Influence of Annealing Conditions on Nanocrystalline and Ultra-Soft Magnetic Properties of Fe75.5Cu1Nb1Si13.5B9 Alloy

The magnetic and structural properties of FINEMET alloy with a composition of Fe75.5Cu1Nb1Si13.5B9 were investigated after primary and secondary crystallization of amorphous ribbon sample.The crystallization behavior and the nanocrystal formation of the samples were performed by differential thermal analysis(DTA) which in turn was supported by X-ray diffraction(XRD) study.Temperature dependence of initial permeability of amorphous and devitrified toroid shaped samples has been measured.Enhancement of Curie temperature of the amorphous alloy has been observed due to the irreversible structural relaxation.With the appearance of nanocrystalline phase the Curie temperature of the residual amorphous phase gradually decrease with the increase of annealing temperature.Their temperature dependence reflects the characteristic annealing temperature evolution of the basic magnetic parameters in these nanocrystalline systems.Saturation magnetization,Ms,increases with annealing temperature Ta for the samples and finally decreases during annealing at a temperature much higher than peak crystallization temperature.     

Influence of annealing on the ferroelectric properties of Pt/Pb(Zr,Ti)O3/Pt thin film capacitors

The deformation in the hysteresis loop of Pt/Pb(Zr,Ti)O₃/Pt capacitors has been investigated by varying the annealing temperature after patterning the top sputter-deposited electrode using reactive ion etching (RIE) with Ar gas. It was observed that as-patterned capacitors were positively poled by the dc plasma potential during RIE of Pt. Voltage shift and slant in the hysteresis loop are found to be due to space charges trapped at domain boundaries during both sputtering and RIE rather than a nonferroelectric second phase. As Zr:Ti ratio decreases, internal bias field increases, and annealing temperature, at which maximum in polarization occurs, also increases due to lower permittivity and higher Curie temperature.     

Preparation of cobalt-zinc ferrite (Co0.8Zn0.2Fe2O4) nanopowder via combustion method and investigation of its magnetic properties

Cobalt-zinc ferrite (Co_0.8Zn_0.2Fe₂O₄) was prepared by combustion method, using cobalt, zinc and iron nitrates. The crystallinity of the as-burnt powder was developed by annealing at 700 °C. Crystalline phase was investigated by XRD. Using Williamson-Hall method, the average crystallite sizes for nanoparticles were determined to be about 27 nm before and 37 nm after annealing, and residual stresses for annealed particles were omitted. The morphology of the annealed sample was investigated by TEM and the mean particle size was determined to be about 30 nm. The final stoichiometry of the sample after annealing showed good agreement with the initial stoichiometry using atomic absorption spectrometry. Magnetic properties of the annealed sample such as saturation magnetization, remanence magnetization, and coercivity measured at room temperature were 70 emu/g, 14 emu/g, and 270 Oe, respectively. The Curie temperature of the sample was determined to be 350 °C using AC-susceptibility technique.     

Strain effects and phase separation tendency in highly strained La0.7Ba0.3MnO3 thin films on LaAlO3 substrates

The magnetic and transport properties of epitaxial La_0.7Ba_0.3MnO₃ films on LaAlO₃ substrates have been investigated and compared with those on SrTiO₃ substrates. It is found that the ferromagnetic and metallic transition temperature of the highly compressive strained films on LaAlO₃ substrates decreases steadily with decreasing film thickness, while it changes little in the lightly strained films on SrTiO₃ substrates. The properties of the films on LaAlO₃ substrates are more sensitive to a post-annealing procedure. A tendency to phase separation, which induces a difference between the insulator-metal transition temperature T_MI and the Curie temperature T_C, is observed for the films with a medium oxygen annealing process. We argue that the phase separation is due to both the highly compressive strain and oxygen deficiency in the films.     

