Institute of Fundamental Technological Research

Oxide Dispersion Strengthened (ODS) ferritic steels are promising materials for the nuclear power sector. This paper presents the results of a study on the sintering process using the Spark Plasma Sintering (SPS) technique, focusing on ODS ferritic steel powders with different contents (0.3 and 0.6 vol.%) of Y2O3. The novelty lies in the analysis of the effect of pre-annealing treatment on powders previously prepared by mechanical alloying on the microstructure, mechanical, and thermal properties of the sinters. Using the SPS method, it was possible to obtain well-densified sinters with a relative density above 98%. Pre-annealing the powders resulted in an increase in the relative density of the sinters and a slight increase in their thermal conductivity. The use of low electron energies during SEM analysis allowed for a fairly good visualization of the reinforcing oxides uniformly dispersed in the matrix. Analysis of the Mössbauer spectroscopy results revealed that pre-annealing induces local atomic rearrangements within the solid solution. In addition, there was an additional spectral component, indicating the formation of a Cr-based paramagnetic phase. The ODS material with a higher Y2O3 content showed increased Vickers hardness values, as well as increased Young’s modulus and nanohardness, as determined by nanoindentation tests.

spark plasma sintering, ODS ferritic steel, mechanical alloying, Mössbauer spectroscopy, nanoindentation

The paper presents a comprehensive investigation of the influence of the main process parameters of spark plasma sintering on the mechanical and microstructural properties of nickel-silicon carbide composites at various scales. Microstructure analysis performed by scanning and transmission electron microscopy revealed a significant interfacial reaction between nickel and silicon carbide due to the decomposition of silicon carbide. The chemical interaction of the matrix and reinforcement results in the formation of a multicomponent interphase zone formed by silicides (Ni31Si12 or/and Ni3Si) and graphite precipitates. Furthermore, several types of structure defects were observed (mainly nano/micropores at the phase boundaries). These significantly influenced the mechanical response of nickel-silicon carbide composites at different levels. At the macroscopic scale, uniaxial tensile tests confirmed that applying a 1000 oC sintering temperature ensured that the manufactured composite was characterised by satisfactory tensile strength, however, with a considerable reduction of material elongation compared to pure nickel. Moreover, the fractography study allowed us to identify a significant difference in the damage mode for certain nickel-silicon carbide samples. Secondly, the interface of the nickel matrix and silicate interphase was tested by bending with microcantilevers to evaluate its deformation behaviour, strength, and fracture characteristics. It was confirmed that a diffusive kind of interface, such as Ni-NiSi, demonstrates unexpected bonding properties with a relatively large range of plastic deformation. Finally, the nanoindentation of three main components of the nickel-silicon carbide composite was executed to evaluate the evolution of nanohardness, Young’s modulus, and elastic recovery due to the application of various spark plasma sintering conditions.

nickel-based composite,silicon carbide,spark plasma sintering,multiscale characterization,mechanical properties,nanoindentation,bending of microcantilevers

This work aims to revise and apply an original discrete element model (DEM) to evaluate effective thermal conductivity of sintered porous materials. The model, based on two-particle sintering geometry, calculates inter-particle neck using Constant Volume (CV) criterion. The model was validated using experimental measurements on sintered porous NiAl. For DEM simulations, heterogeneous samples with real particle size distribution and different densities were obtained by simulation of hot pressing. Neck size evaluated using Coble’s and CV models were compared to show that commonly used Coble’s model overestimates neck size and conductivity. The proposed model was improved by neck-size correction to compensate for non-physical overlaps at higher densities and by adding grain-boundary resistance to account for porosity within necks. Resistance contribution from grain boundaries was shown to decrease with increasing density. Thermal conductivity obtained from the improved model was close to experimental results, suggesting validity of the model.

Discrete element method,Effective thermal conductivity,Porous materials,Sintering,Heat conduction simulation

This paper aims to analyse electrical conduction in partially sintered porous materials using an original resistor network model within discrete element framework. The model is based on sintering geometry, where two particles are connected via neck. Particle-to-particle conductance depends on neck size in sintered materials. Therefore, accurate evaluation of neck size is essential to determine conductance. The neck size was determined using volume preservation criterion. Additionally, grain boundary correction factor was introduced to compensate for any non-physical overlaps between particles, particularly at higher densification. Furthermore, grain boundary resistance was added to account for the porosity within necks. For numerical analysis, the DEM sample was generated using real particle size distribution, ensuring a heterogeneous and realistic microstructure characterized by a maximum-to-minimum particle diameter ratio of 15. The DEM sample was subjected to hot press simulation to obtain geometries with different porosity levels. These representative geometries were used to simulate current flow and determine effective electrical conductivity as a function of porosity. The discrete element model (DEM) was validated using experimentally measured electrical conductivities of porous NiAl samples manufactured using spark plasma sintering (SPS). The numerical results were in close agreement with the experimental results, hence proving the accuracy of the model. The model can be used for microscopic analysis and can also be coupled with sintering models to evaluate effective properties during the sintering process.

Discrete element method, Effective electrical conductivity, Porous materials, Sintering, Resistor network model

The presented paper concerns the technological aspects of the interface evolution in the nickel-silicon carbide composite during the sintering process. The goal of our investigation was to analyse the material changes occurring due to the violent reaction between nickel and silicon carbide at elevated temperatures. The nickel matrix composite with 20 vol pct SiC particles as the reinforcing phase was fabricated by the spark plasma sintering technique. The sintering tests were conducted with variable process conditions (temperature, time, and pressure). It was revealed that the strong interaction between the individual components and the scale of the observed changes depends on the sintering parameters. To identify the microstructural evolution, scanning electron microscopy, energy dispersive spectroscopy, transmission electron microscopy, X-ray diffraction, and Raman spectroscopy were used. The silicon carbide decomposition process progresses with the extension of the sintering time. As the final product of the observed reaction, new phases from the Ni-Si system and free carbon were detected. The step-by-step materials evolution allowed us to reveal the course of the reaction and the creation of the new structure, especially in the reaction zone. The detailed analysis of the SiC decomposition and formation of new components was the main achievement of the presented paper.

We present the deposition and characterization of tungsten-tantalum diboride (W,Ta)B2 coatings prepared by the high-power impulse magnetron sputtering technique. We evaluated the influence of pulse duration and substrate bias on the properties of (W,Ta)B2 films. A high hardness of up to 35 GPa measured by nanoindentation was simultaneously obtained with good elastic properties. Changing the pulse duration greatly affected the B/(W+Ta) atomic ratio, which influenced the properties of the coatings. The deposited films are thermally stable at up to 1000 ◦C in vacuum and are able to withstand oxidation at 500 ◦C.

tungsten diboride, high power impulse magnetron sputtering (HiPIMS), hardness, thermal stability, oxidation resistance

The paper presents the experimental, numerical, and theoretical investigation of the microstructure of nickel aluminide samples manufactured by spark plasma sintering using electron backscatter diffraction and computer assisted software. The aim of the work was to reveal the evolution of the microscopic and macroscopic parameters related to the microstructure of the material and its dependence on the applied sintering parameters—temperature and pressure. The studied porous samples with different relative density were extracted from various planes and then tested by electron backscatter diffraction to evaluate the crystallographic orientation in every spot of the investigated area. On this foundation, the grain structure of the samples was determined and carefully described in terms of the grain size, shape and boundary contact features. Several parameters reflecting the grain morphology were introduced. The application of the electric current resulting in high temperature and the additional external loading leads to the significant changes in the structure of the porous sample, such as the occurrence of lattice reorientation resulting in grain growth, increase in the grain neighbours, or the evolution of grain ellipticity, circularity, grain boundary length, and fraction. Furthermore, the numerical simulation of heat conduction via a finite element framework was performed in order to analyse the connectivity of the structures. The numerical results related to the thermal properties at the micro- and macroscopic scale—local heat fluxes, deviation angles, and effective thermal conductivity—were evaluated and studied in the context of the microstructural porosity. Finally, the effective thermal conductivity of two-dimensional EBSD maps was compared with those obtained from finite element simulations of three-dimensional micro-CT structures. The relationship between the 2D and 3D results was derived by using the analytical Landauer model.

