Microstructural evolution and mechanical properties of Nb-Si-Cr ternary alloys with a tri-phase Nb/Nb5Si3/Cr2Nb microstructure fabricated by spark plasma sintering

In this work, pure Nb, Nb₅Si₃ and Laves Cr₂Nb compound powders were used as raw materials to prepare Nb-Si-Cr ternary alloys by spark plasma sintering (SPS). A comprehensive estimation of the microstructure and properties, including room temperature fracture toughness, high temperature strength and oxidation resistance, of the Nb-Si-Cr ternary alloys as a function of the Nb/Nb₅Si₃/Cr₂Nb phase volume fraction combinations was conducted. The results showed that Nb-Si-Cr ternary samples with the relative density larger than 98.42% were obtained by SPS processing, and the samples all consisted of Nb, Nb₅Si₃ and Cr₂Nb phases that were distributed homogeneously. The fracture toughness K_Q of the Nb/Nb₅Si₃/Cr₂Nb microstructure, which was dominated by the Nb phase, naturally increased with the Nb fraction. As expected, the room-temperature Vickers hardness and the high-temperature strength of the bulk alloys increased monotonically with the increasing of the stiffening Nb₅Si₃ fraction. Interestingly, the binary Cr₂Nb phase played a positive role in the high temperature strength and oxidation resistance. Finally, the fracture modes of the typical Nb/Nb₅Si₃/Cr₂Nb microstructures under bending and compression conditions at room and high temperatures as well as the oxidation mechanism are described and discussed.     

Sintering mechanism of Cu-9Al alloy prepared from elemental powders

The sintering behavior of Cu-9Al alloys prepared from die pressing of elemental powders was investigated. The experimental results and kinetic analysis showed the formation of three consecutive layers of Al₂Cu, Al₄Cu₉, and AlCu phases, with Al₂Cu appearing first in the initial solid phase sintering stage. A liquid phase formed in the intermediate stage, resulting from the eutectic reaction between Al and Al₂Cu phases at 500 °C, which is 47 °C lower than the equilibrium reaction temperature. Swelling occurred when the liquid phase infiltrated the gaps between the copper particles, leaving pores at the original sites of Al particles and Al₂Cu. In the final stage of sintering, the Al-rich phases (Al₂Cu and AlCu) transformed to Al-poor phases (Al₄Cu₉ and α-Cu) in the temperature range of 500–565 °C. Al₄Cu₉ and α-Cu then transformed to AlCu₃ (β) above the eutectoid reaction temperature (565 °C), whereas AlCu₃ transformed to α-Cu and eutectoid phases (α-Cu + Al₄Cu₉) during cooling. The pure copper transformed to AlCu₃, and the pore volume decreased at 1000 °C. The microstructure study helps manipulate precisely the sintering process of Cu-Al alloys and optimize the microstructure with a high dimensional accuracy.     

Effect of sintering temperature on the preparation of Cu–Ti3SiC2 metal matrix composite

Ti3SiC2 has the potential to replace graphite as reinforcing particles in Cu matrix composites for applications in brush,electrical contacts and electrode materials.In this paper the fabrication of Cu-Ti3SiC2 metal matrix composites prepared by warm compaction powder metallurgy forming and spark plasma sintering(SPS) was studied.The stability of Ti3SiC2 at different sintering temperatures was also studied.The present experimental results indicate that the reinforcing particles in Cu-Ti3SiC2 composites are not stable at and above 800℃.The decomposition of Ti3SiC2 will lead to the formation of TiC and/or other carbides and TiSi2.If purity is the major concern,the processing and servicing temperatures of the Cu-Ti3SiC2 composite should be limited to 750℃ or lower.The composites prepared by warm compaction forming and SPS sintering at 750℃ have lower density when compared with the composites prepared by SPS sintering at 950℃,but their electrical resistivity values are very close to each other and even lower.     

超重力反应沉淀法(HGRP)制备纳米BaTiO3的研究

以四氯化钛和氯化钡为钛源和钡源，以NaOH溶液为沉淀剂，首次在实验室采用直接沉淀法与超重力反应器相结合的超重力反应沉淀法 (HGRP)制备了纳米BaTiO₃粉体。产品经TEM、BET、XRD、AES-ICP及化学分析证明该法制备的钛酸钡粒度为30～70nm，晶型为立方相。粉体Ba/Ti摩尔比为 ( 1. 000± 0.005)，且纯度较高。     

