Comparative study of β-Si_3N_4 powders prepared by SHS sintered by spark plasma sintering and hot pressing

β-Si3N4 powders prepared by self-propagating high-temperature synthesis （SHS） with additions of Y2O3 and Al2O3 were sintered by spark plasma sintering （SPS）. The densification, microstructure, and mechanical properties of Si3N4 ceramics prepared using this method were compared with those obtained by hot pressing process. Well densified Si3N4 ceramics with finer and homogeneous microstructure and better mechanical properties were obtained in the case of the SPS technique at 200°C lower than that of hot pressing. The microhardness is 15.72 GPa, the bending strength is 716.46 MPa, and the fracture toughness is 7.03 MPa·m1/2.

Microstructures of mechanically activated Ti-46at.%Al powders and spark plasma sintered ultrafine TiAl alloy

Powder of Ti-46at.%Al was synthesized through mechanical activation （MA） for different milling times, and the 16 h MAed powder was sintered by using a spark plasma sintering （SPS） process at different sintering temperatures. The XRD profiles showed that the MAed Ti-46at,%Al powder for 12, 16, and 20 h contained initial α-Ti and Al phases, and that the SPSed TiAl alloys contained the gamma TiAl and α2-Ti3Al phases. The TEM showed two different types of regions in the 16 h MAed Ti-46at.%Al powder. One type consisted of only Al with a grain size about 80 nm, and the other type a mixture of Al and Ti with a grain size of 30 nm. According to the optical micrographs of MA-SPSed samples, the alloys sintered at higher temperatures showed a coarser microstructure. In the case of the 1473 Ksintering, typical duplex structures （（α2 ＋γ） lamella and γ phases） with interlamellar spacings of 50-400 nm and the grain size either less than 100 nm, or 1000 nm were observed.

Microstructure and fracture toughness of a TiAl-Nb composite consolidated by spark plasma sintering

A TiAl-Nb composite was prepared by spark plasma sintering （SPS） at 1250 °C and 50 MPa for 5 min from prealloyed TiAl powder and elemental Nb powder in a molar ratio of 9：1 for improving the fracture toughness of TiAl alloy at room temperature. The microstructure, phase constitute, fracture surface and fracture toughness were determined by X-ray diffractometry, electron probe micro-analysis, scanning and transmission electron microscopy and mechanical testing. The results show that the sintered samples mainly consist of γ phase, O phase, niobium solid solution （Nbss） phase and B2 phase. The fracture toughness is as high as 28.7 MPa？m1/2 at room temperature. The ductile Nbss phase plays an important role in absorbing the fracture energy in front of the cracks. Moreover, B2 phase can branch the propagation of the cracks. The microhardness of each phase of the composite was also tested.

Microstructure and mechanical properties of Ti-45Al-5.5(Cr,Nb,B,Ta) alloy sintered at different SPS temperatures

TiAl alloy bulk samples with the composition of Ti-45Al-5.5(Cr,Nb,B,Ta) (mole fraction, %) were prepared by high energy mechanical milling and spark plasma sintering (SPS) and then heat treatment. The microstructure and mechanical properties after heat treatment of TiAl alloy prepared by SPS at different temperatures were studied. The results showed that the morphology of high energy mechanically milled powder was irregular and the average grain size was about decades micrometers. X-ray diffraction analysis showed that the mechanically milled powder was composed of two phases of TiAl and Ti3Al. The main phase of TiAl and few phases of Ti3Al and TiB2 were observed in the SPS bulk samples of Ti-45Al-5.5(Cr,Nb,B,Ta) alloy. For samples sintered at 900 °C and 1000 °C, the microstructure was duplex structure with some fine equiaxed gamma grains and thin needly TiB2 phases. With the SPS temperature increasing from 900 °C to 1000 °C, the micro-hardness was changed little, the compression strength increased from 1812 MPa to 2275 MPa and the compression ratio increased from 22.66% to 25.59%. The fractography results showed that the compression fracture transform of the SPS Ti-45Al-5.5(Cr,Nb,B,Ta) alloy was rgranular rupture.