Copper-matrix composites reinforced with silicon carbide (SiC) particles are heat sink materials with potential application in the electronic industry. A major challenge in the manufacturing of these materials, involving sintering process, is to prevent the decomposition of SiC and the subsequent dissolution of silicon in the copper matrix. This is overcome by coating SiC particles with metallic layers. In this study, a combined experimental and computational micromechanics approach was used to investigate thermal conductivity of Cu-matrix composites reinforced with silicon carbide particles coated with chromium, titanium, or tungsten layers. Plasma Vapor Deposition (PVD) was used to produce the metallic layers on SiC particles, while Spark Plasma Sintering (SPS) to consolidate the powder mixtures of copper and coated silicon carbide. Thermal conductivities of the fabricated three-phase composites Cu/SiC/Cr, Cu/SiC/Ti and Cu/SiC/W were evaluated using the Laser Flash technique. Finite Element Method (FEM) and Variational Asymptotic Method (VAM) based homogenization techniques were used for computational modeling of thermal conductivity. In the numerical models complex material microstructures were accounted for using micro-CT images of the sintered compacts. Comparison of the experimental results with simulations highlighted the importance of including the effect of imperfect interfaces to accurately model thermal conductivity of the investigated composites.

metal-matrix composites, powder metallurgy, plasma vapor deposition, imperfect interface, thermal conductivity, numerical modeling

This work presents a comprehensive analysis of heat transfer and thermal conductivity of porous materials manufactured by spark plasma sintering. Intermetallic nickel aluminide (NiAl) has been selected as the representative material. Due to the complexity of the studied material, the following investigation consists of experimental, theoretical and numerical sections. The samples were manufactured in different combinations of process parameters, namely sintering temperature, time and external pressure, and next tested using the laser flash method to determine the effective thermal conductivity. Microstructural characterisation was extensively examined by use of scanning electron microscopy and micro-computed tomography (micro-CT) with a special focus on the structure of cohesive bonds (necks) formed during the sintering process. The experimental results of thermal conductivity were compared with theoretical and numerical ones. Here, a finite element framework based on micro-CT imaging was employed to analyse the macroscopic (effective thermal conductivity, geometrical and thermal tortuosity) and microscopic parameters (magnitude and deviation angle of heat fluxes, local tortuosity). The comparison of different approaches toward effective thermal conductivity evaluation revealed the necessity of consideration of additional thermal resistance related to sintered necks. As micro-CT analysis cannot determine the particle contact boundaries, a special algorithm was implemented to identify the corresponding spots in the volume of finite element samples; these are treated as the resistance phase, marked by lower thermal conductivity. Multiple simulations with varying content of the resistance phase and different values of thermal conductivity of the resistance phase have been performed, to achieve consistency with experimental data. Finally, the Landauer relation has been modified to take into account the thermal resistance of necks and their thermal conductivity, depending on sample densification. Modified theoretical and finite element models have provided updated results covering a wide range of effective thermal conductivities; thus, it was possible to reconstruct experimental results with satisfactory accuracy.

thermal conductivity, porous materials, spark plasma sintering, micro-computed tomography, nickel aluminide, finite element modelling, tortuosity

Magnetron sputtered WB2 coatings doped with 8, 11 and 16 at.% zirconium were analysed using energy dispersive spectroscopy, X-ray diffraction and nanoindentation under the load of 4, 7 and 10 mN. It has been observed that these coatings crystallize in the α-AlB2 and ω-W2B5 prototype structure. Phenomenon responsible for this is an increase of the zirconium content which causes an increase in the ω-W2B5 phase. All the deposited coatings have a hardness of about 45 GPa while Young's modulus drops down from 497 to 480 GPa with increasing zirconium content. Coatings without doping and doped with 16 at.% zirconium were annealed at 650 °C and subjected to cyclic thermal loads using a maximum temperature 600 °C and cooling with a compressed air. It has been observed that addition of zirconium improved coatings phase stability.

superhard coatings, tungsten diboride, zirconia doping, magnetron sputtering, cycling thermal loads, annealing

Metallic coatings are often applied on steel tubes in power generation boilers to improve their performance and extend the lifetime. Besides the high-temperature corrosion and erosion protection, the coatings should manifest good adhesion and cohesion strength, and relatively low residual stresses. In this study, three processing techniques: high velocity oxygen fuel spraying (HVOF), atmospheric plasma spraying (APS), and direct laser cladding were employed to obtain novel NiCr-Re and NiCr-Re-Al2O3 coatings intended for application in combustion boilers. The main objective was to assess the suitability of these three techniques to deposit NiCr-Re and NiCr-Re-Al2O3 composite coatings on a 16Mo3 steel substrate. For this purpose, a comparative analysis of the coatings behavior in selected tests was conducted. Of the three processing techniques, thermal spraying by HVOF turned out to be the optimum choice for the studied coatings. From among several variants of the HVOF-sprayed coatings, namely NiCr+1%Re, NiCr+2%Re, NiCr+1%Re+5%Al2O3, and NiCr+1%Re+10%Al2O3 (all vol.%), the NiCr+1%Re material exhibited the lowest extent of cracking in the disk bend test, the highest tensile strength (405 MPa) in the in-plane tension test, the highest Vickers hardness (379 HV2), the lowest specific wear rate (2.23·10-4 mm3/N m), and the lowest level of average residual tensile stress (120 MPa).

alumina, HVOF, mechanical behavior, nickel-chromium coatings, rhenium, residual stress, wear resistance

Experiments were conducted to investigate, within the framework of a multiscale approach, the mechanical enhancement, deformation and damage behavior of copper–silicon carbide composites (Cu–SiC) fabricated by spark plasma sintering (SPS) and the combination of SPS with high-pressure torsion (HPT). The mechanical properties of the metal–matrix composites were determined at three different length scales corresponding to the macroscopic, micro- and nanoscale. Small punch testing was employed to evaluate the strength of composites at the macroscopic scale. Detailed analysis of microstructure evolution related to SPS and HPT, sample deformation and failure of fractured specimens was conducted using scanning and transmission electron microscopy. A microstructural study revealed changes in the damage behavior for samples processed by HPT and an explanation for this behavior was provided by mechanical testing performed at the micro- and nanoscale. The strength of copper samples and the metal–ceramic interface was determined by microtensile testing and the hardness of each composite component, corresponding to the metal matrix, metal–ceramic interface, and ceramic reinforcement, was measured using nano-indentation. The results confirm the advantageous effect of large plastic deformation on the mechanical properties of Cu–SiC composites and demonstrate the impact on these separate components on the deformation and damage type.

copper–silicon carbide composite, high-pressure torsion, metal–matrix composites, multiscale analysis, nano-indentation, small punch test

In this paper, the discrete element method framework is employed to determine and analyze the stresses induced during and after the powder metallurgy process of particle-reinforced composite. Applied mechanical loading and the differences in the thermal expansion coefficients of metal/intermetallic matrix and ceramic reinforcing particles during cooling produce the complex state of stresses in and between the particles, leading to the occurrence of material defects, such as cracks, and in consequence the composite degradation. Therefore, the viscoelastic model of pressure-assisted sintering of a two-phase powder mixture is applied in order to study the stress field of particle assembly of intermetallic-ceramic composite NiAl/Al2O3. The stress evaluation is performed at two levels: macroscopic and microscopic. Macroscopic averaged stress is determined using the homogenization method using the representative volume element. Microscopic stresses are calculated both in the body of particles and in the contact interface (necks) between particles. Obtained results are in line with the cooling mechanism of the two-phase materials.

sintering, discrete element method, residual stress, particle-reinforced composites

