多元氧族半导体纳米材料的液相合成、生长机理及性能研究
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摘要
多元金属氧族化合物与二元化合物相比,具有组成和结构的多样性,从而体现出丰富的物理化学性质,如光学、电学、磁学、力学、压电性质等。因此多元金属化合物的合成是固体化学中一个十分活跃的领域。对于三元或多元金属纳米材料液相合成,涉及到两种或以上阳离子的反应,如果这些金属阳离子前驱物的反应活性差异很大,则很容易发生相分离,得到异质结构或二元化合物的混合物,尤其容易得到难溶的二元过渡金属氧化物、硫化物、硒化物等,使得含过渡金属的多元氧族化合物纳米材料非常有限。因此,纳米级多元金属氧族半导体材料的溶剂热反应合成和形貌控制合成不仅从合成新的纳米结构、丰富氧族纳米化合物、还是从探索新的无机纳米材料来说都具有理论意义,而且还可以开拓半导体纳米材料的新特性。本文在溶剂热/水热体系中探索和拓展了多元金属氧族纳米材料的化学合成新方法和新技术,为控制合成多元金属氧族纳米材料积累了一些宝贵的经验。通过调控反应前驱物的反应活性和反应环境合成多元氧族化合物,探究多元氧族化合物液相合成的关键问题；发展一种表面活性剂辅助的溶剂热合成高质量多元氧族化合物纳米晶的方法,揭示其形成机理。具体的研究内容包括：
(1) ZnGa2O4等多元氧化物及其固溶体纳米晶的控制合成、形成机理和光学性质研究。通过苯甲醚溶剂热法制备了尺寸约为20 nm的缺角立方状ZnGa2O4纳米晶,该纳米晶在435nm处有较强的蓝光发射。通过控制前驱物中锌的量可以得到立方相γ-Ga2O3和立方相ZnGa2O4的固熔体系列纳米晶,即ZnχGa2O3+χ(0≤χ≤1)。它们的晶格参数基本符合维加定律,带隙宽可以在4.43到3.70 eV间调控。同时其发光波长也可在395到435 nm间进行调控。时间历程分析表明：首先生成介稳态的γ-Ga203,随后生成ZnO并逐渐离解出的锌离子扩散进γ-Ga2O3晶格中得到ZnχGa2O3+χ(0≤χ≤1)固熔体系列纳米晶,最终得到ZnGa2O4纳米晶。在这个Zn2+逐渐扩散到晶格的反应过程中,氧缺陷也逐渐被淬灭,使畸变的Ga-O八面体逐渐成为Ga-O正八面体得到发纯正蓝光的ZnGa2O4纳米晶。我们进一步在水热体系中,以十二烷基苯磺酸钠作表面活性剂成功制备了正八面体形的ZnGa2O4和ZnAl2O4纳米晶。并以发蓝光的ZnGa2O4八面体纳米晶为基底材料,实现了Mn2+和Cr3+的掺杂,分别得到到绿光和红光的荧光材料,实现了三原色纳米荧光材料的合成。
(2)AgGaS2等三元及四元硫化物纳米晶的合成及其光学性质研究。以一些简单无机盐为前驱物,油胺为包覆剂,以环己烷和长链醇的混合溶剂作为反应介质,控制合成了尺寸形貌可控的3D纳米花和胶体状AgGaS2纳米材料。研究表明醇的浓度、醇的碳链长度、油胺的浓度等因素都能导致AgGaS2纳米晶形貌的转变。如果醇的浓度较大,碳链长度很长或油胺的浓度较大,可以充分保护AgGaS2而得到胶状粒子。反之则得到AgGaS2纳米花。通过对AgGaS2纳米花进行高分辨透射电镜和结构分析,AgGaS2纳米花的基本组装单元约为5 nm的小粒子,沿<112>方向取向生长组装成3D纳米结构。AgGaS2纳米花和胶体粒子的室温紫外可见吸收光谱基本相同,而胶体粒子的发光光谱红移了12 nm。AgGaS2纳米花的表面光电压性质与紫外吸收比较吻合,且光电压响应随着外加电场增强而增强,表明在自建电场内AgGaS2能够吸收光子和分离电子-空穴对。在同样的反应体系中,我们也得到了高温正交相的AgInS2纳米晶以及AgInχGa1-χS2(0≤x≤1)四元固熔体纳米晶。
(3) CulnSe2, CuGaSe2, CuInχGa1-χSe2纳米六角片的液相控制合成及生成机理。首次采用两步法,以Vc为还原剂提出了一种全新的解决硒源的方法。并以一些简单的无机盐为前驱体、PVP为包覆剂、DMF为溶剂,通过简单的溶剂热法得到了三元或四元硒化物的纳米六角片。二维CulnSe2六角纳米片为四方晶相的黄铜矿结构,其尺寸约为200 nm,为p型半导体。通过对CulnSe2进行高分辨透射电镜分析,证明所得的三元硒化物为单晶结构,且二维的结构是由于{112}和{001}面的快速生长导致的。进一步的对比实验表明,CulnSe2纳米片的形成和形貌受到多种因素的影响：硒粉的前处理时间、PVP的量、Vc的量、反应时间、温度等。CulnSe2纳米片的乙醇分散性及稳定性测试表明CulnSe2的乙醇均匀分散体系不管是透射光还是背散射光经过7天的测试,此分散体系没有发生沉淀、乳化、絮凝、凝结、分相等现象,能作为丝网印刷的“墨水”,可用于柔性薄膜太阳能电池的吸收材料。同样的体系中也得到CuGaSe2六方纳米片；控制前驱物中In/Ga的比例得到CuInχGa1-χSe2四元纳米硒化物。CuInχGa1-χSe2的紫外吸收光谱图都是吸收介于900～1300 nm之间的连续谱线,它们的带隙宽Eg介于0.95～1.46之间。此两步法在合成硫属化合物方面具有一定的普适性：在乙醇-乙醇胺体系中采用两步法同样可以得到CuInSe2纳米球。利用CuInχGa1-χSe2作为吸收材料制备了Ag/CdS/CuInχGa1-χSe2/FTO结构的太阳能电池。
Comparing with binary compounds, multinary oxygen-group compounds exhibit useful physical and chemical properties such as optical, electronic, magnetic, mechanical, and piezoelectricity properties. Therefore, the synthesis of multinary oxygen-group compounds is becoming an active area of solid state chemistry. Solvothermal reaction is motivated by their potential to provide an access to multinary oxygen-group compounds