In-Situ Synthesis,Microstructure, and Mechanical Properties of TiB2-Reinforced Fe-Cr-Mn-Al Steel Matrix Composites Prepared by Spark Plasma Sintering

In-situ synthesis, microstructure, and mechanical properties of four TiB₂-Reinforced Fe-Cr-Mn-Al Steel Matrix Composites have been researched in this work. The microstructure and phases of the prepared specimens have been characterized by using scanning electron microscopy (SEM), X-ray diffraction technique, and transmission electron microscopy (TEM). The sintered specimens consisted of Fe₂AlCr, CrFeB-type boride, and TiB₂. The mechanical properties, such as hardness and compression strength at room temperature (RT) and at elevated temperatures (600 °C and 800 °C) have been evaluated. The compressive strength and Vickers hardness of the sintered specimens increase with the volume fraction of TiB₂ in the matrix, which are all much higher than those of the ex-situ TiB₂/Fe-15Cr-20Mn-8Al composites and the reported TiB₂/Fe-Cr composites with the same volume fraction of TiB₂. The highest Vickers hardness and compressive strength at room temperature are 1213 ± 35 HV and 3500 ± 20 MPa, respectively. As the testing temperature increases to 600 °C, or even 800 °C, these composites still show relatively high compressive strength. Precipitation strengthening of CrFeB and in-situ synthesis of TiB₂ as well as nanocrystalline microstructure produced by the combination of mechanical alloying (MA) and spark plasma sintering (SPS) can account for the high Vickers hardness and compressive strength.     

Microstructure and Mechanical Properties of Composites Obtained by Spark Plasma Sintering of Ti3SiC2-15 vol.%Cu Mixtures

Method of soft metal (Cu) strengthening of Ti₃SiC₂ was conducted to increase the hardness and improve the wear resistance of Ti₃SiC₂. Ti₃SiC₂/Cu composites containing 15 vol.% Cu were fabricated by Spark Plasma Sintering (SPS) in a vacuum. The effect of the sintering temperature on the phase composition, microstructure and mechanical properties of the composites was investigated in detail. The as-synthesized composites were thoroughly characterized by scanning electron micrography (SEM), optical micrography (OM) and X-ray diffractometry (XRD), respectively. The results indicated that the constituent of the Ti₃SiC₂/Cu composites sintered at different temperatures included Ti₃SiC₂, Cu₃Si and TiC. The formation of Cu₃Si and TiC originated from the reaction between Ti₃SiC₂ and Cu, which was induced by the presence of Cu and the de-intercalation of Si atoms Ti₃SiC₂. OM analysis showed that with the increase in the sintering temperature, the reaction between Ti₃SiC₂ and Cu was severe, leading to the Ti₃SiC₂ getting smaller and smaller. SEM measurements illustrated that the uniformity of the microstructure distribution of the composites was restricted by the agglomeration of Cu, controlling the mechanical behaviors of the composites. At 1000 °C, the distribution of Cu in the composites was relatively even; thus, the composites exhibited the highest density, relatively high hardness and compressive strength. The relationships of the temperature, the current and the axial dimension with the time during the sintering process were further discussed. Additionally, a schematic illustration was proposed to explain the related sintering characteristic of the composites sintered by SPS. The as-synthesized Ti₃SiC₂/Cu composites were expected to improve the wear resistance of polycrystalline Ti₃SiC₂.     

On the Structure and Properties of AlMgB14-TiB2 Composites Obtained from SHS Powders by Spark Plasma Sintering

AlMgB₁₄-TiB₂ composite materials were fabricated by self-propagating high-temperature synthesis (SHS) followed by spark plasma sintering of the obtained SHS products. It was found that, during the SHS, the AlMgB₁₄ phase is formed at a donor (Ti + 2B) to acceptor (Al₁₂Mg₁₇-B) mass ratio of 3:7 and 4:6, respectively. The specimen sintered from the SHS powder with the donor:acceptor mass ratio of 5:5 at a temperature of 1470 °C has a uniform skeletal structure. The average hardness of the obtained specimen is 30.1 GPa.     

