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1.
Fabiane Alexsandra Andrade de Jesus Ronaldo Santos da Silva Zélia Soares Macedo 《Journal of Thermal Analysis and Calorimetry》2010,100(2):537-541
Bismuth germanate ceramic powders were synthesized for the first time by the polymeric precursor method (Pechini’s method).
Differential thermal analysis and thermogravimetric techniques were used to study the decomposition of the resin precursor,
which indicated a suitable calcination temperature at 600 °C. It was observed that the mass loss occurs in two main stages
that are associated with two exothermic reactions. The crystalline phases of the powders were inspected by the X-ray diffraction
technique after thermal treatment between 300 and 600 °C. Single phase Bi4Ge3O12 ceramic bodies were obtained after sintering at 840 °C for 10 h. The sintered ceramics presented a luminescence band emission
centred at around 530 nm when excited with X-rays and UV radiation. 相似文献
2.
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.
Electronic Publication 相似文献
3.
Fe3O4 nanorods and Fe2O3 nanowires have been synthesized through a simple thermal oxide reaction of Fe with C2H2O4 solution at 200–600°C for 1 h in the air. The morphology and structure of Fe3O4 nanorods and Fe2O3 nanowires were detected with powder X-ray diffraction, scanning electron microscopy and transmission electron microscopy.
The influence of temperature on the morphology development was experimentally investigated. The results show that the polycrystals
Fe3O4 nanorods with cubic structure and the average diameter of 0.5–0.8 μm grow after reaction at 200–500°C for 1 h in the air.
When the temperature was 600°C, the samples completely became Fe2O3 nanowires with hexagonal structure. It was found that C2H2O4 molecules had a significant effect on the formation of Fe3O4 nanorods. A possible mechanism was also proposed to account for the growth of these Fe3O4 nanorods.
Supported by the Fund of Weinan Teacher’s University (Grant No. 08YKZ008), the National Natural Science Foundation of China
(Grant No. 20573072) and the Doctoral Fund of Ministry of Education of China (Grant No. 20060718010) 相似文献
4.
L. R. Gonsalves S. C. Mojumdar V. M. S. Verenkar 《Journal of Thermal Analysis and Calorimetry》2011,104(3):869-873
Cobalt zinc ferrite, Co0.8Zn0.2Fe2O4, nanoparticles have been synthesized via autocatalytic decomposition of the precursor, cobalt zinc ferrous fumarato hydrazinate.
The X-ray powder diffraction of the ‘as prepared’ oxide confirms the formation of single phase nanocrystalline cobalt zinc
ferrite nanoparticles. The thermal decomposition of the precursor has been studied by isothermal, thermogravimetric and differential
thermal analysis. The precursor has also been characterized by FTIR, and chemical analysis and its chemical composition has
been determined as Co0.8Zn0.2Fe2(C4H2O4)3·6N2H4. The Curie temperature of the ‘as-prepared oxide’ was determined by AC susceptibility measurements. 相似文献
5.
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
6.
N. I. Kadyrova Yu. G. Zainulin G. S. Zakharova A. P. Tyutyunnik N. V. Mel’nikova 《Russian Journal of Inorganic Chemistry》2011,56(11):1717-1722
Under uniform compression (p = 7.0 GPa) on heating (T = 1100°C), the perovskite-like oxide CaCu2CoV4O12 was obtained for the first time. The crystal structure of the compound was determined by X-ray crystallography (space group Im-3, Z = 2, a = 7.3015(5) Å). The main bond lengths and angles were found. It was established that the high-pressure phase CaCu2CoV4O12 has metallic conduction. Its magnetic properties were studied. 相似文献
7.
