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1.
Electrical conductivity in the monoclinic Li2TiO3, cubic Li1.33Ti1.67O4, and in their mixture has been studied by impedance spectroscopy in the temperature range 20–730 °C. Li2TiO3 shows low lithium ion conductivity, σ300≈10–6 S/cm at 300 °C, whereas Li1.33Ti1.67O4 has 3×10–8 at 20 °C and 3×10–4 S/cm at 300 °C. Structural properties are used to discuss the observed conductivity features. The conductivity dependences
on temperature in the coordinates of 1000/T versus loge(σT) are not linear, as the conductivity mechanism changes. Extrinsic and intrinsic conductivity regions are observed. The change
in the conductivity mechanism in Li2TiO3 at around 500–600 °C is observed and considered as an effect of the first-order phase transition, not reported before. Formation
of solid solutions of Li2–
x
Ti1+
x
O3 above 900 °C significantly increases the conductivity. Irradiation by high-energy (5 MeV) electrons causes defects and the
conductivity in Li2TiO3 increases exponentially. A dose of 144 MGy yields an increase in conductivity of about 100 times at room temperature.
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2.
Sara Goñi Francisca Puertas María Soledad Hernández Marta Palacios Ana Guerrero Jorge S. Dolado Bruno Zanga Fulvio Baroni 《Journal of Thermal Analysis and Calorimetry》2010,102(3):965-973
This research is part of a European project (namely, CODICE project), main objective of which is modelling, at a multi-scale,
the evolution of the mechanical performance of non-degraded and degraded cementitious matrices. For that, a series of experiments
were planned with pure synthetic tri-calcium silicate (C3S) and bi-calcium silicate (C2S) (main components of the Portland cement clinker) to obtain different calcium–silicate–hydrate (C–S–H) gel structures during
their hydration. The characterization of those C–S–H gels and matrices will provide experimental parameters for the validation
of the multi-scale modelling scheme proposed. In this article, a quantitative method, based on thermal analyses, has been
used for the determination of the chemical composition of the C–S–H gel together with the degree of hydration and quantitative
evolution of all the components of the pastes. Besides, the microstructure and type of silicate tetrahedron and mean chain
length (MCL) were studied by scanning electron microscopy (SEM) and 29Si magic-angle-spinning (MAS) NMR, respectively. The main results showed that the chemical compositions for the C–S–H gels
have a CaO/SiO2 M ratio almost constant of 1.7 for both C3S and C2S compounds. Small differences were found in the gel water content: the H2O/SiO2 M ratio ranged from 2.9 ± 0.2 to 2.6 ± 0.2 for the C3S (decrease) and from 2.4 ± 0.2 to 3.2 ± 0.2 for the C2S (increase). The MCL values of the C–S–H gels, determined from 29Si MAS NMR, were 3.5 and 4 silicate tetrahedron, for the hydrated C3S and C2S, respectively, remaining almost constant at all hydration periods. 相似文献
3.
The present work deals with the composite system (CuI)
x
–(Ag2O–TeO2)100–
x
, where x=30, 35, 40, 45, 50, 55, 60, 65, 70 and 75 mol%, respectively, synthesized by a solid-state reaction route. Powder specimens
were analysed using differential scanning calorimetry, X-ray diffraction and Fourier transform infrared techniques. These
studies have revealed the formation of Cu3TeO6, AgI and/or other phases. The ambient temperature electrical conductivities obtained for the samples using a complex impedance
method were found to lie in the range 10–6–10–4 Scm–1, with low activation energies, thus indicating their superionic nature. The typical composition 35CuI–32.5Ag2O–32.5TeO2 was identified as the best conducting one, having an electrical conductivity of 6×10–4 Scm–1 at 296 K and an activation energy of 0.23 eV. Ion transport number measurements carried out using Wagner's polarization technique
as well as by an electromotive force method suggested that silver ions were responsible for the observed transport features
of the composite system.
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4.
Yong Hong Wang Yang Zhang Xing Qin Liu Guang Yao Meng 《Journal of Sol-Gel Science and Technology》2007,41(3):267-275
A simple approach namely sol-coated technique has been developed for the low cost fabrication of macroporous ceramic under
a far below common sintering temperature of alumina with large dimension grains. The prepared green support shows higher sinteractive
than the one treated by wet impregnation method under the same sintering conditions. The support possesses great potential
applications with 6.63–7.71 μm in pore size, 39% open porosity as well as >45 MPa mechanical strength at the sintering temperature
range of 1350°– 1500°C. The results indicate that the nitrogen gas flux and pure water permeation value was 51 252.35 m3 m−2 h−1 bar−1, 98.43 m3 m−2 h−1 bar−1, respectively, which were more dependent on the pore structure and pore size distribution than open porosity. 相似文献
5.
