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1.
Keith Rozenburg Ivar E. Reimanis Hans-Joachim Kleebe Ron L. Cook 《Journal of the American Ceramic Society》2008,91(2):444-450
The sintering kinetics of a pure magnesium aluminate spinel, MgAl2 O4 , and that doped with LiF were determined through the use of the master sintering curve technique developed by Su and Johnson. 20 Powders with 0%, 0.5%, and 1.0% by mass LiF were densified in a vacuum hot press under a range of unaxial pressures. After the sintering mechanisms in each temperature and pressure regime were determined, an optimized vacuum hot-pressing schedule was formulated for spinel powders doped with 1.0% by mass of LiF. In addition to forming a transient liquid phase, the presence of LiF leads to the formation of oxygen vacancies that promote late-stage sintering in MgAl2 O4 . 相似文献
2.
Antonio H. de Aza Juan E. Iglesias Pilar Pena Salvador De Aza 《Journal of the American Ceramic Society》2000,83(4):919-927
Solid-state compatibility and melting relationships in the subsystem Al2 O3 —MgAl2 O4 —CaAl4 O7 were studied by firing and quenching selected samples located in the isopletal section (CaO·MgO)—Al2 O3 . The samples then were examined using X-ray diffractomtery, optical microscopy, and scanning and transmission electron microscopies with wavelength- and energy-dispersive spectroscopies, respectively. The temperature, composition, and character of the ternary invariant points of the subsystem were established. The existence of two new ternary phases (Ca2 Mg2 Al28 O46 and CaMg2 Al16 O27 ) was confirmed, and the composition, temperature, and peritectic character of their melting points were determined. The isothermal sections at 1650°, 1750°, and 1840°C of this subsystem were plotted, and the solid-solution ranges of CaAl4 O7 , CaAl12 O19 , MgAl2 O4 , Ca2 Mg2 Al28 O46 , and CaMg2 Al16 O27 were determined at various temperatures. The experimental data obtained in this investigation, those reported in Part I of this work, and those found in the literature were used to establish the projection of the liquidus surface of the ternary system Al2 O3 —MgO—CaO. 相似文献
3.
An isothermal section of the ternary system MgO–Al2 O3 -Cr2 O3 was determined at 1700°± 15°C to delineate the stability field for spinel crystalline solutions (cs). Crystalline solutions were found between the pseudobinary joins MgAl2 O4 –Cr2 O3 and MgCr2 O4 -Al2 O3 , and the binary join MgAl2 O4 -MgO. The first two crystalline solutions exhibit cation vacancy models while the latter can probably be designated as a cation interstitial model. Precipitation from spinel cs may proceed directly to an equilibrium phase, (Al1-x Crx )2 O3 , with the corundum structure or through a metastable phase of the probable composition Mg(Al1-x Cr )26 O40 . The composition and temperature limits were defined where the precipitation occurs via metastable monoclinic phases. The coherency of the metastable monoclinic phase with the spinel cs matrix can be understood by considering volume changes with equivalent numbers of oxygens and known crystallographic orientation relations. Electron probe and metallographic microscope investigations showed no preferential grain boundary precipitation. 相似文献
4.
Bertha Alicia Vázquez Ángel Caballero Pilar Pena 《Journal of the American Ceramic Society》2005,88(7):1949-1957
Solid-state compatibility and melting relations of MgAl2 O4 in the quaternary system Al2 O3 –CaO–MgO–SiO2 were studied by firing and quenching selected samples located in the 65 wt% MgAl2 O4 , plane followed by microstructural and energy dispersive X-ray analysis. A projection of the liquidus surface of the primary crystallization volume of MgAl2 O4 was constructed from CaO, SiO2 and exceeding Al2 O3 , not involved in stoichiometric MgAl2 O4 formation; those three amounts were recalculated to 100 wt%. The temperature and character of six invariant points, where four solids co-exist with a liquid phase, were defined. One maximum point was localized and the positions of the isotherms were tentatively established. The effect of CaO, SiO2 , and Al2 O3 impurities on the high temperature behavior of spinel materials was also discussed. 相似文献
5.
