Preparation and properties of sintered molybdenum doped with La2O3/MoSi2

Sintered Mo with the addition of La₂O₃/MoSi₂ was prepared via the process of solid–solid doping + powder metallurgy. X-ray diffraction experiment, hardness test, three-point bending test and high-temperature tensile test were carried out to characterize the samples. The XRD pattern of a typical sample shows that the sintered Mo was mainly composed of Mo, La₂O₃ and Mo₅Si₃. Mo₅Si₃ was probably formed through the reaction between MoSi₂ and the Mo matrix. Densities and fracture toughnesses of both doped Mo and pure Mo were measured and contrasted. Sintered Mo with the addition of 0.2 wt% La₂O₃/MoSi₂ has the highest toughness, while more addition of La₂O₃/MoSi₂ has smaller effect on improving toughness or even embrittles Mo. The results of three-point bending test and high-temperature tensile test show that the bending strength and high-temperature tensile strength of doped Mo are both higher than those of pure Mo. The formation of Mo₅Si₃ improves the high-temperature strength. The La₂O₃/Mo₅Si₃ dispersed in the Mo matrix refined the grains, and thus strengthened the Mo matrix by dispersion strengthening and grain refinement.     

Microstructural changes in particles detected during the transformation from β-FeOOH to α-Fe2O3 in dense aqueous suspensions

The hydrothermal transformation from β-FeOOH to α-Fe₂O₃ in dense aqueous suspensions, obtained by partial neutralization of concentrated FeCl₃ solution with concentrated NaOH solution, was investigated. Mössbauer spectroscopy was used for the phase analysis of samples, as well as the complementary techniques XRD and FT-IR. The size and morphology of the particles were inspected with FE-SEM. At the beginning of the crystallization process very fine β-FeOOH particles were formed, which transformed to α-Fe₂O₃ (end-product) with a prolonged time of heating. A small amount or traces of α-FeOOH as an intermediate phase were detected by FT-IR and FE-SEM. Gradual formation of α-Fe₂O₃ double spheres with ring was monitored. Double spheres with ring were formed by the aggregation mechanism. The orientation effect of α-Fe₂O₃ subunits in double spheres with ring was observed. α-Fe₂O₃ double spheres with ring also showed two narrow particle size distributions.     

Synthesis of crystalline γ-Al2O3 with high purity

Crystalline γ-AlO(OH) was synthesized by the precipitation of sodium aluminate and oxalic acids in aqueous solution. And then γ-AlO(OH) was successfully transferred to γ-Al₂O₃ after subsequent high temperature heat treatment. The effects of reaction conditions on formation of γ-AlO(OH) and γ-Al₂O₃ were further investigated in detail. The XRD analysis shows that the complete formation of crystalline γ-Al₂O₃ is at pH 8–9, reaction temperature of 93–96 °C and calcination temperature of higher than 400 °C. The product of γ-Al₂O₃ contains impurity, including iron, calcium and silicon ion with a low content of about 0.01% and has large specific surface area and high pore volume of 269.9 m²/g and 0.57 mL/g, which can be applied in catalysts and catalyst supports.     

Thermal shock behavior of Si3N4-TiN nano-composites

Si₃N₄-TiN nano-composites were fabricated by hot press sintering nano-sized Si₃N₄ and TiN powders. The microstructure, mechanical properties and thermal shock behavior of Si₃N₄-TiN nano-composites were investigated. The addition of proper amount TiN particles can significantly increase the flexural strength and the fracture toughness. Si₃N₄-TiN nano-composites showed both higher critical temperature difference and higher residual strength compared with those of monolithic silicon nitride nano-ceramic when the amount of TiN is less than 15 wt.%. But a further increase in the amount of TiN leaded to a decrease in the thermal shock resistance.     

Role of titanium valence states in optical and electronic features of PbO–Sb2O3–B2O3:TiO2 glass alloys

PbO–Sb₂O₃–B₂O₃ glasses mixed with different concentrations of TiO₂ (ranging from 0 to 1.5 mol.%) were synthesized. The samples are characterized by X-ray diffraction, scanning electron microscopy and DSC techniques. A variety of properties, i.e. optical absorption, photoluminescence, infrared, ESR spectra, magnetic susceptibility, photo-induced birefringence (PIB) and dielectric properties (constant ′, loss tan δ, a.c. conductivity σ_ac over a wide range of frequency and temperature) of these glass–ceramics have been explored. The analysis of these results indicated that Ti ion surrounding ligands play principal role in the observed PIB and the sample crystallized with 0.8 mol.% of TiO₂ is the most suitable for the applications in non-linear optical devices.     

Densification, microstructure, and fracture behavior of TiC/Si3N4 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·m^½) values of Si₃N₄-based ceramics could be achieved at 1550°C. 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.     