The impedance spectra of CeF3/CeF3 bicrystal (two single crystals separated by a single intercrystalline boundary) between Ag-electrodes are studied over a
135 to 410 K temperature interval (including temperatures below room temperature). The bicrystal was prepared by thermal-diffusion
welding under a pressure of 1.5 × 107 Pa at 1473 K in vacuum (∼10−2 Pa). It is shown that the intercrystalline boundary affects but insignificantly the bicrystal bulk impedance. The CeF3/CeF3 ionic conductivity is 3 × 10−6 S/cm at 293 K; it is mainly determined by transfer processes in the single crystal bulk. 相似文献
6.
B. V. Lebedev K. B. Zhogova V. D. Blank R. Kh. Bagramov 《Russian Chemical Bulletin》2000,49(2):280-284
The temperature dependences of the heat capacityC
0
p
of fullerites C60 were studied at temperatures ranging from 5 to 320 K in an adiabatic vacuum calorimeter with an accuracy of 0.4–0.2%. The
fullerite C60 samples were prepared by treating the starting fullerite C60 under 8 GPa at 920 and 1270 K and “quenched” by a sharp decrease in pressure to −105 Pa and in temperature to ∼300 K. Fullerite C60(8 GPa, 920 K), a crystalline polymer with layered structure formed by polymerized fullerene C60 molecules, was obtained at 920 K and 8 GPa. Fullerite C60(8 GPa, 1270 K), a three-dimensional polymer with a graphite-like structure formed by fragments of decomposed C60 molecules and containing many C(sp3)−C(sp3) bonds, was obtained at 1270 K and 8 GPa. Both polymers are metastable polymeric phases. The anomalous character of the temperature
dependence of the heat capacity was revealed in the 49–66 K range for the polymer formed at 1270 K. The thermodynamic functions
of the substances under study were calculated for the 0–320 K region along with entropies of their formation from graphite.
The entropies of transformation of the starting fullerite C60 into metastable phases and that of intertransformation of phases were estimated.
Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 2, pp. 277–281, February, 2000. 相似文献
7.
Marcela Stoia C. Caizer M. Stefanescu P. Barvinschi I. Julean 《Journal of Thermal Analysis and Calorimetry》2007,88(1):193-200
This article presents the results
of our investigation on the obtaining of Ni0.65Zn0.35Fe2O4 ferrite nanoparticles embedded in a SiO2 matrix using
a modified sol–gel synthesis method, starting from tetraethylorthosilicate
(TEOS), metal (FeIII,NiII,ZnII)
nitrates and ethylene glycol (EG). This method consists in the formation of
carboxylate type complexes, inside the silica matrix, used as forerunners
for the ferrite/silica nanocomposites. We prepared gels with different compositions,
in order to obtain, through a suitable thermal treatment, the nanocomposites
(Ni0.65Zn0.35Fe2O4)x–(SiO2)100–x (where x=10,
20, 30, 40, 50, 60 mass%). The synthesized gels were studied by differential
thermal analysis (DTA), thermogravimetry (TG) and FTIR spectroscopy.
The formation of Ni–Zn ferrite in the silica matrix and the behavior
in an external magnetic field were studied by X-ray diffraction (XRD) and
quasi-static magnetic measurements (50 Hz). 相似文献
8.
M. Prabu S. Selvasekarapandian M. V. Reddy B. V. R. Chowdari 《Journal of Solid State Electrochemistry》2012,16(5):1833-1839
Olivine-structured LiCoPO4 is synthesized by a Pechini-type polymer precursor method. The structure and the morphology of the compounds are studied
by the Rietveld-refined X-ray diffraction, scanning electron microscopy, Brunauer, Emmett, and Teller surface area technique,
infrared spectroscopy, and Raman spectroscopy techniques, respectively. The ionic conductivity (σ ionic), dielectric, and electric modulus properties of LiCoPO4 are investigated on sintered pellets by impedance spectroscopy in the temperature range, 27–50 °C. The σ (ionic) values at 27 and 50 °C are 8.8 × 10−8 and 49 × 10−8 S cm−1, respectively with an energy of activation (E
a) = 0.43 eV. The electric modulus studies suggest the presence of non-Debye type of relaxation. Preliminary charge–discharge
cycling data are presented. 相似文献
9.
