In situ reaction mechanism of MgAlON in Al-Al2O3-MgO composites at 1700℃ under flowing N2

The Al-Al₂O₃-MgO composites with added aluminum contents of approximately 0wt%, 5wt%, and 10wt%, named as M₁, M₂, and M₃, respectively, were prepared at 1700℃ for 5 h under a flowing N₂ atmosphere using the reaction sintering method. After sintering, the Al-Al₂O₃-MgO composites were characterized and analyzed by X-ray diffraction, scanning electron microscopy, and energy-dispersive X-ray spectroscopy. The results show that specimen M₁ was composed of MgO and MgAl₂O₄. Compared with specimen M₁, specimens M₂ and M₃ possessed MgAlON, and its production increased with increasing aluminum addition. Under an N₂ atmosphere, MgO, Al₂O₃, and Al in the matrix of specimens M₂ and M₃ reacted to form MgAlON and AlN-polytypoids, which combined the particles and the matrix together and imparted the Al-Al₂O₃-MgO composites with a dense structure. The mechanism of MgAlON synthesis is described as follows. Under an N₂ atmosphere, the partial pressure of oxygen is quite low; thus, when the Al-Al₂O₃-MgO composites were soaked at 580℃ for an extended period, aluminum metal was transformed into AlN. With increasing temperature, Al₂O₃ diffused into AlN crystal lattices and formed AlN-polytypoids; however, MgO reacted with Al₂O₃ to form MgAl₂O₄. When the temperature was greater than (1640 ±10)℃, AlN diffused into Al₂O₃ and formed spinel-structured AlON. In situ MgAlON was acquired through a solid-solution reaction between AlON and MgAl₂O₄ at high temperatures because of their similar spinel structures.     

Thermodynamic analysis and preparation of β-SiC/ZrO2 composites

A predominance area diagram for the Zr-Si-C-O system at 1773 K was plotted according to correlative thermodynamic data. β-SiC/ZrO₂ composites were prepared based on the phase diagram by carbothermal reduction of zircon (ZrSiO₄) in argon atmosphere. Zircon and carbon black were mixed according to the C/ZrSiO₄ mass ratio of 0.2, and with 0, 1wt% and 2wt% extra addition of La₂O₃. Phase evolution of the mixture was investigated at 1723-1803 K by X-ray powder diffraction, and the microstructure of the product prepared at 1803 K for 4 h was examined by scanning electronic microscope. The results show that the decomposition of ZrSiO₄ and the formation of β-SIC can be promoted by increasing the heating temperature and adding La₂O₃. The β-SiC/ZrO₂ composites can be prepared at 1803 K for 4 h in a mixture of zircon, carbon black and La₂O₃, and the contents of β-SIC and m-ZrO₂ in the product sample with 2wt% La₂O₃ reach the highest values of 10.8wt% and 89.2wt%, respectively. The crystal size of the products is about 200 nm.     

Microstructure and electrolysis behavior of self-healing Cu-Ni-Fe composite inert anodes for aluminum electrowinning

The microstructure evolution and electrolysis behavior of (Cu₅₂Ni₃₀Fe₁₈)-xNiFe₂O₄ (x=40wt%, 50wt%, 60wt%, and 70wt%) composite inert anodes for aluminum electrowinning were studied. NiFe₂O₄ was synthesized by solid-state reaction at 950℃. The dense anode blocks were prepared by ball-milling followed by sintering under a N₂ atmosphere. The phase evolution of the anodes after sintering was determined by scanning electron microscopy and energy-dispersive X-ray spectroscopy. The results indicate that a substitution reaction between Fe in the alloy phase and Ni in the oxide phase occurs during the sintering process. The samples were also examined as inert anodes for aluminum electrowinning in the low-temperature KF-NaF-AlF₃ molten electrolyte for 24 h. The cell voltage during electrolysis and the corrosion scale on the anodes were analyzed. The results confirm that the scale has a self-repairing function because of the synergistic reaction between the alloy phase with Fe added and the oxide phase. The estimated wear rate of the (Cu₅₂Ni₃₀Fe₁₈)-50NiFe₂O₄ composite anode is 2.02 cm·a-1.     