Effect of Sintering Temperature and Iron Addition on Properties and Microstructure of High Speed Steel Based Materials Produced by Spark Plasma Sintering Method

Attempts were made to describe the effect of the sintering temperature and pure iron powder addition on the properties of HSS-based materials produced by the spark plasma sintering method (SPS). After sintering, their density, hardness, flexural strength, and tribological properties were determined. The sintered materials were also subjected to microstructural analysis to determine the phenomena occurring at the particle contact boundaries during sintering. On the basis of analysis of the obtained results, it was found that the mechanical properties and microstructure were mainly influenced by the sintering temperature, which was selected in relation to the previously tested steel M3/2, adjusted upwards due to its chemical composition. The use of the temperature of 1050 °C allows materials to be obtained with a density close to the theoretical density (97%), characterized by a high hardness of about 360 HB. The addition of iron slightly reduces the hardness and also increases the flexural strength to 577 MPa. There was no diffusion of the alloying elements from the steel to the iron due to the short time of exposure to the sintering temperature.     

Microstructure and Mechanical Properties of Alumina Composites with Addition of Structurally Modified 2D Ti3C2 (MXene) Phase

This study presents new findings related to the incorporation of MXene phases into ceramic. Aluminium oxide and synthesised Ti₃C₂ were utilised as starting materials. Knowing the tendency of MXenes to oxidation and degradation, particularly at higher temperatures, structural modifications were proposed. They consisted of creating the metallic layer on the Ti₃C₂, by sputtering the titanium or molybdenum. To prepare the composites, powder metallurgy and spark plasma sintering (SPS) techniques were adopted. In order to evaluate the effectiveness of the applied modifications, the emphasis of the research was placed on microstructural analysis. In addition, the mechanical properties of the obtained sinters were examined. Observations revealed significant changes in the MXenes degradation process, from porous areas with TiC particles (for unmodified Ti₃C₂), to in situ creation of graphitic carbon (in the case of Ti₃C₂-Ti/Mo). Moreover, the fracture changed from purely intergranular to cracking with high participation of transgranular mode, analogously. In addition, the results obtained showed an improvement in the mechanical properties for composites with Ti/Mo modifications (an increase of 10% and 15% in hardness and fracture toughness respectively, for specimens with 0.5 wt.% Ti₃C₂-Mo). For unmodified Ti₃C₂, enormously cracked areas with spatters emerged during tests, making the measurements impossible to perform.     

Synthesis and Characterization of a Nearly Single Bulk Ti2AlN MAX Phase Obtained from Ti/AlN Powder Mixture through Spark Plasma Sintering

MAX phases are an advanced class of ceramics based on ternary carbides or nitrides that combine some of the ceramic and metallic properties, which make them potential candidate materials for many engineering applications under severe conditions. The present work reports the successful synthesis of nearly single bulk Ti₂AlN MAX phase (>98% purity) through solid-state reaction and from a Ti and AlN powder mixture in a molar ratio of 2:1 as starting materials. The mixture of Ti and AlN powders was subjected to reactive spark plasma sintering (SPS) under 30 MPa at 1200 °C and 1300 °C for 10 min in a vacuum atmosphere. It was found that the massive formation of Al₂O₃ particles at the grain boundaries during sintering inhibits the development of the Ti₂AlN MAX phase in the outer zone of the samples. The effect of sintering temperature on the microstructure and mechanical properties of the Ti₂AlN MAX phase was investigated and discussed.     

Influence of Ti3C2Tx MXene and Surface-Modified Ti3C2Tx MXene Addition on Microstructure and Mechanical Properties of Silicon Carbide Composites Sintered via Spark Plasma Sintering Method

This article presents new findings related to the problem of the introduction of MXene phases into the silicon carbide matrix. The addition of MXene phases, as shown by the latest research, can significantly improve the mechanical properties of silicon carbide, including fracture toughness. Low fracture toughness is one of the main disadvantages that significantly limit its use. As a part of the experiment, two series of composites were produced with the addition of 2D-Ti₃C₂T_x MXene and 2D-Ti₃C₂T_x surface-modified MXene with the use of the sol-gel method with a mixture of Y₂O₃/Al₂O₃ oxides. The composites were obtained with the powder metallurgy technique and sintered with the Spark Plasma Sintering method at 1900 °C. The effect adding MXene phases had on the mechanical properties and microstructure of the produced sinters was investigated. Moreover, the influence of the performed surface modification on changes in the properties of the produced composites was determined. The analysis of the obtained results showed that during sintering, the MXene phases oxidize with the formation of carbon flakes playing the role of reinforcement. The influence of the Y₂O₃/Al₂O₃ layer on the structure of carbon flakes and the higher quality of the interface was also demonstrated. This was reflected in the higher mechanical properties of composites with the addition of modified Ti₃C₂T_x. Composites with 1 wt.% addition of Ti₃C₂T_x M are characterized with a fracture toughness of 5 MPa × m^0.5, which is over 50% higher than in the case of the reference sample and over 15% higher than for the composite with 2.5 wt.% addition of Ti₃C₂T_x, which showed the highest fracture toughness in this series.     