Klaartje De Buysser Philippe F. Smet Bart Schoofs Els Bruneel Dirk Poelman Serge Hoste Isabel Van Driessche 《Journal of Sol-Gel Science and Technology》2007,43(3):347-353
This paper describes the synthesis of ZrW2O8 by the use of an aqueous citrate-gel method in order to prepare a fine, pure and homogeneous oxide mixture suitable for ceramic
processing. The thermal expansion coefficient thus obtained for α-ZrW2O8 is −10.6 × 10−6 °C−1 (50–125 °C) whereas for the β-ZrW2O8 a value of −3.2 × 10−6 °C−1 (200–300 °C) is obtained. The advantages of the use of a sol–gel method is expressed in the very homogeneous end-products.
The paper describes crystallographic data, morphological structure and the thermal expansion properties of the ZrW2O8 material. Moreover, photoluminescence and photochromic properties specific to the precursor gel are described and analyzed.
These effects support our views that the precursors show homogeneity up to nanometer level. 相似文献
10.
M. Hampl J. Leitner K. Růžička M. Straka P. Svoboda 《Journal of Thermal Analysis and Calorimetry》2007,87(2):553-556
The heat capacity and the heat content of
bismuth niobate BiNb5O14 were
measured by the relaxation time method, DSC and drop method, respectively.
The temperature dependence of heat capacity in the form C
pm=455.84+0.06016T–7.7342·106/T
2 (J K–1
mol–1) was derived by the least squares method
from the experimental data. Furthermore, the standard molar entropy at 298.15
K S
m=397.17 J K–1
mol–1 was derived from the low temperature
heat capacity measurement. 相似文献
11.
Temperature dependence of viscosity of title glasses (x=0, 2, 4, 6, 8, 10, abbreviated as M0, M2, M4, M6, M8, and M10, respectively) was measured by rotational viscometry (high
temperature region: 102−106.5 dPas) and thermomechanical analysis (low temperature region: 108.5−1011.5 dPas) and described by the Vogel-Fulcher-Tammann equation. The MgO/CaO equimolar substitution (i.e. the increasing x value) smoothly shifts the high temperature viscosity to higher values.
In the low temperature region the mixed alkali effect is demonstrated, and the highest viscosities are observed for the glasses
M0 and M10. In the low temperature range the activation energy of viscous flow linearly decreases with the increasing x value (E
act/kJ mol−1=479−9.0x). No significant dependence of activation energy on x was found in the high temperature range (E
act/kJ mol−1=238.1±4.2). The structural relaxation was measured by thermomechanical experiment and theoretically interpreted in the frame
of Tool-Narayanaswamy-Mazurin’s model. The broadening of the relaxation time spectrum was observed for the calcium-magnesium
glasses in comparison with the pure calcium or magnesium glasses. 相似文献
12.
The kinetics of the solvolytic aquation of trans-[Ru (3-Me Py)4Cl2] was studied spectrophotometrically in water – isopropanol in the range (30–90% v/v), and water acetonitrile in the range
(10–70% v/v), and in the temperature range 50–65 °C. Plots of log k versus the reciprocal of the relative permittivity and Grunwald–Winstien gave non-linear plots. This non-linearity is derived from
a large differential effect of solvent structure between the initial and transition states. The plot of log k versus water concentration was also non linear; evidence for the presence of a S
N
1
mechanism. However, extrema in the variation of enthalpy ΔH* and entropy ΔS* of activation correlate well with the extrema in physical properties of the mixtures which are related to changes in solvent
structure. Linear plots of ΔH* versus ΔS* were obtained and the iso- kinetic temperature indicates that the reaction is entropy controlled. 相似文献
13.
Liquid-phase reduction NO
3
−
using monometallic and bimetallic catalysts (5% Rh/Al2O3, 5% Rh-0.5% Cu/Al2O3, 5% Rh-1.5% Cu/Al2O3, 5% Rh-5% Cu/Al2O3 and a physical mixture of 5% Rh/Al2O3 and 1.5% Cu/Al2O3) was studied in a slurry reactor operating at atmospheric pressure. Kinetic measurements were performed for a low concentration
of nitrate (0.4 × 10−3−3.2 × 10−3 mol dm−3) and the temperature range 293–313 K. From the experimental data, it was found that the reduction of nitrate is first order
with respect to nitrate. On the basis of the rate constants, the apparent activation energy was established using a graphic
method.
Published in Russian in Kinetika i Kataliz, 2007, Vol. 48, No. 6, pp. 881–886.
This article was submitted by the authors in English. 相似文献
14.
