Growth characteristics of directionally solidified Al2O3/YAG/ZrO2 ternary hypereutectic in situ composites under ultra-high temperature gradient

Oxide eutectic ceramic in situ composites have attracted significant interest in the application of high-temperature structural materials because of their excellent high-temperature strength,oxidation and creep resistance,as well as outstanding microstructural stability.The directionally solidified ternary Al2O3/YAG/ZrO2 hypereutectic in situ composite was successfully prepared by a laser zone remelting method,aiming to investigate the growth characteristic under ultra-high temperature gradient.The microstructures and phase composition of the as-solidified hypereutectic were characterized by using scanning electron microscopy(SEM),energy dispersive spectroscopy(EDS),and X-ray diffraction(XRD).The results show that the composite presents a typical hypereutectic lamellar microstructure consisting of fine Al2O3 and YAG phases,and the enriched ZrO2 phases with smaller sizes are randomly distributed at the Al2O3/YAG interface and in Al2O3 phases.Laser power and scanning rate strongly affect the sample quality and microstructure characteristic.Additionally,coarse colony microstructures were also observed,and their formation and the effect of temperature gradient on the microstructure were discussed.     

Mineral-phase evolution and sintering behavior of MO-SiO2-Al2O3-B2O3 (M=Ca,Ba) glass-ceramics by low-temperature liquid-phase sintering

In this work, network former SiO₂ and network intermediate Al₂O₃ were introduced into typical low-melting binary compositions CaO·B₂O₃, CaO·2B₂O₃, and BaO·B₂O₃ via an aqueous solid-state suspension milling route. Accordingly, multiple-phase aluminosilicate glass-ceramics were directly obtained via liquid-phase sintering at temperatures below 950℃. On the basis of liquid-phase sintering theory, mineral-phase evolutions and glass-phase formations were systematically investigated in a wide MO-SiO₂-Al₂O₃-B₂O₃ (M=Ca, Ba) composition range. The results indicate that major mineral phases of the aluminosilicate glass-ceramics are Al₂₀B₄O₃₆, CaAl₂Si₂O₈, and BaAl₂Si₂O₈ and that the glass-ceramic materials are characterized by dense microstructures and excellent dielectric properties.     

Preparation and radar-absorbing properties of Al<Subscript>2</Subscript>O<Subscript>3</Subscript>/TiO<Subscript>2</Subscript>/Fe<Subscript>2</Subscript>O<Subscript>3</Subscript>/Yb<Subscript>2</Subscript>O<Subscript>3</Subscript> composite powder

Al₂O₃/TiO₂/Fe₂O₃/Yb₂O₃ composite powder was synthesized via the sol-gel method. The structure, morphology, and radar-absorption properties of the composite powder were characterized by transmission electron microscopy, X-ray diffraction analysis and RF impedance analysis. The results show that two types of particles exist in the composite powder. One is irregular flakes (100-200 nm) and the other is spherical Al₂O₃ particles (smaller than 80 nm). Electromagnetic wave attenuation is mostly achieved by dielectric loss. The maximum value of the dissipation factor reaches 0.76 (at 15.68 GHz) in the frequency range of 2-18 GHz. The electromagnetic absorption of waves covers 2-18 GHz with the matching thicknesses of 1.5-4.5 mm. The absorption peak shifts to the lower-frequency area with increasing matching thickness. The effective absorption band covers the frequency range of 2.16-9.76 GHz, and the maximum absorption peak reaches -20.18 dB with a matching thickness of 3.5 mm at a frequency of 3.52 GHz.     

Dissolution of Al<Subscript>2</Subscript>TiO<Subscript>5</Subscript> inclusions in CaO-SiO<Subscript>2</Subscript>-Al<Subscript>2</Subscript>O<Subscript>3</Subscript> slags at 1823 K

Al-Ti-O inclusions always clog submerged nozzles in Ti-bearing Al-killed steel. A typical synthesized Al₂TiO₅ inclusion was immersed in a CaO-SiO₂-Al₂O₃ molten slag for different durations at 1823 K. The Al₂TiO₅ dissolution paths and mechanism were revealed by scanning electron microscopy (SEM) and energy dispersive spectroscopy (EDS). Decreased amounts of Ti and Al and increased amounts of Si and Ca at the dissolution boundary prove that inclusion dissolution and slag penetration simultaneously occur. SiO₂ diffuses or penetrates the inclusion more quickly than CaO, as indicated by the w(CaO)/w(SiO₂) value in the reaction region. A liquid product (containing 0.7–1.2 w(CaO)/w(SiO₂), 15wt%–20wt% Al₂O₃, and 5wt%–15wt% TiO₂) forms on the inclusion surface when Al₂TiO₅ is dissolved in the slag. Al₂TiO₅ initially dissolves faster than the diffusion rate of the liquid product toward the bulk slag. With increasing reaction time, the boundary reaches its largest distance, the Al₂TiO₅ dissolution rate equals the liquid product diffusion rate, and the dissolution process remains stable until the inclusion is completely dissolved.     

