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1.
The thermal decomposition of ammonium metavanadate supported on aluminium oxide was investigated using DTA, TG and X-ray diffraction techniques.The results obtained revealed that ammonium vanadate decomposed at 225–250°C giving an intermediate compound ((NH4)2V6O16) which decomposed readily at 335–360°C producing V2O5. Alumina was found to chance the formation of the intermediate compound and retard its decomposition. Some of the V5+ ions of V2O5 lattice seemed to be reduced into V4+ and V3+ ions by heating in air at 450°C in the presence of Al2O3. Such a reaction was attributed to dissolution of some Al3+ ions in the V2O5 lattice via location in interstitial positions and/or in cationic vacancies. Al2O3 was found to interact with V2O5 at 650° C giving well-crystalline A1VO4 which decomposed at about 750°C forming well-crystalline δ-Al2O3 and V2O5,. Pure Al2O3, heated in air at 1000°C, existed in the form of the κ-phase which, on mixing with V2O5 (0.5 V2O5:1 Al2O3) and heating in air at 1000°C, was converted entirely to the well-crystalline α-Al2O3 phase.  相似文献   

2.
A V2O5/Al2O3 mixed solids sample was prepared with a molar ratio of 0.41 Na2O (4 and 10 mol%) was added in the form of sodium nitrate prior to calcination in air in the temperature range 500–1000C. Solid-solid interactions between V2O5 and Al2O3 were studied using DTA and TG curves and their derivatives together with XRD techniques.The results obtained showed that Na2O interacted with V2O5 at temperatures starting from 500C to yield a sodium/vanadium compound, Na0.3V2O5 which remained stable and decomposed in part by heating at 1000C. V2O5 exists in orthorhombic and monoclinic forms in the case of pure mixed solids and those containing 4 mol% of Na2O and preheated at 500C, and in monoclinic form in the case of the mixed solid doped with 10 mol% of Na2O.Heating of pure and doped mixed oxide solids at 650C resulted in the conversion of most of the V2O5 into AlVO4. Doping with sodium oxide enhanced the solid-solid interaction between V2O5 and Al2O3 at 650C to produce AlVO4. The produced AlVO4 decomposed completely on heating at 700C to form -Al2O3 and V2O5, (orthorhombic and monoclinic forms).The presence of Na2O was found to decrease the relative intensity of the diffraction lines of -Al2O3 (corundum) produced at 750C which indicated some kind of hindrance of the crystallization process.Heating of pure and doped mixed solids at 1000C resulted in a further crystallization of acorundum together with V2O5 and sodium vanadate, Na0.3V2O5. However, the intensities of diffraction lines relative to those of the sodium vanadium compound were found to decrease markedly by heating at 1000C, indicating partial thermal decomposition into vanadium and aluminium oxides.  相似文献   

3.
The thermal decompositions of pure and mixed manganese carbonate and ammonium molybdate tetrahydrate in molar ratios of 3:1, 1:1 and1:3 were studied by DTA and TG techniques. The prepared mixed solid samples were calcined in air at 500, 750 or 1000°C and then investigated by means of an XRD technique. The results revealed that manganese carbonate decomposed in the range 300–1000°C, within termediate formation of MnO2, Mn2O3 andMn3O4. Ammonium molybdate tetrahydrate first lost its water of crystallization on heating, and then decomposed, yielding water and ammonia. At 340°C,MoO3 was the final product, which melts at 790°C. The thermal treatment of the mixed solids at 500, 750 or 1000°C led to solid-solid interactions between the produced oxides, with the formation of manganese molybdate. At 1000°C, Mn2O3 and MoO3 were detected, due to the mutual stabilization effect of these oxides at this temperature. This revised version was published online in July 2006 with corrections to the Cover Date.  相似文献   