E. Yu. Pikalova V. G. Bamburov A. A. Murashkina A. D. Neuimin A. K. Demin S. V. Plaksin 《Russian Journal of Electrochemistry》2011,47(6):690-696
CeO2-based solid solutions with a fluorite structure are promising materials as electrolytes of medium-temperature electrochemical
devices: electrolytic cells, oxygen sensors, and solid oxide fuel cells. In this work, studies are presented of the effect
of the dopant cation radius and its concentration on the physico-chemical properties of the Ce1 − x
Ln
x
O2 − δ solid solutions (x = 0–0.20; Ln = La, Nd, Sm, Eu, Gd, Dy, Ho, Er, Yb) and also of multicomponent solid solutions of Ce1 − x
Ln
x/2Ln′
x/2O2 − δ (x = 0–0.20; Ln = Sm, La, Gd and Ln′ = Dy, Nd, Y) and Ce1 − x − y
Sm
x
M
y
O2 − δ (M = Ca, Sr, Ba) obtained using the solid-phase synthesis technique. Electric properties of the samples were studied in the
temperature range of 623–1173 K and in the oxygen partial pressure range of 0.01–10−22 MPa. The values of oxygen critical pressure ( pO2 * )\left( {p_{O_2 }^* } \right) are presented, at which the ionic and electron conductivity values are equal. The values were calculated on the basis of
experimental dependences at 1023 K at the assumption that the ionic conductivity value is determined only by the dopant concentration
and its effective ionic radius and is independent of the oxygen partial pressure. 相似文献
15.
The complex impedance method in the temperature range of 291–660 K was used to study conductivity of oxofluoride BiO0.1F2.8 belonging to the tysonite structural type (LaF3). Bismuth oxofluoride was synthesized using a solid-phase method at 770–870 K for 1–2 h in an argon atmosphere. Heterovalent
substitution of fluoride ions F− by oxygen ions O2− in the anionic BiF3 matrix sublattice results in high ionic conductivity (∼0.1 S/cm at 660 K) of BiO0.1F2.8 ceramic samples. 相似文献
16.
Andres Trikkel Merli Keelmann Tiit Kaljuvee Rein Kuusik 《Journal of Thermal Analysis and Calorimetry》2010,99(3):763-769
In the present research, CO2 and SO2 binding ability of different oil shale ashes and the effect of pre-treatment (grinding, preceding calcination) of these ashes
on their binding properties and kinetics was studied using thermogravimetric, SEM, X-ray, and energy dispersive X-ray analysis
methods. It was shown that at 700 °C, 0.03–0.28 mmol of CO2 or 0.16–0.47 mmol of SO2 was bound by 100 mg of ash in 30 min. Pre-treatment conditions influenced remarkably binding parameters. Grinding decreased
CO2 binding capacities, but enhanced SO2 binding in the case of fluidized bed ashes. Grinding of pulverized firing ashes increased binding parameters with both gases.
Calcination at higher temperatures decreased binding parameters of both types of ashes with both gases studied. Clarification
of this phenomenon was given. Kinetic analysis of the binding process was carried out, mechanism of the reactions and respective
kinetic constants were determined. It was shown that the binding process with both gases was controlled by diffusion. Activation
energies in the temperature interval of 500–700 °C for CO2 binding with circulating fluidized bed combustion ashes were in the range of 48–82 kJ mol−1, for SO2 binding 43–107 kJ mol−1. The effect of pre-treatment on the kinetic parameters was estimated. 相似文献
17.
Sorption equilibrium of methanol on new composite sorbents “CaCl<Subscript>2</Subscript>/silica gel”
Yuri I. Aristov Larissa G. Gordeeva Yuri D. Pankratiev Ludmila M. Plyasova I. V. Bikova Angelo Freni Giovanni Restuccia 《Adsorption》2007,13(2):121-127
This paper presents experimental data on methanol sorption on new composite sorbents which consist of mesoporous silica gels
and calcium chloride confined to their pores. Sorption isobars and XRD analysis showed the formation of a solid crystalline
solvate CaCl2⋅2MeOH at low methanol uptake, while at higher uptake the formation of the CaCl2–methanol solution occurred. The solution confined to the silica pores showed the sorption properties similar to those of
the CaCl2–methanol bulk solution. Calorimetric and isosteric analyses showed that the heat of methanol sorption depends on the methanol
uptake, ranging from 38±2 kJ/mol for the solution to 81±4 kJ/mol for the solid crystalline phase CaCl2⋅2MeOH. The above mentioned characterizations allowed the evaluation of the methanol sorption and the energy storage capacities,
clearly showing that the optimal applications of these new composite sorbents are the methanol removal from gaseous mixtures,
heat storage and sorption cooling driven by low temperature heat. 相似文献
18.