Jafar F. Al-Sharab Frederic Cosandey Amit Singhal Ganesh Skandan James Bentley 《Journal of the American Ceramic Society》2006,89(7):2279-2285
Nanostructured MgAl2 O4 spinel was synthesized by a direct conversion process from cubic γ-Al2 O3 . The effect of post-annealing temperature (300°, 500°, and 800°C) on MgAl2 O4 phase formation was investigated using transmission electron microscopy, selected area electron diffraction (SAED), electron energy loss spectroscopy (EELS), and energy-dispersive spectroscopy (EDS). Relative diffraction intensities as well as lattice parameter measurements from SAED revealed that MgAl2 O4 spinel structure starts forming at temperatures as low as 300°C. EELS and EDS spectrum images also revealed an increase in elemental homogeneity with increasing annealing temperature. The degree of ordering of Mg and Al between octahedral and tetrahedral sites has been determined from relative diffraction intensities. Results show that annealing to 800°C leads to a spinel phase with an order parameter of 0.78. 相似文献
6.
J. J. COMER N. C. TOMBS J. F. FITZGERALD 《Journal of the American Ceramic Society》1966,49(5):237-240
Single-crystal and polycrystalline films of Mg-Al2 O4 and MgFe2 O4 were formed by two methods on cleavage surfaces of MgO single crystals. In one procedure, aluminum was deposited on MgO by vacuum evaporation. Subsequent heating in air at about 510°C formed a polycrystalline γ-Al2 O8 film. Above 540°C, the γ-Al2 O, and MgO reacted to form a single-crystal MgAl2 O4 film with {001} MgAl2 O4 ‖{001} MgO. Above 590°C, an additional layer of MgAl2 O4 , which is polycrystalline, formed between the γ-Al2 O3 and the single-crystal spinel. Polycrystalline Mg-Al2 O4 formed only when diffusion of Mg2+ ions proceeded into the polycrystalline γ-Al2 O3 region. Corresponding results were obtained for Mg-Fe2 O4 . MgAl2 O4 films were also formed on cleaved MgO single-crystal substrates by direct evaporation, using an Al2 O3 crucible as a source. Very slow deposition rates were used with source temperatures of ∼1350°C and substrate temperatures of ∼800°C. Departures from single-crystal character in the films may arise through temperature gradients in the substrate. 相似文献
7.
ALEXANDRA NAVROTSKY BARRY A. WECHSLER KAREN GEISINGER FRIEDRICH SEIFERT 《Journal of the American Ceramic Society》1986,69(5):418-422
Solution calorimetry of MgAl2 O4 -Al8/3 O4 solid solutions was performed in a molten 2PbO · B2 O3 solvent at 975 K. The results indicate small negative heats of mixing, relative to spinel standard states for both end-members. These data were combined with information on the energetics of the α-γ transition in Al2 O3 and on the MgAl2 O4 -Al8/3 O4 (MgO-Al2 O3 ) subsolidus phase relations to estimate the partial molar entropy of mixing of γ-Al8/3 O4 in the solid solution. This entropy is much less positive than that calculated from several models for the configurational entropy of mixing of magnesium, aluminum, and vacancies on octahedral and/or tetrahedral sites. The data suggest a good deal of local order to be present in the solid solutions, consistent with negative enthalpies of mixing and entropies of mixing far less than ideal configurational values. 相似文献
8.
Koji Morita Keijiro Hiraga Yoshio Sakka 《Journal of the American Ceramic Society》2002,85(7):1900-1902
High-strain-rate superplasticity is attained in a 3-mol%-Y2 O3 -stabilized tetragonal ZrO2 polycrystal (3Y-TZP) dispersed with 30 vol% MgAl2 O4 spinel: tensile elongation at 1823 K reached >300% at strain rates of 1.7 × 10−2 – 3.3 × 10−1 s−1 . The flow behavior and the microstructure of this material indicate that the MgAl2 O4 dispersion should enhance accommodation processes necessary for grain boundary sliding. Such an effect is assumed to arise from an enhancement of the cation diffusion by the dissolution of Al and Mg ions into the ZrO2 matrix and from stress relaxation due to the dispersed MgAl2 O4 grains. 相似文献
9.
