无机功能材料的湿化学法制备工艺
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摘要
近年来,人们在研究微纳米材料的结构与性质的关系时发现,微纳米材料的性能不仅与其尺寸大小有关,维度、表面结构、暴露晶面等众多与形貌相关的因素对物质的电、磁、光、声、热、力等性质也有着不可忽视的影响。比如,一维微纳米结构的量子尺寸效应以及各向异性,赋予材料独特的物理性质;空心微纳米结构具备较高的比表面积,使材料在催化、输送等方面具有很大的优势。本论文以无机功能微纳米材料为研究主体,以湿化学合成策略为手段,实现了对五氧化二铌以及硼酸镁微纳结构的控制合成。本论文的主要内容包括以下几个方面:
(1)设计了一条以水和乙醇的混合溶剂为反应体系,通过一种简便、通用的水热均相沉淀法制备出了Nb_2O_5棒状材料。研究表明,当有乙醇加入反应体系时,Nb_2O_5棒的直径比没有乙醇加入时的直径大。采用Nb_2O_5棒为模板,进行两步反应,合成出了Nb_2O_5管状结构。
(2)在微波辅助加热条件下,以乙二胺为沉淀剂,通过简单沉淀反应,得到了铌酸球形材料,并通过调节沉淀剂的用量,实现了对铌酸球形前驱物直径的调控;对铌酸前驱物进行水热处理以及烧结处理,制备出了正交相Nb_2O_5空心球。另外,通过常温下的沉淀反应,还合成出了具有表面多孔结构特征的棒状(NH_4)_3Nb(O_2)_2F_4前驱物。
(3)通过简单的水热反应制备出了碱式硼酸镁纳米晶须以及水合硼酸镁空心球纳米结构。研究表明,碱不仅作为反应原料,还作为形貌调控剂;碱的用量对产物的组分和形状起到最至关重要的作用。在较高的碱浓度下,合成出了碱式硼酸镁纳米晶须;在相对较低的碱浓度下,合成出了多级的水合硼酸镁空心球结构。对不同形状和组分的水热产物在7000℃下烧结2小时,得到了其相应的硼酸镁纳米结构。
In recent years,the researchers discover that the properties of materials are related not only with the size of the crystal but also with the morphologies such as the dimension,the exposed planes and the surface structures.All of these factors may play a key role in the properties of materials such as electronic,optical,magnetic,acoustic,thermal and mechanical properties. For example,compared with bulks materials,one-dimensional nanoscale materials,with their possible quantum-confinement effects and anisotropy,exhibit distinct chemical and thermal properties.Hollow nano/microcrystals,with their large surface areas,may have great advantages in the catalyst and transformation of medicine.In this dissertation,systematic explorations have been carried out on new synthetic strategies of functional inorganic nano/micromaterial(Nb_2O_5,Mg_2B_2O_5) and their structure fabrication based on chemical solution method.The main points can be summarized as follows:
A general chemical strategy based on coordination-assisted preferential etching process to fabricating Nb_2O_5(orthorhombic) hollow tubes by a two-step process has been reported.Nb_2O_5 rods serviced as precursors are synthesized by a simple hydrothermal method and the diameter of rods can be tuned by varying the synthetic conditions.The orthorhombic Nb_2O_5 tubes are then obtained by a coordination-assisted preferential etching reaction of the precursors.The controlled interior structure of Nb_2O_5 tubes can also be achieved by tuning reaction time.
The orthorhombic Nb_2O_5 hollow spheres are fabricated through the sacrificial template route.As we know,the formation of the nanocrystals involves two steps:nucleation of an initial 'seed' and growth.So the diameters of the niobic acid spheres are tuned by controlling the concentration of ammonia.The porous(NH_4)_3Nb(O_2)_2F_4 are also be prepared by precipitation at room temperature.