Microstructure and properties of mullite-based porous ceramics produced from coal fly ash with added Al<Subscript>2</Subscript>O<Subscript>3</Subscript>

Using coal fly ash slurry samples supplemented with different amounts of Al₂O₃, we fabricated mullite-based porous ceramics via a dipping-polymer-replica approach, which is a popular method suitable for industrial application. The microstructure, phase composition, and compressive strength of the sintered samples were investigated. Mullite was identified in all of the prepared materials by X-ray diffraction analysis. The microstructure and compressive strength were strongly influenced by the content of Al₂O₃. As the Al/Si mole ratio in the starting materials was increased from 0.84 to 2.40, the amount of amorphous phases in the sintered microstructure decreased and the compressive strength of the sintered samples increased. A further increase in the Al₂O₃ content resulted in a decrease in the compressive strength of the sintered samples. The mullite-based porous ceramic with an Al/Si molar ratio of 2.40 exhibited the highest compressive strength and the greatest shrinkage among the investigated samples prepared using coal fly ash as the main starting material.     

Near-infrared to visible up-conversion emissions of Er^3＋ doped Al2O3 powders derived from the sol-gel method

The Er3 doped Al2O3 powders were prepared by the sol-gel method using the aluminium isopropoxide [Al(OC3H7)3]-derived Al2O3 sols with addition of the erbium nitrate [Er(NO3)3.5H2O]. The different phase structure, including three crystalline types of (Al,Er)2O3 phases, γ, θ, α, and two Er-Al-O phases, ErAlO3 and Al10Er6O24, was obtained with the 1 mol% Er3 doped Al2O3 powders at the different sintering temperatures of 600―1200℃. The green and red up-conversion emissions centered at about 523, 545 and 660 nm, corresponding respectively to the 2H11/2, 4S3/2→4I15/2 and 4F9/2→4I15/2 transitions of Er3 , were detected by a 978 nm semiconductor laser diodes excitation. The phase structure and OH content had evident influence on the up-conversion emissions intensity. The maximum intensities of both the green and red emissions were obtained respectively for the Er3 doped Al2O3 powders sintered at 1200 ℃, which was composed mainly of α-(Al,Er)2O3, less of ErAlO3 and Al10Er6O24 phases, and with the least OH content. The two-photon absorption up-conversion process was involved in the green and red up-conversion emissions of the Er3 doped Al2O3 powders.     

Effects of metal binder on the microstructure and mechanical properties of Al<Subscript>2</Subscript>O<Subscript>3</Subscript>-based micro-nanocomposite ceramic tool material

The Al₂O₃-(W,Ti)C composites with Ni and Mo additions varying from 0vol% to 12vol% were prepared via hot pressing sintering under 30 MPa. The microstructure was investigated via X-ray diffraction (XRD) and scanning electron microscopy (SEM) equipped with energy dispersive spectrometry (EDS). Mechanical properties such as flexural strength, fracture toughness, and Vickers hardness were also measured. Results show that the main phases Al₂O₃ and (W,Ti)C were detected by XRD. Compound MoNi also existed in sintered nanocomposites. The fracture modes of the nanocomposites were both intergranular and transgranular fractures. The plastic deformation of metal particles and crack bridging were the main toughening mechanisms. The maximum flexural strength and fracture toughness were obtained for 9vol% and 12vol% additions of Ni and Mo, respectively. The hardness of the composites reduced gradually with increasing content of metals Ni and Mo.     

