钼酸盐纳米材料的制备及相关性质研究
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摘要
近些年,可控合成具有特定形貌和尺寸的功能纳米材料由于其在光电,磁性,机械等领域的潜在应用价值引起了人们越来越多的兴趣。
金属钼酸盐由于其独特的晶体结构和物理性质而在非常多的领域都有广泛的应用潜力,如光致发光,微波器件,光学纤维,闪烁材料,湿敏器件,催化剂等。因此有关金属钼酸盐的制备技术和应用研究,成为人们非常感兴趣的课题。
本论文选取钼酸亚铁、钼酸钾和钼酸镉纳米材料为研究对象,通过对合成方法和反应条件的研究,探索过程简便、条件温和,成本低廉的新途径,实现对钼酸盐材料的微观结晶形貌的可控合成;对合成的钼酸盐材料进行了各种性能测试。
本文的主要研究内容包括:
(1)用水热法合成了钼酸亚铁纳米棒,利用XRD、XPS、SEM和TEM等分析技术对制备出的材料进行表征,分析并提出了钼酸亚铁纳米棒的生长模型,对钼酸亚铁纳米棒的磁性和塞贝克(Seebeck)系数进行了测试和分析。
(2)以复合熔融盐为溶剂合成了钼酸钾纳米带,通过XRD、SEM和TEM表征,分析了材料的形貌和结构,在室温下测试了材料的光致发光性质,并测试了用钼酸钾纳米带制备的电极在锂电池中的性能。
(3)用沉淀法在室温下制备出了直径为1微米的钼酸镉微球,用XRD和SEM对样品进行了表征,发现微球是由更小的颗粒组成的。
Controllable synthesis of functional materials with the specific morphology and size has aroused growing interest due to its optical, magnetic, mechanical and other areas of potential applications in the past decade.
Metal molybdate due to its unique crystal structure and physical properties have a widely application potential in many fields, such as photoluminescence, microwave devices, optical fiber, scintillating materials, humidity devices, catalysts and so on.
Therefore, the preparation technology and application research of metal molybdate become very interested topic.
This thesis focuses on the materials of ferrous molybdate, cadmium molybdate and molybdate potassium to achieve controllable synthesis methods that are simple, mild and low-cost, and explore the new properties of these materials. The main contents can be summarized as fallowing:
(1) Monoclinic FeMoO_4 nanorods have been prepared by the hydrothermal method in an acid aqueous solution. Scanning electron microscopy, transmission electron microscopy, X-ray diffraction spectrum, X-ray photoelectron spectra and differential scanning calorimetry are used to characterize the structure, morphology and composition of the sample. The growth mechanism of the FeMoO_4 nanorods is proposed. Seebeck effect and magnetic property were investigated.
(2) Potassium molybdate nanoblets was synthesized by molten salt. XRD, SEM and TEM were used to characterizated and analysised the morphology and structure of the material. Photoluminescence properties of materials are tested at room temperature, and electrode performance in lithium batteries of Potassium molybdate nanoblets is also investigated.
(3) CdMoO_4 microspheres have been prepared by stirring reacting solution at room temperature. X-ray diffraction spectrum and scanning electron microscopy were used to characterizated the samples.
金属钼酸盐由于其独特的晶体结构和物理性质而在非常多的领域都有广泛的应用潜力,如光致发光,微波器件,光学纤维,闪烁材料,湿敏器件,催化剂等。因此有关金属钼酸盐的制备技术和应用研究,成为人们非常感兴趣的课题。
本论文选取钼酸亚铁、钼酸钾和钼酸镉纳米材料为研究对象,通过对合成方法和反应条件的研究,探索过程简便、条件温和,成本低廉的新途径,实现对钼酸盐材料的微观结晶形貌的可控合成;对合成的钼酸盐材料进行了各种性能测试。
本文的主要研究内容包括:
(1)用水热法合成了钼酸亚铁纳米棒,利用XRD、XPS、SEM和TEM等分析技术对制备出的材料进行表征,分析并提出了钼酸亚铁纳米棒的生长模型,对钼酸亚铁纳米棒的磁性和塞贝克(Seebeck)系数进行了测试和分析。
(2)以复合熔融盐为溶剂合成了钼酸钾纳米带,通过XRD、SEM和TEM表征,分析了材料的形貌和结构,在室温下测试了材料的光致发光性质,并测试了用钼酸钾纳米带制备的电极在锂电池中的性能。
(3)用沉淀法在室温下制备出了直径为1微米的钼酸镉微球,用XRD和SEM对样品进行了表征,发现微球是由更小的颗粒组成的。
Controllable synthesis of functional materials with the specific morphology and size has aroused growing interest due to its optical, magnetic, mechanical and other areas of potential applications in the past decade.
