Spark plasma sintering versus hot pressing – densification,bending strength,microstructure, and tribological properties of Ti5Al2.5Fe alloys

Ti5Al2.5Fe alloys were fabricated by the spark plasma sintering (SPS) and hot pressing (HP) pressure-assisted sintering techniques from pre-alloyed powders with a particle size of about 200?μm. The powders were sintered at 850 °C for two different holding times (5 and 8 min) and heating rates (50 and 150°C?min^?1) at 25?MPa. The maximum relative densities were 99.70 and 98.78% for SPS and HP samples, respectively. All the alloys prepared by the SPS process had significantly higher bending strengths (1825–2074?MPa) than the alloys prepared by the HP process (648–1330?MPa). A decrease in the heating rate from 150 to 50°C min^?1 enhanced the wear resistance of the Ti5Al2.5Fe alloys prepared by both the SPS and HP processes.     

放电等离子烧结制备超细晶WC-3Co硬质合金的组织和性能

采用高能球磨制备纳米WC-3Co粉末,再通过放电等离子烧结(spark plasma sintering,SPS)制备超细晶WC-3Co硬质合金。研究SPS工艺参数对合金致密度、显微组织和力学性能的影响,并对SPS和热压工艺(hotpressing,HP)进行对比。结果表明:SPS可实现WC-3Co粉末的低温快速致密化。升高温度或提高压力都使得合金的致密度提高,同时导致WC晶粒长大。SPS较HP升温速率快且烧结时间更短,合金组织更加均匀,在1 300℃保温5 min、烧结压力为40 MPa的条件下所制备的合金具有最佳综合性能,其平均晶粒度为0.32μm,相对密度、硬度、抗弯强度、断裂韧性分别为99.3%、2257 HV30、1 906 MPa、10.36 MPa.m1/2。而在1 450℃、压力为50 MPa、保压5 min条件下,热压合金的致密度、硬度和断裂韧性分别为99.6%、2 264 HV30和11.01 MPa.m1/2,但抗弯强度只有1 301 MPa,平均晶粒度为0.47μm。     

Effect of process parameters on the microstructure and mechanical properties of vacuum hot-press sintered Co-50 mass% Cr alloys

In the present research, two different compositions of submicron-structured cobalt (800?±?45?nm) and chromium (700?±?50?nm) powders are mixed to fabricate Co-50 mass% Cr alloys by the vacuum hot-press sintering technique. This study imposes various hot-press sintering temperatures (1150, 1200, 1250 and 1300°C) and pressures (20, 30, 40 and 50?MPa) while maintaining the sintering time at 1?h, respectively. The experimental results show that the optimum parameters of hot-press sintered Co-50 mass% Cr alloys are 1200°C at 50?MPa for 1?h. Meanwhile, the sintered density reaches 7.73?g?cm^?3, the closed porosity decreases to 0.31%, and the hardness and transverse rupture strength values increase to 80.6?±?0.3 HRA and 1052.9?±?17.5?MPa, respectively. Grain growth is not obviously generated after 1200°C hot-press sintering at 50?MPa for 1?h. Consequently, the optimal solid-phase sintering process effectively improved hot-press sintered Co-50 mass% Cr alloys, which resulted in the good properties.     

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.     

The Effect of Cooling Rate on the Strength of Sintered Fe—Cu Compacts

Abstract

The effect of cooling rate from the sintering temperature upon the tensile strength of compacts from a mixture of iron and copper powder was investigated. The compacts were pressed at 450 and 390 MPa and sintered in hydrogen at 1120°C for 40 min. The copper content of the compacts varied from 0 to 12%. For alloys with Cu content >4% the tensile strength was found to be strongly dependent upon the cooling rate in the temperature range between 850 and 600°C, with rapidly cooled specimens being considerably stronger. In specimens with 8%Cu the tensile strength increased from 206 to 343 MPa when the cooling rate was increased from 10 to 200 degC min^?1. In specimens with 2%Cu cooling rates above and below 600 degC min^?1 appear to influence the tensile strength. Possible explanations for the observed effects of cooling rate upon tensile strength in sintered Fe–Cu alloys are discussed.     