Carbothermal synthesis of Si3N4 powders using a combustion synthesis precursor

Si₃N₄ powders were synthesized by a carbothermal reduction method using a SiO₂ + C combustion synthesis precursor derived from a mixed solution consisting of silicic acid (Si source), polyacrylamide (additive), nitric acid (oxidizer), urea (fuel), and glucose (C source). Scanning electron microscopy (SEM) micrographs showed that the obtained precursor exhibited a uniform mixture of SiO₂ + C composed of porous blocky particles up to ～20 μm. The precursor was subsequently calcined under nitrogen at 1200–1550°C for 2 h. X-ray diffraction (XRD) analysis revealed that the initial reduction reaction started at about 1300°C, and the complete transition of SiO₂ into Si₃N₄ was found at 1550°C. The Si₃N₄ powders, synthesized at 1550°C, exhibit a mixture phase of α- and β-Si₃N₄ and consist of mainly agglomerates of fine particles of 100–300 nm, needle-like crystals and whiskers with a diameter of about 100 nm and a length up to several micrometers, and a minor amount of irregular-shaped growths.     

BaAl2S4:Eu溅射靶材合成方法研究

采用放电等离子烧结(SPS)方法和粉末烧结法制备BaAl2S4:Eu溅射靶材,分析了靶材成分和结构特性以及利用靶材制备薄膜的发光特性.实验结果表明,SPS烧结的BaAl2S4:Eu溅射靶材的纯度高,无其它硫化物形成,被氧化的可能性小,靶材致密,气孔少;形成薄膜的PL谱主要是470nm处的蓝光发射.粉末烧结法制备的Ba-Al2S4:Eu溅射靶材的纯度低,靶材被氧化的几率大,气孔多,不致密,呈三维网状结构;在470nm处的蓝光发射峰值相对较弱.放电等离子烧结方法更适合制备BaAl2S4:Eu溅射靶材.     

Purity of SiC powders fabricated by coat-mix

Silicon carbide powders were synthesized by the coat-mix process, with phenolic resin and silicon powders as starting materials. The effects of synthetic conditions, including sintering temperature and the molar ratio of resin-derived carbon to silicon on the composition and the purity of the resultant powders were investigated. The results show that a higher sintering temperature and an appropriate molar ratio of resin-derived carbon to silicon are favorable for producing high purity silicon carbide powders. It is found that the silicon carbide content increases slightly with increasing the sintering temperature during the solid-solid reaction. The temperature gradient plays an important role on this trend. When the sintering temperature is raised up to 1500℃, the formation of silicon earbide is based on the liquid-solid reaction, and high purity (99.8wt%) silicon carbide powders can easily be obtained. It can also be found that the optimum molar ratio of resin-derived carbon to silicon is 1:1.     

Densification behavior of mechanically milled Cu–8 at% Cr alloy and its mechanical and electrical properties

Synthesis and consolidation behavior of Cu–8 at%Cr alloy powders made by mechanical alloying with elemental Cu and Cr powders,and subsequently,compressive and electrical properties of the consolidated alloys were studied.Solid solubility of Cr in Cu during milling,and subsequent phase transformations during sintering and heat treatment of sintered components were analyzed using X-ray diffraction,scanning electron microscopy and transmission electron microscopy.The milled powders were compacted applying three different pressures(200 MPa,400 MPa and 600 MPa)and sintered in H2atmosphere at 900 1C for 30 min and at 1000 1C for 1 h and 2 h.The maximum densification(92.8%)was achieved for the sample compacted at 600 MPa and sintered for 1000 1C for 2 h.Hardness and densification behavior further increased for the compacts sintered at 900 1C for 30 min after rolling and annealing process.TEM investigation of the sintered compacts revealed the bimodal distribution of Cu grains with nano-sized Cr and Cr2O3precipitation along the grain boundary as well as in grain interior.Pinning of grain boundaries by the precipitates stabilized the fine grain structure in bimodal distribution.     

Novel approaches to produce Al2O3– TiC/TiCN– Fecomposite powders directly from ilmenite

Al2O3 –TiC/TiCN–Fe composite powders were successfully prepared directly from ilmenite at 1300–1400℃.The effects of Al/C ratio,sintering atmosphere,and reaction temperature and time on the reaction products were investigated.Results showed that the nitrogen atmosphere was bene cial to the reduction of ilmenite and the formation of Al2O3 –TiC/TiCN–Fe composite powders.When the reaction temperature was between 600 and 1100℃,the intermediate products,TiO2,Ti3O5 and Ti4O7 were found,which changed to TiC or TiCN at higher temperature.Al/C ratio was found to affect the reaction process and synthesis products.When Al addition was 0.5 mol,the Al2O3 phase did not appear.The content of carbon in TiCN rose when the reaction temperature was increased.     

