掺杂氧化铝对纳米钨粉烧结过程的影响

以碳热预还原和氢气深还原两步制备的纳米钨粉作为烧结原料,即先通过碳黑还原脱除三氧化钨中的大部分氧,再以氢还原脱除残留的氧。该方法制备的钨粉颗粒呈球形形貌,平均晶粒度可达90 nm。同时,向钨粉中掺杂质量分数为1%和2%的氧化铝,探究了氧化铝对钨粉烧结行为的影响。通过烧结样品的断口形貌和晶粒的平均尺寸分析发现,氧化铝对烧结后期的晶粒长大有明显的抑制作用,相同的烧结温度下晶粒的尺寸随着氧化铝含量的上升而减小。在1600 ℃时,纯钨粉烧结坯的晶粒平均尺寸为2.75 μm,但添加质量分数为1%和2%氧化铝的烧结样品晶粒平均尺寸约为1.5 μm,这是由于氧化铝能有效地抑制烧结后期的钨粉晶粒长大。纯钨粉和掺杂氧化铝钨粉的烧结坯的硬度随温度升高具有不同的趋势。掺杂钨粉烧结坯的硬度随着温度的升高而升高,且其最大值高于800 HV。但是,纯钨粉烧结坯的硬度随烧结温度增加而先增加后降低,在1400 ℃时取得最大值（473.6 HV）,这是由纯钨粉烧结坯的晶粒在高温下急剧长大所导致。在烧结温度为1600 ℃时,纯钨粉、掺杂质量分数1%和2%的氧化铝掺杂的钨粉的烧结坯的相对密度依次为98.52%、95.43%和93.5%。      

纯钼烧结规律研究

系统研究了在1 000～1 900℃温度范围采用H2气氛中频感应加热烧结纯钼坯过程中不同温度阶段O含量、微观形貌、孔隙、密度、抗弯强度的变化规律。结果表明:随烧结温度提高钼坯O含量逐渐降低,最终降至30mg/kg左右。钼坯密度随温度升高呈增大趋势,致密化的本质是微观形态烧结变化的结果。致密进程可分为4个阶段,各阶段微观晶粒及孔隙作用机制不一致。抗弯强度与致密进程紧密联系但两者随温度变化趋势有所不同。     

粉末形状与松装密度对不锈钢烧结多孔材料制备工艺及其性能的影响

通过选用气雾化及水雾化两种工艺方法制备的不锈钢粉末来制取粉末烧结多孔材料。探讨了粉末形状及松装密度对不锈钢粉末烧结多孔材料制造工艺中的成形压力和烧结温度等工艺参数的影响;研究了原料粉末松装密度对不锈钢粉末烧结多孔材料的透气性、拉伸强度的影响。结果表明:成形压力、烧结温度和制品的透气性受粉末松装密度影响显著。粒度范围为0.18～0.90mm时,气雾化粉末的成形压力比水雾化粉末要高近1倍;当粉末的粒度相同时,采用松装密度大的球形粉末所需的烧结温度比松装密度小的不规则粉末的高60～70℃;粒度为0.45～0.60mm时,选用松装密度为4.13 g/cm3粉末所制备的多孔制品的透气性为3.16×10-10m2,而选用松装密度为2.67 g/cm3的粉末所制备的多孔制品的透气性仅为8.8×10-11m2。不锈钢多孔材料的强度受原料粉末的松装密度影响显著;粒度相同,制备工艺相同时,采用较低松装密度的粉末的制品,能够得到较高的强度。     

THE PREPARATION AND SOME PROPERTIES OF CHROMIC OXIDE-CHROMIUM CERMETS.

Abstract

Compacts of chromium oxide/chromium mixtures have been sintered in vacuum at temperatures up to 1600°C to produce cermets. Two types of chromium powder were used—an electrolytic and an aluminothermic powder. The effect of chromium content and of sintering temperature on the sintered density and microstructure has been studied and supplemented by tests of hardness and compressive strength.

