One of the ways to decrease thermal conductivity is nano structurization. Cobalt triantimonide (CoSb3) samples with added indium or tellurium were prepared by the direct fusion technique from high purity elements. Ingots were pulverized and re-compacted to form electrodes. Then, the pulsed plasma in liquid (PPL) method was applied. All materials were consolidated using rapid spark plasma sintering (SPS). For the analysis, methods such as X-ray diffraction (XRD), scanning electron microscopy (SEM) and scanning transmission electron microscopy (STEM) with a laser flash apparatus (LFA) were used. For density measurement, the Archimedes’ method was used. Electrical conductivity was measured using a standard four-wire method. The Seebeck coefficient was calculated to form measured Seebeck voltage in the sample placed in a temperature gradient. The preparation method allowed for obtaining CoSb3 nanomaterial with significantly lower thermal conductivity (10 Wm–1K–1 for pure CoSb3 and 3 Wm–1K–1 for the nanostructured sample in room temperature (RT)). The size of crystallites (from SEM observations) in the powders prepared was about 20 nm, joined into larger agglomerates. The Seebeck coefficient, α, was about –200 µVK–1 in the case of both dopants, In and Te, in microsized material and about –400 µVK–1 for the nanomaterial at RT. For pure CoSb3, α was about 150 µVK–1 and it stood at –50 µVK–1 for nanomaterial at RT. In bulk nanomaterial samples, due to a decrease in electrical conductivity and inversion of the Seebeck coefficient, there was no increase in ZT values and the ZT for the nanosized material was below 0.02 in the measured temperature range, while for microsized In-doped sample it reached maximum ZT = 0.7 in (600K).
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.
In the paper the multiferroic (ferroelectric-ferromagnetic) composites based on ferroelectromagnetic/ferroelectric (BaFe1/2Nb1/2O3 (BFN)) powder and ferrite powder (zinc-nickel ferrite) were obtained by two technological methods. In the composite samples the ratio of the ferroelectromagnetic/ferroelectric powder to the magnetic powder was equal to 90:10. The ceramic powders were synthesized by the classical technological method using powder calcination/solid state synthesis, while densification of the composite powders (sintering) was carried by two different methods: (i) Free Sintering method (FS), and (ii) Spark Plasma Sintering (SPS).
At the work, a comparison of measurement results for composite samples obtained by two sintering methods was made. The studies included the following analysis: DTA, XRD, SEM, DC electrical conductivity, electric permittivity and magnetic properties. The result of measurements presented in the work revealed that the ceramic composite obtained by two different technological sintering method (classical technology – Free Sintering method and Spark Plasma Sintering technique) can be promising lead-free materials for functional applications, for example in sensors for magnetic and electric field.
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.
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.
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 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.
The dispersion of nanoparticles in the host matrix is a novel approach to enhance the thermoelectric performance. In this work, we incorporate the TiC (x = 0, 1 and 2 wt.%) nanoparticles into a p-type Bi0.5Sb1.5Te3 matrix, and their effects on microstructure and thermoelectric properties were systematically investigated. The existence of TiC contents in a base matrix was confirmed by energy dispersive X-ray spectroscopy analysis. The grain size decreases with increasing the addition of TiC content due to grain boundary hardening where the dispersed nanoparticles acted as pinning points in the entire matrix. The electrical conductivity significantly decreased and the Seebeck coefficient was slightly enhanced, which attributes to the decrease in carrier concentration by the addition of TiC content. Meanwhile, the lowest thermal conductivity of 0.97 W/mK for the 2 wt.% TiC nanocomposite sample, which is ~16% lower than 0 wt.% TiC sample. The maximum figure of merit of 0.90 was obtained at 350 K for the 0 wt.% TiC sample due to high electrical conductivity. Moreover, the Vickers hardness was improved with increase the addition of TiC contents.
In this work, the 316L austenitic steel based milled and sintered composites with 0.33 wt% and 1 wt% SiC ultra-fine particles addition have been prepared. The high efficient attrition milling provided an efficient size reduction of the 316L steel grains and homogeneous distribution of the SiC nanoparticles before sintering process. Spark plasma sintering (SPS) was used for compaction of milled powder mixtures. The effect of SiC addition on the milling efficiency and the structure of the composites have been studied. It was found that the amount of ceramic addition did not influence the efficiency of milling process, powder mixtures with flake like grains have been obtained. On the other hand, the intensive milling assured an optimal coverage of 316L stainless steel grains with submicron sized ceramic particles in both cases. The sintered composites showed high densities with the presence of small amount of closed porosities. Structural, mechanical and tribological examinations of 316L/SiC composites have been performed and presented.
The effect of TiC content on the microstructure and mechanical properties of a nanocrystalline Fe-Mn alloy was investigated by XRD analysis, TEM observation, and mechanical tests. A sintered Fe-Mn alloy sample with nano-sized crystallites was obtained using spark plasma sintering. Crystallite size, which is used as a hardening mechanism, was measured by X-ray diffraction peak analysis. It was observed that the addition of TiC influenced the average size of crystallites, resulting in a change in austenite stability. Thus, the volume fraction of austenite at room temperature after the sintering process was also modified by the TiC addition. The martensite transformation during cooling was suppressed by adding TiC, which lowered the martensite start temperature. The plastic behavior and the strain-induced martensite kinetics formed during plastic deformation are discussed with compressive stress-strain curves and numerical analysis for the transformation kinetics.
We investigated the austenite stability and mechanical properties in FeMnNiC alloy fabricated by spark plasma sintering. The addition of Mn, Ni, and C, which are known austenite stabilizing elements, increases its stability to a stable phase existing above 910°C in pure iron; as a result, austenitic microstructure can be observed at room temperature, depending on the amounts of Mn, Ni, and C added. Depending on austenite stability and the volume fraction of austenite at a given temperature, strain-induced martensite transformation during plastic deformation may occur. Both stability and the volume fraction of austenite can be controlled by several factors, including chemical composition, grain size, dislocation density, and so on. The present study investigated the effect of carbon addition on austenite stability in FeMnNi alloys containing different Mn and Ni contents. Microstructural features and mechanical properties were analyzed with regard to austenite stability.
Due to air pollution, global warming and energy shortage demands new clean energy conversion technologies. The conversion of industrial waste heat into useful electricity using thermoelectric (TE) technology is a promising method in recent decades. Still, its applications are limited by the low efficiency of TE materials in the operating range between 400-600 K. In this work, we have fabricated Cu0.005Bi0.5Sb1.495Te3 powder using a single step gas atomization process followed by spark plasma sintering at different temperatures (623, 673, 723, and 773 K), and their thermoelectric properties were investigated. The variation of sintering temperature showed a significant impact on the grain size. The Seebeck coefficient values at room temperature increased significantly from 127 μVK to 151 μV/K with increasing sintering temperature from 623 K to 723 K due to decreased carrier concentration. The maximum ZT values for the four samples were similar in the range between 1.15 to 1.18 at 450 K, which suggest these materials could be used for power generation in the mid-temperature range (400-600 K).