The paper presents the results of the mechanical, electrical, CCSEM and XRD measurements of hard coal, conducted in simulated conditions of sintering in atmospheres of O2/CO2,. The changes of the coal ash resistivity are correlated with the content of the oxides and with the sintering temperature determined by the mechanical test and Leitz method. The SEM-EDS analysis was conducted for deposits on the probe. The changes of the measured ash samples, observed during sintering process in O2/CO2 atmosphere, were discussed in the ash microstructure point of view.
Using the available analytical methods, including the determination of chemical composition using wavelength-dispersive X-ray fluorescent spectroscopy technique and phase composition determined using X-ray diffraction, microstructural observations in a highresolution scanning microscope equipped with an X-ray microanalysis system as well as determination of characteristic softening and sintering temperatures using high-temperature microscope, the properties of particular chromite sands were defined. For the study has been typed reference sand with chemical properties, physical and thermal, treated as standard, and the sands of the regeneration process and the grinding process. Using these kinds of sand in foundries resulted in the occurrence of the phenomenon of the molding mass sintering. Impurities were identified and causes of sintering of a moulding sand based on chromite sand were characterized. Next, research methods enabling a quick evaluation of chromite sand suitability for use in the preparation of moulding sands were selected.
The results of structure and mechanical properties investigations of tungsten heavy alloy (THA) after cyclic sintering are presented. The material for study was prepared using liquid phase sintering of mixed and compacted powders in hydrogen atmosphere. The specimens in shape of rods were subjected to different number of sintering cycles according to the heating schemes given in the main part of the paper From the specimens the samples for mechanical testing and structure investigations were prepared. It follows from the results of the mechanical studies, that increasing of sintering cycles lead to decrease of tensile strength and elongation of THA with either small or no influence on yield strength. In opposite to that, the microstructure observations showed that the size of tungsten grain increases with number of sintering cycles. Moreover, scanning electron microscope (SEM) observations revealed distinctly more trans-granular cleavage mode of fracture in specimens subjected to large number of sintering cycles compared with that after one or two cycles only.
Currently is the biggest problem of metallurgical companies the increase of fossil fuel prices and strict environmental regulations. As a result of this, companies must look for alternatives that would reduce the amount of fossil fuels and reduce emissions. Wood sawdust has huge energy potential, which can be used in the process of agglomerate production. This type of energy is locally available, has some similar properties as fossil fuels and is economically advantageous. For these reasons, experimental study using laboratory agglomeration pan was realized to study the possibility of agglomerate production with a mixed fuel. Experimental results show the viability of mixed fuel use in the agglomeration process, but also show significant possibility for improvement. The maximum acceptable substitution ratio, which corresponds to qualitatively suitable agglomerate is 20% of pine sawdust. Based on the realized experiments and the obtained results we have acceded to the intensification of the agglomeration process with an objective to increase the amount of added substitution fuel while maintaining the required quality of agglomerate.
Tungsten heavy alloys comprising tungsten, nickel and ferrous were modified, where molybdenum was added in varying weight proportions keeping the ratio of Ni: Fe (8:2) constant. The powders were mixed in a high-energy ball mill and were further fabricated using the spark plasma sintering (SPS) method at a peak temperature of 1000°C with heating rate of 100°C/min. The details of the microstructure and mechanical properties of these various alloy compositions were studied. With the increasing weight composition of the Mo in the alloy, the relative density of the alloy increased with a significant improvement in all the mechanical properties. The yield strength (YS), ultimate tensile strength (UTS) and hardness improved significantly with increase in the proportion of Mo; however, a reduction in elongation percentage was observed. The maximum strength of 1250 MPa UTS was observed in the alloy with a Mo proportion of 24%. The heavy alloy unmixed with Mo has shown distinct white and grey regions, where white (W) grain is due to tungsten and grey region is a combinatorial effect of Ni and Fe. Upon addition of Mo, the white and gray phase differences started to minimize resulting in deep gray and black ‘C’-phase structures because of homogenization of the alloy. The main fracture mode found during this investigation in the alloys was inter-granular mode.
The paper refers to pulverization and sintering of the (Fe80Nb6B14)0.88Tb0.12 high coercive alloy. The powder was sintered using the ultra-fast current aided method. It turned out that too long discharge time leads to appearing of a soft magnetic phase and simultaneously, decrease in coercivity of the compacted powder. Nevertheless, it was possible to establish preference technology parameters, preserving magnetic hardness of the alloy. As a final test, an impact of Co-powder addition on magnetic properties was studied. The introduced soft magnetic phase (about 20 wt. %) caused about 30% increase of magnetic remanence, which is a result of direct exchange interactions between the two phases.
