SnS_2（SnO_2）多级微纳结构的合成及性能
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摘要
SnS_2和SnO_2是重要的锡基氧族化合物，具有优良的光学、催化、电化学、磁学及气敏等性质，在气敏传感器、电阻器、光电探测器、光导材料、发光材料、光催化剂、锂离子电池和太阳能电池等方面具有广泛应前景。多级无机功能微纳米材料综合了物质本征效应、纳米尺度效应和组合效应所产生的多功能性使其成为纳米材料研究领域的热点之一，并在储能、催化、水处理、能量转换等领域展现出巨大的优势。因此，开发简单、可靠的软化学法控制合成多级微纳结构、探索其新的功能将具有重要的理论和实际意义。本论文遵循以设计合成为基础，功能为导向的基本理念。通过反应体系的选择和反应条件的调控，设计合成了一系列SnS_2(SnO_2)及其复合物多级微纳结构，探究了制备多级微纳结构的关键问题；并对这些多级微纳结构的电化学储锂、光学和气敏等性能及其构效关系进行了较为系统和全面的研究。具体内容包括：
(1) L-半胱氨酸辅助水热法合成SnS_2多级微纳结构及性能研究。通过简单地调节L-半胱氨酸的浓度成功合成了三种不同结构的SnS_2多级微球。研究表明反应初期体系中S~(2-)离子的浓度是影响SnS_2多级微纳结构的关键因素，并对SnS_2多级微纳结构的化学成分、结晶性、组装单元、组装形式、比表面积和孔隙结构等具有重要的影响。同时，SnS_2多级微纳结构基本性质也极大地影响了材料的电化学储锂性能、光吸收、光电响应和光降解性能。
(2) SnS_2插层化合物的水热合成及性能研究。采用水热法合成了以CTAB、SDBS、PEG和PVP等为客体，SnS_2为主体的插层化合物。插层化合物的形成是反应体系趋于热力学稳定的过程，同时温度、时间、S~(2-)的释放速度、酸度、插层剂的浓度和分子大小对插层化合物的形成具有重要的影响。进一步采用超声法，通过超声剥离PEG-SnS_2插层化合物，获得具有很强荧光性能的PEG-SnS_2插层化合物量子点，其量子产率最高可达65%。而且PEG的分子量和前驱体的浓度对量子产率和激发波长有十分明显的影响。
(3) SnO_xS_(2-x)/石墨烯复合物的超声法合成及储锂性能。采用超声法成功制备了两种锡基氧化物与硫化物不同比例的SnO_xS_(2-x)/石墨烯的复合物（SnO_(0.6)S_(1.4)/GNS和SnOS/GNS）。由于复合物以SnO_2与SnS_2的微观混合相（S掺杂SnO_2和O掺杂SnS_2）替代纯相的SnO_2或SnS_2与石墨烯复合，电化学性能表明两种复合物都能实现从SnO_2（SnS_2）到锡单质和氧化锂（硫化锂）、最后到锡锂合金电化学储锂过程的全程可逆，并且复合物中SnO_2与SnS_2的比例对于电化学过程的可逆性和稳定性有决定性的影响，如SnOS/GNS复合物具有优良的循环稳定性（40次循环后仍有1066mAh g-1）和倍率性能（2Ag-1时比容量为402mAh g-1）。
(4) SnO_2多级微纳结构及其石墨烯复合物的水热合成和性能。采用硫代乙醇酸辅助水热法成功合成了SnO_2空心微球，并通过碱源的调控合成了SnO_2单晶纳米粒子、纳米短棒和海胆状多级微纳结构，其中基于SnO_2空心微球和海胆状多级微纳结构的气敏元件对于乙醇具有很高的响应，尤其是海胆状结构的SnO_2对100ppm乙醇的灵敏度达到73.7。成功制备了SnO_2纳米棒阵列/石墨烯复合物，这一特殊结构赋予复合物优良的电化学储锂性能（0.2Ag-1循环63次后仍有1154.1mAh g-1的比容量）。
SnS_2and SnO_2are important tin based componds with excellent optical, catalytic,magnetic and gas sensitive properties and have wide applications in gas sensor,resistor, photodevice, photoconductor, luminescent materials, photocatalyst, lithiumion batteries, etc. Recently, inorganic fuctional materials with hierarchicalmicro-/nanostructures have attracted intensive interest for the structure joined theintrinsic effect of bulk materials with the nano-effect of nanomaterials and producedmany combinatory effects. Hierarchical micro-/nanostructures have been showattractive superiority in energy conversion, such as solar cells and photocatalytichydrogen generation, energy storage, such as lithium ion batteries and supercapacitor,sensor, catalysis, water treatment and so on. A solution-phase chemical method wasone of the most promising routes in these reports, due to its low cost and potentialadvantage for large-scale production. Exploration of reasonable synthetic methods forcontrolled construction of hierarchical micro-/nanostructures of tin basedchalcogenide via a chemical self-assembly route is still an intensive and hot researchtopic. In this thesis, we attempted to synthesize hierarchical SnS_2(SnO_2)micro-/nanostructures by new chemical method. The lithium strage, optical and gassensitivity properties of the obtained structures as well as the ralations between theirstructures and performances have been studied. Detailed rerearch contents aresummarized as following:
(1) Controlled synthesis and applications of hierarchical SnS_2micro/nano-structures.
