Mapping complex microstructures in powder metallurgy steels

Abstract

New methods of characterising multiple phase powder metallurgy steels have been investigated. Mapping of microhardness with a lateral resolution of as little as 5 μm and with up to 10⁴ indents can produce distributions of mechanical properties which are characteristic of different steel grades. Maps of these properties can be correlated with the different phases observed in etched microstructures, and quantification of size and interconnectivity of the regions with, for example, different hardness or stiffness is then possible. Electron backscatter diffraction can also produce simultaneously highly detailed maps of the different phases in a powder metallurgy steel with chemical composition information. Percentages of the different phases present can be determined from the crystallography and morphology of the grains observed, but the technique is limited by the speed with which maps can be acquired.     

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.     

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.     

Wear behaviour of Fe3 Al intermetallic particle reinforced PM based iron metal matrix composites

Abstract

The wear behaviour of unreinforced and reinforced PM based iron metal matrix composite, the latter containing 10 and 20 vol.-% nano sized Fe₃Al intermetallic particles, was studied as a function of sliding distance under two different loads and dry lubricated conditions. The intermetallic Fe₃Al nanoparticles were prepared by mechanical alloying and used as particle reinforcement with 10 and 20 vol.-% in the matrix. The processing of the composites included mixing and cold compaction followed by sintering at 1120°C. The influence of Fe₃Al additions on the dry sliding wear behaviour was studied at loads 20 and 40 N over sliding distances 2160, 3240, 4320 and 6480 m. The study showed that the composite exhibited a lower wear rate than that of the unreinforced matrix and the wear rate was influenced by the volume percentage of Fe₃Al particles. It is understood that iron aluminide reinforcement has a beneficial effect on the wear properties. Delamination and microcutting were the chief mechanisms of wear for the composites.     

Effect of boron on vacuum carburising depth of iron powder metallurgy compacts

Abstract

The work was aimed at determining the effect of boron on vacuum carburising of iron compacts with density over 7·2 g cm^–3. An attempt was made to determine the effectiveness of boron on carbon diffusion rate into the material of compacts with no additional effect of interconnected porosity. Vacuum carburising of compacts made of iron powder with an addition of boron was carried out at 1050°C in a laboratory vacuum furnace.

The effect of boron content within 0·005 to 0·02% on the vacuum carburising depth was analysed. It was found that the boron addition up to 0·01% increased the carburising depth by ～0% in comparison with the compacts of pure iron.     

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.     

Thermodynamic and experimental study of role of sintering atmospheres and graphite additions on oxide reduction in Astaloy CrM powder compacts

Abstract

Several atmospheres based on N₂–H₂ gaseous mixtures, with occasional additions of CH₄ were used to study the sintering behaviour of Astaloy CrM at temperatures of 1100 and 1240°C. Theoretical thermodynamic calculations and sintering experiments, with and without admixed graphite additions, were carried out devoting particular attention to the oxide reduction reactions. The role of carbon in the reduction of oxides is discussed with reference to Boudouard's reaction, proposing the indirect carbothermal reduction as the controlling mechanism. The microstructural characterisation of the material included inspection of the powder particles as well as sintered specimens. It was established that the Astaloy CrM particles contain two distinct types of oxides. One associated with the particle surface and another, mainly constituted by Cr, forming a dispersion of internal oxides. These internal oxides were microstructurally characterised, both directly and by carbon extraction replicas. A selection of powder mixtures containing 0 and 0.4%C additions were used for obtaining tensile specimens in order to assess neck development, by the strength and elongation obtained under various atmospheres and temperature combinations.     

Identification of flow instabilities during hot working of powder metallurgy superalloy IN 100

Abstract

A simple instability condition based on the Ziegler's continuum principles as applied to large plastic flow, is extended for delineating the regions of unstable metal flow during hot deformation of powder metallurgy materials. This criterion has been applied to the existing flow stress data of powder metallurgy superalloy IN 100 and compared with the reported microstructural observations. The optimum hot working conditions for the PM superalloy IN 100 are suggested.     

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.     

