Comparison of sintering of titanium and titanium hydride powders

Abstract

The cold compaction and vacuum sintering behaviour of a Ti powder and a Ti hydride powder were compared. Master sintering curve models were developed for both powders. Die ejection force, green strength and green porosity were lower for hydride powder than for Ti powder, all probably resulting from reduced cold welding and friction during compaction. For sintering temperatures above ～1000°C, most of the difference in the sintered density of Ti and hydride is explained by assuming equal densification, while taking into account the lower green porosity of compacts made from hydride powder. However, there is evidence that particle fracture during compaction also contributes to increased sintered density for hydride powder. The Ti powder conformed to a master sintering curve model with apparent activation energy of 160 kJ mol^?. The activation energy for Ti hydride also appeared to be about 160 kJ mol^?, but the model did not fit the experimental data well.     

Meeting the challenges: the early days and start-up of EPMA

Abstract

Magnesium (with density, ρ?=?1.74?g cc^??1) being ～35% lighter than aluminium and ～75% lighter than steel is an attractive and a viable candidate for the fabrication of lightweight structures. Being the designers' choice for weight critical applications, extensive research efforts are underway into the development of magnesium metal matrix composites (Mg-MMCs) through various cost effective fabrication technologies. In recent years, there has been a progressive advancement in utilising the microwave energy to consolidate powder materials, and the present study accentuates the use of energy efficient and environment friendly microwave sintering process to synthesise magnesium based composite materials. The processing advantages of the innovative and cost effective microwave assisted bidirectional rapid sintering technique followed by hot extrusion are first briefly introduced. Subsequently, the properties of various Mg-MMCs containing nanosized ceramic/metal particles, synthesised using this technique, are presented. Special emphasis has been made on the commending mechanical properties displayed by the nanoparticle reinforced Mg composites (Mg-MMNCs). Finally, an account of continuing research initiatives related to the development of novel lightweight Mg composites containing amorphous reinforcement is also highlighted.     

INFLUENCE OF TIN POWDER CHARACTERISTICS ON THE SINTERING OF IRON-TIN-COPPER POWDER COMPACTS

Abstract

In view of increasing industrial interest in the use of tin additions as an aid to the sintering of iron-based powder compacts, an examination has been made of the influence of the characteristics of the tin powder on sintering performance.

The effect of additions of narrow size-range fractions of atomized tin powder on the dimensional changes and tensile properties obtained on sintering Fe-Sn-Cu compacts made with –100 mesh (–152 μm) or – 300 mesh (– 53 μm) sponge iron and – 300 mesh (– 53 μm) atomized copper powders has been determined. The compacts contained tin and copper in the ratio 2:3. The narrow size fractions were separated from – 300 mesh tin powder by air elutriation. It was found that the use of coarse tin powder reduced the tensile strength of – 300 mesh iron-based Fe–1% Sn–1 ½% Cu compacts, but had no influence when this mixture was based on –100 mesh iron powder, or when the mixture composition was Fe–2% Sn–3% Cu. The effects have been examined in relation to the sintering mechanism by scanning electron microscopy and by X-ray microanalysis.     

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.     

THE POWDER METALLURGY OF TITANIUM–TIN ALLOYS CONTAINING UP TO 15% TIN

Abstract

Density measurements and data on the mechanical properties of titanium–tin alloys, fabricated by powder metallurgy from sodium-reduced titanium, are reported.

Low porosities were achieved after a single pressing and sintering operation. A typical set of preparation conditions involved compacting at 40 tons/in.² and sintering, in vacuum, at 1300° C. for 1 hr. With tin contents above 5%, evaporation of tin during sintering could prove troublesome.

The presence of tin strengthened titanium markedly. The addition of 15% tin increased the ultimate tensile stress at room temperature by ～90%, with a corresponding, though less marked, reduction in ductility.     