Considerable densification was achieved by additions of chromium in the range 1–50 wt.-%, with the optimum content at 5–10%. Compressive strengths < 10 tons/in² were attained over a wide range of composition.     

Microstructure,mechanical properties and tribological behaviour of PM Fe-Cu-Zn alloys containing solid lubricants

Abstract

Fe-Cu-Zn alloys containing solid lubricants of graphite and talc produced via cold pressing and sintering technology are investigated. The influence of composition and sintering temperature on open porosity, density, strength and hardness of these alloys is studied. The microstructure is correlated with the mechanical properties of the sintered materials. The tensile tests showed that the peak strength was observed for samples sintered at ≤1000°C. Above this temperature the bending and tensile strength values decrease. Microstructural analysis of sintered materials revealed three phases in the structure: α-Fe, α-brass and talc. Results indicate that the microstructure of sintered samples is sensitive to process variables such as brass and talc contents and sintering temperature.     

Consolidation of aerospace grade aluminum 7055 powder through SPS-forge processing

The objective of this research was to assess the SPS-forge response of fully pre-alloyed aerospace grade 7055 (Al–8Zn–2.1Mg–2.3Cu–0.2Zr) powder. The core variables investigated were the sintering temperature, time, and atmosphere employed, as well as the average particle size and the manner of uni-axial loading. Samples sintered in vacuum at 500°C for 40?min with delayed loading offered the most desirable combination of density, hardness, and bend properties but remained relatively brittle. Hot forging of the sintered preforms was found to impart sizable gains in mechanical properties. The SPS-forge product exhibited tensile yield strength of 603?MPa coupled with a ductility of 9.1% and a hardness of 93 HRB. All such properties were largely equivalent to those measured for the wrought counterpart.     

Structural changes accompanying the sintering of ultrafine aluminum nitride powders

Conclusions An electron-microscopical investigation has established that the sintering of compacts from an ultrafine plasma-chemical AlN powder is determined by the following processes: coagulation, with the formation of strong polycrystalline aggregates (1000–1400°C); coalescence, made possible by a geometric grain boundary match inside the aggregates, and formation of high-angle boundaries between aggregates (1200–1600°C); and collective recrystallization (above 1600°C). In an x-ray diffraction study annealing at temperatures above 1700°C was found to decrease the parameter c of AlN by 0.002 Å as a result of dissolution of oxygen in the lattice without affecting its parametera. The results of both electron-microscopical and x-ray diffraction studies show that annealing at temperatures above 1600°C increases the defectiveness of the wurtzite structure of AlN, brings about twinning and the formation of polytypal interlayers in recrystallized grains, and raises the concentration of other defects causing a broadening of lines in x-ray diffraction photographs. As a result of these phenomena the material experiences a strengthening at sintering temperatures of 1700–1800°C.Translated from Poroshkovaya Metallurgiya, No. 10(226), pp. 35–40, October, 1981.The authors wish to thank A. N. Pilyankevich for helpful discussion.     

烧结温度对碳化硅陶瓷力学性能的影响

采用硼、碳助剂无压烧结制备碳化硅陶瓷。针对烧结温度与碳化硅烧结体密度、抗弯强度以及硬度之间的关系进行了试验研究,并对不同温度下制备的烧结体进行了显微结构形貌观察和XRD图谱分析。结果表明,烧结温度在2190～2220℃范围内可以制备密度高、力学性能好的碳化硅陶瓷。其相对密度超过96%;抗弯强度接近400MPa;维氏硬度23GPa以上。在试验温度范围内,密度与抗弯强度之间的关系近似为线性关系,密度越高抗弯强度和硬度性能越好。     

Synthesis and characterisation of Al2O3/Ni-type composites obtained by spark plasma sintering

