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1.
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
2.
V. M. Sreekumar R. M. Pillai B. C. Pai M. Chakraborty 《Journal of the American Ceramic Society》2007,90(9):2905-2911
An aluminum/MgAl2 O4 in situ metal matrix composite has been synthesized using silica gel containing ∼98% SiO2 in an Al–5Mg alloy. The thermodynamics and kinetics of MgAl2 O4 formation have been discussed in detail. A transition phase of composition between MgO and MgAl2 O4 has been detected in the SEM-EDS analysis of the particles extracted from the composite by a 25% NaOH solution. This confirms the gradual transformation of MgO to MgAl2 O4 by the reaction 3SiO2 ( s )+2MgO( s )+4Al( l )→2MgAl2 O4 ( s )+3Si( l ). The stoichiometry, n , of MgAl2 O4 has been found to sustain close to 1 and the crystallite growth of MgAl2 O4 has been stopped at D ∼30 nm in the composites held at 750°C up to 10 h. 相似文献
3.
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
4.
Daniela Domanski Guillermina Urretavizcaya Facundo J. Castro Fabiana C. Gennari 《Journal of the American Ceramic Society》2004,87(11):2020-2024
MgAl2 O4 spinel was successfully synthesized using a mechanochemical route that avoided the formation and calcination of its precursors at high temperatures. The method involved a single step in which γ-Al2 O3 –MgO, AlO(OH)–MgO, and α-Al2 O3 –MgO mixtures were milled at room temperature under air atmosphere. The formation of MgAl2 O4 occurred faster with γ-Al2 O3 than with AlO(OH) or α-Al2 O3 . After 140 h, the mechanochemical treatment of the γ-Al2 O3 –MgO mixture yielded 99% of MgAl2 O4 . 相似文献
5.
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
6.
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
7.
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
8.
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
9.
Gualtiero Gusmano Giampiero Montesperelli Enrico Traversa Giulia Mattogno 《Journal of the American Ceramic Society》1993,76(3):743-750
Active elements for humidity sensors based upon MgAl2 O4 thin films or sintered pellets were investigated. Thin films were deposited on Si/SiO2 substrates by radiofrequency (rf) sputtering. Sintered MgAl2 O4 pellets were prepared by traditional ceramic processing. Scanning electron microscopy (SEM) analysis showed that the thin films were rather dense and homogeneous, made up of clustered particles of about 20–30 nm, while the pellets showed a wide pore-size distribution. X-ray photoelectron spectroscopy (XPS) demonstrated that the thin films have a stoichiometry close to that of MgAl2 O4 . Sintered MgAl2 O4 is crystalline, while it is disordered in thin-film form. The presence of two different components of the Al 2 p peaks was correlated with the structural difference between pellets and thin films. The relationship between good film–substrate adhesive properties and the chemical composition at the interface was studied. The electrical properties of the sensing elements were studied at 40°C in environments at different relative humidity (RH) values between 2% and 95%, using ac impedance spectroscopy. MgAl2 O4 thin films showed interesting characteristics in terms of their use in humidity-measurement devices. Resistance versus RH sensitivity values showed variations as high as 4 orders of magnitude in the RH range tested for thin films, and 5 orders of magnitude for pellets. The differences in the electrical behavior of MgAl2 O4 pellets and thin films were correlated with their different microstructures. 相似文献
10.
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
11.
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
12.
Formation and Densification Behavior of Magnesium Aluminate Spinel: The Influence of CaO and Moisture in the Precursors 总被引:1,自引:1,他引:0
Ibram Ganesh Kolli Archana Teja Natarajan Thiyagarajan Roy Johnson Benjaram Mahipal Reddy 《Journal of the American Ceramic Society》2005,88(10):2752-2761
Different grades of stoichiometric and non-stoichiometric dense magnesium aluminate spinel (MgAl2 O4 ) grains were prepared by a conventional double-stage firing process using two types of alumina and four types of magnesia raw materials. The MgAl2 O4 spinel formation was found to be highly influenced by CaO and moisture present in the precursor oxides as confirmed by thermogravimetry (TG), differential thermal analysis (DTA), and X-ray diffraction (XRD) techniques. The Fourier transform-infrared spectroscopy (FTIR) study of the precursor oxides revealed the presence of moisture. Influence of alumina and magnesia composition on the densification behavior of MgAl2 O4 spinels was assessed by characterizing bulk density (BD), apparent porosity (AP), water absorption (WA) capacity, and the microstructures of the stoichiometric, the magnesia-rich, and the alumina-rich spinels sintered at 1650°C for 1 h. Sintering studies indicate that to obtain dense stoichiometric spinel grains with >3.35 g/mL BD, <2.0% AP, and <0.5% WA, the spinel powder should possess a median particle size of <2 μm, CaO content of >0.9%, compact (green) density of >1.95 g/mL, and spinel content of >90%. Among various spinels synthesized, the magnesia-rich spinels exhibited superior properties in terms of high BD, low percentage of AP, and low WA capacity, whereas alumina-rich spinels showed inferior properties. Stoichiometric spinels exhibited an average grain size of 10 μm whereas alumina-rich spinels with 90% alumina had an average grain size of 20 μm. The increase in holding time at higher temperatures enhanced the sintering properties of the spinels, particularly the magnesia-rich spinels. Further, raw mixtures having >0.9% CaO exhibited better sintered properties as compared with others. 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.