In-situ fabrication of Al(Zn)-Al2O3 graded composite using the aluminothermic reaction during hot pressing

In this study, the fabrication of multilayer Al(Zn)–Al₂O₃ with different volume fractions of Al₂O₃ was investigated. Al and ZnO powders were milled by a planetary ball mill, after which five-layer functionally graded samples were produced through hot pressing at 580℃ and 90 MPa pressure for 30 min. Formation of reinforcing Al₂O₃ particles occurred in the aluminum matrix via the aluminothermic reaction. Determination of the ignition temperature of the aluminothermic reaction was accomplished using differential thermal and thermogravimetric analyses. Scanning electron microscopy, energy dispersive spectroscopy, and X-ray diffractometery analyses were utilized to characterize the specimens. The thermal analysis results showed that the ignition temperatures for the aluminothermic reaction of layers with the highest and lowest ZnO contents were 667 and 670℃, respectively. Microstructural observation and chemical analysis confirmed the fabrication of Al(Zn)–Al₂O₃ functionally graded materials composites with precipitation of additional Zn in the matrix. Moreover, nearly dense functionally graded samples demonstrated minimum and maximum hardness values of HV 75 and HV 130, respectively.     

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.     

Reaction mechanism for in-situ β-SiAlON formation in Fe3Si-Si3N4-Al2O3 composites

In this work, Fe₃Si-Si₃N₄-Al₂O₃ composites were prepared at 1300℃ in an N₂ atmosphere using fused corundum and tabular alumina particles, Al₂O₃ fine powder, and ferrosilicon nitride (Fe₃Si-Si₃N₄) as raw materials and thermosetting phenolic resin as a binder. The effect of ferrosilicon nitride with different concentrations (0wt%, 5wt%, 10wt%, 15wt%, 20wt%, and 25wt%) on the properties of Fe₃Si-Si₃N₄-Al₂O₃ composites was investigated. The results show that the apparent porosity varies between 10.3% and 17.3%, the bulk density varies from 2.94 g/cm3 and 3.30 g/cm3, and the cold crushing strength ranges from 67 MPa to 93 MPa. Under the experimental conditions, ferrosilicon nitride, whose content decreases substantially, is unstable; part of the ferrosilicon nitride is converted into Fe₂C, whereas the remainder is retained, eventually forming the ferrosilicon alloy. Thermodynamic assessment of the Si₅AlON₇ indicated that the ferrosilicon alloy accelerated the reactions between Si₃N₄ and α-Al₂O₃ fine powder and that Si in the ferrosilicon alloy was nitrided directly, forming β-SiAlON simultaneously. In addition, fused corundum did not react directly with Si₃N₄ because of its low reactivity.     

Microstructure and properties of Ag–Ti3SiC2 contact materials prepared by pressureless sintering

Ti₃SiC₂-reinforced Ag-matrix composites are expected to serve as electrical contacts. In this study, the wettability of Ag on a Ti₃SiC₂ substrate was measured by the sessile drop method. The Ag–Ti₃SiC₂ composites were prepared from Ag and Ti₃SiC₂ powder mixtures by pressureless sintering. The effects of compacting pressure (100–800 MPa), sintering temperature (850–950℃), and soaking time (0.5–2 h) on the microstructure and properties of the Ag–Ti₃SiC₂ composites were investigated. The experimental results indicated that Ti₃SiC₂ particulates were uniformly distributed in the Ag matrix, without reactions at the interfaces between the two phases. The prepared Ag–10wt%Ti₃SiC₂ had a relative density of 95% and an electrical resistivity of 2.76×10-3 mΩ·cm when compacted at 800 MPa and sintered at 950℃ for 1 h. The incorporation of Ti₃SiC₂ into Ag was found to improve its hardness without substantially compromising its electrical conductivity; this behavior was attributed to the combination of ceramic and metallic properties of the Ti₃SiC₂ reinforcement, suggesting its potential application in electrical contacts.     