The mechanical behavior and the change of retained austenite of nanocrystalline Fe-Ni alloy have been investigated by considering the effect of various Ni addition amount. The nanocrystalline Fe-Ni alloy samples were rapidly fabricated by spark plasma sintering (SPS). The SPS is a well-known effective sintering process with an extremely short densification time not only to reach a theoretical density value but also to prevent a grain growth, which could result in a nanocrystalline structures. The effect of Ni addition on the compressive stress-strain behavior was analyzed. The variation of the volume fraction of retained austenite due to deformation was quantitatively measured by means of x-ray diffraction and microscope analyses. The strain-induced martensite transformation was observed in Fe-Ni alloy. The different amount of Ni influenced the rate of the strain-induced martensite transformation kinetics and resulted in the change of the work hardening during the compressive deformation.
Microwave sintering process was employed to agglomerate ferromanganese alloy powders. The effects of sintering temperature, holding time and particle size composition on the properties and microstructure of sintering products were investigated. The results was shown that increasing sintering temperature or holding time appropriately is beneficial to increase the compressive strength and volume density. SEM and EDAX analysis shows that the liquid phase formed below the melting point in the sintering process, which leads to densification. XRD patterns indicate that the main reaction during microwave sintering is the decarbonization and carburization of iron carbide phase. The experiment demonstrate that the optimum microwave sintering process condition is 1150°C, 10 min and 50% content of the powders with the size of –75 μm
439L stainless steel composites blended with fifteen micron SiC particles were prepared by uniaxial pressing of raw powders at 100 MPa and conventional sintering at 1350oC for 2 h. Based on the results of X-ray diffraction analysis, dissolution of SiC particles were apparent. The 5 vol% SiC specimen demonstrated maximal densification (91.5%) among prepared specimens (0-10 vol% SiC); the relative density was higher than the specimens in the literature (80-84%) prepared by a similar process but at a higher forming pressure (700 MPa). The stress-strain curve and yield strength were also maximal at the 5 vol% of SiC, indicating that densification is the most important parameter determining the mechanical property. The added SiC particles in this study did not serve as the reinforcement phase for the 439L steel matrix but as a liquid-phase-sintering agent for facilitating densification, which eventually improved the mechanical property of the sintered product.
Usually porous metals are known as relatively excellent characteristic such as large surface area, light, lower heat capacity, high toughness and permeability for exhaust gas filter, hydrogen reformer catalyst support. The Ni alloys have high corrosion resistance, heat resistance and chemical stability for high temperature applications. In this study, the Ni-based porous metals have been developed with Hastelloy powder by gas atomization and water atomization in order to find the effects of powder shape on porous metal. Each Hastelloy powder is pressed on disk shape of 2 mm thickness with 12 tons using uniaxial press machine. The specimens are sintered at various temperatures in high vacuum condition. The pore properties were evaluated using Porometer and microstructures were observed with SEM.
In this study, two different compositions of submicron-structured titanium (760 nm) and micron-structured chromium (4.66 μm) powders were mixed to fabricate Cr-31.2 mass% Ti alloys by vacuum hot-press sintering. The research imposed various hot-press sintering pressures (20, 35 and 50 MPa), while the sintering temperature maintained at 1250°C for 1 h. The experimental results showed that the optimum parameters of the hot-press sintered Cr-31.2 mass% Ti alloys were 1250°C at 50 MPa for 1 h. Also, the relative density reached 99.94%, the closed porosity decreased to 0.04% and the hardness and transverse rupture strength (TRS) values increased to 81.90 HRA and 448.53 MPa, respectively. Moreover, the electrical conductivity is enhanced to 1.58 × 104 S·cm–1. However, the grain growth generated during the high-temperature and high-pressure of the hot-press sintering process resulted in the grain coarsening phenomenon of the Cr-31.2 mass% Ti alloys after 1250°C hot-press sintering at 50 MPa for 1 h. In addition, the Cr-31.2 mass% Ti alloys were fabricated with the submicron-structured titanium (760 nm) and chromium (588 nm) powders showed more effective compaction than the micron-structured titanium (760 nm) and chromium (4.66 μm) powders did. The closed porosity decreases to 0.02% and the hardness values increase to 83.23 HRA. However, the agglomeration phenomenon of the Cr phase and brittleness of the TiCr2 Laves phases easily led to a slight decrease in TRS (400.54 MPa).
