FePt/Au多层膜的结构和磁性能研究

采用磁控溅射在SiO2<0001>基片上制备了FePt(2nm)/Au(tnm)多层膜,将其在不同温度下进行热处理。利用X射线荧光光谱仪、X射线衍射仪、振动样品磁强计和原子力显微镜对样品的结构和性能进行了研究。结果表明,沉积态样品具有超晶格结构,fccFePt和Au共格生长。经过较低温度热处理后,样品仍然保持超晶格结构。样品经400℃热处理后,开始发生有序化转变。经600℃热处理后,平行于膜面和垂直于膜面的矫顽力分别为811.7和829.2kA·m-1。当t=2.5nm时,最有利于L10-FePt相的形成。在磁化过程中,畴壁移动和磁矩转动机制共存。样品经热处理后,形成了均匀的薄膜。     

Ti衬底层对FePt颗粒膜的微结构和磁特性的影响

在室温下,应用对靶直流磁控溅射设备在普通玻璃基片上制备了FePt(30nm)/Ti(tnm)颗粒膜样品,随后,在真空中进行了原位退火.详细研究了Ti衬底层对FePt颗粒膜的微结构和磁特性的影响.X射线衍射图谱表明样品形成了较有序的L10织构,Ti和FePt形成了三元FePtTi合金.当Ti层厚度t=5 nm、退火温度Ta=500℃时,样品具有高度有序的L10织构、小的颗粒尺寸和优异的磁特性.矫顽力超过了6.7 kOe,饱和磁化强度为620emu/cc.并且具有较小的开关场分布.结果表明FePt/Ti颗粒膜系统可作为超高密度磁记录介质的候选者.     

Ti衬底层对FePt颗粒膜的微结构和磁特性的影响

在室温下,应用对靶直流磁控溅射设备在普通玻璃基片上制备了FePt(30nm)/Ti(tnm)颗粒膜样品,随后,在真空中进行了原位退火.详细研究了Ti衬底层对FePt颗粒膜的微结构和磁特性的影响.X射线衍射图谱表明样品形成了较有序的L10织构,Ti和FePt形成了三元FePtTi合金.当Ti层厚度t=5 nm、退火温度Ta=500℃时,样品具有高度有序的L10织构、小的颗粒尺寸和优异的磁特性.矫顽力超过了6.7 kOe,饱和磁化强度为620emu/cc.并且具有较小的开关场分布.结果表明FePt/Ti颗粒膜系统可作为超高密度磁记录介质的候选者.     

Micromagnetic simulation of Au interlayer in L1_0-FePt nanocomposite recording medium

Owing to the epitaxial inducement of Au atom,Au interlayer was introduced to increase the perpendicular anisotropy and the coercivity in L1_0-FePt nanocomposite film.Micromagnetics can be used to reveal the relationship between microstructure and magnetic properties of materials,and give the information of the perpendicular anisotropy and coercivity.In this work,the effect of the Au interlayer on annealed[Fe(0.5 nm)/Pt(0.5 nm)/Au(d nm)]_(10) nanocomposite recording medium by a micromagnetic model was studied.The model contains three phases:hard magnetic phase,soft magnetic phase,and nonmagnetic phase.The calculated result shows that perpendicular orientation degree of the texture and proportion of a hard magnetic phase to the total phase in the annealed film are both enhanced by increasing Au interlayer thickness.This result can be conducive to the improvement of the perpendicular anisotropy and the coercivity of the FePt nanocomposite film in the experiments.     

（001）-oriented FePt/Ag composite films for perpendicular recording

FePt/Ag thin films were deposited by magnetron sputtering onto 7059 glass substrates, then were annealed at 550 ℃ for 30 min. Nanostructured FePt/Ag films were successfully obtained with the magnetic easy axis of L10 FePt perpendicular to the film plane. It was found that the development of (001) texture depended strongly on the thicknesses of FePt magnetic layer and Ag underlayer. The L10 ordered FePt(15 nm)/Ag(50 nm) with (001) orientation can be obtained. And the perpen-dicular coercivity of FePt(15 nm)/...     

