to square cubic NiSe2with the increase of temperature at a certain Ni/Se ratio of1:2.
(4) Controllable synthesis of pyrite FeS2via hydrothermal method
To obtian the smaller size of FeS2NCs, the hydrothermal method was developed to prepare FeS2NCs. The obtianed FeS2NCs were of pure phase, high crystallization, stable surface, and small size. The FeS2NCs modified by TOPO showed excellent air stability over six months. Meantime, pyrite FeS2with various novel nanostructures had been prepared on a large scale in an ETA/water binary solution. When only pure water was used as solvents, hollow sphere of marcasite FeS2sample were achieved, and it would transform into rod-like structure been piled up with nanoparticles. When ETA was added into the solvent, cubic, flake-like, and two kinds of tetrakaidecahedron shape of pyrite pure FeS2crystals were obtained by adjsuting the volume ratio of ETA and H2O.
(5) Film preparation and solar cell assembly of FeS2NCs
The film was prepared by spin-coating method with the FeS2NCs modified by TOPO. The FeS2NCs dispersed in the colloid of polystyrene and toluene showed uniform and smooth property of the prepared film, while its large thickness and high porosity hindered the absorbance of light and led to the permeation of the film, decreasing photoeclectric response and causing the short circuit. After dispersing the FeS2NCs into chloroform, the obtained film displayed good smoothness and transparency with suitable transmission of optical signals. Finally, the Schottky and nanocrystalline/polymer composite solar cell were assembled, and produced a clear signal of photoelectric response.
引文
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