in nanoscale with obvious quantum confinement effect and size- and/or shape-dependent properties. However, the synthesis such of multiple component nanocrystals has been limited by the reactivities of the precursors and the ease of phase separation of the alloyed constituents. In other words, if the reaction activities of two metal precursors differ from each other, a separated nucleus will be generated and grow into heterostructures or even two compounds, especially to form the less solubility of transition metal oxide, sulfide or selenide, which make the number of known synthetic multinary oxygen-group compounds with metal ions is limited. Thus, structure and/or shape controlled synthesis of multinary oxygen-group semiconductor nanomaterials will not bring the theoretically meanings, but also the application significance which extended the semiconductor materials. In this thesis, we have attempted and extended to synthesis multinary oxygen-group semiconductor nanomaterials with new chemical synthetic method and thought, which gathered experience for controlled synthesis of multinary oxygen-group semiconductor nanomaterials. Detailed rerearch contents are summarized as following:
(1) Controlled synthesis and synthesis mechanism of ZnGa2O4 nanocrystals and their research of optical properties. Truncated cubic shape of ZnGa2O4 nanocrystals with 20 nm have been synthesized via a simple anisole solvothermal method. The as-prepared ZnGa2O4 nanocrystals emitted strong blue light at 435 nm. By adjusting zinc quantum of precursors, solid solutions serial nanocrystals of cubicγ-Ga2O3 and cubic ZnGa2O4 that also be expressed to ZnχGa2O3+χ(0≤χ≤1) could be obtained. The lattice parameters and band gap Eg of ZnχGa2O3+χ(0≤χ≤1) serial nanocrystals changed linearly which consistent with Vegard's law basically. The Eg of ZnχGa2O3+χ(0≤χ≤1) serial nanocrystals ranged from 4.43 to 3.70 eV and could be tuned their emission spectra from 395 to 435nm. The formation of ZnχGa2O3+χ(0<χ<1) and ZnGa2O4 resulted from Zn2+ (came from dissociated amorphous ZnO) diffusing into theγ-Ga2O3 nanocrystal lattice structure. In the process of Zn2+ diffusing into nanocrystal lattice, the oxygen vacancies were gradually extinguished making distorted Ga-O octahedron transforming to regular one which is the self-activated blue emission site. In the hydrothermal reaction system, ZnGa2O4 and ZnAl2O4 nanocrystals with regular octahedron were obtained. With the blue fluorescent material ZnGa2O4 regular octahedrona nanocrystals as basilar material doped with Mn2+ and Cr3+, we successfully gained green and red fluorescent respectively and achieved the three primary colors.