Effect of sintering temperature on the physical properties and electrical contact properties of doped AgSnO<Subscript>2</Subscript> contact materials

AgSnO₂ electrical contact materials doped with Bi₂O₃, La₂O₃, and TiO₂ were successfully fabricated by the powder metallurgy method under different initial sintering temperatures. The electrical conductivity, density, hardness, and contact resistance of the AgSnO₂/Bi₂O₃, AgSnO₂/La₂O₃, and AgSnO₂/TiO₂ contact materials were measured and analyzed. The arc-eroded surface morphologies of the doped AgSnO₂ contact materials were investigated by scanning electron microscopy (SEM). The effects of the initial sintering temperature on the physical properties and electrical contact properties of the doped AgSnO₂ contact materials were discussed. The results indicate that the physical properties can be improved and the contact resistance of the AgSnO₂ contact materials can be substantially reduced when the materials are sintered under their optimal initial sintering temperatures.     

18wt%Cr–8wt%Ni不锈钢中增塑性MnO–Al2O3–SiO2基非金属夹杂物的演变及其浸泡性能

The properties of MnO–Al₂O₃–SiO₂-based plasticized inclusion are likely to change during soaking  process due to its low melting point. In this study, the evolution of the MnO–Al₂O₃–SiO₂-based inclusion of 18wt%Cr?8wt%Ni stainless steel under isothermal soaking process at 1250°C for different times was investigated by laboratory-scale experiments and thermodynamic analysis. The results showed that the inclusion population density increased at the first stage and then decreased while their average size first decreased and then increased. In addition, almost no Cr₂O₃-concentrated regions existed within the inclusion before soaking, but more and more Cr₂O₃ precipitates were formed during soaking. Furthermore, the plasticity of the inclusion deteriorated due to a decrease in the amount of liquid phase and an increase in the high-melting-point-phase MnO–Cr₂O₃ spinel after the soaking process. In-situ observations by high-temperature confocal laser scanning microscopy (CLSM) confirmed that liquid phases were produced in the inclusions and the inclusions grew rather quickly during the soaking process. Both the experimental results and thermodynamic analysis conclude that there are three routes for inclusion evolution during the soaking process. In particular, Ostwald ripening plays an important role in the inclusion evolution, i.e., MnO–Al₂O₃–SiO₂-based inclusions grow by absorbing the newly precipitated smaller-size MnO–Cr₂O₃ inclusions.     

Effect of Al<Subscript>2</Subscript>O<Subscript>3sf</Subscript> addition on the friction and wear properties of (SiC<Subscript>p</Subscript>+Al<Subscript>2</Subscript>O<Subscript>3sf</Subscript>)/Al2024 composites fabricated by pressure infiltration

Aluminum (Al) 2024 matrix composites reinforced with alumina short fibers (Al₂O_3sf) and silicon carbide particles (SiC_p) as wear-resistant materials were prepared by pressure infiltration in this study. Further, the effect of Al₂O_3sf on the friction and wear properties of the as-synthesized composites was systematically investigated, and the relationship between volume fraction and wear mechanism was discussed. The results showed that the addition of Al₂O_3sf, characterized by the ratio of Al₂O_3sf to SiC_p, significantly affected the properties of the composites and resulted in changes in wear mechanisms. When the volume ratio of Al₂O_3sf to SiC_p was increased from 0 to 1, the rate of wear mass loss (K_m) and coefficients of friction (COFs) of the composites decreased, and the wear mechanisms were abrasive wear and furrow wear. When the volume ratio was increased from 1 to 3, the COF decreased continuously; however, the K_m increased rapidly and the wear mechanism became adhesive wear.     

Effect of SiO2 addition on the dielectric properties and microstructure of BaTiO3-based ceramics in reducing sintering

The effect of SiO₂ doping on the sintering behavior, microstructure, and dielectric properties of BaTiO₃-based ceramics has been investigated. Silica was added to the BaTiO₃-based powder prepared by the solid state method with 0.075mol%, 0.15mol%, and 0.3mol%, respectively. The SiO₂-doped BaTiO₃-based ceramic with high density and uniform grain size were obtained, which were sintered in reducing atmosphere. A scanning electron microscope, X-ray diffraction, and LCR meter were used to determine the microstructure as well as the dielectric properties. SiO₂ can form a liquid phase belonging to the ternary system of BaO-TiO₂-SiO₂, leading to the formation of BaTiO₃ ceramics with high density at a lower sintering temperature. The SiO₂-doped BaTiO₃-based ceramics can be sintered to a theoretical density higher than 95% at 1220℃ with a soaking time of 2 h. The dielectric constants of the sample with 0.15mol% SiO₂ addition sintered at 1220℃ is about 9000. Doping with a small amount of silica can improve the sintering and dielectric properties of BaTiO₃-based ceramics.     