4.
The solid-solid interactions between manganese and magnesium oxides in absence and in presence of small amounts of Li2O have been investigated. The molar ratios between manganese and magnesium oxides in the form of Mn2O3 and MgO were varied between 0.05:1 to 0.5:1. The mixed solids were calcined in air at 400-1000°C. The techniques employed were DTA, XRD and H2O2 decomposition at 20-40°C.The results obtained revealed that solid-solid interactions took place between the reacting solids at 600-1000°C yielding magnesium manganates (Mg2MnO4, Mg6MnO8, MgMnO4 besides unreacted portions of MgO, Mn2O3 and Mn3O4). Li2O-doping (0.75-6 mol%) of the investigated system followed by calcination at 600 and 800°C decreased progressively the intensity of the diffraction lines of Mn2O3 (Bixbyite) with subsequent increase in the lattice parameter 'a' of MgO to an extent proportional to the amount of Li2O added. This finding might suggest that the doping process enhanced the dissolution of Mn2O3 in MgO forming solid solution. This treatment led also to the formation of Li2MnO3. Furthermore, the doping with 3 and 6 mol% Li2O conducted at 800°C resulted in the conversion of Mn2O3 into Mn3O4, a process that took place at 1000°C in absence of Li2O. The produced Li2MnO3 phase remained stable by heating at up to 1000°C. Furthermore, Li2O doping of the investigated system at 400-1000°C resulted in a progressive measurable increase in the particle size of MgO.The catalytic activity measurements showed that the increase in the molar ratio of Mn2O3 in the samples precalcined at 400-800°C was accompanied by a significant increase in the catalytic activity of the treated solids. The maximum increase in the catalytic activity expressed as reaction rate constant measured at 20°C (k 20°C) attained 3.14, 2.67 and 3.25-fold for the solids precalcined at 400, 600 and 800°C, respectively. Li2O-doping of the samples having the formula 0.1 Mn2O3/MgO conducted at 400-600°C brought a progressive significant increase in its catalytic activity. The maximum increase in the value of k 20°C due to Li2O attained 1.93 and 2.75-fold for the samples preheated at 400 and 600°C, respectively and opposite effect was found for the doped samples preheated at 800°C.This revised version was published online in November 2005 with corrections to the Cover Date.  相似文献   

5.
The effects of doping with CeO2 and calcination temperature on the physicochemical properties of the NiO/Al2O3 system have been investigated using DTA, XRD, nitrogen adsorption measurements at −196°C and decomposition of H2O2 at 30–50°C. The pure and variously doped solids were subjected to heat treatment at 300, 400, 700, 900 and 1000°C. The results revealed that the specific surface areas increased with increasing calcination temperature from 300 to 400°C and with doping of the system with CeO2. The pure and variously doped solids calcined at 300 and 400°C consisted of poorly crystalline NiO dispersed on γ-Al2O3. Heating at 700°C resulted in formation of well crystalline NiO and γ-Al2O3 phases beside CeO2 for the doped solids. Crystalline NiAl2O4 phase was formed starting from 900°C. The degree of crystallinity of NiAl2O4 increased with increasing the calcination temperature from 900 to 1000°C. An opposite effect was observed upon doping with CeO2. The NiO/Al2O3 system calcined at 300 and 400°C has catalytic activity higher than individual NiO obtained at the same calcination temperatures. The catalytic activity of NiO/Al2O3 system increased, progressively, with increasing the amount of CeO2 dopant and decreased with increasing the calcination temperature.  相似文献   

6.
Mn/Fe mixed oxide solids doped with Al2O3 (0.32-1.27 wt.%) were prepared by impregnation of manganese nitrate with finely powdered ferric oxide, then treated with different amounts of aluminum nitrate. The obtained samples were calcined in air at 700-1000 °C for 6 h. The specific surface area (SBET) and the catalytic activity of pure and doped precalcined at 700-1000 °C have been measured by using N2 adsorption isotherms and CO oxidation by O2. The structure and the phase changes were characterized by DTA and XRD techniques. The obtained results revealed that Mn2O3 interacted readily with Fe2O3 to produce well-crystallized manganese ferrite (MnFe2O4) at temperatures of 800 °C and above. The degree of propagation of this reaction increased by Al2O3-doping and also by increasing the heating temperature. The treatment with 1.27 wt.% Al2O3 followed by heating at 1000 °C resulted in complete conversion of Mn/Fe oxides into the corresponding ferrite phase. The catalytic activity and SBET of pure and doped solids were found to decrease, by increasing both the calcination temperature and the amount of Al2O3 added, due to the enhanced formation of MnFe2O4 phase which is less reactive than the free oxides (Mn2O3 and Fe2O3). The activation energy of formation (ΔE) of MnFe2O4 was determined for pure and doped solids. The promotion effect of aluminum in formation of MnFe2O4 was attributed to an effective increase in the mobility of reacting cations.  相似文献   