In view of their advantageous properties (high hardness, good frictional wear resistance, chemical and thermal stability at elevated temperatures), cubic boron nitride (cBN) and tungsten carbide (WC) are commonly used for the fabrication of cutting tools. The composites were consolidated at a temperature of 1100°C under a load of 100 MPa for 10 min. The density of the thus produced material was close to the theoretical value (about 99.6%), and the hardness HV30 was about 1950. The phases identified in the composite were WC, Co, and cBN. Microstructural examinations revealed that numerous trans-crystalline fractures through the cBN particles occurred in the material. The present study is concerned with the wear of the WCCo and WCCo/cBN composites. Comparative tribological examinations were performed in a tribological tester using the ball-on-disc arrangement under the conditions of dry friction. The counterspecimens were steel and Al2O3 balls. The tests were conducted under a unit load of 10 N. After the tests, the surface of the samples was examined to describe the wear mechanisms active in various composite materials.
In this study, precisely controlled large scale gas atomization process was applied to produce spherical and uniform shaped high entropy alloy powder. The gas atomization process was carried out to fabricate CoCrFeNiMn alloy, which was studied for high ductility and mechanical properties at low temperatures. It was confirmed that the mass scale, single phase, equiatomic, and high purity spherical high entropy alloy powder was produced by gas atomization process. The powder was sintered by spark plasma sintering process with various sintering conditions, and mechanical properties were characterized. Through this research, we have developed a mass production process of high quality and spherical high entropy alloy powder, and it is expected to expand applications of this high entropy alloy into fields such as powder injection molding and 3D printing for complex shaped components.
In this work, vacuum hot pressed Ni-Mn-Sn-In Heusler alloys with different concentration of In (0, 2 and 4 at.%), were investigated. The magneto-structural behaviour and microstructure dependencies on chemical composition and on heat treatment were examined. It was found that the martensite start transformation temperature increases with growing In content and to a lesser extent with increasing temperature of heat treatment. The high energy X-ray synchrotron radiation results, demonstrated that both chemical composition as well as temperature of heat treatment slightly modified the crystal structures of the studied alloys. Microstructural investigation performed by transmission electron microscopy confirmed chemical composition and crystal structure changes in the alloys.
The Mn-Zn ferrite powders prepared by high energy ball milling were heat-treated, subsequently compacted and sintered by spark plasma sintering (SPS). Based on the observation of microstructure, the characteristics of samples after SPS were investigated and compared with ones after conventional sintering. The size of initial powders was approximately 650 nm and decreased to 230 nm after milling at 300 rpm for 3 h. After heat treatment at 973K for 1h, the milled powders became larger to approximately 550 nm in size again and the peaks of Mn2O3 disappeared in XRD patterns. In the samples after SPS, the Fe2O3 and MnZnFe2O4 phases decomposed at the higher temperatures than 1173K and 1373K, respectively, while only MnZnFe2O4 phase was detected in the samples conventionally sintered at 1273~1673K. As the sintering temperature increased, the relative density after SPS increased more quickly than that after conventional sintering. In particular, it reached approximately 99% after SPS at 1473K.
We investigated the effect of pre-sintering process on the penetration behavior of Dy in a NdFeB sintered magnet which was grain boundary diffusion treated with Cu/Al mixed Dy source. The pre-sintering of a magnet was performed at 900oC in vacuum and then the pre-sintered body was dipped in the solutions of DyH2, DyH2 + Cu, and DyH2 + Al, respectively. The dipped pre-sintered body were then fully sintered 4 hours at 1060oC followed by a subsequent annealing. The pre-sintering apparently improved the diffusivity of Dy atoms. The penetration of Dy into the magnet extended almost to 2,000 μm from the surface, about four times deeper than that of the normally sintered and diffusion treated one, when the DyH2 + Al solution was used as a Dy source. However, the resulting increase of coercivity was about 4 kOe, somewhat lower than that of the normally treated one, mostly due to excessive oxide formation that hindered to make a continuous Nd-rich grain boundary phase and a core-shell type structure.
Fe-40wt% TiB2 nanocomposites were fabricated by mechanical activation and spark-plasma sintering of a powder mixture of iron boride (FeB) and titanium hydride (TiH2). The powder mixture of (FeB, TiH2) was prepared by high-energy ball milling in a planetary ball mill at 700 rpm for 3 h followed by spark-plasma sintering (SPS) at various conditions. Analysis of the change in relative sintered density and densification rate during sintering showed that a self-propagating high-temperature synthesis reaction occurs to form TiB2 from FeB and Ti. A sintered body with relative density higher than 98% was obtained after sintering at 1150°C for 5 and 15 min. The microstructural observation of sintered compacts with the use of FE-SEM and TEM revealed that ultrafine particulates with approximately 5 nm were evenly distributed in an Fe-matrix. A hardness value of 83 HRC was obtained, which is equivalent to that of conventional WC-20 Co systems.
