正交试验法优化金刚石复合片合成工艺

 通过正交试验法,以磨耗比、电阻、完整性、硬度为指标,设计了金刚石复合片的合成工艺。正交试验可以减少合成工艺试验次数,优化合成工艺。试验结果表明,较合理的烧结工艺为：合成压力5.5 GPa,升温速度为200 ℃/min,保温时间16 min,冷却时间14 min,烧结温度1 350 ℃。从压力、温度和时间等因素的影响方面讨论了金刚石复合片的性能。认为：适当地提高温度有利于提高磨耗比及硬度;延长加热时间有利于性能均匀性的提高;延长冷却时间可减少残余热应力。     

Multiple-step martensitic transformations in Ni-rich NiTi alloys--an in-situ transmission electron microscopy investigation

Multiple-step martensitic transformations in Ni-rich NiTi shape memory alloys have so far been rationalized on the basis of dislocation stress fields, coherency stress fields around Ni 4 Ti 3 precipitates and evolving Ni concentrations between precipitates during ageing. The primary objective of the present paper is to show that such transformations can also occur owing to heterogeneous microstructures that form during ageing of solution annealed defect-free materials. These microstructures are characterized by Ni 4 Ti 3 grain-boundary precipitation and by precipitate-free grain interiors. Two microstructures which give rise to two and three distinct differential scanning calorimetry (DSC) peaks on cooling from the B2 regime are subjected to in-situ cooling and heating cycles in the transmission electron microscope. Martensitic transformations are directly studied and the observations provide a new explanation for multiple-step martensitic transformations in Ni-rich NiTi alloys. Most importantly the results of the present study allow us to understand why DSC chart features on cooling from the B2 regime change during ageing, where they lose their one-step character (after solution annealing at 1123 K for 900 s) and evolve from two-step (after ageing at 773 K for 3.6 ks) to three-step (after ageing at 773 for 36 ks K) transformations.     

纯钨红外光谱发射率特性研究

光谱发射率是一个重要的热物性参数,在辐射测温、热传输计算等领域有着广泛的应用。钨作为一种重要的金属,关于其光谱发射率的研究报道较少。利用黑体炉、傅里叶红外光谱仪、加热装置和光学系统搭建了一套能量对比法光谱发射率测量装置,该装置能够测量3~20μm的光谱发射率,测量装置的整体不确定度优于5%。利用该装置测量了纯钨在4个温度点(573, 673, 773和873 K)的法向光谱发射率,重点探讨了氧化、温度、波长和加热时间对纯钨光谱发射率的影响。研究结果表明:纯钨在表面未氧化的情况下,光谱发射率在几个温度点的变化规律基本一致,且数值相差较小,而当其表面发生氧化后光谱发射率迅速增加,在某些波长处出现了强烈的振荡。表面未氧化时纯钨的光谱发射率受温度的影响较小,随着温度的增加仅出现微小的增加,但是当表面发生氧化后,随温度的升高而迅速增大。纯钨的光谱发射率整体上随着波长的增加而减小,但是当表面发生氧化后,由于表面氧化膜与钨金属基底发生干涉效应,在4, 9, 12.5和16.5μm处均出现了峰值。在573和673 K,纯钨的光谱发射率随着加热时间的增加无明显变化。然而,随着温度的升高,在773和873 K时,光谱发射率随着加热时间增加而增大,在773 K时光谱发射率随加热时间的增加增幅较大,因为在该温度点,纯钨表面刚开始发生氧化,氧化速率较大,在873 K时光谱发射率随加热时间的增加增幅较为平缓,并且随着加热时间的增长呈现稳定的趋势。综上,纯钨的光谱发射率在温度较低和表面未氧化时较为稳定。随着温度的升高,当表面发生氧化后,光谱发射率迅速增大,并且在多个波长位置出现了强烈的振荡。由此可见,纯钨光谱发射率受温度、波长、加热时间的影响较大,在实际应用过程中,特别是在辐射测温过程中,如果把纯钨的光谱发射率看做常数将会带来较大的测量误差。该研究将进一步丰富钨的光谱发射率数据,并为其在科学研究和应用中提供数据支持。     

Thermal hysteresis of a simulated Al<Subscript>2</Subscript>O<Subscript>3</Subscript> system

