过渡金属氧化物纳米晶的软化学合成和表征
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摘要
本论文主要研究使用软化学方法,不同形貌及尺寸的过渡金属氧化物纳米晶的可控合成和性质表征。研究了合成方法、合成条件的改变对纳米材料的形貌、尺寸的影响,并对材料的磁、电学等物理性质进行了表征,在深入理解这些因素的基础上,探求软化学合成条件下,对过渡金属氧化物纳米材料的可控合成方面做了一些工作。
以简单的醋酸锰为锰源,直链烷基胺为水解剂并提供还原性环境,首次在室温溶液中合成出hausmannite型Mn_3O_4纳米片;磁性测试表明该纳米样品常温表现顺磁性,低温为铁磁性。
以二价铁盐和直链烷基胺为原料,在室温条件下合成出反尖晶石型立方相Fe_3O_4纳米粒子并对其物相和形貌进行了表征。该样品常温表现为超顺磁。
以乙醇、丙酮、N,N-二甲基甲酰胺、二甲亚砜、乙腈等有机试剂为溶剂,在低温溶剂热条件下制备出不同尺寸的hausmannite型Mn_3O_4纳米粒子。分别对上述反应的形成机理进行了探讨,合理的解释了不同溶剂、反应温度和水解剂的种类等因素对纳米晶体形貌尺寸的影响。
首次在水热条件下,合成出固体氧化物燃料电池电解质材料Aurivillius相Bi_4V_2O_(11)纳米晶并对其进行B位掺杂。对产物物相和形貌做了细致的表征,用复合阻抗法测试了所合成样品的中温电导率。
本论文分为五个部分。第一部分绪论,着重介绍纳米材料的概况、纳米尺寸的Mn_3O_4和Fe_3O_4的研究现状和制备方法、磁学性质概述和固体燃料电池的基本介绍;第二部分Mn_3O_4纳米片和Fe_3O_4纳米粒子的室温制备及表征;第三部分Mn_3O_4纳米粒子的溶剂热制备及表征;第四部分氧离子导体Bi_4V_2O_(11)纳米晶的水热合成与掺杂;第五部分结论和展望。
本论文旨在探索过渡金属氧化物纳米材料更简便、更高效且可以宏量制备的软化学方法,并研究了制备体系中的化学反应,纳米粒子的成核过程和晶体生长机制。同时详细分析了样品的磁电学性质,为未来更深入的实际应用奠定基础。
Transition metal oxide nanomaterials have attracted considerable attentions due to their potential applications in many fields such as optics, electricity, magnetics, catalyst and biomedicine. Great efforts have been contributed on the morphology and particle size of transition metal oxide nanocrystals because of their excellent performance. Controlled sythesis and preparation of nanomaterials are the keys to investigate the properties and put the materials into use. Moreover, the mechanism of the nucleation and growth is rather important.
Developing a low cost, low energy consumption and environment benign synthetic method for shape and size controlled nanocrystals is a challenge for chemists. Especially the room temperature synthetic route is rare oweing to complicated factors.
Hydrothermal/solvothermal synthesis method is a simple, reliable, soft chemical synthetic method. It has been more than a hundred years since the method was introduced into the synthetic chemistry. It has been adopted not only in the growth of giant crystals such as organic/ inorganic hybrid materials, but also in the synthesis of nanoparticles such as transition oxide and complex metal oxides etc.
In this study, we focus on room temperature synthetic route and hydrothermal /solvothermal synthesis of the transition metal oxide nanocrystals with different morphologies and size. The behavior of nano-sized materials strongly depends on the size, shape and morphology of their internal structures. We investigate the effect on the size, shape and morphology of nanocrystals by adjusting the extrinsic factors including solvent, heating temperature, mediate etc.
Mn_3O_4 nanoplates have been successfully prepared through redox reaction in the presence of short straight chain n-alkylamine at room temperature. N-alkylamine plays an important role in the reaction as a weak basic and reducing medium. The as-prepared Mn_3O_4 nanoplates were proved to be single crystal in nature. The average particle size is about 22×19 nm. A series of experiments were carried out to investigate the effects on the formation of Mn_3O_4 nanoplates by varying the reaction parameters such as the volume of n-alkylamine, manganese source and the different short chain n-alkylamine. The formation of Mn_3O_4 nanoplates may proceed by a dissolution-growth process. Because of its higher yield, this method could potentially offer large-scale synthesis of Mn_3O_4 nanocrystallites in the future. This room temperature route could be considered as an economical and facile approach to prepare Mn_3O_4 nanoparticles.
