利用FeAl下底层在低温条件下制备L10相FePt纳米颗粒

用FeAl合金作为下底层,用MgO作为中间层,在MgO（001）基片上生长了FePt薄膜．对FeAl下底层在300℃以上进行热处理,可以使其相结构转变为有序的B2相．热处理温度为400℃时,FeAl下底层内因热运动产生的空位没有在表面发生聚集,因而其表面最为平整．由于MgO,FeAl和FePt三者间良好的晶格匹配关系,使得FePt薄膜的生长具有垂直取向．FeAl下底层可以有效地降低FePt薄膜的相转变温度,而MgO中间层可以有效地避免层问扩散．在400℃的较低温度条件下,获得了尺寸约为10nrn的垂直取向L10相FePt均匀颗粒,室温矫顽力达到～20kOe．这种薄膜有希望应用于垂直磁记录介质．     

沉积厚度对L10-FePt薄膜(001)织构和磁性的影响

采用直流磁控溅射方法在表面氧化的Si(001)基片上制备不同厚度的FePt薄膜, 并利用原子力显微镜(AFM)、 X射线衍射(XRD)和振动样品磁强计(VSM)表征样品的形貌、结构和磁性. 结果表明: 将薄膜样品在H₂气氛中经600 ℃退火1 h, 得到了L1₀-FePt薄膜; 薄膜具有(001)织构或明显的(001)取向生长, 随着沉积厚度
的增加, FePt的晶粒尺寸变大, 样品的有序化程度增大, (001)取向生长呈减弱的趋势; 样品均具有明显的垂直磁各向异性, 随着薄膜厚度的增加, 平行膜面矫顽力增大, 垂直膜面矫顽力先增大后减小, 当沉积厚度为10 nm时, 样品的垂直磁各向异性最佳.     

Ag/FePt/C薄膜的结构和磁性

采用直流和射频磁控溅射在Si(001)基片上制备Ag/FePt/C薄膜,并将其在不同温度下进行真空热处理,得到了具有高矫顽力的L10-FePt薄膜.利用X射线荧光(XRF)、X射线衍射(XRD)和振动样品磁强计(VSM)研究样品的成分、结构和磁性.结果表明,样品经400℃热处理后发生了无序—有序相转变,以Ag元素为底层可降低有序化温度,添加Ag和C可抑制晶粒生长.随着热处理温度的升高,FePt的晶粒尺寸和矫顽力逐渐增大,经600℃热处理后,样品中FePt的平均晶粒尺寸为14nm,垂直膜面和平行膜面的矫顽力分别为798.16kA/m和762.35kA/m.     

Structure and magnetic properties of [FePt／Ag]10 multilayer films

[FePt/Ag]10 multilayers were deposited on glass substrates by magnetron sputtering. After being annealed at 550℃ for 30 rain, the coercivities of [FePt/Ag]10 multilayer films were observably improved. Magnetic properties of[FePt/Ag]10 multilayer films are influenced by the Ag content. The highest coercivity is obtained for those multilayer films that the Ag content is about 25%. The analysis for the remanence curves shows that the lower FePt layer thickness is favorable for decreasing the intergranular interaction. Result of XRD shows that a thick Ag layer can enhance the intensity of FePt(001) peak. A magnetic activation volume of the order of 10^-24 m^3 is obtained by the measurement of magnetic viscosity, showing that it is promising to be ultrahigh density recording media.     

(001)取向FePt薄膜的有序化过程及磁性

在加热到400°C的MgO(001)单晶基片上,用磁控溅射法沉积了25 nm厚的FePt薄膜,在Ta=[500°C,800°C]温度范围进行5 h的热处理.用X射线衍射仪、振动样品磁强计和可外加磁场的磁力显微镜分析了薄膜的结构和磁性.结果表明,未经热处理的薄膜能够在MgO(001)单晶基片的诱导下实现(001)取向生长,但仍处于无序的A1相,呈软磁性.Ta=500°C,薄膜结构没有明显改变.Ta=600°C,FePt发生部分有序化,薄膜中A1相和L10相(有序相)共存,形成一种具有磁各向异性的特殊硬磁-软磁复合体.软磁相的磁性主要表现在沿平行于膜面方向施加磁场的磁化曲线中,但矫顽力可以达到10 kOe(1Oe=103/4πA m-1),硬磁相的磁性主要表现在沿垂直于膜面方向施加磁场的磁化曲线中,矫顽力却只有5kOe.这说明薄膜中硬磁相和软磁相之间存在强烈的交换耦合,形成了磁性弹簧.当Ta提高到700°C,薄膜基本完成有序化,磁化易轴彻底转向垂直于膜面的方向,矫顽力大于20 kOe.原子力显微镜和磁力显微镜观察表明,薄膜由岛状颗粒构成,在Ta=700°C时大部分颗粒内部形成多磁畴结构,在不太大的磁场作用下依靠畴壁移动和消失变为单磁畴,磁化反转过程应该主要依靠形核.     

