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1.
Carmen Paraschiv B. Jurca Adelina Ianculescu Oana Carp 《Journal of Thermal Analysis and Calorimetry》2008,94(2):411-416
Two bismuth ferrite potential precursors systems, namely Fe(NO3)3·9H2O-Bi(NO3)3·9H2O-glycine/urea with different metal nitrate/organic compound molar ratios have been investigated in order to evaluate their
suitability as BiFeO3 precursors. The presence into the precursor of both reducing (glycine and urea) and oxidizing (NO3−) components, modifies dramatically their thermal behaviour comparative with the raw materials, both from the decomposition
stoichiometries and temperature occurrence intervals points of view. Also, the thermal behaviour is dependent on the fuel
nature but practically independent with the fuel content. The fuel nature influences also some characteristics of the resulted
oxides (phase composition, morphologies). In the case of the oxides prepared using urea as fuel, a faster evolution toward
a single phase composition with the temperature rise is evidenced, the formation of the BiFeO3 perovskite phase being completed in the temperature range of 500–550°C. 相似文献
2.
V. Ya. Yablokov I. L. Smel’tsova I. A. Zelyaev S. V. Mitrofanova 《Russian Journal of General Chemistry》2009,79(8):1704-1706
Rates of thermal decomposition of glycine, alanine, and serine are described by the equation of first order reaction in the
temperature range 200–300°C. Apparent rate constants and apparent activation energies of decomposition of α-amino acids were
evaluated. It was found that the main gaseos reaction product is carbon dioxide. 相似文献
3.
A. Zalga Z. Moravec J. Pinkas A. Kareiva 《Journal of Thermal Analysis and Calorimetry》2011,105(1):3-11
The preparation and characterization of the M′–M′′–O nitrate–tartrate (M′ = Ca, Ba, Gd and M′ = W, Mo) precursor gels synthesized
by simple, inexpensive, and environmentally benign aqueous sol–gel method is reported. The obtained gels were studied by thermal
(TG/DSC) analysis. TG/DSC measurements revealed the possible decomposition pathway of synthesized M′–M′′–O nitrate–tartrate
gels. For the synthesis of different metal tungstates and molybdates, the precursor gels were calcined at different temperatures
(650, 800, and 900 °C). According to the X-ray diffraction (XRD) analysis data, the crystalline compounds CaMo1-x
W
x
O4 doped with Ce3+ ions, BaMo1-x
W
x
O4 doped with Eu3+ ions and Gd2Mo3O12 were obtained from nitrate–tartrate gels annealed at 650–900 °C temperatures. The XRD data confirmed that the fully crystalline
single-phase powellite, scheelite, or Gd2(MoO4)3 structures were formed already at 650 °C. Therefore, the suggested sol–gel method based on the complexation of metal ions
with tartaric acid is suitable for the preparation of mixed tungstates–molybdates at relatively low temperature in comparison
with solid-state synthesis. 相似文献
4.
E. Arico F. Tabuti F. C. Fonseca D. Z. de Florio A. S. Ferlauto 《Journal of Thermal Analysis and Calorimetry》2009,97(1):157-161
The thermal behavior of the yttria-stabilized zirconia (YSZ) and nickel oxide (YSZ–NiO) composite mixtures with the addition
of graphite, multiwall carbon nanotubes and functionalized multiwall carbon nanotubes was studied. The YSZ–NiO composite is
the precursor of the YSZ–Ni anode of solid oxide fuel cells. The anode exhibits a porous structure, which is usually obtained
by the addition of carbon containing pore formers. Thermal analysis and X-ray diffraction evidenced that the properties of
carbonaceous materials (C) and atmosphere have a strong influence on the thermal evolution of the reactions taking place upon
heating the anode precursor. The dependence of both the carbon content and the chemical nature of the ceramic matrix on the
thermal behavior of the composite were investigated. The discussed results evidenced important features for optimized processing
of the anode. 相似文献
5.
Oxidative degradation and pyrolysis of polyvinyl chloride in the temperature range 200–500°C in binary mixtures containing
sodium, potassium, and calcium nitrates and nitrites and calcium hydroxide were studied. A scheme of oxidative degradation
of polyvinyl chloride and of binding of chlorine and carbon present in the polymer in the reactions of the degradation products
with the mixture components was suggested. 相似文献
6.