Conductivity of a new pyrophosphate Sn0.9Sc0.1(P2O7)1−δ prepared by an aqueous solution method

New pyrophosphate Sn_0.9Sc_0.1(P₂O₇)_1−δ was prepared by an aqueous solution method. The structure and conductivity of Sn_0.9Sc_0.1(P₂O₇)_1−δ have been investigated. XRD analysis indicates that Sn_0.9Sc_0.1(P₂O₇)_1−δ exhibits a 3 × 3 × 3 super structure. It was found that Sn_0.9Sc_0.1(P₂O₇)_1−δ prepared by an aqueous method is not conductive. The total conductivity of Sn_0.9Sc_0.1(P₂O₇)_1−δ in open air is 2.35 × 10⁻⁶ and 2.82 × 10⁻⁹ S/cm at 900 and 400 °C respectively. In wet air, the total conductivity is about two orders of magnitude higher (8.1 × 10⁻⁷ S/cm at 400 °C) than in open air indicating some proton conduction. SnP₂O₇ and Sn_0.92In_0.08(P₂O₇)_1−δ prepared by an acidic method were reported fairly conductive but prepared by similar solution methods are not conductive. Therefore, the conductivity of SnP₂O₇-based materials might be related to the synthetic history. The possible conduction mechanism of SnP₂O₇-based materials has been discussed in detail.     

Toughening and strengthening mechanism of plasma sprayed nanostructured Al2O3–13 wt.%TiO2 coatings

The starting materials of Al₂O₃, TiO₂, ZrO₂ and CeO₂ nanoparticles were agglomerated into sprayable feedstock powders and plasma sprayed to form nanostructured coatings. There were net structures and fused structures in plasma sprayed nanostructured Al₂O₃–13 wt.%TiO₂ coatings. The net structures were derived from partially melted feedstock powders and the fused structures were derived from fully melted feedstock powders. The nanostructured Al₂O₃–13 wt.%TiO₂ coatings possessed higher hardness, bonding strength and crack growth resistance than conventional Metco 130 coatings which were mainly composed of lamellar fused structures. The higher toughness and strength of nanostructured Al₂O₃–13 wt.%TiO₂ coatings were mainly related to the obtained net structures.     

Deposition and characterization of CrN/Si3N4 and CrAlN/Si3N4 nanocomposite coatings prepared using reactive DC unbalanced magnetron sputtering

Nanocomposite coatings of CrN/Si₃N₄ and CrAlN/Si₃N₄ with varying silicon contents were synthesized using a reactive direct current (DC) unbalanced magnetron sputtering system. The Cr and CrAl targets were sputtered using a DC power supply and the Si target was sputtered using an asymmetric bipolar-pulsed DC power supply, in Ar + N₂ plasma. The coatings were approximately 1.5 μm thick and were characterized using X-ray diffraction (XRD), nanoindentation, X-ray photoelectron spectroscopy and atomic force microscopy. Both the CrN/Si₃N₄ and CrAlN/Si₃N₄ nanocomposite coatings exhibited cubic B1 NaCl structure in the XRD data, at low silicon contents (< 9 at.%). A maximum hardness and elastic modulus of 29 and 305 GPa, respectively were obtained from the nanoindentation data for CrN/Si₃N₄ nanocomposite coatings, at a silicon content of 7.5 at.%. (cf., 24 and 285 GPa, respectively for CrN). The hardness and elastic modulus decreased significantly with further increase in silicon content. CrAlN/Si₃N₄ nanocomposite coatings exhibited a hardness and elastic modulus of 32 and 305 GPa, respectively at a silicon content of 7.5 at.% (cf., 31 and 298 GPa, respectively for CrAlN). The thermal stability of the coatings was studied by heating the coatings in air for 30 min in the temperature range of 400-900 °C. The microstructural changes as a result of heating were studied using micro-Raman spectroscopy. The Raman data of the heat-treated coatings in air indicated that CrN/Si₃N₄ and CrAlN/Si₃N₄ nanocomposite coatings, with a silicon content of approximately 7.5 at.% were thermally stable up to 700 and 900 °C, respectively.     

采用Ti/Ag-Cu/Cu中间层钎焊连接Si3N4陶瓷和TiAl合金的界面结构及性能

采用Ti/Ag-Cu/Cu中间层实现了Si₃N₄陶瓷与TiAl合金的钎焊连接,获得了良好的接头.利用SEM,EDS等微观手段,分析了接头界面结构和元素分布情况.结果表明,Si₃N₄陶瓷/Ti/Ag-Cu/Cu/TiAl典型界面微观结构可能为:Si₃N₄/TiN/Ti-Si/Cu-Ti+Ag（s,s）+Cu（s,s）/AlCuTi/TiAl.在连接温度1 133 K、保温时间30 min、接头压力0.040 MPa时,接头四点弯曲强度达到最大值170 MPa.     

