Fabrication of Ti<Subscript>3</Subscript>AlC<Subscript>2</Subscript> ceramic material by mechanical alloying

Ti₃AlC₂ has the properties of ceramics and metals. These excellent properties indicate that Ti₃AlC₂ is a very promising material to extensive applications. Ti₃AlC₂ ceramic material was prepared by mechanical alloying. The effects of milling time and sintering temperature on the fracture, microstructure and mechanical properties of Ti₃AlC₂ ceramic material were analyzed by laser particle analyzer, X-ray diffraction, and scanning electron microscopy. The experimental results showed that Ti₃AlC₂ had the best comprehensive properties after the composite powder was milled for 3 h and sintered at 1630°C for 2 h. The relative density, bending strength, and hardness of the sample reached 92.23%, 345.2 MPa, and HRA 34.1, respectively. The fracture surface indicated that the fracture of the material belonged to ductile rapture.     

Sintering characteristics and microstructure of WC-Co-VC/Cr<Subscript>3</Subscript>C<Subscript>2</Subscript> ultrafine cemented carbides

The sintering characteristics, microstructure, and mechanical properties of ultrafine WC-12%Co-0.2%VC/0.5%Cr₃C₂ cemented carbides were investigated. Dilatometric and differential thermal analyses (DTA) indicate that the compacts start to shrink at 600°C, the shrinkage rate peak is at 1190°C, and the liquid formation temperature is lower than the W-C-Co eutectic temperature (1330°C). Microstructure analysis results show that the cemented carbides with fine and homogeneous microstructure were obtained when sintered at 1430°C. Continuous and discontinuous grain growth was suppressed due to the synergistic action of VC/Cr₃C₂. The transverse rupture strength (TRS) of the samples reaches 4286 MPa, with the hardness HRA 92.1. The fine and homogeneous microstructure, alloy strengthening, and different phase constitutions of binder in the cemented carbides result in high hardness and TRS. Continuous and discontinuous grain growth was observed in the cemented carbide sintered at 1450°C, which results in significant decreases of hardness and TRS. It indicates that VC/Cr₃C₂ additions in the cemented carbides can only suppress the grain growth at a certain temperature.     

Microstructure and Physical Properties of Tb<Subscript>2</Subscript>TiO<Subscript>5</Subscript> Neutron Absorber Synthesized by Ball Milling and Sintering

Tb₂TiO₅ neutron absorber was synthesized by ball milling and sintering. Microstructure character of ball-milled Tb₄O₇-17.605%TiO₂ (mass fraction, %) powders and sintered bulks was analyzed using XRD, SEM and TEM. The microhardness, coefficient of thermal expansion and thermal conductivity of sintered bulks were measured. The experiment results showed that the nanocrystalline solid solution was obtained during ball milling. After 96 h of ball milling, TiO₂ was completely solved in Tb₄O₇ and the crystal size of Tb₄O₇ was up to 37 nm. The bulk materials prepared by cold isostatic pressing were sintered at 1300 °C. Tb₂TiO₅ bulks with an orthorhombic structure were obtained. The microhardness of sintered bulks, as well as the thermal conductivity, increased firstly with increasing ball milling time and then decreased. The coefficient of thermal expansion decreased initially and then increased with increasing ball milling time. For the sintered bulk with powder milled for 48 h, the highest values of both microhardness and thermal conductivity were observed, whereas the lowest coefficient of thermal expansion was exhibited. In addition, with increasing testing temperature, the thermal conductivity of sintered bulks initially fell and then rebounded while an opposite trend was found in the coefficient of thermal expansion.     