A. L. Zharnyl’skaya V. V. Vol’khin H. Reuther 《Russian Journal of Applied Chemistry》2009,82(8):1364-1369
Samples of a precursor for an aluminum oxide ceramics reinforced with zirconium oxide were synthesized by hydrolysis of various
aluminum salts in the presence of a ZrO2 sol under conditions of urea decomposition at 90°C and pH < 4 maintained, with hydrolysis products deposited onto the surface
of ZrO2 sol particles. It was found that the nature of a salt anion affects the interaction of hydrolysis products of the aluminum
cation with the surface of ZrO2 sol particles. The structure of products formed in thermal treatment of samples of a precursor for Al2O3-ZrO2 (T = 1250°C) was characterized by X-ray phase analysis and scanning electron microscopy. The phase transition temperatures of
the oxides Al2O3 and ZrO2 contained in the precursor were estimated using the results of thermal analysis of the samples in the temperature range 20–1300°C. 相似文献
8.
Maria N. Mancheva Reni S. Iordanova Yanko B. Dimitriev Georgi G. Tyuliev Tzvetoslav Ch. Iliev 《Central European Journal of Chemistry》2011,9(3):460-465
ZrMo2O7(OH)2·2H2O was obtained from ZrOCl2·2H2O and Na2MoO4·2H2O by a coprecipitation method. The phase and structural changes occurred during the heat-treatment of ZrMo2O7(OH)2·2H2O were investigated by XRD, IR and XPS analysis. The sequence of phase transformation can be divided into three stages: (1)
transformation of ZrMo2O7(OH)2·2H2O to orthorhombic LT-ZrMo2O8 up to 300°C; (2) obtaining of mixture of both polymorphs of ZrMo2O8: cubic and trigonal at 400°C; (3) conversion to single trigonal (α) ZrMo2O8 above 450°C. The microstructure of the obtained trigonal (α) ZrMo2O8 was observed by scanning electron microscopy (SEM). The particle sizes were below 0.5 μm. The specific surface area was measured
by modified BET method. The photocatalytic activity of the obtained trigonal (α) ZrMo2O8 powders was investigated by degradation of a model aqueous solution of Malachite Green (MG) upon UV-light irradiation. 相似文献
9.
P. Schwendt D. Dudášová J. Chrappová M. Drábik J. Marek 《Journal of Thermal Analysis and Calorimetry》2008,91(1):293-297
The compound [Ni(NH3)6][VO(O2)2(NH3)]2 was prepared and characterized by elemental analysis and vibrational spectra. The single crystal X-ray study revealed that
the structure consists of [Ni(NH3)6]2+ and [VO(O2)2(NH3)]− ions. As a result of weak interionic interactions V′···Op (Op-peroxo oxygen), ([VO(O2)2(NH3)]−)2 dimers are formed in the solid-state. The thermal decomposition of [Ni(NH3)6][VO(O2)2(NH3)]2 is a multi-step process with overlapped individual steps; no defined intermediates were obtained. The final solid products
of thermal decomposition up to 600°C were Ni2V2O7 and V2O5. 相似文献
10.
Magnetic Co3O4 nanoparticles were prepared by using microporous regenerated cellulose films as sacrificial scaffolds. The cellulose macromolecules
and the porous structure of the films made them used as spatially confined reacting sites where Co(OH)2 nanoparticles could be synthesized in situ. When the cellulose matrix was removed by sintering at 500 °C, Co3O4 nanoparticles were obtained. XRD and XPS indicated that the prepared nanoparticles were pure Co3O4 without any impurity. TEM and SEM images revealed that the particle size of the nanoparticles was smaller than 100 nm. The
nanoparticles had weak ferromagnetic properties at 25 °C. Furthermore, the pronounced quantum confinement effects of the synthesized
nanoparticles have been observed, the optical bandgap energies determined were about 1.92 ~ 2.12 and 2.74 ~ 2.76 eV for O2− → Co3+ and O2− → Co2+ charge-transfer processes, respectively. Furthermore, the resulted Co3O4 nanoparticles behaved stable electrochemical performance with promising applications in the electrode for lithium ion battery. 相似文献
11.