Formation mechanism of calcium hexaluminate

To investigate the formation mechanism of calcium hexaluminate (CaAl₁₂O₁₉, CA₆), the analytically pure alumina and calcia used as raw materials were mixed in CaO/Al₂O₃ ratio of 12.57:137.43 by mass. The raw materials were ball-milled and shaped into green specimens, and fired at 1300–1600°C. Then, the phase composition and microstructure evolution of the fired specimen were studied, and a first principle calculation was performed. The results show that in the reaction system of CaO and Al₂O₃, a small amount of CA₆ forms at 1300°C, and greater amounts are formed at 1400°C and higher temperatures. The reaction is as follows: CaO·2Al₂O₃ (CA₂) + 4Al₂O₃ → CA₆. The diffusions of Ca2+ in CA₂ towards Al₂O₃ and Al3+ in Al₂O₃ towards CA₂ change the structures in different degrees of difficulty. Compared with the difficulty of structural change and the corresponding lattice energy change, it is deduced that the main formation mechanism is the diffusion of Ca2+ in CA₂ towards Al₂O₃.     

Fabrication and densification enhancement of SiC-particulate-reinforced copper matrix composites prepared via the sinter-forging process

The fabrication of copper (Cu) and copper matrix silicon carbide (Cu/SiC_p) particulate composites via the sinter-forging process was investigated. Sintering and sinter-forging processes were performed under an inert Ar atmosphere. The influence of sinter-forging time, temperature, and compressive stress on the relative density and hardness of the prepared samples was systematically investigated and subsequently compared with that of the samples prepared by the conventional sintering process. The relative density and hardness of the composites were enhanced when they were prepared by the sinter-forging process. The relative density values of all Cu/SiC_p composite samples were observed to decrease with the increase in SiC content.     

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.     

Fracture behavior and microstructure analysis of Al2O3–MgO–CaO castables for steel-ladle purging plugs

Three different castables based on the Al₂O₃–MgO–CaO system were prepared as steel-ladle purging plug refractories: corundum- based low-cement castable (C-LCC), corundum-spinel-based low-cement castable (C-S-LCC), and corundum-spinel no-cement castable (C-S-NCC) (hydratable alumina (ρ-Al₂O₃) bonded). The fracture behavior at room temperature was tested by the method of “wedge-splitting” on samples pre-fired at different temperatures; the specific fracture energy G′_f and notched tensile strength σ_NT were obtained from these tests. In addition, the Young’s modulus E was measured by the method of resonance frequency of damping analysis (RFDA). The thermal stress resistance parameter R′′′′ calculated using the values of G′_f, σ_NT, and E was used to evaluate the thermal shock resistance of the materials. According to the microstructure analysis results, the sintering effect and the bonding type of the matrix material were different among these three castables, which explains their different fracture behaviors.     

单斜相SrAl2Si2O8陶瓷的烧结及其对Sr的固化

Monoclinic SrAl₂Si₂O₈ ceramics for Sr immobilization were prepared by a liquid-phase sintering method. The sintering temperature, mineral phase composition, microstructure, flexural strength, bulk density, and Sr ion leaching characteristics of the SrAl₂Si₂O₈ ceramics were investigated. A crystalline monoclinic SrAl₂Si₂O₈ phase formed through liquid-phase sintering at 1223 K. The introduction of four flux agents (B₂O₃, CaO·2B₂O₃, SrO·2B₂O₃, and BaO·2B₂O₃) to the SrAl₂Si₂O₈ ceramics not only reduced the densification temperature and decreased the volatilization of Sr during high-temperature sintering but also impacted the mechanical properties of the ceramics. Product consistency tests showed that the leaching concentration of Sr ions in the sample with flux agent B₂O₃ was the lowest, whereas that of Sr ions in the sample with flux agent BaO·2B₂O₃ was the highest. These results show that the leaching concentration of Sr ions depends largely on the amorphous phase in the ceramics. Meanwhile, the formation of mineral analog ceramics containing Sr is an important factor to improve Sr immobilization.     

