Atomic force microscope study of WC-10Co cemented carbide sintered from nanocrystalline composite powders

In order to compare the spark plasma sintedng （SPS） process plus hot isostatic press （HIP） with vacuum sintedng plus HIP, an investigation was carried out on the topography, microstructure and gain size distribution of nanocrystalline WC-10Co composite powder and the sintered specimens prepared by SPS plus HIP and by vacuum sintering plus HIP by means of atomic force microscopy （AFM）. The mechanical properties of the sintered specimens were also investigated. It is very easy to find cobalt lakes in the specimen prepared by vacuum sintering plus HIP process. But the microstructure of the specimen prepared by SPS plus HIP is more homogeneous, and the grain size is smaller than that prepared by vacuum sintering plus HIP. The WC-10Co ultrafine cemented carbide consolidated by SPS plus HIP can reach a relative density of 99.4%, and the transverse rupture strength （TRS） is higher than 3540 MPa, the Rockwell A hardness （HRA） is higher than 92.8, the average grain size is smaller than 300 nm, and the WC-10Co ultrafine cemented carbide with excellent properties is achieved. The specimen prepared by SPS with HIP has better properties and microstructure than that prepared by vacuum sintering with HIP.     

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.     

Influence of mechanical alloying time on the properties of Fe_3Al intermetallics prepared by spark plasma sintering

The Fe3Al-based intermetallics were prepared by mechanical alloying and spark plasma sintering (SPS), and the influence of milling time on the properties of materials was investigated. The phase identification was investigated by X-ray, and the surface morphology and fractography were observed by scanning electron microscope (SEM). The mechanical properties such as bending strength, strain, and microhardness were tested. The results show that Fe reacts with Al completely to form Fe3Al during short SPS processing time. The relative densities of the sintered samples were nearly 100/. The mechanical properties of the sintered samples can be improved along with the milling time. The representative values are the bend strength of 1327 MPa and the microhardness of 434.     

Influence of mechanical alloying time on the properties of FeaAl intermetallics prepared by spark plasma sintering

The Fe3Al-based intermetallics were prepared by mechanical alloying and spark plasma sintering （SPS）, and the influence of milling time on the properties of materials was investigated. The phase identification was investigated by X-ray, and the surface morphology and fractography were observed by scanning electron microscope （SEM）. The mechanical properties such as bending strength, strain, and microhardness were tested. The results show that Fe reacts with Al completely to form Fe3Al during short SPS processing time. The relative densities of the sintered samples were nearly 100%. The mechanical properties of the sintered samples can be improved along with the milling time. The representative values are the bend strength of 1327 MPa and the microhardness of 434.     

Effect of CaO doping on mechanical properties and thermal shock resistance of 10NiO-NiFe2O4 composite ceramics

The CaO doped 10NiO-NiFe2O4 composite ceramics were prepared by the cold isostatic pressing-sintering process, and the effects of CaO content on the phase composition, mechanical property and thermal shock resistance of 10NiO-NiFe2O4 composite ceramics were studied. The results show that the samples mainly consist of NiO and NiFe2O4 when content of CaO is less than 4%（mass fraction）, bending strength increases obviously by CaO doping. Bending strength of the samples doped with 2% CaO is above 185 MPa, but that of the samples without CaO is only 60 MPa. Fracture toughness is improved obviously by CaO doping, the samples doped with 2% CaO have the maximum fracture toughness of 2.12 MPa·m^1/2, which is about two times of that of the undoped ceramics. CaO doping is bad to thermal shock resistance of 10NiO-NiFe2O4 composite ceramics.     

