Grain Refining and Decoupling in FePt/SiO2 Nanogranular Films for Magnetic Recording

FePt/SiO₂ nanogranular thin films have been prepared by molecular-beam epitaxy system on MgO (001) substrates with the method of insertion dual SiO₂ layers into Fe/Pt multilayer films. We report the relationships between the inserting thickness of SiO₂ layers and the microstructural and magnetic properties of FePt thin films. It indicated the nanogranular FePt thin films were successfully formed by inserting amorphous SiO₂ layers into the Fe/Pt films. The reduction of grain/domain size and isolation of FePt particles can be achieved by such insertion and maintain (001) texture. The average grain size of FePt films with 5-nm SiO₂ insert layers is estimated to be around 8 nm, while domain rotation is enhanced depicting a decoupling of intergrain interaction. The isolated grains are less magnetically coupled in the rotation mode and the reversal of magnetization is more independent     

SiO2/聚四氟乙烯复合薄膜的制备及力学性能

采用空气辅助干法共混、冷压烧结并车削成膜的方法制备了SiO₂填充量为35wt%、厚度为50 μm的聚四氟乙烯（PTFE）基复合薄膜。系统研究了SiO₂颗粒粒径对SiO₂/PTFE薄膜复合材料的孔洞缺陷和力学性能等的影响,并研究了SiO₂在PTFE中的分散情况及分子间相互作用对其性能变化的影响机制。结果表明,随SiO₂粒径的逐渐增大,其在PTFE中的分散趋于均匀,同时PTFE能更好地包覆粒子,因此SiO₂/PTFE薄膜孔洞缺陷逐渐减少,力学性能逐渐增强;当SiO₂的粒径D₅₀为12 μm时,其在PTFE中的分散均匀性最佳,SiO₂/PTFE复合薄膜孔洞缺陷最少,具有较好的力学性能,断裂伸长率达19.5%,拉伸强度达9.2 MPa。      

SiO2-TiO2/聚四氟乙烯复合材料的制备及热膨胀性能

为了使微波基板材料与Cu金属衬底的热膨胀性能匹配,对陶瓷/聚四氟乙烯（PTFE）微波复合基板材料的热膨胀性能进行了研究。采用湿法工艺制备了以SiO₂和TiO₂为填料的SiO₂-TiO₂/PTFE复合材料,研究了复合材料密度、填料粒度和填料体积分数对SiO₂-TiO₂/PTFE复合材料热膨胀性能的影响。结果表明,当SiO₂的体积分数由0增至40%（TiO₂ ：34%~26%）时,SiO₂-TiO₂/PTFE复合材料的线膨胀系数（CTE）由50.13×10^-6 K^-1减小至10.03×10^-6K^-1。陶瓷粉体粒径和复合材料密度减小会导致CTE减小。通过ROM、Turner和Kerner模型计算CTE发现,ROM和Kerner模型与实验数据较相符,而实验值与Turner模型预测值之间的差异随PTFE含量的升高而逐渐增大。     

Low temperature ordering of FePt films by in-situ heating deposition plus post deposition annealing

FePt thin films with 40 nm thickness were prepared on thermally oxidized Si (001) substrates by dc magnetron sputtering at the nominal growth temperature 375 °C. The effects of annealing on microstructure and magnetic properties of FePt thin films were investigated. The as-deposited FePt thin films show soft magnetic properties. After the as-deposited FePt thin films were annealed at various temperatures and furnace cooled, it is found that the ordering temperature of L1₀ FePt phase could be reduced to 350 °C. For FePt thin films annealed at 350 °C, the in-plane and out-of-plane coercivities of the films increased to 510 and 543 kA/m, respectively, and the films had hard magnetic properties. A highly (001) orientation was obtained, when FePt thin films were annealed at 600 °C. And the hysteresis loops of FePt thin films annealed at 600 °C show out-of-plane magnetic anisotropy.     