Copper-alumina composites of the interpenetrating networks type are interesting materials for many applications because of their properties. On the base of preliminary investigations and practical works, in order to obtain a material with high resistance to friction wear as well as good dissipation of heat generated during work, it was decided that a developed material would be prepared on the base of the Cu-Al2O3 composite, with a graded composition. In this paper, we present the developed method of manufacturing dense copper–alumina FGMs, using ceramic preform with a graded porosity infiltrated with molten copper. The article also presents the full characterization of the obtained materials and mainly the impact of microstructure on the useful properties. The produced gradient material of a Cu-Al2O3 brake disk underwent tribological tests under conditions resembling real conditions. These disks also went through a series of abrasive wear trials at different operation stages. In comparison with the reference material (i.e., grey cast iron), the obtained gradient materials are characterized by a lower degree of wear when retaining a similar coefficient of friction value due to the ceramic phase addition. Additionally, it was found that using the copper-based gradient material guarantees faster heat dissipation from the contact area.

composites, interpenetrating network materials, functionally gradient materials, brake disc

This paper presents the results of studies concerning the production and characterization of Al-SiC/W and Cu-SiC/W composite materials with a 30% volume fraction of reinforcing phase particles as well as the influence of corrosion and thermal shocks on the properties of selected metal matrix composites. Spark plasma sintering method (SPS) was applied for the purpose of producing these materials. In order to avoid the decomposition of SiC surface, SiC powder was coated with a thin tungsten layer using plasma vapour deposition (PVD) method. The obtained results were analysed by the effect of the corrosion and thermal shocks on materials density, hardness, bending strength, tribological and thermal properties. Qualitative X-ray analysis and observation of microstructure of sample surfaces after corrosion tests and thermal shocks were also conducted. The use of PVD technique allows us to obtain an evenly distributed layer of titanium with a constant thickness of 1.5 μm. It was found that adverse environmental conditions and increased temperature result in a change in the material behaviour in wear tests.

metal-matrix composites, silicon carbide, wear resistance, corrosion, thermal shocks

The thermal and oxidation resistance of elements found in the combustion boilers of power generation plants are some of the most important factors deciding their effectiveness. This paper shows the experimental results of the influence of NiCr-based material composition on the microstructure and phase changes occurring during the oxidation and corrosion process. NiCr alloy was modified by the addition of rhenium and aluminum oxide. Materials were densified using the spark plasma sintering method at a sintering temperature of 1050 °C. Oxidation tests conducted up to 1100 °C under synthetic airflow revealed the formation of a thin Cr2O3 layer protecting the material against in-depth oxidation. Results of electrochemical corrosion in a 0.5 M NaCl solution indicated a positive role of Re and Al2O3 addition, confirmed by low corrosion current density values in comparison to the other reference materials. According to the provided positive preliminary test results, we can conclude that a NiCr-Re-Al2O3 system in coating form was successfully obtained by the plasma spraying method.

NiCr, rhenium, aluminium oxide, metal matrix composites, oxidation, corrosion

The high-velocity oxy-fuel technique (HVOF) was used to produce dense NiCrRe coating on boiler steel substrate with a minimal amount of oxide impurities and low porosity. Microstructure analysis, tribology and nano-hardness measurement have been realized with the aim to characterize the systems. The microstructure was studied using scanning electron microscopy and Energy-dispersive X-ray spectroscopy. Tribological characteristics have been studied under the dry sliding condition at applied loads of 5, 10 and 20 N using the ball-on-flat technique with SiC ball at room temperature. Nano-hardness was investigated in continuous stiffness measurement (CSM) mode, the indentation depth limit was 1500 nm. Microstructure analyses proved that the HVOF sprayed layer, with a thickness approximately 870 µm, contains a relatively low volume fraction of porosity with a chemical composition based on Nickel, Chromium, with white areas of Rhenium. The wear rate of the coating is significantly lower than the wear rate of 16Mo3 steel. The average values of indentation modulus and hardness were EIT = 237.6 GPa and HIT = 6.3 GPa, respectively.

HVOF, mechanical properties of NiCrRe, NiCrRe coating

This paper presents a numerical and experimental analysis of manufacturing of intermetallic ceramic composites by powder metallurgy techniques. The scope of the paper includes the formulation and development of an original numerical model of powder metallurgy of two-phase material within the framework of the discrete element method, simulations of powder metallurgy processes for different combinations of process parameters, and a verification of the numerical model based on own experimental results. Intermetallic-based composite NiAl–Al2O3 has been selected as representative material for experimental and numerical studies in this investigation. Special emphasis was given to the interactions between the intermetallic and ceramic particles by formulating the special model for adhesive contact bond. In order to properly represent a real microstructure of a two-phase sintered body, a discrete element specimen was generated using a special algorithm. Numerical validation showed the correct numerical representation of a sintered two-phase composite specimen. Finally, micromechanical analysis was performed to explain the macroscopic behavior of the sintered sample. The evolution of the coordination number, a number of equilibrium contacts, and the distribution of the cohesive neck size with respect to time are presented.

powder metallurgy, sintering, discrete element method, modeling, intermetallic matrix composites

The presented research investigation comprises the study of the mechanical properties of modified copper–silicon carbide composites at the micro- and macroscopic scale. The improvement of a copper–silicon carbide composite refers to the addition of a protective layer at the ceramic reinforcement in order to prevent the dissolution of silicon in the copper matrix. The macromechanical behaviour has been evaluated by the performance in a small punch test. The investigation has been carried out with samples with varying volume content of ceramic reinforcement and different protective layers of the silicon carbide particles. Moreover, the influence of temperature during the strength test has been studied. Next, the results have been referred to the interfacial bonding strength of Cu and SiC particles. SEM characterization of samples has been performed to link the composites' microstructure with the mechanical behaviour. Finally, the experimental results of the small punch test have been predicted via a numerical approach. Finite element analysis has been employed to reproduce the response of the composite specimen during the test. Satisfactory agreement with the experimental curve has been obtained.

metal matrix composites, silicon carbide, metallic layers deposition, small punch, interface strength, finite element method

This investigation examines the problem of homogenization in metal matrix composites (MMCs) and the methods of increasing their strength using severe plastic deformation (SPD). In this research MMCs of pure copper and silicon carbide were synthesized by spark plasma sintering (SPS) and then further processed via high-pressure torsion (HPT). The microstructures in the sintered and in the deformed materials were investigated using Scanning Electron Microscopy (SEM) and Scanning Transmission Electron Microscopy (STEM). The mechanical properties were evaluated in microhardness tests and in tensile testing. The thermal conductivity of the composites was measured with the use of a laser pulse technique. Microstructural analysis revealed that HPT processing leads to an improved densification of the SPS-produced composites with significant grain refinement in the copper matrix and with fragmentation of the SiC particles and their homogeneous distribution in the copper matrix. The HPT processing of Cu and the Cu–SiC samples enhanced their mechanical properties at the expense of limiting their plasticity. Processing by HPT also had a major influence on the thermal conductivity of materials. It is demonstrated that the deformed samples exhibit higher thermal conductivity than the initial coarse-grained samples.

copper, silicon carbide, high-pressure torsion, spark plasma sintering, thermal conductivity

The study presents a detailed analysis of the impact of the coating type of silicon carbide particles and its share by volume on the microstructure and micromechanical properties of Cu-SiC composites. In order to protect the carbide from decomposition during the manufacturing of the composites, the surface of SiC was modified via a plasma vapour deposition technique with a layer of metals (W, Cr, Ti and Ni). Composites with a variable share of the ceramic phase (10–50 %vol.) were obtained at a temperature of 950 °C using spark plasma sintering. An analysis of the structures of the composites, especially in the metal-ceramic boundary region, was conducted with the use of scanning and transmission electron microscopy. The mechanical properties of the composites in the Cu-interface-SiC system were studied via a nanoindentation technique. The comparison of the results of hardness and Young's modulus studies were completed in relation to the actual structures of the materials, which in turn made it possible to determine the impact of the interfacial structure on the global properties of the composite materials.

copper-silicon carbide composites, nanoindentation, SPS, interface study

The performance of the present-day scanning electron microscopy (SEM) extends far beyond delivering electronic images of the surface topography. Oxide dispersion strengthened (ODS) steel is on of the most promising materials for the future nuclear fusion reactor because of its good radiation resistance, and higher operation temperature up to 750°C. The microstructure of ODS should not exceed tens of nm, therefore there is a strong need in a fast and reliable technique for their characterization. In this work, the results of low-kV SEM characterization of nanoprecipitates formed in the ODS matrix are presented. Application of highly sensitive photo-diode BSE detector in SEM imaging allowed for the registration of single nm-sized precipitates in the vicinity of the ODS alloys. The composition of the precipitates has been confirmed by TEM-EDS.