Mn改性Na0.5Bi2.5Nb2O9高温压电陶瓷的研究

采用固相法获得了Mn改性的Na0.5Bi2.5Nb2O9(NBN+xmol%MnCO3,0≤x≤10.0)铋层状压电陶瓷,并系统地研究了Mn(掺杂)对NBN基陶瓷显微结构与电性能的影响.结果表明,所有获得的样品都是居里点在700℃以上的单一相铁电体.加入Mn显著地提高了NBN系列陶瓷的机械品质因素Qm,明显改善了陶瓷的压电与机电性能.当MnCO3掺杂量为8.0mol%时,陶瓷获得最佳电性能:tanδ=0.749%,d33=20 pC/N,Qm=3120,kp=12.37%,kt=21.09%,Pr=7.01μC/cm2.NBN+xmol%MnCO3(x=8.0)陶瓷经700℃退极化处理后,其d33保持为原来的75%(~15 pC/N),表明该材料在高温领域下具有良好的应用前景.     

Magnetic properties of nano-crystalline Li0.35Cd0.3Fe2.35O4 ferrite prepared by modified citrate precursor method

Single phase nano-crystalline lithium cadmium ferrite Li_0.35Cd_0.3Fe_2.35O₄ is synthesized by a modified citrate gel precursor technique in different pH media. The modified citrate precursor technique reduces the formation of the impurity phase α-Fe₂O₃ in the inverse spinel phase of lithium ferrite. X-ray diffraction (XRD) and transmission electron microscopy (TEM) confirmed the average crystallite size. As-prepared sample shows the paramagnetic behaviour of M–H curve measured by vibrating sample magnetometer (VSM). The coercivity (H_c) and magnetization (M) both increase with decrease in temperature from 300 K to 80 K. Temperature dependent magnetic properties below the Curie point are defined by the Bloch's law and Neel relaxation relations. The effect of annealing on magnetic properties at different temperature is studied.     

Formation of A15-phase in Ta/ Nb3Al0.75Ge0.25-powder - and Nb/ Nb3Al0.75Ge0.25-powder - composites and their superconducting properties

The experiments were done using a powder mixture of Nb, Al and Ge with a particle diameter of less than 50 μm which was filled into Ta- or Nb-tubes. These composites were cold-worked and heated from 400°C (10°C/min) up to 850 or 900°C and annealed 20 min on this temperature. By this heat treatment in many areas the intermetallic compound Nb(Al,Ge)3is formed within the powder mixture. After a second cold deformation the composites were annealed at 1000, 1200 or 1300°C with different annealing times. Microprobe analysis was used to investigate the phase distribution. The formation of the A15-phase was also investigated by transition temperature measurements, which were done by the inductive method. The highest transition temperature was found after 1300°C furnace annealing. Maximum critical current was achieved by short-time resistive annealing at 1200°C of 0.5 mm θ wire. The reason for the high current carrying capacity of the short-time annealed samples can be seen from the Tc-measurements which show that a A15-phase with high transition temperature is formed even after a short annealing time. Possible improvements of superconductors made from powder mixtures are discussed.     

Insulating properties of rapid thermally processed Bi2Ti2O7 thin films by a chemical solution decomposition technique

Crack-free Bi₂Ti₂O₇ thin films on silicon substrates were prepared using chemical solution decomposition technique, and then treated by rapid thermal annealing. The microstructure of the films was studied by scanning electron microscopy. The effects of different fabricating procedures and various annealing temperatures and times on the leakage current density were investigated. The results show that the leakage current density decreases with increasing annealing temperature, while increases with increasing annealing time. Annealing temperature has a much stronger effect on the insulating properties of Bi₂Ti₂O₇ thin films than that of annealing time.     