Effect of sintering atmosphere on composition and properties of NiFe_2O_4 ceramic

Ni Fe2O4 ceramics were prepared in different sintering atmospheres. The phase compositions, microstructures and mechanical properties were studied. The results show that the stoichiometric compound Ni Fe2O4 cannot be obtained in vacuum or atmospheres with oxygen contents of 2×10-5, 2×10-4 and 2×10-3, respectively. All the samples sintered in above-mentioned atmospheres contain phases of Ni Fe2O4 and Ni O. With increasing oxygen content, Ni Fe2O4 content in the ceramic increases, while Ni O content appears a contrary trend. In vacuum, Ni Fe2O4 ceramic has average grain size of 3.94 μm, and bending strength of85.12 MPa. The changes of the phase composition and mechanical properties of Ni Fe2O4 based cermets are mainly caused by the alteration of their properties of Ni Fe2O4 ceramic.     

Effect of sintering atmosphere on composition and properties of NiFe2O4 ceramic

Ni Fe2O4 ceramics were prepared in different sintering atmospheres. The phase compositions, microstructures and mechanical properties were studied. The results show that the stoichiometric compound Ni Fe2O4 cannot be obtained in vacuum or atmospheres with oxygen contents of 2×10-5, 2×10-4 and 2×10-3, respectively. All the samples sintered in above-mentioned atmospheres contain phases of Ni Fe2O4 and Ni O. With increasing oxygen content, Ni Fe2O4 content in the ceramic increases, while Ni O content appears a contrary trend. In vacuum, Ni Fe2O4 ceramic has average grain size of 3.94 μm, and bending strength of85.12 MPa. The changes of the phase composition and mechanical properties of Ni Fe2O4 based cermets are mainly caused by the alteration of their properties of Ni Fe2O4 ceramic.     

Effect of sintering additives on properties of Si3N4-BN composites fabricated via die pressing and precursor infiltration and pyrolysis route

The Si3N4-BN composites have been prepared via die pressing and precursor infiltration and pyrolysis route using borazine as precursor, and the effect of sintering additives on properties of the composites has been investigated. After sintering additives are adopted, the α to β phase transition of Si3N4 and the mechanical properties of the composites at both room temperature and high temperature are all increased with small extent. When using Y2O3+Al2O3 as additives, the phase transition of Si3N4 and the mechanical properties of the composites have better results. The β-Si3N4 content is 17.47%. The fl exural strength, elastic modulus and fracture toughness of the composites are 188.74 MPa, 84.34 GPa and 2.96 MPa?m1/2, respectively. After exposed at 1 000 ℃ in the air for 15 min, the fl exural strength of the composites is 154.62 MPa with a residual ratio of 81.92%. The elongated β-Si3N4 grains appear in all composites with different sintering additives. Relatively more rod like β-Si3N4 grains can be observed in composites with Y2O3+Al2O3 as additives, making it to possess better mechanical properties.     

Fabrication and Microstructure of BN Matrix Composites with Electrical COnductivity

BN ceramic is advanced engineering ceramics with excellent thermal shock resistance,good workability and excellent dielectricity.TiB2 ceramic has excellent electric conductivity,high melting points,and corrosion resistance to molten metal.Therefore,the composite consisting of BN and TiB2 ceramics is expected to have a combination of above-mentionaed properties,thereby can be used as self-heating crucible.In this puper,hot pressing technology was used to fabricate the high performance BN-TiB2 composite materials,microstructure and electric conducting mechanism were studied,and the relationship between the microstructure and physical property was discussed.the results show that the microstructure of composites has a great influence on the physical property of composites.The BN-TiB2 composites with excellent mechanical strength and stable resistivity can be obtained by optimizing the processing parameter and controlling the microstructure of composites.     

Effect of annealing on microstructure and properties of Si_3N_4-AlN composite ceramics

Aiming at developing novel microwave-transparent ceramics with low dielectric loss,high thermal conductivity and high strength,Si3N4-AlN(30%,mass fraction) composite ceramics with La2O3 as sintering additive were prepared by hot-pressing at 1 800 °C and subsequently annealed at 1 450 °C and 1 850 °C for 2 h and 4 h,respectively.The materials were characterized by XRD and SEM.The effect of annealing process on the phase composition,sintering performance,microstructure,bending strength,dielectric loss and the...     