(2) Shape-Controlled synthesis of AgGaS2 nanocrystals and their research of optical properties. Nearly monodispersed AgGaS2 nanocrystals with flower-like or colloidal shape were synthesized in a simple solution system, in which a mixture of 1-octyl alcohol and cyclohexane was used as reactive medium and oleylamine as surfactant. The shape and size of these as-prepared nanocrystals could be tuned effectively by controlling the reaction conditions, such as the ratio of octanol to cyclohexane, the length of carbon chain of fatty alcohol and the concentration of oleylamine. The results showed that fatty alcohol play key factor for the shape and size transformation of AgGaS2 from 3D nanoflowers (50 nm) to colloids (10-20 nm), and a plausible shape evolution and crystal growth mechanism have been suggested for the formation of 3D nanoflowers and colloids. The simple reaction system might provide a new approach to controlled synthesis ternary nanomaterials and understood the reaction mechanism along with the growth kinetics of nanocrystals. Oleylamine combined with alcohol to absorb the AgGaS2 nanocrystals which could reduce the total surface energy and protect the nanocrystals. From the HRTRM and crystal structure analysis, monodispersed AgGaS2 nanoflowers were built by primary spherical nanoparticles with 5nm which prefer to grow along<112> direction. There were no obvious difference in UV-vis spectra between AgGaS2 nanoflower-like particles and colloids and the room temperature photoluminescence spectra of AgGaS2 colloids red-shifted 12 nm compared to that of AgGaS2 nanoflowers. The surface photovoltage (SPV) properties of AgGaS2 nanoflower powders were consistent with their UV absorption and their photovoltage response became stronger when an extra electric field increased which implies that AgGaS2 can absorb photons and separate electron- hole pairs in the built-in electric field. In the same reaction system, we can also obtained orthorhombic AgInS2 nanocrystals and AgInχGa1-χS2 (O≤x≤1) quaternary solid state serial nanocrystals.
(3) Solution-controlled synthesis of CulnSe2, CuGaSe2, CuInxGa1-χSe2 hexangular nanoplatelets. We first applied two-step and DMF solvothermal method to synthesize ternary or quaternary selenide hexangular nanoplatelets, which provided a new strategy to resolve selenic source with Vc as reduce regent. CulnSe2 hexangular nanoplatelets with two dimensions were tetragonal chalcopyrite structure and their size was about 200 nm. From the HRTEM and crystal structure analysis, it was proved that CulnSe2 hexangular nanoplatelets with monocrystalline structure originated the preferentially growth along<112> and<001> two directions and the growth of <101> direction was limited. Moreover, the formation and/or crystal phase of monodisperse CulnSe2 hexangular nanoplatelets were strongly influenced by many external factors, e.g., pre-treating time, PVP quantum, Vc quantum, temperature, reaction time, etc. The 7days stability analysis of CulnSe2 hexangular nanoplatelets dispersed in alcohol proved that there was no change from transmission light and backscattering light. In other words, there was no phenomenon such as precipitate, emulsification, flocculation, condense, phase seperation, edc. in the 7days and could be a good "ink" for screen painting that was applied to make soft film solar cell. In the same reaction system, we can also obtained CuGaSe2 hexangular nanoplatelets. By adjusting the proportion of In/Ga, CuInχGa1-χSe2 quaternary selenide hexangular nanoplatelets also could be obtained. UV-vis absorption spectra of CuInχGa1-χSe2 (0≤x≤1) serial nanocrystals ranged 900～1300 nm and their Eg value ranged 0.95-1.46. The two-step method was widespread application for synthesis of multinary chalcogenidometalates. Spherical CuInSe2 in nano scale was obtained in the reaction system of CH3CH2OH-HOCH2CH2NH2. Using of CuInχGa1-χSe2 as absorption material, Ag/CdS/CuInχGa1-χSe2/FTO solar cell has been completed.