ODS steels, scanning electron microscopy, spark plasma sintering

The purpose of this paper is to elaborate on mechanical alloying conditions for a composite powder consisting of copper and brittle aluminium oxides. Detailed analysis of the Cu-Al2O3 powder mixture structure obtained in the mechanical alloying process allows for the study of the homogenization phenomena and for obtaining grains (in composite form) with a high degree of uniformity. The Cu-5 vol.%Al2O3 composites were obtained by means of the spark plasma sintering technique. The results presented herein were studied and discussed interms of the impact of using a different form of aluminium oxide powder and a different shape of copper powder on composite properties. Research methodology included microstructure analysis as well as its relation to the strength of Cu-Al2O3 interfaces. It transpires from the results presented below that the application of electrocor undum as a reinforcement phase in composites decreases poro sity in the ceramic phase, thus improving thermal properties and interfacial strength.

metal matrix composites, spark plasma sintering, thermal conductivity, interfacial strength

graphene, liquid Cu, Raman spectroscopy, reactivity, sessile drop, wettability

Wettability between liquid Ag and graphene-coated SiC single crystal has been investigated by dispensed drop method at T = 970 oC under vacuum accompanied with subsecond recording of the drop/substrate images (100 frames per second) by high-speed high-resolution CCD camera. Non-contact heating method coupled with capillary purification of the Ag drop procedure has been applied. Scanning electron microscopy combined with EDS analysis and scanning probe microscopy combined with Raman spectroscopy techniques has been utilized for microstructure and surface characterization of samples before and after high-temperature wetting tests. Immediately after its detachment from the capillary, the Ag drop showed non-wetting behavior (h > 90o) forming a high contact angle of h = 114o. Surface characterization of the drop surface after wettability tests evidenced the presence of graphene and Si transferred from the substrate to the top of Ag drop. These findings suggest chemical interaction phenomena occurring at the interface. Locally, an intimate contact between liquid Ag and SiC substrate was allowed by the appearance of discontinuities in the graphene layer basically produced by thermomechanical stress. Local dissolution of carbon into liquid Ag and its reorganization (by segregation, nucleation and growth) as secondary graphene layer at the Ag surface was also observed.

Ag/graphene, Ag/SiC, dispensed drop, sessile drop method, wetting at high temperature

Cu-SiC composites are very promising materials which have high thermal and electrical conductivity and may find many applications. Unfortunately, the main disadvantage of these materials is the dissolution of silicon in copper at elevated temperature, which significantly reduces their properties. In order to overcome this problem particles can be coated with a protective material before sintering. In this paper– the influence of three different metallic coatings on bonding strength were investigated. SiC particles were coated with tungsten, chromium or titanium. As reference a material with uncoated particles was prepared. The experiments were carried out with the use of microtensile tester. The highest increase in strength was observed in the case of chromium coating. On the other hand, the titanium coating, which was of very poor quality, decrease the bonding strength in comparison with uncoated particles. Furthermore, scanning electron and optical microscopes were used to determine the mechanism of debonding.

interfacial bonding strength, metal matrix composites, tensile strength, silicon carbide particles

In the presented paper a coating of SiC particles with a metallic layer were used to prepare copper matrix composite materials. The role of the layer was to protect the silicon carbide from decomposition and dissolution of silicon in the copper matrix during the sintering process. The SiC particles were covered by chromium, tungsten and titanium using Plasma Vapour Deposition method. After powder mixing of components, the final densification process via Spark Plasma Sintering (SPS) method at temperature 950C was provided. The almost fully dense materials were obtained (> 97.5%). The microstructure of obtained composites was studied using scanning electron microscopy as well as transmission electron microscopy. The microstructural analysis of composites confirmed that regardless of the type of deposited material, there is no evidence for decomposition process of silicon carbide in copper. In order to measure the strength of the interface between ceramic particles and the metal matrix, the micro tensile tests have been performed. Furthermore, thermal diffusivity was measured with the use of the laser pulse technique. In the context of performed studies, the tungsten coating seems to be the most promising solution for heat sink application. Compared to pure composites without metallic layer, Cu-SiC with W coating indicate the higher tensile strength and thermal diffusitivy, irrespective of an amount of SiC reinforcement. The improvement of the composite properties is related to advantageous condition of Cu-SiC interface characterized by well homogenity and low porosity, as well as individual properties of the tungsten coating material.

metal matrix composites, silicon carbide, metallic layers deposition, thermal conductovity, interface strength

This paper presents the numerical and experimental analysis of hot pressing of NiAl powder with an emphasis on the best possible representation of its main stages: initial powder compaction and pressure-assisted sintering. The numerical study has been performed within the discrete element framework. In the paper, an original viscoelastic model of hot pressing has been used. In order to ensure that the applied values of material parameters in numerical simulations are appropriate, the reference literature has been reviewed. It produced the relations and equations to estimate the values of all required sintering material parameters of the considered viscoelastic model. Numerical simulations have employed the geometrical model of the initial dense specimen generated by a special algorithm which uses the real grain distribution of powder. The numerical model has been calibrated and validated through simulations of the real process of hot pressing of intermetallic NiAl material. The kinetics of compaction, sintering and cooling stage indicated by the evolution of density, shrinkage and densification rate have been studied. The comparison of numerical and experimental results has shown a good performance of the developed numerical model.

Powder metallurgy, Hot pressing, Sintering, Simulation, Discrete element method, Nickel aluminide

This paper presents the numerical modelling of initial powder compaction and pressure-assisted sintering performed by original viscoelastic discrete element model. The research is focused on the influence of the type of the model representing an elastic part of interparticle force. Two elastic contact models—linear and nonlinear Hertz model—have been implemented and used to analyse interaction of NiAl powder particles during compaction and sintering process. Numerical models have been validated using own experimental results. Microscopic effects (particle penetration) and macroscopic changes (relative density) have been compared. It has been shown that although both models represent properly macroscopic behaviour of the material at the sintering process, the Hertz model produces the results closer to the real experimental ones during the initial compaction stage. Evaluation of macroscopic quantities enables implementation of the discrete element model in the framework of the multiscale modelling framework which is currently developed for sintering processes.

powder metallurgy, sintering, initial compaction, elasticity, discrete element method

This paper analyses the technological aspects of the interface formation in the copper-silicon carbide composite and its effect on the material's microstructure and properties. Cu-SiC composites with two different volume content of ceramic reinforcement were fabricated by hot pressing (HP) and spark plasma sintering (SPS) technique. In order to protect SiC surface from its decomposition, the powder was coated with a thin tungsten layer using plasma vapour deposition (PVD) method. Microstructural analyses provided by scanning electron microscopy revealed the significant differences at metal-ceramic interface. Adhesion force and fracture strength of the interface between SiC particles and copper matrix were measured. Thermal conductivity of composites was determined using laser flash method. The obtained results are discussed with reference to changes in the area of metal-ceramic boundary.

copper matrix composites, silicon carbide, interface, thermal conductivity, adhesion