在MgO(001)基板上生长连续的L10-FePt 纳米薄膜

用磁控溅射法在加热到400℃的MgO(001)基片上沉积了总厚度为25 nm 的[Fe(0.6 nm)/Fe_30.5Pt_69.5(1.9nm)]₁₀ 多层连续薄膜, 并对其在[500, 900]℃的温度范围进行了3h 的真空热处理. 结果表明, 薄膜在沉积过程中发生了层间扩散, 形成A1 相的FePt 合金, 表现为软磁特性; 热处理温度高于700℃时, 薄膜内形成L1₀ 相的(001)织构, 其单轴磁晶各向异性能高于2.5×10⁷ erg cc^-1; 薄膜能在800℃以下保持形貌连续. 借助于半导体载流子扩散和复合模型, 对薄膜在高温下形貌保持连续的机理进行了探讨. 分析认为, 虽然薄膜在沉积过程中发生了层间扩散, 但内部仍然残存微弱的周期性成分起伏, 这可以有效阻碍热处理过程中因相变而引起的Pt 元素析出, 从而抑制了因形成富Pt 晶界而导致的形貌不连续. 这种薄膜可以方便地用于微加工制作磁性阵列和隧道结.     

Synthesis and magnetic properties of Fe<Subscript>3</Subscript>O<Subscript>4</Subscript>/helical carbon nanofiber nanocomposites from the catalytic pyrolysis of ferrocene

High purity Fe3O4 /helical carbon nanofiber composites were obtained on a large scale by the catalytic pyrolysis of ferrocene in the presence of tin powder at 500°C over 12 h. The sizes of Fe 3 O 4 nanoparticles are 35–65 nm in size, and the diameters of the helical carbon nanofibers range from 40–70 nm. The shapes and compositions of the nanocomposites are simply controlled by adjusting the reaction temperatures. On the basis of the obtained experimental results the formation of the helical Fe3O4/carbon nanofiber composites was investigated and discussed. The magnetic hysteresis loop of the products shows ferromagnetic behavior with saturation magnetization (M s ), remanent magnetization (M r ) and coercivity (H c ) values of ca. 29.8 emu/g, 9.6 emu/g and 306.6 Oe, respectively.     

Research on C<Subscript>3</Subscript>N<Subscript>4</Subscript> superhard compound thin film and its application

By combination of DC reactive magnetron sputtering with multiple arcplating, the alternating C₃N₄/TiN compound film is deposited onto HSS. The core level binding energy and the contents of carbon and nitrogen are characterized by X-ray photoelectron spectrum. X-ray diffraction (XRD) shows that compound thin film contains hard crystalline phases of α-C₃N₄ and β-C₃N₄. The Knoop microhardness in the load range of 50, 5–54, 1 GPa is measured. According to acoustic emission scratch test, the critical load values for the coatings on HSS substrates are in the range of 40–80 N. The metal coated with C₃N₄/TiN compound films has a great improvement in the resistance against corrosion. Many tests show that such a coating has a very high wearability. Compared with the uncoated and TiN coated tools, the C₃N₄/TiN coated tools have a much longer cutting life. Foundation item: Supported by the National Natural Science Foundation of China (19875037) Biography: Wu Da-we( (1941-), male, Professor, research direction; thin film and its application.     

