Search Results (34)

This paper presents the possibilities of using the reaction sintering method for the production of tool steel used in medicine. The applied method enables the sintering of powders in one technological process. The SPS (spark plasma sintering) process is a technology in which electric pulses generate heat and pressure, which allows for the quick and effective connection of powder particles into a homogeneous material with high density and good mechanical properties. As a result, a product of small dimensions and a precisely defined chemical composition, established at the stage of preparing the powder mixture, is obtained. The advantages of the applied production process are the sintering time and small amounts of post-production waste compared to conventional methods of producing a finished product from steel. The method of producing a semi-finished product is particularly useful in the case of small-scale and small-sized production. The subject of the research was the analysis of the conditions for obtaining X30Cr13 martensitic steel used for the production of surgical instruments. This paper analyzes the effect of sintering temperature and time on sinterability and on selected physical and mechanical properties of the obtained materials. The sintering parameters of the starting mixture have been optimized to obtain the highest possible sinter properties, such as density and hardness. Based on the analysis of the results, it was found that the powder preparation method for the SPS process and the grain size significantly affect the microstructure and mechanical properties of the final product. The optimal sintering parameters for X30Cr13 steel are a temperature of 950 °C and a sintering time of 12 min. Furthermore, the use of the SPS method allows for a reduction in the manufacturing costs of martensitic steel semi-finished products. Full article

The development of thermoelectric modules based on skutterudite materials requires stable, low-resistance interfaces between segments operating at different temperature ranges. This study investigates the microstructure, thermoelectric performance, and thermal stability of the following two joints: In_0.4Co₄Sb₁₂/Co₄Sb_10.8Te_0.6Se_0.6 (n-type) and CeFe₃Co_0.5Ni_0.5Sb₁₂/In_0.25Co₃FeSb₁₂ (p-type), fabricated by pulse plasma sintering (PPS). Scanning electron microscopy (SEM) and energy-dispersive spectroscopy (EDS) analyses confirmed the formation of well-bonded interfaces without pores or cracks. Aging at 773 K for 168 h did not result in morphological or chemical degradation, and phase composition remained unchanged according to X-ray diffraction (XRD). Surface Seebeck coefficient mapping and contact resistance measurements showed negligible changes after annealing, confirming electrical stability. To provide context for potential applications, theoretical energy conversion efficiencies were estimated based on measured thermoelectric properties, yielding 13.2% and 10.1% for the n- and p-type segmented legs, respectively. Additionally, measured coefficients of thermal expansion (CTE) indicated low mismatch between jointed materials, supporting good mechanical compatibility. The results demonstrate that the selected material combinations are thermally, chemically, and electrically stable and can be effectively used in segmented thermoelectric legs for intermediate-temperature applications. Full article

Iron-based superconductors are under study for their potential for high-field applications due to their excellent superconducting properties such as low structural anisotropy, large upper critical fields and low field dependence of the critical current density. Between them, Fe(Se,Te) is simple to be synthesized and can be fabricated as a coated conductor through laser ablation on simple metallic templates. In order to make all the steps simple and fast, we have applied the spark plasma sintering technique to synthesize bulk Fe(Se,Te) to obtain quite dense polycrystals in a very short time. The resulting polycrystals are very well connected and show excellent superconducting properties, with a critical temperature onset of about 16 K. In addition, when used as targets for pulsed laser ablation, good thin films are obtained with a critical current density above 10⁵ A cm⁻² up to 16 T. Full article

This work demonstrates the capabilities and advantages of a novel sintering technique to fabricate bulk composition gradient materials. Pressure distribution calculations were used to compare several tooling geometries for use with current-activated, pressure-assisted densification or spark plasma sintering to densify a gradient along the long dimension of the specimen. The selected rectangular tooling design retains a low aspect ratio to ensure a uniform pressure distribution during consolidation by using a side loading configuration to form the gradient along the longest dimension. Composition gradients of NixCu_1−x, MoxNb_1−x, and MoNbTaWHf_x (x from 0 to 1) were fabricated with the tooling. The microstructure, composition, and crystal structure were characterized along the gradient in the as-sintered condition and after annealing to partially homogenize the layers. The successful fabrication of a composition gradient in a difficult-to-process material like the refractory multi-principal element alloy system MoNbTaWHf_x shows the utility of this approach for high-throughput screening of large material composition spaces. Full article

