Graphene-reinforced aluminum matrix composites prepared by spark plasma sintering

Graphene-reinforced 7055 aluminum alloy composites with different contents of graphene were prepared by spark plasma sintering（SPS）. The structure and mechanical properties of the composites were investigated. Testing results show that the hardness, compressive strength, and yield strength of the composites are improved with the addition of 1wt% graphene. A clean, strong interface is formed between the metal matrix and graphene via metallurgical bonding on atomic scale. Harmful aluminum carbide（Al_4C_3） is not formed during SPS processing. Further addition of graphene（above 1wt%） results in the deterioration in mechanical properties of the composites. The agglomeration of graphene plates is exacerbated with increasing graphene content, which is the main reason for this deterioration.

Densification mechanism of stereolithographical dense Si_(3)N_(4) ceramics with CeO_(2) as sintering additive by field assisted sintering

Combining sintering additive with field assisted sintering,stereolithographical dense Si3N4 ceramics was successfully fabricated.Owing to a large amount of polymer during the stereolithography,the green parts have the characteristics of low powder loading and high porosity.Adjusting the process parameters such as sintering temperature and soaking time can effectively improve the density of the specimens.The stress exponent n of all specimens is in a range of 1 and 2,which is derived from a modified sintering kinetics model.The apparent activation energy Qd of stereolithographic Si_(3)N_(4) ceramics sintered with applied pressures of 30 MPa,40 MPa,and 50 MPa is 384.75,276.61 and 193.95 kJ/mol,respectively,suggesting that the densification dynamic process is strengthened by raising applied pressure.The grain boundary slipping plays a dominating role in the densification of stereolithographic Si3N4 ceramics.The Vickers hardness and fracture toughness of stereolithographic Si3N4 ceramics are HV10/10(1347.9±2.4)and(6.57±0.07)MPaAbstract:Combining sintering additive with field assisted sintering,stereolithographical dense Si3N4 ceramics was successfully fabricated.Owing to a large amount of polymer during the stereolithography,the green parts have the characteristics of low powder loading and high porosity.Adjusting the process parameters such as sintering temperature and soaking time can effectively improve the density of the specimens.The stress exponent n of all specimens is in a range of 1 and 2,which is derived from a modified sintering kinetics model.The apparent activation energy Qd of stereolithographic Si3N4 ceramics sintered with applied pressures of 30 MPa,40 MPa,and 50 MPa is 384.75,276.61 and 193.95 kJ/mol,respectively,suggesting that the densification dynamic process is strengthened by raising applied pressure.The grain boundary slipping plays a dominating role in the densification of stereolithographic Si3N4 ceramics.The Vickers hardness and fracture toughness of stereolithographic Si3N4 ceramics are HV10/10(1347.9±2.4)and(6.57±0.07)MPa·m^(1/2),respectively.

Preparation of Superfine-Cemented Carbide by Spark Plasma Sintering

92WC-8Co puwder mixture with superfine-tungsten carbide was respectively sintered by spark plasma sintering（ SPS ） and sintering isostutic pressure （SIP）. Complete dense samples with 200 nm WC grains and 94.2HRA hardness were prepared by spark plasma sintering at 1 150 ℃ and under 4.5 kN for 5 minutes. SIP was carried out at 1 400 ℃ for 30 minutes with a result of 300-400 nm WC grains and 93 HRA hardness. The results show that sintering temperature is greatly decreased by SPS, sintering time is largely shortened and WC grain growth is effectively retarded. Micropores and drawb（wks in superfine-cemented carbide made by SPS are greatly declined, which is very useful to improving nwehanical properties.

The Influences of Controlling Sintering Mechanism on Electrical Properties of Multilayer PTCR Chip

Experiments were designed to investigate the influence of controlling sintering mechanism on electrical properties of multilayer PTCR chip. During the preparation process, heating rate, sintering temperature, high-temperature holding time and cooling method were respectively regulated to prepare multilayer PTCR chip with good performance. After the process of organic casting, the casting PTCR green films were sintered at 1 260-1 280 ~C for 0.5 h at reduction atmosphere, which was heated at the rate of 400 ℃/h. Then selecting 300 ℃/h as the cooling rate, the ceramics were oxidated at 850 ℃ for 1 h. The prepared multilayer PTCR chips exhibited room temperature resistivity of below 100 Ω.cm, and resistance rising rate more than 104 unit through the Curie temperature.