Magnesium borates with controlled compositions and morphologies are successfully fabricated through a two-step synthetic process.Without any organic additive or catalyst, MgBO_2(OH) nanorods and Mg_7B_4O_(13)·7H_2O hollow spheres can be prepared by controlling the concentration of hydroxide ions in hydrothermal condition.Hydroxide ions used here not only act as precipitator but also as shape-directing agent to change the relative specific surface energies of various planes and eventually influence the nucleation and growth of crystal. Mg_2B_2O_5 and Mg_3B_2O_6 with corresponding morphology can be obtained through a simple heat treatment process of MgBO_2(OH) and Mg_7B_4O_(13)·7H_2O precursors at 700℃for 2 h under air atmosphere
(1)设计了一条以水和乙醇的混合溶剂为反应体系,通过一种简便、通用的水热均相沉淀法制备出了Nb_2O_5棒状材料。研究表明,当有乙醇加入反应体系时,Nb_2O_5棒的直径比没有乙醇加入时的直径大。采用Nb_2O_5棒为模板,进行两步反应,合成出了Nb_2O_5管状结构。
(2)在微波辅助加热条件下,以乙二胺为沉淀剂,通过简单沉淀反应,得到了铌酸球形材料,并通过调节沉淀剂的用量,实现了对铌酸球形前驱物直径的调控;对铌酸前驱物进行水热处理以及烧结处理,制备出了正交相Nb_2O_5空心球。另外,通过常温下的沉淀反应,还合成出了具有表面多孔结构特征的棒状(NH_4)_3Nb(O_2)_2F_4前驱物。
(3)通过简单的水热反应制备出了碱式硼酸镁纳米晶须以及水合硼酸镁空心球纳米结构。研究表明,碱不仅作为反应原料,还作为形貌调控剂;碱的用量对产物的组分和形状起到最至关重要的作用。在较高的碱浓度下,合成出了碱式硼酸镁纳米晶须;在相对较低的碱浓度下,合成出了多级的水合硼酸镁空心球结构。对不同形状和组分的水热产物在7000℃下烧结2小时,得到了其相应的硼酸镁纳米结构。
In recent years,the researchers discover that the properties of materials are related not only with the size of the crystal but also with the morphologies such as the dimension,the exposed planes and the surface structures.All of these factors may play a key role in the properties of materials such as electronic,optical,magnetic,acoustic,thermal and mechanical properties. For example,compared with bulks materials,one-dimensional nanoscale materials,with their possible quantum-confinement effects and anisotropy,exhibit distinct chemical and thermal properties.Hollow nano/microcrystals,with their large surface areas,may have great advantages in the catalyst and transformation of medicine.In this dissertation,systematic explorations have been carried out on new synthetic strategies of functional inorganic nano/micromaterial(Nb_2O_5,Mg_2B_2O_5) and their structure fabrication based on chemical solution method.The main points can be summarized as follows:
A general chemical strategy based on coordination-assisted preferential etching process to fabricating Nb_2O_5(orthorhombic) hollow tubes by a two-step process has been reported.Nb_2O_5 rods serviced as precursors are synthesized by a simple hydrothermal method and the diameter of rods can be tuned by varying the synthetic conditions.The orthorhombic Nb_2O_5 tubes are then obtained by a coordination-assisted preferential etching reaction of the precursors.The controlled interior structure of Nb_2O_5 tubes can also be achieved by tuning reaction time.
The orthorhombic Nb_2O_5 hollow spheres are fabricated through the sacrificial template route.As we know,the formation of the nanocrystals involves two steps:nucleation of an initial 'seed' and growth.So the diameters of the niobic acid spheres are tuned by controlling the concentration of ammonia.The porous(NH_4)_3Nb(O_2)_2F_4 are also be prepared by precipitation at room temperature.
Magnesium borates with controlled compositions and morphologies are successfully fabricated through a two-step synthetic process.Without any organic additive or catalyst, MgBO_2(OH) nanorods and Mg_7B_4O_(13)·7H_2O hollow spheres can be prepared by controlling the concentration of hydroxide ions in hydrothermal condition.Hydroxide ions used here not only act as precipitator but also as shape-directing agent to change the relative specific surface energies of various planes and eventually influence the nucleation and growth of crystal. Mg_2B_2O_5 and Mg_3B_2O_6 with corresponding morphology can be obtained through a simple heat treatment process of MgBO_2(OH) and Mg_7B_4O_(13)·7H_2O precursors at 700℃for 2 h under air atmosphere
引文
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