Magnesium (Mg) and its alloys offer promise for aerospace, railway, and 3D technology applications, yet their inherent limitations, including inadequate strength, pose challenges. Magnesium matrix composites, particularly with metallic reinforcements like titanium (Ti) and its alloys, present a viable solution. Therefore, this study investigates the impact of Ti6Al4V reinforcement on AZ31 magnesium alloy composites produced using pulse plasma sintering (PPS). Results show enhanced microhardness of the materials due to improved densification and microstructural refinement. However, Ti6Al4V addition decreased corrosion resistance, leading to strong microgalvanic corrosion and substrate dissolution. Understanding these effects is crucial for designing Mg-based materials for industries like petrochemicals, where degradation-resistant materials are vital for high-pressure environments. This research provides valuable insights into developing Mg-Ti6Al4V composites with tailored properties for diverse industrial applications, highlighting the importance of considering corrosion behavior in material design. Further investigation is warranted to establish predictive correlations between Ti6Al4V content and corrosion rate for optimizing composite performance. Full article

In this paper, a novel power sintering technique, named fast hot-pressing sintering (FHP), which is able to achieve an ultrahigh heating rate similar to the spark plasma sintering (SPS) technique, but at a much lower cost, was applied to prepare a series of Al/Si composites with different Si volume ratios (12 vol.% to 70 vol.%) to meet the requirements of advanced packaging materials for electronic devices. In contrast to SPS, the FHP oven possesses a safe and budget-friendly current power supply, rather than a complex and expensive pulse power supply, for its heating power. The optimized sintering parameters (temperature, pressure and holding time) of FHP for preparing Al/Si composites were investigated and determined as 470 °C, 300 MPa and 5 min, respectively. In order to characterize the potential of Al/Si composites as packaging materials, thermal conductivities and coefficients of thermal expansion were studied. The thermal conductivity of the Al-40Si composite sintered by the FHP method is higher than that of the conventional SPS method (139 to 107 W m⁻¹ K⁻¹). With the increase in Si, the thermal conductivities and coefficients of thermal expansion on both decreases. Furthermore, the thermal conductivities obey the Agari model, whereas the coefficient of thermal expansion and Si volume ratios obey additivity. The numeric modeling would help develop required packaging materials based on the thermal performances of the substrate materials, like Si or GaAs semiconductor devices. Full article

The influence of WEDM parameters (Spark gap voltage, Pulse-on time, Spark frequency, and Wire speed) on the recast layer thickness and surface roughness of Spark Plasma Sintered SiC-TiB₂-TiC ceramic composite was investigated. For this, an orthogonal L9 Taguchi design was used, and grey relational analysis was carried out for multi-response WEDM parameter optimization in order to determine the minimum RLT and SR. It was noticed that for RLT, the Pulse-on time was observed as the most significant process parameter, followed by Spark gap voltage. On the other hand, Spark frequency and Wire speed had no significance for RLT. Moreover, Spark frequency was observed as the most significant process parameter, followed by Pulse-on time and Spark gap voltage, while Wire speed had a negligible effect on SR. It was found that at optimal process parameters (U = 48V; Ton = 1.0 µs; f = 10 kHz; q = 8 m/min), we obtained an RLT of 3.16 µm and an SR of Ra = 0.847 µm. The confirmation test showed a decrease in RLT and SR by 43.67% and 7.12%, respectively, in comparison to the initial machining conditions. Full article

In this paper, spark plasma sintering was used to obtain and investigate (Pb_0.97Ba_0.03)(Zr_0.98Ti_0.02)_1−xSn_xO₃ (PBZTS) ceramic materials for x = 0, 0.02, 0.04, 0.06, and 0.08. Crystal structure, microstructure, dielectric and ferroelectric properties, and electrical conductivity tests of a series of samples were carried out. The SPS sintering method ensures favorable dielectric and ferroelectric properties of PBZTS ceramic materials. X-ray studies have shown that the material has a perovskite structure. The samples have a densely packed material structure with properly crystallized grains. The fine-grained microstructure of the PZBZTS material with high grain homogeneity allows the application of higher electric fields. Ceramic samples obtained by the SPS method have higher density values than samples obtained by the classical method (FS). The permittivity at room temperature is in the range of 245–282, while at the phase transition temperature is in the range of 10,259–12,221. At room temperature, dielectric loss factor values range from 0.006 to 0.036. The hysteresis loops of PBZTS ceramics have a shape typical for ferroelectric hard materials, and the remnant polarization values range from 0.32 to 0.39 µC/cm². The activation energy E_a values of the PBZTS samples result mainly from the presence of oxygen vacancies. The PZT material doped with Ba and Sn and sintered via the SPS method has favorable physical parameters for applications in modern devices such as actuators or pulse capacitors. Full article