The effect of nitrogen flow rate on Acrawax C decomposition and its removal during sintering of Alumix 431D grade powder

Alumix 431D pre-alloyed powder (ECKA Granules GmbH) containing 1.5 mass% of Acrawax C was used to study the effect of nitrogen flow rate on delubrication and sintering evolution. Mass loss of compacts during heating was controlled by the TG method using a STA Netzsch apparatus coupled with a mass spectrometer. The latter was used to identify the volatile lubricant’s decomposition products. Macro- and microstructural observations of sintered compacts were also performed. The results documented a strong influence of nitrogen flow rate on delubrication and thus on the sintering behaviour of examined powder. High nitrogen flow rate is required to produce the desired sintered compacts. In contrast, at low nitrogen velocity, the lubricant removal is not complete, which leads to the formation of carbonaceous residuals in the form of soot, which in turn significantly impedes densification and deteriorates the sintered products.     

Sintering Characteristics of Al–Pb/Fly-Ash Metal Matrix Composites

Aluminum–lead/10 wt% fly-ash powder mixtures containing 0–20 wt% lead (Pb) were prepared. These powder mixes were compacted in the pressure range of 200–400 MPa by single action die compaction process. The prepared compacts were sintered in the temperature range of 500, 530, 560 and 590 °C in an argon gas atmosphere for duration of 45 min. For the sintered compacts, the sintered density, hardness and compressive strength were reported. Sintered density, hardness and compressive strength increased with the increase in compaction pressure. Sintered density increased whereas the hardness and the compressive strength decreased with the addition of Pb.     

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.     

Recyclability assessment of Al 7075 chips produced by cold comminution and consolidation using spark plasma sintering

A solid-state recycling route for processing aluminium alloy 7075 chips is proposed. This process involves pulverizing the chips using an industrial scale comminution line to produce a broad particle size distribution of granulated products and powders. Upon sieving, the ?140 mesh fraction of the pulverised material was consolidated by spark plasma sintering into fully dense compacts, i.e. >99%. The properties of the pulverised powders and compacts were compared to commercially available aluminium alloy 7075 powder used in industrial press-sinter applications. The comminution line produced powder particles which possessed a 7·9?±?0·6-nm thick native oxide layer with adhering exogenous contaminants, and aluminium oxide particles dispersed throughout the powder. The presence of the oxide layer and exogenous contaminants was found to be deleterious to the powder consolidation and mechanical properties. A flexural strength and strain and hardness of 94·7?±?7·2?MPa, 2·1?±?0·3% and 69·3?±?5·2 HV were obtained, respectively.     

Investigation of the strengthening mechanism and corrosion behaviours of Vanadis 4 extra tool steel adding ZrC−TiC powders through vacuum sintering,and sub-zero and heat treatments

ABSTRACT

In the present research, different ratios of zirconium carbide (ZrC) and titanium carbide (TiC) powders were added to Vanadis 4 Extra (V4 Extra) steel powders. The composite powders (V4 Extra?ZrC?TiC) utilised vacuum sintering at 1275, 1300, 1325 and 1350°C for 1?h, respectively. The experimental results showed that good mechanical properties were obtained by the addition of 1.8 mass% ZrC and 1.2 mass% TiC (Z1.8T1.2) sintered at 1350°C for 1?h. Meanwhile, the apparent porosity was decreased to 0.02 vol.-%, and the transverse rupture strength (TRS) and hardness reached 1872?±?24?MPa and 82.5 HRA, respectively. When optimally sintered V4 Extra composites (Z1.8T1.2) underwent a series of heat treatments, the TRS value was obviously enhanced to 2007?±?17?MPa after quenching, and sub-zero and tempering heat treatments. Moreover, the sub-zero and heat treatments improved the distribution of MC carbides, which effectively enhanced the strength of sintered V4 Extra composites.     

Spark plasma sintering of cryomilled copper powder

Abstract

The densification and sintering behaviour of a cryomilled copper powder (grain size of 17±2 nm and dislocation density of 6·26±0·04×10¹⁶ m^?2) were investigated and compared to those of an atomised copper powder with the same mean particle size in order to highlight the effect of the nanostructure on spark plasma sintering (SPS). Oxygen and nitrogen contamination of the cryomilled powder gives rise to extensive degassing during SPS up to 400°C. The cryomilled powder is more resistant to plastic deformation than the atomised one, but the huge density of dislocations and grain boundary activates sintering at low temperature. Densification is therefore promoted by deformation in the atomised powder and by sintering shrinkage in the cryomilled one. As a consequence, in the SPS conditions investigated, the atomised specimen is densified but not sintered, while the cryomilled one is effectively sintered and consequently densified.     

