New technological approach to fabrication of high density PM parts by cold pressing sintering

Abstract

A new technological approach to the fabrication of high density powder metallurgy (PM) parts via single pressing sintering, allowing cold compaction to be performed without admixed lubricants, has been studied. The influence of in pore gas on the compacts' green density and their sintered properties were evaluated. A mathematical expression relating in pore gas pressure in the compacts to the green density was developed. The expression showed that in order to reduce the negative influence of gases trapped in the pores it is necessary to ensure effective air drainage from the compaction zone. In order to ensure sufficient air evacuation during cold compaction, a new design of porous die was developed. The behaviour of powder mixes with different lubricants during cold compaction in porous die was investigated. All the test conditions were evaluated in terms of green and sintered properties, including the ejection force, green and sintered densities, tensile strength and surface hardness. In the context of the experimental work, compaction in porous die promoted the improved combination of green and sintered properties compared with compaction in conventional dies.     

Role of reinforcement in sintering of SiC/316L stainless steel composite

Abstract

Austenitic stainless steels with improved corrosion resistance are gaining wide popularity. However, their applications are limited because of their poor tribological properties. The present work was undertaken to improve the overall performance of 316L stainless steel by reinforcing it with SiC. During the processing of the 316L SS composite, the 316L SS matrix was found to interact strongly with the SiC at 1100°C resulting in the formation of low melting Fe–SiC phase. An attempt to process SiC/316L SS composite above this temperature resulted in complete melting of the composite compact.     

Transient liquid phase sintering of high density Fe3Al using Fe and Fe2Al5–FeAl2 powders Part 2 – Densification mechanism analysis

Abstract

The use of Fe₂Al₅–FeAl₂ prealloyed powders and heating rates >150 K min^?1 overcomes the formation of density restricting Kirkendall porosity in the Fe–Al system. X-ray diffraction, electron probe micro analysis and differential thermal analysis suggest that the absence of a persistent liquid, experienced when liquid phase sintering with elemental powders, is overcome. Homogenisation is greater during heating at a rate of 20 K min^?1 than for 150, 250 or 400 K min^?1 and homogenous Fe₃Al forms across the compact at temperatures below the melting point of the liquid forming constituent, indicating that a liquid will not form under such processing conditions. The maximum density achieved under the processing conditions in the present study is 92% of theoretical density. The presence of large pores shortly after liquid formation suggests that the remaining porosity is largely due to powder agglomeration during mixing.     

Porous tungsten with controlled porosity by low temperature sintering

Abstract

Porous tungsten as a high current density cathode is one of the important applications of the metal, which is mostly used in high temperature conditions due to its exceptional resistance to melting (T _m = 3410±20°C). Its porous form has been a crucial component of dispenser cathodes used in electronic valves and high power lamps. Porous tungsten skeleton forms the matrix, which is then impregnated with an electron emissive compound. Upon every emission from the surface, new material has to be fed into the surface pores via the open pore channels. Hence it may be proposed that a uniform porosity is needed for a better performance. However, a controlled porosity has not been achieved yet. Moreover, sintering of tungsten has always been difficult due to the extreme process conditions. A high sintering temperature (T _s≥2000°C) and a strong reductive atmosphere (hydrogen) have been the absolute necessity in making these parts. This study further explores an alternative sintering technique being developed. The idea is based on the reactive sintering concept. The energy output from the exothermic reactive system of tungsten oxide and aluminium has been the heat source for sintering porous tungsten. As a result, sintering temperature and time have been reduced considerably. Higher homogeneity, thus more uniform pore distribution, was observed. A better control of porosity related to the pressing and sintering conditions was achieved by the characterisation method previously developed. Microhardness has been a useful monitor of the scatter in porosity of the parts. Throughout the study, SEM was used to observe the porous structures and powder morphologies. DSC and XRD were useful to follow the microstructural evolution in the reactive system.     

Microstructural development during liquid phase sintering of Fe and Fe–Mo alloys containing elemental boron additions

Abstract

The sintering behaviour of Fe and Fe–Mo prealloyed powder compacts containing from 0·5 to 3·5 wt-%Mo and fixed boron additions has been studied with special emphasis on the microstructural development, the formation of the liquid phase and the liquid phase sintering mechanisms involved during the densification process. The basic phenomena involving the formation of a liquid phase and the temperature at which the liquid is generated is strongly influenced by the Mo/B ratio in the initial powder mixture. The effect produced by Mo and its concentration, both, on the final microstructure and on the behaviour of boron prior to, during and after the formation of the liquid phase, was studied under both the optical and the scanning electron microscope. For this purpose interrupted sintering experiments followed by water quenching from specific temperatures and times within the sintering cycle have been carried out. The study shows that the formation of a liquid phase is preceded by noticeable enhancement of solid state sintering at intermediate temperatures. This is accompanied by boron diffusion into the metallic particles, generating inter- and intragranular precipitates in amounts dependent on the Mo concentration. At a later stage boron is found to be preferentially located at the boundaries as the formation of a continuous Fe/Mo/B liquid phase with excellent wetting characteristics proceeds thus producing densification by pore filling and shape accommodation. Final densities up to 7·82 g cm^?3 were obtained for these alloys.     