This paper describes the process of obtaining Cu-SiC-Cu systems by way of spark plasma sintering. A monocrystalline form of silicon carbide (6H-SiC type) was applied in the experiment. Additionally, silicon carbide samples were covered with a layer of tungsten and molybdenum using chemical vapour deposition (CVD) technique. Microstructural examinations and thermal properties measurements were performed. A special attention was put to the metal-ceramic interface. During annealing at a high temperature, copper reacts with silicon carbide. To prevent the decomposition of silicon carbide two types of coating (tungsten and molybdenum) were applied. The effect of covering SiC with the aforementioned elements on the composite's thermal conductivity was analyzed. Results were compared with the numerical modelling of heat transfer in Cu-SiC-Cu systems. Certain possible reasons behind differences in measurements and modelling results were discussed.

copper matrix composites, silicon carbide, interface, thermal conductivity, modelling

Antimony telluride (Sb2Te3) is an intermetallic compound crystallizing in a hexagonal lattice with R-3m space group. It creates a c lose packed structure of an ABCABC type. As intrinsic semiconductor characterized by excellent electrical properties, Sb2Te3 is widely used as a low-temperature thermoelectric material. At the same time, due to unusual properties (strictly connected with the structure), antimony telluride exhibits nonlinear optical properties, including saturable absorption. Nanostructurization, elemental doping and possibilities of synthesis Sb2Te3 in various forms (polycrystalline, single crystal or thin film) are the most promising methods for improving thermoelectric properties of Sb2Te3.Applications of Sb2Te3 in optical devices (e.g. nonlinear modulator, in particular saturable absorbers for ultrafast lasers) are also interesting. The antimony telluride in form of bulk polycrystals and layers for thermoelectric and optoelectronic applications respectively were used. For optical applications thin layers of the material were formed and studied. Synthesis and structural characterization of Sb2Te3 were also presented here. The anisotropy (packed structure) and its influence on thermoelectric properties have been performed. Furthermore, preparation and characterization of Sb2Te3 thin films for optical uses have been also made

antimony telluride, thermoelectric materials, thin films, PVD magnetron sputtering, topological insulator

The presented paper investigates the relationship between the microstructure and thermal properties of copper–silicon carbide composites obtained through hot pressing (HP) and spark plasma sintering (SPS) techniques. The microstructural analysis showed a better densification in the case of composites sintered in the SPS process. TEM investigations revealed the presence of silicon in the area of metallic matrix in the region close to metal ceramic boundary. It is the product of silicon dissolving process in copper occurring at an elevated temperature. The Cu-SiC interface is significantly defected in composites obtained through the hot pressing method, which has a major influence on the thermal conductivity of materials.

metal matrix composites, silicon carbide, interface, spark plasma sintering, thermal conductivity

A two-scale modeling framework for sintering processes has been presented. Formulation of the micromechanical model of sintering developed in the discrete element method and basic relationships in the macroscopic model of sintering have been briefly reviewed. The methodology to determine macroscopic quantities–stress, strains, and constitutive viscous properties-from the discrete element simulations has been presented. This methodology has been applied to modeling of NiAl sintering. First, the discrete element model (DEM) has been calibrated by fitting the numerical densification curve to the experimental data. The DEM model with calibrated parameters has been used in simulations specially conceived to give macroscopic viscous moduli of the sintered material. Using the averaging procedures macroscopic stresses and strains have been calculated. Strain rates have been obtained differentiating the strain curves with respect to time. Finally, the viscous constitutive properties of the sintered material have been determined. The dependence of the shear and volumetric viscous moduli on the relative density (or equivalently) on the porosity has been obtained. It has been found that the numerical simulations predict a similar dependence as that assumed in the phenomenological macroscopic models. Thus, the validity of the micro-macro relationships obtained from the discrete element simulations of powder sintering has been confirmed. The proposed methodology allows us to use the discrete element model in the framework of multiscale modeling of sintering.

discrete element method, sintering, simulation, micro-macro relationships, multiscale modeling

This paper constitutes an analysis of the effect of heat treatment time on the properties of Cr-Re-Al2O3 composite materials. It was found that as a result of sintering, rhenium is dissolved in chromium to create chromium-rhenium solid solution. This process is time-dependent, therefore as the time extends, the structure of material becomes homogenous, which improves its mechanical properties. Within the frame of herein presented studies, a series of technological tests have been carried out for a constant sintering temperature (1450°C) and pressure (30 MPa), with the use of a variable holding time in the maximum temperature. As a result, changes in the structure of Crsingle bondRe matrix have been determined and the resulting changes in the properties of composite. Based on those tests, optimal conditions of the sintering process have been determined from the point of view of obtaining a homogenous structure and the most beneficial properties of Cr-Re-Al2O3 composites.

Metal-matrix composites (MMCs), Mechanical properties, Mechanical testing, Sintering

In this paper the results of numerical simulations and experimental studies are presented which describe potential and limitation of applications of single-layer (SLG) and multi-layer (MLG) graphene for thermal conductivity enhancement (TCE) of copper. A series of composite structures were studied which are representative of most widely used systems. The influence of structural parameters on the macroscopic thermal conductivity was analyzed, both experimentally and by numerical simulations. Analytical and Finite Element Method modeling were carried out to investigate a wide range of phenomena, including the effect of copper-MLG interface, copper grain size, volume fraction, thickness and orientation of MLG platelets as well as spatial distribution of MLG defined by percolation factor. Both modeling and the experimental results show that the volume fraction of MLG regions, their size, orientation and spatial distribution may significantly affect the thermal conductivity of metal matrix composites. TCE can be obtained for the laminate-like structure or particulate composites with highly aligned MLG regions. The thermal conductivity of such composites is strongly anisotropic and enhanced in the direction perpendicular to the layers. The results obtained in this study predict that SLG will have a negative effect on the thermal conductivity of copper matrix composites.

Thermal conductivity, Composites, Graphene, Finite element method

Dense chromium–alumina composites doped with rhenium have been developed by the hot pressing method (bulk composite) and plasma spraying (composite coating). The obtained materials show superior mechanical properties, insensitivity to chemically aggressive environment, good resistance to frictional wear and oxidation at elevated temperature. These enhanced properties make the Cr/Re/Al2O3 composites interesting structural materials for energy and transport applications operating in demanding service conditions, e.g. fluidal boilers in power plants or valve seats in combustion engines.

Metal–ceramic composites, Powder technology, Mechanical properties, Coatings

This paper comprises the results of studies of the changes in the structure of Cr-Re-Al2O3 metal matrix depending on heat treatment time in sintering temperature. The density of material with the following composition: 95%(75%Cr-25%Al2O3)+5%Re was increased using the technique of sintering under pressure (30MPa) at the temperature of 1450°C. As a result, materials characterized by a high relative density (< 97% of theoretical density) were obtained. Next, they were subjected to structural tests including scanning and transmission electron microscopy as well as X-ray diffraction. Changes in the phase composition, grains size and parameters of crystallographic structure depending on heat treatment time were analysed. It was found that during sintering rhenium is dissolved in the chromium matrix and Cr-Re solid solution is formed. When sintering time is extended to 120 min, the matrix of the composite becomes completely homogenous, which results in an increased strength of the composite.

