放电等离子烧结Ti-Al系金属间化合物

用机械合金化法(MA)制备了Ti-45% Al纳米晶合金粉末,并对其进行放电等离子烧结(SPS),烧结时间仅为5min.用D-maxIIA型X射线衍射仪、JEM-2000EX型透射电子显微镜对粉末和烧结块体的微观组织及机械性能进行了研究.研究表明:Ti和Al的粉末随着球磨时间的延长,粉末有明显的细化趋势,球磨5h即有非晶产生,球磨20h后得到接近完全非晶相;采用SPS烧结技术,在1200℃下能够制备出较高硬度的TiAl金属间化合物块体材料.     

高纯多晶LaB6纳米块体阴极材料的制备及表征

采用放电等离子烧结技术, 以氢直流电弧法制备的La-LaH₂纳米粉末为原料, 制备了高纯LaB₆多晶纳米块体热阴极材料. 系统研究了LaH₂的脱氢反应、SPS合成LaB₆的烧结反应式, 并用XRD、SEM、TEM和AFM对LaB₆烧结块体的相与结构进行了表征. 实验结果表明, LaH2在796.4℃时发生脱氢反应; SPS制备得到了单相LaB₆纳米多晶块体, 纯度达到99.867%, 相对密度达到99.2%, 和其他烧结方法相比, 样品显微硬度及抗弯强度等性能显著提高. 晶体为大小均匀, 形态规则完整的等轴晶, 50MPa, 烧结温度1250～1350℃范围内平均晶粒尺寸为120nm, 随烧结温度的升高, 晶粒尺寸逐渐增大.     

Influence of Sintering Temperatures on the Phase Structure and Magnetic Properties of Spark Plasma Sintered SmCo5 Magnets

Journal of Superconductivity and Novel Magnetism - SmCo5 magnets were prepared by spark plasma sintering (SPS) technique. The phase constitutions, magnetic properties, and microstructures of...     

制备工艺对n型Bi_2Te_3基材料热电性能和抗压强度的影响

以商用区熔(ZM)n型Bi2Te3基材料为原料,采用简单研磨结合放电等离子烧结技术(ZM+SPS)和熔体旋甩(MS)结合放电等离子烧结技术(MS+SPS)制备了n型Bi2Te3基块体热电材料.对三种不同工艺制备出样品的微结构、热电性能和力学性能进行了研究.FESEM微结构表征结果表明:区熔样品的晶粒粗大,有较强的取向性;经SPS烧结后,晶粒细化,取向性大为降低;而区熔样品经MS+SPS后,晶粒得到进一步细化,且没有明显的取向性.对三组样品进行的热电性能和抗压强度测试,结果表明:区熔原料最大ZT值为0.72(430K),抗压强度仅为40MPa;经SPS后,样品的最大ZT值为0.68(440K),抗压强度为110MPa,相比区熔样品提高了175%;MS+SPS样品的最大ZT值为0.96(320K),其室温ZT值相比区熔样品提高了64%,抗压强度相比区熔样品提高了400%,达到200MPa.     

Zirconia nanoceramic via redispersion of highly agglomerated nanopowder and spark plasma sintering

A 2.7 mol% yttria stabilizing tetragonal zirconia (2.7Y-TZP) nanopowder was synthesized and stored for five years. Humidity and unsatisfactory storage conditions gradually caused heavy agglomeration. Within a few months, 2.7Y-TZP nanopowder became useless for any technological application. A bead-milling deagglomeration technique was applied to recover the heavily agglomerated yttria-stabilized zirconia nanopowder. Low-temperature sintering and spark plasma sintering (SPS) were performed, resulting in fully dense nanostructured ceramics. Compacts formed with heavily agglomerated powder present low sinterability and poor mechanical properties. Bead-milling suspension formed compacts exhibit mechanical properties in the range of the values reported for nanostructured zirconia. This observation confirms the effectiveness of bead-milling in the deagglomeration of highly agglomerated nanopowders. The high value of Vickers hardness of 13.6 GPa demonstrates the success of the processing technique for recovering long-time-stored oxide nanopowders.     