Rapid Sintering of Alumina in Low Pressure RF Plasma

Three kinds of high-purity Al₂O₃ powders, whose average particle size is 0.1, 0.3 and 3.0 mμ respectively, were used as the starting power, and their compacts were fired in the radio-frequency plasma generated at a pressure of 80 Pa using N, as the working gas.Experimental results show that the 0. 1 and 0.3 mp powder compacts can be sintered to nearly the theoretical density within 60 s and this sintering is almost finished in the heating period. It is concluded that the mechanism of liquid sintering, the electric charge effect of Al₂O₃ powder, and the effect of tempetrature gradient in the compacts can affect simultaneously on the rapid densification of the compacts in the plasma sintering.     

Fabrication of Fe–TiC–Al2O3 composites on the surface of steel using a TiO2–Al–C–Fe combustion reaction induced by gas tungsten arc cladding

The aim of the present study was to fabricate Fe–TiC–Al₂O₃ composites on the surface of medium carbon steel. For this purpose, TiO₂–3C and 3TiO₂–4Al–3C–xFe (0 ≤ x ≤ 4.6 by mole) mixtures were pre-placed on the surface of a medium carbon steel plate. The mixtures and substrate were then melted using a gas tungsten arc cladding process. The results show that the martensite forms in the layer produced by the TiO₂–3C mixture. However, ferrite–Fe₃C–TiC phases are the main phases in the microstructure of the clad layer produced by the 3TiO₂–4Al–3C mixture. The addition of Fe to the TiO₂–4Al–3C reactants with the content from 0 to 20wt% increases the volume fraction of particles, and a composite containing approximately 9vol% TiC and Al₂O₃ particles forms. This composite substantially improves the substrate hardness. The mechanism by which Fe particles enhance the TiC + Al₂O₃ volume fraction in the composite is determined.     

Effect of NaCl on synthesis of ZrB2 by a borothermal reduction reaction of ZrO2

ZrB₂ powders were synthesized via a borothermal reduction reaction of ZrO₂ with the assistance of NaCl under a flowing Ar atmosphere. The optimal temperature and reaction time were 1223 K and 3 h, respectively. Compared with the reactions conducted without the addition of NaCl, those performed with the addition of an appropriate amount of NaCl finished at substantially lower temperatures. However, the addition of too much NaCl suppressed this effect. With the assistance of NaCl, a special morphology of polyhedral ZrB₂ particles covered with ZrB₂ nanosheets was obtained. Moreover, the experimental results revealed that the special morphology was the result of the combined effects of B₂O₃ and NaCl. The formation of the special microstructure is explained on the basis of the "dissolution-recrystallization" mechanism.     

功能梯度Ni?W/Er2O3稀土纳米颗粒复合膜的电沉积

Multi-layered functionally graded (FG) structure Ni?W/Er₂O₃ nanocomposite films were prepared by continuously changing the deposition parameters, in which the Er₂O₃ and W contents varied with thickness. The microstructure and chemical composition of the electrodeposited Ni?W/Er₂O₃ films were determined by scanning electron microscopy (SEM) and energy-dispersive X-ray spectroscopy (EDS). The anti-corrosion and wear properties of the electrodeposition films were investigated by electrochemical measurement and ball-on-disk friction test. The microhardness distribution of the cross section of nanocomposites was measured by nanoindentation. The results showed that with decreasing agitation rate or increasing average current density, the contents of Er₂O₃ nanoparticles and tungsten were distributed in a gradient along the thickness, and the contents on the surface were larger. By comparison, FG Ni?W/Er₂O₃ films had better anti-corrosion and wear properties than the uniform Ni?W/Er₂O₃ films. Atomic force microscopy (AFM) and profilometry measurements indicated that Er₂O₃ nanoparticles had an effect on the surface roughness.