Metal matrix composites, Rhenium, Hot pressing, Microstructure analysis, XRD

Combination of extreme service conditions and complex thermomechanical loadings, e.g., in electronics or power industry, requires using advanced materials with unique properties. Dissipation of heat generated during the operation of high-power electronic elements is crucial from the point of view of their efficiency. Good cooling conditions can be guaranteed, for instance, with materials of very high thermal conductivity and low thermal expansion coefficient, and by designing the heat dissipation system in an accurate manner. Conventional materials such as silver, copper, or their alloys, often fail to meet such severe requirements. This paper discusses the results of investigations connected with Cu-C (multiwall carbon nanotubes (MWNTs), graphene nanopowder (GNP), or thermally reduced graphene oxide (RGO)) composites, produced using the spark plasma sintering technique. The obtained composites are characterized by uniform distribution of a carbon phase and high relative density. Compared with pure copper, developed materials are characterized by similar thermal conductivity and much lower values of thermal expansion coefficient. The most promising materials to use as heat dissipation elements seems to be copper-based composites reinforced by carbon nanotubes (CNTs) and GNP.

copper matrix composites, graphene, spark plasma sintering, thermal properties

This study investigated the influence of the particle size on the adhesion force between ceramic particles and metal matrix in ceramic-reinforced metal matrix composites. The Cu-Al2O3 composites with 5 vol.% of ceramic phase were prepared by a powder metallurgy process. Alumina oxide powder as an electrocorundum (Al2O3) powder with different particle sizes, i.e., fine powder <3 µm and coarse powder of 180 µm was used as a reinforcement. Microstructural investigations included analyses using scanning electron microscopy with an integrated EDS microanalysis system and transmission microscopy. In order to measure the adhesion force (interface strength), we prepared the microwires made of the investigated materials and carried out the experiments with the use of the self-made tensile tester. We have observed that the interface strength is higher for the sample with coarse particles and is equal to 74 ± 4 MPa and it is equal to 68 ± 3 MPa for the sample with fine ceramic particles.

adhesion, interface strength, metal matrix composites, nanocomposites, tensile test

Functionally graded materials (FGMs) belong to a new, continuously developing group of materials, finding application in various branches of industry. The idea of freely designing their construction profile, restricted only by the available manufacturing techniques, enables obtaining materials with composition and structure gradients having unprecedented properties. In this paper, selected results of works carried out by the authors and relating to the application of the developed metal-ceramic composites were presented in order to manufacture functionally graded materials for target purposes. Gradient structures with various construction profiles that can play different roles were produced on the basis on the following material pairs: Cr-Al2O3, NiAl-Al2O3 and Cu-AlN. Manufacturing conditions, microstructure characteristics and selected properties, crucial from the point of view of future applications, were presented.

metal-ceramic functionally graded materials, manufacturing, characterization, application

W niniejszym artykule zaprezentowano wyniki modelowania zagęszczania proszku stanowiącego wstępny etap procesu prasowania na gorąco. Modelowanie numeryczne zrealizowano metodą elementów dyskretnych z wykorzystaniem kulistych cząstek. Analizę skoncentrowano na badaniu mechanizmów zagęszczania proszku przy ciśnieniu do 50 MPa oraz poszukiwaniu modeli odpowiednich przy zastosowanych warunkach realizacji procesu. Symulacje numeryczne wykonano wykorzystując dwa modele oddziaływania cząstek proszku: sprężysty model Hertza-Mindlina-Deresiewicza oraz plastyczny model Storåkersa. Wyniki numeryczne zostały porównane z wynikami laboratoryjnymi prasowania proszku NiAl. Otrzymano dużą zgodność wyników eksperymentalnych i numerycznych.

This paper presents the results of discrete element simulation of powder compaction which is the initial stage in the hot pressing process. Numerical simulation has been performed by discrete element method with using spherical particles. The research has been focused on densification mechanisms under pressure 50 MPa and models appropriate for these conditions. Numerical simulations have been carried out for two contact models: elastic Hertz-Mindlin-Deresiewicz and plastic - Storåkers. Numerical results and results from laboratory test of the uniaxial pressing of NiAl powder have been compared. The obtained results of numerical simulation and laboratory tests showing a good agreement.

metoda elementów dyskretnych, prasowanie proszków, materiały intermetaliczne, discrete element method, powder compaction, intermetallics

This paper presents numerical studies of powder compaction in cold uniaxial pressing. The powder compaction in this work is considered as an initial stage of a hot pressing process so it is realized with relatively low pressure (up to 50 MPa). Hence the attention has been focused on the densification mechanisms at this range of pressure and models suitable for these conditions. The discrete element method employing spherical particles has been used in the numerical studies. Numerical simulations have been performed for two different contact models—the elastic Hertz–Mindlin–Deresiewicz model and the plastic Storåkers model. Numerical results have been compared with the results of laboratory tests of the die compaction of the NiAl powder. Comparisons have shown that the discrete element method is capable to represent properly the densification mechanisms by the particle rearrangement and particle deformation.

Discrete element method, Simulation, Powder compaction, Cold uniaxial pressing

This paper presents the method for measurement of the adhesion force and fracture strength of the interface between ceramic particles and metal matrix in ceramic reinforced-metal matrix composites. Three samples with the following Cu to Al2O3 ratio (in vol.%) were prepared: 98.0Cu/2.0Al2O3, 95.0Cu/5.0Al2O3 and 90Cu/10Al2O3. Furthermore, microwires which contain a few ceramic particles were produced by means of electro etching. The microwires with clearly exposed interface were tested with use of the microtensile tester. The microwires usually break exactly at the interface between the metal matrix and ceramic particle. The force and the interface area were carefully measured and then the fracture strength of the interface was determined. The strength of the interface between ceramic particle and metal matrix was equal to 59 ± 8 MPa and 59 ± 11 MPa in the case of 2% and 5% Al2O3 to Cu ratio, respectively. On the other hand, it was significantly lower (38 ± 5 MPa) for the wires made of composite with 10% Al2O3.

Nanocomposites, Metal matrix composites, Adhesion, Interface

Evolution of the density and the microstructure during hot pressing of NiAl/Al2O3 composite has been investigated in the present paper. In particular, the effect of the process parameters, viz. compacting pressure, sintering temperature and sintering time, on the evolution of the density of the intermetallic–ceramic composite has been studied. Evolution of the density has been related to microstructure changing. Porosity, pore structures and grains rearrangement have been analysed in microscopic observations.

hot pressing, sintering, intermetallic–ceramic composite, density evolution, microstructure

This paper presents investigation of macroscopic stresses in powder metallurgy process modelled with the discrete element method. The discrete element model belongs to the class of micromechanical models. In the DEM model the material is represented by an assembly of particles interacting by contact forces and the method is formulated in terms of forces and displacements. In order to evaluate macroscopic stresses a special upscaling procedure is necessary. The paper presents basic formulation of the discrete element method with special attention for the contact interaction models for powder compaction and sintering. A method to evaluate macroscopic stresses based on the two level averaging is presented. The discrete element model of sintering is verified using own experimental results. Macroscopic stresses are calculated for the whole process including loading, heating, sintering, cooling and unloading. It has been found out that the macroscopic stresses are consistent with changing process parameters. The procedure is suitable for multiscale modelling of sintering.

sintering, modeling, discrete element method, macroscopic stresses

In this paper we present the results of experimental measurements and numerical modeling of the effect of particle size on the residual thermal stresses arising in sintered metal–matrix composites after cooling down from the fabrication temperature. On example of novel Cr(Re)/Al2O3 composites processed by (i) spark plasma sintering and (ii) hot pressing the residual thermal stresses are measured by neutron diffraction technique and determined by a FEM model based on micro-CT scans of the material microstructure. Then numerical model of microcracking induced by residual stresses is applied to predict the effective Young modulus of the damaged composite. Comparison of the numerical results with the measured data of the residual stresses and Young’s modulus is presented and fairly good agreement is noted.

Metal–matrix composites (MMC), Residual/internal stress, Finite element analysis (FEA), Sintering

The influence of hot pressing conditions on mechanical properties of nickel aluminide/alumina composite has been investigated in the present paper. In particular, effect of the process parameters, viz. compacting pressure, sintering temperature and sintering time on the evolution of density, elastic constants and tensile strength properties of the intermetallic-ceramic composite has been studied. Elastic constants, the Young's modulus and Poisson's ratio, have been evaluated using an ultrasonic testing method, and the tensile strength has been determined by a Brazilian-type splitting test. Microscopic observations of microstructure evolution complemented the experimental procedure. Experimental results have been confronted with theoretical models showing a good agreement between the data compared.