Synthesis and characterisation of quasicrystalline Al based composites

Abstract

Al matrix composites reinforced by Al–Cu–Fe quasicrystalline (QC) phase particles were produced from a mixture of Al and QC powders using electrical current heating and conventional sintering. A combination of X-ray diffractrometry, transmission and scanning electron microscopy was used to characterise the microstructure of consolidated specimens. The metallic bonding of the Al matrix and particles was improved by higher temperature sintering or electrical current heating. However, the dissolution of QC particles into the Al matrix was inevitable during heating and resulted in the formation of ω and/or β phases. The dissolution of QC particles was effectively reduced using prealloyed Al powder containing 2 at.-%Cu. This had led to an increase in microhardness from 96 to 139 HV for specimens using pure Al to prealloyed Al powders. A homogeneous distribution of QC particles within the Al matrix could be achieved by mechanical milling followed by consolidation.     

INFLUENCE OF THIN OXIDE FILMS ON THE MECHANICAL PROPERTIES OF SINTERED METAL-POWDER COMPACTS

Abstract

The influence of thin oxide films, in the range 200–1200Å thick, on the mechanical properties of sintered iron, copper, and nickel powder compacts has been investigated. As the thickness of the oxide film on the metal powders increased, the properties studied, namely, densification parameter, hardness, and tensile strength improved and attained a maximum at a critical oxide-film thickness, the value of which was ～ 625 Å for iron and nickel and ～ 500 Å for copper. Further increase in thickness to ～ 1200 Å led to a gradual decline in the properties. The improvement in the properties obtained with powders having the optimum oxide thickness was independent of the sintering atmosphere. A probable explanation in terms of activated sintering is given.     

Fabrication of in situ TiB2–TiC reinforced steel matrix composites by spark plasma sintering

Abstract

In situ TiB₂ and TiC particulates reinforced steel matrix composites have been fabricated using cheap ferrotitanium and boron carbide powders by spark plasma sintering (SPS) technique. The sintering behaviour and the formation mechanism of the composite were studied. The results show that when the composite was sintered at 1050°C for 5 min, the maximum relative density and hardness of the composite are 99·2% and 83·8 HRA respectively. The phase evolution of the composite during sintering indicates that the TiB₂ and TiC reinforcements were formed in situ as follows: first, the solid/solid interface reaction between Fe₂Ti and B₄C, resulting in the formation of a small amount of TiB₂ and TiC below 950°C; second, the solid–liquid solution precipitation reaction in the Fe–Ti–B–C system, resulting in the formation of the main TiB₂ and TiC reinforcements at ～1000°C.     

SINTERING KINETICS OF OXIDE-FILMCOATED COPPER POWDER

Abstract

The sintering kinetics of pure copper powder and of copper powder coated with a critical oxide (CU₂O) film thickness (～,500Å), has been studied by following the densification of the compacts as a function of temperature and time in pure dry hydrogen and in vacuum. The activation energy for the sintering of pure copper powder in hydrogen was 55,000 cal/mole, suggesting that the volume self-diffusion mechanism predominates during the sintering process. In the case of the oxide-coated powder the corresponding value was 37,000 cal/mole. The high rate of sintering of the coated powder in hydrogen and in vacuum is explained in terms of an activated sintering mechanism.     

Microstructure characteristics in Al-C system after mechanical alloying and high temperature treatment

Abstract

In this work elemental powders of Al and 2 wt-% graphite were mechanically alloyed in a high energy horizontal attritor under purified argon atmosphere for 0·5-2 h. Powder mixes were then cold pressed at 1200 MPa and sintered at 550°C for between 2-32 h under the same protective atmosphere. Structural evolution was characterised by X-ray diffraction, scanning electron microscopy and transmission electron microscopy techniques. Results revealed that mechanical alloying was very effective in pulverising the powder mix, where after 2 h, the mix was fine enough to oxidise rigorously when exposed to open air. In general however, mechanical alloying was found to be inefficient to synthesise Al with C. But after sintering, Al₄C₃ phase nanosized particles were formed in the microstructure. When the duration of sintering was prolonged, the particle population multiplied in number. Hence because of improvement in dispersion strengthening, the room temperature hardness of the material increased gradually.     