7.
Various nickel aluminium mixed hydroxide samples of different compositions were prepared by co-precipitation from their nitrate solutions using dilute NH4OH. Additional samples were prepared by impregnation of hydrated Al2O3, preheated at 600 and 900°C, with nickel nitrate solution in an equimolar ratio. The thermal decomposition of different mixed solids was studied using DTA. The X-ray investigation of thermal products of the mixed solids was also studied.The results obtained revealed that the presence of NiO up to 33.3 mole % with aluminium oxide much enhanced the degree of crystallinity of the γ-Al2O3 phase. In contrast, the presence of Al2O3 much retarded the crystallization process of the NiO phase. With the exception of samples containing 20 mole% NiO, all the mixed hydroxide samples, when heated in air at 900°C, led to the formation of well-crystalline Ni Al2O4 spinel, alone, or together with either NiO or γ-Al2O3, depending on the composition of the mixed oxide samples. The solid containing 20% NiO and heated at 900°C was constituted of amorphous NiO dispersed in γ-Al2O3. Heating the nickel nitrate-impregnated Al2O3 in air at 800–1000°C led to the formation of Ni Al2O4 together with non-reacted NiO and γ-Al2O3. The degree of crystallinity of the spinel was found to increase by increasing the calcination temperature of the impregnated solids from 800 to 1000°C and by increasing the preheating temperature of the hydrated Al2O3 employed from 600 to 900°C.  相似文献   

8.
The thermal decomposition of the only known antimony nitrate antimony(III) oxide hydroxide nitrate Sb4O4(OH)2(NO3)2, whose synthesis routes were reviewed and optimized was followed by TG-DTA under an argon flow, from room temperature up to 750°C. Chemical analysis (for hydrogen and nitrogen) performed on samples treated at different temperatures showed that an amorphous oxide hydroxide nitrate appeared first at 175°C, and decomposed into an amorphous oxide nitrate above 500°C. Above 700°C, Sb6O13 and traces of -Sb2O4 crystallized.Author to whom all correspondence should be addressed  相似文献   

9.
The thermal reactivities of MgV6O16.9H2O, Mg(HV6O16)2.17H2O and their anhydrous forms were studied within the temperature range 20–1000°C. Both hydrates are thermally unstable. After dehydration, they decompose to V2O5 and Mg(VO3)2. The mixture of decomposition products of MgV6O16.9H2O is stable. After decomposition of the second compound, additional reactions take place above 750°C.
Zusammenfassung Innerhalb des Temperaturbereiches 20–1000° wurde die thermische Reaktivität von MgV6O16.9H2O, Mg(HV6O16)2.17H2O sowie deren wasserfreier Formen untersucht. Beide Verbindungen sind wärmaunbeständig. Nach der Dehydratation zerfallen sie in V2O5 und Mg(VO3)2. Das Gemisch der Zersetzungsprodukte von MgV6O16.9H2O is beständig. Nach der Zersetzung der zweiten Verbindung treten oberhalb 750° weitere Reaktionen auf.
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10.
The orientation, surface and optical properties of sol-gel derived Y2O3 films have been investigated. Transparent Y2O3 films were prepared on quartz glass substrates by sol-gel processes using YCl3·6H2O as a starting material. The water droplet contact angles of the films reached constant values between 79° and 90° after the films were left for 8 to 10 days in air at ambient temperature, indicating that the film surface exhibited hydrophobicity. When 2-(2-methoxyethoxy)ethanol (MEE) was added to the sol, yttria in the films crystallized to a strongly oriented cubic phase at firing temperatures between 400°C and 500°C. The intensity of the XRD peaks increased as the firing temperature was increased to 900°C. However, yttria crystallized to a non-oriented cubic phase when MEE was not used. The refractive index and packing density of the Y2O3 films increased from 1.55 to 1.68 and from 0.67 to 0.79, respectively, as the firing temperature was raised from 400°C to 900°C, indicating that sol-gel derived Y2O3 films are lower in density than evaporated ones.  相似文献   