Nanostructured Composite Materials with Improved Deformation Behavior

The recent progress in the development of nanostructured composites is described for Zr‐base multicomponent alloys as a typical example for such materials. These advanced composite materials are attractive candidates for structural as well as functional applications. The combination of high strength with high elastic strain of fully nanocrystalline and glassy alloys renders them quite unique in comparison to conventional (micro‐)crystalline materials. However, one major drawback for their use in engineering applications is the often limited macroscopic plastic deformability, despite the fact that some of these alloys show perfectly elastic‐plastic deformation behavior. To improve the room temperature ductility of either fully nanocrystalline or amorphous alloys, the concept of developing a heterogeneous microstructure combining a glassy or nanostructured matrix with second‐phase particles with a different length‐scale, has recently been employed. This review describes the composition dependent metastable phase formation in the Zr‐(Ti/Nb)‐Cu‐Ni‐Al alloy system, which in turn alters the mechanical properties of the alloys. We emphasize the possibilities to manipulate such composite microstructures in favor of either strength or ductility, or a combination of both, and also discuss the acquired ability to synthesize such in‐situ high‐strength composite microstructures in bulk form through inexpensive processing routes.     

B掺杂Si80Ge20合金的快速制备及热电性能

采用电弧熔炼、快速球磨结合放电等离子烧结快速制备了单相Si80Ge20Bx(x=0.5、1、1.5、2)热电材料,对烧结后试样进行了物相结构分析和热电性能表征.结果表明,B的引入导致样品载流子浓度增加,电导率随着B掺量增加而大幅增加,而Seebeck系数反之下降.B的固溶增加试样中点缺陷浓度而导致声子散射增加,热导率下...     

Phase Stability in Nanostructures

Nanostructured materials provide access to tailor‐made materials properties by microstructural design. Excellent mechanical properties such as high strength or wear resistance are often found in nanocrystalline materials. For magnetic materials, the design of nanostructured composites offers advantages if the structural scales match the intrinsic magnetic length scales. In some cases, as in the new nanocrystalline soft magnetic alloys, the combination of amorphous and nanocrystalline phases is necessary to obtain the desired properties. This rises the question of the limiting size for a stable crystalline structure, especially in contact with an amorphous phase. These considerations, which have been of interest for basic research in the context of the microcrystalline model for amorphous materials, are of technical importance for the optimization of nanostructured composites. Recent model experiments about the stability of thin Fe‐based glass forming alloy films are reviewed. A relationship between phase stability, composition, and interface density has been established. The implications of the results for the design of nanostructured alloy systems are discussed.     

纳米结构陶瓷涂层的制备技术

与传统的微米级陶瓷涂层相比,纳米结构陶瓷涂层的结合强度、断裂韧性、耐磨性等会显著提高,目前已在军民领域开始应用。纳米陶瓷涂层的制备存在一定的特殊性和较大难度,并且制备工艺会对涂层的组织和性能产生直接影响。本文对纳米结构陶瓷涂层的制备技术进行了详细介绍。     

Spark plasma sintering on nanometer scale WC–Co powder

Nanometer scale WC–11Co powder was sintered by spark plasma sintering (SPS) process in order to improve the properties of the cemented carbides. Properties such as density and hardness were measured. The microstructures of sintered WC–11Co cemented carbides were observed. The grain size of WC in alloys was also obtained. The results showed that spark plasma sintering could lower the sintering temperature, increased the density and circumscribed the growth of grain size of WC. Besides, the hardness of the sintered cemented alloys that was dependent on the grain size and densification could also be improved by SPS. SPS was an effective method to get WC–11Co cemented carbides with fine grain size and good properties.     

放电等离子烧结(SPS)技术与新材料研究

放电等离子烧结(SPS)作为一种材料的绿色制备新技术,正成为国内外材料领域的研究热点.介绍了SPS的工艺特点和装置、国内外发展状况以及特殊的烧结机理;阐述了SPS在功能梯度材料、生物材料、超细或纳米晶WC-Co硬质材料、镁合金等新材料制备方面的应用及优势.最后分析了SPS技术亟待解决的问题和今后的发展趋势.     