Texture of copper films on Ta35Si18N47 and Ti33Si23N44 underlayers

The crystallographic texture and the grain size have been measured by X-ray diffraction techniques for about 200 nm-thick Cu films sputter-deposited on amorphous Ta₃₅Si₁₈N₄₇ and Ti₃₃Si₂₃N₄₄ underlayers, and for comparison also on TiN underlayers and oxidized silicon, all on Si (100) substrates. The (111) texture of the as-deposited Cu films increases in the sequence TiN233Si₂₃N₄₄35Si₁₈N₄₇. Amorphous Ta₃₅Si₁₈N₄₇ and Ti₃₃Si₂₃N₄₄ layers evidently promote quite effectively the growth of highly (111) textured Cu films. After vacuum annealing at 450°C for 30 min the texture of Cu rises on Ti₃₃Si₂₃N₄₄, falls on Ta₃₅Si₁₈N₄₇, while that on TiN and on SiO₂ changes little and the sequence becomes TiN235Si₁₈N₄₇33Si₂₃N₄₄. The grain size of the as-deposited Cu films increases in the sequence Ti₃₃Si₂₃N₄₄235Si₁₈N₄₇47N₅₃ and rises moderately upon annealing, least for TiN and most for SiO₂ and Ti₃₃Si₂₃N₄₄.     

Deposition of HfO2 thin films on ZnS substrates

HfO₂ thin films with columnar microstructure were deposited directly on ZnS substrates by electron beam evaporation process. SiO₂ thin films, deposited by reactive magnetron sputtering, were used as buffer layers, HfO₂ thin films of granular microstructure were obtained on SiO₂ interlayer by this process. X-ray diffraction patterns demonstrate that the as-deposited HfO₂ films are in an amorphous-like state with small amount of crystalline phase while the HfO₂ films annealed at 450 °C in O₂ for 30 min and in Ar for 150 min underwent a phase transformation from amorphous-like to monoclinic phase. Antireflection effect in certain infrared wave band, such as 3–6 μm, 4–12 μm, 4–8 μm and 3–10 μm, can be observed, which was dependent on the thickness of thin films. The cross-sectional images of HfO₂ films, obtained by field emission scanning electron microscopy, revealed that there was no distinct morphological change upon annealing.     

Modeling and characterization of viscoelasticity of PI/SiO2 nanocomposite films under constant and fatigue loading

In this paper, the viscoelastic behavior of PI/SiO₂ nanocomposite thin films under constant and fatigue tensile loading was studied. The cyclic hardening and viscous dissipation of PI/SiO₂ nanocomposite thin films during the fatigue process were experimentally investigated and analyzed by storage modulus, loss modulus and phase lag. The time-dependent deformation under constant and fatigue loading was simulated based on two viscoelastic models known as Burger model and Findley power law. Standard parameter analysis methodology was employed to interpret the structure–property relationship and deformation mechanisms of this kind of nanocomposites. In addition, the effects of nano-silica content, stress level and loading pattern (constant or fatigue loading) on the creep resistance of materials were discussed as well.     

强磁靶共溅射法制备具有室温磁电阻特性的Co-TiO2纳米复合薄膜

Co-TiO₂纳米复合薄膜作为一种新型自旋电子材料, 由于具有良好的生物相容性, 近年来受到广泛关注。但在制备过程中, 磁性金属Co处于氧化气氛, 容易部分氧化, 从而影响薄膜的隧道磁电阻性能。为了抑制磁性金属的氧化, 提高金属态含量, 本研究通过强磁靶共溅射法制备了Co-TiO₂纳米复合薄膜。该方法采用的强磁靶头, 磁场强度高、分布均匀, 可以提高溅射粒子的能量和溅射速率, 降低因高能粒子碰撞而发生氧化的概率。因此强磁靶共溅射法能明显抑制金属Co的氧化, 提高纳米复合薄膜的自旋极化率。所制备的Co-TiO₂纳米复合薄膜主要由非晶态的TiO₂基体和分散其中的Co颗粒组成。通过调节金属Co颗粒尺寸和分布状态, 在电学上实现了金属态向绝缘态转变, 在磁学上实现了铁磁性向超顺磁性转变。Co含量为51.3at%时, Co-TiO₂纳米复合薄膜表现为高金属态和高电阻率, 并且实现了高达8.25%的室温隧道磁电阻。强磁靶共溅射法使Co-TiO₂纳米复合薄膜的室温磁电阻性能得到了进一步提高, 这对于磁性金属—氧化物纳米复合薄膜的研究有着重要的意义。     