High-temperature mechanical properties and deformation behavior of high Nb containing TiAl alloys fabricated by spark plasma sintering

A high Nb containing TiA1 alloy was prepared from the pre-alloyed powder of Ti-45Al-8.5Nb-0.2B-0.2W-0.02Y （at%） by spark plasma sintering （SPS）. Its high-temperature mechanical properties and compressive deformation behavior were investigated in a temperature range of 700 to 1050℃ and a strain rate range of 0.002 to 0.2 s 1. The results show that the high-temperature mechanical properties of the high Nb containing TiA1 alloy are sensitive to deformation temperature and strain rate, and the sensitivity to strain rate tends to rise with the deformation temperature increasing. The hot workability of the alloy is good at temperatures higher than 900℃, while fracture occurs at lower temperatures. The flow curves of the samples compressed at or above 900℃ exhibit obvious flow softening after the peak stress. Un- der the deformation condition of 900-1050℃ and 0.002-0.2 s 1, the interrelations of peak flow stress, strain rate, and deformation tempera- ture follow the Arrhenius＇ equation modified by a hyperbolic sine function with a stress exponent of 5.99 and an apparent activation energy of 441.2 kJ.mol-1.

Process optimization,microstructures and mechanical/thermal properties of Cu/Invar bi-metal matrix composites fabricated by spark plasma sintering

An orthogonal experiment scheme was designed to investigate the effects of the Cu content,compaction pressure,and sintering temperature on the microstructures and mechanical and thermal properties of(30−50)wt.%Cu/Invar bi-metal matrix composites fabricated via spark plasma sintering(SPS).The results indicated that as the Cu content increased from 30 to 50 wt.%,a continuous Cu network gradually appeared,and the density,thermal conductivity(TC)and coefficient of thermal expansion of the composites noticeably increased,but the tensile strength decreased.The increase in the sintering temperature promoted the Cu/Invar interface diffusion,leading to a reduction in the TC but an enhancement in the tensile strength of the composites.The compaction pressure comprehensively affected the thermal properties of the composites.The 50wt.%Cu/Invar composite sintered at 700℃ and 60 MPa had the highest TC(90.7 W/(m·K)),which was significantly higher than the TCs obtained for most of the previously reported Cu/Invar composites.

Microstructures and mechanical properties of TiAl alloy prepared by spark plasma sintering

A fine-grained TiAl alloy with a composition of Ti-47%Al(mole fraction)was prepared by double mechanical milling(DMM)and spark plasma sintering(SPS).The relationship among sintering temperature,microstructure and mechanical properties of Ti-47%Al alloy was studied by X-ray diffractometry(XRD),scanning electron microscopy(SEM)and mechanical testing.The results show that the morphology of double mechanical milling powder is regular with size of 20-40μm.The main phase TiAl and few phases Ti3Al and Ti2Al were observed in the SPS bulk samples.For samples sintered at 1 000℃,the equiaxed crystal grain was achieved with size of 100-250 nm.The samples exhibited compressive and bending properties at room temperature with compressive strength of 2 013 MPa,compression ratio of 4.6%and bending strength of 896 MPa.For samples sintered at 1 100 ℃,the size of equiaxed crystal grain was obviously increased.The SPS bulk samples exhibited uniform microstructures,with equiaxed TiAl phase and lamellar Ti3Al phase were observed.The samples exhibited compressive and bending properties at room temperature with compressive strength of 1 990 MPa,compression ratio of 6.0%and bending strength of 705 MPa.The micro-hardness of the SPS bulk samples sintered at 1 000℃is obviously higher than that of the samples sintered at 1 100℃.The compression fracture mode of the SPS TiAl alloy samples is intergranular fracture and the bending fracture mode of the SPS TiAl alloy samples is intergranular rupture and cleavage fracture.

Spark Plasma Sintering Properties of Ultrafine Ti(C,N)-based Cermet

Ultrafine Ti(C,N)-based cermet was sintered by SPS from 1050℃ to 1450℃ and its sintering properties,such as porosity,mechanical properties and phase transformation,were investigated by optical microscopy (OM),scanning electron microscopy (SEM),X-ray diffraction (XRD),and differential scanning calorimeter (DSC).It is found that the spark plasma sintering properties of Ti(C,N)-based cermet differ from those of conventional vacuum sintering.The liquid phase appearance is at least lower by 150℃ than that in vacuum sintering.The porosity decreases sharply below 1 200℃ and reaches minimum at 1 200℃,and afterwards it almost keeps invariable and no longer increases.SPS remarkably accelerates the phase transformation of Ti(C,N)-based cermet and it has a powerful ability to remove oxides in Ti(C,N)-based cermets.Above 1 350℃,denitrification occurred.Fresh graphite phase formed above 1 430℃.Both the porosity and graphite are responsible for the poor TRS.