Preparation and characterization of nanostructured Al<Subscript>2</Subscript>O<Subscript>3</Subscript>-13wt.%TiO<Subscript>2</Subscript> ceramic coatings by plasma spraying

Nanostructured and conventional Al₂O₃-13wt.%TiO₂ ceramic coatings were prepared by plasma spraying with nanostructured agglomerated and conventional powders, respectively. The microstructure and microhardness of the coatings were investigated using scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS), and microhardness measurement. Meanwhile, the friction and wear behaviors were analyzed and compared using a ball-on-disk tribometer. The results show that the conventional coating has lamellar stacking characteristic and has some pores. However, the nanostructured coating shows a bimodal microstructure, which is composed of both fully melted regions and partially melted regions. According to the microstructural difference, the partially melted regions can be divided into liquid-phase sintered regions (a three-dimensional net or skeleton-like structure: Al₂O₃-rich submicron particles embedded in the TiO₂-rich matrix) and solid-phase sintered regions (remained nanoparticles). The microstructural characteristics of the liquid-phase sintered region are formed due to the selective melting of TiO₂ nanoparticles during plasma spraying. On the other hand, the TiO₂ and Al₂O₃ nanoparticles of the solid-phase sintered regions are all unmelted during plasma spraying. Due to the existence of nanostructured microstructures, the nanostructured coating has a higher microhardness, a lower friction coefficient, and a better wear resistance than the conventional coating.     

Grain refinement and mechanism of CAl_（0.5）W_（0.5） compound in Mg-Al alloys

The effect of CAl0.5W0.5(CAW) compound on the grain refinement of Mg-Al based alloys was investigated.The results show that CAW compound is an effective and active grain refiner.The grain size of binary Mg-Al alloys is more than 500 μm,and it is changed to about 110 μm with a 1 wt.% CAW addition.The hardness increased with the decease of grain size monotonously.The mechanical properties are improved by the addition.The fine grain size is mainly ascribed to the dispersed Al2CO particles,which are very potent nucleating substrates for Mg-Al alloys.The nucleation cores formed by chemical reaction directly are well-distributed in the matrix.     

Influence of processing parameters on the phase composition of ZrN-Si<Subscript>3</Subscript>N<Subscript>4</Subscript> synthesized from zircon

The optimum parameters were determined for synthesizing ZrN-Si₃N₄ composite powder from zircon by carbothermal reduction-nitridation (CTRN) process. The samples were prepared by mixing the carbon black of an average particle size less than 30 μm and the zircon of 40 μm with C/ZrSiO₄ mass ratios of 0.2, 0.3, 0.4, and 0.5. The prepared samples were subjected to the CTRN process at temperatures of 1673, 1723, 1753, and 1773 K for 6, 9, and 12 h. The CTRN process was conducted in an atmosphere-controlled tubular furnace in a nitrogen gas flow of 1.0 L/min. All the products were examined by X-ray powder diffraction to determine the transformation. The results showed that the proper transformation of ZrN-Si₃N₄ occurred at 1773 K for 12 h with a C/ZrSiO₄ mass ratio of 0.4.     

Preparation and magnetic properties of Fe<Subscript>2</Subscript>O<Subscript>3</Subscript> microtubules prepared by sol-gel template method

Fe(OH)₃ precursor sol was prepared by a sol-gel method. The precursor sol was dipped onto the absorbent cotton, and gel was formed on the absorbent cotton template after the volatilization of moisture. Fe₂O₃ microtubules were synthesized after the process of self-propagation or calcination. The phase, morphology, and particle diameter of the samples were examined by X-ray diffraction (XRD) and scanning electron microscopy (SEM), and the magnetic properties of the samples were measured using a vibrating sample magnetometer (VSM). The external diameters of Fe₂O₃ microtubules ranged between 8 and 13 μm, and the wall thicknesses ranged between 0.5 and 2 μm. The type of the calcination method plays a significant role in developing the Fe₂O₃ phase and the variation in the magnetic properties in the sol-gel template complexing method. γ-Fe₂O₃ was synthesized by a self-propagation method. However, α-Fe₂O₃ was synthesized after calcination at 400°C for 2 h. The coercivity of the samples synthesized by calcination at 400°C for 2 h after self-propagation was found to increase significantly, thereby presenting hard magnetic properties.     