Hot pressing, sintering, intermetallic-ceramic composite, elastic properties, Brazilian test, tensile strength, ultrasonic method

Chromium–alumina composites are well known for their good mechanical properties in comparison to pure ceramics or metals. These composites are characterized by high hardness and high mechanical strength. The aim of the present work was to improve the properties of chromium–alumina composites even more and expand the range of their possible applications by addition of rhenium. To achieve this goal, chromium–alumina composites containing 2 and 5 vol.% of rhenium were produced via powder metallurgy. The microstructural characterization of the processed material was performed using light microscopy, scanning and transmission electron microscopy as well as X-ray diffraction analysis. Measurement of selected properties such as Young's modulus, bend strength and hardness revealed an advantageous influence of rhenium additions. The results are discussed in terms of the influence of rhenium volume content on the microstructure and on the physical and mechanical properties of the chromium–alumina composites. The solid solution is only partially formed. The properties strongly depend on the amount and distribution of both aluminium oxide and rhenium content.

It is commonly known that the properties of sintered materials are strongly related to technological conditions of the densification process. This paper shows the sintering behavior of a NiAl-Al2O3 composite, and its individual components sintered separately. Each kind of material was processed via the powder metallurgy route (hot pressing). The progress of sintering at different stages of the process was tested. Changes in the microstructure were examined using scanning and transmission electron microscopy. Metal-ceramics interface was clean and no additional phases were detected. Correlation between the microstructure, density, and mechanical properties of the sintered materials was analyzed. The values of elastic constants of NiAl/Al2O3 were close to intermetallic ones due to the volume content of the NiAl phase particularly at low densities, where small alumina particles had no impact on the composite’s stiffness. The influence of the external pressure of 30 MPa seemed crucial for obtaining satisfactory stiffness for three kinds of the studied materials which were characterized by a high dense microstructure with a low number of isolated spherical pores.

ceramics, composites, electron, intermetallic, metallic matrix, microscopy, powder metallurgy, sintering, structural

This paper presents an original viscoelastic model of powder sintering developed within the discrete element framework. The viscous model used by other authors has been enriched by adding a spring connected in series to the viscous rheological element. In this way elastic and viscous effects in the particle interaction during sintering are treated using the Maxwell viscoelasticity. The new numerical model has been verified through simulation of simple problems of free sintering and sintering under pressure. Sintering processes have been treated as isothermic. In order to accelerate the analysis an algorithmic mass scaling has been used allowing to use larger time steps in the explicit time integration scheme. The results obtained using the new model are consistent with the standard viscous model. At the same time, a much better efficiency of the new model in comparison to the standard viscous one has been found because the critical time steps required by the viscoelastic model are much larger than those required by the viscous model. The new model has been applied to the simulation of real process of sintering of NiAl powder. The kinetics of sintering indicated by the evolution of density has been studied. The comparison of numerical and experimental results has shown a good performance of the developed numerical model.

Powder sintering, Simulation, Discrete element method, Viscoelastic model

Copper-based composites could be widely used in automotive, electronic or electrical industry due to their very promising thermal properties. In the present paper, Cu-AlN metal matrix composites with ceramic volume fractions between 0.1 and 0.4 were fabricated by hot pressing method in vacuum. Dependence of the coefficient of thermal expansion (CTE) and the thermal conductivity (TC) on the chemical composition of composites has been investigated. The measured values of the thermal expansion coefficient have been compared with the analytical models’ predictions. A numerical model based on FEAP 7.5 in 3D space has been used to evaluate the influence of the porosity on the thermal properties (thermal conductivity) of the composite. A fairly good correlation between the FEM results and the experimental measurements has been obtained.

thermal properties, porosity, copper-based composites

Celem pracy było zbadanie wpływu dodatku renu na właściwości termomechaniczne i użytkowe kompozytów Cr-Al2O3 wytwarzanych metodą spiekania pod ciśnieniem w prasie HP oraz metodą Spark Plasma Sintering (SPS). Uzyskano kompozyty o gęstości przekraczającej 98% gęstości teoretycznej. Właściwości mechaniczne (m.in. moduł Younga, wytrzymałość na zginanie, twardość, odporność na pękanie, granica plastycznośći) oraz odporność na utlenianie wytworzonych materiałów są obiecujące. Zbudowano model numeryczny do obliczeń wielkości naprężeń resztkowych obecnych w materiałach faz kompozytu po procesie spiekania oraz modułów sprężystości. Wykorzystano w tym celu obrazy rzeczywistej mikrostruktury kompozytu otrzymane z tomografii komputerowej. Uzyskano dobrą zgodność wyników modelu z wynikami pomiarów naprężeń metodą XRD. Przedstawiono ponadto porównanie wyników obliczeń numerycznych i pomiarów modułu Younga przy zastosowaniu różnych metod

kompozyty MMC, metalurgia proszków, modelowanie MES, mikrotomografia komputerowa, naprężenia resztkowe

This paper presents numerical simulation of powder sintering. The numerical model introduced in this work employs the discrete element method which assumes that material can be modelled by a large assembly of discrete elements (particles) of spherical shape interacting among one another. Modelling of sintering requires introduction of the cohesive interaction among particles representing interparticle sintering forces. Numerical studies of sintering have been combined with experimental studies which provided data for calibration and validation of the model. In the laboratory tests evolution of microstructure and density during sintering have been studied. Comparison of numerical and experimental results shows a good performance of the numerical model developed

Powder Sintering, Simulation, Discrete Element Method

Thermal stresses induced during the cooling of Cr–Al2O3 (MMC) processed by sintering are modeled numerically using the FEA. The composite microstructure is modeled as (i) random distribution of ceramic particles (voxels) in the metal matrix, and (ii) using micro-CT scans of the real microstructure transformed into a FE mesh. Numerical simulations of the thermal residual stresses are compared with the test data measured by X-ray diffraction. A simple numerical model is then proposed to predict the overall elastic properties of the composite with account of the porosity and damage induced by the thermal stresses. Comparison of the model predictions with the measured data for Young’s modulus is presented.

Metal-matrix composites (MMCs), Residual/internal stress, Finite element analysis (FEA), Sintering

W niniejszym artykule zostały przedstawione nowe wyniki modelowania procesu spiekania metodą elementów dyskretnych. W sformułowaniu teoretycznym dla części sprężystej zastosowano model kontaktu Hertza w celu lepszego odwzorowania oddziaływania elementów kulistych w trakcie prasowania. Sformułowanie i implementację modelu rozszerzono na przypadek spiekania materiałów dwufazowych. Na podstawie badań literaturowych wyznaczono parametry materiałowe procesu, które zostały następnie zweryfikowane za pomocą wyników eksperymentalnych. Wyniki numeryczne ewolucji gęstości próbki porównano z wynikami doświadczalnymi otrzymując dużą zgodność.

materiały dwufazowe, metalurgia proszków, spiekanie, metoda elementów dyskretnych

This paper presents numerical modelling of powder sintering. The numerical model introduced in this work employs the discrete element method which assumes that material can be modelled by a large assembly of discrete elements (particles) of spherical shape interacting among one another. Modelling of sintering requires introduction of the cohesive interaction among particles representing inter-particle sintering forces. Numerical studies of sintering have been supplemented with experimental studies which provided data for calibration and validation of the model. In the laboratory tests evolution of microstructure and density during sintering have been studied. Comparison of numerical and experimental results shows a good performance of the numerical model developed.

powder sintering, powder metallurgy, simulation, discrete element method

This work is focused on the modeling of thermal stresses induced during the fabrication of the metal/ceramic composites. On example of Cr-Al2O3 composite processed by powder metallurgy, thermal stresses after fabrication are determined by FEM model for different contents of metal and ceramic phases. Numerical model of microcracking induced by thermal stresses is then proposed and applied to compute the overall elastic properties of the damaged composite. Comparison of the model predictions with the measur ed data for Young's modulus is presented.

