Papers by Keyword: Spark Plasma Sintering (SPS)

Abstract: This paper reported results of an investigation aiming at finding what affected the orientated grain growth of Bismuth titanate niobate (Bi3TiNbO9) by spark plasma sintering process (SPS). Single phase of textured Bi3TiNbO9 (BTNO) ceramics were prepared by a two-step sintering method: synthesizing seed-crystal platelets by molten-salt method with oxide mixture as precursors and then sintering the platelets under different SPS conditions such as heating rate, holding time, sintering temperature and pressure, etc. The possible effects of these factors upon the textured microstructure have been analyzed in detail. Textured Bi3TiNbO9 ceramics with different orientation degree was obtained by controlling the conditions during SPS process.

Abstract: The fabrication of MB2-SiC and MB2-MC-SiC (M=Zr, Hf, Ta) Ultra High Temperature Ceramics (UHTCs) is investigated in this work by combining Self-propagating High-temperature Synthesis (SHS) and Spark Plasma Sintering (SPS). Zr, Hf or Ta, B4C, Si, and graphite powders are first reacted by SHS to successfully form in-situ the desired composites. For the case of the Tabased systems, a 20 min ball milling treatment is also required to mechanically activate the SHS reactions. The resulting powders are subsequently consolidated by SPS at 1800 °C and P=20 MPa, thus obtaining products with densities greater than 96% within 30 min of total processing time. Hardness, fracture toughness, and oxidation resistance of the resulting dense UHTCs are among the best when compared to the corresponding values reported in the literature relative to analogous products synthesized by alternative, more energy-consuming and less rapid methods. Thermogravimetric analysis results evidenced the beneficial effect of SiC on the oxidation resistance of the composite materials, while the presence of transition metal carbides appears to be inconvenient from this point of view. This is because, they rapidly oxidize at high temperature to form MxOy and carbon oxides which lead to an increase in sample porosity thus enhancing product oxidation.

Abstract: Functionally Grated Materials (FGMs) have usually been expected as candidates for a wide variety of industrial applications due to their desirable properties such as high heat resistance capability, good wear resistance, bio-compatibility, chemical stability and so on. Scaling-up and three dimensional (3-D) near-net shape forming technique for FGMs are one of the most important key-factor to produce the industrial engineering components and products in practical use. On the other hand, it is generally well known that the Spark Plasma Sintering (SPS) method is a novel process to produce homogeneous FGMs, nano-structural sintered compact, thermoelectric semiconductors and bio-medical materials in shorter sintering time with finer microstructure. This paper will present development of FGMs fabricated by SPS and future prospects of SPS on research and industrialization activities in Japan. A brief historical review progress of SPS technology is also given and the applicable field is exemplified. Then, the paper is focused on manufacturing processes on FGM by SPS technology.

Abstract: This study was carried out to produce and characterize B4C - TiB2 ceramics by spark plasma sintering. Initial B4C and TiB2 powders were mixed in ethanol solution with YSZ balls for 1 hour. Sintering was performed with 5, 10, 15 and 20 volume % TiB2 containing mixtures respectively in disc-shaped graphite dies. The applied pressure was 40 MPa at 1760 °C for 5 minute sintering duration. The improvement of low sinterability and low strength of B4C was investigated as well as strength of flexibility, hardness and fracture toughness. The obtained products were characterized by X-ray diffraction and SEM imaging. The hardness values were measured under 1000 g load and the density values were measured with Archimedes' principle. The 3-point bending tests and modulus of elasticity measurements were also conducted.

Abstract: The aim of this study was to produce dense and mechanically strong boron carbide ceramics with the help of different oxide additives. Physical properties of two different grades of pure boron carbide powders were analysed and sintered by Spark Plasma Sintering method. Starting powders were prepared by ball milling with the addition of 5 wt. % Y2O3, Al2O3, SiO2 and Y2O3 + Al2O3. In the sintering step, powder mixtures were sintered by SPS method in round-shaped graphite dies under 50 MPa for 5 minutes in the range of 1700-1800oC. In the characterization step, sintered sample compositions and microstructures were characterized by XRD and SEM analysis respectively. The hardness values were measured under 1000 g load and the density values were measured with Archimedes' principle. The fracture toughness analysis were also carried out.

Abstract: Nanocrystalline alumina (Al2O3) powders were sintered by Spark Plasma Sintering (SPS) method in a vacuum atmosphere to obtain highly dense and fine grained final ceramic products. In the first section of experiments, 0.4 % wt MgO doped and 0.4 wt % Y2O3 doped Al2O3 were sintered at high temperatures and under high pressure with a SPS system. Later sintering procedures were carried out with codoping Y2O3 with the cathodic ratio of 0.4 wt % in order to investigate dopant effects on spark plasma sintered alumina. The microstructures of all samples were observed using scanning electron microscope and the properties such as density, hardness and fracture toughness were examined.

Abstract: The densification mechanism during the park-plasma-sintering (SPS) processing was examined in high purity MgAl2O4 spinel. As the density ρt increases, that is, as the effective stress σeff decreases, stress exponent n evaluated from σeff dependence of densification rate varies from n ≥ 4 in the low ρt region, n ≈ 2 in the intermediate ρt region to n ≈ 1 in the high ρt region. TEM observation shows that significant stacking faults caused by partial dislocations are observed in the low ρt region, but limited in the high ρt region. The ρt dependent densification behavior and microstructure suggest that the predominant densification mechanism during the SPS processing changes with ρt from plastic flow by partial dislocation motion for the low ρt region (n ≥ 4) to diffusion-related creep for the high ρt region (n ≈ 1).

Abstract: A macro-scale model of spark plasma sintering (SPS) that couples electrical, thermal, stress-strain and densification components is presented. The continuum theory of sintering is incorporated enabling the evolution of the densification based on local conditions, thus a true spatial density distribution could be obtained. Specimen behavior is described through a non-linear viscous constitutive relation. The simulation is based on an FEM computer code. Several examples are shown and results are compared with experimental data available.

Abstract: Si3N4 based composites containing different amounts of SiC and SiAlON were produced by reactive spark plasma sintering of Si3N4, SiO2 and C black. Y2O3 and AlN were added as sintering additives. The SPS process was carried out at sintering temperature of 1650 0C for 5 min with uniaxial pressure of 40 MPa in a nitrogen atmosphere.The mechanic properties and morphology of Si3N4 ceramic composite were determined. Microstructures of the sintered samples were observed by SEM images and phase compositions were analysed by XRD.

Abstract: Magnesium powders were sintered by using spark plasma sintering (SPS) and conventional pressureless sintering (PLS) techniques at sintering temperatures ranged from 552°C to 605°C to investigate effect of sintering method on microstructure and mechanical properties of sintered magnesium. High densed magnesium could be obtained by using spark plasma sintering technique compared to conventional presureless sintering at the same sintering temperature. It was found that the ultimate tensile strength increased with increasing sintering temperature for both the materials sintered by PLS and SPS. The magnesium samples prepared by SPS showed better mechanical properties than those prepared by PLS. The microstructural observations revealed that the grain growth was not significant in SPS process compared to PLS, which would enhance the mechanical properties of the SPS sintered magnesium.