Fe_3O_4 nanoparticles were also prepared successfully by room temperature synthetic route. XRD pattern of Fe_3O_4 samples showed that it belong to cubic phase with space group of Fd-3m(227), lattice constant a = 8.391?. Morphology and the particle size of the as-prepared Fe_3O_4 nanoparticles were investigated by TEM. The products are made of spheral nanoparticles with average particle size of 9.6nm. The result of magnetic test indicated that the as-prepared Fe_3O_4 sample showed strong ferro- magnetic at room temperature.
Hausmannite Mn_3O_4 nanocrystals were successfully synthesized via a facile one-step solvothermal route. The data of XRD showed that the nanostructure of Mn_3O_4 can be obtained in a wide temperature range (60°C~140°C) and in mediate of many different solvent (acetone, ethanol, DMF, DMSO). The morphology and size were investigated by TEM. It was found that the particle size of the Mn_3O_4 samples could be tailed by varying the organic solvent. Control experiments showed that the ability of which the organic solvent and Mn (Ⅱ) form Manganese complex is a crucial influencing factors on the particle size of the products. The particle size increased with the rising of reaction temperature when the solvent is the same. The magnetic properties of the as-prepared samples were studied using a superconducting quantum interference device (SQUID) magnetometer. A plausible mechanism is also presented.
Metal cation substituted bismuth vanadate (BIMEVOX) possesses high oxygen ion conductivity at lower temperatures. The ionic conductivity of this material at 300°C is 50–100 times more than any other solid electrolyte; in the order of 10-3 Scm-1 at 300°C. To our knowledge, there isn’t any report on the BIMEVOXes by hydrothermal synthesis.
The parent compound Bi_2V_4O_(11) and Ag substituted bismuth vanadate (BIAGVOX ) high temperature stabilized phaseγ-Bi_4Ag_(0.2)V_(1.8)O_(11-δ) were prepared by mild hydrothermal method. The TG measurement indicated no visible change of the as-prepared powder mass. The DTA scan for the sample exhibited no thermal effects. It showed that no phase transition occurred in the as-prepared sample. The results of electrical conductivity measurements revealed that the as-prepared samples showed relatively high electrical conductivity at 700°C comparing to other reports in the literature.
In summary, we developed a novel, facile, room temperature synthetic route to prepare Mn_3O_4 and Fe_3O_4 nanocrystals. The as-prepared samples showed excellent properties. This synthetic route could be considered as an economical approach to prepare transition metal oxide nanocrystals. Moreover, we extend hydrothermal/ solvothermal method to prepare Aurivillius phase Bi_2V_4O_(11) and Ag substituted BIAGVOX compound. The electrical properties of the as-prepared samples were investigated and the results showed that they are potentially good electrolyte in the solid oxide fuel cell field.
以简单的醋酸锰为锰源,直链烷基胺为水解剂并提供还原性环境,首次在室温溶液中合成出hausmannite型Mn_3O_4纳米片;磁性测试表明该纳米样品常温表现顺磁性,低温为铁磁性。
以二价铁盐和直链烷基胺为原料,在室温条件下合成出反尖晶石型立方相Fe_3O_4纳米粒子并对其物相和形貌进行了表征。该样品常温表现为超顺磁。
以乙醇、丙酮、N,N-二甲基甲酰胺、二甲亚砜、乙腈等有机试剂为溶剂,在低温溶剂热条件下制备出不同尺寸的hausmannite型Mn_3O_4纳米粒子。分别对上述反应的形成机理进行了探讨,合理的解释了不同溶剂、反应温度和水解剂的种类等因素对纳米晶体形貌尺寸的影响。
首次在水热条件下,合成出固体氧化物燃料电池电解质材料Aurivillius相Bi_4V_2O_(11)纳米晶并对其进行B位掺杂。对产物物相和形貌做了细致的表征,用复合阻抗法测试了所合成样品的中温电导率。
本论文分为五个部分。第一部分绪论,着重介绍纳米材料的概况、纳米尺寸的Mn_3O_4和Fe_3O_4的研究现状和制备方法、磁学性质概述和固体燃料电池的基本介绍;第二部分Mn_3O_4纳米片和Fe_3O_4纳米粒子的室温制备及表征;第三部分Mn_3O_4纳米粒子的溶剂热制备及表征;第四部分氧离子导体Bi_4V_2O_(11)纳米晶的水热合成与掺杂;第五部分结论和展望。
本论文旨在探索过渡金属氧化物纳米材料更简便、更高效且可以宏量制备的软化学方法,并研究了制备体系中的化学反应,纳米粒子的成核过程和晶体生长机制。同时详细分析了样品的磁电学性质,为未来更深入的实际应用奠定基础。
Transition metal oxide nanomaterials have attracted considerable attentions due to their potential applications in many fields such as optics, electricity, magnetics, catalyst and biomedicine. Great efforts have been contributed on the morphology and particle size of transition metal oxide nanocrystals because of their excellent performance. Controlled sythesis and preparation of nanomaterials are the keys to investigate the properties and put the materials into use. Moreover, the mechanism of the nucleation and growth is rather important.