IRON-COPPER-TIN SINTERED COMPACTS

Abstract

A wide range of copper and tin powder additions to iron powder sintered compacts hasbeen studied. From mechanical-property tests it has been shown that when using sinteririg temperatures of 900–1100°C in nitrogen/10% hydrogen atmospheres there is an optimum copper: tin ratio of 15:2. The mechanical properties obtained from compacts pressed from iron mixed with 4% copper+tin in this ratio and sintered at 900°C were similar to those obtained from iron ?l0% copper powder compacts sintered at 1100°C. Moreover, the iron-copper-tin components showed improved dimensional accuracy.

In a further series of experiments, it was shown that tin additions to iron-copper alloy compacts increased the solubility of iron in the liquid phase at the sintering temperature and simultaneously decreased the rate of diffusion of copper into the iron particles. At the same time, tin improved the wettability of the liquid, reducing its surface tension and allowing it to disperse more completely throughout the matrix. The mechanical properties of compacts containing larger amounts of tin were decreased by the presence of brittle compounds, although the sintering rate was increased. It is concluded that the optimum properties of iron-copper-tin compacts are obtained by making correct additions of copper and tin to the iron powder and giving careful consideration to the sintering atmosphere.     

Compaction and Sintering Behavior of Niobium Powder for Making Consumable Electrodes

Niobium consumable electrodes of 10?mm dia?×?50?mm length were prepared by cold isostaic pressing with compaction pressure of 125?C250?MPa. The compacts were sintered under vacuum at different temperatures in the range of 1000?C1800?oC. The CIPed and sintered electrodes were characterized with respect to chemical analysis, density, microstructure and bend strength. The results showed that there is a marginal improvement in density at a sintering temperature in the range of 1000?C1400?oC, while a significant improvement in density was observed at sintering temperature in the range of 1600?C1800?oC. The bend strength of sintered electrode was found to increase with increasing sintering temperature and that attains a highest value at a sintering temperature in the range of 1600?C1800?oC. Sintering at a temperature higher than 1400?oC leads to decrease in oxygen content of the electrodes. The oxygen content was decreased from 2000 to 500?ppm when electrode was sintered at 1800?oC.     

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.     

PM processing of elemental and prealloyed 6061 aluminium alloy with and without common lubricants and sintering aids

Abstract

A comparison has been made between compaction, sintering, microstructural and mechanical properties of the 6061 aluminium alloy prepared via premixed elemental (EL) and prealloyed (PA) powders (as received and degassed) with and without additions of sintering aids and various solid and/or liquid lubricants. Both EL and PA powders were cold pressed at different pressures, ranging from 250 to 770 MPa, and sintered under vacuum in the range 580–640^°C for 30–120 min. and then under pure nitrogen atmosphere for comparison. Vacuum degassing of the PA powder provided better compressibility and thus higher green densities than those for the as received PA or the premixed EL powder compacts pressed at compaction pressures ≥340 MPa. Near full sintered densities of , ～98%TD were obtained for both EL and PA 6061 Al alloys. Degassed PA Al with 0·6 wt-% paraffin wax (PW) or with only 0·12 wt-%Pb addition as sintering aid and no lubricant, and premixed EL with only 0·12 wt-%Pb addition and no lubricant gave the best optimum properties. It became apparent that additions of some solid lubricants such as lithium stearate (LS) and acrawax to both the premixed EL and PA powders provided reasonable green densities, but had deleterious effect on sintered densities and microstructures, particularly under vacuum sintering. Heating data curves during the sintering cycle, revealed formation of both transient and persistent liquid phases for the EL and mainly supersolidus liquid phase sintering (SLPS) mechanism for the PA. Tensile properties of the degassed, vacuum or nitrogen sintered PA Al alloy in T6 condition were higher than those of the equivalent alloy prepared by EL mixing with the former giving a tensile strength of 330 MPa and 6–8% elongation to failure, which are similar to those of the commercial (wrought) 6061 Al alloys.     