The scientific goal of this paper is to study and explain the relationship between the microstructure of a ceramic–intermetallic composite fabricated by consolidating a mixture of Al₂O₃ and NiAl-Al₂O₃ using the PPS technique and its basic mechanical properties. Six series of composites were manufactured. The obtained samples differed in the sintering temperature and content of compo-powder. The base powders, compo-powder, and composites were investigated using SEM equipped with an EDS and XRD. Hardness tests and K_IC measurements were applied to estimate the mechanical properties of the fabricated composites. The wear resistance was evaluated using a “ball-on-disc” method. The results demonstrate that the density of the obtained composites increases with the increased temperature of the sintering. The content of NiAl + 20 wt.% Al₂O₃ did not have a determining effect on the hardness of the manufactured composites. The highest hardness, contacting 20.9 ± 0.8 GPa, was found for the composite series sintered at 1300 °C and 2.5 vol.% of compo-powder. The highest K_IC value from all the studied series equaled 8.13 ± 0.55 MPa·m^0.5 and was also achieved for the series manufactured at 1300 °C (2.5 vol.% of compo-powder). The average friction coefficient during the ball-friction test with the Si₃N₄ ceramic counter-sample was between 0.8 and 0.95. Full article

As part of extensive research on the properties of nickel-aluminum alloys, corrosion tests of sintered materials produced by the innovative HPHT/SPS (high pressure, high temperature/spark plasma sintering) method were performed in 0.1 molar H₂SO₄ acid. The hybrid, unique device used for this purpose (one of only two such devices operating in the world) is equipped with a Bridgman chamber, which allows heating with high-frequency pulsed current and sintering of powders under high pressure in the range of 4–8 GPa and at temperatures up to 2400 °C. Using this device for the production of materials contributes to the generation of new phases not obtainable by classical methods. In this article, the first test results obtained for the nickel-aluminum alloys never before produced by this method are discussed. Alloys containing 25 at.% Al, 37 at.% Al and 50 at.% Al were produced. The alloys were obtained by the combined effect of the pressure of 7 GPa and the temperature of 1200 °C generated by the pulsed current. The time of the sintering process was 60 s. The electrochemical tests, such as OCP (open circuit potential), polarization tests and EIS (electrochemical impedance spectroscopy), were carried out for the newly produced sinters and the results were compared with the reference materials, i.e., nickel and aluminum. The corrosion tests showed good corrosion resistance of the produced sinters, with corrosion rates of 0.091, 0.073 and 0.127 mm per year, respectively. It leaves no doubt that the good resistance of materials synthesized by powder metallurgy is due to the proper selection of the manufacturing process parameters, ensuring a high degree of material consolidation. This was further confirmed by the examinations of microstructure (optical microscopy and scanning electron microscopy) and the results of density tests (hydrostatic method). It has been shown that the obtained sinters were characterized by a compact, homogeneous and pore-free structure, though at the same time differentiated and multi-phase, while the densities of individual alloys reached a level close to the theoretical values. The Vickers hardness of the alloys was 334, 399 and 486 HV10, respectively. Full article

Spark plasma sintering (SPS), also called pulsed electric current sintering (PECS) or field-assisted sintering technique (FAST) is a technique for sintering powder under moderate uniaxial pressure (max. 0.15 GPa) and high temperature (up to 2500 °C). It has been widely used over the last few years as it can achieve full densification of ceramic or metal powders with lower sintering temperature and shorter processing time compared to conventional processes, opening up new possibilities for nanomaterials densification. More recently, new frontiers of opportunities are emerging by coupling SPS with high pressure (up to ~10 GPa). A vast exciting field of academic research is now using high-pressure SPS (HP-SPS) in order to play with various parameters of sintering, like grain growth, structural stability and chemical reactivity, allowing the full densification of metastable or hard-to-sinter materials. This review summarizes the various benefits of HP-SPS for the sintering of many classes of advanced functional materials. It presents the latest research findings on various HP-SPS technologies with particular emphasis on their associated metrologies and their main outstanding results obtained. Finally, in the last section, this review lists some perspectives regarding the current challenges and future directions in which the HP-SPS field may have great breakthroughs in the coming years. Full article

Aluminum-based ceramics exhibit excellent wear resistance and hot hardness that are suitable for various responsible applications allowing products to work under extreme mechanical and thermal loads (up to 1000 °C). The problem of high-precision forming complex-shaped parts is a known engineering challenge due to the insulating properties of aluminum-containing ceramics and the formation of chemically active carbides in a hydrocarbon medium. The alternative approach for electrical discharge machining non-conductive sintered Al₂O₃ in the water-based medium using nickel-chrome plasma-vapor-deposed coating of 12 mm, SnO powder suspension (particle diameter of ⌀10 µm, concentration of 150 g/L), and brass wire-tool is proposed. The productivity was evaluated by calculating the material removal rate and discharge gap for various combinations of pulse frequency and duration. The maximal material removal rate of 0.0014 mm³/s was achieved for a pulse frequency of 30 kHz and pulse duration of 1.7–2.5 μs. The recommended value of the interelectrode gap is 48.0 ± 4.9 µm. The possibility of electrical discharge machining aluminum-containing insulating ceramics without using hydrocarbons, carbon and copper-group assisting measures was proposed and shown for the first time. The chemical content of the debris in the interelectrode gap between components of the materials was thermochemically analyzed. Full article