Thermal hysteresis in a simulated Al₂O₃ system has been investigated using a Molecular Dynamics (MD) method. Simulations were done in the basic cube under periodic boundary conditions containing 3000 ions with Born-Mayer type pair potentials. The system was cooled down from 7000 K to 0 K and heated up from 0 K to 7000 K by the same cooling/heating rate of 1.7178×10¹⁴ K/s. The temperature dependence of the system density upon cooling and heating shows thermal hysteresis. The differences between structure and dynamics of the models obtained by cooling (MOBC) and heating (MOBH) at three different temperatures of 2100 K, 3500 K and 5600 K have been detected. Calculations show that the differences in the dynamics of the systems are more pronounced than those in the structure. Furthermore, dynamical heterogeneities in MOBC and MOBH at the temperature of 2100 K have been studied through a non-Gaussian parameter and comparison of partial radial distribution functions (PRDFs) for the 10% most mobile or immobile particles with their corresponding mean ones. Cluster size distributions of the 10% most mobile or immobile particles in MOBC and MOBH at the temperature of 2100 K have been obtained. Calculations show that differences in dynamical heterogeneities are pronounced.     

Hall mobility of undoped n-type conducting strontium titanate single crystals between 19 K and 1373 K

The Hall mobility of undoped n-type conducting SrTiO₃ single crystals was investigated in a temperature range between 19 and 1373 K. Field calculations were used to estimate the influence of sample shape and electrode geometry on the measured values. Between 19 and 353 K samples, which were quenched under reducing conditions, show an impurity scattering behavior at low temperature and high carrier concentrations and a phonon scattering mechanism at room temperature. In this temperature region, no carrier-density-dependent mobility was found. In conjunction with measurements of the mass difference before and after reoxidation, the oxygen deficiency and the oxygen vacancy concentration could be determined. The oxygen vacancies proved to be singly ionized. Above 873 K, Hall mobility and carrier concentration had been determined as a function of both oxygen partial pressure and temperature for the first time. In this temperature range the mobility does not depend on carrier concentration, but shows aT ^–1.5 dependence.     

Synthesis and characterization of a nano-scaled barium cerate perovskite powder using starch as polymerization agent

The preparation of nano-sized BaCeO₃ powder using starch as a polymerization agent is described herein. Phase evolution during the decomposition process of a (BaCe)-gel was monitored by XRD. A phase-pure nano-sized BaCeO₃ powder was obtained after calcining of the (BaCe)-gel at 920 °C. The resulting powder has a specific surface area of 15.4 m²/g. TEM investigations reveal particles mainly in the size range of 30 to 65 nm. The shrinkage and sintering behavior of resulting powder compacts were studied in comparison to a coarse-grained mixed-oxide BaCeO₃ powder (S_BET = 2.1 m²/g). Dilatometric measurements show that the beginning of shrinkage of compacts from the nano-sized powder is downshifted by 300 °C compared to mixed-oxide powder. Compacts from the nano-sized powder reach a relative density of 91% after sintering at 1450 °C for 10 h.     

Quick preparation and thermal transport properties of nanostructured β-FeSi2 bulk material

This paper reports that the nanostructured β-FeSi2 bulk materials are prepared by a new synthesis process by combining melt spinning(MS) and subsequent spark plasma sintering(SPS).It investigates the influence of linear speed of the rolling copper wheel,injection pressure and SPS regime on microstructure and phase composition of the rapidly solidified ribbons after MS and bulk production respectively,and discusses the effects of the microstructure on thermal transport properties.There are two crystalline phases(α-Fe2Si5 and ε-FeSi) in the rapidly solidified ribbons;the crystal grains become smaller when the cooling rate increases(the 20 nm minimum crystal of ε-FeSi is obtained).Having been sintered for 1 min above 1123 K and annealed for 5 min at 923 K,the single-phase nanostructured βFeSi2 bulk materials with 200-500 nm grain size and 98% relative density are obtained.The microstructure of β-FeSi2 has great effect on thermal transport properties.With decreasing sintering temperature,the grain size decreases,the thermal conductivity of β-FeSi2 is reduced remarkably.The thermal conductivity of β-FeSi2 decreases notably(reduced 72% at room temperature) in comparison with the β-FeSi2 prepared by traditional casting method.     

