第四周期过渡金属氧化物的结构控制合成研究
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摘要
第四周期过渡金属氧化物以其独特的物理化学性质在电化学储能、光电器件、催化等领域都发挥着举足轻重的作用。随着对材料科学的深入认识及纳米科技的蓬勃发展,人们越发意识到除了材料的元素组成,其结构要素如晶相结构、微纳结构形态对无机材料的功能性同样具有重要影响。材料的结构控制合成对于深入研究材料物性与结构的紧密关联、并最终实现按照人们的意愿控制合成具有预期结构从而能表现出优良性能的功能材料具有重要意义,已成为当今材料科学的研究热点。本论文以第四周期过渡金属氧化物这类具有重要技术应用背景的材料为研究对象,对化学合成中晶相结构、微纳结构形态的控制进行了系统的探索研究,同时还考察研究了这两种结构要素对材料的超级电容器储能性能及光学性质的影响。论文的主要内容包含以下三方面：
1.开展了镍基氧化物混合晶相结构、纳米片组装结构的控制合成研究。基于S042-诱导的晶相选择机制,实现了对包含α-Ni(OH)2与(3-Ni(OH)2双组分混合晶相结构的控制合成,超级电容器储能测试表明晶相组成对Ni(OH)2作为电极材料的性能具有重要影响,混合晶相结构由于具有更多的电化学活性位从而表现出优于单一相材料的储能性能；基于水热条件下α-Ni(OH)2向β-Ni(OH)2的晶相转化,实现了对包含α-Ni(OH)2、β-Ni(OH)2和α-Co(OH)2三组分混合晶相结构的控制合成,该多组分混合相镍基氧化物应用于超级电容器中表现出在大电流密度使用条件下的性能优势；基于低温热处理条件下α-Ni(OH)2/α-Co(OH)2纳米片组装结构前躯体向NiCo2O4的形貌保持转化,实现了对NiCo2O4纳米片组装结构的控制合成,化学沉淀合成前躯体过程中的超声振荡处理能抑制纳米片组装体的聚集生长,利于合成得到分散性良好的NiCo2O4纳米片组装结构粉体,从而作为超级电容器电极材料应用可获得较高的比容量。
2.开展了锌基氧化物中空纳米结构、大孔结构和纳米组装结构的控制合成研究。基于奥氏熟化排空生长机制,实现了对Zn02中空纳米结构的控制合成,并考察了中空纳米结构对Zn02紫外-可见吸收性能的影响及亚稳相Zn02的热稳定性；基于Zn02中空纳米结构前躯体在溶剂热条件下分解释放的O2作为气泡模板对大孔结构的构建机制,实现了对ZnO大孔结构的控制合成,气泡模板合成法省去了传统模板法常需要的模板移除过程,简化了合成工艺流程；基于两相界面限域发生的自组装过程,实现了对ZnO纳米棒逐级构建的多级组装结构以及ZnO纳米棒、纳米片阵列型组装结构的控制合成,丰富了纳米组装结构的控制合成方法。
3.开展了钛、锰基氧化物中空纳米结构、一维纳米结构的控制合成,以及二氧化钛多种晶相结构的选择性控制合成研究。基于配体对Ti06八面体基本结构单元连接方式的动力学调控作用,在高浓度溶胶前体的使用条件下实现了对TiO2板钛矿、锐钛矿不同晶相结构的选择性控制合成；基于配体调控促发的奥氏熟化排空生长方式,在低浓度溶胶前体的使用条件下实现了对锐钛矿TiO2中空纳米结构的控制合成,并将这一中空纳米结构的控制合成体系拓展应用于MoO2,考察了微纳结构对TiO2紫外-可见吸收性能的影响以及中空纳米结构MoO2电极的超级电容器及锂离子电池储能性能；基于自晶种生长机制,实现了对MnO2一维纳米结构的无模板控制合成,自晶种生长机制的提出丰富了MnO：一维纳米结构无模板生长机制的类型。
The fourth-period transition metal oxides have been widely applied in electrochemical energy storage, optoelectric devices, catalysis, and etc., owing to their unique physical and chemical properties. Benefiting from the tremendous development of material science and significant progress of nanotechnology achieved in the past decades, the key roles of structure factors (crystal phase, micro-/nano-structure) in determining the property of functional inorganic materials have been understood. Structure-controlled synthesis is accordingly of significance both for study on the structure-property relationships, and rational design of functional materials with prospective structures and thus exhibiting excellent functionality, which has become an intense topic in material science. In this dissertation, we studied on rational tuning of crystal phase, micro-/nano-structure of the fourth-period transition metal oxides that are technically important in multiple critical applications. Also the effect of above key structure factors on the supercapacitive performance and optical property of the transition metal oxide materials was investigated. The three main sections of this dissertation are summarized as follows.