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.     

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.     

Enhanced sintering and mechanical properties of 316L stainless steel with silicon additions as sintering aid

Abstract

Compaction, effect of ball milling, vaccum sintering, microstructures, volume shrinkage, interconnected porosity, thermal reactions and mechanical properties of 316L stainless steel with and without additions of elemental silicon have been investigated. It was found that the silicon addition enhanced the sintering process by providing a series of liquid phase reactions with the base powder which took place at temperatures below their melting points and the normal solidus range for stainless steels. Differential thermal analysis confirmed formation of liquid phases at three different temperatures which are believed to be responsible for the enhanced sintering process.The first two appeared at ~1060 and 1155°C by two exothermic peaks and the third one at ~1190°C by an endothermic peak. The ball milling operation provided higher green and sintered densities resulting in better mechanical properties due to less agglomorations with finer and much more uniform particle size distribution. Sintered densities of up to 7·44 g cm^-3 with tensile strength of 482 MPa, hardness value of 153 HV10 and 15% elongation were obtained with ball milled plus 3 wt-%Si addition. Low levels of interconnected porosities (~4%) were recorded within the temperature range 1250-1300°C suggesting the possibility of good corrosion resistance.

The sintered microstructures consisted of ferrite and austenite (duplex structure), complex silicide and eutectic phases within grains and at grain boundaries, pools of liquid (rich in Si) and some medium and small pores preventing full density to be achieved despite the liquid phase formation.     

Fe3Al/TiC nanocomposite produced by mechanical alloying

Abstract

The aims of this work were to produce nanocrystalline powder by mechanical alloying of FeTi₂–Al–C powder mixture in a high energy ball mill and to study the phase transformation that took place during 20 h milling time. The microstructure and the phase transformations in the powder during milling were examined as a function of milling time and heat treatment. The phases of the product were evaluated by X-ray diffraction technique. The microstructural evolution during mechanical alloying was analysed using SEM. The results obtained showed that high energy ball milling, as performed in this work, led to the formation of a bcc phase identified as Fe(Al) solid solution and TiC_x after 2 h milling and nanocrytalline AlFe₃ and TiC_x after 5 h milling. The increase in the milling time resulted in the formation of AlFe₃C_x. By heat treatment of the body after 20 h milling at 1000°C, AlFe3C_x disappeared, showing that this phase is unstable.     

(Ti,V)C钢结硬质合金的烧结行为、物相及组织结构

以钛粉、钒铁粉、碳粉、铬铁粉、钼铁粉和铁粉为原料,用原位烧结法制备了(Ti,V)C钢结硬质合金.利用XRD、SEM和EDS对相组成、组织结构和微区成分进行了分析.结果表明:最佳烧结时间是1 h;烧结温度影响致密化程度,(Ti,V)C钢结硬质合金的最佳烧结温度是1 400 ℃;TiC钢结硬质合金的最佳烧结温度是1 420 ℃.(Ti,V)C钢结硬质合金的主要相组成为α-Fe、Fe3C、(Cr,Fe)7C3、(Ti,V)C.与TiC硬质相颗粒相比,(Ti,V)C颗粒形态更加圆整.     

Characterisation of powder metallurgy H13 steels prepared from water atomised powders

ABSTRACT

In this paper, powder metallurgy (PM) H13 steels were investigated based on the characterisation of water atomised H13 powders. Vacuum sintering was carried out from 1150 to 1265°C for sintering densification. The relative density of the as-sintered sample reached to 95% and mechanical properties were released above 1200°C. To eliminate the residual pores, subsequent forging was performed. The relative density increased to above 99%. As the concentration of Si elements on the powder surface was higher than the nominal composition, there was Si segregation in the form of silicon oxides (1–3?μm). Although oxide particles such as SiO₂ were inevitable, the mechanical performance of PM H13 steels was still comparable to that of ingot metallurgy products. The tempered PM H13 steels exhibited high tensile strength of 1460?MPa in YS, 1737?MPa in UTS and 8.7% in elongation. Besides, the impact toughness was as high as 14.7?J?cm^?2.     