Effect of addition of N on L10 transformation and atomic diffusion in FePt films

The effect of nitrogen incorporation on the kinetics of L1₀ transformation in FePt alloy films was studied. Films with a maximum possible amount of nitrogen were prepared by sputtering a FePt compound target with pure nitrogen. As-prepared films consisting of nano-grains of Pt and Fe_0.7N_0.3 transformed to face-centered cubic FePt phase with a certain amount of nitrogen incorporated in the grains after annealing at 573 K. It was found that the presence of N results in faster kinetics of L1₀ transformation compared with pure FePt alloy films, as well as a substantial reduction in grain size. Detailed structural and diffusion measurements were carried out to elucidate the mechanism of enhanced transformation kinetics as well as grain size reduction. The activation energy for volume diffusion of Fe in FePtN films was found to be 0.27 ± 0.14 eV, while that in FePt was 0.50 ± 0.17 eV. Faster atomic diffusion in nitrogen-containing films was the cause of an enhanced rate of L1₀ transformation. Further studies reveal that, in partially transformed FePtN alloy films, N is incorporated mainly in the grain boundary region, which hinders grain growth and results in a smaller grain size.     

锆-2合金在过热蒸汽中形成氧化膜的电子显微镜研究

应用电子显微镜研究了锆-2合金在613k和773k过热蒸汽中形成的氧化膜,对节状腐蚀也进行研究。黑色氧化膜中存在立方、四方和单斜三种晶体结构的氧化锆,随着温度升高,立方和四方的比例减少。当氧化膜变成白色后,完全转变成了单斜结构。从高分辩电子衍衬图象中可以看到黑色氧化膜的晶体是由～20nm大小的嵌锒块组成,在(100)和(101)晶面上存在一些晶面间距较大的地区,这可能与锡原子的聚集片有关。在氧化膜与金属界面处,节状腐蚀斑形似“花菜”向金属基体内生长,“花菜”表面留下波纹痕迹,这可能与节状腐蚀生长快的特性有关。在白色氧化膜中,可以观察到晶界上存在空洞(<10nm)。根据本实验结果,对作者过去提出的节状腐蚀形成模型作了进一步的讨论。     

机械合金化制备具有纳米相复合结构的Al-Pb互不溶体系中Pb相的粗化动力学和添加Cu对其粗化的影响

利用X射线衍射仪、扫描电子显微镜和透射电子显微镜研究了机械合金化制备的具有纳米相复合结构的Al-Pb互不溶体系中Pb相的粗化动力学和添加Cu对其粗化的影响。结果表明在573、623、673和723 K退火不同时间后，尽管Al-Pb纳米相复合结构合金中组成相的尺寸均在纳米量级，Pb相的平均颗粒尺寸与退火时间之间仍满足三次方定律。Pb相的粗化激活能为84.80 kJ/mol，此值接近于基体Al的晶界自扩散激活能。这表明Pb相的粗化受晶界扩散控制。添加Cu降低了Pb相的粗化速率，这与Cu在Al和Pb相的界面偏聚，降低了Al/Pb的界面能有关。添加Cu后，Pb相的长大激活能增加。     

Shape memory behavior of Ti–20Zr–10Nb–5Al alloy subjected to annealing treatment

The effects of annealing temperature on microstructures, phase transformation, mechanical properties, and shape memory effect of Ti–20Zr–10Nb–5Al alloy were investigated. X-ray diffraction(XRD) patterns show that the alloy is composed of single hexagonal ɑ'-martensite phase for both as-rolled sample and sample annealed at773 K for 30 min, while single orthorhombic ɑ' phase exists in the samples annealed at 873 and 973 K for30 min. The optical observations indicate that the alloy is recrystallized when annealed at 873 K, and the grain size of the sample annealed at 973 K is about five times larger than that annealed at 873 K. Both of the samples annealed at 873 and 973 K show almost the same reverse martensite transformation start temperature of 483 K as demonstrated by thermal dilatation tests. The critical stress values for martensite reorientation(σ_M) are 392 and 438 MPa for the alloys annealed at 873 and 973 K, respectively. The maximum shape memory strain is 2.8 %, which is obtained in the alloy annealed at 873 K due to the lower σ_M. Moreover,the sample annealed at 873 K exhibits larger tensile stress and tensile strain due to the smaller grain size.     

Effect of annealing on properties of lithium aluminum germanium phosphate electrolyte thick films prepared by aerosol deposition

Li_1.5[Al_0.5Ge_1.5(PO₄)₃] glass-ceramic powder was used for the deposition of thick films on silicon substrate by aerosol deposition. The deposited films were annealed at 873 K and 1023 K for 6 h in air. The thickness of the films was 10–12 m and the relative density was 78%–82%. As-deposited films had nano-scale grains and amorphous regions while in the annealed films, the grain growth and improved crystallinity were observed. The grain size was increased from 12 nm to 25 nm and 97 nm after annealing at 873 K and 1023 K, respectively. The ionic conductivity of the as-deposited film was 8.49 × 10^?9 S cm^?1, which increased to 1.06 × 10^?5 S cm^?1 and 1.16 × 10^?4 S cm^?1 after annealing at 873 K and 1023 K, respectively. The increased ionic conductivity is explained in terms of the increased grain size as well as the improved crystallinity.     