Different hierarchical SnS_2micro-/nanostructures were successfully synthesizedthrough an one-pot hydrothermal method by controlling the ratio of SnCl4andL-cysteine. The concentration of S~(2-)in the early stage is very important to thesysnthesis of hierarchical SnS_2micro/nano-structures. The chemical composition,crystalline property, building blocks, assembling format and porous structure ofthe hierarchical SnS_2micro/nano-structures can be affected by the concentration of L-cys. And they have great effects on the lithium storage, optical, photoelectricresponse, photocatalysis and adsorption properties of these hierarchical SnS_2structures.
(2) Hydrothermal synthesis and optical properties of SnS_2intercalationcompounds.
It is general, facilate and economic that introducing hydrothermal method to thedirect synthesis of SnS_2intercalation compounds. The intercalated objects can besurfactants or polymers, such as CTAB, SDBS, PVP and PEG. The formation ofSnS_2intercalation compounds can be controlled by thermodynamics and affectedby the molecue weight and concentration of intercalated objects, reactiontemperature, reaction time and the release rate of S~(2-). The PEG intercalated SnS_2can be easily exfoliated to single layer of PEG-SnS_2QDs by solvent underultrasonication. These QDs have strong fluorescence with a quantum yield of65%and can be affected by the molecule weight of PEG and the concentrationsof precursors.
(3) Synthesis and lithium storage properties of SnO_xS_(2-x)/GNS composites.
Two types of composite with different ratios between SnO_2and SnS_2(SnO_(0.6)S_(1.4)/GNS and SnOS/GNS) have been synthesized by ultrasonication.Electrochemical measurements show both composite can realize the fullyreversible lithium storage of tin based chalcogenide. The key reasons may beattribute to the GNS composite and mixed phase of SnO_2and SnS_2, which dopedwith each other in the nano-level. The ratios between SnO_2and SnS_2can greatlyaffect the lithium storage performances and SnOS/GNS exhibited respectivelygood cycling performance (0.2A g-1,1066mAh g-1after40cycles) and ratecapability (2A g-1,402mAh g-1).
(4) Hydrothermal synthesis of hierarchical SnO_2micro-/nanostructures.
Divers SnO_2structures, such as hollow microspheres, nanoparticles, nanorodsand urchin-like hierarchical micro-/nanostructures are synthesized though amercaptoacetic acid assisted hydrothermal method by controlling alkali types.Gas sensors based on hollow microspheres and urchin like structures haveextremely high sensitivity to alcohol, and the sensitivity of100ppm ethanol ofurchin like structures can reach to73.7. SnO_2nanorods array/GNS composite canbe synthesize by adding graphene oxide to the reaction system of urchin likestructures. And the composite show superior lithium storage properties (0.2A g-1,63cycles,1154.1mAh g-1). The high performance can put down to the layered porous structure of graphene nanosheets with in-situ growth SnO_2nanorodsarray。
(1) L-半胱氨酸辅助水热法合成SnS_2多级微纳结构及性能研究。通过简单地调节L-半胱氨酸的浓度成功合成了三种不同结构的SnS_2多级微球。研究表明反应初期体系中S~(2-)离子的浓度是影响SnS_2多级微纳结构的关键因素，并对SnS_2多级微纳结构的化学成分、结晶性、组装单元、组装形式、比表面积和孔隙结构等具有重要的影响。同时，SnS_2多级微纳结构基本性质也极大地影响了材料的电化学储锂性能、光吸收、光电响应和光降解性能。
(2) SnS_2插层化合物的水热合成及性能研究。采用水热法合成了以CTAB、SDBS、PEG和PVP等为客体，SnS_2为主体的插层化合物。插层化合物的形成是反应体系趋于热力学稳定的过程，同时温度、时间、S~(2-)的释放速度、酸度、插层剂的浓度和分子大小对插层化合物的形成具有重要的影响。进一步采用超声法，通过超声剥离PEG-SnS_2插层化合物，获得具有很强荧光性能的PEG-SnS_2插层化合物量子点，其量子产率最高可达65%。而且PEG的分子量和前驱体的浓度对量子产率和激发波长有十分明显的影响。
(3) SnO_xS_(2-x)/石墨烯复合物的超声法合成及储锂性能。采用超声法成功制备了两种锡基氧化物与硫化物不同比例的SnO_xS_(2-x)/石墨烯的复合物（SnO_(0.6)S_(1.4)/GNS和SnOS/GNS）。由于复合物以SnO_2与SnS_2的微观混合相（S掺杂SnO_2和O掺杂SnS_2）替代纯相的SnO_2或SnS_2与石墨烯复合，电化学性能表明两种复合物都能实现从SnO_2（SnS_2）到锡单质和氧化锂（硫化锂）、最后到锡锂合金电化学储锂过程的全程可逆，并且复合物中SnO_2与SnS_2的比例对于电化学过程的可逆性和稳定性有决定性的影响，如SnOS/GNS复合物具有优良的循环稳定性（40次循环后仍有1066mAh g-1）和倍率性能（2Ag-1时比容量为402mAh g-1）。
(4) SnO_2多级微纳结构及其石墨烯复合物的水热合成和性能。采用硫代乙醇酸辅助水热法成功合成了SnO_2空心微球，并通过碱源的调控合成了SnO_2单晶纳米粒子、纳米短棒和海胆状多级微纳结构，其中基于SnO_2空心微球和海胆状多级微纳结构的气敏元件对于乙醇具有很高的响应，尤其是海胆状结构的SnO_2对100ppm乙醇的灵敏度达到73.7。成功制备了SnO_2纳米棒阵列/石墨烯复合物，这一特殊结构赋予复合物优良的电化学储锂性能（0.2Ag-1循环63次后仍有1154.1mAh g-1的比容量）。