Microstructure and Mechanical Performance of Cu-SnO_2-rGO based Composites Prepared by Plasma Activated Sintering

A novel chemical technique combined with unique plasma activated sintering（PAS） was utilized to prepare consolidated copper matrix composites（CMCs） by adding Cu-SnO2-rGO layered micro powders as reinforced fillers into Cu matrix. The repeating Cu-SnO2-rGO structure was composed of inner dispersed reduced graphene oxide（r GO）, SnO2 as intermedia and outer Cu coating. SnO2 was introduced to the surface of rGO sheets in order to prevent the graphene aggregation with SnO2 serving as spacer and to provide enough active sites for subsequent Cu deposition. This process can guarantee rGO sheets to suffi ciently disperse and Cu nanoparticles to tightly and uniformly anchor on each layer of rGO by means of the SnO2 active sites as well as strictly control the reduction speed of Cu^2＋. The complete cover of Cu nanoparticles on rGO sheets thoroughly avoids direct contact among rGO layers. Hence, the repeating structure can simultaneously solve the wettability problem between rGO and Cu matrix as well as improve the bonding strength between rGO and Cu matrix at the well-bonded Cu-SnO2-rGO interface. The isolated rGO can effectively hinder the glide of dislocation at Cu-rGO interface and support the applied loads. Finally, the compressive strength of CMCs was enhanced when the strengthening effi ciency reached up to 41.

Influence of Yb_2O_3-MgO on Mechanical Properties and Thermal Conductivity of Silicon Nitride Ceramics via Gas Pressure Sintering

In this work,Yb2O3 and Mg O were used as sintering aids in preparing silicon nitride ceramics by gas pressure sintering（ 0. 6 MPa N2atmosphere） to investigate how the amounts of Yb2O3- Mg O influence the mechanical properties and thermal conductivity of silicon nitride ceramics. The total contents of Yb2O3- Mg O added were 1 mol%,2 mol%,4 mol%,6 mol%,8 mol%,10 mol%,12 mol%,14 mol%,keeping the Yb2O3-Mg O molar ratio of 1 ∶ 1 steadily. Curves of the relative density,thermal conductivity and bending strength plotted against the aids content present a ‘mountain＇shape with a maximum at nearly 10 mol% aids. The fracture toughness increased with the amounts of additives up to10 mol% and decreased slightly thereafter. The mechanical properties and thermal conductivity were almost proportional to the amount of the additives before10 mol%. When the content of aids exceeded 10 mol%,it would weaken the mechanical properties and thermal conductivity of the ceramics. The optimum content of Yb2O3- Mg O was 10 mol% by gas pressure sintering（ 0. 6MPa） at 1 850 ℃ for 4 h,which led to a relative density of 98. 9%,a flexural strength of（ 966 ± 38）MPa as well as a fracture toughness of（ 6. 29 ± 0. 29）MPa·m1 /2and thermal conductivity of 82 W /（ m·K）.

Sintering Mechanism of Stainless Steel in Powder Injection Molding

Stainless steel samples were made by Powder injection Molding (PIM) process with-400 mesh powder in order to investigate the sintering mechanism in this system and develop the PIM of stainless steels. The process included mixing, injection molding, debin- ding and sintering. Neck growth model was used to analyze the sintering mechanism. The results show that lattice (volume) diffusion is the main mechanism in the sintering process, the products with higher density (>95%) and properties are obtained. At lower temperatures, grain boundary diffusion may play a role in the sintering densification.

Reaction Mechanism and Microstructure Evolution of Reaction Sintered h-BN

Hexagonal boron nitride ceramic（h-BN） based on the nitridation of B powders was obtained by reaction sintering method. The effects of sintering temperature on the mechanical properties and microstructure of the resultant products were investigated and the reaction mechanism was discussed. Results showed that the reaction between B and N2 occurred vigorously at temperatures ranging from 1 000 ℃ to 1 300 ℃, which resulted in the generation of t-BN. When the temperature exceeded 1 450 ℃, transformation from t-BN to h-BN began to occur. As the sintering temperature increased, the spherical particles of t-BN gradually transformed into fine sheet particles of h-BN. These particles subsequently displayed a compact arrangement to achieve a more uniform microstructure, thereby increasing the strength.