1. Controlled synthesis of mixed-phase structured, nanosheet-assembly structured nickel-based oxides was studied. Based on the SO42--induced crystal phase selective mechanism, this study realized controlled synthesis of mixed-phase α,β-Ni(OH)2that contains both a-Ni(OH)2component and β-Ni(OH)2component. The electrochemical test revealed that the crystal phase structure affected significantly on the supercapacitive performance of Ni(OH)2electrode materials. The mixed-phase a, P-Ni(OH)2electrode was better than both α-Ni(OH)2and β-Ni(OH)2electrodes benefiting from its more electrochemical active sites when applied in supercapacitors; Based on the crystal phase evolution from a-Ni(OH)2to β-Ni(OH)2under hydrothermal conditions, this study realized controlled synthesis of a mixed-phase nickel-based oxide containing a-Ni(OH)2, β-Ni(OH)2and α-Co(OH)2three components, which exhibited notable performance advantage when charged/discharged at high rate in supercapacitor applications. Based on the shape-preserving conversion from a-Ni(OH)2/a-Co(OH)2nanosheet-assembly precursor to NiCo2O4under low temperature calcination conditions, this study realized the controlled synthesis of NiCo2O4nanosheet assemblies. The ultrasonication processing can prevent the severe aggregation of nanosheet assemblies during the chemical precipitation of precursor so that well-separated NiCo2O4powder particles were obtained, thus the NiCo2O4powder electrode materials can deliver high specific capacitance when applied in supercapacitors.
2. Controlled synthesis of hollow nanostructured, macroporous structured, and self-assembly nanostructured zinc-based oxides was studied. Based on the Ostwald ripening evacuation mechanism, this study realized controlled synthesis of ZnO2hollow nanostructures, and further investigated the significant effect of hollow nanostructure on the UV-Vis absorption property of ZnO2. and studied the thermal stability of ZnO2hollow nanostructures; Based on the bubble template functionality of O2that was generated by decomposition of hollow nanostructured ZnO2precursor under solvothermal treatment, this study realized controlled synthesis of ZnO macroporous nanostructures. Bubble template-directed synthesis avoided the template-elimination procedure that is commonly needed in conventional template synthesis, and thus simplified the synthesis process; Based on the self-assembly process occurred at the interphase area, this study realized controlled synthesis of ZnO multi-scale nano-assemblies that were constructed by ZnO nanorod building blocks via two-step assembly, and arrayed nano-assemblies that were constructed by ZnO nanorod or nanosheet building blocks. This work provided new routes to synthesis of nano-assemblies.
3. Controlled synthesis of hollow nanostructured, one-dimensional (1D) nanostructured titanium, manganese-based oxides, and selective crystallization of different TiO2polymorphs were studied. Based on the ligand-induced phase selective mechanism, this study realized selective crystallization of brookite and anatase microcrystals when high-concentration sol precursor was employed; When low-concentration sol precursor was employed, this study realized controlled synthesis of anatase TiO2hollow nanostructures based on the ligand-induced Ostwald ripening evacuation mechanism. This hollowing route can also be extended to synthesis of MoO2hollow nanostructures. The effect of micro-/nano-structure on the UV-Vis absorption property of TiO2, and the electrochemical energy storage performance of MoO2hollow nanostructures applied in both lithium-ion batteries and supercapacitors were further studied; Based on the self-seeding growth mechanism, this study realized controlled synthesis of1D MnO2nanostructures. This novel growth mechanism provided new insight into the template-free growth of transition metal oxide1D nanostructures.