The subsolidus phase equilibrium diagram for the pseudobinary join MgAl2 O4 -Ga2 O3 was determined. The shape of the exsolution boundary was obtained by heat-treating samples pre- equilibrated at 1600°C. Crystalline solubility of Ga2 O3 in MgAl2 O4 decreased from 73 mole % at 1600°C to 55 mole % at 1200°C. The crystalline solution was formed by the replacement of Mg2+ ions by Ga3+ ions to produce a cation defect spinel. The phase precipitated was the mono-clinic δ-Ga2 O3 (=δ-Al2 O3 structure). Changes in the ratios of relative X-ray diffraction intensities indicated that the crystalline solutions also disorder with temperature. 相似文献
10.
K. Thomas Jacob Kampurath P. Jayadevan Yoshio Waseda 《Journal of the American Ceramic Society》1998,81(1):209-212
The standard Gibbs energy of formation of the spinel MgAl2 O4 from component oxides, MgO and α-Al2 O3 , has been determined in the temperature range 900 to 1250 K using a solid-state cell incorporating single-crystal CaF2 as the solid electrolyte. The cell can be represented as—Pt,O2 ,MgO+MgF2 |CaF2 |MgF2 +MgAl2 O4 +α-Al2 O3 ,O2 ,Pt—The standard Gibbs energy of formation from binary oxides, computed from the reversible emf, can be represented by the expression—capdelta G °f,ox =−23600 − 5.91 T (±150) J/mol—The 'second-law' enthalpy of formation of MgAl2 O4 obtained in this study is in good agreement with high-temperature solution calorimetric studies reported in the literature. 相似文献
11.
Magnesium aluminate (MgAl2 O4 ) spinel powders of irregular and spherical morphologies were obtained from the bi-component water-based sols following the sol–gel and sol–emulsion–gel methods, respectively. For the synthesis of the oxide microspheres, the surfactant concentration and viscosity of the sols were found to affect the characteristics of the derived microspheres. The gel and calcined powders were investigated by using thermogravimetry analysis, differential thermal analysis, X-ray diffraction (XRD), optical and scanning electron microscopy (SEM), Fourier transformed infrared spectroscopy, and particle size analysis. XRD results indicated crystallization of the only phase MgAl2 O4 spinel from 200° to 1000°C. Formation of hollow microspheres with a single cavity was identified by SEM. 相似文献
12.
Ko Ikeda Yoshinori Nakamura Kiyoshi Masumoto Hiromi Shima 《Journal of the American Ceramic Society》1997,80(10):2672-2676
Unpolarized optical spectra were measured in the wavelength range 322–1666 nm by the diffuse reflection technique from spinel powders synthesized in the system MgAl2 O4 –MgCr2 O4 . The spectra were interpreted by the crystal-field theory on the basis of trigonally distorted spinel octahedra with D3d symmetry. For chromium-rich solid solutions, including the MgCr2 O4 end-member, results after peak fittings showed octahedral D3d local symmetry around Cr3+ ions, identical to the crystallographic site symmetry. For chromium-poor solid solutions, however, octahedral C3v local symmetry was suggested around Cr3+ ions, different from the D3d crystallographically expected. 相似文献
13.
Chuei-Tang Wang Lang-Sheng Lin Sheng-Jenn Yang 《Journal of the American Ceramic Society》1992,75(8):2240-2243
High-sinterability MgAl2 O4 powder has been produced from alkoxide precursors via a freeze-drying method. Clear alumina sol and magnesium methoxide were used as starting materials in the process. The spinel powders were characterized by various techniques, such as thermal analysis, X-ray diffraction, scanning electron microscopy, and transmission electron microscopy. The tap density and sinterability of the spinel power are affected by the ball-milling techniques. Highly dense, transparent, polycrystalline MgAl2 O4 has been obtained from these powders by sintering and hot isostatic pressing. Bimodal grain-size microstructure is observed in a HIPed sample. 相似文献
14.