11.
The effect of ferric and manganese oxides dopants on thermal and physicochemical properties of Mn-oxide/Al2O3 and Fe2O3/Al2O3 systems has been studied separately. The pure and doped mixed solids were thermally treated at 400–1000°C. Pyrolysis of pure and doped mixed solids was investigated via thermal analysis (TG-DTG) techniques. The thermal products were characterized using XRD-analysis. The results revealed that pure ferric nitrate decomposes into Fe2O3 at 350°C and shows thermal stability up to1000°C. Crystalline Fe3O4 and Mn3O4phases were detected for some doped solids precalcined at 1000°C. Crystalline γ-Al2O3 phase was detected for all solids preheated up to 800°C. Ferric and manganese oxides enhanced the formation of α-Al2O3 phase at1000°C. Crystalline MnAl2O4 and MnFe2O4 phases were formed at 1000°C as a result of solid–solid interaction processes. The catalytic behavior of the thermal products was tested using the decomposition of H2O2 reaction. This revised version was published online in August 2006 with corrections to the Cover Date.  相似文献   

12.
The phase generation in the Lu(Gd)–Ti–O systems is studied at 20–1000° using a co-precipitation method. During a thermal treatment of co-precipitation products after a sublimation dehydration, for a composition with the Lu : Ti cation ratio of 1 : 1, an Lu2Ti2O7 phase with a fluorite structure forms at 650°. At 730–750°C the phase undergoes a fluorite pyrochlore transition. Above 750°C its structure is that of disordered pyrochlore, in which antistructural defects occur in Lu and Ti positions (up to 18%). Above 900°C the structure of pyrochlore becomes ordered, and the number of defects in Lu and Ti positions decreases, which affects the temperature dependence of permittivity of Lu2Ti2O7. In Gd–Ti–O system, Gd2Ti2O7 is crystallized, which has a pyrochlore structure only at 740–900°. Electroconductivity and permittivity of Lu2Ti2O7 and Gd2Ti2O7 are measured.  相似文献   