Effects of nano-TiO<Subscript>2</Subscript> dispersion on thermoelectric properties of Co<Subscript>4</Subscript>Sb<Subscript>11.7</Subscript>Te<Subscript>0.3</Subscript> composites

Nano-TiO2/Co4Sb11.7Te0.3 composites were prepared by mechanical alloying (MA) and cold isostatic pressing (CIP) process.The phase composition,microstructure,and thermoelectric properties were characterized.The diffraction spectra of all samples well corresponds to CoSb3 skutterudite diffraction plane.TiO2 agglomerates into irregular clusters.They locate at the grain boundaries or some are distributed on the surface of Co4Sb11.7Te0.3 particles.For composites with high TiO2 content (0.6% and 1.0% TiO2),the phonon scattering by TiO2 particle,pores,and small size grains can result in a remarkable reduction in thermal conductivity.The maximum value of ZT is 0.79 for sample with 0.6 wt.% TiO2 at 700 K,which is 11% higher than that of non-dispersed sample.     

PTCR characteristics and microstructure of porous (Ba,Sr)TiO<Subscript>3</Subscript> ceramics prepared by spark plasma sintering

Porous Y-doped (Ba,Sr)TiO₃ ceramics were prepared by the spark plasma sintering of (Ba,Sr)TiO₃ powders with different amounts of carbon black, and by subsequently burning out the carbon black acting as a pore precursor. The microstructure, PTCR and gas-sensing characteristics for porous Y-doped (Ba,Sr)TiO₃ ceramics were investigated. Spark plasma sintered (Ba,Sr)TiO₃ ceramics revealed a very fine microstructure containing submicron-sized grains with a cubic phase and revealed an increased porosity after the carbon black was burned out. As a result of reoxidation treatment, the grain size of the (Ba,Sr)TiO₃ ceramics increased to a few μm and the cubic phase transformed into a tetragonal phase. The phase transformation of (Ba,Sr)TiO₃ ceramics was affected by grain size. The PTCR jump in the (Ba,Sr)TiO₃ ceramics prepared by adding 40 vol.% carbon black showed an excellent value of 4.72 × 10⁶, which was ten times higher than the PTCR jump in (Ba,Sr)TiO₃ ceramics. The electrical resistivity of the porous (Ba,Sr)TiO₃ ceramics was recovered as the atmosphere changed from a reducing gas (N₂) to an oxidizing gas (O₂) under consecutive heating and cooling cycles.     

Mechano-thermal treatment of TiO<Subscript>2</Subscript>-Al powder mixture to prepare TiAl/Al<Subscript>2</Subscript>O<Subscript>3</Subscript> composite

In this research, a composite comprising an intermetallic matrix and dispersed Al₂O₃ particles was processed. A mixture of TiO₂ and Al was mechanically activated in the presence of a process control agent and/or without it, in a high-energy planetary ball mill. As a subsequent process, the sample was sintered at various temperatures. The phase composition and morphology of the samples were evaluated by XRD and SEM techniques, respectively. The thermal behavior of the samples milled for 8 h with PVA and/or without it, were also assessed by the DTA technique and compared with one another. The DTA results revealed that addition of PVA shifted the aluminothermic reduction of TiO₂ to higher temperatures; therefore, final composite phases were developed at higher temperatures. The results also showed that addition of PVA during milling caused the final microstructure to coarsen. The XRD pattern of the sample sintered at 700 °C exhibits the existence of TiAl, Ti₃Al, and Al₂O₃ phases. In the sample sintered at 850 °C, the remaining Ti₃Al peak was attenuated and completely disappeared at 1000 °C.     