Developing a low cost, low energy consumption and environment benign synthetic method for shape and size controlled nanocrystals is a challenge for chemists. Especially the room temperature synthetic route is rare oweing to complicated factors.
Hydrothermal/solvothermal synthesis method is a simple, reliable, soft chemical synthetic method. It has been more than a hundred years since the method was introduced into the synthetic chemistry. It has been adopted not only in the growth of giant crystals such as organic/ inorganic hybrid materials, but also in the synthesis of nanoparticles such as transition oxide and complex metal oxides etc.
In this study, we focus on room temperature synthetic route and hydrothermal /solvothermal synthesis of the transition metal oxide nanocrystals with different morphologies and size. The behavior of nano-sized materials strongly depends on the size, shape and morphology of their internal structures. We investigate the effect on the size, shape and morphology of nanocrystals by adjusting the extrinsic factors including solvent, heating temperature, mediate etc.
Mn_3O_4 nanoplates have been successfully prepared through redox reaction in the presence of short straight chain n-alkylamine at room temperature. N-alkylamine plays an important role in the reaction as a weak basic and reducing medium. The as-prepared Mn_3O_4 nanoplates were proved to be single crystal in nature. The average particle size is about 22×19 nm. A series of experiments were carried out to investigate the effects on the formation of Mn_3O_4 nanoplates by varying the reaction parameters such as the volume of n-alkylamine, manganese source and the different short chain n-alkylamine. The formation of Mn_3O_4 nanoplates may proceed by a dissolution-growth process. Because of its higher yield, this method could potentially offer large-scale synthesis of Mn_3O_4 nanocrystallites in the future. This room temperature route could be considered as an economical and facile approach to prepare Mn_3O_4 nanoparticles.
Fe_3O_4 nanoparticles were also prepared successfully by room temperature synthetic route. XRD pattern of Fe_3O_4 samples showed that it belong to cubic phase with space group of Fd-3m(227), lattice constant a = 8.391?. Morphology and the particle size of the as-prepared Fe_3O_4 nanoparticles were investigated by TEM. The products are made of spheral nanoparticles with average particle size of 9.6nm. The result of magnetic test indicated that the as-prepared Fe_3O_4 sample showed strong ferro- magnetic at room temperature.
Hausmannite Mn_3O_4 nanocrystals were successfully synthesized via a facile one-step solvothermal route. The data of XRD showed that the nanostructure of Mn_3O_4 can be obtained in a wide temperature range (60°C~140°C) and in mediate of many different solvent (acetone, ethanol, DMF, DMSO). The morphology and size were investigated by TEM. It was found that the particle size of the Mn_3O_4 samples could be tailed by varying the organic solvent. Control experiments showed that the ability of which the organic solvent and Mn (Ⅱ) form Manganese complex is a crucial influencing factors on the particle size of the products. The particle size increased with the rising of reaction temperature when the solvent is the same. The magnetic properties of the as-prepared samples were studied using a superconducting quantum interference device (SQUID) magnetometer. A plausible mechanism is also presented.
Metal cation substituted bismuth vanadate (BIMEVOX) possesses high oxygen ion conductivity at lower temperatures. The ionic conductivity of this material at 300°C is 50–100 times more than any other solid electrolyte; in the order of 10-3 Scm-1 at 300°C. To our knowledge, there isn’t any report on the BIMEVOXes by hydrothermal synthesis.
The parent compound Bi_2V_4O_(11) and Ag substituted bismuth vanadate (BIAGVOX ) high temperature stabilized phaseγ-Bi_4Ag_(0.2)V_(1.8)O_(11-δ) were prepared by mild hydrothermal method. The TG measurement indicated no visible change of the as-prepared powder mass. The DTA scan for the sample exhibited no thermal effects. It showed that no phase transition occurred in the as-prepared sample. The results of electrical conductivity measurements revealed that the as-prepared samples showed relatively high electrical conductivity at 700°C comparing to other reports in the literature.
In summary, we developed a novel, facile, room temperature synthetic route to prepare Mn_3O_4 and Fe_3O_4 nanocrystals. The as-prepared samples showed excellent properties. This synthetic route could be considered as an economical approach to prepare transition metal oxide nanocrystals. Moreover, we extend hydrothermal/ solvothermal method to prepare Aurivillius phase Bi_2V_4O_(11) and Ag substituted BIAGVOX compound. The electrical properties of the as-prepared samples were investigated and the results showed that they are potentially good electrolyte in the solid oxide fuel cell field.
引文
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