镁橄榄石合成反应动力学研究

以分析纯氧化镁、高纯熔融石英以及电熔镁砂颗粒为原料,研究了固相法合成镁橄榄石的反应动力学.利用X射线衍射和扫描电子显微镜等手段,研究了合成温度和保温时间对镁橄榄石生成速率的影响,分析了MgO与SiO2的反应机理.根据实验结果,建立了1100~1300℃下MgO与SiO2反应的动力学方程,并求出了表观反应活化能.研究结果表明,随着合成温度的提高和保温时间的延长,镁橄榄石生成率逐渐增加.在反应初期,MgO与SiO2反应生成了镁橄榄石和顽火辉石,在合成反应中后期时Mg2+通过产物层扩散而进一步反应,MgO与SiO2反应合成镁橄榄石的反应过程由Mg2+扩散所控制,反应的表观活化能为(220±20)kJ/mol.     

Effect of sintering temperature on phase evolution of Al_(86)Ni_6Y_(4.5)Co_2La_(1.5) bulk amorphous composites synthesized via mechanical alloying and spark plasma sintering

Al_(86)Ni_6Y_(4.5)Co_2La_(1.5) amorphous powders were synthesized by mechanical alloying for 200 h. Subsequent consolidation was performed via spark plasma sintering in the temperature range of 250 ℃ to 500 ℃ at the pressure of 500 MPa. The role of viscous flow on densification was investigated by studying the viscosity change of the amorphous phase at different consolidation temperatures. The decrease in viscosity at higher sintering temperatures resulted in better particle bonding and densification of consolidated samples. The formation of only FCC Al was observed in the consolidated samples at sintering temperatures ≤ 300 ℃ and the intermetallic phases formed at temperatures ≥ 400 ℃. The mechanical properties of the bulk samples were measured by Vickers microhardness and nanoindentation tests. The testing results showed that the average values of microhardness, nanohardness and elastic modulus of the sample consolidated at 500 ℃ were 3.06 ± 0.14 GPa,4.85 ± 1.14 GPa and 89.53 ± 9.25 GPa, respectively. The increase in hardness and elastic modulus of the higher temperature consolidated samples is attributed to the improvement in particle bonding, densification and distribution of various hard intermetallic phases in the amorphous matrix.     

脉冲电流烧结Al2O3颗粒的广义热弹性分析

脉冲电流烧结过程的颈部形成机理,特别是非导电粉末材料,是需要着重研究的核心问题。以非导电Al_2O_3粉末为研究对象,引入L-S(Lord and Shulman)型广义热弹性方程,初步探究烧结初期非导电粉末颈部局部高温形成以及快速烧结机理。利用Comsol Multiphysics模拟得到脉冲电流烧结过程中颗粒内部的温度场和应力场分布以及烧结颈部的化学势和空位浓度变化规律。数值结果表明,热以波的形式在烧结颈部产生叠加,形成局部高温。化学势变化表明:烧结初期表面扩散占主要作用,空位浓度差的突变使烧结颈部产生局部空位浓度梯度,促进烧结颈长过程,缩短烧结时间。     

Preparation of sol-gel derived microcrystalline corundum abrasives with hexagonal platelets

The effects of different additives on the mechanical properties, microstructures, and wear behavior of corundum abrasives were investigated. When the number of additive phases increases, the sintering temperature and wear rate decrease, while the densification and mechanical properties increase. The additive SiO₂ is responsible for the development of equiaxed grains, whereas both CaO and MgO promote the development of platelike grains. By controlling the molar ratio of additives, it is possible to obtain different microstructures. With SiO₂-MgO-CaO (molar ratio, 2:1:1) as the additives and nano α-Al₂O₃ powders as the seed, microcrystalline corundum abrasives with hexagonal platelets were obtained using sol-gel process by sintering at 1300℃ for 0.5 h. The average diameter and thickness of hexagonal platelets are 1.38 μm and 360 nm respectively, the single-particle compressive strength is 26.44 N, and the wear rate is (3.06±0.21)×10?7 mm3/(N·m).     

实验参数和Al质量分数对燃烧合成Ti3AlC2的影响

以Ti、Al和C粉为原料,采用XRD、SEM方法研究压坯压力、保护气氛以及不同Al质量分数对自蔓延燃烧合成Ti3AlC2的影响.结果表明,在150 MPa压力下的试样生成主晶相Ti3AlC2,且其质量分数明显高于过高和过低压力下的试样.其他实验条件相同时氩气保护更有利于主晶相Ti3AlC2的生成.Ti/C=1.5时,Ti3AlC2的衍射峰强度随着原料中Al质量分数的增加而加强.     

