低维CdS、ZnS和ZnO等纳米材料的固相合成及表征
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摘要
金属氧化物和硫化物等纳米材料具有独特的物理、化学性质,探索其制备过程、反应机制,对深入研究其尺寸及物性关联、最终设计功能材料具有重要意义。传统合成往往是在溶液或气相中进行,由于诸多缺点受到限制。
本文从简单合成、绿色高效要求出发,选择金属氧化物和硫化物等低维纳米材料为研究对象,以固相反应为基础,通过改变反应温度、加热方式等因素,用低温固相、熔盐和添加剂与微波辅助等方法进行了合成研究,详细探索了合成反应机理,对产物结构、形貌和光、电等性能进行了表征测试。
在系统研究不同反应温度、不同添加剂条件下低温固相反应合成硫化镉纳米粒子的基础上,发现粒子尺寸、产物晶型和紫外-可见吸收性能的变化,推测了硫化镉纳米粒子的尺寸和晶型控制机理;研究了对苯二甲酸存在条件下合成硫化镉纳米粒子的反应,发现对苯二甲酸以特殊复合物的形式有效地阻止了产物粒子的长大;以氯化胆碱为熔盐通过特殊的低温反应获得了六方CdS纳米粒子;研究了微波辅助合成CdS纳米粒子的反应,发现微波辐射时间和方式影响着粒子的尺寸和晶型。针对不同合成反应的比较,发现低温固相反应合成硫化镉纳米粒子在合成方面存在较大优势。在系统研究不同反应温度、不同反应时间、不同添加剂条件下低温固相反应合成硫化锌纳米粒子的基础上,发现粒子尺寸和产物紫外-可见吸收性能的变化,发现十二烷基胺以不同的反应方式在较高温度下保持着粒子的较小粒径,推测了其粒子的尺寸控制机理;研究了NaCl存在下熔盐合成六棱柱状ZnS纳米材料的形貌与紫外-可见吸收性能和发光性能,发现原始反应物、不同熔盐、添加剂等因素均控制着产物的形貌。针对不同合成反应的比较,发现对于不同形貌和性能的硫化锌纳米粒子可选择合适的合成方法。
在变换熔盐种类及原始反应物的条件下,研究了熔盐合成不同形貌ZnO纳米材料的反应,发现产物的形貌对熔盐和反应物的依赖性;研究了熔盐来源对ZnO纳米粒子尺寸的影响,发现外加熔盐为粒子的长大提供了合适的环境;研究了ZnO一维纳米材料的微波辐射和添加剂PEG400的辅助合成反应,发现微波辐射有利于纳米棒的形成,添加剂PEG400可以控制产物某些晶面的生长,从而获得不同形貌和发光性能的产物。
在NaCl-KCl混合熔盐存在条件下,研究了合成Co_3O_4纳米棒的反应,结果表明熔盐阴离子Cl-促进了纳米棒的生成,发现不同尺寸的钴粒子前驱体、不同熔盐控制着不同形貌产物的生成;通过不同添加剂、不同熔盐的共同作用又得到了具有较好电容性能的Co_3O_4纳米粒子。两种方法具有不同的优点,为不同形貌四氧化三钴纳米材料的合成提供了不同选择。
研究了微波辐射和添加剂辅助合成金属镍和氧化镍的反应,发现反应温度、加热时间、前驱体与添加剂的混合方式等因素影响着最终产物的类型和尺寸,产物具有较好的循环伏安特性和充放电性能。
在上面研究基础上,对合成产物的种类进行扩展。研究了金属Ag单质和金属配位化合物PbC_2O_4的简单快速合成;研究了微波辐射时间和方式对产物金属铜形成过程的影响,以及产物的紫外-可见光吸收性能。
针对金属氧化物和金属硫化物等纳米材料的这些研究是对固相反应的较为深入地发展,可以为不同形貌及性能纳米材料的获得和大批量生产及应用提供一定的参考,具有较重要的学术价值和广阔的应用前景。
Nanostructured metal oxides and sulfides have exhibited unique physical chemical properties. Preparing and investigating their general formation mechanism may be a solution to the precise control of their sizes and properties. Conventional synthesis is always performed in solution or gas, and it is being excluded due to many problems more and more.
In this dissertation, according to command of energy-economical and green effective production, different sulfides and oxides have been synthesized and characterized by low-temperature solid-state, molten salt and microwave solid-state in the presence of addition, respectively. Their formation mechanism has been explored, and their optical and electrical properties have been also characterized.
