Spark plasma sintering of tungsten-based WTaVCr refractory high entropy alloys for nuclear fusion applications

W-based WTaVCr refractory high entropy alloys (RHEA) may be novel and promising candidate materials for plasma facing components in the first wall and diverter in fusion reactors. This alloy has been developed by a powder metallurgy process combining mechanical alloying and spark plasma sintering (SPS). The SPSed samples contained two phases, in which the matrix is RHEA with a body-centered cubic structure, while the oxide phase was most likely Ta2VO6through a combined analysis of X-ray diffraction (XRD),energy-dispersive spectroscopy (EDS), and selected area electron diffraction (SAED). The higher oxygen affinity of Ta and V may explain the preferential formation of their oxide phases based on thermodynamic calculations. Electron backscatter diffraction (EBSD) revealed an average grain size of 6.2μm. WTaVCr RHEA showed a peak compressive strength of 2997 MPa at room temperature and much higher micro-and nano-hardness than W and other W-based RHEAs in the literature. Their high Rockwell hardness can be retained to at least 1000°C.

One step sintering of homogenized bauxite raw material and kinetic study

A one-step sintering process of bauxite raw material from direct mining was completed, and the kinetics of this process was analyzed thoroughly. The results show that the sintering kinetics of bauxite raw material exhibits the liquid-phase sintering behavior. A small portion of impurities existed in the raw material act as a liquid phase. After X-ray diffraction analyses, scanning electron microscopy observations, and kinetics calculations, sintering temperature and heating duration were determined as the two major factors contributing to the sintering process and densification of bauxite ore. An elevated heating temperature and longer duration favor the densification process. The major obstacle for the densification of bauxite material is attributed to the formation of the enclosed blowhole during liquid-phase sintering.

Microstructure and properties of Ag–Ti_3SiC_2 contact materials prepared by pressureless sintering

Ti3SiC2-reintbrced Ag-maJxix composites are expected to serve as eleclrical contacts. In this study, the wettability of Ag on a Ti3SiC2 subslxate was measured by the sessile drop melkod. The Ag-Ti3SiC2 composites were prepared from Ag mad Ti3SiC2 powder mix- tures by pressureless sintering. The effects of compacting pressure （100-800 MPa）, sintering temperature （850-950~C）, mad soaking time （0.5-2 h） on the microslxucture mad properties of the Ag-Ti3SiC2 composites were investigated. The experimental results indicated that Ti3SiC2 paxticulates were uniformly distxibuted in flae Ag matrix, wiflaout reactions at the interthces between flae two phases. The prepared Ag-10wt%Ti3SiC2 had a relative density of 95% mad an electrical resistivity of 2.76 x 10 3 m~）＇cm when compacted at 800 MPa mad sintered at 950~C for 1 h. The incorporation of Ti3SiC2 into Ag was found to improve its hardness without substantially compromising its electrical conductivity; INs behavior was attxibuted to the combination of ceramic and metallic properties of the Ti3SiC2 reinforcement, suggesting its potential application in electrical contacts.

Effect of sintering temperature on the physical properties and electrical contact properties of doped AgSnO_2 contact materials

AgSnO_ 2 electrical contact materials doped with Bi_2O_3,La_2O_3,and TiO_2 were successfully fabricated by the powder metallurgy method under different initial sintering temperatures.The electrical conductivity,density,hardness,and contact resistance of the Ag Sn O_2/Bi_2O_3,AgSnO_2/La_2O_3,and AgSnO_2/Ti O_2 contact materials were measured and analyzed.The arc-eroded surface morphologies of the doped AgSnO_2 contact materials were investigated by scanning electron microscopy(SEM).The effects of the initial sintering temperature on the physical properties and electrical contact properties of the doped AgSnO_2 contact materials were discussed.The results indicate that the physical properties can be improved and the contact resistance of the AgSnO_2 contact materials can be substantially reduced when the materials are sintered under their optimal initial sintering temperatures.

