熔融盐法制备钛酸钡和钛酸镁的研究
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摘要
钛酸钡是典型的铁电、压电、介电陶瓷材料,广泛应用于陶瓷电容器、热敏元件、铁电、压电器件,被称为电子陶瓷工业的支柱。钛酸镁是重要的微波介质陶瓷材料,具有介电损耗低、介电常数低等特点,在现代通信领域具有广阔的应用前景。因此,钛酸钡和钛酸镁的制备及应用成为当今研究的热点。本论文通过熔融盐法分别制备钛酸钡和钛酸镁,系统考察了各种因素对制备钛酸钡和钛酸镁的影响。
本论文分别采用熔融盐法和改进的熔融盐法制备钛酸钡纳米颗粒及钛酸钡亚微米棒。采用X-射线衍射仪(XRD)、傅里叶变换红外光谱仪(FTIR)、扫描电子显微镜(SEM)等测试手段对样品进行表征。结果表明,当采用熔融盐法制备钛酸钡时,得到的钛酸钡为纳米颗粒,平均粒径约为50nm,钡钛比为1.018。当采用改进的熔融盐法制备钛酸钡时,成功地制备出钛酸钡亚微米棒,棒的直径在200nm左右,长达几微米；以溶胶-凝胶法制备的Ba-Ti前驱体,使钡源和钛源达到原子水平混合,有利于钛酸钡亚微米棒在熔盐中的形成。最后根据实验现象和测试结果,讨论了钛酸钡纳米颗粒以及钛酸钡亚微米棒在熔盐中的形成过程。
在论文的最后一章,采用熔融盐法制备钛酸镁,分别采用XRD、SEM以及透射电镜(TEM)对样品进行表征。结果表明,以MgCl2·6H2O为镁源,可以成功制备出平均尺寸约为300nm、厚度40nm左右的钛酸镁六方片,并探讨了片状钛酸镁的形成机理。
Barium titanate is a typical ferroelectric, piezoelectric, and dielectric material, which is widely applied in ceramic capacitor, thermistor, ferroelectric and piezoelectric devices. It is called as "Backbone of Electronic Ceramic Industry". Magnesium titanate, possessing low dielectric loss and constant, is an important microwave dielectric ceramic material. It has a broad application prospect in modern communication field. Therefore, many researches are focused on preparation, application of barium titanate and magnesium titanate. In this paper, barium titanate and magnesium titanate were prepared by molten salt method, and the influence of various factors on the preparation was investigated.
In the current work, barium titanate nanoparticle and submicro-rod were prepared by molten salt method and modified molten salt method, respectively. The as-prepared samples were characterized by X-ray diffraction (XRD), Fourier transform infrared spectrometry (FTIR), Scanned electron microscope (SEM) and so on. The results indicate that using molten salt method, the as-prepared barium titanate is nanoparticle which is about50nm in diameter, the ratio of Ba and Ti is1.018. Barium titanate submicro-rod is successfully synthesized by modified molten salt method. The average diameter of the rod is around200nm, and the length is up to several micrometers. Ba-Ti precursor prepared by sol-gel, is mixed at an atomic level, which is favorable for the formation of barium titanate submicro-rod in the molten salt. Finally, according to the experimental phenomena and test results, the formation processes of barium titanate nanoparticle and submicro-rod in the molten salt are discussed.
In the last chapter, magnesium titanate was prepared by molten salt method. The samples were analyzed by XRD, SEM, and Transmission electron microscope (TEM), respectively. The results show that using MgCl2·6H2O as Mg source, magnesium titanate hexagonal flake is synthesized, which is about300nm in diameter, around40nm in thickness. The mechanism for flake-like magnesium titanate is proposed.
本论文分别采用熔融盐法和改进的熔融盐法制备钛酸钡纳米颗粒及钛酸钡亚微米棒。采用X-射线衍射仪(XRD)、傅里叶变换红外光谱仪(FTIR)、扫描电子显微镜(SEM)等测试手段对样品进行表征。结果表明,当采用熔融盐法制备钛酸钡时,得到的钛酸钡为纳米颗粒,平均粒径约为50nm,钡钛比为1.018。当采用改进的熔融盐法制备钛酸钡时,成功地制备出钛酸钡亚微米棒,棒的直径在200nm左右,长达几微米；以溶胶-凝胶法制备的Ba-Ti前驱体,使钡源和钛源达到原子水平混合,有利于钛酸钡亚微米棒在熔盐中的形成。最后根据实验现象和测试结果,讨论了钛酸钡纳米颗粒以及钛酸钡亚微米棒在熔盐中的形成过程。
在论文的最后一章,采用熔融盐法制备钛酸镁,分别采用XRD、SEM以及透射电镜(TEM)对样品进行表征。结果表明,以MgCl2·6H2O为镁源,可以成功制备出平均尺寸约为300nm、厚度40nm左右的钛酸镁六方片,并探讨了片状钛酸镁的形成机理。
Barium titanate is a typical ferroelectric, piezoelectric, and dielectric material, which is widely applied in ceramic capacitor, thermistor, ferroelectric and piezoelectric devices. It is called as "Backbone of Electronic Ceramic Industry". Magnesium titanate, possessing low dielectric loss and constant, is an important microwave dielectric ceramic material. It has a broad application prospect in modern communication field. Therefore, many researches are focused on preparation, application of barium titanate and magnesium titanate. In this paper, barium titanate and magnesium titanate were prepared by molten salt method, and the influence of various factors on the preparation was investigated.