Electrical conductivity optimization of the Na3AlF6-Al2O3-Sm2O3 molten salts system for Al-Sm intermediate binary alloy production

Metal Sm has been widely used in making Al-Sm magnet alloy materials. Conventional distillation technology to produce Sm has the disadvantages of low productivity, high costs, and pollution generation. The objective of this study was to develop a molten salt electrolyte system to produce Al-Sm alloy directly, with focus on the electrical conductivity and optimal operating conditions to minimize the energy consumption. The continuously varying cell constant (CVCC) technique was used to measure the conductivity for the Na₃AlF₆-AlF₃-LiF-MgF₂-Al₂O₃-Sm₂O₃ electrolysis medium in the temperature range from 905 to 1055℃. The temperature (t) and the addition of Al₂O₃ (W(Al₂O₃)), Sm₂O₃ (W(Sm₂O₃)), and a combination of Al₂O₃ and Sm₂O₃ into the basic fluoride system were examined with respect to their effects on the conductivity (κ) and activation energy. The experimental results showed that the molten electrolyte conductivity increases with increasing temperature (t) and decreases with the addition of Al₂O₃ or Sm₂O₃ or both. We concluded that the optimal operation conditions for Al-Sm intermediate alloy production in the Na₃AlF₆-AlF₃-LiF-MgF₂-Al₂O₃-Sm₂O₃ system are W(Al₂O₃) + W(Sm₂O₃)=3wt%, W(Al₂O₃):W(Sm₂O₃)=7:3, and a temperature of 965 to 995℃, which results in satisfactory conductivity, low fluoride evaporation losses, and low energy consumption.     

Chemical quenching and inhibition of positronium in Cr<Subscript>2</Subscript>O<Subscript>3</Subscript>/Al<Subscript>2</Subscript>O<Subscript>3</Subscript> catalysts

The pore structure of Cr2O3/Al2O3 catalysts and the surface chemical properties of these pores were characterized by positron lifetime and coincidence Doppler broadening (CDB) measurements. Four lifetime components could be resolved from the positron lifetime spectrum, with two long lifetime components and two short lifetime components. The two long lifetimes τ4 and τ3 are attributed to ortho-positronium (o-Ps) annihilation in large pores and microvoids, respectively. With increasing Cr2O3 content, both τ4 and its intensity I4 show sharp decrease, while τ3 and its intensity I3 keep nearly unchanged. The Doppler broadening S parameters also show sharp decrease with increasing Cr2O3 content. Detailed analysis of the CDB spectrum reveals that the parapositronium (p-Ps) intensity also decreases with increasing Cr2O3 content. This indicates that the change of o-Ps lifetime τ4 is due to the chemical quenching by Cr2O3 but not spin-conversion of positronium. The decrease of o-Ps intensity I4 indicates that Cr2O3 also inhibits positronium formation.     

Character and fabrication of Al/Al<Subscript>2</Subscript>O<Subscript>3</Subscript>/Al tunnel junctions for qubit application

The superconductive Josephson junction is the key device for superconducting quantum computation. We have fabricated Al/Al2O3/Al tunnel junctions using a double angle evaporation method based on a suspended shadow mask. The Al2O3 junction barrier has been formed by introducing pure oxygen into the chamber during the fabrication process. We have adjusted exposure conditions by changing either the oxygen pressure or the oxidizing time during the formation of tunnel barriers to control the critical current density Jc and the junction specific resistance Rc. Measurements of the leakage in Al/Al2O3/Al tunnel junctions show that the devices are suitable for qubit applications.     

Synthesis of highly ordered SnO2／Fe2O3 composite nanowire arrays by electrophoretic deposition method

Highly ordered SnO2/Fe2O3 composite nanowire arrays have been synthesized by electrophoretic deposition method. The morphology and chemical composition of SnO2/Fe2O3 composite nanowire arrays are characterized by SEM, TEM, EDX, XPS, and XRD. The results show that the SnO2/Fe2O3 composite nanowires are about 180 nm in width and tens of microns in length, and they are composed of small nanoparticles of tetraganal SnO2 and rhombohedral α-Fe203 with diameters of 10-15nm. The SnO2/Fe2O3 composite nanowires are formed by a series of chemical reactions.     

Effect of Fe<Subscript>2</Subscript>O<Subscript>3</Subscript> on the crystallization behavior of glass-ceramics produced from naturally cooled yellow phosphorus furnace slag

CaO-Al₂O₃-SiO₂ (CAS) glass-ceramics were prepared via a melting method using naturally cooled yellow phosphorus furnace slag as the main raw material. The effects of the addition of Fe₂O₃ on the crystallization behavior and properties of the prepared glass-ceramics were studied by differential thermal analysis, X-ray diffraction, and scanning electron microscopy. The crystallization activation energy was calculated using the modified Johnson-Mehl-Avrami equation. The results show that the intrinsic nucleating agent in the yellow phosphorus furnace slag could effectively promote the crystallization of CAS. The crystallization activation energy first increased and then decreased with increasing amount of added Fe₂O₃. At 4wt% of added Fe₂O₃, the crystallization activation energy reached a maximum of 676.374 kJ·mol-1. The type of the main crystalline phase did not change with the amount of added Fe₂O₃. The primary and secondary crystalline phases were identified as wollastonite (CaSiO₃) and hedenbergite (CaFe(Si₂O₆)), respectively.     