Cr-Al2O3 composite, mechanical properties, thermal stress modeling, microcracking, Young’s modulus modeling

Heat transfer by conduction is involved in the use of heat sinks dissipitating heat from electronic devices. Effective transfer of heat requires using materials of high thermal conductivity. In addition, it requires appropriate values of thermal expansion, matched to the semiconductor materials, high purity of materials used and good contact between bonded elements across which heat transfer occurs. The conventional materials are not able to fulfil still raising and complex requirements. The solutions of this problem could be using the composites materials, where the combinations of different properties is possible to use. This study presents the technological tests and the analysis of correlation between processing parameters and the properties of copperaluminium nitride composites. Composite materials were obtained by mixing in planetary ball mill and then densified using the sintering under pressure or hot pressing method. The microstructure of obtained composite materials using optical microscopy and scanning electron microscopy were analyzed. Coefficient of thermal expansion (CTE) and thermal conductivity (TC) were investigated depending on the process conditions

Composite Material, Hot-Pressing, Sintering, Thermal Conductivity (TC), Thermal Diffusivity, Thermal Expansion Coefficient

The development of technologies for joining advanced materials is connected with an introduction of new materials and new applications of their bonds, to work in ever more difficult conditions. One of possibilities of obtaining this type of joints is using the friction welding technique. This paper presents the results of joining intermetallics (Fe-Al and Ni-Al type) with steel (S235JR) and ceramics (Al2O3) using friction welding technique. The focus of the investigations was selecting: appropriate rotational speed (10000-25000rpm) of joining elements, welding pressure and time (1500-4500ms) of its application and swelling time (1000-7000ms). The paper presents the results of microstructure investigations, investigations of microhardness (perpendicularly to joint surface) and mechanical properties (tensile strength).

friction welding, intermetallics, microstructure of joints, microhardness, tensile strength

Alumina/copper composites have been used where high thermal conductivity, high absorption and dissipation of heat, high resistance to thermal fatigue and good frictional wear resistance are required. This kind of composites may be applied in medicine, electronic and automotive industry. Both the physical and mechanical properties of this type of composites are strongly influenced by the properties of its individual constituents and, also, by the properties of interface layer between ceramic and metal. One of the solution, from the point of view of the best properties’ achievements (especially thermal, structural and shape stability), is the production of ceramic-metal composites with interpenetrating networks structure. They can be produced using porous alumina performs, which are infiltrated (pressure or pressureless) by molten metal or sintered with metallic powders. The subject of the presented paper is the development of the interpenetrating network Al2O3-Cu composites, processed by sintering porous ceramic perform (85 and 90% porosity) with copper powder. The paper presents the new developed technology, results of microstructure investigations, measurements of the selected physical and mechanical properties and the analysis of the influence of the processing conditions on the properties and interface morphology between ceramic and copper

W artykule przedstawiono badania doświadczalne oraz modelowanie numeryczne procesu spiekania proszków metalicznych. W części eksperymentalnej pracy badano ewolucję mikrostruktury oraz gęstości spieku w trakcie procesu spiekania. Jako metodę modelowania wybrano metodę elementów dyskretnych, w której zakłada się, że materiał jest reprezentowany przez liczny zbiór elementów dyskretnych (cząstek) o kształcie sferycznym oddziałujących między sobą. Modelowanie spiekania wymaga wprowadzenia oddziaływania kohezyjnego między cząstkami reprezentującego naprężenia powstające między ziarnami w trakcie spiekania. W artykule przedstawiono wstępne wyniki numeryczne pokazujące ewolucję naprężenia w trakcie spiekania między dwoma ziarnami spiekanego proszku.

spiekanie, metalurgia proszków, związki międzymetaliczne, modelowanie, metoda elementów dyskretnych

In the case of the sintering of composite materials exhibiting mutual solubility, intermediate phases with varying concentrations of elements may appear during the densification process. Microstructural and structural changes, especially in the area of the interface, strongly influence mechanical or thermal properties [1]. A good example of such materials is nickel – silicon carbide composites. At elevated temperatures nickel reacts with silicon carbide, which causes total SiC decomposition, and as a result, new Ni-Si phases are formed and free carbon is precipitated within the reaction zone. In this work, nickel-silicon carbide composites were obtained via the Spark Plasma Sintering method. The detailed microstructural analyses using X-ray diffraction, Raman spectroscopy, scanning electron microscopy and transmission electron microscopy revealed the material’s evolution during sintering. To investigate the correlation between microstructure and properties of obtained materials, the mechanical test at three different length scales (in macro-, micro- and nanoscale) was conducted. To evaluate the strength of Ni-SiC composites at a macroscopic scale the uniaxial tensile and compression tests were employed. The sample deformation and failure mechanism for different stages of sintering were analyzed. The strength of the nickel-silicon carbide interface was determined by bending tests of micro-cantilever beams. Nanoindentation was used to evaluate the hardness of each composite component. The conducted research revealed a strong relation between mechanical strength and sintering conditions.

W niniejszym artykule zaprezentowano wyniki modelowania, zagęszczania proszku stanowiącego wstępny etap procesu prasowania na gorąco, metodą elementów dyskretnych opisaną w [1]. Modelowanie numeryczne zrealizowano metodą elementów dyskretnych, z wykorzystaniem kulistych cząstek. Badania skoncentrowano na mechanizmach zagęszczania proszku przy ciśnieniu 50 MPa oraz modelach odpowiednich przy zastosowanych warunkach procesu. Numeryczne symulacje wykonano z wykorzystaniem dwóch modeli: pierwszy - elastyczny Hertz-Mindlin-Deresiewicz, drugi - plastyczny Storakers, opisanych w pracy [2]. Wyniki symulacji numerycznych zostały porównane z wynikami laboratoryjnymi zagęszczania proszku NiAl w matrycy. W rezultacie otrzymano dużą zgodność wyników eksperymentalnych i numerycznych.

metoda elementów dyskretnych, modelowanie, zagęszczanie proszków, prasowanie

Chromium based composites reinforced with alumina particles combineenhanced thermal, oxidation and wear resistance with mechanical strength and hardness. Because of these valuable properties Cr/Al2O3 composites can be used e.g. in the automotive sector for elements of powertrain. Rhenium due to its good mechanical and thermal properties is primarily used as an admixture of nickel superalloys in the aerospace and chemical industries. In the present paper a powder metallurgy route was used to manufacture dense Cr/Re/Al2O3 bulk composites with rhenium admixture of 2vol% and 5vol%. Composites were processed by hot pressing (HP) and by spark plasma sintering (SPS) techniques. The density of the sintered composites exceeded 98% of the theoretical value. Microstructural characterisation revealed that a solid solution of rhenium in chromium was partially formed. Mechanical properties such as Young’s modulus, bending strength, hardness, plastic limit are promising so are oxidation and corrosion resistance. A numerical FE model was developed for the prediction of thermal residual stresses (TRS) and damage generated in the metal and ceramic phase during cooling from high sintering temperature down to room temperature. The model uses micro-CTimages of the real material microstructure as the input data. A good agreement of the simulation results for TRS and the measurements of by neutron diffraction was achieved. The obtained Cr/Re/Al2O3composites were already tested as demonstrators of valve seats in combustion engines and good preliminary results were reported.

Chromium-alumina MMC, rhenium admixture, powder metallurgy, thermal residual stresses, microCT FEM

This paper presents the method for measurement of the adhesion force and fracture strength of the interface between ceramic particles and metal matrix in ceramic reinforced-metal matrix composites. Three samples with the following Cu to Al 2 O 3 ratio (in vol.%) were prepared: 98.0Cu/2.0Al 2 O 3, 95.0Cu/5.0Al 2 O 3 and 90Cu/10Al 2 O 3. Furthermore, microwires which contain a few ceramic particles were produced by means of electro etching. The microwires with clearly exposed interface were tested with use of the microt ensile tester (Fig. 1). The microtensile tester consists of two stages, to which two endings of the microwire are fixed. The first stage is able to measure force with the precision equal to 0.1 mN. The microwires usually break exactly at the interface between the metal matrix and ceramic particle. The force and the interface area were carefully measured and then the fracture strength of the interface was determined. The strength of the interface between ceramic particle and metal matrix was equal to 59 ±8 MPa and 59±11 MPa in the case of 2% and 5% Al 2 O 3 to Cu ratio, respectively. On the other hand, it was significantly lower (38±5 MPa) for the wires made of composite with 10% Al2O3