Effects of silver powder particle size on the microstructure and properties of Ag-Yb_2O_3 electrical contact materials prepared by spark plasma sintering

mg-Yb203 electrical contact materials were fabricated by spark plasma sintefing （SPS）. The effects of silver powder particle size on the microstructure and properties of the samples were investigated. The surface morphologies of the sintered samples were examined by optical microscope （OM）, and the fracture morphologies were observed by scanning electron microscopy （SEM）. The physical and mechanical properties such as density, electrical resistivity, microhardness, and tensile strength were also tested. The results show that the silver powder particle size has evident effects on the sintered materials. Comparing with coarse silver powder （5 ktm）, homogeneous and fme microstmcture was obtained by fine silver powder （_〈0.5-1am）. At the same time, the electrical conductivity, microhardness, and tensile strength of the sin- tered samples with fine silver powder were higher than those of the samples with coarse silver powder. However, silver powder particle size has little influence on the relative densities, which of all samples （both by free and coarse silver powders） is more than 95%. The fracture characteristics are ductile.

The effect of sintering and cooling process on geometry distortion and mechanical properties transition of PTFE/Al reactive materials

In this research,the effect of the sintering and cooling process on geometry distortion and mechanical properties of PTFE/Al reactive material is investigated.Six particularly selected sintering temperatures,three different cooling modes(annealing cooling,normalizing cooling and rapid cooling),three different initial cooling temperature s,as well as six different final cooling temperatures were designed to compare the effects of sintering temperature,cooling rate,initial cooling temperature and final cooling temperature on the properties of reactive materials.Geometry distortion was quantitatively analyzed by a statistic on the dimensional changes of the specimens and microscopic morphology.A mechanical response properties transition from brittle to ductile was found and analyzed.By combining the thermodynamic properties of PTFE and unsteady heat conduction theory,mechanisms of cooling induced morphology change,temperature induced distortion and strength decrease were obtained.The results showed that the cooling rate has the most significant effect on the morphology transformation,while initial cooling temperature has more significant effect on the dimensional distortion than final cooling temperature.As to the mechanical properties transition from brittle to plastic,a more prominent effect of initial cooling temperature than cooling rate and final temperature was revealed.

Influence of porogen type and copper powder morphology on property of sintering copper porous materials

Copper porous materials have been manufactured by the method of powder metallurgy.Electrolytic copper powders and atomized copper powders are used as matrix material.Methylcellulose and paraffin are used as porogen.The influence of porogen type and copper powder morphology on the property of copper porous materials is investigated as well.The results show that copper porous materials with paraffin as porogen have lower porosity and permeability compared with materials using methylcellulose as porogen,due to the different pore-forming mechanisms.The pore forming mechanism of methylcellulose is thermal decomposition,while the pore forming mechanism of paraffin is melting–evaporation.The morphology of copper powders affects the contact state between adjacent powders,which further influence the sintering shrinkage.The porous materials using arborescent copper powders as matrix have lower porosity,smaller pore size and lower permeability,compared with materials with atomized copper powders as matrix.

IGNITING SHS BY LASER AND ITS APPLICATION TO SELECTIVE LASER SINTERING OF METALLIC POWDER MATERIAL

How to directly fabricate metallic functional parts with selective laser sintering (SLS) process is a potential technique that scientists are researching. Existent problems during directly fabricating metal part by use of SLS are analyzed. For the sake of solving the problems, a new idea of adding self-propagating high-temperature synthesis (SHS) material into metallic powder material to form new type of SLS metallic powder material is put forward. This powder material can release controllable amount of heat during its interaction with the laser beam energy to reduce the requirement to laser power during directly sintering metallic part, to prolong the time of metallic liquid phase existing, and to improve the intensity and accuracy of SLS part. For this reason, SHS material′s interaction with the CO2 laser beam energy is researched, which proves that CO2 laser beam energy may instantly ignite SHS reaction. On the basis of the above-mentioned researches, the effect of sintering the metal powder material mixing SHS material with CO2 laser is also researched, which shows: there is an optimal blending ratio of various material in the new metallic powder material. Under the optimal blending ratio and SLS process parameters, this new metallic powder material can indeed release amount of heat and SHS reaction may be controlled within the laser sintering. This research result makes it possible that the metallic part is directly sintered with small CO2 laser (less than 50W), which may greatly reduce the volume, cost and running expenditure of SLS machine, be propitious to application.