烧结温度对钴基耐磨合金微观组织和性能的影响

在真空环境下采用粉末冶金法制备碳化物增强钴基耐磨合金,利用扫描电子显微镜(scanning electron microscope,SEM)、电子探针显微分析仪(electron probe microanalyzer,EPMA)、X射线衍射仪(X-ray diffractometer,XRD)等设备观察和分析烧结温度对合金微观组织的影响,研究了增强相的物相及其形成机制。研究结果表明:粉末冶金法制备的钴基耐磨合金基体由面心立方(face center cubic,FCC)结构的γ-Co和密排六方(hexagonal closed-packed,HCP)结构的ε-Co相组成,增强相为M6C和M_(23)C_6型碳化物。当固相烧结温度为1250℃时,块状M6C型碳化物和颗粒状M_(23)C_6型碳化物弥散分布于基体中;当烧结温度升高至1340℃,M6C型碳化物呈尖锐的棱角状,平均尺寸大于30μm,颗粒状M_(23)C_6消失;烧结温度继续升高至1360℃,M6C型碳化物呈骨架状,ε-Co相消失。对合金的力学性能测试结果表明,当烧结温度为1270℃时,钴基合金的综合性能最佳,硬度大于HRC 60,抗压强度为1921 MPa,抗拉强度为203 MPa,摩擦系数为0.561。     

Sintering transformations in mixtures of austenitic and ferritic stainless steel powders

Abstract

The microstructural transformations and the dimensional evolution of green specimens obtained by pressing mixtures of austenitic and ferritic stainless steel powders have been investigated by sintering at 1120 and 1240°C. Dilatometry experiments show that the linear shrinkage is influenced by the amount of ferritic powder. Moreover, during sintering Ni diffuses into the ferritic grains causing austenite destabilisation and the formation of a mixed constituent, whose constitution has been investigated by means of EDXS and interpreted on the basis of the Schaeffler diagram. Sigma phase also forms during sintering of the duplex mixtures.     

Characterisation and sintering studies of mechanically milled nano tungsten powder

Abstract

Elemental tungsten powder was mechanically milled by planetary mill for 100 h. Particles were thinned down to nanometre scale. The shape of the milled powders was flat cylindrical with average diameter and length 12˙5 and 46˙5 nm respectively. The corresponding crystallite size obtained by X-ray diffraction (XRD) was 26˙96 nm. The results obtained by XRD and small angle X-ray scattering were well supported by transmission electron microscopy and high resolution transmission electron microscopy results. The maximum shrinkage of the compact has been observed at ～1500 K, which has been used as a guideline for sintering experiments. The powders sintered at 1773 K have resulted in 96% relative density.     

Fracture micromechanics of static subcritical growth and coalescence of microcracks in sintered Fe–1·5Cr–0·2Mo–0·7C steel

Abstract

Nucleation of microcracks, their growth and coalescence are analysed in powder metallurgy (PM). Fe–1·5Cr–0·2Mo–0·7C steel by fractography allied to surface replica microscopy – at several stress levels as the maximum tensile stress in three-point bend specimens was raised to 99·6% of the transverse rupture strength TRS of 1397 MPa. The fatigue limit in this material is ～240 MPa, at which stress level no microcracks were detected in static loading. Numerous microcracks, ranging in size from <5 to ～20 μm, however, were nucleated above ～800 MPa, i.e. beyond the yield strength of ～620 MPa. With increasing stress, some microcracks became dormant, whilst others grew subcritically, stress step-wise, to some 400 μm. Of particular importance are observations of the coalescence of two and three of such microcrack systems to produce a critical, propagating crack. The then estimated stress intensity factor K _a, could reach K _1C, independently estimated to be ～36 MPa m^1/2. Microcrack coalescence was associated with easy paths for crack growth, principally prior particle boundaries linking pores. Ways of making subcritical crack growth more difficult and hence improving both static and dynamic mechanical properties, are considered.