Microstructure and properties of high-fraction graphite nanoflakes/6061Al matrix composites fabricated via spark plasma sintering

30-50 wt.%graphite nanoflakes(GNFs)/6061Al matrix composites were fabricated via spark plasma sintering(SPS)at 610℃.The effects of the sintering pressure and GNF content on the microstructure and properties of the composites were investigated.The results indicated that interfacial reactions were inhibited during SPS because no Al4C3 was detected.Moreover,the agglomeration of the GNFs increased,and the distribution orientation of the GNFs decreased with increasing the GNF content.The relative density,bending strength,and coefficient of thermal expansion(CTE)of the composites decreased,while the thermal conductivity(TC)in the X−Y direction increased.As the sintering pressure increased,the GNFs deagglomerated and were distributed preferentially in the X−Y direction,which increased the relative density,bending strength and TC,and decreased the CTE of the composites.The 50wt.%GNFs/6061Al matrix composite sintered at 610℃ under 55 MPa demonstrated the best performance,i.e.,bending strength of 72 MPa,TC and CTE(RT−100℃)of 254 W/(m·K)and 8.5×10^(−6)K^(−1)in the X−Y direction,and 55 W/(m·K)and 9.7×10^(−6)K^(−1)in the Z direction,respectively.

Microstructure and Properties of W-15Cu Alloys Prepared by Mechanical Alloying and Spark Plasma Sintering Process

W-15Cu composite powders prepared by mechanical alloying （MA） of raw powders were consolidated by spark plasma sintering （SPS） process at temperature ranged 1 230-1 300 ℃ for 10 min and under a pressure of 30 MPa. By using high energy milling, particles containing very fine tungsten grains embedded in copper, called composite particles, could be produced. The W grains were homogeneously dispersed in copper phase, which was very important to obtain W-Cu alloy with high mechanical properties, fine and homogeneous microstructure. The microstructure and properties of W-15Cu alloys prepared by SPS processes at different temperature were researched. The results show that W-15Cu alloys consolidated by SPS can reach 99.6 % relative density, and transverse rupture strength （TRS） is 1 400.9 MPa, Rockwell C hardness （HRC） is 45.2, the thermal conductivity is 196 W/m-K at room temperature, the average grain size is less than 2 μm, and W-15Cu alloy with excellent properties, homogeneous and fine microstructure is obtained.

Synthesis and Sintering of Mg_2Si Thermoelectric Generator by Spark Plasma Sintering

Raw Mg,Si powder were used to fabricate Mg2Si bulk thermoelectric generator by spark plasma sintering （SPS）.The optimum parameters to synthesize pure Mg2Si powder were found to be 823 K,0 MPa,10 min with excessive content of 10wt% Mg from the stoichiometric Mg2Si.Mg2Si bulk was synthesized and densified simultaneously at low temperature （823 K） and high pressure （higher than 100 MPa） from the raw powder,but Mg,Si could not react completely,and the sample was not very dense with some microcracks on the surface.Then,Mg,Si powder reacted at 823 K,0 MPa,10 min in SPS chamber to form Mg2Si green compact,again sintered by SPS at 1023 K,20 MPa,5 min.The fabricated sample only contained Mg2Si phase with fully relative density.

Densification,microstructure,and fracture behavior of TiC/Si_3N_4 composites by spark plasma sintering

TiC/Si3N4 composites were prepared using the β-Si3N4 powder synthesized by self-propagating high-temperature synthesis （SHS） and 35 wt.% TiC by spark plasma sintering. Y2O3 and Al2O3 were added as sintering additives. The almost full sintered density and the highest fracture toughness （8.48 MPa·m1/2） values of Si3N4-based ceramics could be achieved at 1550℃. No interfacial interactions were noticeable between TiC and Si3N4. The toughening mechanisms in TiC/Si3N4 composites were attributed to crack deflection, microcrack toughening, and crack impedance by the periodic compressive stress in the Si3N4 matrix. However, increasing microcracks easily led to excessive connection of microcracks, which would not be beneficial to the strength.

Structure evolution of cubic boron nitride under spark plasma sintering

Cubic boron nitride(CBN) micro powders and mixture of CBN micro powders with Al or Ti powders were fast heated at 1 300,1 400,1 450,1 500℃,and then kept for 5 min under spark plasma sintering (SPS).The obtained powders were analyzed with XRD.The results show that,simple CBN kept cubic structure after heated at 1 300℃;when the temperature rose to 1 400℃,some CBN was transformed into hexagonal structured boron nitride(hBN).As for CBN micro powders mixed with aluminum or titanium micro powders,the onset transforming temperature of CBN to hBN get raised.This results indicated that the structural transformation of boron nitride begun from the surface of CBN crystal particle,different coexist elements affect the surface situation of CBN particles.As the stabilities of CBN crystal particle surface improved,the onset structural transform temperature of CBN was also increased.