INFLUENCE OF ZnO AND BaO CONTENTS ON SINTERING AND CRYSTALLIZATION OF GLASSCERAMIC DECORATIVE MATERIALS

In this paper ,the influence of ZnO and BaO contents on sintering and crystallization of decorative materi-al in the system of CaO-Al2O3-SiO2wwas studied. The opti-mum ZnO 9 BaO contents and sintering or crystallization tem-perature for the glass-ceramic were determined.

Effect of Atmosphere on Sintering Behavior of Chromium Oxide Materials

The chromium oxide materials were prepared using Cr2O3 micropowder as main starting material, TiO2 micropowder as sintering aid, polyvinyl alcohol as binder, by a series of processes such as slurrying, spraying granulation, machine moulding and cold isostatic pressing, and firing at 1 500 ℃ for 3 h in air （ oxygen partial pressure was 2. 1× 10^4 Pa ）, industrial nitrogen （ oxygen partial pressure was 1×10^3 Pa ） , pure nitrogen （ oxygen partial pressure was 10 Pa） , high purity nitrogen （ oxygen partial pressure was 0.1 Pa ） , and carbon cake embedded atmosphere （ oxygen partial pressure wtas 2.3×10-12 Pa ）. Effects of oxygen partial pressures on the sintering behavior of Cr2 O3 materials were investiga- ted. The results show that （ 1 ） for 3 wt% TiO2-doped specimeas, there is a substantial dependence of sintering on oxygen partial pressure （0. 1 Pa - 2. 1 ×10^4 Pa ） , and the bulk density increases and apparent porosity decreases with oxygen partial pressure decreasing; （2） even if the oxygen partial pressure is 0. 1 Pa, the specimen without TiO2 cannot reach densification sintering; （3） under very low oxygen partial pressure of carbon embedded atmosphere, Cr2O3 materials containing TiO2 or not can attain denzification.

Coating processes towards selective laser sintering of energetic material composites

This research aims to contribute to the safe methodology for additive manufacturing(AM)of energetic materials.Coating formulation processes were investigated and evaluated to find a suitable method that may enable selective laser sintering(SLS)as the safe method for fabrication of high explosive(HE)compositions.For safety and co nvenie nce reasons,the co ncept demonstration was conducted using inert explosive simulants with properties quasi-similar to the real HE.Coating processes for simulant RDXbased microparticles by means of PCL and 3,4,5-trimethoxybenzaldehyde(as TNT simulant)are reported.These processes were evaluated for uniformity of coating the HE inert simulant particles with binder materials to facilitate the SLS as the adequate binding and fabrication method.Suspension system and single emulsion methods gave required particle near spherical morphology,size and uniform coating.The suspension process appears to be suitable for the SLS of HE mocks and potential formulation methods for active HE composites.The density is estimated to be comparable with the current HE compositions and plastic bonded explosives(PBXs)such as C4 and PE4,produced from traditional methods.The formulation method developed and understanding of the science behind the processes paves the way toward safe SLS of the active HE compositions and may open avenues for further research and development of munitions of the future.

Study on Squeeze Casting Metal-zirconium Composite Die Material by Hot Press Sintering

ZrO_(2)-5CrMnMo composite samples were prepared by hot press sintering.When NiCoCrAlY powders were used as the bonding layer and the different mixtures of NiCoCrAlY alloy and 3YSZ (3mol% yttria stabilized zirconia) ceramic powders were used as the transition layers,the connection between zirconia ceramic and 5CrMnMo steel were strengthened.Three composite samples with different structures were fabricated by heat spraying and hot press sintering.Shear and thermal shock cycle tests were conducted to characterize connection strength and thermal shock resistance of these samples.The shear strength reached 95.69 MPa,and the heating shock cycles achieved to the maximum value of 27.7 times.Microstructures and connection interfaces were analyzed by scanning electron microscopy.The hardness and wearing resistance of 3YSZ coat and 5CrMnMo substrate were compared,and the heat insulation property of composite samples were also discussed.It is shown that these composite materials fabricated in this research are benefited to be used as squeeze casting dies.