SnS_2and SnO_2are important tin based componds with excellent optical, catalytic,magnetic and gas sensitive properties and have wide applications in gas sensor,resistor, photodevice, photoconductor, luminescent materials, photocatalyst, lithiumion batteries, etc. Recently, inorganic fuctional materials with hierarchicalmicro-/nanostructures have attracted intensive interest for the structure joined theintrinsic effect of bulk materials with the nano-effect of nanomaterials and producedmany combinatory effects. Hierarchical micro-/nanostructures have been showattractive superiority in energy conversion, such as solar cells and photocatalytichydrogen generation, energy storage, such as lithium ion batteries and supercapacitor,sensor, catalysis, water treatment and so on. A solution-phase chemical method wasone of the most promising routes in these reports, due to its low cost and potentialadvantage for large-scale production. Exploration of reasonable synthetic methods forcontrolled construction of hierarchical micro-/nanostructures of tin basedchalcogenide via a chemical self-assembly route is still an intensive and hot researchtopic. In this thesis, we attempted to synthesize hierarchical SnS_2(SnO_2)micro-/nanostructures by new chemical method. The lithium strage, optical and gassensitivity properties of the obtained structures as well as the ralations between theirstructures and performances have been studied. Detailed rerearch contents aresummarized as following:
(1) Controlled synthesis and applications of hierarchical SnS_2micro/nano-structures.
Different hierarchical SnS_2micro-/nanostructures were successfully synthesizedthrough an one-pot hydrothermal method by controlling the ratio of SnCl4andL-cysteine. The concentration of S~(2-)in the early stage is very important to thesysnthesis of hierarchical SnS_2micro/nano-structures. The chemical composition,crystalline property, building blocks, assembling format and porous structure ofthe hierarchical SnS_2micro/nano-structures can be affected by the concentration of L-cys. And they have great effects on the lithium storage, optical, photoelectricresponse, photocatalysis and adsorption properties of these hierarchical SnS_2structures.
(2) Hydrothermal synthesis and optical properties of SnS_2intercalationcompounds.
It is general, facilate and economic that introducing hydrothermal method to thedirect synthesis of SnS_2intercalation compounds. The intercalated objects can besurfactants or polymers, such as CTAB, SDBS, PVP and PEG. The formation ofSnS_2intercalation compounds can be controlled by thermodynamics and affectedby the molecue weight and concentration of intercalated objects, reactiontemperature, reaction time and the release rate of S~(2-). The PEG intercalated SnS_2can be easily exfoliated to single layer of PEG-SnS_2QDs by solvent underultrasonication. These QDs have strong fluorescence with a quantum yield of65%and can be affected by the molecule weight of PEG and the concentrationsof precursors.
(3) Synthesis and lithium storage properties of SnO_xS_(2-x)/GNS composites.
Two types of composite with different ratios between SnO_2and SnS_2(SnO_(0.6)S_(1.4)/GNS and SnOS/GNS) have been synthesized by ultrasonication.Electrochemical measurements show both composite can realize the fullyreversible lithium storage of tin based chalcogenide. The key reasons may beattribute to the GNS composite and mixed phase of SnO_2and SnS_2, which dopedwith each other in the nano-level. The ratios between SnO_2and SnS_2can greatlyaffect the lithium storage performances and SnOS/GNS exhibited respectivelygood cycling performance (0.2A g-1,1066mAh g-1after40cycles) and ratecapability (2A g-1,402mAh g-1).
(4) Hydrothermal synthesis of hierarchical SnO_2micro-/nanostructures.
Divers SnO_2structures, such as hollow microspheres, nanoparticles, nanorodsand urchin-like hierarchical micro-/nanostructures are synthesized though amercaptoacetic acid assisted hydrothermal method by controlling alkali types.Gas sensors based on hollow microspheres and urchin like structures haveextremely high sensitivity to alcohol, and the sensitivity of100ppm ethanol ofurchin like structures can reach to73.7. SnO_2nanorods array/GNS composite canbe synthesize by adding graphene oxide to the reaction system of urchin likestructures. And the composite show superior lithium storage properties (0.2A g-1,63cycles,1154.1mAh g-1). The high performance can put down to the layered porous structure of graphene nanosheets with in-situ growth SnO_2nanorodsarray。
引文
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