CdS nanomaterials had been synthesized by low-temperature solid-state reaction in the condition of different reaction temperature, different time and different additions, and UV-vis properties depend on diameter and crystal pattern of products. Crystal pattern and diameter of CdS nanoparticles can be controlled by different additions and reaction temperature, and their formation mechanic has been explored; Diameter of CdS nanoparticles can also control by adding template terephthalic acid in the reaction; Hexagonal CdS nanoparticles are synthesized by using choline chloride as molten salt under low reaction temperature; CdS nanoparticles had also been synthesized by microwave-assisted solid-state reaction, and radiation time and radiation pattern have some effect on diameter and crystal pattern of products; On the contrast, CdS nanoparticles synthesized by low-temperature solid-state reaction got best qulity.
Diameter of ZnS nanoparticles is affected by reaction temperature, reaction time and additions, and ZnS nanoparticles with small diameter can be obtained by using dodecylamine as addition; ZnS hexagonal prism can be synthesized simply by using NaCl as molten salt, and the effects of reactants, molten-salts and additions on product morphologies have been studied; On the contrast, different methods can be chosed to obtain ZnS with different morphologies and different properties.
In the condition of changing molten salts and reactants, ZnO with different morphologies can be obtained, and product morphologies depend on molten-salt and reactants; The effect of molten-satle on ZnO nanoparticles had studied, and results show that additional molten-satle provided a favorable environment for growth of ZnO particles; In the presence of PEG400, ZnO nanorods had been synthesized, and studies show that microwave radiation can lead to fast synthesis of ZnO nanorods and PEG400 can confine the growth rate in some directions. Thus, ZnO products with different morphologies and different properties had been obtained.
Co_3O_4 nanorods had been obtained by employing Co nanoparticles as precursor and using NaCl-KCl molten salt, results show that Cl- leads to formation of Co_3O_4 nanorods, and different precursors and different molten-salts have great effects on products morphologies; Co_3O_4 nanoparticles with a fine electrochemical stability had been synthesized in the presence of addition and molten-salt. Different methods can be chosed to obtain Co_3O_4 with different morphologies.
Metal Ni and electrode materials NiO have been synthesize through microwave-assisted and addition-assisted reactions, and studies show that reaction temperature, reaction time and mixed state between precursor and addition all had important effects on formation and sizes of the products.
In addition, metal Ag and metal coordinate compound PbC_2O_4 had been synthesized by low-temperature solid-state reaction. Metal Cu has been also obtained by microwave radiation in the presence of PEG400, and radiation time has an important effect on formation of Cu nanoparticles.
The studies about metal oxides and sulfides are a new development of solid-state reaction, and it can provide useful reference for synthesis of nanomaterials with different morphologies and different properties, and large-scale produce and application of nanomaterials, and it may have an important research value and wide application future.
本文从简单合成、绿色高效要求出发,选择金属氧化物和硫化物等低维纳米材料为研究对象,以固相反应为基础,通过改变反应温度、加热方式等因素,用低温固相、熔盐和添加剂与微波辅助等方法进行了合成研究,详细探索了合成反应机理,对产物结构、形貌和光、电等性能进行了表征测试。
在系统研究不同反应温度、不同添加剂条件下低温固相反应合成硫化镉纳米粒子的基础上,发现粒子尺寸、产物晶型和紫外-可见吸收性能的变化,推测了硫化镉纳米粒子的尺寸和晶型控制机理;研究了对苯二甲酸存在条件下合成硫化镉纳米粒子的反应,发现对苯二甲酸以特殊复合物的形式有效地阻止了产物粒子的长大;以氯化胆碱为熔盐通过特殊的低温反应获得了六方CdS纳米粒子;研究了微波辅助合成CdS纳米粒子的反应,发现微波辐射时间和方式影响着粒子的尺寸和晶型。针对不同合成反应的比较,发现低温固相反应合成硫化镉纳米粒子在合成方面存在较大优势。在系统研究不同反应温度、不同反应时间、不同添加剂条件下低温固相反应合成硫化锌纳米粒子的基础上,发现粒子尺寸和产物紫外-可见吸收性能的变化,发现十二烷基胺以不同的反应方式在较高温度下保持着粒子的较小粒径,推测了其粒子的尺寸控制机理;研究了NaCl存在下熔盐合成六棱柱状ZnS纳米材料的形貌与紫外-可见吸收性能和发光性能,发现原始反应物、不同熔盐、添加剂等因素均控制着产物的形貌。针对不同合成反应的比较,发现对于不同形貌和性能的硫化锌纳米粒子可选择合适的合成方法。
在变换熔盐种类及原始反应物的条件下,研究了熔盐合成不同形貌ZnO纳米材料的反应,发现产物的形貌对熔盐和反应物的依赖性;研究了熔盐来源对ZnO纳米粒子尺寸的影响,发现外加熔盐为粒子的长大提供了合适的环境;研究了ZnO一维纳米材料的微波辐射和添加剂PEG400的辅助合成反应,发现微波辐射有利于纳米棒的形成,添加剂PEG400可以控制产物某些晶面的生长,从而获得不同形貌和发光性能的产物。
在NaCl-KCl混合熔盐存在条件下,研究了合成Co_3O_4纳米棒的反应,结果表明熔盐阴离子Cl-促进了纳米棒的生成,发现不同尺寸的钴粒子前驱体、不同熔盐控制着不同形貌产物的生成;通过不同添加剂、不同熔盐的共同作用又得到了具有较好电容性能的Co_3O_4纳米粒子。两种方法具有不同的优点,为不同形貌四氧化三钴纳米材料的合成提供了不同选择。
研究了微波辐射和添加剂辅助合成金属镍和氧化镍的反应,发现反应温度、加热时间、前驱体与添加剂的混合方式等因素影响着最终产物的类型和尺寸,产物具有较好的循环伏安特性和充放电性能。