Effect of sintering temperature on magneto-transport properties of La0.67Ba0.33MnO3/Ba0.7Sr0.3TiO3 composites

La_0.67Ba_0.33MnO₃-20 wt.%-Ba_0.7Sr_0.3TiO₃ composites were sintered at different temperatures in order to explore the possibility of improving the magneto-transport properties of the composites. Detail studies on the magnetic and electrical transport properties for the sintered composite samples have been performed. Results show that the sintered composites have identical ferromagnetic to paramagnetic transition temperature and filamentary feature of metallic phase. When sintering temperature higher than 1300 °C, the composites show Efros-Shklovskii-like variable-range hopping in the temperature range lower than Curie temperature. For samples sintered lower than 1100 °C, a dome-like resistance peak appears at a temperature well below the Curie temperature. Magnetoresistance behavior indicates the existence of spin polarized tunneling in the low temperature range. Considering the contributions from Efros-Shklovskii-like variable-range hopping and spin polarized tunneling, the resistance peak can be well fitted.     

TiO2/SiO2复合薄膜的晶化特征和结构转变研究

对TiO2／SiO2复合薄膜的晶化特征进行了分析，研究表明，随着TiO2含量的增加，其晶化温度降低，而由锐钛矿相完全转变为金红石相的速度减慢．SiO2的析晶温度也随着TiO2含量的增加而降低，即TiO2具有诱导SiO2析晶的作用．锐钛矿晶粒尺寸的增加幅度随着TiO2含量的降低和热处理温度的升高而增大．其晶粒尺寸的大小与热处理时间的平方根成正比．认为由于TiO2含量的不同，造成薄膜中由锐钛矿相完全转变成金红石相的速度差异主要来自于薄膜中应力的作用．     

Fe45Co7Cr15Mo10Y2B6C15大块非晶合金的晶化动力学研究

为了明确Fe基块体非晶材料的晶化过程,通过铜模吸铸法制备了Fe45Co7Cr15Mo10Y2B6C15块体非晶合金,采用连续和等温差热扫描量热法对非晶合金在1 000 K以下的晶化动力过程进行了研究.研究表明:在973 K时效后的晶化产物为铁的碳化物;晶化过程的激活能达到了555.9 kJ/mol,非晶热稳定性良好;Avrami常数n值接近2,随着退火温度的变化,n值没有明显的变化,非晶晶化机理没有发生改变,而放热峰宽随着退火温度的降低明显宽化,说明非晶晶化过程是一个二维扩散控制的形核与长大过程.     

In situ investigation of thermally influenced phase transformations in (pb0.92sr0.08) (zr0.65ti0.35)o3 thin films using micro-raman spectroscopy and x-ray diffraction

Thin films of ferroelectric strontium-doped lead zirconate titanate [PSZT, (Pb_0.92Sr_0.08)(Zr_0.65Ti_0.35)O₃] deposited by RF magnetron sputtering have been analyzed by in situ analysis techniques. The in situ techniques employed for this study include micro-Raman spectroscopy and X-ray diffraction (XRD), and variations in thin film structure and orientations for temperatures up to 350degC and 750degC for the respective techniques have been studied. The samples analyzed were PSZT thin films deposited on platinum-coated silicon substrates at either room temperature or at 750degC. In situ measurements using micro-Raman spectroscopy and XRD techniques have been used to identify the Curie point for poly-crystalline PSZT thin films and to determine the temperature-activating significant grain growth for room-temperature-deposited PSZT thin films. To study the presence of hysteresis, analysis was carried out during both temperature ramp-up and ramp-down cycles. Raman measurements showed expected bands (albeit weak), and the in situ measurements have detected variations in the crystal structure of the thin film samples, with negligible variations between the heating and cooling cycles. A combination of the Raman and XRD results has shown that the temperature activating significant grain growth for the room-temperature deposited films is about 275degC and the Curie point lies between 325 and 400degC. This relatively high Curie point makes these films suitable for wide temperature range applications.     