Preparation and optical properties of Y<Subscript>2</Subscript>O<Subscript>3</Subscript>/SiO<Subscript>2</Subscript> powder

Y(NO3)3 and NH3·H2O were used as a raw materials,and nano-Y2O3 powder was successfully synthesized by a precipitation method.Employing TEOS as a raw material,SiO2 powder was successfully prepared by a alkoxide-hydrolysis method,and a Y2O3/SiO2 composite powder was obtained by coating.The Y2O3,SiO2,and Y2O3/SiO2 powders were characterized using X-ray diffraction(XRD),scanning electron microscopy(SEM),and Fourier transform infrared spectrophotometer(FT-IR);the Y2O3 and Y2O3/SiO2 powders were further examined ...     

Solvothermal synthesis and thermoelectric properties of skutterudite compound Fe（0.25）Ni（0.25）Co（0.5）Sb3

Nanostructured skutterudite-related compound Fe_0.25Ni_0.25Co_0.5Sb₃ was synthesized by a solvothermal method using FeCl₃, NiCl₂, CoCl₂, and SbCl₃ as the precursors and NaBH₄ as the reductant. The solvothermally synthesized powders consisted of fine granules with an average particle size of tens of nanometers. The bulk material was prepared by hot pressing the powders. Transport property measurements indicated a heavily doped semiconductor behavior with n-type conduction. The thermal conductivity is about 1.83 W·m⁻¹·K⁻¹ at room temperature and decreases to 1.57 W·m⁻¹·K⁻¹ at 673 K. The low thermal conductivity is attributed to small grain size and high porosity. A maximum dimensionless figure of merit of 0.15 is obtained at 673 K.     

Influence of Feedstock Powder Modification by Heat Treatments on the Properties of APS-Sprayed Al<Subscript>2</Subscript>O<Subscript>3</Subscript>-40% TiO<Subscript>2</Subscript> Coatings

The formation and decomposition of aluminum titanate (Al₂TiO₅, tialite) in feedstock powders and coatings of the binary Al₂O₃-TiO₂ system are so far poorly understood. A commercial fused and crushed Al₂O₃-40%TiO₂ powder was selected as the feedstock for the experimental series presented in this paper, as the composition is close to that of Al₂TiO₅. Part of that powder was heat-treated in air at 1150 and 1500 °C in order to modify the phase composition, while not influencing the particle size distribution and processability. The powders were analyzed by thermal analysis, XRD and FESEM including EDS of metallographically prepared cross sections. Only a maximum content of about 45 wt.% Al₂TiO₅ was possible to obtain with the heat treatment at 1500 °C due to inhomogeneous distribution of Al and Ti in the original powder. Coatings were prepared by plasma spraying using a TriplexPro-210 (Oerlikon Metco) with Ar-H₂ and Ar-He plasma gas mixtures at plasma power levels of 41 and 48 kW. Coatings were studied by XRD, SEM including EDS linescans of metallographically prepared cross sections, and microhardness HV1. With the exception of the powder heat-treated at 1500 °C an Al₂TiO₅-Ti₃O₅ (tialite–anosovite) solid solution Al_2?xTi_1+xO₅ instead of Al₂TiO₅ existed in the initial powder and the coatings.     

超细硬质合金中晶粒非均匀长大机理

采用市售的粒度为0.8μm的WC粉末和粒度为1.6μm的Co粉制备了WC-10%Co超细硬质合金,通过金相显微镜﹑扫描电子显微镜观察了不同烧结温度下制备的试样WC晶粒形貌,对超细晶粒硬质合金非均匀长大现象及机理进行了研究。结果表明:粉末湿磨后的粗大颗粒在烧结过程中起晶核作用,是引起晶粒非均匀长大的关键因素。固相烧结时,烧结体中细小颗粒受到张力的作用发生旋转,当其取向与邻近的大颗粒取向一致时,形成共格界面,以粗大晶粒为核心以并合的方式非均匀长大;液相烧结时,细小晶粒溶解并优先地在大晶粒的某些低能量晶面如(0001)和(1010)面析出,引起晶粒异常长大。本研究中,当烧结温度达到1 410℃时,WC晶粒可异常长大为接近20μm的粗大晶粒。     