Novel In Situ Nanostructure-Dendrite Composites in Zr-Base Multicomponent Alloy System

The evolution of a nanostructure-dendrite composite microstructure of two Zr-base alloys solidified through different casting routes is presented. The alloys were designed by adding different amounts of Nb to the Zr-based multicomponent glass-forming alloy system. The refractory metal Nb promotes the formation of a primary phase having dendritic morphology, whereas the residual melt solidifies to a nanostructured/amorphous matrix. The volume fraction and the morphology of the dendritic phase varied with the Nb content and the adopted casting route. A correlation between the alloy composition and adopted casting method with evolved microstructures and mechanical properties is revealed. These composites exhibit a unique combination of high fracture strength up to 1922 Mpa, as well as plastic strain over 15.8% under uniaxial compression testing at room temperature. The high strength of these composites is imparted by the nanostructured matrix, whereas the large plastic strain is a consequence of the retardation of excessive localized shear banding in the matrix by ductile dendrites. The significant work hardening of the composites prior to fracture is attributed to dislocation multiplication in the solid solution-strengthened dendritic phase.     

超声化学结合放电等离子烧结制备In4Se3化合物的热电性能研究

采用超声化学和后续还原热处理工艺合成了单相In4Se3化合物粉体,并结合放电等离子烧结技术(SPS)制备了致密的块体材料.对所得的块体材料的微结构和热电传输性能进行了系统研究.结果表明,块体样品的晶粒细小、排列紧密并存在显著的择优取向,同时样品中存在大量精细的层状结构,这使得块体样品的电热传输性能也表现出明显的各向异性.由于具有较高的Seebeck系数和较低的热导率,沿着SPS压力方向上样品表现出较好的热电性能,其最大ZT值在700 K可达到0.56,这与其它物理技术制备的In4Se3多晶材料的性能相当.     

LED用荧光玻璃的制备及性能研究

以行星球磨得到的SiO₂粉体和商用Ce:YAG荧光粉为原料, 采用放电等离子体烧结技术(简称SPS)成功制备块体荧光玻璃。利用XRD、SEM、紫外/可见光分光光度计和荧光光谱仪等研究了Ce:YAG荧光玻璃的物相、显微结构、吸收和发光性能等。研究结果表明: SPS烧结制备的块体荧光玻璃样品主体是非晶相, 同时荧光粉颗粒在玻璃基质中均匀分布, 颗粒大小也未发生变化, 这表明荧光粉晶体在SPS烧结过程中没有发生化学分解反应, 在玻璃基体中得到很好地保存。该荧光玻璃吸收峰在460 nm左右, 发射波长在530 nm左右。通过对不同含量荧光粉的荧光玻璃进行发光性能表征, 发现荧光粉含量为3wt%的荧光玻璃性能最佳, 以此封装的白光LED样品在800 mA电流驱动下, 获得白光输出, 色坐标为(0.33, 0.38)。     

Fabrication of Ti–Nb–Ag alloy via powder metallurgy for biomedical applications

Ti and some of its alloys are widely used as orthopedic implants. In the present study, Ti–26Nb–5Ag alloys were prepared by mechanical alloying followed by vacuum furnace sintering or spark plasma sintering (SPS). The microstructure and mechanical properties of the Ti–Nb–Ag alloys were investigated using X-ray diffraction (XRD), scanning electron microscopy (SEM) combined with energy-dispersive X-ray spectroscopy (EDX), compressive and micro-hardness tests. The effect of different sintering methods on the microstructure and properties of Ti–Nb–Ag alloy was discussed. The results showed that the titanium alloy sintered by vacuum furnace exhibited a microstructure consisting of α, β and a small amount of α″ martensite phase; whilst the SPS sintered alloy exhibited a microstructure consisting of α, β and a small amount of α″ martensite phase, as well as a nanostructured Ag homogeneously distributed at the boundaries of the β phases. The Ti–Nb–Ag alloy sintered by SPS possessed fracture strength nearly 3 times of the alloy sintered by vacuum furnace.     

Functional properties of silicon nanocrystals in oxygen-rich amorphous matrices formed by laser irradiation of substoichiometric silicon oxides

Silicon-based nanostructured thin films have been obtained through laser irradiation of amorphous silicon oxides. The optoelectronic properties of nanostructured films largely differ from their amorphous counterpart, exhibiting optical gap narrowing, wavelength-dependent spectral modification of the photoluminescence (PL) and conduction mechanism variations. In particular, following the hydrogen effusion and related defect density increase, a spectral red shift and PL intensity quenching is detected for λ_exc=514.5 nm, whereas PL enhancement and spectral blue shift is observed at λ_exc=632.8 nm. Different thermal activation regimes of conductivity are also detected by conductivity measurements.Such results are discussed in terms of microstructural changes from an hydrogenated amorphous network to a nanostructured two-phase material where wavelength-selective excitation of radiative recombination channels and temperature-dependent conductivity paths occurs.     

