Synthesis of MnZn Ferrite Nanoscale Particles by Hydrothermal Method

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Effects of La~(3 ) doping on MnZn ferrite nanoscale particles synthesized by hydrothermal method

1　INTRODUCTIONMnZnferritesarewidelyusedinelectronicappli cationsbecauseoftheirhigh permeabilityandlowmagneticlossesathighfrequencies[1,2 ] .Theproper tiesofferritesdependlargelyontheirmicrostructure ,sothenano techniqueisintroducedtocontroltheirultramicrostructure ,insteadofthetraditionalceramicway .Additionally ,aprecisesmallamountofcationicsubstitutionisusedusually .ThemagneticlossofMnZn ferritesdopedwithCaO SiO2 athighfrequencyisdiminishedforincreasesofresistivitylayersatgrainbound…     

Effects of La^3＋ doping on MnZn ferrite nanoscale particles synthesized by hydrothermal method

MnZn ferrite nanoscale particles were synthesized by hydrothermal method. The effects of amount of addition La³⁺ on the products were discussed. The product was characterized by X-ray diffraction (XRD) and transmission electron microscope (TEM). The results show that the sample with 0.2% La³⁺ (mass fraction) or without La³⁺ has only spinel phase, but the sample with mass fraction of La³⁺ exceeding 0.4% posses second phase besides the spinel one; and the nano-MnZn ferrites change from cube to hexagon when the mass fractions of La³⁺ is up to 1.2%. TEM image of the sample with 1.2% La³⁺ indicates that the homogeneous hexagonal crystal is obtained and the particles are larger than those of undoped; the addition of La³⁺ has great influence on the crystallization of hydrothermal process and can change the shape of particles and improve their growth. The saturation magnetization of the sample with 1.2% La³⁺ (2.64 A · m² · kg⁻¹) is lower than that of undoped (17.54 A · m² · kg⁻¹) and it behaves superparamagnetically. Foundation item: Project (2001BA90A09) supported by the Tenth Five-Plan of China     

高磁导率MnZn铁氧体的研究进展

MnZn铁氧体是一种重要的磁性材料.20世纪30年代以来,由于该材料固有的特性,人们对这种材料产生了浓厚的兴趣,并开展了广泛的研究.MnZn铁氧体的磁学性能与该材料的成份和组织有着密切的关系,MnZn铁氧体的制备方法也对其性能有着显著的影响.介绍了高(μMnZn铁氧体的研发历史和该材料在信息产业发展过程中的意义和作用,同时从配方优化、烧结工艺、测试方法等方面综述了目前国内外的研究与发展现状.通过对MnZn铁氧体的研究进展的总结,将有助于对高性能磁性材料开展深入的研究.     

预烧温度对高磁导率MnZn铁氧体性能的影响

采用氧化物法陶瓷工艺制备高磁导率MnZn铁氧体材料,经过电镜扫描,得到烧结样品的微观结构。针对高性能的高磁导率MnZn铁氧体材料,分析了不同预烧温度对高磁导率MnZn铁氧体微观结构及电磁性能的影响,研究了MnZn铁氧体微观结构对其磁导率的影响,得到了高磁导率MnZn铁氧体材料最佳预烧温度为960℃,及良好的微观结构有利于降低比损耗。960℃预烧样品经过1 400℃气氛烧结,可得到磁导率为9 500左右的高性能高导MnZn铁氧体材料。     

Surfactant-assisted synthesis and magnetic properties of monodispersed manganese ferrite nanocrystals

Monodispersed manganese ferrite (MnFe₂O₄) nanocrystals could be successfully synthesized in large quantities via a facile synthetic technique based on the pyrolysis of organometallic compound precursor, in which octadecene was used as solvent, and oleic acid and oleylamine were used as capping ligands. MnFe₂O₄ nanocrystals were obtained with size in a tunable range of 4–15 nm and their morphologies could be tuned from spherical to triangle-shaped by varying the surfactants. The phase structure, morphology, and size of the products were characterized in detail by X-ray diffraction (XRD) and transmission electron microscopy (TEM). Magnetic properties of MnFe₂O₄ nanocrystals with different morphologies were measured using a superconducting quantum interference device (SQUID). Both monodisperse MnFe₂O₄ nanocrystals with spherical and triangle-shapes are superparamagnetic at room temperature while ferromagnetic at 2 K. The pyrolysis method may provide an effective route to synthesize other spinel ferrites or metal oxides nanocrystals.     