Hui Sun Xiang-yu Mao Wei Wang Xiao-bing Chen 《Journal of Sol-Gel Science and Technology》2009,52(2):197-201
SrBi4Ti4O15 (SBTi), SrBi3.89La0.1Ti3.97V0.03O15 (SBLTV) thin films have been fabricated on Pt/Ti/SiO2/Si by the sol–gel method. Well-saturated hysteresis loops with remnant polarization around 46.7 μC/cm2 are obtained on Pt/SBLTV/Pt capacitors. The capacitor shows excellent fatigue resistance with no polarization reduction up
to 109 switching cycles even at low test frequency of 50 kHz. The improvement of ferroelectric and fatigue-endurance properties
are attributed to the La3+ and V5+ co-substitution, which brings about the concentration decrease and the mobility weakening of the defects. 相似文献
19.
Shiming Liu Xiaoliang Qian Jianzhong Xiao 《Journal of Sol-Gel Science and Technology》2007,44(3):187-193
Nano-crystalline La0.8Sr0.2Co0.5Fe0.5O3±δ powder has been successfully synthesized by microwave assisted sol–gel (MWSG) method. The decomposition and crystallization
behavior of the gel-precursor was studied by Fourier transform infrared spectroscopy (FT-IR) and X-ray diffraction (XRD) analysis.
From the result of FT-IR and X-ray diffraction patterns, it is found that a perovskite La0.8Sr0.2Co0.5Fe0.5O3±δ was formed by irradiating the precursor at 700 W for 3 min, but the well-crystalline perovskite La0.8Sr0.2Co0.5Fe0.5O3±δ was obtained at 700 W for 35 min. Morphological and specific area analysis of the powder were done by transmission electron
microscopy (TEM), scanning electron microscope (SEM) and Brunauer–Emmett–Teller (BET). The surface areas measured was 38.9 m2/g and the grain size was ∼23 nm. Electrochemical properties of pure LSCF cathode on YSZ electrolyte at intermediate temperatures
were investigated by using AC impedance analyzer, which shows a low area specific resistance (0.077 Ω cm2 at 1073 K and 0.672 Ω cm2 at 953 K). Moreover, the synthesis period of 20 h usually observed for conventional heating mode is reduced to a few minutes.
Thus, the MWSG method is proved to be a novel, extremely facile, time-saving and energy-efficient route to synthesize LSCF
powders. 相似文献
20.
V. Kharton A. Kovalevsky E. Tsipis A. Viskup E. Naumovich J. Jurado J. Frade 《Journal of Solid State Electrochemistry》2002,7(1):30-36
Deficiency in the A sublattice of perovskite-type Sr1–
y
Fe0.8Ti0.2O3–δ (y=0–0.06) leads to suppression of oxygen-vacancy ordering and to increasing oxygen ionic conductivity, unit cell volume, thermal
expansion, and stability in CO2-containing atmospheres. The total electrical conductivity, predominantly p-type electronic in air, decreases with increasing
A-site deficiency at 300–700 K and is essentially independent of the cation vacancy concentration at higher temperatures.
Oxygen ion transference numbers for Sr1–
y
Fe0.8Ti0.2O3–δ in air, estimated from the faradaic efficiency and oxygen permeation data, vary in the range from 0.002 to 0.015 at 1073–1223 K,
increasing with temperature. The maximum ionic conductivity was observed for Sr0.97Fe0.8Ti0.2O3–δ ceramics. In the system Sr0.97Fe1–
x
Ti
x
O3–δ (x=0.1–0.6), thermal expansion and electron-hole conductivity both decrease with x. Moderate additions of titanium (up to 20%) in Sr0.97(Fe,Ti)O3–δ result in higher ionic conductivity and lower activation energy for ionic transport, owing to disordering in the oxygen sublattice;
further doping decreases the ionic conduction. It was shown that time degradation of the oxygen permeability, characteristic
of Sr(Fe,Ti)O3–δ membranes and resulting from partial ordering processes, can be reduced by cycling of the oxygen pressure at the membrane
permeate side. Thermal expansion coefficients of Sr1–
y
Ti1–
x
Fe
x
O3–δ (x=0.10–0.60, y=0–0.06) in air are in the range (11.7–16.5)×10–6 K–1 at 350–750 K and (16.6–31.1)×10–6 K–1 at 750–1050 K.
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