Mechanochemical synthesis and spark plasma sintering of hafnium carbonitride ceramics

Submicron powder of non-stoichiometric hafnium carbonitrides (HC_0.5N_0.2) was fabricated by the mechanochemical synthesis method. It was shown that during the first milling stages, primarily reaction between hafnium and carbon took place. The nitridation occurred later when fresh metal surfaces started to form through defragmentation of the brittle layer of a carbon-solid solution. The synthesized powder was consolidated by spark plasma sintering approach to producing dense bulk hafnium carbonitride ceramics. Hardness and fracture toughness measured on consolidated samples were 20.8 ± 1 GPa и 3.5 ± 0.2 MPa?m^1/2, respectively. The obtained results were compared with previously reported data.     

Rapid synthesis of Ti alloy with B addition by spark plasma sintering

The in situ TiB/Ti–4.0Fe–7.3Mo composites were fabricated by plasma spark sintering (SPS) technique using mechanical alloying of Ti, Fe65Mo and B powder. The effects of sintering temperature on densification of the composites and microstructure of the in situ synthesized TiB were investigated using scanning electron microscope (SEM) and transmission electron microscope (TEM). A dense composite was obtained after sintering at 1000 °C for 5 min. Under proper ball milling and SPS conditions in situ TiB reinforced Ti–4.0Fe–7.3Mo composites have been prepared. The in situ TiB showed a typical needle shape grow along [0 1 0] direction. The transverse cross-section of TiB grain is a hexagonal shape with the planes of (1 0 0), (1 0 1) and . The stacking faults in the (1 0 0) plane were observed in the TiB needles.     

Low-temperature spark plasma sintering of NiO nanoparticles

NiO nanoparticles of 20 nm in diameter were spark plasma sintered between 400 °C and 600 °C for 5 and 10 min durations. Application of 100 MPa pressure from room temperature resulted in densities between 75% and 92%. The final grain size was between 26 nm and 68 nm. Lower densities were recorded when 100 MPa was applied at the SPS temperature. Two shrinkage rate maxima of ∼3.4 × 10⁻³ s⁻¹ and ∼2 × 10⁻³ s⁻¹ were observed around 390 ± 10 °C and at the SPS temperature. The two shrinkage rate maxima were related to densification by particle sliding followed by diffusional grain boundary sliding during the heating. The strong effects of the surface and interfacial processes which are active during the SPS were highlighted.     

Effect of Re on microstructural evolution and densification kinetics during spark plasma sintering of nanocrystalline W

In the present investigation, nanocrystalline W and W-xRe (x = 3, 5 wt.%) alloy powders were produced by mechanical milling/alloying using high energy ball milling. The nanocrystalline nature (∼50 nm) of these powders was validated by the Rietveld refinement of their respective X-Ray diffraction patterns. Subsequently, spark plasma sintering of the ball milled powders was carried out. It was observed that pure W was not able to densify completely (relative density of 93%) at a temperature of 1500 °C. However, the addition of 5 wt.% Re resulted in near complete densification (relative density of 97%) at the same sintering temperature. The enhanced densification of W-Re powders is mainly attributed to the ductilising effect of Re assisted by the nanocrystallinity of powders, and the application of pressure during sintering.     

Microstructure and thermal conductivity of spark plasma sintering AlN ceramics

Abstract

Dense aluminium nitride ceramics were prepared by spark plasma sintering at a lower sintering temperature of 1700°C with Y₂O₃, Sm₂O₃ and Dy₂O₃ as sintering additives respectively. The effects of three kinds of sintering additives on the phase composition, microstructure and thermal conductivity of AlN ceramics were investigated. The results showed that those sintering additives not only facilitated the densification via the liquid phase sintering mechanism, but also improved thermal conductivity by decreasing oxygen impurity. Sm₂O₃ could effectively improve thermal conductivity of AlN ceramics compared with Y₂O₃ and Dy₂O₃. Observation by scanning electron microscopy showed that AlN ceramics prepared by spark plasma sintering method manifested quite homogeneous microstructures, but AlN grain sizes and shapes and location of secondary phases varied with the sintering additives. The thermal conductivity of AlN ceramics was mainly affected by the additives through their effects on the growth of AlN grain and the location of secondary phases.     

