In situ reaction mechanism of MgAlON in Al–Al2O3–MgO composites at 1700°C under flowing N2

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

Novelty phase synthesis mechanism and morphology in resin-bonded Al–Al2O3–TiO2 composites at high temperatures under flowing N2

An Al–AlN core–shell structure is beneficial to the performance of Al–Al2O3 composites. In this paper, the phase evolution and microstructure of Al–Al2O3–TiO2 composites at high temperatures in flowing N2 were investigated after the Al–AlN core–shell structure was created at 853 K for 8 h. The results show that TiO2 can convert Al into Al3Ti(~1685 K), which reduces the content of metal Al and rearranges the structure of the composite. Under N2 conditions, Al3Ti is further transformed into a novelty non-oxide phase, TiCN. The transformation process can be expressed as follows: Al3Ti reacts with C and other carbides(Al4C3 and Al4O4C) to form TiCx(x < 1). As the firing temperature increases, Al3Ti transforms into a liquid phase and produces Ti(g) and TiO(g). Finally, Ti(g) and TiO(g) are nitrided and solid-dissolved into the TiCx crystals to form a TiCN solid solution.

A new synthetic route to MgO–MgAl2O4–ZrO2 highly dispersed composite material through formation of Mg5Al2.4Zr1.7O12 metastable phase: synthesis and physical properties

Mg_5Al_(2.4)Zr_(1.7)O_(12) metastable phase was successfully synthesized from analytical-grade Mg O,α-Al_2O_3,MgAl_2O_4,and ZrO_2 under an N_2 atmosphere.The sintering temperature was varied from 1650 to 1780°C,and the highest amount of Mg_5Al_(2.4)Zr_(1.7)O_(12) appeared in the composite material when the sintering temperature was 1760°C.According to our research of the formation mechanism of Mg_5Al_(2.4)Zr_(1.7)O_(12),the formation and growth of MgAl_2O_4 dominated when the temperature was not higher than 1650°C.When the temperature was higher than 1650°C,MgO and ZrO_2 tended to diffuse into MgAl_2O_4 and the Mg_5Al_(2.4)Zr_(1.7)O_(12) solid solution was formed.When the temperature reached 1760°C,the formation of Mg_5Al_(2.4)Zr_(1.7)O_(12) was completed.The effect of Mg Al_2O_4 spinel crystals was also studied,and their introduction into the composite material promoted the formation and growth of Mg_5Al_(2.4)Zr_(1.7)O_(12).A highly dispersed MgO–Mg Al_2O_4–ZrO_2 composite material was prepared through the decomposition of the Mg_5Al_(2.4)Zr_(1.7)O_(12) metastable phase.The as-prepared composite material showed improved overall physical properties because of the good dispersion of MgO,MgAl_2O_4,and ZrO_2 phases.

Morphology characterization of periclase–hercynite refractories by reaction sintering

A periclase？hercynite brick was prepared via reaction sintering at 1600℃for 6 h in air using magnesia and reaction-sintered hercynite as raw materials. The microstructure development of the periclase-hercynite brick during sintering was investigated using X-ray diffraction, X-ray photoelectron spectroscopy, and scanning electron microscopy in combination with energy-dispersive X-ray spectroscopy. The results show that during sintering, Fe^2＋, Fe^3＋ and Al^3＋ ions in hercynite crystals migrate and react with periclase to form（Mg1-xFex）（Fe2-yAly）O4 spinel with a high Fe/Al ratio. Meanwhile, Mg^2＋ in periclase crystals migrates into hercynite crystals and occupies the oxygen tetrahedron vacancies. This Mg^2＋ migration leads to the formation of（Mg1-uFeu）（Fe2-vAlv）O4 spinel with a lower Fe/Al ratio and results in Al3＋ remaining in hercynite crystals. Cation diffusion between periclase and hercynite crystals promotes the sintering process and results in the formation of a microporous structure.

Formation mechanism of calcium hexaluminate

To investigate the formation mechanism of calcium hexaluminate（CaAl_（12）O_（19）, CA_6）, the analytically pure alumina and calcia used as raw materials were mixed in CaO/Al_2O_3 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 Al_2O_3, a small amount of CA_6 forms at 1300°C, and greater amounts are formed at 1400°C and higher temperatures. The reaction is as follows： CaO ·2Al_2O_3（CA_2） ＋ 4Al_2O_3 → CA_6. The diffusions of Ca^（2＋） in CA_2 towards Al_2O_3 and Al^（3＋） in Al_2O_3 towards CA_2 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 Ca^（2＋） in CA_2 towards Al_2O_3.

Reaction behavior of trace oxygen during combustion of falling FeSi75 powder in a nitrogen flow

To explore the reaction behavior of trace oxygen during the flash combustion process of falling FeSi75 powder in a nitrogen flow, a flash-combustion-synthesized Fe-Si;N;sample was heat-treated to remove SiO;. The samples before and after the treatment were investigated by X-ray diffraction, scanning electron microscopy, and transmission electron microscopy, and the formation mechanism of SiO;was investigated. The results show that SiO;in the Fe-Si;N;is mainly located on the surface or around the Si;N;particles in dense areas, existing in both crystalline and amorphous states; when the FeSi75 particles, which are less than 0.074 mm in size, fell in up-flowing hot N;stream, trace oxygen in the N;stream did not significantly hinder the nitridation of FeSi75 particles as it was consumed by the surface oxidation of the generated Si;N;particles to form SiO;. At the reaction zone, the oxidation of Si;N;particles decreased the oxygen partial pressure in the N;stream and greatly reduced the opportunity for FeSi75 particles to be oxidized into SiO;; by virtue of the SiO;film developed on the surface, the Si;N;particles adhered to each other and formed dense areas in the material.

Morphology of α-Si_3N_4 in Fe–Si_3N_4 prepared via flash combustion

The state and formation mechanism of α-Si3N4 in Fe-Si3N4 prepared by flash combustion were investigated by X-ray diffraction, scanning electron microscopy, and transmission electron microscopy. The results indicate that α-SiaN4 crystals exist only in the Fe-Si3N4 dense areas. When FeSi75 particles react with N2, which generates substantial heat, a large number of Si solid particles evaporate. The product between Si gas and N2 is a mixture of α-Si3N4 and β-Si3N4. At the later stage of the flash combustion process, α-Si3N4 crystals dissolve and reprecipitate as α-Si3N4 and the β-Si3N4 crystals grow outward from the dense areas in the product pool. As the temperature decreases, the α-SiaN4 crystals cool before transforming into β-SiaN4 crystals in the dense areas of Fe-Si3N4. The phase composition of flash-combustion-synthesized Fe-SiaN4 is controllable through manipulation of the gas-phase reaction in the early stage and the α→β transformation in the later stage.