A bulk metal/ceramic composite material with a cellular structure

Metal/ceramic composite materials can be divided into two groups: one is ceramic reinforced metal matrix composite, and the other is metal toughened ceramic matrix composite. The research on these materials mainly focuses on the mechanical properties due …     

纳米α-Al2O3粉体的机械化学合成法制备及其表征

以分析纯的结晶氯化铝和碳酸氢铵为原料,可溶性淀粉为分散剂,采用机械化学合成法制备了纳米α-Al2O3粉体.经X射线衍射实验证明,产品为α相,Scherrer公式计算得粉体粒径为26.40 nm.用透射电子显微镜(TEM)测得粉体呈球形,粒径为30～40 nm.该法克服了单纯的固相法产品颗粒不均匀和形状难以控制,以及液相法颗粒易团聚的缺点,同时兼顾了二者工艺简单,生产成本低,产品质量稳定、纯度高等优点,适用于大型工业化生产.     

Isothermal oxidation behavior and mechanism of a nickel-based superalloy at 1000℃

The oxidation behavior of a nickel-based superalloy at 1000℃ in air was investigated through X-ray diffraction, scanning electron microscopy, and energy-dispersive spectroscopy analysis. A series of oxides, including external oxide scales (Cr₂O₃, (TiO₂ + MnCr₂O₄)) and internal oxides (Al₂O₃,TiN), were formed on the surface or sub-surface of the substrate at 1000℃ in experimental still air. The oxidation resistance of the alloy was dependent on the stability of the surface oxide layer. The continuity and density of the protective Cr₂O₃ scale were affected by minor alloying elements such as Ti and Mn. The outermost oxide scale was composed of TiO₂ rutile and MnCr₂O₄ spinel, and the growth of TiO₂ particles was controlled by the outer diffusion of Ti ions through the pre-existing oxide layer. Severe internal oxidation occurred beneath the external oxide scale, consuming Al and Ti of the strength phase γ' (Ni₃(Al,Ti)) and thereby severely deteriorating the surface mechanical properties. The depth of the internal oxidation region was approximately 35 μm after exposure to experimental air at 1000℃ for 80 h.     

Preparation of high emissivity NiCr<Subscript>2</Subscript>O<Subscript>4</Subscript> powders with a spinel structure by spray drying

Spray-drying was used to produce the high emissivity NiCr₂O₄ powders with a spinel structure. Preliminary investigations focused on fabricating the high emissivity powders for infrared radiation coatings and finding the relationship between microstructure and emissivity. The NiCr₂O₄ powders were characterized for composition, microstructure, and infrared emissivity by X-ray diffraction (XRD), scanning electron microscopy (SEM), infrared radiant instrument, and Fourier transform infrared spectra (FT-IR). Thermogravimetry and differential thermal analysis show that the appropriate baking temperature for NiCr₂O₄ powder preparation is about 1200°C. The emissivity measurement and FT-IR spectra show that, because of the special spinel structure, the NiCr₂O₄ powders have a high emissivity about 0.91. Spray-drying is a suitable method to produce the high emissivity ceramic powders.     

机械合金化改善反应合成Ti3SiC2的条件

为改善Ti3SiC2的合成条件，利用机械合金化的方法处理原料粉末，并与通常采用的原始粉末直接混合粉末进行比较分析。结果表明，机械合金化有助于合成Ti3SiC2。根据DTA曲线确定合理的烧结工艺，对合成产物进行的XRD、断口的SEM以及EDAX分析，进一步证实了机械合金化粉末可以在较低的温度下(温度降低25℃)、较短的时间(时间缩短20％)内通过反应合成得到Ti3SiC2。     

Chemical quenching and inhibition of positronium in Cr<Subscript>2</Subscript>O<Subscript>3</Subscript>/Al<Subscript>2</Subscript>O<Subscript>3</Subscript> catalysts

The pore structure of Cr2O3/Al2O3 catalysts and the surface chemical properties of these pores were characterized by positron lifetime and coincidence Doppler broadening (CDB) measurements. Four lifetime components could be resolved from the positron lifetime spectrum, with two long lifetime components and two short lifetime components. The two long lifetimes τ4 and τ3 are attributed to ortho-positronium (o-Ps) annihilation in large pores and microvoids, respectively. With increasing Cr2O3 content, both τ4 and its intensity I4 show sharp decrease, while τ3 and its intensity I3 keep nearly unchanged. The Doppler broadening S parameters also show sharp decrease with increasing Cr2O3 content. Detailed analysis of the CDB spectrum reveals that the parapositronium (p-Ps) intensity also decreases with increasing Cr2O3 content. This indicates that the change of o-Ps lifetime τ4 is due to the chemical quenching by Cr2O3 but not spin-conversion of positronium. The decrease of o-Ps intensity I4 indicates that Cr2O3 also inhibits positronium formation.