This paper presents the influence of sintering on the structure, morphology and compressing strength of alumina/nickel composite compacts obtained by spark plasma sintering (SPS). Al₂O₃/Ni composites were prepared by SPS in argon atmosphere at temperatures in the range of 1000–1200 –C with a holding time of 2, 5 and 10?minutes. The heating rate was 200 C?min^?1. These composites have been characterised by X-ray diffraction, SEM and EDX. The relative density and compressive strength of the as-obtained compacts were determined. The results showed that the alumina particles are uniformly dispersed in a quasi-continuous Ni network, and there was no sign of phase changes during sintering. The maximum strength of the alumina/nickel composite with a content of 75 vol. ? Al₂O₃ and 25 vol. ? Ni was about 240?MPa for the samples sintered at 1200?C for 10?minutes.

Special block from the conference RoPM2017 guest edited by Ionel Chicinas, Technical University, Cluj-Napoca.     

The Effects of Sample Position and Gas Flow Pattern on the Sintering of a 7xxx Aluminum Alloy

The effects of sample position and gas flow pattern on the sintering of a 7xxx aluminum alloy Al-7Zn-2.5Mg-1Cu in flowing nitrogen have been investigated both experimentally and numerically. The near-surface pore distribution and sintered density of the samples show a strong dependency on the sample separation distance over the range from 2?mm to 40?mm. The open porosity in each sample increases with increasing separation distance while the closed porosity remains essentially unchanged. A two-dimensional computational fluid dynamics (CFD) model has been developed to analyze the gas flow behavior near the sample surfaces during isothermal sintering. The streamlines, velocity profile, and volume flow rate in the cavity between each two samples are presented as a function of the sample separation distance at a fixed nitrogen flow rate of 6?L/min. The CFD modeling results provide essential details for understanding the near-surface pore distribution and density of the sintered samples. It is proposed that the different gas flow patterns near the sample surfaces result in variations of the oxygen content from the incoming nitrogen flow in the local sintering atmosphere, which affects the self-gettering process of the aluminum compacts during sintering. This leads to the development of different near-surface pore distributions and sintered densities.     

微波烧结对粉末冶金铁基材料性能的影响

采用微波烧结新技术研究了粉末冶金铁基材料的烧结工艺与性能，并同常规真空烧结工艺进行了比较。结果表明：微波烧结粉末冶金铁基材料在1280℃的烧结温度下保温10min时，可达到95．8％的相对密度；烧结温度降低。烧结时间大幅度缩短，且微波烧结制品的孔隙明显减小或消失，硬度、抗弯强度、抗拉强度均有较大幅度提高。     

Fabrication,microstructures and properties of 50 vol.-% SiCp/6061Al composites via a pressureless sintering technique

Commercial F500 SiC powder and 6061 Al powder were chosen to fabricate the 50?vol.-% SiCp/6061Al composites via pressureless sintering. Effects of pre-treatment of the SiC powder and sintering temperature on the microstructures and properties of the composites were studied. Densification mechanism and interfacial reaction of the composites were also investigated. The results show that the composites have a high sintering ability and a low interfacial reaction activity. The density, bending strength and thermal conductivity of the composites are all sensitive to the sintering temperature. The composites sintered at 680°C are nearly fully dense and have the following optimal properties: the relative density of 98.5%, the bending strength of 495?MPa, the TC of 153?W/(m?K) and the coefficient of thermal expansion of 8.1?×?10^?6/°C (50–100°C), which are superior to most of the SiCp/Al composites of the similar composition reported previously.     