Epitaxial and polycrystalline BaFe12O19 thin films grown by chemical vapour deposition

Epitaxial and polycrystalline barium hexaferrite BaFe₁₂O₁₉ thin films were prepared by metalorganic chemical vapour deposition (MOCVD). Films were grown by a liquid MOCVD technique which aim is to control precisely the precursor vapour pressures. Two kinds of substrates were used: sapphire (001) and silicon thermally oxidized. On Si/SiO₂ films are polycrystalline and the magnetization is isotropic. On Al₂O₃ (001), structural studies reveal the films to be predominantly single phase, well crystallized without annealing procedure and with the c-axis perpendicular to the film plane; epitaxial relationships between the film and the substrate were determined. The magnetic parameters, deduced from vibrating sample magnetometer measurements, show a high dependence of the magnetization with the orientation of the field with respect to the surface of the film.     

High-density perpendicular magnetic recording media of granular-type (FePt/MgO)/soft underlayer

Perpendicular magnetic recording media, composed of granular-type FePt-MgO films on Fe-Ta-C soft magnetic underlayer (SUL), have been fabricated on to 2.5-in glass disks. [001] textured FePt granular films with high-perpendicular magnetic anisotropy were obtained by annealing the FePt/MgO multilayer films. The FePt grain size, perpendicular coercivity, magnetic activation volume, and the exchange coupling between the FePt grains were found to be strongly dependent on the initial multilayer structures and the annealing conditions. The recording performance of the disks was evaluated by a spin-stand. The obtained results reveal a close correlation between the recording performance and magnetic properties. The thermal stability of the granular-type FePt media was studied using high-temperature magnetic force microscopy (MFM) technique, equipped with in situ sample heating, in the temperature range 25/spl deg/C-200/spl deg/C. The estimated signal decay at high temperature is ascribed to the temperature dependent magnetic anisotropy behavior.     

MBE growth and characterization of buried silicon oxide films on Si(100)

Silicon molecular beam epitaxy (Si-MBE) has been used to produce silicon oxide (SiO_x) films by evaporating Si on a heated Si(100) substrate in an ultra high vacuum system with an O₂ pressure of 10⁻⁶ to 10⁻⁴ mbar. Then the SiO_x films were overgrown with pure Si. The influence of the substrate temperature, the O₂ pressure and the Si deposition rate on the oxygen content in the SiO_x films and on the crystalline quality of the Si top-layer was investigated by Rutherford backscattering spectrometry and ion channeling. Epitaxial growth of the Si top-layer was observed up to a maximum concentration of ≈20 at.% oxygen content in the SiO_x film. Cross-sectional transmission electron microscopy shows that the structure of the SiO_x film changes duringa subsequent annealing procedure. Electron energy loss spectrometry proves that amorphous SiO₂ is formed and the development of holes indicates that the density of the as-grown SiO_x film is much lower than that of SiO₂. The specific for the as-grown SiO_x films was determined by I–V measurements.     

Preparation of strontium titanate thin films by mirror-confinement-type electron cyclotron resonance plasma sputtering

Using mirror-confinement-type electron cyclotron resonance (ECR) plasma sputtering method, strontium titanate (SrTiO₃) thin films have been prepared on Si and Pt/Ti/SiO₂/Si substrates at a low substrate temperature (below 450 K) in a low pressure (2.7×10⁻² Pa) environment of pure Ar and Ar/O₂ mixture. Prepared film surfaces were very smooth regardless of high deposition rate (8.5 nm/min). The composition ratio Sr/Ti of Sr to Ti in the films varied with the distance between the target and the substrate. All as-deposited films on Si substrates were found to be amorphous and were crystallized by post-deposition annealing using an electric furnace at 650 K, i.e. approximately 250 K lower than annealing for films obtained by conventional RF magnetron sputtering. Post-deposition annealing of these films using millimeter-wave radiation decreased the crystallization temperature to a value of 550 K. Furthermore, all as-deposited films on Pt/Ti/SiO₂/Si substrates by a plasma of Ar and O₂ gas mixture were found to be crystallized regardless of no substrate heating.     