High-Pressure (HP) technology allows new possibilities of processing by Spark Plasma Synthesis (SPS). This process is mainly involved in the sintering process and for bonding, growing and reaction. High-Pressure tools combined with SPS is applied for processing polycrystalline diamond without binder (binderless PCD) in this current work. Our described innovative Ultra High Pressure Spark Plasma Sintering (UHP-SPS) equipment shows the combination of our high-pressure apparatus (Belt-type) with conventional pulse electric current generator (Fuji). Our UHP-SPS equipment allows the processing up to 6 GPa, higher pressure than HP-SPS equipment, based on a conventional SPS equipment in which a non-graphite mold (metals, ceramics, composite and hybrid) with better mechanical properties (capable of 1 GPa) than graphite. The equipment of UHP-SPS and HP-SPS elements (pistons + die) conductivity of the non-graphite mold define a Hot-Pressing process. This study presents the results showing the ability of sintering diamond powder without additives at 4–5 GPa and 1300–1400 °C for duration between 5 and 30 min. Our described UHP-SPS innovative cell design allows the consolidation of diamond particles validated by the formation of grain boundaries on two different grain size powders, i.e., 0.75–1.25 μm and 8–12 μm. The phenomena explanation is proposed by comparison with the High Pressure High Temperature (HP-HT) (Belt, toroidal-Bridgman, multi-anvils (cubic)) process conventionally used for processing binderless polycrystalline diamond (binderless PCD). It is shown that using UHP-SPS, binderless diamond can be sintered at very unexpected P-T conditions, typically ~10 GPa and 500–1000 °C lower in typical HP-HT setups. This makes UHP-SPS a promising tool for the sintering of other high-pressure materials at non-equilibrium conditions and a potential industrial transfer with low environmental fingerprints could be considered. Full article

The paper presents the effect of diamond particle size (varying between 2.5 µm and 20 µm) on the microstructure, density and hardness of WC-Co/diamond composites. The obtained materials contained 30% vol. diamond. The advanced sintering method Pulse Plasma Sintering (PPS) was used for the production of composites. The sintering process was carried out in two stages at a pressure of 50 and 100 MPa and a temperature of 1050 °C. Depending on the size of the diamond particles, composites with a density of 91–99% were obtained. Microstructure studies were performed employing scanning electron microscopy, along with an analysis of the chemical composition in micro-areas. Additionally, the phase composition was investigated by means of X-ray diffraction. In addition, hardness tests were performed. It was found that the size of the diamond particles significantly influenced the microstructure of the tested materials, as well as the density and hardness. As a result of PPS sintering of composites containing the finest diamond particles (2.5–5 µm), the presence of a metastable type of diamond—graphite was found. Full article

NiAl-Al₂O₃ composites, fabricated from the prepared composite powders by mechanical alloying and then consolidated by pulse plasma sintering, were presented. The use of nanometric alumina powder for reinforcement of a synthetized intermetallic matrix was the innovative concept of this work. Moreover, this is the first reported attempt to use the Pulse Plasma Sintering (PPS) method to consolidate composite powder with the contribution of nanometric alumina powder. The composite powders consisting of the intermetallic phase NiAl and Al₂O₃ were prepared by mechanical alloying from powder mixtures containing Ni-50at.%Al with the contribution of 10 wt.% or 20 wt.% nanometric aluminum oxide. A nanocrystalline NiAl matrix was formed, with uniformly distributed Al₂O₃ inclusions as reinforcement. The PPS method successfully consolidated NiAl-Al₂O₃ composite powders with limited grain growth in the NiAl matrix. The appropriate sintering temperature for composite powder was selected based on analysis of the grain growth and hardness of Al₂O₃ subjected to PPS consolidation at various temperatures. As a result of these tests, sintering of the NiAl-Al₂O₃ powders was carried out at temperatures of 1200 °C, 1300 °C, and 1400 °C. The microstructure and properties of the initial powders, composite powders, and consolidated bulk composite materials were characterized by SEM, EDS, XRD, density, and hardness measurements. The hardness of the ultrafine-grained NiAl-Al₂O₃ composites obtained via PPS depends on the Al₂O₃ content in the composite, as well as the sintering temperature applied. The highest values of the hardness of the composites were obtained after sintering at the lowest temperature (1200 °C), reaching 7.2 ± 0.29 GPa and 8.4 ± 0.07 GPa for 10 wt.% Al₂O₃ and 20 wt.% Al₂O₃, respectively, and exceeding the hardness values reported in the literature. From a technological point of view, the possibility to use sintering temperatures as low as 1200 °C is crucial for the production of fully dense, ultrafine-grained composites with high hardness. Full article