Densification and mechanical properties of fine-grained Al2O3-ZrO2 composites consolidated by spark plasma sintering

Alumina matrix composites containing 5 and 10 wt% of ZrO₂ were sintered under 100 MPa pressure by spark plasma sintering process. Alumina powder with an average particle size of 600 nm and yttria-stabilized zirconia with 16 at% of Y₂O₃ and with a particle size of 40 nm were used as starting materials. The influence of ZrO₂ content and sintering temperature on microstructures and mechanical properties of the composites were investigated. All samples could be fully densified at a temperature lower than 1400 °C. The microstructure analysis indicated that the alumina grains had no significant growth (alumina size controlled in submicron level 0.66-0.79 μm), indicating that the zirconia particles provided a hindering effect on the grain growth of alumina. Vickers hardness and fracture toughness of composites increased with increasing ZrO₂ content, and the samples containing 10 wt% of ZrO₂ had the highest Vickers hardness of 18 GPa (5 kg load) and fracture toughness of 5.1 MPa m^1/2.     

Improved high-Q microwave dielectric resonator using ZnO-doped La(Co1/2Ti1/2)O3 ceramics

The microwave dielectric properties and the microstructures of ZnO-doped La(Co_1/2Ti_1/2)O₃ ceramics prepared by conventional solid-state route have been studied. Doped with ZnO (up to 0.75 wt%) can effectively promote the densification of La(Co_1/2Ti_1/2)O₃ ceramics with low sintering temperature. At 1320 °C, La(Co_1/2Ti_1/2)O₃ ceramics with 0.75 wt% ZnO addition possesses a dielectric constant (_r) of 30.2, a Q × f value of 73,000 GHz (at 8 GHz) and a temperature coefficient of resonant frequency (τ_f) of −35 ppm/°C.     

Transport anisotropy and pseudo-gap state in oxygen deficient ReBa2Cu3O7−δ (Re = Y, Ho) single crystals

The temperature dependence of the transport anisotropy of ReBa₂Cu₃O_7−δ (Re = Y, Ho) single crystals is investigated. We experimentally determine the parallel and perpendicular conductivity in oxygen deficient single crystals. It is found that, in these single crystals, oxygen deficiency results to uneven oxygen distribution within their volume that leads to the formation of superconducting phases with different critical temperatures. We present an analysis regarding the agreement of the experimental data with the predictions of different theoretical models. It is determined that, the absolute values of the energy gaps along and perpendicular to the basis plane are changed, with different signs of their derivatives. When the value of Δ_c increases, the value of the pseudo-gap decreases and vice versa, testifying that the PG regime is suppressed, with a synchronous strengthening of the localization effects. In distinction to YBa₂Cu₃O_7−δ, the temperature dependence of the anisotropy of the resistivity ρ_c/ρ_ab(T) for the HoBa₂Cu₃O_7−δ samples is well described, by the universal “law of 1/2” for the thermally activated hopping conductivity.     

Bulk WC-Al2O3 composites prepared by spark plasma sintering

WC and WC-Al₂O₃ materials without metallic binder addition were densified by spark plasma sintering in the range of 1800-1900 °C. The densification behavior, phase constitution, microstructure and mechanical properties of pure WC and WC-Al₂O₃ composite were investigated. The addition of Al₂O₃ facilitates sintering and increases the fracture toughness of the composites to a certain extent. An interesting phenomenon is found that a proper content of Al₂O₃ additive helps to limit the formation of W₂C phase in sintered WC materials. The pure WC specimen possesses a hardness (HV₁₀) of 25.71 GPa, fracture toughness of 4.54 MPa·m^1/2, and transverse fracture strength of 862 MPa, while those of WC-6.8 vol.% Al₂O₃ composites are 24.48 GPa, 6.01 MPa·m^1/2, and 1245 MPa respectively. The higher fracture toughness and transverse fracture strength of WC-6.8 vol.% Al₂O₃ are thought to result from the reduction of W₂C phase, the crack-bridging by Al₂O₃ particles and the local change in fracture mode from intergranular to transgranular.     

Comparison of ZrB2-SiC ceramics with Yb2O3 additive prepared by hot pressing and spark plasma sintering

This work compared phase composition, microstructures and mechanical properties of ZrB₂—20 vol.% SiC—5 vol.%Yb₂O₃ prepared by hot pressing (HP) and spark plasma sintering (SPS) in vacuum. Despite the same raw material composition, the two densification techniques led to the appearance of different secondary phases. The HP ceramics had coarsened microstructure, predominantly intergranular fracture characteristic and high fracture toughness. The SPS ceramics exhibited refined microstructure, transgranular fracture model and high bending strength.     