13.
Summary Reactions taking place in the systems graphite—boron carbide—a third component in the controlled temperature range of 1000–2000° C have been investigated by the spectrochemical and X-ray diffraction methods. It has been found that boron evaporates at 1200° C when NaF or LiF were added, at 1600° C when ZnF2 was added and at 1900° C when CaF2 was added as a third component.In the boron carbide-graphite-magnesium oxide system, magnesium borate, Mg3(BO3)2, was found to be formed at high temperatures. A new phase, aluminium borate, 9 Al2O3·2 B2O3, was also found with addition of aluminium trioxide as the third component. Vanadium pentoxide added forms vanadium boride, VB2. In the graphite—boron carbide—silicon dioxide system several phases are found but not identified. With calcium fluoride as the third component no changes occured up to 1900° C, while at 2000° C there is a hardly visible formation of calcium hexaboride. In the case of sodium fluoride new phases are sometimes found, but not identified.
Hochtemperaturreaktionen in spektralanalytisch wichtigen Systemen1. Reaktionen in den Systemen von Graphit und Borcarbid mit einer dritten Komponente
Zusammenfassung Die Reaktionen wurden im Bereich von 1000–2000° C durch Spektralanalyse und Röntgendiffraktometrie untersucht. Dabei wurde gefunden, daß Bor bei 1200° C verdampft, wenn NaF oder LiF zugesetzt werden, bei 1600° C bei Zugabe von ZnF2 und bei 1900° C bei Zusatz von CaF2. Im System Borcarbid-Graphit-MgO wurde bei hohen Temperaturen Mg3(B03)2 gebildet. Bei Gemischen mit Al2O3 wurde 9 Al2O3·2 B2O3 gefunden. Bei Zusatz von V2O5 wurde VB2 gebildet. Mehrere Phasen, die aber nicht identifiziert wurden, konnten im System Graphit—Borcarbid—SiO2 gefunden werden. Mit CaF2 wurden bis 1900° C keine Veränderungen beobachtet, während bei 2000° C CaB6 in geringen Mengen auftritt. Im Falle von NaF treten gelegentlich neue Phasen auf, die jedoch nicht identifiziert wurden.
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14.
The effect of γ-irradiation on surface and catalytic properties of CuO/Al2O3, NiO/Al2O3 and Fe2O3/Al2O3 was investigated. The techniques employed were XRD, nitrogen adsorption at −196 °C and catalytic conversion of ethanol and isopropanol at 250–400 °C using micropulse technique. The results showed that the supported solids being calcined at 400 °C consisted of well crystallized CuO, NiO, Fe2O3 and AlOOH phases. The AlOOH crystallized into a poorly crystalline γ-Al2O3 upon heating at 600 °C. All phases present in different solids calcined at 400 and 600 °C showed that these solids are of nanocrystalline nature measuring an average crystallite size between 6 and 85 nm. The crystallite size of crystalline phases present was found to be much affected by the dose of γ-rays and the nature of the metal oxide. This treatment resulted in a progressive increase in the specific surface area reaching to a maximum limit at a dose of 0.8 MGy. The dose of 1.6 MGy exerted a measurable decrease in the S BET. A radiation dose of 0.2 to 0.8 MGy brought about a progressive significant decrease in the catalytic activity of all the catalytic systems investigated. All the catalytic systems retained their high activity upon exposure to a dose of 1.6 MGy. The rise in precalcination temperature of the systems investigated from 400 to 600 °C brought about a measurable increase in their catalytic activity in the conversion of alcohols.  相似文献   

15.
The crystallization processes in the synthesis of composite glass-ceramics in the systems fluorapatite (FA)-MgO·SiO2 gel-glass (GG) and FA-MgO·Al2O3·SiO2 (GG) have been studied. The composites were prepared by mixing of MgO·SiO2 and MgO·Al2O3·2SiO2 gel-glasses with FA (from 20 mol% to 80 mol%). The obtained samples were thermally treated at 950°C, 1050°C, 1150°C and 1250°C for 2 hours and the structural changes were investigated, applying XRD-analysis, IR-spectroscopy, Raman spectroscopy and SEM. It has been proved that depending on the chemical composition of the gel-glass and the temperature of treatment, composite glass-ceramics may be prepared consisting only FA, FA and a silicate phase or FA, other phosphate phases and a silicate phase. Because of the absence of calcium or aluminum ions in the composition of the GG, FA is easily decomposed and phases as 7CaO·2MgO·3P2O5 and MgO·2P2O5 are formed.  相似文献   

16.
Summary Reactions between graphite and magnesium, silicon, vanadium and aluminium oxides in graphite electrodes have been investigated by spectrochemical and X-ray diffraction methods. Samples were ignited by means of an evaporator up to controlled temperatures. In the range of 1000–1900°C magnesium oxide does not react with graphite. Aluminium trioxide first forms -Al2O3 and at 1900°C Al4C3. Silicon dioxide forms silicon carbide at about 1400°C. Vanadium pentoxide is first reduced to VO2 and than at higher temperatures (1200° C) forms -VC. At about 1400° C MgO and SiO2 mixed with graphite powder form magnesium silicate, Mg2SiO4, and this silicate was stable at higher temperatures (up to 2000°C).
Hochtemperaturreaktionen in spektralanalytisch wichtigen SystemenII. Reaktionen von Graphit mit den Oxiden von Magnesium, Silicium, Vanadium und Aluminium
Zusammenfassung Die Reaktionen wurden durch Spektralanalyse und Röntgendiffraktometrie untersucht. Die Proben wurden in einem Evaporator auf kontrollierte Temperaturen erhitzt. Im Bereich von 1000–1900° C reagiert MgO nicht mit Graphit. Al2O3 bildet zunächst -Al2O3 und bei 1900°C Al4C3. SiO2 bildet bei etwa 1400°C SiC. V2O5 wird zunächst zu VO2 reduziert und geht dann bei höheren Temperaturen (1200°C) in -VC über. MgO und SiO2 im Gemisch mit Graphit bilden Mg2SiO4, das bei hohen Temperaturen (bis 2000°C) noch beständig ist.
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17.
Summary The nitrogen/oxygen-Analyzer TC-436 (LECO-Instruments) has been used to perform a two-step technique of the carrier gas-hot extraction method to avoid perturbations in the determination of bulk oxygen in solids. In the first step surface contaminations and organic admixtures are removed at 1000°C. The second step involves controlled heating-straight ramping or a simple impulse — to determine oxygen bound in oxides. The application of the method is shown by two example-chips of an FeBSi-alloy and powdered Si/Al2O3.  相似文献   