Study of the Influence of Sintering Atmosphere and Mechanical Activation on the Synthesis of Bulk Ti2AlN MAX Phase Obtained by Spark Plasma Sintering

The influence of the mechanical activation process and sintering atmosphere on the microstructure and mechanical properties of bulk Ti₂AlN has been investigated. The mixture of Ti and AlN powders was prepared in a 1:2 molar ratio, and a part of this powder mixture was subjected to a mechanical activation process under an argon atmosphere for 10 h using agate jars and balls as milling media. Then, the sintering and production of the Ti₂AlN MAX phase were carried out by Spark Plasma Sintering under 30 MPa with vacuum or nitrogen atmospheres and at 1200 °C for 10 min. The crystal structure and microstructure of consolidated samples were characterized by X-ray Diffraction, Scanning Electron Microscopy, and Energy Dispersive X-ray Spectroscopy. The X-ray diffraction patterns were fitted using the Rietveld refinement for phase quantification and determined their most critical microstructural parameters. It was determined that by using nitrogen as a sintering atmosphere, Ti₄AlN₃ MAX phase and TiN were increased at the expense of the Ti₂AlN. In the samples prepared from the activated powders, secondary phases like Ti₅Si₃ and Al₂O₃ were formed. However, the higher densification level presented in the sample produced by using both nitrogen atmosphere and MAP powder mixture is remarkable. Moreover, the high-purity Ti₂AlN zone of the MAX-1200 presented a hardness of 4.3 GPa, and the rest of the samples exhibited slightly smaller hardness values (4.1, 4.0, and 4.2 GPa, respectively) which are matched with the higher porosity observed on the SEM images.     

Microstructure and Mechanical Properties of TiN–TiB2–hBN Composites Fabricated by Reactive Hot Pressing Using TiN–B Mixture

In this study, TiN–TiB₂–hBN composite ceramics were prepared via reactive hot pressing using TiN and amorphous B powders as raw materials. Different sintering temperatures and composition ratios were studied. The results show that the 70 vol% TiN–17.6 vol% TiB₂–12.4 vol% hBN ceramic composites obtained ideal comprehensive properties at 1600 °C. The relative density, Vickers hardness, bending strength, and fracture toughness were 99%, 11 GPa, 521 MPa, and 4.22 MPa·m^1/2, respectively. Densification was promoted by the highly active reaction product TiB₂, and the structural defects formed in the grains. Meanwhile, the good interfacial bonding between TiN and TiB₂ grains and the uniform dispersion of ultrafine hBN in the matrix contributed to the excellent bending strength. Moreover, the toughening mechanism of crack deflection and grain pull-out improved the fracture toughness.     

Synthesis and Tribological Characterization of Ti3SiC2/ZnO Composites

Dense Ti₃SiC₂/ZnO composites were sintered at different temperatures by spark plasma sintering (SPS). The effects of sintering temperature on composition and mechanical properties of Ti₃SiC₂/ZnO composites were studied. The tribological behaviors of Ti₃SiC₂/ZnO composites/Inconel 718 alloy tribo-pairs at elevated temperature from 25 °C to 800 °C were discussed. The experimental results showed that the initial decomposition temperature of the Ti₃SiC₂/ZnO composite was 1150 °C, and Ti₃SiC₂ decomposed into TiC. When the decomposition temperature was higher than 1150 °C, the compositions of the Ti₃SiC₂/ZnO composites were Ti₃SiC₂, ZnO, and TiC. It was found that Ti₃SiC₂/ZnO composites had better self-lubricating performance than Ti₃SiC₂ at elevated temperature from 600 °C to 800 °C, which was owing to material transfers of tribo-pairs and sheared oxides generated by tribo-oxidation reactions.     