白铜热氧化过程中光谱发射率特性研究

随着科技的发展,工业领域对白铜产品质量的要求日益提升;利用辐射测温技术对白铜在冶炼和加工时的温度进行精确测量,是决定产品质量的重要手段,因此研究白铜的光谱发射率特性就显得尤为重要。基于傅里叶红外光谱仪搭建的光谱发射率测量装置,测量了白铜在四个温度点（673,773,873和973 K）,波长范围2～22 μm内的光谱发射率,分别研究了波长、温度、加热时间和氧化对白铜光谱发射率的影响。研究发现,在氮气环境下白铜的光谱发射率随温度的升高而增加,随波长的增加而减少。当白铜暴露在空气环境中,随着温度的升高,其光谱发射率迅速增加。673 K时,白铜表面生成一层细微的氧化物颗粒,阻止白铜进一步氧化,这些氧化物颗粒的光谱发射率大于白铜基底,所以此温度下短波处的光谱发射率略微增加。773 K时,白铜表面氧化物的主要成分是Cu₂O,在实验过程中也观察到白铜表面逐渐变红的现象,这也是白铜在773 K温度下其光谱发射率迅速增加的原因。873 K时,白铜表面氧化物的种类和含量明显增多,氧化膜的厚度满足干涉效应条件,在白铜的光谱发射率曲线中可以明显地观察到干涉极值的演变,随着加热时间的增加,干涉极值逐渐向长波移动。随着温度的升高,白铜的抗氧化能力下降。973 K时,白铜表面的氧化程度最深,在XRD图中氧化物的峰值也最大,因此氧化1 h后由于干涉效应产生的干涉极值数最多。综上所述,波长、温度和氧化对白铜的光谱发射率有重要的影响,在运用辐射测温技术测量白铜温度时应充分考虑上述因素的影响。该研究丰富了白铜的光谱发射率数据,为辐射测温提供了真实可靠的数据支撑。     

Consolidation of cryomilled Al–Si using spark plasma sintering

Cryomilled eutectic aluminum–12% silicon powder was sintered using spark plasma sintering (SPS) to create bulk compacts. The cryomilling serves to break up and disperse the eutectic phase in the powder to create a well-distributed Si phase throughout the matrix and to modify the morphology of the Si phase from plate-like to spherical, whilst refining the aluminium grain size to the nanometric level. The effects of different sintering times and temperatures using SPS on the densification of the powder, the aluminium grain size evolution, the growth of the Si phase and the morphology change of the Si phase were investigated. The compacts were analysed using X-ray diffraction, scanning electron microscopy and optical microscopy. The initial stages of densification appear to be highly dependent on the yield strength of the powder. An estimate of the temperature gradient seen in the powder bed was made and calculated to be near 200?°C at the highest point. The Al and Si phase growth was investigated and it was observed that the Si coarsening rate is increased due to the increased volume of grain boundaries. As the Si coarsens, any pinning effect on the Al grains is lost, resulting in a highly unstable microstructure that coarsens rapidly.     

冷却速率对液态金属Cu凝固过程中微观结构演变影响的模拟研究

采用Quantum Sutton-Chen(Q-SC)多体势对液态金属Cu在四个不同冷却速率下的凝固过程进行了分子动力学模拟研究. 通过双体分布函数、键型指数、配位数、均方位移及可视化分析, 结果表明：冷却速率对液态金属Cu的微观结构演变有决定性影响. 当冷却速率为1.0×10¹⁴K/s时得到非晶态结构；当冷速分别为1.0×10¹³K/s，1.0×10¹²K/s和1.3×10¹¹K/s时，系统形成以1421键型为主体的面心立方(fcc)与六角密集(hcp)共存的混合晶体结构；且其结晶温度分别为373K，773K和873K，即冷速越慢，其结晶温度越高，结晶程度也越高；且冷速越慢，1421键型越多，混合晶体中面心立方(fcc)结构所占的比例越高. 同时发现，原子的平均配位数的变化与1551，1441，1661键型的变化密切相关, 反映出体系对称性结构的变化规律与配位数的变化有关. 在可视化分析中，进一步采用中心原子法展现出非晶态与晶体结构的2D截面，及在3D下混合晶体中两个基本原子团分别为面心立方(fcc)与六角密集(hcp)基本原子团的具体结构. 关键词： Q-SC多体势 液态金属Cu 凝固过程 分子动力学模拟     