Effects of sintering pressure and temperature on microstructure and tribological characteristic of Cu-based aircraft brake material

A novel Cu-based P/M aircraft brake material was prepared and the effects of sintering pressure and temperature on microstructure and tribological characteristic were investigated. For the constant sintering temperature, when the sintering pressure increases from 0.5 MPa to 1.5 MPa, the porosity, wear loss and friction coefficient decrease remarkably. When the sintering pressure increases from 1.5 MPa to 2.5 MPa, the porosity further decreases but in a little degree and wear behaviors are improved slightly. However, once the sintering pressure is larger than 2.5 MPa, it has no obvious effect on microstructure and tribological characteristic. For the constant sintering pressure, when the sintering temperature increases from 900 ℃ to 930 ℃, the sintered density remarkably increases, and wear behaviors are obviously improved. For further increasing sintering temperature to 1 000 ℃, the density keeps on increasing, but wear behaviors change slightly.

Selective sintering of magnesia-calcia materials by utilizing hot spots during induction sintering process

Magnesia-calcia refractories are widely used in the production process of clean steel due to their excellent high-tem-perature stability,slag resistance and ability to purify molten steel.However,there are still problems such as difficult sintering and easy hydration.Magnesia-calcia materials with various calcium oxide contents were prepared by using induction sintering,and the sintering property combined with the hydration resistance of the materials was investigated.The experimental results showed that the magnesia-calcia materials prepared under induction field had higher density,microhardness and hydration resistance.In particular,the relative density of induction sintered magnesia-calcia materials with 50 mo1%CaO was greater than 98%,and the average grain size of CaO was 4.56μm,which was much larger than that of traditional sintered materials.In order to clarify the densification and microstructure evolution mechanism of the magnesia-calcia materials,the changes in temperature and magnetic field throughout the sintering process were analyzed by using finite element simulation.The results showed that the larger heating rate and higher sintering temperature under the induction sintering mode were beneficial to the rapid densification.In addition,the hot spots generated within the material due to the difference in high-temperature electric conductivity between MgO and CaO were the critical factor to realize selective sintering in MgO-CaO system,which provides a novel pathway to solve the problem of difficult sintering and control the microstructure of high-temperature composite material used in the field of high-purity steel smelting.

Investigation of Loss Weight and Densification of SiC-Al_2O_3-Y_2O_3 Ceramic Composite on Sintering

α-SiC, Al_2O_3 and Y_2O_3 powders were all used as raw materials. The SiC-Al_2O_3-Y_2O_3 ceramic composites were made by pressureless liquid phase sintering technology. The effects of sintering temperature, loss weight and coordination number on sintering densification were studied. The reason for producing loss weight on sintering was analysed. The results show that the primary reason for producing loss weight on sintering in SiC-Al_2O_3-Y_2O_3 ceramic composite was that chemical reactions between SiC and Al_2O_3 are happened during sintering, and given out volatile gases. If sintering temperature is excessively lower, grain size would be finer, and coordination number would be higher, well then material would be on no sintering densification. If sintering temperature is excessively higher, grains would grow up, though small coordination number would benefit to make pore eliminate and shrink, but coarse microstructure would also block gliding and resetting of grains, together affected by expansion stress from volatile gas, the material densification would instead go down. Only under the sintering process of 1850 ℃ for 30 min, material densification is better, and the mechanical property of ceramic composites is also improved.

Volume change of macropores of titanium foams during sintering

The porosity of titanium foams obtained from the space holder technique was theoretically analyzed in the cases of volume shrinking, retaining and expanding during sintering. The relationship between porosity and spacer content was compared under different conditions. The kind of volume change of macropores during sintering was discussed. The results indicate that the relationship between porosity and spacer content depends on the decreased volume of macropores and the volume of micropores in cell-walls in the first case, while the porosity will be greater than the spacer content for the other two cases. It proves that the volume change of macropores during sintering decreases based on theory and practice.