Structure and magnetic properties of sputtered FePtM (M = Ti,Nb) thin films

FePt thin films doped with various Ti and Nb concentrations ranging from 2.9 to 9.1 at.% were prepared by r.f. magnetron sputtering. The structural and magnetic properties of Ti- and Nb-doped FePt thin films were investigated. Structural studies revealed that the long range ordering in FePt thin films depends on the doping concentration and annealing temperature of FePt thin films. The addition of Ti and Nb is found to enhance the grain refining in FePt thin films. The effects of doping concentration on the magnetic properties of FePt thin films were studied and discussed.     

Preparation and properties of radiofrequency sputtered X-ray amorphous films in the system SiO2–ZrO2

Amorphous films in the system SiO₂–ZrO₂ were prepared by radiofrequency sputtering method and their density, refractive index, elastic constants, and thermal expansion coefficient were measured. All of the physical properties had a similar compositional dependence; that is, they increased, but not proportionally, with increasing ZrO₂ content. The coordination states of cations in these amorphous films were estimated by the compositional dependence of volume and molar refractivity. The coordination state of silicon ions in the amorphous films did not change, but the coordination number of zirconium ions changed from 8 to 6, depending on ZrO₂ content. These results indicate that, in amorphous films in the system SiO₂–ZrO₂, the change of the coordination state of zirconium ions in the amorphous films has an important effect on the properties.     

High concentration erbium doping of silicon-rich SiO2 thin films on silicon

In this work, high concentration erbium doping in silicon-rich SiO₂ thin films is demonstrated. Si plus Er dual-implanted thermal SiO₂ thin films on Si substrates have been fabricated by using a new method, the metal vapor vacuum arc ion source implantation with relatively low ion energy, strong flux and very high dose. X-Ray photoelectron spectroscopy measurement shows that very high Er concentrations on the surfaces of the samples, corresponding to 10 at.% or the doping level of 10²¹ atoms cm⁻³, are achieved. This value is much higher than that obtained by using other fabrication methods such as the high-energy ion implantation and molecular beam epitaxy. Reflective high-energy electron diffraction, atomic force microscopy and cross-section high-resolution transmission electron microscopy observations show that the excess Si atoms in SiO₂ matrix accumulate to form Si clusters and then crystallize gradually into Si nanoparticles embedded in SiO₂ films during dual-ion implantation followed by rapid thermal annealing. Er segregation and precipitates are not formed. Photoluminescence at the wavelength of 1.54 μm exhibits very weak temperature dependence due to the introduction of Si nanocrystals into the SiO₂ matrix. The 1.54-μm light emission signals from annealed samples decrease by less than a factor of 2 when the measuring temperature increases from 77 K to room temperature.     

Sol–gel deposition and characterization of Mn-doped silicate phosphor films

Mn²⁺-doped Zn₂SiO₄ and Mg₂Gd₈(SiO₄)₆O₂ phosphor films were deposited on silicon and quartz glass substrates by sol–gel process (dip-coating). The variations of sol viscosity with time and film thickness with the number of layers were investigated in Zn₂SiO₄: Mn system. The results of XRD and IR showed that the Zn₂SiO₄: Mn films remained amorphous below 700°C and crystallized completely around 1000°C. From AFM studies, it was observed that the grains with 0.5–0.8 μm size packed closely in Zn₂SiO₄: Mn films, which were uniform and crack free. The luminescence properties of Zn₂SiO₄: Mn films were characterized by absorption, excitation and emission spectra as well as luminescence decay. These properties were discussed in detail by a comparison with those of Mn²⁺ (and Pb²⁺)-doped Mg₂Gd₈(SiO₄)₆O₂ phosphor films.     

