溶液法化学合成微纳米结构金属氧化物
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摘要
近年来,金属氧化物微纳米结构材料由于在电学、催化、光学、气体传感器等方面的广泛应用而倍受关注。合成新颖的金属氧化物微纳米结构、探索其生长过程,进而实现对尺寸、结构及物性的调控,对于深入研究结构与物性的联系、最终实现按照人们的意愿去设计合成材料具有重要意义。本论文以金属氧化物微纳米材料为研究主体,以液相化学合成为手段,从材料新结构和新方法的探索出发,致力于液相合成微纳米结构金属氧化物过程中形成规律的研究。实现了对金属氧化物微纳结构的控制合成,并建立了一些微纳米结构体系的化学合成新途径。本论文的主要内容包括以下几个方面:
1.以纳米结构器件和量子器件为背景的纳米阵列组装体系已成为纳米材料研究的热点,论文提出了以同步自组装路线制备金属氧化物纳米阵列结构的方法。具体内容是:基于原电池的原理,采用氯离子溶液腐蚀法合成了ZnO纳米棒阵列。并通过研究纳米棒阵列结构的形成机制,揭示了通过腐蚀法合成金属氧化物纳米阵列的一般性规律;采用准六方结构的Nb_2O_5纳米棒阵列为前驱物,通过相转移合成了单斜结构的Nb_2O_5纳米管阵列。
2.人们对于中空结构的合成有浓厚的兴趣是因为它们在很多领域都有潜在的应用价值,论文分别采用自牺牲模板法和原位模板法合成了金属氧化物中空微米球和中空管状材料。具体内容是:基于对反应物和生成物之间离子溶度积竞争规律的认识,提出了中空结构微米球的自牺牲模板合成法。以微溶性Zn_5(CO_3)_2(OH)_6微米球作为自牺牲模板,成功合成了ZnO中空结构材料,中空结构的形成过程可以用克肯达耳空位效应来解释:依据ZnO晶体结构极性生长的特征,提出了以醋酸为化学刻蚀剂制备中空ZnO管的原位模板法,中空管是通过醋酸在ZnO模板表面发生逐步刻蚀而形成的。
3.金属氧化物材料具有非常优异的特性及广阔的应用前景,系统地研究和开发新型微纳米结构金属氧化物具有重要的意义,论文提出了以碱式碳酸镁为反应前驱物通过溶液化学路线制备多种金属氧化物微纳米材料的方法。具体内容是:依据碱式碳酸镁的片状生长特征,以碱式碳酸镁作为前驱体合成了由纳米片构成的等级结构氧化镁,碱式碳酸镁是在均匀成核溶液体系下制备的;依据碱式碳酸镁在溶液中的微溶解特性,以碱式碳酸镁为反应物,提出了一种制备多种金属氧化物微纳米材料的普适性方法,成功地合成了各种金属氧化物微纳米结构材料,包括Mn_2O_3、ZnO、CuO、CdO、CaO和Al_2O_3,并实现了微结构的有效调控。
In recent years,metal oxide micro/nano structures have stimulated much scientific and technological interest because of their promising applications in electronics,catalyst,optics, gas sensors,etc.Chemical preparation of novel micro/nanostructures and the investigation of their general formation processes may be a solution to the precise control of their sizes, structures and properties.It is of great significance to tailor the property of materials in a controllable way by altering their structure,morphology,or composition.In this dissertation, systematic explorations have been carried out on new synthetic strategies of metal oxides based on the chemical solution method.We have realized the control of micro/nano structures of materials during the synthesis process,and established some new routes to fabricate metal oxide materials.The main points can be summarized as follows:
1.Nanoarrays based on nanodevice and quantum device have been a hot research topic, solution-based routes were developed to the chemical synthesis and simultaneous assembly of nanostructures into metal oxide nanoarrays.Specifically,a corrosion-based strategy has been successfully designed to synthesize ZnO nanorod arrays in the Cl~- anion solution by employing cell reaction.The gerenal principle for the synthesis of nanorod arrays materials has been discovered by exploring their formation processes.In particular,a phase transformation has been discovered for the preparation of monoclinic Nb_2O_5 nanotube arrays through using pseudo-hexagonal Nb_2O_5 nanorod arrays as the precursor.
2.Hollow structured materials have attracted much attention because of their great potential applicatios in many fields,hollow metal oxide microspheres and tubes were prepared through the sacrificial template and in situ template method,respectively. Specifically,based on the solubility difference between reactant and production,hollow ZnO microspheres were fabricatred by the sacrificial template route.ZnO hollow microspheres were prepared by employing Zn_5(CO_3)_2(OH)_6 as the in situ sacrificial template at room temperature.The Kirkendall vacancy effect was used to interpret the formation process of hollow ZnO microspheres.According to ZnO characteristics of surface polarity and chemical activities,the hollow ZnO tubes were prepared through in situ template method based on acetic acid etching strategy.The etching of ZnO template with acetic acid results in the formation of tubular structures.
3.Meal oxide micro/nano structured materials have a variety of special properties,hence it is very important in both fundamental research and commercial applications,several metal oxide materials were fabricated by employintg Mg_5(CO_3)_4(OH)_2·4H_2O as the reaction precursors through chemical solution method.Specifically,according to the growth habit of Mg_5(CO_3)_4(OH)_2·4H_2O sheet-like structures,MgO hierachical structures consisted of nanosheets were fabricated by using Mg_5(CO_3)_4(OH)_2·4H_2O as the precursors,which were prepared by a homogeneous reaction.Based on the fact that Mg_5(CO_3)_4(OH)_2·4H_2O is a slightly soluble salt,a spontaneous ion replacement route by employing Mg_5(CO_3)_4(OH)_2·4H_2O as the reagent to synthesize a number of metal oxides has been established.We present a comprehensive study on the ion replacement reaction for the chemical control synthesis of micro/nano structured Mn_2O_3,ZnO,CuO,CdO,Al_2O_3,and CaO samples.