Synthesis and characterization of wormhole-like mesoporous Ce0.6Zr0.35Y0.05O2 solid solutions

Nanoparticles of Ce0.6Zr0.35Y0.05O2 (CZY) solid solution have been prepared by the CTAB (hexadecyl-trimethyl ammonium bromide), CTAB-EG (ethylene glycol) templating, and CTAB-EG-NaCl (in which the pores of the precursor synthesized by the CTAB-EG method is filled by a certain amount of NaCl) method, respectively. The physical properties of these materials were characterized by means of tech-niques such as X-ray diffraction (XRD), high resolution scanning electron microscopy (HRSEM), transmission electron microscopy (TEM), selected area electron diffraction (SAED), and N2 adsorp-tion-desorption measurements. The CZY samples synthesized by the above three methods display wormhole-like mesoporous morphology and cubic crystal structures. The materials are narrow in pore size distribution (averaged pore diameter = 5.3―7.1 nm), high in surface areas (95―119 m2/g), and large in pore volumes (0.16―0.18 cm3/g). It has been demonstrated that the introduction of NaCl is capable of retaining the pore structures of solid nanomaterials at high-temperature calcination.     

Nd<Subscript>2</Subscript>Fe<Subscript>17</Subscript> nanograins effect on the coercivity of HDDR NdFeB magnets with low boron content

Relationships between the coercivity of hydrogenation disproportionation desorption recombination (HDDR) Nd_12.5Fe_81.5−x Co₆B _x bonded magnets and boron content were investigated. Nd₂Fe₁₇ phase with planar magnetic anisotropy is present in the microstructure when x= 4at%–5.88at%, which does not reduce the coercivity of the bonded magnets. High-resolution transmission electron microscopy (TEM) images show that Nd₂Fe₁₇ phase exists in the form of nanocrystals in the Nd2Fe14B matrix. There is an exchange-coupling interaction between the two phases so that the coercivity of HDDR Nd_12.5Fe_81.5−x Co₆B _x bonded magnets is hardly reduced with a decrease in boron content.     

Photoluminescence and cathodoluminescence properties of CaLaGa<Subscript>3</Subscript>O<Subscript>7</Subscript>:Eu<Superscript>3+</Superscript> phosphors

The CaLaGa₃O₇:Eu³⁺ phosphor was prepared by a chemical co-precipitation method. Field emission scanning electron microscopy (FE-SEM), laser particle size analysis, X-ray diffraction (XRD), photoluminescence (PL), and cathodoluminescence (CL) spectra were utilized to characterize the synthesized phosphor. The results revealed that the phosphor was composed of microspheres with a slight agglomerate phenomenon and was spherically shaped. The average grain size was about 1.0 μm. Eu³⁺ ions, as luminescent centers, substituted La³⁺ ions into the single crystal lattice of CaLaGa₃O₇ with the sites of C_s. Although the CL spectrum was greatly different from the PL spectrum, it had the strongest red emission corresponding to the ⁵D₀ →⁷F₂ transition of Eu³⁺. Under the excitation of UV light (287 nm) and electron beams (1.0–7.0 kV), the chromaticity coordinates of the phosphor were found to be in the nearly red and orange light regions, respectively.     

Electrical conductivity optimization of the Na3AlF6-Al2O3-Sm2O3 molten salts system for Al-Sm intermediate binary alloy production

Metal Sm has been widely used in making Al-Sm magnet alloy materials. Conventional distillation technology to produce Sm has the disadvantages of low productivity, high costs, and pollution generation. The objective of this study was to develop a molten salt electrolyte system to produce Al-Sm alloy directly, with focus on the electrical conductivity and optimal operating conditions to minimize the energy consumption. The continuously varying cell constant (CVCC) technique was used to measure the conductivity for the Na₃AlF₆-AlF₃-LiF-MgF₂-Al₂O₃-Sm₂O₃ electrolysis medium in the temperature range from 905 to 1055℃. The temperature (t) and the addition of Al₂O₃ (W(Al₂O₃)), Sm₂O₃ (W(Sm₂O₃)), and a combination of Al₂O₃ and Sm₂O₃ into the basic fluoride system were examined with respect to their effects on the conductivity (κ) and activation energy. The experimental results showed that the molten electrolyte conductivity increases with increasing temperature (t) and decreases with the addition of Al₂O₃ or Sm₂O₃ or both. We concluded that the optimal operation conditions for Al-Sm intermediate alloy production in the Na₃AlF₆-AlF₃-LiF-MgF₂-Al₂O₃-Sm₂O₃ system are W(Al₂O₃) + W(Sm₂O₃)=3wt%, W(Al₂O₃):W(Sm₂O₃)=7:3, and a temperature of 965 to 995℃, which results in satisfactory conductivity, low fluoride evaporation losses, and low energy consumption.     