(1) ZnGa2O4等多元氧化物及其固溶体纳米晶的控制合成、形成机理和光学性质研究。通过苯甲醚溶剂热法制备了尺寸约为20 nm的缺角立方状ZnGa2O4纳米晶,该纳米晶在435nm处有较强的蓝光发射。通过控制前驱物中锌的量可以得到立方相γ-Ga2O3和立方相ZnGa2O4的固熔体系列纳米晶,即ZnχGa2O3+χ(0≤χ≤1)。它们的晶格参数基本符合维加定律,带隙宽可以在4.43到3.70 eV间调控。同时其发光波长也可在395到435 nm间进行调控。时间历程分析表明：首先生成介稳态的γ-Ga203,随后生成ZnO并逐渐离解出的锌离子扩散进γ-Ga2O3晶格中得到ZnχGa2O3+χ(0≤χ≤1)固熔体系列纳米晶,最终得到ZnGa2O4纳米晶。在这个Zn2+逐渐扩散到晶格的反应过程中,氧缺陷也逐渐被淬灭,使畸变的Ga-O八面体逐渐成为Ga-O正八面体得到发纯正蓝光的ZnGa2O4纳米晶。我们进一步在水热体系中,以十二烷基苯磺酸钠作表面活性剂成功制备了正八面体形的ZnGa2O4和ZnAl2O4纳米晶。并以发蓝光的ZnGa2O4八面体纳米晶为基底材料,实现了Mn2+和Cr3+的掺杂,分别得到到绿光和红光的荧光材料,实现了三原色纳米荧光材料的合成。
(2)AgGaS2等三元及四元硫化物纳米晶的合成及其光学性质研究。以一些简单无机盐为前驱物,油胺为包覆剂,以环己烷和长链醇的混合溶剂作为反应介质,控制合成了尺寸形貌可控的3D纳米花和胶体状AgGaS2纳米材料。研究表明醇的浓度、醇的碳链长度、油胺的浓度等因素都能导致AgGaS2纳米晶形貌的转变。如果醇的浓度较大,碳链长度很长或油胺的浓度较大,可以充分保护AgGaS2而得到胶状粒子。反之则得到AgGaS2纳米花。通过对AgGaS2纳米花进行高分辨透射电镜和结构分析,AgGaS2纳米花的基本组装单元约为5 nm的小粒子,沿<112>方向取向生长组装成3D纳米结构。AgGaS2纳米花和胶体粒子的室温紫外可见吸收光谱基本相同,而胶体粒子的发光光谱红移了12 nm。AgGaS2纳米花的表面光电压性质与紫外吸收比较吻合,且光电压响应随着外加电场增强而增强,表明在自建电场内AgGaS2能够吸收光子和分离电子-空穴对。在同样的反应体系中,我们也得到了高温正交相的AgInS2纳米晶以及AgInχGa1-χS2(0≤x≤1)四元固熔体纳米晶。
(3) CulnSe2, CuGaSe2, CuInχGa1-χSe2纳米六角片的液相控制合成及生成机理。首次采用两步法,以Vc为还原剂提出了一种全新的解决硒源的方法。并以一些简单的无机盐为前驱体、PVP为包覆剂、DMF为溶剂,通过简单的溶剂热法得到了三元或四元硒化物的纳米六角片。二维CulnSe2六角纳米片为四方晶相的黄铜矿结构,其尺寸约为200 nm,为p型半导体。通过对CulnSe2进行高分辨透射电镜分析,证明所得的三元硒化物为单晶结构,且二维的结构是由于{112}和{001}面的快速生长导致的。进一步的对比实验表明,CulnSe2纳米片的形成和形貌受到多种因素的影响：硒粉的前处理时间、PVP的量、Vc的量、反应时间、温度等。CulnSe2纳米片的乙醇分散性及稳定性测试表明CulnSe2的乙醇均匀分散体系不管是透射光还是背散射光经过7天的测试,此分散体系没有发生沉淀、乳化、絮凝、凝结、分相等现象,能作为丝网印刷的“墨水”,可用于柔性薄膜太阳能电池的吸收材料。同样的体系中也得到CuGaSe2六方纳米片；控制前驱物中In/Ga的比例得到CuInχGa1-χSe2四元纳米硒化物。CuInχGa1-χSe2的紫外吸收光谱图都是吸收介于900～1300 nm之间的连续谱线,它们的带隙宽Eg介于0.95～1.46之间。此两步法在合成硫属化合物方面具有一定的普适性：在乙醇-乙醇胺体系中采用两步法同样可以得到CuInSe2纳米球。利用CuInχGa1-χSe2作为吸收材料制备了Ag/CdS/CuInχGa1-χSe2/FTO结构的太阳能电池。
Comparing with binary compounds, multinary oxygen-group compounds exhibit useful physical and chemical properties such as optical, electronic, magnetic, mechanical, and piezoelectricity properties. Therefore, the synthesis of multinary oxygen-group compounds is becoming an active area of solid state chemistry. Solvothermal reaction is motivated by their potential to provide an access to multinary oxygen-group compounds in nanoscale with obvious quantum confinement effect and size- and/or shape-dependent properties. However, the synthesis such of multiple component nanocrystals has been limited by the reactivities of the precursors and the ease of phase separation of the alloyed constituents. In other