The effect of multilayer structure on magnetic properties of FePt thin films

The Fe/Pt multilayer films with different structures were deposited by RF magnetron sputtering on glass substrates, and the L1₀-FePt films were obtained after theas-deposited samples were subjected to vacuum annealing at various temperatures. Results show that the Fe/Pt multilayer structure can effectively reduce the ordering temperature of FePt film, and the in-plane coercivity of [Fe (5.2 nm)/Pt (5.2 nm)]₇ multilayers can reach 161.2 kA/m after annealed at 350 ℃ for 30 min. When Fe and Pt layer thickness is equal, the coercivity of the film is the largest. On the other hand, the different Fe-Pt crystalline phases such as Fe₃Pt and FePt₃ phases are formed after annealing when the thickness ratio of Fe/Pt deviates from 1 after annealing. When Fe and Pt have the same thickness, the thinner single layer gets the lower ordering temperature and the larger coercivity.     

Micromagnetic studies of perpendicular recording FePt media with controllable grain size distributions

A 3-dimensional (3D) micromagnetic model combined with Fast Fourier Transform (FFT) method was built up to study the writability in the L10 FePt perpendicular medium. The effects of controllable grain size distributions were studied by grain growth simulation. It is found that the cross-track-averaged magnetization changes little between the L10 FePt medium with uniform or non-uniform grain size distribution.     

L1_0有序FePt薄膜的研究进展

L1_0有序FePt合金由于其极大的磁晶各向异性常数而成为下一代超高密度磁记录的候选材料,如何制备具有L1_0有序FePt薄膜成为近年来的研究热点。介绍了制备具有L1_0有序FePt薄膜的方法,包括选择合适的基底材料、单原子层沉积多层膜结构、引入下底层或中间层、添加合金元素或第三组元等,并阐述了这几种方法的主要特点和存在的问题,展望了今后FePt薄膜的发展方向。     

Preparation of epitaxial and polycrystalline bismuth titanate thin films on single crystal (100) MgO by chemical solution deposition

Epitaxial and polycrystalline Bi₄Ti₃O₁₂ thin films were prepared on single crystal (100) MgO substrates by a chemical solution deposition process using metal naphthenates as starting materials. Pyrolyzed films (at 500°C) were annealed for 30 min in air at 650, 700, 750 and 800°C, respectively. The effects of annealing temperature on the crystallinity, epitaxy and surface morphology of the films were investigated by X-ray diffraction θ-2θ scans, pole-figure analysis, and atomic force microscopy (AFM). Epitaxially grown films annealed at 700 and 750°C, respectively, showed growth of three-dimensional needle-shaped grains. During annealing at 800°C, grain growth of Bi₄Ti₃O₁₂ may be suppressed by the formation of a titanium-rich phase such as Bi₂Ti₂O₇ owing to Bi volatilization, resulting in lower root mean square roughness than that of film annealed at 750°C.     

Low field magnetoresistance properties of (La0.75Sr0.25)1.05Mn0.95O3 polycrystalline thin films on a-SiO2/Si substrates prepared by ex-situ solid phase crystallization

We report the low field magnetoresistance (LFMR) properties of (La_0.75Sr_0.25)_1.05Mn_0.95O₃(LSMO) films on a-SiO₂/Si substrates, prepared by ex-situ solid phase crystallization of amorphous films deposited by dc-magnetron sputtering at room temperature. The average grain size of the LSMO films was gradually increased with increasing annealing temperature (T _an ) and film thickness. High T _an also caused the growth of an amorphous inter-diffusion layer between a-SiO₂ and LSMO. The highest LFMR values of 16 and 1.0 % were achieved at 100 K, 1.2 kOe and 300 K, 0.5 kOe, respectively, from an LSMO film of 200 nm thickness annealed at 900 °C. In accordance with a modified brick layer model, grain boundary areal resistance gradually increased with increasing T _an and decreasing film thickness due to the penetration of the amorphous inter-diffused phase into the LSMO grain boundary. Improved LFMR values are attributable to modification of the LSMO grain boundary into a more effective spin-dependent scattering center.     

Microstructural characteristics of Nd2Fe14B/α-Fe nanocomposite ribbons bearing Nb element

The effects of Nb on the microstructure and magnetic properties of (Nd0.9Dy0.1)9.5Fe79-xCo5NbxB6.5(x=0, 1) nanocomposite magnets were investigated. A fine and uniform microstructure was achieved for the ribbons annealed at 710℃ for 4min, enhancing the interaction coupling between grains and improving the magnetic properties. The results of three-dimensional atom probe (3DAP) indicated that Fe-Nb-B inter granular phase existed at the grain boundaries, suppressing the grain growth during the crystallization process. The coercivity was improved from 224 to 643 kA/m for the modification of the microstructure.     