Teresa Durán Sara Serena Pilar Pena Ángel Caballero Salvador De Aza Antonio H. De Aza 《Journal of the American Ceramic Society》2008,91(2):535-543
The isoplethal sections CaAl2 O4 –MgO and CaAl4 O7 –MgO of the Al2 O3 –MgO–CaO ternary system have been experimentally established at 1 bar total pressure and air of normal humidity. The sections obtained provide new data and information that are in disagreement with thermodynamic evaluations and optimizations of the Al2 O3 –MgO–CaO ternary system published to date. These differences arise mainly from the inclusion, or exclusion, of the binary compound Ca12 Al14 O33 , mayenite, as a stable phase in the reported studies of the system. The presence or absence of this compound within the system has an important impact on the solid state and melting relationships of the whole ternary system. The present study confirms the solid-state compatibility CaAl2 O4 –MgO and CaAl2 O4 –MgO–MgAl2 O4 up to 1372°± 2°C, the peritectic melting point of the later mentioned subsystem. 相似文献
15.
Nanocrystalline MgAl2 O4 spinel powder was synthesized by pyrolysis of complex compounds of aluminum and magnesium with triethanolamine (TEA). The soluble metal ion–TEA complexes formed the precursor material on complete dehydration of the complexes of aluminum–TEA and magnesium–TEA. Single-phase MgAl2 O4 spinel powder resulted after heat treatment of the precursor material at 675°C. The precursor and the heat-treated powders were characterized by X-ray diffractometry (XRD), differential thermal and thermogravimetric analysis, and transmission electron microscopy (TEM). The average crystallite size as measured from the X-ray line broadening was around 14 nm and the average particle size from TEM studies was around 20 nm. 相似文献
16.
A MgAl2 O4 (MA) spinel layer was synthesized on Ti3 AlC2 substrate through the molten salt synthesis (MSS) method. The Ti3 AlC2 substrate was immersed in MgCl2 ·6H2 O powders and treated at 800°, 850°, and 900°C for 4 h in air. A continuous and 10-μm-thick MgAl2 O4 layer was obtained at 900°C, by which the surface hardness of Ti3 AlC2 can be effectively improved. The combined scanning electron microscopy observations and crystal morphology simulation further revealed that the as-formed MgAl2 O4 presents tetragonal bipyramids morphology with (400)-orientation. 相似文献
17.
B. D. ROITER 《Journal of the American Ceramic Society》1964,47(10):509-511
Phase relations in the spinel region of the system FeO-Fe2 O3 -Al2 O3 were determined in CO2 at 1300°, 1400°, and 15000°C and for partial oxygen pressures of 4 × 10−7 and 7 × 10−10 atmospheres at 15OO°C. The spinel field extends continuously from Fe3 O4-x to FeAl2 O4+z . 相似文献
18.
MgAl2 O4 spinel precursor was prepared using a heterogeneous sol–gel process. The effect of high-energy milling on the precursor decomposition and spinel formation was investigated. The milling decreased the Al(OH)3 dehydroxylation temperature from 190° to about 130°C. The activation energy for spinel formation decreased from 688 kJ/mol for the as-prepared precursors to 468 kJ/mol for the precursors milled for 5 h. Milling of the precursor lowered the incipient temperature of spinel formation from 900° to 800°C, and the temperature of complete MgAl2 O4 spinel formation from >1280° to ∼900°C. 相似文献
19.
Microhardness anisotropy profiles for the (100) and (111) planes of single-crystal stoichiometric MgAl2 O., spinel were determined at room temperaturé. The (100) microhardness profile has ahardness maximum in tiie [001] and a minimum in the [O11], which supports the previous suggestion that the primary slip system is the {111}〈11¯0〉. The microhardness of the (111) plane is independent of indenter orientation, also consistent, with a {111}〈11¯0〉 primary slip system. It is concluded that these microhardness profiles are in accord with other experimental observations that the {111}〈11¯0〉 is the primary slip system in stoichiometric MgAl2 O4 spinel. 相似文献
20.
Phase relations in air at 1300°C were determined for the system MgO-Cr2 O3 −Fe2 O3 by conventional quenching techniques. Details of the phase equilibria were established for: (1) the sesquioxide solid solution between Cr2 O3 and Fe2 O3 , (2) the spinel solid solution field between MgCr2 O4 and MgFe2 O4 , and (3) the periclase solid solution field for MgO. Selected tie lines connecting coexisting compositions were established with X-ray diffractometer data. Diffuse reflectance spectra, diffractometer intensity ratios, and lattice parameter measurements were obtained for quenched samples to study the structural inversion in the spinel series MgCr2 O4-MgFe2 O4 . 相似文献