words, if the reaction activities of two metal precursors differ from each other, a separated nucleus will be generated and grow into heterostructures or even two compounds, especially to form the less solubility of transition metal oxide, sulfide or selenide, which make the number of known synthetic multinary oxygen-group compounds with metal ions is limited. Thus, structure and/or shape controlled synthesis of multinary oxygen-group semiconductor nanomaterials will not bring the theoretically meanings, but also the application significance which extended the semiconductor materials. In this thesis, we have attempted and extended to synthesis multinary oxygen-group semiconductor nanomaterials with new chemical synthetic method and thought, which gathered experience for controlled synthesis of multinary oxygen-group semiconductor nanomaterials. Detailed rerearch contents are summarized as following:
(1) Controlled synthesis and synthesis mechanism of ZnGa2O4 nanocrystals and their research of optical properties. Truncated cubic shape of ZnGa2O4 nanocrystals with 20 nm have been synthesized via a simple anisole solvothermal method. The as-prepared ZnGa2O4 nanocrystals emitted strong blue light at 435 nm. By adjusting zinc quantum of precursors, solid solutions serial nanocrystals of cubicγ-Ga2O3 and cubic ZnGa2O4 that also be expressed to ZnχGa2O3+χ(0≤χ≤1) could be obtained. The lattice parameters and band gap Eg of ZnχGa2O3+χ(0≤χ≤1) serial nanocrystals changed linearly which consistent with Vegard's law basically. The Eg of ZnχGa2O3+χ(0≤χ≤1) serial nanocrystals ranged from 4.43 to 3.70 eV and could be tuned their emission spectra from 395 to 435nm. The formation of ZnχGa2O3+χ(0<χ<1) and ZnGa2O4 resulted from Zn2+ (came from dissociated amorphous ZnO) diffusing into theγ-Ga2O3 nanocrystal lattice structure. In the process of Zn2+ diffusing into nanocrystal lattice, the oxygen vacancies were gradually extinguished making distorted Ga-O octahedron transforming to regular one which is the self-activated blue emission site. In the hydrothermal reaction system, ZnGa2O4 and ZnAl2O4 nanocrystals with regular octahedron were obtained. With the blue fluorescent material ZnGa2O4 regular octahedrona nanocrystals as basilar material doped with Mn2+ and Cr3+, we successfully gained green and red fluorescent respectively and achieved the three primary colors.