Fracture Behavior of W-Ni-Fe Heavy Alloys

Heavy alloys were liquid phase sintered from compacts of mixed W, Ni, and Fe powders. The alloy compositions ranged from 93 to 97 wt pct W, with the Ni:Fe ratio maintained at 7:3. Sintering was performed under hydrogen in the 1465 to 1485 °C temperature range, giving full density within the first 15 minutes. The room temperature strength and ductility showed major degradation with sintering times in excess of two hours. Tensile tests and bend tests have been performed to isolate the fracture mode and the property determining features. Initial cracking occurs at the tungsten-tungsten grain boundaries and in the tungsten grains. These latter cracks propagate through the structure to give eventual failure. The ductility to failure is shown to be governed by the strength of the tungsten-matrix interface. The maximum elongation depends on the contiguity, which in turn is set by the alloy composition. Formerly a Postdoctoral Fellow at RPI under a fellowship from the Korea Science and Engineering Foundation     

The properties of tungsten processed by chemically activated sintering

Two tungsten powders have been treated with small concentrations of sintering activators to provide for enhanced low temperature sintering. The experimental study focused on the determination of the processing effects on properties such as sintered density, grain size, hardness, and strength. Variables in the plan included tungsten particle size, type of activator, amount of activator, compaction pressure, and sintering temperature. The sintered density is found to have a dominant effect on strength and hardness. The various processing variables are analyzed in terms of their effects on density. At high sintered densities, grain growth acts to degrade the strength. Additionally, the nature of the sintering activator influences the fracture strength. In this study optimal strength occurred with a 0.7 μm tungsten powder treated with 0.29 wt pct Ni, sintered at 1200 °C for one hour. The resulting density was 18.21 g/cm³, with aR _A hardness of 69 and a transverse rupture strength of 460 MPa.     

Kinetics of Densification and Grain Growth of Pure Tungsten During Spark Plasma Sintering

The kinetics of densification and grain growth of tungsten during spark plasma sintering (SPS) was studied under isothermal conditions. The results show that using SPS, high-density (>97?pct) pure tungsten can be produced without the addition of sintering aids. The estimated sintering exponent (m?=?0.4 ± 0.03) suggests that the rate-controlling mechanism of sintering is diffusion along the grain contacts into the interparticles neck region. The activation energy of tungsten self-diffusion was calculated (Q?=?277?±?15?kJ/mol) in the temperature range 1523?K to 1773?K (1250?°C to 1500?°C). The activation energy is smaller than the values in previous studies using conventional sintering. This suggests that there may be some differences in the sintering conditions and mechanisms during SPS processing compared to conventional sintering. Grain-growth kinetics was studied in the range 1873?K to 2073?K (1600?°C to 1800?°C) and classified as normal grain growth according to the estimated grain-growth exponent (m?=?2?±?0.2). The grain-growth activation energy was calculated as 231?±?15?kJ/mol.     

W-Ni-Cu-Sn系高比重合金的研究

本文研究了烧结温度、保温时间以及添加锡对W-Ni-Cu合金性能的影响。结果表明,不添加锡的93W-Ni-Cu合金与添加1%Sn的85W-Ni-Cu-Sn合金相比,其烧结温度由1320℃降至1140℃,即烧结温度降低约200℃;抗拉强度从686N/mm2提高到980N/mm2;热膨胀系数提高了28%。获得了较好的综合性能。     

粉末冶金旋压无缝钨管的组织性能及使用情况

用粉末冶金法制坯,以旋压法加工无缝钨管为试样,测定了加工过程中硬度、密度和组织变化,测定了钨管的再结晶温度,并描述了钨管的实际使用情况。不同变形率下钨管的组织是:11%变形率时还有未变形的组织;66%变形率时能看到细长的烧结孔洞;77%变形率时晶粒已破碎,烧结孔洞全部消失。用于钨铼热电偶标定炉的高精度无缝薄壁钨管结果是:φ40×0.25×540mm者,在中心位置100mm范围内,1200℃、1400℃和1600℃的轴向温差分别为±1℃、±6℃和±7℃;φ30×0.25×286mm者,等温区允许误差在1377±12℃,该区长度为120mm。     

Synthesis and Characterization of Ti/(TiB + TiC) Hybrid in-situ Composites by Spark Plasma Sintering