在上面研究基础上,对合成产物的种类进行扩展。研究了金属Ag单质和金属配位化合物PbC_2O_4的简单快速合成;研究了微波辐射时间和方式对产物金属铜形成过程的影响,以及产物的紫外-可见光吸收性能。
针对金属氧化物和金属硫化物等纳米材料的这些研究是对固相反应的较为深入地发展,可以为不同形貌及性能纳米材料的获得和大批量生产及应用提供一定的参考,具有较重要的学术价值和广阔的应用前景。
Nanostructured metal oxides and sulfides have exhibited unique physical chemical properties. Preparing and investigating their general formation mechanism may be a solution to the precise control of their sizes and properties. Conventional synthesis is always performed in solution or gas, and it is being excluded due to many problems more and more.
In this dissertation, according to command of energy-economical and green effective production, different sulfides and oxides have been synthesized and characterized by low-temperature solid-state, molten salt and microwave solid-state in the presence of addition, respectively. Their formation mechanism has been explored, and their optical and electrical properties have been also characterized.
CdS nanomaterials had been synthesized by low-temperature solid-state reaction in the condition of different reaction temperature, different time and different additions, and UV-vis properties depend on diameter and crystal pattern of products. Crystal pattern and diameter of CdS nanoparticles can be controlled by different additions and reaction temperature, and their formation mechanic has been explored; Diameter of CdS nanoparticles can also control by adding template terephthalic acid in the reaction; Hexagonal CdS nanoparticles are synthesized by using choline chloride as molten salt under low reaction temperature; CdS nanoparticles had also been synthesized by microwave-assisted solid-state reaction, and radiation time and radiation pattern have some effect on diameter and crystal pattern of products; On the contrast, CdS nanoparticles synthesized by low-temperature solid-state reaction got best qulity.
Diameter of ZnS nanoparticles is affected by reaction temperature, reaction time and additions, and ZnS nanoparticles with small diameter can be obtained by using dodecylamine as addition; ZnS hexagonal prism can be synthesized simply by using NaCl as molten salt, and the effects of reactants, molten-salts and additions on product morphologies have been studied; On the contrast, different methods can be chosed to obtain ZnS with different morphologies and different properties.
In the condition of changing molten salts and reactants, ZnO with different morphologies can be obtained, and product morphologies depend on molten-salt and reactants; The effect of molten-satle on ZnO nanoparticles had studied, and results show that additional molten-satle provided a favorable environment for growth of ZnO particles; In the presence of PEG400, ZnO nanorods had been synthesized, and studies show that microwave radiation can lead to fast synthesis of ZnO nanorods and PEG400 can confine the growth rate in some directions. Thus, ZnO products with different morphologies and different properties had been obtained.
Co_3O_4 nanorods had been obtained by employing Co nanoparticles as precursor and using NaCl-KCl molten salt, results show that Cl- leads to formation of Co_3O_4 nanorods, and different precursors and different molten-salts have great effects on products morphologies; Co_3O_4 nanoparticles with a fine electrochemical stability had been synthesized in the presence of addition and molten-salt. Different methods can be chosed to obtain Co_3O_4 with different morphologies.
Metal Ni and electrode materials NiO have been synthesize through microwave-assisted and addition-assisted reactions, and studies show that reaction temperature, reaction time and mixed state between precursor and addition all had important effects on formation and sizes of the products.
In addition, metal Ag and metal coordinate compound PbC_2O_4 had been synthesized by low-temperature solid-state reaction. Metal Cu has been also obtained by microwave radiation in the presence of PEG400, and radiation time has an important effect on formation of Cu nanoparticles.
The studies about metal oxides and sulfides are a new development of solid-state reaction, and it can provide useful reference for synthesis of nanomaterials with different morphologies and different properties, and large-scale produce and application of nanomaterials, and it may have an important research value and wide application future.
引文
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