Microwave sintering of Ca<Subscript>0.6</Subscript>La<Subscript>0.2667</Subscript>TiO<Subscript>3</Subscript> microwave dielectric ceramics

Ca_0.6La_0.2667TiO₃ ceramics were prepared by conventional and microwave sintering techniques and their sinterability, microstructure, and microwave dielectric properties were investigated in detail for comparison. Densified Ca_0.6La_0.2667TiO₃ ceramics were obtained by microwave sintering at 1350°C for 30 min and by conventional sintering at 1450°C for 4 h. An unusual phenomenon was found that some larger grains (grain size range: 8–10 μm) inclined to assemble in one area but some smaller ones (grain size range: 2–4 μm) inclined to gather in another area in the microwave sintered ceramics. The microwave dielectric properties of Ca_0.6La_0.2667TiO₃ ceramics prepared by microwave sintering at 1350°C were as follows: dielectric constant (ɛ _r) = 119.6, quality factor (Qf) = 17858.5 GHz, and temperature coefficient of resonant frequency (τ _f) = 155.5 ppm/°C. In contrast, the microwave dielectric properties of the ceramics prepared by conventional sintering at 1450°C were ɛ _r = 117.4, Qf = 13375 GHz, and τ _f = 217.2 ppm/°C.     

溶胶-凝胶法制备FePt纳米颗粒及其性质研究

通过溶胶-凝胶法制备了L10相FePt纳米颗粒,并利用X射线衍射(XRD)、振动样品磁强计(VSM)、透射电子显微镜(TEM)等测试手段对所制备的样品进行了结构和磁性表征.XRD及TEM分析表明,700℃所制备的FePt纳米颗粒为面心四方(FCT)结构,颗粒形状为球形且分散性较好,晶粒尺寸约为12 nm.磁性测试结果表明,L10相的FePt纳米颗粒室温下具有铁磁性,其矫顽力为1 887 Oe.     

Multi-color long-lasting phosphorescence of rare earth ions in CdSiO<Subscript>3</Subscript> matrix

A series of rare earth ions doped CdSiO3:RE^3 (RE=Y, La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho,Er, Tin, Yb, Lu) multi-color long-lasting phosphorescence phosphors are prepared by the conventional hightemperature solid-state method. The results of XRD measurement indicate that the products fired under 1050~C for 3h have a good crystallization without any detectable amount of impurity phase. Rare earth ions doped CdSiO3 phosphors possess excellent Inmiuescence properties. When rare earth ions such as Y^3 , La^3 , Gd^3 , Lu^3 , Ce^3 , Nd^3 , Ho^3 , Er^3 ,Tm^3 and Yb^3 are introduced into the CdSiO3 host, one broadband centered at about 420 nm resulting from traps can be observed. In the case of other earth ions such as Pr^3 ,Sm^3 , Eu^3 , Tb^3 and Dy^3 , their characteristic line emitting as well as the -420 nm broadband luminescence can be obtained. The mixture of their characteristic line emitting with the -420 nm broadband Inminescence results in various afterglow color.     

Synthesis and Magnetic Properties of Spin-Liquid Tb2Ti2O7

Polycrystalline samples of a novel spin-liquid compound Tb2Ti2O7 were prepared by a standard solid-state reaction. X-ray diffraction at room temperature confirms that the synthesized compound of Tb2Ti2O7 is single phase with cubic unit cell constant a0 of 1.015 44 nm. Magnetic susceptibility measurements in the temperature range between 100 and 300 K give an effective moment of 9.44 μB and Curie-Weiss temperature of 12.68 K, respectively, indicating the dominance of antiferromagnetic interactions. However, below 50 K, the magnetic behavior of Tb2Ti2O7 deviates from Curie-Weiss law, whose origin remains suspicion.     