Optimising grey iron powder compacts

Abstract

The grey iron microstructure Fe–2C–2Si powder based compact is tailored by different kinds of in situ and post sintering processing. This has been achieved by combining thermodynamic and kinetics modelling of microstructure development with sintering and controlled heat treatment experiments of tensile test specimens die compacted at 600 MPa. Applying optimised sintering conditions led to a grey iron like microstructure with 95% relative sintered density. Sinter hardening the compacts led to 500 MPa in yield strength and 600 MPa in ultimate tensile strength in combination with ductile fracture. Quenched and tempered condition showed the same strength values, but combined with brittle fracture due to martensitic structure. Pore rounding and partial pore filling by graphite were obtained by austenising isothermal hold during the cooling of the sintering cycle.     

Effect of compacting pressure on microstructure and mechanical properties of carbide cutting tools

Abstract

The effects of compaction pressure on properties of carbide cutting tools containing 80·5 wt-%WC, 5 wt-%TiC, 5 wt-%TaC–NbC and 9·5 wt-%Co were studied. These tools were formed by powder metallurgy with different compacting pressures ranging from 77 to 231 MPa (5–15 tons in^?2) and sintered in a vacuum furnace at a constant sintering temperature (1450°C) and at a constant heating and cooling rate of 5°C min^?1. Green and bulk densities, shrinkage and hardness of the produced compacts were measured. Tool cutting performance has been assessed based on machining a medium alloyed steel workpiece under different cutting conditions and measuring the tool flank wear and the workpiece surface roughness. The microstructure of the compacts was metallographically examined using scanning electron microscopy. The results have revealed that both densities and hardness figures increase with increasing compaction pressures, while shrinkage decreases. Cutting performance has not demonstrated a substantial improvement of the tool's performance and life due to the increasing compacting pressure of these tools.     

Spark plasma sintering of Al-Si-Cu-Fe quasi-crystalline powder

This article presents the results of a study on the microstructure and mechanical properties of Al-Si-Cu-Fe specimens produced by the spark plasma sintering (SPS) technique. The microstructure of the starting powder and bulk specimens was analyzed by means of X-ray diffraction (XRD), scanning electron microscopy (SEM), and transmission electron microscopy (TEM). The formation of the icosahedral and decagonal quasi-crystalline phases in the as-gas-atomized powders is described for the first time. It is then shown that these metastable phases transformed into the 1/1 cubic-approximant phase upon heating at about 600 °C. Second, the effects of SPS process parameters such as the temperature and time have been investigated. Owing to the generation of a spark discharge between neighboring powder particles, dense cylindrical samples were obtained after a short sintering time of 30 minutes at the temperature of 650 °C. The highest values of the Vickers microhardness, about 8.9 GPa, were obtained when the powders were sintered in the temperature range of 600 °C to 650 °C for a holding time of 30 minutes, while the fracture toughness was found to be inversely proportional to the sintering temperature. However, at the sintering temperature of 650 °C, the fracture toughness increased from about 1.40 to 1.52 MPa √m as the holding time increased from 10 to 60 minutes. As compared to cast specimens, the enhanced mechanical properties are explained by the refined microstructure resulting from the low temperature and short sintering time applied during SPS processing.     

Spark plasma sintering of Al-Si-Cu-Fe quasi-crystalline powder

This article presents the results of a study on the microstructure and mechanical properties of Al−Si−Cu−Fe specimens produced by the spark plasma sintering (SPS) technique. The microstructure of the starting powder and bulk specimens was analyzed by means of X-ray diffraction (XRD), scanning electron microscopy (SEM), and transmission electron microscopy (TEM). The formation of the icosahedral and decagonal quasi-crystalline phases in the as-gas-atomized powders is described for the first time. It is then shown that these metastable phases transformed into the 1/1 cubicapproximant phase upon heating at about 600°C. Second, the effects of SPS process parameters such as the temperature and time have been investigated. Owing to the generation of a spark discharge neighboring powder particles, dense cylindrical samples were obtained after a short sintering time of 30 minutes at the temperature of 650°C. The highest values of the Vickers microhardness, about 8.9 GPa, were obtained when the powders were sintered in the temperature range of 600°C to 650°C for a holding time of 30 minutes, while the fracture toughness was found to be inversely proportional to the sintering temperature. However, at the sintering temperature of 650°C, the fracture toughness increased from about 1.40 to 1.52 MPa √m as the holding time increased from 10 to 60 minutes. As compared to cast specimens, the enhanced mechanical properties are explained by the refined microstructure resulting from the low temperature and short sintering time applied during SPS processing     

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.