Effects of Yb^3＋ codoping on visible and near infrared emissions of Er^3＋-Yb^3＋ codoped Al2O3 powders by the sol-gel method

The 0.1 mol% Er^3＋ and 0-2 mol% Yb^3＋ codoped Al2O3 powders were prepared by the sol-gel method, and the phase structure, including only two crystalline types of doped Al2O3 phase, γ-（Al,Er, Yb）2O3 and θ-（Al,Er, Yb）2O3, was detected at the sintering temperature of 1000℃. The visible and near infrared emissions properties depended strongly on the Yb^3＋ codoping, and the corresponding maximal peak intensities centered at about 523, 545, 660 and 1533 nm were obtained respectively for the 0.1 mol% Er^3＋ and 0.5 mol% Yb^3＋ codoped Al2O3 powders, which were composed of θ-（Al,Er,Yb）2O3 and a small amount of γ-（Al,Er, Yb）2O3 phases. The two-photon absorption process was responsible for the visible up-conversion emissions, and the one-photon absorption process was involved in the near infrared emissions of the Er^3＋-yb^3＋ codoped Al2O3 powders.     

Reinforcing effect of graphene on the mechanical properties of Al<Subscript>2</Subscript>O<Subscript>3</Subscript>/TiC ceramics

Multilayer graphene (MLG)-reinforced Al₂O₃/TiC ceramics were fabricated through hot pressing sintering, and the reinforcing effect of MLG on the microstructure and mechanical properties of the composites was investigated by experiment and simulation. The simulation of dynamic crack initiation and propagation was investigated based on the cohesive zone method. The results show that the composite added with 0.2wt% MLG has excellent flexural strength and high fracture toughness. The major reinforcing mechanisms are the synergistic effect by strong and weak bonding interfaces, MLG pull-out, and grain refinement resulting from the addition of MLG. In addition, the aggravating of crack deflection, branching, blunting, and bridging have indispensable contribution to the improvement of the as-designed materials.     

Preparation of Al<Subscript>72</Subscript>Ni<Subscript>8</Subscript>Ti<Subscript>8</Subscript>Zr<Subscript>6</Subscript>Nb<Subscript>3</Subscript>Y<Subscript>3</Subscript> amorphous powders and bulk materials

Amorphous Al₇₂Ni₈Ti₈Zr₆Nb₃Y₃ powders were successfully fabricated by mechanical alloying. The microstructure, glass-forming ability, and crystallization behavior of amorphous Al₇₂Ni₈Ti₈Zr₆Nb₃Y₃ powders were investigated by X-ray diffraction (XRD), transmission electron microscopy (TEM), and differential scanning calorimetry (DSC). The isothermal crystallization kinetics was analyzed by the Johnson–Mehl–Avrami equation. In the results, the supercooled liquid region of the amorphous alloy is as high as 81 K, as determined by non-isothermal DSC curves. The activation energy for crystallization is as high as 312.6 kJ·mol?1 obtained by Kissinger and Ozawa analyses. The values of Avrami exponent (n) imply that the crystallization is dominated by interface-controlled three-dimensional growth in the early stage and the end stage and by diffusion-controlled two- or three-dimensional growth in the middle stage. In addition, the amorphous Al₇₂Ni₈Ti₈Zr₆Nb₃Y₃ powders were sintered under 2 GPa at temperatures of 673 K and 723 K. The results show that the Vickers hardness of the compacted powders is as high as Hv 1215.     

<Emphasis Type="Italic">In situ</Emphasis> synthesis of TiC reinforced Cu<Subscript>47</Subscript>Ti<Subscript>34</Subscript>Zr<Subscript>11</Subscript>Ni<Subscript>8</Subscript> bulk metallic glass composites

In situ synthesized TiC particles and β-Ti dendrites reinforced Cu47Ti34Zr11Ni8 bulk metallic glass (BMG) composite ingots were prepared by the suction casting method.The ingots with diameters from 1 up to 4mm were successfully obtained. It was shown that introducing TiC micro-sized particles into the amorphous matrix did not disturb the glass forming ability (GFA) of the matrix,while the yield strength and ductility could be well improved.The phase constitution, microstructure and elements distribution in the composites were studied by OM, XRD, SEM and EDS.It was shown that the in situ synthesized TiC particles acting as heterogeneous nucleation sites promoted the precipitation of β-Ti dendrites, resulting in the formation of the TiC particles and β-Ti dendrites co-reinforced BMG composites. The compressive tests were employed to probe the yield strength and ductility of BMG composites.     