Influence of MXene (Ti3C2) Phase Addition on the Microstructure and Mechanical Properties of Silicon Nitride Ceramics

This paper discusses the influence of Ti₃C₂ (MXene) addition on silicon nitride and its impact on the microstructure and mechanical properties of the latter. Composites were prepared through powder processing and sintered using the spark plasma sintering (SPS) technic. Relative density, hardness and fracture toughness, were analyzed. The highest fracture toughness at 5.3 MPa·m^1/2 and the highest hardness at HV5 2217 were achieved for 0.7 and 2 wt.% Ti₃C₂, respectively. Moreover, the formation of the Si₂N₂O phase was observed as a result of both the MXene addition and the preservation of the α-Si₃N₄→β-Si₃N₄ phase transformation during the sintering process.     

Low-Temperature Rapid Sintering of Dense Cubic Phase ZrW2−xMoxO8 Ceramics by Spark Plasma Sintering and Evaluation of Its Thermal Properties

In this study, we report a low-temperature approach involving a combination of a sol–gel hydrothermal method and spark plasma sintering (SPS) for the fabrication of cubic phase ZrW_2−xMo_xO₈ (0.00 ≤ x ≤ 2.00) bulk ceramics. The cubic-ZrW_2−xMo_xO₈ (0.00 ≤ x ≤ 1.50) bulk ceramics were successfully synthesized within a temperature range of 623–923 K in a very short amount of time (6–7 min), which is several hundred degrees lower than the typical solid-state approach. Meanwhile, scanning electron microscopy and density measurements revealed that the cubic-ZrW_2−xMo_xO₈ (0.00 ≤ x ≤ 1.50) bulk ceramics were densified to more than 90%. X-ray diffraction (XRD) results revealed that the cubic phase ZrW_2−xMo_xO₈ (0.00 ≤ x ≤ 1.5) bulk ceramics, as well as the sol–gel-hydrothermally synthesized ZrW_2−xMo_xO₇(OH)₂·2H₂O precursors correspond to their respective pure single phases. The bulk ceramics demonstrated negative thermal expansion characteristics, and the coefficients of negative thermal expansion were shown to be tunable in cubic-ZrW_2−xMo_xO₈ bulk ceramics with respect to x value and sintering temperature. The cubic-ZrW_2−xMo_xO₈ solid solution can thus have potential applications in electronic devices such as heat sinks that require regulation of thermal expansion.     

Characterization of Al2O3 Samples and NiAl–Al2O3 Composite Consolidated by Pulse Plasma Sintering

The paper describes an investigation of Al₂O₃ samples and NiAl–Al₂O₃ composites consolidated by pulse plasma sintering (PPS). In the experiment, several methods were used to determine the properties and microstructure of the raw Al₂O₃ powder, NiAl–Al₂O₃ powder after mechanical alloying, and samples obtained via the PPS. The microstructural investigation of the alumina and composite properties involves scanning electron microscopy (SEM) analysis and X-ray diffraction (XRD). The relative densities were investigated with helium pycnometer and Archimedes method measurements. Microhardness analysis with fracture toughness (K_IC) measures was applied to estimate the mechanical properties of the investigated materials. Using the PPS technique allows the production of bulk Al₂O₃ samples and intermetallic ceramic composites from the NiAl–Al₂O₃ system. To produce by PPS method the NiAl–Al₂O₃ bulk materials initially, the composite powder NiAl–Al₂O₃ was obtained by mechanical alloying. As initial powders, Ni, Al, and Al₂O₃ were used. After the PPS process, the final composite materials consist of two phases: Al₂O₃ located within the NiAl matrix. The intermetallic ceramic composites have relative densities: for composites with 10 wt.% Al₂O₃ 97.9% and samples containing 20 wt.% Al₂O₃ close to 100%. The hardness of both composites is equal to 5.8 GPa. Moreover, after PPS consolidation, NiAl–Al₂O₃ composites were characterized by high plasticity. The presented results are promising for the subsequent study of consolidation composite NiAl–Al₂O₃ powder with various initial contributions of ceramics (Al₂O₃) and a mixture of intermetallic–ceramic composite powders with the addition of ceramics to fabricate composites with complex microstructures and properties. In composites with complex microstructures that belong to the new class of composites, in particular, the synergistic effect of various mechanisms of improving the fracture toughness will be operated.     