Morphologies of hydroxyapatite nanoparticles adjusted by organic additives in hydrothermal synthesis

Properties of hydroxyapatite (HA, Ca₁₀(PO₄)₆(OH)₂), including bioactivity, biocompatibility, solubility and adsorption could be tailored over wide ranges by the control of particle composition, particle size and morphology. In order to satisfy various applications, well-crystallized pure HA nanoparticles were synthesized at moderate temperatures by hydrothermal synthesis, and HA nanoparticles with different lengths were obtained by adding organic additives. X-ray diffractometry (XRD) and Fourier transform infrared (FTIR) spectrometry were used to characterize these nanoparticles, and the morphologies of the HA particles were observed by transmission electron microscopy (TEM). The results demonstrate that shorter rod-like HA particles can be prepared by adding cetyltrimethylammonium bromide (CTAB), as the additive of CTAB can block the HA crystal growth along with c-axis. And whisker HA particles are obtained by adding ethylenediamine tetraacetic acid (EDTA), since EDTA may have effect on the dissolution-reprecipitation process of HA.     

Co-precipitation/hydrothermal synthesis of BiFeO<Subscript>3</Subscript> powder

A coprecipitation/hydrothermal route was utilized to fabricate pure phase BiFeO3 powders using FeCl3·6H2O and Bi（NO3）3·5H2O as starting materials, ammonia as precipitant and NaOH as mineralizer. The synthesized powders were characterized by XRD, SEM and DSC-TG analysis. In the process, single-phase BiFeO3 powders could be obtained at a hydrothermal reaction temperature of 180 ℃, with NaOH of 0.15 mol/L, in contrast to 200 ℃ and 4 mol/L for conventional hydrothermal route. Meanwhile, the micro-morphology of synthesized BiFeO3 powders changed with different reaction temperatures and concentrations of NaOH. The N6el temperature, Curie temperature and decomposition temperature of the synthesized BiFeO3 powders were detected to be 301 ℃, 828 ℃ and 964 ℃, respectively. The hydrothermal reactions mechanism to fabricate BiFeO3 powders were discussed based on the in-situ transformation process.     

Coalescence of the crystallites under hydrothermal conditions (II)

Cuprite (Cu₂O) particles are synthesized by hydrothermal method. Most crystalline particles have long column morphology. Particles which are regarded as assembling of the crystallites in definite directions are observed. The typical example is the particles formed by assembling six columns in three perpendicular directions. The cone surfaces are visible at the tops of the columns. The results revealed that the coalescence of the crystallites did happen under hydrothermal conditions in which the crystallite connected with other crystallite on certain structure compatible surfaces to form a crystalline particle with a special morphology. This phenomenon is called the second kind of coalescence. The Cu₂O structure unit is determined by its crystal structure. It is concluded that the tetragonal prism and three tetragonal prism-like growth units are the favorable units after stability energy calculation was performed on different kinds of growth units. It is believed that the first kind of coalescence exists commonly. The second kind of coalescence is unlikely to occur for all crystallites under hydrothermal conditions. The occurrence is dependent on the crystal structure.     

六方相NaEuF4纳米纺锤体和纳米棒的水热控制合成

通过一种简单的水热方法,在较低的温度下合成了六方相NaEuF4纳米纺锤体和纳米棒.通过对F^-/Eu^3＋摩尔比、母体溶液pH值和反应时间的控制,实现了对产物形貌的控制合成.用X射线衍射仪（XRD）、透射电子显微镜（TEM）、高分辨电子显微镜（HRTEM）等对样品的形貌和晶体结构进行表征.结果显示,反应条件对其形貌和尺寸的影响很大,添加的螯合剂EDTA对产物形貌和纯度至关重要.用稳态荧光光谱仪分析其光学性能,在室温下观察到了橙色和红色发光.     

The growth units and hydrothermal preparation of lead tungstate (PbWO4) crystallites

The crystal structure of lead tungstate (PbWO4) can be regarded as ordered combination of the tungsten oxide tetrahedrons (WO4) and lead ions (Pb2 ). According to the growth unit model, the growth units of lead tungstate are the aggregations of the tungsten oxide tetrahedrons and lead cations with various geometry configurations. It is suggested that the favorable growth units of lead tungstate crystal are pyramidal, tetragonal prism and quadrangular units corresponding to geometric orientations of the simple forms of the crystal. Under low restricted growth conditions, the growth form of lead tungstate crystallites is the aggregation of the geometric configurations of these favorable growth units. The above conclusions are completely confirmed by the experiment on hydrothermal preparation of lead tungstate crystallites.     