Strengthening and toughening forming of Al/Al2O3 composite in pseudo-semi-solid state

A new technology—thixo-die-forging of the composite in pseudo-semi-solid state was proposed based on the powder metallurgy technology combing with semi-solid metal process, and the cup shells with Al/Al₂O₃  composite was prepared successfully. The metallographic analysis and performance test show that the microstructure of parts is dense and mechanical properties are excellent with the volume fraction of Al is 37 %. The bend strength and fracture toughness of the composite are about 570-690 MPa and 8.5-16.8 MPa m^1/2, respectively. Comparing with reaction in situ and high temperature oxidation technologies the bending strength and fracture toughness are improved greatly. At the same time, it shows that the technology parameters have great influences on the properties. So it is feasible to prepare metal/ceramics composites by the proposed technology.     

Structure and mechanical properties of TiAlSiN/Si3N4 multilayer coatings

TiAlSiN/Si₃N₄ multilayer coatings which have different separate layer thicknesses of TiAlSiN or Si₃N₄ were deposited onto glass sheets, single-crystal silicon wafers and polished WC-Co substrates by reactive magnetron co-sputtering. The morphology, crystalline structure and thickness of the as-prepared multilayer coatings were characterized by TEM, SEM, XRD and film thickness measuring instrument. The mechanical properties of the coatings were evaluated by a nanoindenter. The effects of monolayer thickness on the microstructure and properties of TiAlSiN/Si₃N₄ multilayer coatings were explored. The coatings showed the highest hardness when the thickness of Si₃N₄ and TiAlSiN monolayers was 0.33 nm and 5.8 nm, respectively. The oxidation characteristics of the coatings were studied at temperatures ranging from 700 °C to 900 °C for oxidation time up to 20 h in air. It was found that the coatings displayed good oxidation resistance.     

Preparation of nanometric CeO2–ZrO2–Nd2O3 solid solution and its catalytic performances

A kind of nanometric CeO₂–ZrO₂–Nd₂O₃ (CZN) solid solution for a carrier in the automotive three-way catalysts was synthesized by a coprecipitation method and characterized by means of X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), nitrogen adsorption–desorption (BET), scanning electron microscopy (SEM) and oxygen storage capacity (OSC). For the purpose of comparison, an unincorporated CeO₂–ZrO₂ (CZ) was also synthesized. The XRD measurements disclose the prepared CeO₂–ZrO₂–Nd₂O₃ have a face-centered cubic fluorite structure and nanoparticle sizes. According to the results of XPS, Nd³⁺ ions can enter the CZ lattice and form a homogenous solid solution. Oxygen storage capacity measurements reveal that CeO₂–ZrO₂–Nd₂O₃ display high oxygen mobility at a low temperature. The results of the activity tests show that the catalyst exhibits good three-way catalytic activity and fairly wide range of air-to-fuel ratios.     

The oxidation of cobalt based alloys containing partially dissolved particles of Si3N4 at 1000°C

The isothermal oxidation behavior of Co-Cr and Co-Cr-Si alloys with and without 5, 10, and 15 vol.% dispersions of unstable Si₃N₄ particles was studied in 1 atm of oxygen at 1000°C. The dispersion of Si₃N₄ which dissolved partially in the matrix, greatly reduced the oxidation rate of Co-Cr alloys. Silicon nitride was found to promote the formation of continuous Cr₂O₃ layers at low chromium concentrations. Furthermore, the unstable Si₃N₄ was more effective in reducing the oxidation rate than an alloy containing an equivalent amount of silicon. Additions of 15vol.% Si₃N₄ tended to increase the oxidation rate by forming nonprotective SiO₂ particles which disrupted the protective Cr₂O₃ scale. The mechanism of oxidation was altered due to the Si₃N₄ additions. Marker experiments indicated oxygen diffusion inward via the CoO lattice, rather than a combination of both oxygen and metal ion motion which is encountered in Co-Cr alloys.     

Influences of annealing temperature on microstructure and mechanical properties of Mo-La2O3

Influences of annealing temperature on the microstructure and mechanical properties of Mo-La₂O₃ were investigated. Effects of annealing temperature on tensile properties, fracture toughness, and microhardness are discussed. Microstructure and fracture morphology of Mo alloys are observed by optical microscope, SEM, and TEM. The results indicate that grain size increased while tensile strength, fracture toughness, and microhardness decreased with increasing annealing temperature. Larger La₂O₃ particles are located at grain boundaries or sub-boundaries, while the majority of smaller La₂O₃ particles are located within the grain. The strengthening effect is quantitatively assessed, which yielded a predicted yield strength in good agreement with measurements.