1.开展了镍基氧化物混合晶相结构、纳米片组装结构的控制合成研究。基于S042-诱导的晶相选择机制,实现了对包含α-Ni(OH)2与(3-Ni(OH)2双组分混合晶相结构的控制合成,超级电容器储能测试表明晶相组成对Ni(OH)2作为电极材料的性能具有重要影响,混合晶相结构由于具有更多的电化学活性位从而表现出优于单一相材料的储能性能；基于水热条件下α-Ni(OH)2向β-Ni(OH)2的晶相转化,实现了对包含α-Ni(OH)2、β-Ni(OH)2和α-Co(OH)2三组分混合晶相结构的控制合成,该多组分混合相镍基氧化物应用于超级电容器中表现出在大电流密度使用条件下的性能优势；基于低温热处理条件下α-Ni(OH)2/α-Co(OH)2纳米片组装结构前躯体向NiCo2O4的形貌保持转化,实现了对NiCo2O4纳米片组装结构的控制合成,化学沉淀合成前躯体过程中的超声振荡处理能抑制纳米片组装体的聚集生长,利于合成得到分散性良好的NiCo2O4纳米片组装结构粉体,从而作为超级电容器电极材料应用可获得较高的比容量。
2.开展了锌基氧化物中空纳米结构、大孔结构和纳米组装结构的控制合成研究。基于奥氏熟化排空生长机制,实现了对Zn02中空纳米结构的控制合成,并考察了中空纳米结构对Zn02紫外-可见吸收性能的影响及亚稳相Zn02的热稳定性；基于Zn02中空纳米结构前躯体在溶剂热条件下分解释放的O2作为气泡模板对大孔结构的构建机制,实现了对ZnO大孔结构的控制合成,气泡模板合成法省去了传统模板法常需要的模板移除过程,简化了合成工艺流程；基于两相界面限域发生的自组装过程,实现了对ZnO纳米棒逐级构建的多级组装结构以及ZnO纳米棒、纳米片阵列型组装结构的控制合成,丰富了纳米组装结构的控制合成方法。
3.开展了钛、锰基氧化物中空纳米结构、一维纳米结构的控制合成,以及二氧化钛多种晶相结构的选择性控制合成研究。基于配体对Ti06八面体基本结构单元连接方式的动力学调控作用,在高浓度溶胶前体的使用条件下实现了对TiO2板钛矿、锐钛矿不同晶相结构的选择性控制合成；基于配体调控促发的奥氏熟化排空生长方式,在低浓度溶胶前体的使用条件下实现了对锐钛矿TiO2中空纳米结构的控制合成,并将这一中空纳米结构的控制合成体系拓展应用于MoO2,考察了微纳结构对TiO2紫外-可见吸收性能的影响以及中空纳米结构MoO2电极的超级电容器及锂离子电池储能性能；基于自晶种生长机制,实现了对MnO2一维纳米结构的无模板控制合成,自晶种生长机制的提出丰富了MnO：一维纳米结构无模板生长机制的类型。
The fourth-period transition metal oxides have been widely applied in electrochemical energy storage, optoelectric devices, catalysis, and etc., owing to their unique physical and chemical properties. Benefiting from the tremendous development of material science and significant progress of nanotechnology achieved in the past decades, the key roles of structure factors (crystal phase, micro-/nano-structure) in determining the property of functional inorganic materials have been understood. Structure-controlled synthesis is accordingly of significance both for study on the structure-property relationships, and rational design of functional materials with prospective structures and thus exhibiting excellent functionality, which has become an intense topic in material science. In this dissertation, we studied on rational tuning of crystal phase, micro-/nano-structure of the fourth-period transition metal oxides that are technically important in multiple critical applications. Also the effect of above key structure factors on the supercapacitive performance and optical property of the transition metal oxide materials was investigated. The three main sections of this dissertation are summarized as follows.