Suitability of nickel as alloying element in titanium sintered in solid state

Abstract

The suitability of nickel as an alloying element in titanium alloys produced using the blended elemental powder metallurgy approach has been explored. Nickel initially accelerates sintering, providing greater densification at lower temperature than observed for unalloyed titanium. However, it provides only a minor improvement in the density achieved after long sintering times or at high solid state sintering temperatures. Swelling is observed under liquid phase sintering conditions. The highest density was achieved by sintering at just below the solidus temperature. Nickel also accelerates the Ostwald ripening of the pore structure and the conversion of open porosity into closed porosity.     

Analysis of compaction behaviour of wet granulated aluminium alloy powder

Abstract

The compaction behaviours of wet granulated aluminium powder were examined by uniaxial die compaction, and their effect on rearrangement and plastic deformation was analysed by using the Cooper–Eaton equation. Based on the calculation results and structure/morphology of the granulated powder, a new compaction model for granulated powder, which consists of three compaction mechanisms (macrorearrangement, microrearrangement, and plastic deformation), and a modified equation has been proposed in this study. A macrorearrangement indicates it to be a dominant factor on the compaction behaviour of granulated powder and the modified equation is sufficient to analyse the compaction behaviour.     

Numerical simulation of die compaction and sintering

Abstract

A method to simulate die compaction and sintering is presented. By implementing user defined routines for both processes into the general purpose finite element program ABAQUS quantitative predictions of density distributions and shape distortions can be obtained as well as the stresses in the tool components. By computational optimisation of the individual production steps suggestions can be made to improve the final properties. As an example for both die pressing and sintering a complex three-dimensional part is simulated and suggestions to improve dimensional accuracy are made. Finally, stresses in the tools are calculated showing that the deflections are large enough to cause punch to punch contact so that tool wear must be expected.     

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.     

Process and compressive properties of porous nickel materials

Abstract

Compressive properties are investigated for the porous Ni materials processing by innovated powder metallurgical (PM) method. The porous Ni materials first show a short elastic region, then a long and oblique stress yield region within the strain range of about 10–50%, and finally, a densification region where the stress increases rapidly.     

Liquid phase sintering of ferrous powder by carbon and phosphorus control

Abstract

Powder mixtures composed of liquid forming master alloy powder and coarse iron powder were sintered to near full density by having a high amount (20 wt-%) of liquid phase during sintering. This was made possible by the use of the Fe-P-C system with or without Cu. Without post-sintering treatment, a brittle microstructure was obtained. By means of altered C and P control and decarburisation heat treatment of the as sintered material, the final non-brittle microstructure was achieved. Using the open porosity and liquid phase as a diffusion path, rapid decarburisation is created and the local combination of carbon and phosphorus in the microstructure is avoided. In this way, iron phosphide is not formed on grain and/or particle boundaries. Presence of pores is confirmed to be beneficial for grain growth control.     

Swelling during sintering of titanium alloys based on titanium hydride powder

Abstract

Compacts were prepared by pressing titanium and titanium hydride powders mixed with nickel powder and sintering under vacuum. Severe swelling was observed only for compacts based on TiH₂ powder. Pressure changes in the vacuum furnace, dilatometry results and mass loss data all indicate that dehydrogenation of TiH₂ powder compacts occurs at lower temperature than any significant sintering. Swelling appears to have been caused by a contaminant in the TiH₂ powder rather than hydrogen. The onset of severe swelling during heating was associated with the formation of liquid phase as the solidus was crossed. However, some swelling appears to take place under solid state sintering conditions. Various results indicate that the mechanism of swelling is high gas pressure within closed pores. Large pores appear to form by breakage of ligaments between small pores followed by opening of the pore. It appears that the use of (uncontaminated) TiH₂ powder in place of Ti powder would allow the benefit of lower green porosity to be retained during sintering to achieve low sintered porosity.     

Effect of welding consumables on hydrogen induced cracking of armour grade quenched and tempered steel welds

Abstract

Armour grade quenched and tempered (Q&T) steels are susceptible to hydrogen induced cracking (HIC) in the heat affected zone after welding. Austenitic stainless steel (ASS) consumables are selected for welding Q&T steels as they have higher solubility for hydrogen in the austenitic phase and it is the most beneficial method for controlling HIC in Q&T steel welds. Recent studies reveal that high nickel steel and low hydrogen ferritic steel consumables can be used to weld Q&T steels, which can give very low hydrogen levels in the weld deposits. In this investigation, an attempt has been made to study the effect of welding consumables on hydrogen induced cracking of Q&T steel welds by implant testing. Shielded metal arc (SMAW) welding process has been used for making welds using three different consumables, namely austenitic stainless steel, low hydrogen ferritic steel (LHF) and high nickel steel (HNS) to assess HIC by implant testing. The high nickel steel consumables exhibited a higher value of lower critical stress (LCS) and thus they offered a greater resistance to hydrogen induced cracking of armour grade Q&T steel welds than other consumables. The diffusible hydrogen content and the value of the LCS meets the specified limit for armour grade Q&T steel welds and hence, the LHF consumables can be accepted as an alternative to the to the traditionally used ASS consumables and the proposed HNS consumables.     