Comparative study of β-Si3N4 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℃ 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.     

Preparation of MWNTs/Al<Subscript>2</Subscript>O<Subscript>3</Subscript> composites and their mechanical and electrical properties

Since their discovery by Iijima[1], carbon nanotubes (CNTs) have been the focus in novel materials research. Theoretical and experimental studies show[2-9] that CNTs have extraordinary mechanical and electrical properties. Krishnan et al.[2] have reported that the mean value of Young’s modulus of single-wall nanotubes (SWNTs) is 1.25 TPa. Yu et al.[3] measured Yang’s modulus of multi-wall nanotubes (MWNTs) between 270 and 950 GPa and breaking strength between 11 and 63 GPa. The ele…     

Thermoelectric properties of Ca3Co4O9 ceramics

Ca₃Co₄O₉ ceramics were prepared using the sol-gel process with ordinary pressing sintering and their thermoelectric properties were measured from room temperature to 673 K. The experimental results show that single phase Ca₃Co₄O₉ can be fabricated at 750–900 °C in different citrate acid molar proportions for 0.2–1.0. For all the oxides, both the Seebeck coefficients S and the electrical conductivities κ increase with the increasing temperature. The Seebeck coefficients S are all positive. The thermal conductivities k increase with the increasing temperature also and the lattice thermal conductivity κ _l plays an important role to the thermal conductivity κ. The citrate acid molar proportions have a large influence on the particle sizes, which influences the thermoelectric properties of the ceramics. The figure of merit increases with the increasing temperature and reaches 4.5×10⁻⁵ K⁻¹ at 573 K for the sample in the citrate acid molar proportion of 0.46.     

Low-temperature sintering and microwave dielectric properties of Li2MgTi3O8 ceramics doped with BaCu（B2O5）

The influences of BaCu(B₂O₅) (BCB) addition on sintering, microstructure and microwave dielectric properties of Li₂MgTi₃O₈ ceramics were investigated using X-ray diffractometry, scanning electron microscopy and microwave dielectric measurements. The experimental results show that a small amount of BaCu(B₂O₅) addition can effectively reduce the sintering temperature to 900 °C, and induce only a limited degradation of the microwave dielectric properties. Typically, the best microwave dielectric properties of ɛ _r=24.5, Q×f =24 622 GHz, τ _f=4.2×10⁻⁶ °C⁻¹ are obtained for 1.0% BCB-doped Li₂MgTi₃O₈ ceramics sintered at 900 °C for 3 h. The BCB-doped Li₂MgTi₃O₈ ceramics can be compatible with Ag electrode, which may be a strong candidate for low temperature co-fired ceramics applications.     

Effects of different iron sources on the performance of LiFePO4/C composite cathode materials

Olivine LiFePO₄/C composite cathode materials were synthesized by a solid state method in N₂ + 5vol% H₂ atmosphere. The effects of different iron sources, including Fe(OH)₃ and FeC₂O₄·2H₂O, on the performance of as-synthesized cathode materials were investigated and the causes were also analyzed. The crystal structure, the morphology, and the electrochemical performance of the prepared samples were characterized by X-ray diffractometry (XRD), scanning electron microscopy (SEM), laser particle-size distribution measurement, and other electrochemical techniques. The results demonstrate that the LiFePO₄/C materials obtained from Fe(OH)₃ at 800°C and FeC₂O₄·2H₂O at 700°C have the similar electrochemical performances. The initial discharge capacities of LiFePO₄/C synthesized from Fe(OH)₃ and FeC₂O₄·2H₂O are 134.5 mAh·g⁻¹ and 137.4 mAh·g⁻¹ at the C/5 rate, respectively. However, the tap density of the LiFePO₄/C materials obtained from Fe(OH)₃ are higher, which is significant for the improvement of the capacity of the battery.     