Comparative study of the fabrication of ultrafine Ti(C,N)-based cermets by spark plasma sintering and conventional vacuum sintering

Spark plasma sintering (SPS) and conventional vacuum sintering (VS) wereemployed to fabricate ultrafine Ti(C,N)-based cermets. The shrinkage behavior, microstracture, andporosity and mechanical properties of the samples fabricated by SPS were compared with those of thesamples sintered by VS using optical microscopy, scanning electron microscopy, universal testingmachine, and rockwell tester. The results are as follows: (1) The shrinkage process occurred mainlyin the range of 1000-1300 deg C during the VS process, and only a 0.2 percent linear shrinkage ratioappeared below 800 deg C; during the SPS process, a 60 percent dimensional change occurred below800 deg C as a result of pressure action. (2) By utilizing the SPS technique, it is difficult forobtaining fully dense Ti(C,N)-based cermets. Due to the much existence of pores and un-combinedcarbon, the mechanical properties of the sintered samples by SPS are inferior to sintered ones byVS. (3) grain size of the samples sintered by SPS is still below 0.5 urn, but not by VS; because oflow sintering temperature, there are no typical core/rim structures formed in the sintered samplesby SPS1; the main microstructures of the sintered samples by SPS2 are a white core/grey shellstructure, whereas by VS show a typical black core/grey shell structure.

Effect of sintering parameters on warm compacted iron-based material

Iron-based powder metallurgy material was prepared by warm compaction at 125 ℃ using a compacting pressure of 700 MPa. Sintering temperature ranging from 1 100 ℃ to 1 300 ℃ and sintering time ranging from 40 min to 80 min were used to study the effects of sintering parameters on the compacts. Die wall lubrication polytetrafluoroethylene(PTFE) emulsion was also applied in combination with warm compaction in hope to increase the compact density and the mechanical properties of the sintered material. Green and sintered density, spring back effect and sinter shrinkage were measured. Mechanical properties of both as-sinter and heat treated samples were also measured. Results show that mechanical properties of the sintered compacts increase with the increase of sintering temperature and sintering time. Sample prepared by die wall lubricated warm compaction always shows higher density and mechanical properties.

Structural characteristics and magnetic properties of bulk nanocrystalline Fe_(84)Zr_2Nb_4B_(10) alloy prepared by mechanical alloying and spark plasma sintering consolidation

Magnetic properties of Fe84Zr2Nb4B10 sample were investigated. The sample was produced from nanocrystalline powders made by the mechanical alloying (MA) and consolidation using the spark plasma sintering (SPS) technique. Effects of milling time on phase transformation, structural characteristics, and magnetic properties of powders were examined by X-ray diffraction (XRD), scanning electron microscopy (SEM), and physical property measure system (PPMS), respectively. Results show that nanostructured α-Fe supersaturated solid solution is obtained in the final MAed products. The saturation magnetization (Ms) increased with increasing milling time and became constant at 130 h, but the coercivity (Hc) increased firstly and then decreased. The consolidated bulk sample exhibited a high density of 6.893 g·cm-3, there was no phase change during SPS process, and the saturation magnetization and susceptibility of the SPSed bulk sample improved in comparison with the milled powders. The variation of magnetic parameters can be explained by nano-scale effect and Herzer model.

Preparation of multi-walled carbon nanotube-reinforced TiNi matrix composites from elemental powders by spark plasma sintering

Carbon nanotube (CNT)-reinforced TiNi matrix composites were synthesized by spark plasma sintering (SPS) employing elemental powders.The phase structure,morphology and transformation behaviors were studied.It was found that thermoelastic martensitic transformation be-haviors could be observed from the samples sintered above 800 ℃ even with a short sintering time (5min),and the transformation tempera-tures gradually increased with increasing sintering temperature because of more Ti-rich TiNi phase formation.Although decreasing the sin-tering temperature and time to 700 ℃ and 5min could not protect defective MWCNTs from reacting with Ti,still-perfect MWCNTs re-mained in the specimens sintered at 900 ℃.This method is expected to supply a basis for preparing CNT-reinforced TiNi composites.