El-Shobaky G. A. Radwan N. R. E. Radwan F. M. 《Journal of Thermal Analysis and Calorimetry》2002,68(1):275-287
The results obtained showed that the addition of small amounts of LiNO3 to the reacting mixed solids, consisting of equimolar proportion of Fe2O3 and basic MgCO3 much enhanced the thermal decomposition of magnesium carbonate. The addition of 12 mol% LiNO3 (6 mol% Li2O) decreased the decomposition temperature of MgCO3 from 525.5 to362°C. MgO underwent solid–solid interaction with Fe2O3 at temperatures starting from800°C yielding MgFe2O4. The amount of ferrite produced increased by increasing the precalcination temperature of the mixed solids. However, the
completion of this reaction required prolonged heating at elevated temperature above 1100°C. Doping with Li2O much enhanced the solid–solid interaction between the mixed oxides leading to the formation of MgFe2O4 phase at temperatures starting from 700°C. The addition of 6 mol% Li2O to the mixed solids followed by precalcination at 1050°C for 4 h resulted in complete conversion of the reacting oxides
into magnesium ferrite. The heat treatment of pure and doped solids at 900–1050°C effected the disappearance of most of IR
transmission bands of the free oxides with subsequent appearance of new bands characteristic for MgFe2O4 structure. The promotion effect of Li2O towards the ferrite formation was attributed to an effective increase in the mobility
of the various reacting cations. The activation energy of formation (ΔE) of magnesium ferrite was determined for pure and variously doped solids and the values obtained were 203, 126, 95 and 61
kJ mol−1 for pure mixed solids and those treated with 1.5, 3.0 and 6.0 mol% Li2O, respectively.
This revised version was published online in August 2006 with corrections to the Cover Date. 相似文献
7.
M. R. Barati 《Journal of Sol-Gel Science and Technology》2009,52(2):171-178
Nanocrystalline Mg–Cu–Zn ferrite powders were successfully synthesized through nitrate–citrate gel auto-combustion method.
Characterization of the nitrate–citrate gel, as-burnt powder and calcined powders at different calcination conditions were
investigated by using XRD, DTA/TG, IR spectra, EDX, VSM, SEM and TEM techniques. IR spectra and DTA/TGA studies revealed that
the combustion process is an oxidation–reduction reaction in which the NO3
− ion is oxidant and the carboxyl group is reductant. The results of XRD show that the decomposition of the gel indicated a
gradual transition from an amorphous material to a crystalline phase. In addition, increasing the calcination temperature
resulted in increasing the crystallite size of Mg–Cu–Zn ferrite powders. VSM measurement also indicated that the maximum saturation
magnetization (64.1 emu/g) appears for sample calcined at 800 °C while there is not much further increase in M
s at higher calcination temperature. The value of coercivity field (H
c) presents a maximum value of 182.7 Oe at calcination temperature 700 °C. TEM micrograph of the sample calcined at 800 °C
showed spherical nanocrystalline ferrite powders with mean size of 36 nm. The toroidal sample sintered at 900 °C for 4 h presents
the initial permeability (μ
i) of 405 at 1 MHz and electrical resistivity (ρ) of 1.02 × 108 Ω cm. 相似文献
8.
R. Lach M. M. Bućko K. Haberko M. Szumera R. Gajerski 《Journal of Thermal Analysis and Calorimetry》2013,112(2):727-730
Co-precipitation of alumina/YAG precursor from aluminum and yttrium nitrates solution with ammonium carbonate results in dawsonite (NH4Al(OH)2CO3). Its crystallographic parameters differ from the compound precipitated without the yttrium additive. It indicates that yttrium ions become incorporated into the dawsonite structure. The DSC/TG and X-ray measurements show decomposition of dawsonite at elevated temperature resulting in γ-Al2O3 which transforms to δ and θ modifications at still higher temperatures. The full transformation to α-Al2O3 and YAG occurs at temperatures higher than 1,230 °C. 相似文献
9.
S. F. Santos M. C. de Andrade J. A. Sampaio A. B. da Luz T. Ogasawara 《Journal of Thermal Analysis and Calorimetry》2007,87(3):743-746
TiO2–CeO2 oxides
for application as ceramic pigments were synthesized by the Pechini method.
In the present work the polymeric network of the pigment precursor was studied
using thermal analysis. Results obtained using TG and DTA showed the occurrence
of three main mass loss stages and profiles associated to the decomposition
of the organic matter and crystallization. The kinetics of the degradation
was evaluated by means of TG applying different heating rates. The activation
energies (E
a) and
reaction order (n) for each stage were
determined using Horowitz–Metzger, Coats–Redfern, Kissinger and
Broido methods. Values of E
a
varying between 257–267 kJ mol–1 and n=0–1 were found. According to the kinetic
analysis the decomposition reactions were diffusion controlled. 相似文献
10.