Effect of nitrogen introduction methods on the microstructure and properties of gradient cemented carbides

Gradient cemented carbides with the surface depleted in cubic phases were prepared following normal powder metallurgical pro-cedures.Gradient zone formation and the influence of nitrogen introduction methods on the microstructure and performance of the alloys were investigated.The results show that the simple one-step vacuum sintering technique is doable for producing gradient cemented carbides.Gradient structure formation is attributed to the gradient in nitrogen activity during sintering,but is independent from nitrogen introduced methods.A uniform carbon distribution is found throughout the materials.Moreover,the transverse rupture strength of the cemented carbides can be increased by a gradient layer.Different nitrogen carriers give the alloys distinguishing microstructure and mechanical properties,and a gradient alloy with ultrafine-TiC0.5N0.5 is found optimal.

Preparation and Arc Erosion Characteristics of Ultrafine Crystalline CuCr50 Alloy by MA-SPS

The ultrafine crystalline CuCr50（Cr 50 wt%） alloys were fabricated by a combination of mechanical alloying and spark plasma sintering process. The effects of milling time on crystallite size and solid solubility of the CuCr50 composite powders were investigated. The results showed that crystallite size of powders decreases gradually and solid solubility of Cr in Cu was extended with increasing milling time. The minimal crystallite size about 10 nm and the maximum solid solubility about 8.4 at%（i e, 7 wt%） were obtained at 60 h. The microstructure of ultrafine crystalline CuCr50 alloy was analyzed by SEM and TEM, which contains two kinds of size scale Cr particles of 2 μm and 50-150 nm, distributing homogeneously in matrix, respectively. The arc erosion characteristics of ultrafine crystalline CuCr50 alloy were investigated by the vacuum contact simulation test device in low D.C. voltage and low current（24 V/10 A）. A commercial microcrystalline CuCr50 alloy was also investigated for comparison. Experiments indicate that the cathode mass loss of ultrafine crystalline CuCr50 contact material is higher than that of microcrystalline CuCr50 material, but its eroded surface morphology by the arc is uniform without obvious erosion pits. While the surface of microcrystalline CuCr50 contact is seriously eroded in local area by the arc, an obvious erosion pit occurred in the core part. Therefore, the ability of arc erosion resistance of ultrafine crystalline CuCr50 alloy is improved compared to that of microcrystalline CuCr50 material.

In situ investigation on densification mechanism of Ti-20Al-19Nb(at.%)alloy by TiH_(2)-assisted pressureless sintering

Dense Ti-20Al-19Nb(at.%)alloys can be cost-effectively fabricated by TiH_(2)-assisted pressureless sintering;nevertheless,the densification mechanism remains controversial without understanding the entire sintering process.By in situ observing the surface morphology of the Ti/Al/Nb and Ti/TiH_(2)/Al/Nb compacts upon heating,the densification mechanism of the Ti-20Al-19Nb alloys was elucidated in this study.In addition to the reported reason that the dehydrogenation of TiH_(2)provided reactive Ti,the densification of Ti-20Al-19Nb alloy was found to be strongly associated with the phase transformations upon sintering.The TiH_(2)participated in the reverse eutectoid transformation,α-Ti+δ-TiH_(2)→β-Ti,inducing theα/βand TiH_(2)/βgrain boundaries for the rapid diffusion of Al.The reaction of Ti(s)+Al(s)→TiAl_(3)(s)was then accelerated,and the majority of the Al phase was consumed in the solid state,which significantly reduced the pores from the transient liquid Al.The activation energy of the Ti-Al reaction decreased with the addition of TiH_(2),and the growth mode of the TiAl_(3)phase was changed.By removing the large pores at 700℃,the Ti-Al intermetallic phases were well connected,forming the continuous interdiffusion route for Ti,Al,and Nb.The diffusion of Nb,as well as the phase transformation ofα2→B2,was then promoted,and the ripening time for the B2 phase was increased.As a result,the density and mechanical properties were improved.The initial results of this study provided a foundation for the cost-effective fabrication of high-strength Ti-Al alloys containing refractory elements.