Al-Mg-Sc-Ti合金中Al3(Scx,Ti1-x)粒子的析出行为

用激冷铸造法制备Al-5.5Mg-0.25Sc-0.04Ti合金,研究了在不同温度退火后其硬度随时间的变化,并用金相显微镜(OM)和透射电镜(TEM)研究了这种合金中Al₃(Sc_x,Ti_1-x)第二相粒子的存在形式和形成机制。结果表明：用急冷铸造法制备的Al-5.5Mg-0.25Sc-0.04Ti铸态合金中Sc和Ti原子主要以固溶的形式存在于α(Al)基体中,在电镜下很难观察到这些粒子。铸态合金在较低温度(低于250℃)下退火时其硬度提高得比较慢,退火较长时间才能出现硬度的峰值;而在比较高的温度(高于350℃)退火硬度提高得非常快,很快出现峰值。但是,硬度出现峰值后继续退火则大幅度降低;在300℃退火硬度的热稳定性比较高。硬度的变化,与次生Al₃(Sc_x,Ti_1-x)粒子的析出密切相关。在较低温度下次生Al₃(Sc_x,Ti_1-x)粒子的析出不充分且粒径较小,对晶界、亚晶界和位错的钉扎作用较弱;而在过高的温度下Al₃(Sc_x,Ti_1-x)粒子发生粗化,使合金的性能降低。     

Al2O3掺杂BaTi0.85Sn0.15O3陶瓷的制备及性能表征

通过传统固相二次烧结法来制备x wt% Al₂O₃（x=0、1.0、1.5）/BaTi_0.85Sn_0.15O₃（BTS）陶瓷。研究了掺杂不同含量Al₂O₃对BTS陶瓷的微观结构、介电性能及挠曲电性能的影响。结果表明,掺杂Al₂O₃的BTS陶瓷不改变陶瓷的晶体结构,仍为标准钙钛矿结构晶型;Al₂O₃的掺入能够有效降低晶粒尺寸,具有明显的细晶作用。随着Al₂O₃含量的增大,Al₂O₃/BTS陶瓷的介电常数减小,介电损耗得到明显改善,居里峰逐渐宽化且向温度高的方向偏移。Al₂O₃/BTS陶瓷的挠曲电系数随着Al₂O₃含量的增加和测试环境温度的升高均减小。此外,Al₂O₃/BTS陶瓷的挠曲电系数和介电常数之间存在一种近线性关系,但当温度非常接近于居里温度时,这种线性关系减弱。     

振动球磨制备的LaFe11.44Si1.56化合物的结构和磁性

利用振动球磨工艺制备了LaFe11.44Si1.56化合物,结果表明,在1100℃仅需要热处理30min,该化合物就能形成NaZn13型立方晶体结构;与电弧熔炼工艺制备的试样相比较,振动球磨工艺制备的试样的居里温度提高了15K,但最大磁熵变有所减小。因此,利用振动球磨工艺合成La(Fe,Si)13化合物有进一步研究的价值。     

Varistors based on n-BaTiO3 ceramics

Stable and highly reproducible voltage-limiting characteristics have been observed at room temperature for polycrystalline ceramics prepared from donor-doped BaTiO₃ solid solutions containing isovalent lattice substitute ions that lower the Curie point T_c. When the ambient temperature T_a is decreased such that T_a < T_c, the same ceramics show current-limiting behaviour. The leakage current, the breakdown voltage and the non-linear coefficient ( = 30−50) could be varied with grain-boundary layer (GBL) modifiers and postsintering annealing. The magnitude of the abnormally high dielectric constant (ε_r 10⁵) indicates the prevalence of GBL capacitance in these ceramics. Analyses of the current-voltage relations show that GBL conduction at T_a < T_c corresponds to tunnelling across asymmetric barriers formed under steady state Joule heating. At T_a > T_c, trap-related conduction gives way to tunnelling across symmetric barriers as the field strength increases.     