The TG and DTA of a new series of Mn(II) and Cu(II) complexes with a number of newly prepared bisazo-dianil ligands were studied
in the temperature range (20-700°C). The TG and DTG curves display to main steps, the first one within the temperature range
(25-330°C) correspond to the elimination of water or and ethanol from the complexes. The second step within the range (350-625°C)
is due to the decomposition of the complexes yielding the metal oxides as the final product. The rate constants of the dehydration
and decomposition reactions were determined, from which some kinetic parameters were evaluated. The DTA curves show that the
dehydration of the metal complexes is an endothermic reaction. In all cases the anhydrous metal complexes undergo exothermic
decomposition reactions to give the metal oxide. The thermodynamic parameters (ΔE, ΔH, ΔS, ΔG) for the occurring processes
are calculated. The electrical conductivities of the solid complexes were measured and the activation energy of the complex
and its free ligand are also calculated.
This revised version was published online in August 2006 with corrections to the Cover Date. 相似文献
11.
Camila S. Xavier R. A. Candeia M. I. B. Bernardi S. J. G. Lima E. Longo C. A. Paskocimas L. E. B. Soledade A. G. Souza Iêda M. G. Santos 《Journal of Thermal Analysis and Calorimetry》2007,87(3):709-713
Magnesium and zinc ferrites
have been prepared by the polymeric precursor method. The organic material
decomposition was studied by thermogravimetry (TG) and differential thermal
analysis (DTA). The variation of crystalline phases and particle morphology
with calcination temperature were investigated using X-ray diffraction (XRD)
and scanning electronic microscopy (SEM), respectively. The colors of the
ferrites were evaluated using colorimetry. Magnesium ferrite crystallizes
above 800°C, presenting a yellow- orange color with a reflectance peak
at the 600–650 nm range, while zinc ferrite crystallizes at 600°C,
with a reflectance peak between 650–700 nm, corresponding to the red-brick
color. 相似文献
12.
A. I. Bulavchenko A. T. Arymbaeva M. G. Demidova E. A. Maksimovskii 《Colloid Journal》2011,73(6):748-752
A procedure is elaborated for preparing powders of ammonium and potassium nitrates with microsized particles and stable sols
with particle sizes of 7–16 nm based on isothermal mass crystallization from Tergitol NP-4-stabilized water-in-oil microemulsions
in decane. The crystallization process is studied by turbidimetry and photon-correlation spectroscopy. The isolated powders
are characterized by scanning electron microscopy, while sols and microemulsions are studied by photon-correlation spectroscopy.
Evaporation of water from microemulsion droplets upon stirring water-in-oil micellar solutions at 25–45°C is shown to be the
reason for the salt crystallization. It is ascertained that the time of the onset of crystallization and the morphology of
resulting particles depend on temperature, content of an aqueous pseudophase, and the nature of a salt. A desolubilization-emulsion
hypothesis is proposed for explaining the formation of nanoparticle powders and organosols. 相似文献
13.
Y. S. Malghe S. R. Dharwadkar K. Krishnan K. D. Singh Mudher 《Journal of Thermal Analysis and Calorimetry》2009,96(1):49-52
The phase transitions in the LaCrO3 were studied using bulk dilatometry and high temperature X-ray diffractometry from room temperature to 1050 and 1200°C, respectively.
LaCrO3 was prepared at 500°C from oxalate precursor employing microwave heating technique. Bulk shrinkage measurements on LaCrO3 pellets were carried out using dilatometer designed and fabricated in our own laboratory. Dilatometric curves of LaCrO3 showed two peaks in ΔL/L vs. temperature curves in the range 200–400 and 800–1000°C, respectively. These phase transitions have been confirmed using
high temperature X-ray diffractometry. The role of simple technique like bulk dilatometry in detecting and monitoring the
polymorphic transformations in solids is discussed for lanthanum chromates. 相似文献
14.