Synthesis and grain growth kinetics of in-situ FeAl matrix nanocomposites （ Ⅱ ）： Structural evolution and grain growth kinetics of mechanically alloyed Fe-Al-Ti-B composite powder during heat treatment

Morphological changes, structural evolutions and grain growth kinetics of mechanically alloyed（MAed） Fe50Al50, Fe42.5Al42.5Ti5B10 and Fe35Al35Ti10B20 （mole fraction, %） powders were investigated by XRD and SEM, when being isothermally annealed at 1 073-1 373 K. The effect of different Ti and B addition on the grain growth of FeAI phase was also discussed. The results show that the nanocrystalline FeAI and in-situ TiB2/FeAl nanocomposite powders can be synthesized by subsequent heat treatment. Besides the relaxation of crystal defects and lattice stress, the transformation from Fe-based solid solution into B2-FeAl and TiB2 occurs upon heating of the MA-processed alloys. Although the grain growth takes place, the grain sizes of both FeAl and TiB2 are still in nanometer scale. The activation energies for the nanocrystalline FeAl growth in the three alloys are calculated to be 534.9, 525.6 and 1 069.6 kJ/mol respectively, according to kinetics theory of nanocrystalline growth. Alloys with different TiB2 contents exhibit unequal thermal stability. The presence of higher content TiB2 plays significant role in the impediment of grain growth.     

Microstructure and nanomechanical properties of Mn-rich Ni–Mn–Ga thin films

We report the effect of post-annealing on the crystalline phase, grain growth, magnetic and mechanical properties of Ni–Mn–Ga thin films deposited at room temperature followed by post-annealing at different temperatures. The phase and microstructural analysis reveal that amorphous to crystalline transformation occurs in as-deposited films after post-annealing above 873 K. The transformation of disordered phase into nanocrystalline phase by the influence of annealing has been confirmed by transmission electron microscopy. The crystalline films exhibit soft magnetic behavior with the Curie temperature of 314 K, while the amorphous films exhibit the Pauli-paramagnetic behavior even down to 4 K. The mechanical properties like hardness and elastic modulus of the films also show a strong dependence on the annealing temperature with crystalline film exhibiting maximum values of 6 GPa and 103 GPa, respectively. The Ni–Mn–Ga film annealed at 873 K exhibits enhanced nanomechanical properties and room temperature ferromagnetism which make this a potential candidate for use in MEMS devices.     

Synthesis and grain growth kinetics of in-situ FeAl matrix nanocomposites (Ⅱ): Structural evolution and grain growth kinetics of mechanically alloyed Fe-Al-Ti-B composite powder during heat treatment

Morphological changes, structural evolutions and grain growth kinetics of mechanically alloyed(MAed) Fe50Al50, Fe42.5Al42.5Ti5B10 and Fe35Al35Ti10B20 (mole fraction, %) powders were investigated by XRD and SEM, when being isothermally annealed at 1 073-1 373 K. The effect of different Ti and B addition on the grain growth of FeAl phase was also discussed. The results show that the nanocrystalline FeAl and in-situ TiB2/FeAl nanocomposite powders can be synthesized by subsequent heat treatment. Besides the relaxation of crystal defects and lattice stress, the transformation from Fe-based solid solution into B2-FeAl and TiB2 occurs upon heating of the MA-processed alloys. Although the grain growth takes place, the grain sizes of both FeAl and TiB2 are still in nanometer scale. The activation energies for the nanocrystalline FeAl growth in the three alloys are calculated to be 534.9, 525.6 and 1 069.6 kJ/mol respectively, according to kinetics theory of nanocrystalline growth. Alloys with different TiB2 contents exhibit unequal thermal stability. The presence of higher content TiB2 plays significant role in the impediment of grain growth.     

退火工艺对二氧化钛薄膜光催化性能的影响

利用磁控溅射法制备得到二氧化钛薄膜,将薄膜在高温管式炉中分别进行退火,利用XRD、AFM和紫外-可见光谱仪研究了不同温度下退火前后薄膜的晶相结构、光学性能和光催化性能。结果表明,随着退火温度的升高二氧化钛的晶相由锐钛矿向金红石转变,600℃时为两相共存,表面颗粒大小也会有相应变化,锐钛矿相表现出了更好的光催化性能。