La1-xNdxB6阴极材料的制备及性能研究

以高纯金属La块、Nd块和B粉为原料, 通过蒸发-冷凝与放电等离子烧结(SPS)结合的技术成功制备了高纯高致密的多元稀土六硼化物La_1-xNd_xB₆块体材料。系统研究了La_1-xNd_xB₆材料的物相组成、力学性能、电阻率及热电子发射性能。结果表明, 采用上述工艺制备了高纯高致密的La_1-xNd_xB₆单相块体材料。烧结样品的维氏硬度和抗弯强度可达26.70 GPa和230.48 MPa。热电子发射性能测试结果表明, La_0.1Nd_0.9B₆成分块体具有最佳的热发射性能, 在1600℃, 4 kV外加电压条件下, 发射电流密度达到32.04 A/cm², 零场电流密度达到12.72 A/cm², 在同样条件下优于纯LaB₆和NdB₆块体材料的热发射性能。计算得到La_0.1Nd_0.9B₆在不同温度下的平均有效逸出功为2.72 eV, 表明适当比例的复合可以降低逸出功, 提高热电子发射性能。     

High-rate deposition of nanostructured SiC films by thermal plasma PVD

With ultrafine SiC powder as starting material, thermal plasma physical vapor deposition has been applied successfully to the deposition of SiC films on Si substrates. The control of processing parameters such as substrate temperature, powder feeding rate and composition of plasma gases, permits the deposition of SiC films on a wide area of around 400 cm² with a variety of microstructures from amorphous to nanostructured and with various morphologies from dense to columnar. For the nanostructured case, the crystallite size was between 3 and 15 nm and the maximum deposition rate calculated based on the actual deposition duty time reached 200 nm/s. The deposition mechanism is discussed briefly.     

The new trends in fabrication of bulk nanostructured materials by SPD processing

During the past decade, fabrication of bulk nanostructured metals and alloys using severe plastic deformation (SPD) has been evolving as a rapidly advancing direction of nanomaterials science and technology aimed at developing materials with new mechanical and functional properties for advanced applications. The principle of these developments is based on grain refinement down to the nanoscale level via various SPD techniques. This paper is focused on investigation and development of new SPD processing routes enabling fabrication of fully dense bulk nanostructured metals and alloys with a grain size of 40–50 nm and smaller, namely, SPD-consolidation of powders, including nanostructured ones, as well as SPD-induced nanocrystallization of amorphous alloys. We also consider microstructural features of SPD-processed materials that are responsible for enhancement of their properties.     

机械合金化和SPS工艺制备9CrWTi-Y2O3/铁素体-马氏体钢

采用机械合金化(MA)和放电等离子体烧结(SPS)工艺制备了9CrWTi-0.35%Y₂O₃氧化物弥散强化铁素体-马氏体钢(9CrWTi-0.35%Y₂O₃/FMs)。利用SPS温度和位移测量装置、 OM、 FE-SEM、 TEM、 EDX表征了材料烧结收缩曲线及热处理前后的显微组织和成分, 并采用电子拉伸试验机测试了室温拉伸性能。结果表明: 9CrWTi/FMs和9CrWTi-0.35%Y₂O₃/FMs在烧结过程出现液相烧结特征。提高烧结温度和压力, 9CrWTi-0.35%Y₂O₃/FMs孔隙度减小, 密度提高, 晶粒变细, 抗拉强度增加, 但延伸率仅为2%左右。富集Y-Ti-O的弥散相颗粒大小为5～20 nm, 较均匀地分布在基体上。9CrWTi-0.35%Y₂O₃/FMs烧结态、 10%盐水淬火态及750 ℃高温回火态的显微组织分别为等轴铁素体、 细长板条马氏体及等轴和残余铁素体。9CrWTi-0.35%Y₂O₃/FMs烧结体经盐水淬火、 回火后, 抗拉强度、 屈服强度和总延伸率由1554 MPa、 1430 MPa、 1.8%变为1198 MPa、 1006 MPa和12.8%。