Highly <Emphasis Type="Italic">C</Emphasis>-axis oriented LiNbO<Subscript>3</Subscript> thin film on amorphous SiO<Subscript>2</Subscript> buffer layer and its growth mechanism

LiNbO3 waveguiding films with highly C-axis orieatation and superior crystallographic quality have been deposited on the amorphous SiO2 buffer layer of Si wafer by pulsed laser deposition (PLD) technique. X-ray diffraction,high-resolution electron transmission microscopy and atomic force microscopy were applied to characterizing the quality and orientaion of LiNbO3 thin film, and the optimized depositioa coaditioas have been determined for C-axis oriented growth. LiNbO3 thin films on amorphous SiO2 buffer layer were composed of intimate arrangements of quadrangular single crystal domain (150 nm x 150 nm) with C-axis orientatioa, and displayed sharp interface structures. The measurements of prism coupling technique indicate that the laser can be coupled into the LiNbO3 film and TE and TM waveguiding modes were detected. In addition, the possible mechanism of oriented growth on amorphous buffer layer and “film-substrate effects“ were discussed briefly, which suggests that its growth mechanism is likely analogous to the Voimer model with characteristics of three-dimensional islands nucleation on the smooth crystal surface.     

Structural and electrical properties of HCl-polyaniline-Ag composites synthesized by polymerization using Ag-coated (NH4)2S2O8 powder

Ag nanoparticles were sputter-deposited on ammonium persulfate ((NH₄)₂S₂O₈) powder to obtain (NH₄)₂S₂O₈-Ag powder, which was used to synthesize the HCl-doped polyaniline-Ag (HCl-PANI-Ag) composite via a polymerization procedure. The Ag nanoparticles were dispersed in the HCl-PANI matrix, and their sizes mainly ranged from 3 to 6 nm. The Ag nanoparticles did not affect the structure of emeraldine salt in the composite, and they increased the ordered crystalline regions in the HCl-PANI matrix. The HCl-PANI-Ag composite had a conductivity of (6.8 ±0.1) S/cm, which is about four times larger than that of the HCl-PANI. The charge transport mechanism in the composite is explained by the three-dimensional Mott variable-range hopping (3D-Mott-VRH).     

Preparation and radar-absorbing properties of Al<Subscript>2</Subscript>O<Subscript>3</Subscript>/TiO<Subscript>2</Subscript>/Fe<Subscript>2</Subscript>O<Subscript>3</Subscript>/Yb<Subscript>2</Subscript>O<Subscript>3</Subscript> composite powder

Al₂O₃/TiO₂/Fe₂O₃/Yb₂O₃ composite powder was synthesized via the sol-gel method. The structure, morphology, and radar-absorption properties of the composite powder were characterized by transmission electron microscopy, X-ray diffraction analysis and RF impedance analysis. The results show that two types of particles exist in the composite powder. One is irregular flakes (100-200 nm) and the other is spherical Al₂O₃ particles (smaller than 80 nm). Electromagnetic wave attenuation is mostly achieved by dielectric loss. The maximum value of the dissipation factor reaches 0.76 (at 15.68 GHz) in the frequency range of 2-18 GHz. The electromagnetic absorption of waves covers 2-18 GHz with the matching thicknesses of 1.5-4.5 mm. The absorption peak shifts to the lower-frequency area with increasing matching thickness. The effective absorption band covers the frequency range of 2.16-9.76 GHz, and the maximum absorption peak reaches -20.18 dB with a matching thickness of 3.5 mm at a frequency of 3.52 GHz.     

Giant magneto-optical faraday effect of nanometer Fe-In<Subscript>2</Subscript>O<Subscript>3</Subscript> granular films

The giant magneto-optical Faraday effect of nanometer ferromagnetic metal-semiconductor matrix Fe-ln2O3 granular films prepared by the radio frequency sputtering are studied. The result shows that the Faraday rotation angle θF value of the granular film samples with Fe volume fraction x = 35% is of the order of 10^5（°）/cm at room temperature. Temperature dependence of the Faraday rotation angle θF of Fe0.35（In2O3）0.65 granular films shows that θF value below 10 K increases rapidly with the decrease of the temperature, and when T= 4.2 K, θF value is 106（°）/cm. Through the study of the dependence of low field susceptibility on temperature and the hysteresis loops at different temperatures, it has been found that when the temperature decreases to a critical point Tp = 10 K, the transformation of state from ferro-agnetic to spin-glass-like occurs in Fe0.35（In2O3）0.65 granular films. The remarkable increase of the Faraday rotation angle θF value of Fe0.35（In2O3）0.65 granular films below 10 K seems to arise from the sp-d exchange interaction of the granular film samples in the spin-glass-like state.