Development and characterisation of direct laser sintering multicomponent Cu based metal powder

Abstract

Recent advances in direct metal laser sintering (DMLS) have improved this technique considerably; however, it still remains limited in terms of material versatility and controllability of laser processing. In the present work, a multicomponent Cu based metal powder, which consisted of a mixture of Cu, Cu–10Sn and Cu–8·4P powder, was developed for DMLS. Sound sintering activities and high densification response were obtained by optimising the powder characteristics and manipulating the processing conditions. Investigations on the microstructural evolution in the laser sintered powder show that liquid phase sintering with partial or complete melting of the binder (Cu–10Sn), but non-melting of the cores of structural metal (Cu) acts as the feasible mechanism of particle bonding. The additive phosphorus acts as a fluxing agent to protect the Cu particles from oxidation and shows a concentration along grain boundaries owing to the low solubility of P in Cu and the short thermal cycle of laser sintering. A directionally solidified microstructure consisting of significantly refined grains is formed, which may be ascribed to laser induced non-equilibrium effects such as high temperature gradient and rapid solidification.     

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.     

Numerical simulation of powder compaction for two multilevel ferrous parts,including powder characterisation and experimental validation

Abstract

The paper presents a summary of two case studies that were carried out by the scientific team in the Thematic Network PM Modnet. During the life of this project, the compaction of complex multilevel ferrous components was investigated. These formed a vehicle to explore methods to characterise the yield and friction properties of the powder, perform simulation of the compression stage of the forming process, complete experimental trials, and compare experimental and simulated results. Density comparisons were made with results from Archimedes, quantitative metallography, and computerised tomography and force levels were compared with recordings from the pressing trials. The results highlight differences between equipment and experimental techniques used in characterising powders. They also show that hardness, metallographic analysis, and computerised tomography may be used to measure density variations throughout the compact. The prediction of density variation was reasonably consistent when using different simulations, whereas punch force prediction showed good consistency. It was found that predicted and measured density distributions agree within 0·05 to 0·5 g cm^-3 and that punch force levels may be predicted within 10 to 30%. The study effectively establishes a benchmark with which to compare and improve future simulations.     

On deformation control of dental crowns prepared by titanium powder process

Abstract

This study describes the identification of the main cause of deformation of titanium dental copings prepared by a new powder metallurgy method. The deformation was observed during the process development and needed to be explained to achieve an approved fit. The coping fabrication process was divided into stages to find the main cause of deformation. Each individual stage was investigated to find the cause. Primarily the pressing, milling and sintering steps and the tooth preparation dies (mandrels) were studied. The main cause of the deformation was found to be a deformation of the tooth preparation die during the pressing phase. The other stages were all shown to contribute only slightly or not measurably to the deformation. When using tooth preparation dies of a stronger material (stainless steel) the dies did not deform measurably during cold isostatic pressing and copings of various individual forms with an approved fit could be prepared.     

Plasma densification of agglomerated Cr2O3 powder for thermal spray coating

Abstract

Double plasma flame treatments were carried out on spray dried Cr₂O₃ agglomerated powders to increase their apparent density. The powders that were subjected to the first densification treatment didn't show the entirely melted state, and were fully melted only after the second plasma treatment. Plasma densification resulted in powder size decreasing as well as apparent density of particles and also resulted in the fluidity increasing due to the powder melting and surface smoothing effects. However, some parts of the particles after the second treatment showed a hollowed structure, especially for a particle size above 30 µm. The influence of the thermal conductivity of powder and the gas pressure within aggregates exposed to the plasma flame in the particle densification process was discussed in detail. The powder density strongly influenced the structure of plasma sprayed coatings. The dense coatings with high hardness and high bond strength was achieved in the coatings produced from Cr₂O₃ powders after plasma densification.     

Water based processing of iron powder utilising starch consolidation

Abstract

The effects of water based shaping, by means of starch consolidation (SC), of an iron powder system regarding oxygen/carbon content and sintering performance were evaluated. Specifically, the influence of the drying conditions and the use of two different thickeners, xanthan gum and cellulose ether, were studied. The results showed that cellulose ether gave lower sintered density than xanthan gum, mainly because of less favourable rheological impact and air/gas entrapment at mould filling and consolidation. Due to less oxidation at drying and less removal of carbon at sintering, freeze dried specimens sintered to a higher density than room temperature air dried ones. The degree of oxidation and removal of carbon also influenced the as sintered microstructure. Ferrite grains surrounded by iron phosphide were found in both air dried and freeze dried specimens. However, the higher carbon content in freeze dried specimens also resulted in a significant amount of iron carbide grains (inclusions), which can be a potential strength limiting factor.     