Electro-deoxidation of V<Subscript>2</Subscript>O<Subscript>3</Subscript> in molten CaCl<Subscript>2</Subscript>-NaCl-CaO

The electro-deoxidation of V₂O₃ precursors was studied. Experiments were carried out with a two-terminal electrochemical cell, which was comprised of a molten electrolyte of CaCl₂ and NaCl with additions of CaO, a cathode of compact V₂O₃, and a graphite anode under the potential of 3.0 V at 1173 K. The phase constitution and composition as well as the morphology of the samples were studied by X-ray diffraction (XRD) and scanning electron microscopy (SEM). 3 g of V₂O₃ could be converted to vanadium metal powder within the processing time of 8 h. The kinetic pathway was investigated by analyzing the product phase in samples prepared at different reduction stages. CaO added in the reduction path of V₂O₃ formed the intermediate product CaV₂O₄.     

Bulk Al-Al3Zr composite prepared by mechanical alloying and hot extrusion for high-temperature applications

Bulk Al/Al₃Zr composite was prepared by a combination of mechanical alloying (MA) and hot extrusion processes. Elemental Al and Zr powders were milled for up to 10 h and heat treated at 600℃ for 1 h to form stable Al₃Zr. The prepared Al₃Zr powder was then mixed with the pure Al powder to produce an Al-Al₃Zr composite. The composite powder was finally consolidated by hot extrusion at 550℃. The mechanical properties of consolidated samples were evaluated by hardness and tension tests at room and elevated temperatures. The results show that annealing of the 10-h-milled powder at 600℃ for 1 h led to the formation of a stable Al₃Zr phase. Differential scanning calorimetry (DSC) results confirmed that the formation of Al₃Zr began with the nucleation of a metastable phase, which subsequently transformed to the stable tetragonal Al₃Zr structure. The tension yield strength of the Al-10wt%Al₃Zr composite was determined to be 103 MPa, which is approximately twice that for pure Al (53 MPa). The yield stress of the Al/Al₃Zr composite at 300℃ is just 10% lower than that at room temperature, which demonstrates the strong potential for the prepared composite to be used in high-temperature structural applications.     

Preparation of high emissivity NiCr<Subscript>2</Subscript>O<Subscript>4</Subscript> powders with a spinel structure by spray drying

Spray-drying was used to produce the high emissivity NiCr₂O₄ powders with a spinel structure. Preliminary investigations focused on fabricating the high emissivity powders for infrared radiation coatings and finding the relationship between microstructure and emissivity. The NiCr₂O₄ powders were characterized for composition, microstructure, and infrared emissivity by X-ray diffraction (XRD), scanning electron microscopy (SEM), infrared radiant instrument, and Fourier transform infrared spectra (FT-IR). Thermogravimetry and differential thermal analysis show that the appropriate baking temperature for NiCr₂O₄ powder preparation is about 1200°C. The emissivity measurement and FT-IR spectra show that, because of the special spinel structure, the NiCr₂O₄ powders have a high emissivity about 0.91. Spray-drying is a suitable method to produce the high emissivity ceramic powders.     

Characteristics of Al<Subscript>2</Subscript>O<Subscript>3</Subscript>, MnS,and TiN inclusions in the remelting process of bearing steel

The Al₂O₃, MnS, and TiN inclusions in bearing steel will deteriorate the steel's mechanical properties. Therefore, elucidating detailed characteristics of these inclusions in consumable electrode during the electroslag remelting process is important for achieving a subsequently clean ingot. In this study, a confocal scanning violet laser microscope was used to simulate the remelting process and observe, in real time, the behaviors of inclusions. The obtained images show that, after the temperature exceeded the steel solidus temperature, MnS and TiN inclusions in the specimen began to dissolve. Higher temperatures led to faster dissolution, and the inclusions disappeared before the steel was fully liquid. In the case of an observed Al₂O₃ inclusion, its shape changed from angular to a smooth ellipsoid in the region where the solid and liquid coexisted and it began to dissolve as the temperature continued to increase. This dissolution was driven by the difference in oxygen potential between the inclusion and the liquid steel.