The β-phase Titanium (β-Ti) alloys have been under the spotlight in the recent past for their use as biomedical prosthetic materials owing to their excellent properties such as low elastic modulus, high corrosion resistance and tensile strength. Recently, Niobium (Nb) has gained a lot of attention as a β-phase stabilizing element in Ti alloys to replace Vanadium (V) due to its excellent solubility in Ti, low elastic modulus and biocompatibility. In this work, low cost Ti-20Nb binary alloy has been fabricated via powder metallurgy procedures. The blended powder mixtures of Ti and Nb were sintered at 900°C for 20 mins by the Spark Plasma Sintering (SPS) with an applied uniaxial pressure of 40 MPa. The heating rate was fixed at 50°C/min. The sintered alloy was subject to heat treatments at 1200°C in vacuum condition for various time durations. The characterizations of microstructure obtained during this process were done using FE-SEM, EDS and XRD. By increasing heat treatment time, as understood, the volume of residual Nb particles was decreased resulting in accelerated diffusion of Nb into Ti. Micro hardness of the alloy increased from 340 to 355 HV with the increase in β phase content from 30 to 45%. The resultant alloys had relatively high densities and homogenized microstructures of dispersed lamellar β grains in α matrix.
New graphite tools were designed and produced to fabricate a semi-finished product from which nine cutting inserts were obtained in one spark plasma sintering process. As a result, WC-5Co cemented carbides were spark plasma sintered and the effect of various sintering parameters such as compacting pressure, heating rate and holding time on the main mechanical properties were investigated. It was shown that WC-5Co cemented carbides spark plasma sintered at 1200°C, 80 MPa, 400°C/min, for 5 min are characterized by the best relation of hardness (1861 ±10 HV30) and fracture toughness (9.30 MPa·m1/2). The microstructure of these materials besides the WC ceramic phase and Co binder phase consists of a synthesized Co3W3C complex phase. Comparison with a commercial WC-6Co cutting insert fabricated by conventional powder metallurgy techniques shows that spark plasma sintering is a very effective technique to produce materials characterized by improved mechanical properties.
The microstructure and corrosion properties of spark plasma sintered yttria dispersed and yttria free duplex and ferritic stainless samples were studied. Spark plasma sintering (SPS) was carried out at 1000°C by applying 50 MPa pressure with holding time of 5 minutes. Linear sweep voltammetry (LSV) tests were employed to evaluate pitting corrosion resistance of the samples. Corrosion studies were carried out in 0.5, 1 and 2 M concentration of NaCl and H2SO4 solutions at different quiet time of 2, 4, 6, 8 and 10 seconds. Yttria dispersed stainless steel samples show more resistance to corrosion than yttria free stainless steel samples. Pitting potential decreases with increase in reaction time from 2 to 10 seconds. Similarly, as concentration of NaCl and H2SO4 increases from 0.5 M to 2 M the corrosion resistance decrements due to the availability of more Cl¯ and SO4 2¯ ions at higher concentration.
The effects of carbon content on the austenite stability and strain-induced transformation of nanocrystalline Fe-11% Ni alloys were investigated using X-ray analysis and mechanical tests. The nanocrystalline FeNiC alloy samples were rapidly fabricated using spark plasma sintering because of the extremely short densification time, which not only helped attain the theoretical density value but also prevented grain growth. The increased austenite stability resulted from nanosized crystallites in the sintered alloys. Increasing compressive deformation increased the volume fraction of strain-induced martensite from austenite decomposition. The kinetics of the strain-induced martensite formation were evaluated using an empirical equation considering the austenite stability factor. As the carbon content increased, the austenite stability was enhanced, contributing to not only a higher volume fraction of austenite after sintering, but also to the suppression of its strain-induced martensite transformation.
The effects of different types of process control agents (PCA) on the microstructure evolution of Ni-based oxide dispersion-strengthened superalloy have been investigated. Alloy synthesis was performed on elemental powders having a nominal composition of Ni-15Cr-4.5Al-4W-2.5Ti-2Mo-2Ta-0.15Zr-1.1Y2O3 in wt % using high energy ball milling for 5 h. The prepared powders are consolidated by spark plasma sintering at 1000oC. Results indicated that the powder ball-milled with ethanol as PCA showed large particle size, low carbon content and homogeneous distribution of elemental powders compared with the powder by stearic acid. The sintered alloy prepared by ethanol as PCA exhibited a homogeneous microstructure with fine precipitates at the grain boundaries. The microstructural characteristics have been discussed on the basis of function of the PCA.