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
15.
Yoshikazu Suzuki Naoki Kondo Tatsuki Ohji 《Journal of the American Ceramic Society》2003,86(7):1128-1131
Porous CaZrO3 /MgAl2 O4 composites were synthesized in air by pressureless reactive sintering of an equimolar mixture of dolomite (CaMg(CO3 )2 ), monoclinic zirconia ( m -ZrO2 ), and α-alumina powders, with a 0.5 wt% lithium fluoride additive. The reaction behavior of the mixed powders (with/without LiF additive) was studied using high-temperature X-ray diffraction. A bulk porous composite resulted from sintering at 1300°C for 2 h (in a nearly closed container, so as to increase the LiF-doping effect), which consisted of fine grains (CaZrO3 and MgAl2 O4 , ∼0.5–1 μm) and well-grown idiomorphic ones (MgAl2 O4 octahedra ∼ 2–4 μm). The idiomorphic spinel grains were located around the inner walls of relatively large pores. The composite showed appreciably high bending strength (σf = 110 ± 8 MPa for a porosity of 31%). The porous CaZrO3 /MgAl2 O4 composites can be applied as high-temperature filters and lightweight structural components. 相似文献
16.
Shaowei Zhang Daniel Doni Jayaseelan Goutam Bhattacharya William Edward Lee 《Journal of the American Ceramic Society》2006,89(5):1724-1726
MgAl2 O4 (MA) spinel powder was synthesized by heating an equimolar composition of MgO and Al2 O3 in LiCl, KCl, or NaCl. The synthesis temperature can be decreased from >1300°C (required by the conventional solid–solid reaction process) to ∼1100°C in LiCl, or to ∼1150°C in KCl or NaCl. The molten salt synthesized MA powder was pseudomorphic and retained, to a large extent, the size and morphology of the original Al2 O3 raw material, indicating that a "template formation mechanism" plays an important role in the synthesis process. 相似文献
17.
Surface Modification of Sapphire by Magnesium-Ion Implantation 总被引:9,自引:0,他引:9
Jihong Li Steven R. Nutt Kevin W. Kirby 《Journal of the American Ceramic Society》1999,82(11):3260-3262
Single crystals of Al2 O3 were implanted at a temperature of 25°C with magnesium ions that were accelerated at 200 keV and then annealed in oxygen gas for 15 h at 1500°C. The microstructure and composition in the implanted region were examined using analytical electron microscopy techniques, with an emphasis on identification of the microstructural changes that were caused by implantation and annealing. Implantation created a damage zone 0.3 µm thick in the near-surface region of sapphire, and implanted magnesium ions were distributed in this zone without detectable precipitation. Annealing in oxygen gas caused redistribution of the implanted magnesium ions and the formation of a discrete buried layer of spinel (MgAl2 O4 ) that was epitactic with both the substrate and the cap layer. 相似文献
18.
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
19.
Chang Wei Zheng Shu Ya Wu Xiang Ming Chen Kai Xin Song 《Journal of the American Ceramic Society》2007,90(5):1483-1486
MgAl2 O4 microwave dielectric ceramics were modified by Zn substitution for Mg, and their dielectric characteristics were evaluated, along with their structures. Dense (Mg1− x Zn x )Al2 O4 ceramics were obtained by sintering at 1550°–1650°C in air for 3 h, and the (Mg1− x Zn x )Al2 O4 solid solution was determined in the entire composition range. With Zn substitution for Mg, the dielectric constant ɛ of MgAl2 O4 just varied from 7.90 to 8.56, while the Q × f value had significantly improved up to a maximal value of 106 000 GHz at x =1.0. Moreover, the τf of MgAl2 O4 ceramics had declined from −73 to −63 ppm/°C. 相似文献
20.
The electrical conductivities of single crystal and polycrystalline MgAl2 O4 and Y3 Al5 O12 were measured to 1260 K using a three-contact, guard-ring technique. The electrical conduction mechanisms change with temperature, with anomalous oxygen pressure and time-dependent inflections in log σ versus T−1 curves between 900 to 1000 K. The conduction processes of Y3 Al5 O12 and MgAl2 O4 appear to be similar and possibly related to A13+ ion diffusion. 相似文献