放电等离子固相烧结制备高密度LaB_6阴极性能

采用放电等离子烧结(SPS)技术,以碳化硼还原法制备的LaB6粉末为原料,制备了高致密LaB6多晶块体阴极,并系统研究了烧结温度、压力对LaB6烧结样品的物相、结构和性能的影响。确定了SPS烧结LaB6的最佳工艺为:压力50MPa,烧结温度1650℃,保温时间10min。实验结果表明:与其它LaB6多晶制备方法相比,SPS制备得到的LaB6烧结块体的力学及发射性能均有大幅提高,样品相对密度达到96.2%,维氏硬度达到1720kg/mm2,抗弯强度达到203.2MPa。样品在1520℃温度下发射电流密度达到17.41A/cm2,功函数为2.40eV。SPS制备法显著降低了LaB的烧结温度,缩短了烧结时间。     

Molecular dynamics simulation of neck growth in laser sintering of different-sized gold nanoparticles under different heating rates

The neck growth in the laser sintering of different-sized gold (100) nanoparticles under different heating rates is investigated using a molecular dynamics method. The numerical simulations are carried out for four pairs of two spherical nanoparticles under three different heating rates. For each pair, one nanoparticle has the same diameter of 4 nm and the other nanoparticle’s diameter is varied, ranging from 4 nm to 20 nm. The results show that the solid state sintering automatically takes place by local potential at room temperature. The stable neck width increases as the size of the other nanoparticle increases. Once the limit stable neck width is reached, it no longer is affected by the nanoparticle size. For the subsequent laser heating to the same final temperature, a lower heating rate results in a larger stable neck width due to the longer sintering process. The neck growth mechanisms and rate under various sintering conditions are discussed.     

Improved microstructure, dielectric and ferroelectric properties of microwave-sintered Sr0.5Ba0.5Nb2O6

Ferroelectric strontium barium niobate (SBN) powder was synthesized by solid-state route. The green compacts were sintered in the temperature range 1250–1350 °C in a microwave furnace. The microstructural study, using SEM, revealed the grain size in the range 2–20 μm without microcracks, depending on the sintering temperature. This is in contrast to that obtained conventionally for sintered SBN powder synthesized by solid-state route, which resulted in duplex microstructure with microcracks [N.S. VanDamme, A.E. Sutherland, L. Jones, K. Bridger, S.R. Winzer, J. Am. Ceram. Soc. 74 (1991) 1785; P.K. Patro, A.R. Kulkarni, C.S. Harendranath, Ceram. Int. 30 (2004) 1405; P.K. Patro, Trans. Ind. Inst. Metals 59 (2006) 229]. Impedance analyzer and ferroelectric hysteresis loop tracer were used for the dielectric, ferroelectric, I–V and electric fatigue measurements. Microwave sintering also resulted in a dielectric maxima ε_max 2590 at 1 kHz (compared to 1103 for conventional sintering [P.K. Patro, A.R. Kulkarni, C.S. Harendranath, Ceram. Int. 30 (2004) 1405]) for the sintering temperature of 1350 °C. Similar improvement in microwave-sintered SBN was observed depending on their sintering condition. The origin of this difference is attributed to microstructural differences arising from difference in heating method. In this paper the observed dielectric and ferroelectric behavior have been correlated with different sintering conditions and consequent microstructure due to microwave sintering.     

Dependence of the magnetic and magnetoelastic properties of cobalt ferrite on processing parameters

The dependence of the magnetic and magnetoelastic properties of highly magnetostrictive cobalt ferrite on processing parameters has been investigated. The cobalt ferrite samples used in this study were prepared via conventional ceramic processing methods. The processing parameters of interest were sintering temperature, holding time at the sintering temperature and powder compaction pressure. It was observed that the crystal structure, composition and saturation magnetization of the samples studied did not vary with changes in processing parameters but coercive field decreased with increasing sintering temperature. The amplitude of peak to peak magnetostriction was dependent on the holding time and powder compaction pressure. The strain derivative on the other hand was found to depend on powder compaction pressure at any given sintering temperature or holding time. The results show how the magnetoelastic properties of cobalt ferrite can be varied by changing the processing parameters.     