Research Progress on Preparation and Properties of Zirconium Carbide Matrix Composites

Zirconium carbide（ZrC） exhibits considerable potential for applications as aerospace thermal protection and the Generation-Ⅳ nuclear fuel inert materials due to its high melting point,exceptional hardness,good ablation resistance and low neutron absorption cross-section.Nevertheless,low sinterability of ZrC powders and poor fracture toughness and reliability of bulk ceramics limit their wide applications in extreme environments.This paper reviews the state of the art of preparation and properties of ZrC composites.Optimizing the sintering process and tailoring the chemical constituents of raw powders and sintering aids could improve sinterability to produce dense bulk ceramics.Different additives such as refractory metals,carbides,silicides,oxides,or carbon fibers are introduced into the ZrC matrix in order to improve fracture toughness,oxidation resistance or thermal shock resistance,etc.Further studies are needed to explore the effects of intrinsic defects（vacancies,dislocations,and grain or phase boundaries,etc.） and additives on microstructure and properties at elevated temperatures.

Influence of Spark Plasma Sintering Temperature on the Densification, Microstructure and Mechanical Properties of Al-4.5 wt.%Cu Alloy

The effect of sintering temperature on the densification mechanisms, microstructural evolution and mechanical properties of spark plasma sintered （SPS） compacts of a gas atomized Al-4.5 wt.%Cu alloy was investigated. The powder particles whose size varied between 10 to 500μm was subjected to SPS at 400, 450 and 500℃ at a pressure of 30 MPa. The compact sintered at 500℃ exhibited fully dense microstructure which was characterized by a uniform distribution of the secondary phase, free of dendrites and micro-porosity. Microscopy and the SPS data reveal that the events such as particle rearrangement, localized deformation and bulk deformation appear to be the sequence of sintering mechanisms depending on the size range of powder particles used for consolidation. The compact sintered at 500℃ exhibited the highest hardness and compression strength since the microstructure was characterized by fine distribution of precipitates, large fraction of submicron grains and complete metallurgical bonding.

Hot pressing sintering process and sintering mechanism of W-La_(2)O_(3)-Y_(2)O_(3)-ZrO_(2)

The W-La_(2)O_(3)-Y_(2)O_(3)-ZrO_(2)materials were prepared by vacuum hot pressing sintering process.The microstructure was characterized by scanning electron microscopy(SEM).The effects of sintering temperature,sintering pressure,holding time and heating rate on relative density,hardness and microstructure were studied.The sintering activation energy of the powder was calculated.Based on the result,the best sintering parameters by vacuum hot pressing sintering are as follows:sintering temperature of 1600℃,sintering pressure of 60 MPa and holding time of 60 min.The heating rate is 10℃·min^(-1)from room temperature to 1000℃and 4℃·min^(-1)from1000 to 1600℃.Using this process,the grain size is about3 lm in diameter with relative density at 99.7%,and the hardness is HV 528.5.The sintering characteristic index(n)of the specimen is 4,and the sintering mechanism mainly depends on the diffusion from the surface to the intragranular in the volume diffusion.The sintering activation energy of W-La_(2)O_(3)-Y_(2)O_(3)-ZrO_(2)material is286.2 k J·mol^(-1),which indicates that the powder has higher activity in sintering process.

Microstructure and mechanical properties of ZrO_2(Y_2O_3)-Al_2O_3 nanocomposites prepared by spark plasma sintering

Zirconia （yttria）-alumina ceramic nanocomposites were fabricated from different powders by spark plasma sintering （SPS）. One powder was a commercially available nanocomposite powder TZP-3Y2OA, consisting of 3 mol% yttria-stabilized zirconia （3-YSZ） reinforced with 20wt% alumina, and the other, used as a comparison, was a conventional mechanically mixed powder 3YSZ-2OA, a blend made of 3 mol% yttria-stabilized zirconia powder ZrO2 （3Y） and 20 wt% ,x-alumina powder. The effect of the sintering temperature on the densification, the sintering behavior, the mechanical properties and the microstructure of the composites was investigated. The results showed that the density increased with increasing sintering temperature, and thus, the mechanical properties were strengthened because of the increased densification. The nanocomposite powder TZP-3Y20A was easily sintered, and good mechanical properties were achieved as compared with the powder from the conventional mechanically mixed method, the maximum flexural strength and fracture toughness of which were 967 MPa and 5.27 MPa m 1/2, respectively.