Three solid wastes generated from the vegetable tanning of bovine skin in the Leather Industry (shavings, trimmings and buffing dust) were mixed together in the same proportions in which they were produced and the mixture was then used as a pyrolysis precursor for this research study. The optimal pyrolysis conditions for obtaining energy from the generated fractions (char, tar and gas fraction), and the preparation of activated carbons from the carbonaceous material (char), were established. The final conditions were chosen from two different points of view, the thermogravimetric results (TG/DTG) obtained at different heating rates (2–20 °C/min) and an optimization of the pyrolysis parameters by means of experiments carried out in a conventional furnace. The pyrolysis conditions finally selected were: heating rate (5 °C/min), final temperature (750 °C), and time at final temperature (60 min) and inert gas flow (N2 150 ml/min). The carbonaceous material (char) obtained exhibits good properties as a solid fuel due to its high calorific value and relatively low ash content. It also shows suitable characteristics as a precursor for the preparation of activated carbons. The condensable fraction has a predominantly phenolic nature and contains significant amounts of nitrogen compounds (nitriles, diketopiperazines, etc.), alkanes, alkenes, acids and esters, derived from the decomposition of tannins and collagen, with possible industrial applications in the preparation of chemical products. The gaseous phase is rich in carbon monoxide and carbon dioxide, and also contains a certain amount of methane and hydrogen. The syngas content increases with the pyrolysis temperature. A kinetic study of the pyrolysis was carried out using a model of independent reactions. The variation in the heating rate produced a slight shift to higher temperatures of the decomposition peaks, although this did not significantly affect either the kinetic parameters of the degradation processes or the percentage weight losses. 相似文献
15.
Yong-yong Wu Fang-li Jing Shi-zhong Luo Wei Chu Hong-zhi Ni 《Journal of Sol-Gel Science and Technology》2011,58(1):142-147
Metal (Cu, Zn, Al) nitrates and chlorides were used for preparing CuZnAl xerogels by a sol–gel route with propylene oxide
as gelation initiator. The CuZnAl mixed-metal oxides were further obtained by thermal treatment the xerogels at 500 °C for
5 h in air. Thermal decomposition behavior of the CuZnAl xerogels, the microstructures and the reducibility of the calcined
xerogels were investigated by thermogravimetry (TG), scanning electron microscope (SEM), powder X-ray diffraction (XRD), N2 adsorption/desorption (BET, BJH) and temperature-programmed reduction (TPR) techniques. The catalytic activity in dehydrocyclization
of ethylenediamine (ED) with 1, 2-propyleneglycol (PG) to 2-methylpyrazine (2-MP) was carried out at 380 °C. The results displayed
that the CuZnAl mixed-metal oxides prepared using nitrates as the metal precursors had a higher metallic Cu dispersion and
a superior low-temperature reducibility than those prepared by chlorides, which results in a higher catalytic activity for
the synthesis of 2-methylpyrazine. Especially when the molar ratio of Cu/Zn/Al = 2:1:2, the catalyst using nitrates as the
metal precursors improved the selectivity of 2-MP to 87.5%. 相似文献
16.
Dariusz Szychowski Barbara Pacewska Grzegorz Makomaski Janusz Zieliński Wiesława Ciesińska Tatiana Brzozowska 《Journal of Thermal Analysis and Calorimetry》2012,107(3):893-900
The purpose of this study was to determine the possibility of producing hydrophobic mesoporous mineral–carbon sorbents from
aluminum hydroxide and compositions of coal tar pitch–polymers on carbonization at 600 °C in a nitrogen atmosphere. Blends
of the products of co-precipitation of aluminum hydroxide in the carbonaceous substances medium were subjected to carbonization
process. The extent of porous structure development was evaluated using low temperature nitrogen adsorption, adsorption of
benzene vapors, and adsorption of iodine from aqueous solution. The highest value of BET surface area of about 370 m2/g was achieved for the carbonization product obtained from co-precipitated raw components with 10 wt% compositions coal tar
pitch–polymer. These materials demonstrated high capacity to reduce organic pollutions from sewage. Pitch–polymer composition
containing poly(ethylene terephthalate) or phenol–formaldehyde resin was studied by the means of DSC method in order to determine
the high-temperature transformations taking place under the conditions of carbonization. DSC method enables to determine i.a.
the decomposition temperatures of carbonizates produced from pitch–polymer compositions and the evaluation of their sorption
abilities. The additive of poly(ethylene terephthalate) and phenol–formaldehyde resin caused the increase of thermal resistance
of the pitch expressed by higher decomposition temperatures. 相似文献
17.
V. Balek E. R. Vance V. Zeleňák Z. Málek J. Šubrt 《Journal of Thermal Analysis and Calorimetry》2007,88(1):93-98
Emanation thermal
analysis (ETA) was used to characterize the thermal reactivity of amorphous
brannerite mineral of general formula U1–xTi2+xO6
(locality El Cabril, near Cordoba, Spain). It was demonstrated that on sample
heating up to 880°C microstructure changes taking place in the sample
were accompanied by the formation of new radon diffusion paths, followed by
their closing up during the final transformation of amorphous to crystalline
brannerite in the range 900–1020 °C. Relative changes in structure
irregularities that served as radon diffusion paths during heating and subsequent
cooling of the sample to temperatures of 300, 550, 750, 880, 1020 and 1130°C,
respectively, were determined from the ETA results. Mass losses in temperature
ranges of 230–315, 570–760 and 840–1040°C were observed
by thermogravimetry. Mass spectrometry indicated the release of CO2 mainly
due to the decomposition of minor carbon amount in the brannerite mineral
sample. 相似文献
18.