Since Ti alloys exhibit inferior wear resistance and suffer considerable loss in mechanical strength at high temperature, it is aimed at synthesis an in-situ Ti/(TiB + TiC) hybrid composite. In order to synthesis Ti/(TiB + TiC) in-situ composite, B₄C particulate was mixed with titanium powder and sintered at 1400 °C at different time intervals by spark plasma sintering. Sintering parameters were optimized according to the complete in-situ reactions. Density of the sintered compacts was measured by Archimedes principle. Energy dispersive spectroscope and optical microscope observations of the sintered samples revealed that with increasing sintering time TiB and TiC particulates were gradually transforming into needle like structure and near equiaxed structure, respectively.     

The oxygen permeability of stabilized zirconia electrolytes at high temperatures

Abstract

The use of oxygen or air as a reference electrode in an electrochemical cell incorporating the solid-oxide electrolyte ZrO₂–YO_1.5 and a gaseous electrode of controlled oxygen pressure has been investigated between 1000°–1600°C. In the upper temperature range, 1400°-1600°C, and lower oxygen partial pressure range, the EMF's were observed to be between 25 and 300 mv lower than theoretical values. These low values have resulted mainly from the oxygen permeability of the electrolyte tube. A study of oxygen permeability through commercial electrolyte tubes shows that the transport mechanism for permeation appears to involve the migration of either neutral oxygen atoms or oxygen ions and positive holes. This phenomenon is inherent in the electrolyte material which was impervious to Ar, N₂, CO and CO₂ over the whole temperature range.

To minimize the effect of oxygen permeation, a reference electrode of low oxygen partial pressure, such as a solid metal/metal oxide reference electrode Mo-MoO₂, was more suitable for use under the present conditions. As a part of the study, the standard molar free energy of formation of MoO₂ was determined electrochemically between 1000°–1600°C using the CO-CO₂ gaseous electrode.

Résumé

Les auteurs ont étudié le comportement d'une cellule électrochimique comprenant l'électrolyte solide ZrO₂-YO_1.5, une électrode à référence d'air ou d'oxygène et une électrode d'oxygène à pression contrôlable, entre 1000 et 1600°C. Entre 1400 et 1600°C et aux basses pressions d'oxygene les valeurs de la F.E.M. étaient inférieures de 25 à 300 mV aux valeurs théoriques. Ces basses valeurs seraient dues à la perméabilite du tube d'electrolyte à l'oxygène, le mécanisme de transport étant la migration d'atomes neutres d'oxygène, d'ions oxygène et de trous positifs. Ce phénomène est une caractéristique du matériau électrolytique; celui-ci est toutefois imperméable à Ar, N₂, CO et CO₂ dans toute la gamme des températures.

Pour minimiser les effets de cette perméabilité, il est indiqué d'utiliser, dans les présentes conditions, une électrode de référence à basse pression de O₂, telle que celle fixée par l'équilibre hétérogène Mo-MoO₂-O₂. L'enthalpie libre de formation du MoO₂ entre 1000 et 1600°C a été déterminée par voie électrochimique en utilisant une pression de O₂ fixée par l'équilibre homogène CO-CO₂-O₂.     

放电等离子烧结制备无粘结相SiCw/WC硬质合金

以碳化硅晶须(SiC whiskers,SiC_w)作为增韧相,通过放电等离子烧结制备了无粘结相SiC_w/WC硬质合金。考察了放电等离子烧结温度及SiC_w添加量对SiC_w/WC硬质合金组织性能的影响。结果表明,采用放电等离子烧结在1800℃下可获得相对密度高于99%的WC烧结体,其维氏硬度和断裂韧性分别达到25.99 GPa和4.99 MPa·m^1/2。添加适量的SiC_w可以改善SiC_w/WC烧结性能和断裂韧性,在SiC_w的质量分数为0.6%时,断裂韧性达到6.80 MPa·m^1/2,当添加过量的SiC_w时,增韧效果减弱。