18.
Conclusions Capture and reversible high-temperature chemisorption of hydrogen is observed on catalysts containing reduced V2O5 supported on MgO and Al2O3 which have been heated to 500°C. The amount of hydrogen taken up in chemisorption varies with the concentration of V2O5 and the nature of the carrier, the latter factor determining the relative ease of desorption.Translated from Izvestiya Akademii Nauk SSSR, Seriya Khimicheskaya, No. 7, pp. 1464–1466, July, 1982.The authors wish to thank G. V. Shakhnovich, who furnished the V2O5-MgO catalysts.  相似文献   

19.
Thin films of vanadium oxide were grown on vanadium metal surfaces (i) in air at ambient conditions, (ii) in 5 mM H2SO4 (aq), pH 3, (iii) by thermal oxidation at low oxygen pressure (10?5 mbar) at temperatures between 350 and 550 °C and (iv) at near‐atmospheric oxygen pressure (750 mbar) at 500 °C. The oxide films were investigated by atomic force microscopy (AFM), X‐ray photoelectron spectroscopy (XPS), X‐Ray diffraction (XRD) and Rutherford backscattering spectrometry (RBS) and nuclear reaction analysis (NRA). The lithium intercalation properties were studied by cyclic voltammetry (CV). The results show that the oxide films formed in air at room temperature (RT), in acidic aqueous solution, and at low oxygen pressure at elevated temperatures are composed of V2O3. In air and in aqueous solution at RT, the oxide films are ultra‐thin and hydroxylated. At 500 °C, nearly atmospheric oxygen pressure is required to form crystalline V2O5 films. The oxide films grown at pO2 = 750 mbar for 5 min are about 260‐nm thick, and consist of a 115‐nm outer layer of crystalline V2O5. The inner oxide is mainly composed of VO2. For all high temperature oxidations, the oxygen diffusion from the oxide film into the metal matrix was considerable. The oxygen saturation of the metal at 450 °C was found, by XPS, to be 27 at.% at the oxide/metal interface. The well‐crystallized V2O5 film, formed by oxidation for 5 min at 500 °C and 750 mbar O2, was shown to have good lithium intercalation properties and is a promising candidate as electrode material in lithium batteries. Copyright © 2005 John Wiley & Sons, Ltd.  相似文献   

20.
Transparent and porous boehmite, -Al2O3 (500°C) and -Al2O3 (900° and 1000°C) thin sheets (50–100 m) have been prepared from boehmite sols. -Al2O3 shows about 48% porosity and 292 m2/g surface area. On transformation from -Al2O3 (500°C) to -Al2O3 (900°C), the porosity still remains high, i.e. 45%; however, the surface area becomes 138 m2/g. The porosity and surface area of -Al2O3 become about 41% and 97 m2/g respectively on further heating to 1000°C. A gradual increase of average pore radius during this thermal treatment suggests that coarsening of the pore occurred during the densification process. Both -Al2O3 and -Al2O3 show high degree of transmission from UV to NIR wavelength region. Cerium exists in +4 oxidation state in the boehmite as well as in the - and -Al2O3. The ultraviolet absorption edge of the alumina was tailored by varying the concentration of cerium.  相似文献   

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