Aluminium-based amorphous and nanocrystalline alloys with Fe impurity

Aluminium-based rapidly quenched alloys of nominal composition of Al₉₀Fe₇Nb₃ and Al₉₄Fe₂V₄ were studied by Mössbauer spectroscopy. Samples annealed up to 573K showed amorphous structure represented by quadrupole-split doublets. From the corrected spectra areas, the values of f-factor and Debye temperature were calculated for both samples in the as-cast state. In the case of AlFeNb sample, f-factor was estimated to be f = 0.26 and for AlFeV, f = 0.31. High-temperature annealing at 773K and 873K induced a formation of nano-and microcrystalline structures. Mössbauer spectra of both compositions (with vanadium as well as with niobium) annealed at 773K showed superposition of crystalline phases with dominant contribution of Al₃Fe alloy. During annealing at 873K, phases with large grains and a small amount of the FeAl metastable phase were developed.     

Trap distribution changes in quenched KCl by heating or pressure

Pure Potassium chloride, when quenched rapidly from melt shows pronounced glow peak at 250°K. The intensity of the glow peak has been found to decrease by heating the specimen to around 450°K, or by subjecting it to pressure. A qualitative interpretation of these effects has been offered on the basis of quenched —in cation —anion vacancy pairs.     

Characterization of a spark discharge for dust cloud ignition

Spark discharges are widely used to ignite flammable gases, liquids, or dust. For a better understanding of the interaction between the spark discharge and the ignited media (gas, liquid, or dust), it is necessary to measure some key parameters of the spark, especially the space‐time variation of its temperature. Determination of temperature gradients would allow a more precise and realistic simulation of the ignition process. In fact, electrons and particles in the discharge zone get their energy with increasing temperature before interacting with particles of the media to ignite the flame. In this study, optical emission spectroscopy of the spark discharge between two tungsten electrodes was performed. Assuming excitation balance between the WI lines, a Boltzmann plot after an Abel inversion gives the excitation temperature and its space‐time variation. For a 100‐μs time discharge, at 80‐μs delay, we measured 7,000 K at the centre of the column zone, 4,100 K at the centre of the cathode zone, and 3,600 K at the centre of the anode zone. Assuming a singly ionized tungsten plasma and excitation equilibrium, we used also the Saha–Boltzmann equation to calculate the plasma composition. The electron density at the column zone was about 3 × 10¹⁷ cm^?3, which is two orders of magnitude higher than in the rest of the spark.     

Thermoluminescence of pretreated NaCl: Sr crystals

Thermal glow curves of thermally pretreated NaCl:Sr crystals have been recorded after irradiation with ultraviolet light at room temperature. The observed glow curves exhibit a prominent glow peak at 380°K only when the specimen is annealed and quenched from 750°C. This peak is attributed to the dipole clusters which disintegrate after heating the specimen beyond 380°K     

Successive phase transformation in ferromagnetic shape memory alloys Co37Ni34Al39 melt-spun ribbons

The martensitic transformation in Co37Ni34Al29 ribbon is characterized in detail by means of in-situ thermostatic x-ray diffraction and magnetic measurements.The results show a structural transition from the body-centred cubic to martensite with a tetragonal structure during cooling.Comparison between the results of the diffraction intensity with the magnetic susceptibility measurements indicates that the martensitic transformation takes place in several different steps during cooling from 273 to 163 K.During heating from 313 to 873 K,the peak width becomes very wide and the intensity turns very low.The γ-phase(face-centred cubic structure) emerges and increases gradually with temperature increasing from 873 to 1073 K.     

大面积环状LaB6阴极

 介绍了一种用于管状电子束发射的大面积LaB₆阴极电子源，其阴极发射面积为115 mm²，LaB₆发射体用钼作基底，在LaB₆与钼之间用耐高温的碳化物粘合剂填充以防止LaB₆与钼发生反应。采用电子束轰击的方式加热LaB₆发射体，当阴极温度为1 873 K时，加热功率为173 W，直流发射电流密度达到40 A/cm²。与用石墨加热LaB₆发射体相比，该电子源加热功率降低了66%。阴极在室温下反复暴露于大气后其发射性能稳定。