Metal molybdate due to its unique crystal structure and physical properties have a widely application potential in many fields, such as photoluminescence, microwave devices, optical fiber, scintillating materials, humidity devices, catalysts and so on.
Therefore, the preparation technology and application research of metal molybdate become very interested topic.
This thesis focuses on the materials of ferrous molybdate, cadmium molybdate and molybdate potassium to achieve controllable synthesis methods that are simple, mild and low-cost, and explore the new properties of these materials. The main contents can be summarized as fallowing:
(1) Monoclinic FeMoO_4 nanorods have been prepared by the hydrothermal method in an acid aqueous solution. Scanning electron microscopy, transmission electron microscopy, X-ray diffraction spectrum, X-ray photoelectron spectra and differential scanning calorimetry are used to characterize the structure, morphology and composition of the sample. The growth mechanism of the FeMoO_4 nanorods is proposed. Seebeck effect and magnetic property were investigated.
(2) Potassium molybdate nanoblets was synthesized by molten salt. XRD, SEM and TEM were used to characterizated and analysised the morphology and structure of the material. Photoluminescence properties of materials are tested at room temperature, and electrode performance in lithium batteries of Potassium molybdate nanoblets is also investigated.
(3) CdMoO_4 microspheres have been prepared by stirring reacting solution at room temperature. X-ray diffraction spectrum and scanning electron microscopy were used to characterizated the samples.
引文
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[2]王世敏,许祖勋,傅晶.纳米材料制备技术[M].北京:化学工业出版社, 2002.
[3]尾崎又治,架集诚一郎.纳米微粒导论[M].赵健泽,张联盟译.武汉:武汉工业大学出版社, 1991.
[4]唐一科,许静,韦立凡,纳米材料制备方法的研究现状与发展趋势[J].重庆大学学报(自然科学版) [J]. 2005, 58(1): 5.
[5]张立德,牟季美.纳米材料和纳米结构[M].北京:科学出版社,2001.146.
[6]周世杰,张喜燕,贾冲,夏宝玉,周明哲.纳米材料制备技术的研究现状[J].材料导报,2005,19:2-16.
[7] M. Rontani, Quantum phases in artificial molecules[J]. Solid State Commun., 2001 (119): 30.
[8] N. N. Ledenstoy,Crystalline growth characteristics[J].Mater Pmgtl, 998,35(2—4):289.
[9]刘跃进,李振民,等.水热法合成云母氧化铁结晶条件.化工学报,2004,55(5):20.
[10]希忠,张禹,刘国权,等.CVD金刚石膜{100}取向生长的原子尺度仿真[J].北京科技大学学报.2002,24(2):143.
[11]王富耻.材料现代测试分析方法[M].北京,北京理工大学出版社,2006:1-289.
[12]吴刚.材料结构表征及应用[M].北京,化学工业出版社,2001:1-379 .
[13]周小菊,张嫦,刘东,李永康,吴莉莉.纳米材料的性质及应用[J].西南民族学院学报, 2002, 28(4): 566.
[14]江今朝,涂向真.纳米材料的性质和应用[J].江西化工, 2002, 2: 18.
[15] N. N. Leyzerovich, K. G.Bramnik, T. Buhrmester, H. Ehrenberg and H. Fuess, Electrochemical intercalation of lithium in ternary metal molybdates MMoO4 (M: Cu, Zn, Ni and Fe) [J]. J. of Power Sources, 2004, 127: 76-84.
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