(2) Shape-Controlled synthesis of AgGaS2 nanocrystals and their research of optical properties. Nearly monodispersed AgGaS2 nanocrystals with flower-like or colloidal shape were synthesized in a simple solution system, in which a mixture of 1-octyl alcohol and cyclohexane was used as reactive medium and oleylamine as surfactant. The shape and size of these as-prepared nanocrystals could be tuned effectively by controlling the reaction conditions, such as the ratio of octanol to cyclohexane, the length of carbon chain of fatty alcohol and the concentration of oleylamine. The results showed that fatty alcohol play key factor for the shape and size transformation of AgGaS2 from 3D nanoflowers (50 nm) to colloids (10-20 nm), and a plausible shape evolution and crystal growth mechanism have been suggested for the formation of 3D nanoflowers and colloids. The simple reaction system might provide a new approach to controlled synthesis ternary nanomaterials and understood the reaction mechanism along with the growth kinetics of nanocrystals. Oleylamine combined with alcohol to absorb the AgGaS2 nanocrystals which could reduce the total surface energy and protect the nanocrystals. From the HRTRM and crystal structure analysis, monodispersed AgGaS2 nanoflowers were built by primary spherical nanoparticles with 5nm which prefer to grow along<112> direction. There were no obvious difference in UV-vis spectra between AgGaS2 nanoflower-like particles and colloids and the room temperature photoluminescence spectra of AgGaS2 colloids red-shifted 12 nm compared to that of AgGaS2 nanoflowers. The surface photovoltage (SPV) properties of AgGaS2 nanoflower powders were consistent with their UV absorption and their photovoltage response became stronger when an extra electric field increased which implies that AgGaS2 can absorb photons and separate electron- hole pairs in the built-in electric field. In the same reaction system, we can also obtained orthorhombic AgInS2 nanocrystals and AgInχGa1-χS2 (O≤x≤1) quaternary solid state serial nanocrystals.
(3) Solution-controlled synthesis of CulnSe2, CuGaSe2, CuInxGa1-χSe2 hexangular nanoplatelets. We first applied two-step and DMF solvothermal method to synthesize ternary or quaternary selenide hexangular nanoplatelets, which provided a new strategy to resolve selenic source with Vc as reduce regent. CulnSe2 hexangular nanoplatelets with two dimensions were tetragonal chalcopyrite structure and their size was about 200 nm. From the HRTEM and crystal structure analysis, it was proved that CulnSe2 hexangular nanoplatelets with monocrystalline structure originated the preferentially growth along<112> and<001> two directions and the growth of <101> direction was limited. Moreover, the formation and/or crystal phase of monodisperse CulnSe2 hexangular nanoplatelets were strongly influenced by many external factors, e.g., pre-treating time, PVP quantum, Vc quantum, temperature, reaction time, etc. The 7days stability analysis of CulnSe2 hexangular nanoplatelets dispersed in alcohol proved that there was no change from transmission light and backscattering light. In other words, there was no phenomenon such as precipitate, emulsification, flocculation, condense, phase seperation, edc. in the 7days and could be a good "ink" for screen painting that was applied to make soft film solar cell. In the same reaction system, we can also obtained CuGaSe2 hexangular nanoplatelets. By adjusting the proportion of In/Ga, CuInχGa1-χSe2 quaternary selenide hexangular nanoplatelets also could be obtained. UV-vis absorption spectra of CuInχGa1-χSe2 (0≤x≤1) serial nanocrystals ranged 900～1300 nm and their Eg value ranged 0.95-1.46. The two-step method was widespread application for synthesis of multinary chalcogenidometalates. Spherical CuInSe2 in nano scale was obtained in the reaction system of CH3CH2OH-HOCH2CH2NH2. Using of CuInχGa1-χSe2 as absorption material, Ag/CdS/CuInχGa1-χSe2/FTO solar cell has been completed.
引文
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