Effect of cerium/lanthanum addition on microstructure and mechanical properties of Al7075 alloy via mechanical alloying and sintering

The effect of the Al-6Ce-3La（ACL） on the microstructural behavior of the Al7075 was investigated. Materials were synthesized by mechanical alloying with variation in the ACL content and milling time. Products were characterized and studied in the as-milled condition and mechanically evaluated after sintering. The synergetic effect of milling time and ACL content in the modified materials led to a reduction in the particle size. Results from electron microscopy showed a homogeneous dispersion of Ce/La phases up to 20 wt.% of ACL content after 10 h of milling. Mechanical evaluation under compressive test showed an improved performance for those alloys reinforced with 0.2 wt.% and 0.5 wt.% of ACL.

Microstructures and properties of CuZrAl and CuZrAlTi medium entropy alloys prepared by mechanical alloying and spark plasma sintering

Equiatomic CuZrAl and CuZrAlTi medium entropy alloys were designed and synthesized by mechanical alloying and spark plasma sintering technique.The alloying behavior,phase evolutions,microstructures and properties of samples were investigated by X-ray diffraction,differential scanning calorimetry,field emission scanning electron microscopy,microscopy/Vickers hardness testing and electrochemical polarization measurement.The results indicate that the final products of as-milled alloys consist of amorphous phases.Ti addition improves the glass forming ability of as-milled alloys.The as-sintered CuZrAl alloy contains face-centered cubic（fcc）solid solution,Al_（1.05）Cu_（0.95） Zr and AlZr_2 phases at different sintering temperatures.With Ti addition,the as-sintered sample is only composed of intermetallics at 690°C,while fcc1,fcc2 and CuTi3phases are formed at 1100°C.CuZrAlTi-1100°C alloy exhibits the highest hardness value of 1173HV0.2owing to the high sintering density,solid solution strengthening and homogeneous precipitation of nano-size crystalline phase.CuZrAlTi-690°C alloy presents a similar corrosion resistance with304 Lstainless steel in seawater solution and further possesses the lower corrosion rate.

Mechanism of conductive powder microstructure evolution in the process of SPS

Spark plasma sintering(SPS)is an advanced sintering technology that has been recently developed in the world.Contrast to many reports about experimental investigations on the methods of new materials preparation,there are very few systematic studies on the special sintering mechanism of SPS technology.In the present paper,by using the pure electrolytic copper powders as the raw material,a series of sintering experiments have been designed and carried out.The evolution of the powder microstructures during SPS has been systematically studied,and for the first time a“self-adjusting mechanism”of the microstructure evolution is proposed,from which the essential for the advantages of materials preparation by SPS in the respects of high density,homogeneity and fine grain structure can be well understood.In addition,the changes of the relative density during SPS are quantitatively predicted by a theoretical model and confirmed by the experimental measurements.

Ablation effects and mechanism of sintered silicon carbide ceramics by an ArF excimer laser

The ablation of sintered silicon carbide ceramics by an ArF excimer laser was studied. Three zones are generated： the ablation zone that presented molten morphology and was composed by the Si and C phase; the condensation zone formed by vaporized SiC; and the oxidation zone that showed the characteristics of thermal oxidation. The ablation depth and oxidation range increase linearly with fluence and pulses within 0.5-4 J/cm2, but the normalized ablation efficiency is constant （3.60± 0.60 μm · mm2/J）. The theoretical photochemical ablation depth supplies 25% of the total depth at 1 J/cm2 but decreases to 16% at 4 J/cm2. The ablation is dominated by the photothermal effect and conforms to the thermal evaporation mechanism.