1. Controlled synthesis of mixed-phase structured, nanosheet-assembly structured nickel-based oxides was studied. Based on the SO42--induced crystal phase selective mechanism, this study realized controlled synthesis of mixed-phase α,β-Ni(OH)2that contains both a-Ni(OH)2component and β-Ni(OH)2component. The electrochemical test revealed that the crystal phase structure affected significantly on the supercapacitive performance of Ni(OH)2electrode materials. The mixed-phase a, P-Ni(OH)2electrode was better than both α-Ni(OH)2and β-Ni(OH)2electrodes benefiting from its more electrochemical active sites when applied in supercapacitors; Based on the crystal phase evolution from a-Ni(OH)2to β-Ni(OH)2under hydrothermal conditions, this study realized controlled synthesis of a mixed-phase nickel-based oxide containing a-Ni(OH)2, β-Ni(OH)2and α-Co(OH)2three components, which exhibited notable performance advantage when charged/discharged at high rate in supercapacitor applications. Based on the shape-preserving conversion from a-Ni(OH)2/a-Co(OH)2nanosheet-assembly precursor to NiCo2O4under low temperature calcination conditions, this study realized the controlled synthesis of NiCo2O4nanosheet assemblies. The ultrasonication processing can prevent the severe aggregation of nanosheet assemblies during the chemical precipitation of precursor so that well-separated NiCo2O4powder particles were obtained, thus the NiCo2O4powder electrode materials can deliver high specific capacitance when applied in supercapacitors.
2. Controlled synthesis of hollow nanostructured, macroporous structured, and self-assembly nanostructured zinc-based oxides was studied. Based on the Ostwald ripening evacuation mechanism, this study realized controlled synthesis of ZnO2hollow nanostructures, and further investigated the significant effect of hollow nanostructure on the UV-Vis absorption property of ZnO2. and studied the thermal stability of ZnO2hollow nanostructures; Based on the bubble template functionality of O2that was generated by decomposition of hollow nanostructured ZnO2precursor under solvothermal treatment, this study realized controlled synthesis of ZnO macroporous nanostructures. Bubble template-directed synthesis avoided the template-elimination procedure that is commonly needed in conventional template synthesis, and thus simplified the synthesis process; Based on the self-assembly process occurred at the interphase area, this study realized controlled synthesis of ZnO multi-scale nano-assemblies that were constructed by ZnO nanorod building blocks via two-step assembly, and arrayed nano-assemblies that were constructed by ZnO nanorod or nanosheet building blocks. This work provided new routes to synthesis of nano-assemblies.
3. Controlled synthesis of hollow nanostructured, one-dimensional (1D) nanostructured titanium, manganese-based oxides, and selective crystallization of different TiO2polymorphs were studied. Based on the ligand-induced phase selective mechanism, this study realized selective crystallization of brookite and anatase microcrystals when high-concentration sol precursor was employed; When low-concentration sol precursor was employed, this study realized controlled synthesis of anatase TiO2hollow nanostructures based on the ligand-induced Ostwald ripening evacuation mechanism. This hollowing route can also be extended to synthesis of MoO2hollow nanostructures. The effect of micro-/nano-structure on the UV-Vis absorption property of TiO2, and the electrochemical energy storage performance of MoO2hollow nanostructures applied in both lithium-ion batteries and supercapacitors were further studied; Based on the self-seeding growth mechanism, this study realized controlled synthesis of1D MnO2nanostructures. This novel growth mechanism provided new insight into the template-free growth of transition metal oxide1D nanostructures.
引文
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