利用飞秒光谱研究CdTe纳米晶的超快动力学

利用飞秒时间分辨瞬时吸收光谱技术,研究了甲苯溶液中CdTe纳米晶的超快动力学过程.结果表明,CdTe的最大吸收强度随泵浦光强线性变化,这说明在所用泵浦光强下,样品没有发生光退化.当固定泵浦光强时,测量得到的不同光学密度时的瞬时吸收光谱可以用双指数函数很好地拟合,这意味着CdTe中的载流子弛豫过程主要包含两个过程,分别为较快的表面态电子俘获过程和较慢的表面态电子与价带底空穴的复合过程.实验结果表明,当光学密度增加时较快过程的弛豫时间随光学密度的增加而增加,这是由于CdTe纳米晶间的相互作用增强,阻碍了能量向周围溶剂的扩散;而较慢过程的弛豫时间却是减小的,这是由光学密度对CdTe纳米晶表面态的影响导致的.     

Pr6O11对SrFe12O19磁性能的影响及作用机理

为了探讨稀土氧化物Pr₆O₁₁作为添加剂对M型锶永磁铁氧体磁性能的影响及其作用机理，以添加稀土氧化物Pr₆O₁₁的BMS-4永磁铁氧体预烧料(SrFe₁₂O₁₉)作为原料，经过球磨、沉淀、成型、烧结等工艺制成样品.采用扫描电镜、磁性材料自动测试装置、沉降粒度测试仪、X射线衍射仪等分析测试仪对样品进行了性能检测和物相分析.结果表明：Pr³⁺离子部分取代了Sr²⁺离子，而具有4f²电子组态的Pr³⁺离子提供了3.58μB自旋向上的磁矩，并起到抑制晶粒增长的作用，可明显改善M型锶永磁铁氧体的磁性能.     

水热晶化法制备纳米TiO2的动力学研究

用水热晶化法一步制得D101晶面尺寸为10～16 nm的具有较好结晶度的锐钛矿型的纳米TiO2.XRD结果和热力学分析表明,当水热晶化温度控制在体系的沸点时,所得到的锐钛矿型纳米TiO2的粒度最小.用水热晶化法制得的具有锐钛矿型纳米TiO2在100 ℃焙烧后就开始向金红石型转变.起始相变温度大大地低于文献报道的250 ℃.从而有效地避免了高温焙烧制备金红石型TiO2过程中的粒子团聚现象.动力学分析表明,在实验温度范围内(100～800 ℃)焙烧,低温段(t<500 ℃)的晶粒生长速率大于高温段(t>500 ℃)的晶粒生长速率.其晶粒生长表观活化能分别为:当t<500 ℃时,EA(锐钛矿)＝18.76 KJ/mol,ER(金红石)=38.49 KJ/mol;当t>500 ℃时,EA(锐钛矿)＝70.76 KJ/mol,ER(金红石)=75.66 KJ/mol.低温段(t<500 ℃)有利于锐钛矿型晶粒的生长,相比较而言,高温比低温更有利于金红石型晶粒的生长.     

Coalescence of the crystallites under hydrothermal conditions (II) —— The morphology and stability energy calculation of cuprite

The coalescence of crystallite under hydrothermal conditions was discussed in our previous paper[1]. When the solute concentration exceeds the supersaturation, the nucleation and growth process take place. The initial crystallites are only several nanometers. They have high surface-to-volume ratio, high index surfaces, and therefore have high surface energy. As the hydrothermal reactions proceed in the alkaline medium, the crystallite surfaces are apt to absorb polar solvate ions such as OH-,…     

Effects of oxalic acid addition on the hydrothermal synthesis of kaolinite

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Effect of acicular ferrite on banded structures in low-carbon microalloyed steel

The effect of acicular ferrite （AF） on banded structures in low-carbon microalloyed steel with Mn segregation during both iso- thermal transformation and continuous cooling processes was studied by dilatometry and microscopic observation. With respect to the iso- thermal transformation process, the specimen isothermed at 550℃ consisted of AF in Mn-poor bands and martensite in Mn-rich bands, whereas the specimen isothermed at 450℃ exhibited two different morphologies of AF that appeared as bands. At a continuous cooling rate in the range of 4 to 50℃/s, a mixture of AF and martensite formed in both segregated bands, and the volume fraction of martensite in Mn-rich bands was always higher than that in Mn-poor bands. An increased cooling rate resulted in a decrease in the difference of martensite volume fraction between Mn-rich and Mn-poor bands and thereby leaded to less distinct microstrucmral banding. The results show that Mn segregation and cooling rate strongly affect the formation of AF-containing banded structures. The formation mechanism of microstructural banding was also discussed.