Effect of Annealing Process on Microstructure and Mechanical Properties of Ultrafine Copper Prepared by Spark Plasma Sintering

The spark plasma sintering （SPS） method is used to prepare the ultrafine copper with the average grain size less than 10 μm and the tensile strength greater than 280 MPa.The ultrafine copper is annealed at different temperatures for 60 min,and the annealing microstructure is observed and the hardness and the deformation behavior of the bulk copper are tested.The results indicate that the grains grow very slowly when the annealing temperature is less than 450 ℃.However,the grain growth becomes remarkable when the annealing temperature exceeds 450 ℃.And the plasticity of the bulk copper is the best when the annealing temperature of 450 ℃ is adopted.After stamping and spin forming,the deformed copper is recrystallized completely and the grain is refined when the copper is annealed at 500 ℃ for 30 min.

Temperature Field Distribution in Spark Plasma Sintering of BN

This paper studies the temperature distribution of BN, an insulating material, sintered in the Spark Plasma Sintering ( SPS) system. The temperature distributions of BN at different heating rates were measured , which showed that seeking for an over high heating rate in SPS is not as desirable as controlling of a suitable heating rate in order to have a fast sintering with a uniform temperature distribution.

Porous Alumina Ceramics Fabricated by Spark Plasma Sintering

Porous alumina of regular spherical particles was fabricated with the spark plasma sintering （SPS） and then compared to those obtained through conventional hot pressing （HP）. The effects of the parameters of the heating process on porosity were also investigated, Microstructural studies suggest that porous ingots including regular pores be made out of regular spherical alumina particles due to the close sphere packages. A comparative study on the relative necks of the specimens produced by SPS and HP indicates an enhancement of neck growth with SPS. Contrasting the theoretical values to the experimental results over the relative necks indicates that a proper relationship between the relative necks and the porosity can be established by a sintering model.

The Densification of Cu/Ti System by Spark Plasma Sintering

In order to unclose the dynamics of SPS densification, a special sintering sample (Cu/Ti wires compact) was designed. Characters of the shrinkage rates during sintering process and microstructures of products fabricated by the spark plasma sintering(SPS) and hot-press sintering were investigated. The experimental results reveal that a higher temperature field is formed at the connected area and conductive net of the compact. These high-temperature parts deformed more easily than other parts, which is believed to be the main cause of SPS fast densification, according to a hard-core and soft-hell material model.

Spark Plasma Sintering Bulk Sm2 Fe17NxMagnets

High performance Sm2Fe17Nx magnetic powders were fabricated by ball-milling method and were compacted using spark plasma sintering(SPS) technique.Effects of processing conditions on the magnetic properties and decomposition dynamic of the magnets were investigated.It is found that higher sintering temperature improves the densification of the magnets, while deteriorates their magnetic properties simultaneously due to the decomposition of the Sm2Fe17Nx.Sintering at lower temperature can preserve the crystal structure of Sm2Fe17Nx compound, while the powders cannot be consolidated into a fully dense compact.An increased compressive pressure leads to better magnetic properties and higher density for the magnet at the same sintering temperature.

Corrosion behaviors of NdFeB magnets prepared by spark plasma sintering

The spark plasma sintering (SPS) technique was introduced into the field ofNdFeB preparation due to its own advantages. High property NdFeB magnets with fine grains wereprepared by SPS method. The corrosion behaviors of SPS NdFeB were studied by electrochemicalmeasurements and 92 percent RH hyther tests at 353 K. The results were compared with those of thetraditional sintered NdFeB magnets. It shows that both the SPS NdFeB and the traditional sinteredNdFeB have good corrosion resistance in alkaline environment due to surface passivation; while, thefine grain microstructure of SPS NdFeB results in a more homogeneous phase composition distributionand thus reduces the electrochemical inhomogenity between the ferromagnetic phase and the Nd-richinter-granular phase in the magnet. Therefore, the SPS NdFeB exhibits better corrosion resistancethan the traditional sintered NdFeB in neutral and weak acidic environment.

Microstructure and properties of p-type (Bi_(0.25)Sb_(0.75))_2Te_3 fabricated by spark plasma sintering

P-type thermoelectric material(Bi0.25Sb0.75)2Te3 was sintered by spark plasma sintering(SPS) process in the temperature range of 320-420 ℃. The microstructures of sintered materials were found to be well aligned,particularly when sintered at lower sintering temperatures. The electrical conductivity of the material became larger as the sintering temperature increased. The Seebeck coefficient showed a general decreasing tendency with an increase in sintering temperature. In terms of the power factor,the optimum sintering temperature was found to be 380 ℃ for a maximum value of around 2.6 mW/K.