Spark plasma sintering as advanced PM sintering method

Abstract

A short overview of works on spark plasma sintering (SPS) is given in the present paper. SPS is a newly developed rapid sintering technique with a great potential for achieving fast densification results with minimal grain growth in a short sintering time. It is proven by obtained experimental data that enhanced sinterability of powders subjected to SPS mainly associated with particle surface activation and increased diffusion rates on the contact zones caused by applied pulse current. Application of rapid heating results in bypassing of low temperature regions where surface transport controlled sintering is dominant. This preserves the powder surface area to temperature levels where bulk transport is significant. However, the nature of activation effects, especially in its regards to acceleration of diffusion processes, is not clearly established. A lot of research work reports about the occurrence of plasma during the application of pulse current. However, the appearance of thermal plasma during SPS is a controversial issue and plasma-particle interaction is a complex phenomenon. Presently the industrial application of SPS processing is considered mainly in the areas where it is difficult or extremely difficult to obtain high performance materials and where normally HP or hipping processes are applied. Apparently significantly more work is required in this field for better understanding of the entire process and for making a stable ground for more extended industrial application of SPS.     

Pressing vacuum sintering of multipowders for manufacturing novel engine valve seat on Gleeble 1500 simulator

Abstract

Patented Fe based multipowders for manufacturing novel engine valve seat were compacted and sintered using a Gleeble 1500 thermal simulator system. Microstructures and properties of the sintered alloy have been studied by hardness test, optical microscopy (OM), scanning electron microscopy (SEM), energy dispersive X-ray analysis (EDX) and X-ray diffraction (XRD) analysis. Results indicate that a sintered alloy with a hardness of 38 HRC and a density of 7·23 g cm^?3 can be obtained when the green compacts are sintered at 1240°C for 30 min. It is found that lattice parameters of the alloy matrix increase with increasing sintering temperature. Additionally, the investigation of green compacts' shrinkage during sintering shows that there is a threshold value for the density of the green compacts. When the density of the green compacts is lower than that value, the density of the sintered alloy remains almost constant with increasing density of green compacts. An equation to calculate the threshold density has been suggested as νρ² = C ₁ ρ² + C ₂ m² + C ₃ m ρ.     

Modelling of steel shrinkage and optimisation of mould taper for high speed continuous casting

Abstract

In high speed continuous casting, optimisation of mould taper is key for intensifying heat transfer and for improving the quality of the cast products. Mathematical modelling has been carried out by combining heat transfer, steel shrinkage and parabolic continuous taper model in order to optimise the mould taper profile. These models have been assembled to a set of software, the inputs of which include the steel grade, casting speed, casting temperature, length and the cross-section of mould tube, while the outputs consist of surface temperature of the strand, thickness of solidified shell, thermal linear expansion coefficient, steel shrinkage, distortion of the mould tube wall, the actual air gap, total taper and the continuous taper profile. Optimum mould taper has a parabolic profile which is tapered inwards that changes continuously along the length of the strand in order to achieve reduction in air gap while avoiding distortion of the mould tube.     

New method to prepare iron particles with different morphologies: a way to get high green strength metal compacts

Abstract

Metaliron powders of well controlled size and morphology were synthesised by thermal decomposition under hydrogen of precipitated ferrous oxalates. Green compacts were prepared by uniaxial pressing of metal powders at 290 MPa. The bending green strengths of compacts were measured.

The precipitation of β-FeC₂O₄.2H₂O oxalate from ammonium oxalate gives rise to the formation of spherical particles by aggregation ofelongated grains. Thermal decomposition of this oxalate from 400 to 500°C under hydrogen permits metal iron particles with a rough surface to be obtained. Decomposition occurring above 500°C induces a smoothness of the particle surface. Metal particles synthesised at 500°C show both surface roughness and micrometer sized primary grains.This specific microstructure has allowed the highest value ofcompact green strength (31·7 MPa) to be obtained.

Acicular shaping of the β-FeC₂O₄.2H₂O particles precipitated from oxalic acid involves, after decomposition, an increase in the surface roughness and shape irregularity of the metal particles, owing to an entanglement of the elementary grains. An exceptional value (about 60 MPa) for the metal compact green strength was thus obtained for this type of powder.     

Optimised sintering route for cold work tool steels

Abstract

Two different powder metallurgy cold work tool steels, D7 and a nickel alloyed D7 modification, were compacted to full density by utilisation of super solidus liquid phase sintering in vacuum and nitrogen atmospheres. The experiments were carried out with respect to the fabrication of wear resistant metal matrix composites. These materials exhibit a higher durability than cast materials and are increasingly used in the mineral and mining industry. In the present paper, sintering exhibits a more cost effective processing of these materials compared with hot isostatic pressing. The experiments were supported by thermodynamic calculations with Thermo-Calc. Significant differences of the sintering behaviour in vacuum and nitrogen atmospheres were detected. Full density could be obtained at a sintering temperature as low as 1210°C.