Processing of porous Ti and Ti5Mn foams by spark plasma sintering

Titanium and its alloys are one of the best metallic biomaterials to be used for implant application. In this study, porous Ti and Ti5Mn alloy with different porosities were successfully synthesized by powder metallurgy process with the addition of NH₄HCO₃ as space holder and TiH₂ as foaming agent. The consolidation of powder was achieved by spark plasma sintering process (SPS) at 16 MPa and pressureless conditions. The morphology of porous structure was investigated by using scanning electron microscopy (SEM) and X-ray micro-tomography (μ-CT). Nano-indentation tester was used to evaluate Young’s modulus of the porous Ti and Ti5Mn alloy. Experimental results showed that pure Ti sample, which sintered under pressure of 16 MPa, full relative density was achieved even at a relative low sintering temperature 750 °C; however, in the case of pressureless condition at sintering temperature 1000 °C the porosity was 53% and Young’s modulus was 40 GPa. The Ti5Mn alloy indicated a good pore distribution, and the porosity decreased from 56% to 21% by increasing the sintering temperature from 950 °C to 1100 °C. Young’s modulus was increased from 35 GPa to 51.83 GPa with increasing of the sintering temperatures from 950 °C to 1100 °C.     

A comparative study of nickel and alumina sintering using spark plasma sintering (SPS)

Nickel and alumina powders with particle sizes of 4.3 μm and 108 nm, respectively, have been sintered in moulds of different sizes. Only the diameter (inner and/or outer) of moulds has been varied. The dimension modification is responsible for sample microstructure variation because set temperature, heating rate, dwell time and pressure were identical in all experiments. The influence of the die (or sample) dimension on the sample microstructure appears to depend strongly on the electric characteristics of the powder. The present paper is an attempt to correlate the bulk microstructure evolution with the die and sample size and the electrical current distribution within the system.     

Joining of AlN and graphite disks using interlayer tapes by spark plasma sintering

AlN and graphite disks were successfully joined using a polymer plasticized ceramic tape as the interlayer by spark plasma sintering (SPS). The tape contains either composite powders of AlN and graphite or AlN powders without graphite. Both tapes contained 5 mass% Y₂O₃ as the sintering aid of AlN. The joining was carried out at 1700–1900 °C and 30 MPa for 5 min. No other reaction phase except for Al₂Y₄O₉ was identified in the joints. The maximum tensile strength of the joints was obtained when the AlN–graphite composite interlayer tape was used. The joining mechanism is attributed not to the chemical bonding, but to the physical bonding of the Al₂Y₄O₉ phase, which is solidified from the molten Al–Y–O squeezing into the porous graphite under pressure during SPS.     

Effect of particle size on densification of pure magnesium during spark plasma sintering

The effect of particles size ranges (<38 μm, 75–150 μm, 270–550 μm) of atomized magnesium powders on densification mechanisms during spark plasma sintering (SPS) process was investigated. The intrinsic driving force, local pressure and current of Mg powders with different particle sizes were analyzed by theoretical calculation. The results obviously indicate that the densification of pure magnesium can be improved by the reduction of particle size, suggesting the intrinsic driving force, local pressure and current intensity are enhanced significantly by a decrease in the particle size at the same sintering conditions, which can promote shrinkage of pores, formation of the sintering neck and mass transportation in the SPS process. Not only that, rapid densification is also interpreted in term of mechanical movement of particles, Joule heating effect and plastic deformation. However, the mechanical movement of the large particles is higher than that of small particles due to high punch displacement, and plastic deformation, detected by scanning electron microscopy, plays a main role in densification for large particles in the case during the sintering. Joule heating effect is the key factor for densification of small Mg particles, and high densification degree can be obtained by sintering small particles.     

Partially alloyed filler sheet for brazing of Ti and its alloys fabricated by spark plasma sintering method

Partially alloyed filler metals in the form of powders and laminated foils were used for the brazing of Ti and Ti alloys to lower the manufacturing cost. In this study, by using a raw elemental powder mixture, a multi-component filler sheet with a nominal composition of 37.5Ti–37.5Zr–15Cu–10Ni was fabricated using a Spark Plasma Sintering (SPS) machine in the temperature range from 650 °C to 785 °C for 1 min. As the sintering temperature was increased from 650 °C to 750 °C, the bending strength of the sheets tended to rise, but the bending strength at 785 °C was drastically reduced. The melting range of the sheets became similar to that of the as-cast alloy. The sheets sintered at 750 °C showed the highest bending strength of 259 MPa, which was much higher than that of the as-cast material, and the melting range of this sheet was from 800 °C to 852 °C. The relatively high strength of the sheet was due to the remaining elemental powders such as Ti or Zr, but the brittle intermetallics, such as Ti₂Cu and (Ti,Zr)₂Ni Laves phases, formed in the sheet during the sintering process deteriorated its mechanical strength. The partially developed eutectic phase between the remaining Ti or Zr powder caused the sheet to exhibit melting behavior similar to that of the as-cast alloy. The brazability of the sheet sintered at 750 °C was examined with commercially pure Ti at 870 °C for 5–60 min. The tensile strength of the Ti joint brazed for 30 min was 431 MPa, which was close to that of the base metal.