Hot working characteristics of powder metallurgy Nimonic AP-1 superalloy

Abstract

A simple instability condition based on the Ziegler's continuum principles as applied to large plastic flow, is extended for delineating the regions of unstable metal flow during hot deformation of Nimonic AP-1 superalloy. The optimum hot working conditions for this material are suggested.     

Effects of powder processing on densification of titanium diboride based cermets

Abstract

The sinterability of TiB₂-Ni₃(Al,Ti) based cermets has been significantly improved by aggressive milling of the starting TiB₂-Ni-TiAl₃ powder mixtures. This technique improves not only liquid spreading by reducing TiAl₃ particle size but also eliminates alumina agglomerates and the associated porosity found after vacuum sintering. Liquid phase sintering of TiB₂-Ni-TiAl₃ powder mixtures involves the presence of Ni based secondary borides at low temperatures (1200°C), which react afterwards with TiAl₃ particles leading to the formation of the final TiB₂-Ni₃(Al,Ti) eutectic liquid. Apart from improving liquid spreading around TiB₂ grains, aggressive milling is also found to disperse alumina agglomerates, which reduces the porosity associated to these particles. By this refined procedure, the amount of binder phase required for full densification of TiB₂ cermets by sinter hipping has been reduced from a previous limit of 16 vol.-% to 10 vol.-%. The hardness of these TiB₂-10 vol.-%Ni₃(Al,Ti) cermets is in the range of ultrafine WC-Co hardmetals in spite of their much coarser microstructure.     

Relationship between physical structure and machinability of green compacts

Abstract

The dependence of green machinability on compact density and strength was investigated for room temperature and warm compacted steel powder compacts containing two different types of lubricant. Brazilian disc compression tests were employed to determine green strength, while machinability was assessed in terms of response to drilling.

For the room temperature compacted materials, it was found that high compact densities and strength were not, in most cases, associated with improvements in machinability. Furthermore, it was shown that lubrication (both type and quantity) and compaction pressure plays a critical role in determining the level of breakouts observed. In contrast, the use of warm compaction, in conjunction with specially designed lubricants, has been shown to be a suitable method of producing high density, high strength compacts while retaining good green machining characteristics. Mechanisms responsible for the observed behaviours of both the room temperature and warm compacted specimens have been forwarded in the present paper.     

Microstructural and mechanical properties of injection moulded gas and water atomised 17-4 PH stainless steel powder

Abstract

This paper describes the microstructural and mechanical properties of injection moulded 17-4 PH stainless steel gas and water atomised powder. Gas and water atomised stainless steel powders were injection moulded with wax based binder. The critical powder loading for injection moulding were 62·5 and 55 vol.-% for gas and water atomised powders respectively. Binder debinding was performed using solvent and thermal method. After dedinding the samples were sintered at different temperatures for 1 h in pure H₂. Metallographic studies were conducted to determine to extend densification and the corresponding microstructural changes. The results show that gas atomised powder could be sintered to a maximum (98·7%) of theoretical density, and water atomised powder could be sintered to a maximum (97·08%) of theoretical density. Maximum tensile strength was obtained for gas atomised powder sintered at 1350°C. The tensile strength of the water atomised powder sintered at the same temperature was lower owing to higher porosity. Finally, mechanical tests show that the water atomised powder has lower mechanical properties than gas atomised powder.     

Strain hardening behaviour of powder metallurgy alloys

Abstract

A model to describe the strain hardening behaviour of porous alloys, produced by powder metallurgy, is presented. It accounts for the influence of the matrix strain hardening ability, the initial porosity content and the pore geometry, and its predictive ability is verified with reference to sintered iron and an Fe–0·3%C sintered alloy. The necessity to introduce in the model a parameter able to account for the internal notch strengthening effect exerted by pores is emphasised. This parameter is found to be dependent on the sintering degree of the materials.