Processing and Properties of Tungsten-Steel Composites and FGMs Prepared by Spark Plasma Sintering

Tungsten is the prime candidate material for the plasma-facing components of fusion reactors. For the joining of tungsten armor to the cooling system or support structure, composites or graded interlayers can be used to reduce the stress concentration at the interface. These interlayers can be produced by several technologies. Among these, spark plasma sintering appears advantageous because of its ability to fabricate fully dense parts at lower temperatures and in a shorter time than traditional powder metallurgy techniques, thanks to the concurrent application of temperature, pressure, and electrical current. In this work, spark plasma sintering of tungsten-steel composites and functionally graded layers (FGMs) was investigated. As a first step, pure tungsten and steel powders of different sizes were sintered at a range of temperatures to find a suitable temperature window for fully dense compacts. Characterization of the sintered compacts included structure (by SEM); porosity (by the Archimedean method and image analysis); thermal diffusivity (by the flash method) and mechanical properties (microhardness and flexural strength). Compacts with practically full density and fine grains were obtained; while the temperature needed to achieve full sintering decreased with decreasing powder size (down to about 1500 °C for the 0.4 μm powder). For fully sintered compacts, the hardness and thermal diffusivity increased with decreasing powder size. Composites with selected tungsten/steel ratios were produced at several conditions and characterized. At temperatures of 1100 °C or above, intermetallic formation was observed in the composites; nevertheless, without a detrimental effect on the mechanical strength. Finally, the formation of graded layers and tungsten-steel joints in various configurations was demonstrated.     

Functionally Graded Al2O3–CTZ Ceramics Fabricated by Spark Plasma Sintering

We studied the fabrication of functionally graded Al₂O₃–CeO₂-stabilized-ZrO₂ (CTZ) ceramics by spark plasma sintering. The ceramic composite exhibits a gradual change in terms of composition and porosity in the axial direction. The composition gradient was created by layering starting powders with different Al₂O₃ to CTZ ratios, whereas the porosity gradient was established with a large temperature difference, which was induced by an asymmetric graphite tool configuration during sintering. SEM investigations confirmed the development of a porosity gradient from the top toward the bottom side of the Al₂O₃–CTZ ceramic and the relative pore volume distributed in a wide range from 0.02 to 100 µm for the samples sintered in asymmetric configuration (ASY), while for the reference samples (STD), the size of pores was limited in the nanometer scale. The microhardness test exhibited a gradual change along the axis of the ASY samples, reaching 10 GPa difference between the two opposite sides of the Al₂O₃–CTZ ceramics without any sign of delamination or cracks between the layers. The flexural strength of the samples for both series showed an increasing tendency with higher sintering temperatures. However, the ASY samples achieved higher strength due to their lower total porosity and the newly formed elongated CeAl₁₁O₁₈ particles.     

Microstructure and Mechanical Properties of Ti-25Nb-4Ta-8Sn Alloy Prepared by Spark Plasma Sintering

As the commercially most-used Ti-6Al-4V alloy has a different modulus of elasticity compared to the modulus of elasticity of bone and contains allergenic elements, β-Ti alloy could be a suitable substitution in orthopedics. The spark plasma sintering (SPS) method is feasible for the preparation of materials, with very low porosity and fine-grained structure, leading to higher mechanical properties. In this study, we prepared quaternary Ti-25Nb-4Ta-8Sn alloy using the spark plasma sintering method. The material was also heat-treated in order to homogenize the structure and compare the microstructure and properties in as-sintered and annealed states. The SPS sample had a modulus of elasticity of about 63 ± 1 GPa, which, after annealing, increased to the value of 73 ± 1 GPa. The tensile yield strength (TYS) of the SPS sample was 730 ± 52 MPa, ultimate tensile strength (UTS) 764 ± 10 MPa, and ductility 22 ± 9%. Annealed samples reached higher values of TYS and UTS (831 ± 60 MPa and 954 ± 48 MPa), but the ductility decreased to the value of 3 ± 1%. The obtained results are discussed considering the observed microstructure of the alloy.     