Microstructure and microwave dielectric properties of CaO-B2O3-SiO2 glass ceramics with various B2O3 contents

The effects of B2O3 addition on both the sintering behavior and microwave dielectric properties of CaO-B2O3-SiO2 (CBS) glass ceramics were investigated by Fourier transform infrared spectroscopy (FTIR),X-ray diffractometry (XRD) and scanning electron microscopy (SEM).The results show that the increasing amount of B2O3 causes the increase of the contents of [BO3],[BO4] and [SiO4],which deduces the increase of CaB2O4 and α-SiO2 and the decrease of CaSiO3 correspondingly.No new phase is observed throughout the...     

Si3N4-doped Zr50Al15Ni10Cu25 glassy alloy by mechanical alloying and sintering process

Zr₅₀Al₁₅Ni₁₀Cu₂₅ amorphous powder was synthesized by mechanical alloying. The effect of Si₃N₄ addition on the crystallization behavior of the alloy during sintering process was studied. Thermal stability of the powders was performed by differential scanning calorimetry (DSC). The phase and microstructure of the powders and bulk specimens sintered were determined by X-ray diffractometry (XRD) and scanning electron microscopy (SEM). The results show that, introducing 0.05% (mass fraction) Si₃N₄ can enhance the crystallization activation energy of the Zr₅₀Al₁₅Ni₁₀Cu₂₅ amorphous powders, which indicates that Si₃N₄ addition has hindrance effect on forming crystals from Zr₅₀Al₁₅Ni₁₀Cu₂₅ amorphous powder. However, 0.10% Si₃N₄ results in the decrease of the crystallization activation energy, which makes its crystallization process easy to occur.     

Preparation of BN／SiO2 ceramics by PIP method

The precursor infiltration and pyrolysis(PIP) method for preparation of BN/SiO2 composites was used to improve mechanical properties, dielectric properties and feasibility of high temperature dielectric parts with large dimensions and complex shapes. In the processing procedure, the porous BN ceramic matrix was first successfully prepared by compacting the mixed powders of B and BN and then sintering them at a certain temperature under normal pressure of N2. The polycarbosilane(PCS) solution was vacuum infiltrated into porous BN ceramics at the room temperature and then at 800℃ in the air to depolimerize out amorphous SiO2, and sintered further at 1 300℃ in N2 to get BN/SiO2 composites. The microstructure of materials was studied by means of X-ray diffraction and electron probe micro analysis. The thermo-decomposition mechanism of PCS was investigated by a TG-DTA and infrared (IR) spectrum analysis. The flexural strengths were measured by the three-point bending method. The dielectric constant and the loss tangent were measured by the wave-guide method. The results show BN/SiO2 composites were fabricated. The obtained composites posses a flexural strength of 61.96 - 93.31 MPa, the dielectric constant in the range of 3.50 - 3.78 and the order of magnitude of the loss tangent at 10^-3 , which are good for the high tempera turedielectric parts with large size and complex shapes.     

Preparation and sintering of nano Fe coated Si3N4 composite powders

Fe/Si₃N₄ composite powder was synthesized by the heterogeneous precipitation-thermal reduction process, and then pressed into flakes under a pressure of 10 MPa. Flakes were sintered by pressureless and hot-pressing at 1 600 °C under 0.1 MPa N₂. The chemical composition, phases and microstructure of composite powder and sintered flakes were investigated by energy dispersive spectroscopy (EDS), X-ray diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The results show that the structure of composite powders is Si₃N₄ coated by nano Fe. The crystal phases of sintered flakes by pressureless are Fe(Si) compound, SiC and Si₃N₄. The crystal phases of the sintered samples by hot-pressing are Fe, Fe(Si) compound and Si₃N₄. It is found that crystal phases flakes obtained by pressureless and hot-pressing are very different. Foundation item: Project(50804016) supported by the National Natural Science Foundation of China