Al<Subscript>2</Subscript>O<Subscript>3</Subscript>-TiC Composite Prepared by Spark Plasma Sintering Process: Evaluation of Mechanical and Tribological Properties

Al₂O₃-10TiC composites were synthesized by spark plasma sintering (SPS) process. Microstructural and mechanical properties of the composite reveal homogeneous distribution of the fine TiC particles in the matrix. The samples were produced with different sintering temperature, and it shows that the hardness and density gradually increases with increasing sintering temperature. Abrasion wear test result reveals that the composite sintered at 1500 °C shows high abrasion resistance (wt. loss ~ 0.016 g) and the lowest abrasion resistance was observed for the composite sample sintered at 1100 °C (wt. loss ~ 1.459 g). The profilometry surface roughness study shows that sample sintered at 1100 °C shows maximum roughness (R_a = 6.53 µm) compared to the sample sintered at 1500 °C (R_a = 0.66 µm) corroborating the abrasion wear test results.     

Fabrication of Al matrix composite reinforced with submicrometer-sized Al<Subscript>2</Subscript>O<Subscript>3</Subscript> particles formed by combustion reaction between HEMM Al and V<Subscript>2</Subscript>O<Subscript>5</Subscript> composite particles during sintering

To fabricate an Al-V matrix composite reinforced with submicron-sized Al₂O₃ and Al_xV_y (Al₃V, Al₁₀V) phases, high energy mechanical milling (HEMM) and sintering were employed. By increasing the milling time, the size of mechanically milled powder was significantly reduced. In this study, the average powder size of 59 μm for Al, and 178 μm for V₂O₅ decreased with the formation of a new product, Al-Al₂O₃-Al_xV_y, with a size range from 1.3 μm to 2.6 μm formed by the in-situ combustion reaction during sintering of HEM milled Al and V₂O₅ composite powders. The in-situ reaction between Al and V₂O₅ during the HEMM and sintering transformed the Al₂O₃ and Al_xV_y (Al₃V, Al₁₀V) phases. Most of the reduced V reacted with excess the Al to form Al_xV_y (Al₃V, Al₁₀V) with very little V dissolved into Al matrix. By increasing the milling time and weight percentage of V₂O₅, the hardness of the Al-Al₂O₃-Al_xV_y composite sintered at 1173 K increased. The composite fabricated with the HEMM Al-20wt.%V₂O₅ composite powder and sintering at 1173 K for 2 h had the highest hardness.     

Microstructure and hardness of Mg-based composites reinforced with Mg<Subscript>2</Subscript>Si particles

Magnesium powders were mechanically alloyed with SiO₂ powder particles having different particle sizes using high-energy ball milling techniques under Ar atmosphere for 1 h. The powders were consolidated with cold pressing under 560 MPa. They were then sintered at 550°C for 45 min under Ar atmosphere. The composites obtained on the Mg-SiO₂ system were investigated using the Archimedes principle, a differential scanning calorimeter, X-ray diffraction, optic microscopy, and scanning electron microscopy. For the mechanically alloyed powders, the solid-state reaction of the synthesis of Mg₂Si and MgO progressed further during sintering of the materials. The results showed that the strengthening mechanisms were dependent on dispersion hardening of fine Mg₂Si and MgO particulates dispersed homogeneously in the matrix.     