Richard R. Baker 《Thermochimica Acta》1976,17(1):29-63
When tobacco is pyrolysed under non-isothermal flow conditions in an inert atmosphere, variation of the inert gas or its space velocity has only a minor effect on the profiles of formation rate versus temperature for seven product gases. Thus, mass transfer processes between the tobacco surface and the gas phase are very rapid, and the products are formed at an overall rate which is determined entirely by that of the chemical reactions.The effect of radical chain inhibitors (nitrogen oxides) on the pyrolysis is complex because of the resultant oxidation. Nevertheless, no evidence was found for the occurrence of radical chain reactions in the gas phase. A small proportion (less than 10%) of all the gases monitored are formed by homogeneous decomposition of volatile and semi-volatile intermediate products, in the furnace used.At temperatures above about 600°C the reduction of carbon dioxide to carbon monoxide by the carbonaceous tobacco residue becomes increasingly important. However, when tobacco is pyrolysed in an inert atmosphere, only a small amount of carbon dioxide is produced above 600°C and consequently its reduction to carbon monoxide contributes only a small proportion to the total carbon monoxide formed above that temperature. The rate of the tobacco/carbon dioxide reaction is controlled by chemical kinetic rather than mass transfer effects. Carbon monoxide reacts with tobacco to a small extent.When the tobacco is pyrolysed in an atmosphere containing oxygen (9–21% v/v), some oxidation occurs at 200°C. At 250°C the combustion rate is controlled jointly by both kinetic and mass transfer processes, but mass transfer of oxygen in the gas phase becomes increasingly important as the temperature is increased, and it is dominant above 400°C. About 8% of the total carbon monoxide formed by combustion is lost by its further oxidation.The results imply that inside the combustion coal of a burning cigarette the actual reactions occurring are of secondary importance, the rate of supply of oxygen being the dominant factor in determining the combustion rate and heat generation. In contrast, in the region immediately behind the coal, where a large proportion of the products which enter mainstream smoke are formed by thermal decomposition of tobacco constituents, the chemistry of the tobacco substrate is critical, since the decomposition kinetics are controlled by chemical rather than mass transfer effects. tobacco substrate is critical. In addition, the heat release or absorption due to the pyrolytic reactions occurring behind the coal will depend on the chemical composition of the substrate. Thus, together with the differing thermal properties of the tobacco, the temperature gradient behind the coal should depend on the nature of the tobacco. 相似文献
19.
Nanocrystalline BaSnO3 with a primary particle size of 40–60 nm was prepared through hydrolysis of a barium tin isopropoxide and following crystallization.
The thermal decomposition, the crystallization and the microstructure of the obtained powders were investigated with the help
of TG-DTA, IR, XRD, HRSEM and HRTEM. The organic rest groups in the as-prepared powder decompose thermally at 350°C, which
is accompanied by the building of BaCO3 that disappear again at 600°C. The crystallization of BaSnO3 takes place at 500–600°C. Single-phase BaSnO3 powders have been obtained at a temperature as low as 600°C. The amorphous as-prepared powder shows a cluster structure.
Nucleation of BaSnO3 beginning at 350°C was observed under HRTEM, and the spherical nano-particles of BaSnO3 calcined at 760°C crystallize well and are strongly aggregated. The presented results indicate a heterogeneous nucleation
and growth mechanism by the formation of BaSnO3. 相似文献
20.
The effects of the additives of iron, nickel, zinc, and their oxides on the process of coal gasification with carbon dioxide
at temperatures of 550–800°C was studied. It was found that the additives used did not exhibit noticeable activity upon mixing
with coal. Impregnation with nickel was found most efficient; it caused a notable increase in the rate of the process and
a higher degree of CO2 conversion, as compared with the thermodynamically equilibrium conversion for a given temperature. Thus, impregnation with
5% nickel made it possible to decrease the reaction temperature by 80°C with the retention of the yield of CO at about 100%.
Kinetic models for describing noncatalytic and catalytic gasification reactions were considered and a mechanism of the process
in the presence of nickel was proposed. 相似文献