Effect of Holding Time on Densification,Microstructure and Selected Properties of Spark Plasma Sintered AA7075-B4C Composites

The paper presents the effect of the holding time, varying between 1 min 15 s and 10 min, on the microstructure evolution and development of selected properties of spark plasma sintered AA7075-based composites reinforced with 3, 5 and 10 wt% sub-micro B₄C powder. The sintering temperature and the compaction pressure were 500 °C and 80 MPa, respectively. Composites with a near full density of 96–97% were obtained. Microstructure studies were performed employing the techniques of light microscopy and 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 and flexural strength tests were performed. It was found that the holding time did not significantly influence the microstructures of the examined materials nor the hardness or flexural strength. The sintered composites had a fine-grained microstructure with a strengthening phase located at the grain boundaries. As a result of the spark plasma sintering process, fine precipitates of intermetallic phases were also observed in the aluminum grains, suggesting partial supersaturation, which occurred during fast cooling.     

Microstructure and Tribological Properties of Spark-Plasma-Sintered Ti3SiC2-Pb-Ag Composites at Elevated Temperatures

Ti₃SiC₂-PbO-Ag composites (TSC-PA) were successfully prepared using the spark plasma sintering (SPS) technique. The ingredient and morphology of the as-synthesized composites were elaborately investigated. The tribological properties of the TSC-PA pin sliding against Inconel 718 alloys disk at room temperature (RT) to 800 °C were examined in air. The wear mechanisms were argued elaborately. The results showed that the TSC-PA was mainly composed of Ti₃SiC₂, Pb, and Ag. The average friction coefficient of TSC-PA gradually decreased from 0.72 (RT) to 0.3 (800 °C), with the temperature increasing from RT to 800 °C. The wear rate of TSC-PA showed a decreasing trend, with the temperature rising from RT to 800 °C. The wear rate of Inconel 718 exhibited positive wear at RT and negative wear at elevated temperatures. The tribological property of TSC-PA was related to the tribo-chemistry, and the abrasive and adhesive wear.     

Effects of TiO2 Nanoparticle Addition on Microstructure and Selected Properties of Ag–xTiO2 Composites

The paper presents the results of a study of the microstructure and selected properties of silver-based composites reinforced with TiO₂ nanoparticles, produced by the powder metallurgy method. Pure silver powders were mixed with TiO₂ reinforcement (5 and 10 wt%) and 5 mm steel balls (100Cr6) for 270 min in a Turbula T2F mixer to produce a homogeneous mixture. The composites were made in a rigid die with a single-action compaction press under a pressure of 400 MPa and 500 MPa and then sintered under nitrogen atmosphere at 900 °C. Additionally, to improve the density and mechanical properties of the obtained sinters, double pressing and double sintering operations were conducted. As a result, compacts with a density of 90–94% were obtained. The microstructure of the sintered compacts consists of uniform grains, and the TiO₂ reinforcement phase particles are located on the grain boundaries. There were no discontinuities at the Ag–TiO₂ contact boundary, which was confirmed by SEM and TEM analysis. The use of a higher pressure had a positive effect on the hardness and flexural strength of the tested materials. It was found that the composites with 5 wt% TiO₂ pressed under 500 MPa are characterized by the highest level of mechanical properties. The hardness of these composites is 57 HB, while the flexural strength is 163 MPa.     

Modelling and Characterisation of Residual Stress of SiC-Ti3C2Tx MXene Composites Sintered via Spark Plasma Sintering Method

This article presents an attempt to determine the effect of the MXene phase addition and its decomposition during sintering with the use of the spark plasma sintering method on mechanical properties and residual stress of silicon carbide based composites. For this purpose, the unreinforced silicon carbide sinter and the silicon carbide composite with the addition of 2 wt.% of Ti₃C₂T_x were tested. The results showed a significant increase of fracture toughness and hardness for composite, respectively 36% and 13%. The numerical study involving this novel method of modelling shows the presence of a complex state of stress in the material, which is related to the anisotropic properties of graphitic carbon structures formed during sintering. An attempt to determine the actual values of residual stress in the tested materials using Raman spectroscopy was also made. These tests showed a good correlation with the constructed numerical model and confirmed the presence of a complex state of residual stress.