In the current work, barium titanate nanoparticle and submicro-rod were prepared by molten salt method and modified molten salt method, respectively. The as-prepared samples were characterized by X-ray diffraction (XRD), Fourier transform infrared spectrometry (FTIR), Scanned electron microscope (SEM) and so on. The results indicate that using molten salt method, the as-prepared barium titanate is nanoparticle which is about50nm in diameter, the ratio of Ba and Ti is1.018. Barium titanate submicro-rod is successfully synthesized by modified molten salt method. The average diameter of the rod is around200nm, and the length is up to several micrometers. Ba-Ti precursor prepared by sol-gel, is mixed at an atomic level, which is favorable for the formation of barium titanate submicro-rod in the molten salt. Finally, according to the experimental phenomena and test results, the formation processes of barium titanate nanoparticle and submicro-rod in the molten salt are discussed.
In the last chapter, magnesium titanate was prepared by molten salt method. The samples were analyzed by XRD, SEM, and Transmission electron microscope (TEM), respectively. The results show that using MgCl2·6H2O as Mg source, magnesium titanate hexagonal flake is synthesized, which is about300nm in diameter, around40nm in thickness. The mechanism for flake-like magnesium titanate is proposed.
引文
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[2]R(?)rvik P M, Lyngdal T, S(?)terli R, et al. Influence of volatile chlorides on the molten salt synthesis of ternary oxide nanorods and nanoparticles [J]. Inorganic Chemistry, 2008,47:3173-3181.
[3]Mao Y B, Banerjee S, Wong S S. Large-scale synthesis of single-crystalline perovskite nanostructures [J]. Journal of the American Chemical Society,2003,125:15718-15719.
[4]Wang T X, Liu S Z, Chen J. Molten salt synthesis of SrTiO3 nanocrystals using nanocrystalline TiO2 as a precursor [J]. Powder Technology,2011,205:289-291.
[5]王海华.二氧化钛纳米粒的制备及其性能[D].长沙：中南大学化学化工学院,2009.
[6]Goto T, Toyoura K, Tsujimura H, et al. Formation and control of zinc nitride in a molten LiCl-KCl-Li3N system [J]. Materials Science and Engineering A,2004,380:41-45.
[7]Jiang Z Y, Xu T, Xie Z X, et al. Molten Salt Route toward the growth of ZnO nanowires in unusual growth directions [J]. Journal of Physical Chemistry B,2005,109: 23269-23273.
[8]Xu T, Zhou X, Jiang Z Y, et al. Syntheses of nano/submicrostrucutred metal oxides with all polar surface exposed via a molten salt route [J]. Crystal Growth & Design,2009, 9:192-196.
[9]朱建华,梁飞,汪小红等.微波介质陶瓷材料介电性能间的制约关系[J].电子元件与材料,2005,24(3)：32-35.
[10]杨红星.中温烧结钛酸钡基X8R陶瓷研究[D].天津：天津大学电子信息工程学院,2009.
[11]Yun W S, Urban J J, Gu Q, et al. Ferroelectric properties of individual barium titanate nanowires investigated by scanned probe microscopy [J]. Nano Letters,2002,2: 447-450.
[12]Qiu J H, Ding J N, Yuan N Y, et al. Phase diagram and ferroelectric behaviors of BaTiO3 Nanowires [J]. Journal of Applied Physics,2011,109:054103.
[13]Rath M K, Pradhan G K, Verma H C, et al. Synthesis, characterization and dielectric properties of europium-doped barium titante nanopowders [J]. Materials Letters,2008, 62:2136-2139.
[14]Du XH, Wang Q M, Belegundu U, et al. Crystal orientation dependence of piezoelectric properties of single crystal barium titante [J]. Materials Letters,1999,40:109-113.
[15]Kishi H, Mizuno Y, Chazono H. Base-metal electrode-multilayer ceramic capacitors:Past, Present and Future perspective [J]. Japanese Journal of Applied Physics,2003,42: 1-15.
[16]Scott J F. Applications of modern ferroelctrics [J]. Science,2007,315:954-959.
[17]Yuk J, Troczynski T. Sol-gel BaTiO3 thin film for humidity sensors [J]. Sensors and Actuators B,2003,94:290-293.
[18]Wang L J, He Y, Hu J H, et al. DC humidity sensing properties of BaTiO3 nanof iber sensors with different electrode materials [J]. Sensors and Actuators B,2011,153:460-464.
[19]Bernard J, Houivet D, Fallah J E, et al. MgTiO3 for Cu base metal multilayer ceramic capacitors [J]. Journal of the European Ceramic Society,2004,24:1877-1881.
[20]Bernard J, Belnou F, Houivet D, et al. Low sintering temperature of MgTiO3 for type I capacitors [J]. Journal of the European Ceramic Society,2005,25:2779-2783.
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