1.以纳米结构器件和量子器件为背景的纳米阵列组装体系已成为纳米材料研究的热点,论文提出了以同步自组装路线制备金属氧化物纳米阵列结构的方法。具体内容是:基于原电池的原理,采用氯离子溶液腐蚀法合成了ZnO纳米棒阵列。并通过研究纳米棒阵列结构的形成机制,揭示了通过腐蚀法合成金属氧化物纳米阵列的一般性规律;采用准六方结构的Nb_2O_5纳米棒阵列为前驱物,通过相转移合成了单斜结构的Nb_2O_5纳米管阵列。
2.人们对于中空结构的合成有浓厚的兴趣是因为它们在很多领域都有潜在的应用价值,论文分别采用自牺牲模板法和原位模板法合成了金属氧化物中空微米球和中空管状材料。具体内容是:基于对反应物和生成物之间离子溶度积竞争规律的认识,提出了中空结构微米球的自牺牲模板合成法。以微溶性Zn_5(CO_3)_2(OH)_6微米球作为自牺牲模板,成功合成了ZnO中空结构材料,中空结构的形成过程可以用克肯达耳空位效应来解释:依据ZnO晶体结构极性生长的特征,提出了以醋酸为化学刻蚀剂制备中空ZnO管的原位模板法,中空管是通过醋酸在ZnO模板表面发生逐步刻蚀而形成的。
3.金属氧化物材料具有非常优异的特性及广阔的应用前景,系统地研究和开发新型微纳米结构金属氧化物具有重要的意义,论文提出了以碱式碳酸镁为反应前驱物通过溶液化学路线制备多种金属氧化物微纳米材料的方法。具体内容是:依据碱式碳酸镁的片状生长特征,以碱式碳酸镁作为前驱体合成了由纳米片构成的等级结构氧化镁,碱式碳酸镁是在均匀成核溶液体系下制备的;依据碱式碳酸镁在溶液中的微溶解特性,以碱式碳酸镁为反应物,提出了一种制备多种金属氧化物微纳米材料的普适性方法,成功地合成了各种金属氧化物微纳米结构材料,包括Mn_2O_3、ZnO、CuO、CdO、CaO和Al_2O_3,并实现了微结构的有效调控。
In recent years,metal oxide micro/nano structures have stimulated much scientific and technological interest because of their promising applications in electronics,catalyst,optics, gas sensors,etc.Chemical preparation of novel micro/nanostructures and the investigation of their general formation processes may be a solution to the precise control of their sizes, structures and properties.It is of great significance to tailor the property of materials in a controllable way by altering their structure,morphology,or composition.In this dissertation, systematic explorations have been carried out on new synthetic strategies of metal oxides based on the chemical solution method.We have realized the control of micro/nano structures of materials during the synthesis process,and established some new routes to fabricate metal oxide materials.The main points can be summarized as follows:
1.Nanoarrays based on nanodevice and quantum device have been a hot research topic, solution-based routes were developed to the chemical synthesis and simultaneous assembly of nanostructures into metal oxide nanoarrays.Specifically,a corrosion-based strategy has been successfully designed to synthesize ZnO nanorod arrays in the Cl~- anion solution by employing cell reaction.The gerenal principle for the synthesis of nanorod arrays materials has been discovered by exploring their formation processes.In particular,a phase transformation has been discovered for the preparation of monoclinic Nb_2O_5 nanotube arrays through using pseudo-hexagonal Nb_2O_5 nanorod arrays as the precursor.
2.Hollow structured materials have attracted much attention because of their great potential applicatios in many fields,hollow metal oxide microspheres and tubes were prepared through the sacrificial template and in situ template method,respectively. Specifically,based on the solubility difference between reactant and production,hollow ZnO microspheres were fabricatred by the sacrificial template route.ZnO hollow microspheres were prepared by employing Zn_5(CO_3)_2(OH)_6 as the in situ sacrificial template at room temperature.The Kirkendall vacancy effect was used to interpret the formation process of hollow ZnO microspheres.According to ZnO characteristics of surface polarity and chemical activities,the hollow ZnO tubes were prepared through in situ template method based on acetic acid etching strategy.The etching of ZnO template with acetic acid results in the formation of tubular structures.
3.Meal oxide micro/nano structured materials have a variety of special properties,hence it is very important in both fundamental research and commercial applications,several metal oxide materials were fabricated by employintg Mg_5(CO_3)_4(OH)_2·4H_2O as the reaction precursors through chemical solution method.Specifically,according to the growth habit of Mg_5(CO_3)_4(OH)_2·4H_2O sheet-like structures,MgO hierachical structures consisted of nanosheets were fabricated by using Mg_5(CO_3)_4(OH)_2·4H_2O as the precursors,which were prepared by a homogeneous reaction.Based on the fact that Mg_5(CO_3)_4(OH)_2·4H_2O is a slightly soluble salt,a spontaneous ion replacement route by employing Mg_5(CO_3)_4(OH)_2·4H_2O as the reagent to synthesize a number of metal oxides has been established.We present a comprehensive study on the ion replacement reaction for the chemical control synthesis of micro/nano structured Mn_2O_3,ZnO,CuO,CdO,Al_2O_3,and CaO samples.
引文
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