Fabrication by Electrophoretic Deposition of Nano-Fe<Subscript>3</Subscript>O<Subscript>4</Subscript> and Fe<Subscript>3</Subscript>O<Subscript>4</Subscript>@SiO<Subscript>2</Subscript> 3D Structure on Carbon Fibers as Supercapacitor Materials

Core–shell nanostructured magnetic Fe₃O₄@SiO₂ with particle size ranging from 3 nm to 40 nm has been synthesized via a facile precipitation method. Tetraethyl orthosilicate was employed as surfactant to prepare core–shell structures from Fe₃O₄ nanoparticles synthesized from pomegranate peel extract using a green method. X-ray diffraction analysis, Fourier-transform infrared and ultraviolet–visible (UV–Vis) spectroscopies, transmission electron microscopy, and scanning electron microscopy with energy-dispersive spectroscopy were employed to characterize the samples. The prepared Fe₃O₄ nanoparticles were approximately 12 nm in size, and the thickness of the SiO₂ shell was?~?4 nm. Evaluation of the magnetic properties indicated lower saturation magnetization for Fe₃O₄@SiO₂ powder (~?11.26 emu/g) compared with Fe₃O₄ powder (~?13.30 emu/g), supporting successful wrapping of the Fe₃O₄ nanoparticles by SiO₂. As-prepared powders were deposited on carbon fibers (CFs) using electrophoretic deposition and their electrochemical behavior investigated. The rectangular-shaped cyclic voltagrams of Fe₃O₄@CF and Fe₃O₄@C@CF samples indicated electrochemical double-layer capacitor (EDLC) behavior. The higher specific capacitance of 477 F/g for Fe₃O₄@C@CF (at scan rate of 0.05 V/s in the potential range of ??1.13 to 0.45 V) compared with 205 F/g for Fe₃O₄@CF (at the same scan rate in the potential range of?~???1.04 to 0.24 V) makes the former a superior candidate for use in energy storage applications.     

Preparation and characterization of nanostructured Bi<Subscript>2</Subscript>Se<Subscript>3</Subscript> and Sn<Subscript>0.5</Subscript>-Bi<Subscript>2</Subscript>Se<Subscript>3</Subscript>

Nanostructured Bi₂Se₃ and Sn_0.5-Bi₂Se₃ were successfully synthesized by hydrothermal coreduction from SnCl₂·H₂O and the oxides of Bi and Se. The products were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), and field emission scanning electron microscope (FESEM). Bi₂Se₃ powders obtained at 180°C and 150°C consist of hexagonal flakes of 50–150 nm in side length and nanorods of 30–100 nm in diameter and more than 1 μm in length. The product obtained at 120°C is composed of thin irregular nanosheets with a size of 100–200 nm and several nanometers in thickness. The major phase of Sn_0.5-Bi₂Se₃ synthesized at 180°C is similar to that of Bi₂Se₃. Sn_0.5-Bi₂Se₃ powders are primarily nanorod structures, but small amount of powders demonstrate irregular morphologies.     

Microstructure and Room-Temperature Mechanical Properties of FeCrMoVTi<Subscript><Emphasis Type="Italic">x</Emphasis></Subscript> High-Entropy Alloys

FeCrMoVTi _x (x values represent the molar ratio, where x = 0, 0.5, 1.0, 1.5, and 2.0) high-entropy alloys were prepared by a vacuum arc melting method. The effects of Ti element on the microstructure and room-temperature mechanical properties of the as-cast FeCrMoVTi _x alloys were investigated. The results show that the prepared alloys exhibited typical dendritic microstructure and the size of the microstructure became fine with increasing Ti content. The FeCrMoV alloy exhibited a single body-centered cubic structure (BCC1) and the alloys prepared with Ti element exhibited BCC1 + BCC2 mixed structure. The new BCC2 phase is considered as (Fe, Ti)-rich phase and was distributed in the dendrite region. With the increase of Ti content, the volume fraction of the BCC2 phase increased and its shape changed from a long strip to a network. For the FeCrMoV alloy, the fracture strength, plastic strain, and hardness reached as high as 2231 MPa, 28.2%, and 720 HV, respectively. The maximum hardness of 887 HV was obtained in the FeCrMoVTi alloy. However, the fracture strength, yield stress, and plastic strain of the alloys decreased continuously as Ti content increased. In the room-temperature compressive test, the alloys showed typical brittle fracture characteristics.