Al2O3纤维对SiO2基陶瓷型芯的烧缩阻滞

向SiO₂基体粉料中添加Al₂O₃纤维,采用热压注法制备Al₂O₃/SiO₂陶瓷型芯。分析Al₂O₃纤维含量对陶瓷型芯性能的影响。研究结果表明：Al₂O₃纤维含量对Al₂O₃/SiO₂陶瓷型芯的线收缩率、体积密度和抗弯强度均有较大的影响。当Al₂O₃纤维含量大于1wt%时,Al₂O₃/SiO₂陶瓷型芯的线收缩率大幅度降低,稳定在0.335%左右,体积密度随之降低,稳定在1.790 g · cm^-3左右;当Al₂O₃纤维含量为1wt%时,陶瓷型芯抗弯强度达最大值20.48 MPa。分析了Al₂O₃纤维对Al₂O₃/SiO₂陶瓷型芯烧结收缩的阻滞作用机制。     

Thickness measurement of SiO2 films thinner than 1 nm by X-ray photoelectron spectroscopy

The thickness measurement of ultra-thin SiO₂ films thinner than 1 nm was studied by X-ray photoelectron spectroscopy (XPS). Amorphous SiO₂ thin films were grown on amorphous Si films to avoid the thickness difference due to the crystalline structure of a substrate. SiO₂ thin films were grown by ion beam sputter deposition under oxygen gas flow and the thickness was measured by in situ XPS. The attenuation length was determined experimentally by a SiO₂ film with a known thickness. The straight line fit between the measured thickness using XPS and the nominal thickness showed a good linear relation with a gradient of 0.969 and a small offset of 0.126 nm. The gradient measured at the range of 3.4–0.28 nm was very close to that measured at sub-nanometer range of 1.13–0.28 nm. This result means that the reliable measurement of SiO₂ film thickness below 1 nm is possible by XPS.     

疏水耐环境型SiO2/TiO2/SiO2-TiO2太阳能宽光谱增透膜的制备及性能研究

利用TFCcal设计软件构建膜系结构, 采用溶胶-凝胶工艺和提拉法在超白玻璃上制备出厚度精确可控的宽光谱、高增透型SiO₂/TiO₂/SiO₂-TiO₂减反膜, 同时结合甲基三乙氧基硅烷(MTES)改性碱催化的SiO₂溶胶, 通过提拉法一次制备出高透过率疏水型薄膜。研究表明, 高增透型三层宽光谱减反膜的理论膜层厚度依次为: 80.9 nm(内层SiO₂-TiO₂)、125.0 nm(中间层TiO₂)、95.5 nm(外层SiO₂), 其在400~700 nm可见光范围内平均透过率实际可高达97.03%以上。多层膜经过退火处理后, 膜面的水接触角高达131.5°, 同时陈化两个月以后的多层膜透过率仅下降0.143%, 表明制备的SiO₂/TiO₂/ SiO₂-TiO₂多层减反膜具有优良的疏水和耐环境性能。     

Ambient temperature synthesis and magnetic properties of aluminum borate—Fe nanocomposites

Nanocomposites in which fine Fe particles are dispersed in a ceramic aluminum borate Al_xB_yO_z matrix were synthesized at ambient temperatures by simultaneous hydrolysis of aluminum butoxide and reduction of Fe²⁺ with sodium borohydride. The nanocomposites were characterized by X-ray powder diffraction, transmission electron microscopy, SQUID magnetometry, and Mössbauer spectroscopy. The as-prepared samples consist of crystalline Fe particles dispersed in an amorphous aluminum borate matrix, which on annealing in H₂ atmosphere at T ≥ 800 °C transforms to crystalline aluminum borate; the crystalline aluminum borate exhibits a needle-like morphology. The as-prepared samples all seem to consist of a mixture of ferromagnetic and superparamagnetic Fe particles. The superparamagnetic fraction vanishes completely on annealing in H₂ atmosphere at 900 °C. The magnetic results are supported by Mössbauer spectra recorded at room temperature.