分凝对Pb(Mg1/3Nb2/3)O3-38%PbTiO3单晶的成分及介电、压电性能的影响

研究了用改进的Bridgman法生长的PMNT62／38单晶在其生长过程中的分凝现象，研究了分凝导致的成分不均匀及其对介电和压电性能的影响。XRFA分析表明，PMNT62／38单晶底部的PbTiO3(PT)含量为x=35.2mol%，而顶部的PT含量为43mol%。底部晶体（001），（110）和（111）三种切型的晶片加电场极化后，其介电和压电性能出现了异常的现象。（110）切型的压电模量最大，为1200pC/N；（111）次之，为789pC/N；（001）最低，为371pC/N。极化后的（110）和（111）晶片在室温、1kHz频率下的相对介电常数（两种切型的εr都在10000左右），约为（001）晶片（εr-5000)的1倍，并且介电常数在低温端有上升的趋势。     

Effects of N2-annealing conditions on the sensing properties of Pt/HfO2/SiC Schottky-diode hydrogen sensor

Hafnium oxide (HfO₂) used as the gate insulator of metal-insulator-SiC Schottky-diode hydrogen sensors is annealed in nitrogen at different temperatures and durations for achieving a better performance. The hydrogen-sensing properties of these samples are compared with each other by taking measurements under various temperatures and hydrogen concentrations using a computer-controlled measurement system. The sensor response of the device is found to increase with the annealing temperature and time because higher annealing temperature and longer annealing time can enhance the densification of the HfO₂ film; improve the oxide stoichiometry and facilitate the growth of an interfacial layer to give better interface quality, thus causing a significant reduction of the current of the sensor under air ambient. The effects of hydrogen adsorption on the barrier height and conduction mechanism of the devices are also investigated.     

Influence of annealing treatments for ZnO-doped Zr0.8Sn0.2TiO4 thin films by RF magnetron sputtering

Zirconium tin titanium oxide doped 1 wt.% ZnO thin films on n-type Si substrate were deposited by rf magnetron sputtering at a fixed rf power of 300 W, a substrate temperature of 450 °C, a deposition pressure of 5 mTorr and an Ar/O₂ ratio of 100/0 with various annealing temperatures and annealing times. Electrical properties and microstructures of 1 wt.% ZnO-doped (Zr_0.8Sn_0.2)TiO₄ thin films prepared by rf magnetron sputtering on n-type Si(100) substrates at different annealing temperatures (500 °C-700 °C) and annealing times (2 h-6 h) have been investigated. The structural and morphological characteristics analyzed by X-ray diffraction (XRD) and atomic force microscope (AFM) were sensitive to the treatment conditions such as annealing temperature and annealing time. At an annealing temperature of 600 °C and an annealing time of 6 h, the ZnO-doped (Zr_0.8Sn_0.2)TiO₄ thin films possess a dielectric constant of 46 (at f = 10 MHz), a dissipation factor of 0.059 (at f = 10 MHz), and a low leakage current density of 3.8 × 10^− 9 A/cm² at an electrical field of 1 kV/cm.     

Effects of interfacial structure on the magnetic properties of ultrathin Fe/Pt(111) films with Ag buffer layer

For Fe/Pt(111) grown at 180 K, the easy axis of magnetization changes from out-of-plane to in-plane while the surface structure changes from fcc(111) to bcc(110). The Curie temperature for 1 ML Fe/Pt(111) is close to room temperature. After insertion of submonolayer Ag, no significant change for the Curie temperature is observed. By thermally annealing Ag/Pt(111) at 550 K to form a Ag-Pt surface alloy, we demonstrate that the Curie temperature of the deposited Fe films is elevated to be higher than room temperature. For an ultrathin Fe/Ag/Fe/Pt(111) sandwich system, the strong interaction between the two Fe layers is superior due to the effect of the double Fe/Ag interfaces. This causes that the easy axis of the magnetization switches back to the in-plane direction during the deposition of Fe overlayer on the surface of a Ag/Fe/Pt(111) film.