M. M. Godneva D. L. Motov M. P. Rys’kina 《Russian Journal of Inorganic Chemistry》2011,56(9):1363-1369
The ZrO(NO3)2-H3PO4-CsF-H2O system was studied at 20°C along the section at a molar ratio of PO43−/Zr = 0.5 (which is of the greatest interest in the context of phase formation) at ZrO2 concentrations in the initial solutions of 2–14 wt % and molar ratios of CsF: Zr = 1−6. The following compounds were isolated
for the first time: crystalline fluorophosphates CsZrF2PO4 · H2O, amorphous oxofluorophosphate Cs2Zr3O2F4(PO4)2 · 3H2O, and amorphous oxofluorophosphate nitrate CsZr3O1.25F4(PO4)2(NO3)0.5 · 4.5H2O. The compound Cs3Zr3O1.5F6(PO4)2 · 3H2O was also isolated, which forms in a crystalline or glassy form, depending on conditions. The formation of the following
new compounds was established: Cs2Zr3O1.5F5(PO4)2 · 2H2O, Cs2Zr3F2(PO4)4 · 4.5H2O, and Zr3O4(PO4)1.33 · 6H2O, which crystallize only in a mixture with known phases. All the compounds were studied by X-ray powder diffraction, crystal-optical,
thermal, and IR spectroscopic analyses. 相似文献
12.
Monika Bosacka 《Journal of Thermal Analysis and Calorimetry》2007,88(1):43-46
It has been demonstrated that Co2V2O7
and InVO4 react with each other forming a new compound
of the Co2InV3O11
formula, when their molar ratio is equal to 1:1, or among CoCO3,
In2O3 and V2O5,
mixed at a molar ratio of 4:1:3. This compound melts incongruently at the
temperature of 960±5°C, depositing crystals of InVO4.
It crystallizes in the triclinic system and the unit cell parameters amount
to: a=0.6524(6) nm, b=0.6885(5)
nm, c=1.0290(4) nm, α=96.5°, β=104.1°,
γ=100.9°, Z=2. The phase equilibria
being established in the Co2V2O7–InVO4
system over the whole components concentration range up to the solidus line
were described. 相似文献
13.
ZrWMoO8 powders with different morphologies were obtained using ammonium tungstate, molybdate tungstate and zirconium tungstate as
the starting materials by dehydrating the precursor ZrWMoO7(OH)2(H2O)2. The precursor was studied by thermo-gravimetric and differential scanning calorimetry (TG-DSC). The influence of the gelling
agents (HCl, HClO4, HNO3, H2SO4 and H3PO4) on the crystallization process and crystal morphology of the products prepared was investigated by X-ray powder diffraction
(XRD), scanning electron micrograph (SEM) and X-ray fluorescence spectrometer (XRF). Results showed that the morphology of
the ZrWMoO8 particles can be simply adjusted by changing the gelling agents, and the thermal expansion coefficients of cubic ZrWMoO8 prepared in HCl solution are −3.84 × 10−6 K−1 from 100°C to 700°C.
__________
Translated from Chemical Journal of Chinese University, 2007, 28(3): 397–401 [译自: 高等学校化学学报] 相似文献
14.
A. Sakunthala M. V. Reddy S. Selvasekarapandian B. V. R. Chowdari H. Nithya P. Chirstopher Selvin 《Journal of Solid State Electrochemistry》2010,14(10):1847-1854
The compound, lithium trivanadate (LiV3O8), was synthesized by the polymer precursor method, using the polymer polyvinylpyrrolidone. The electrochemical performance
of LiV3O8 was compared with LiV3O8 synthesized by the solid state reaction method. The prepared compounds were characterized by X-ray diffraction, scanning
electron microscopy, and high-resolution transmission electron microscopy techniques. The electrochemical performances were
studied by cyclic voltammetry and galvanostatic cycling in the voltage range of 2.0 to 4.0 V at room temperature (25 °C).
The compound prepared by the polymer precursor method was found to have a good cycling stability. A reversible capacity value
of 203 mAh/g (2.18 mol of Li) and 170 mAh/g (1.83 mol of Li) was obtained at the end of the 70th cycle, at a current density
of 30 and 120 mA/g, respectively. 相似文献
15.
Sagrario M. Montemayor L. A. García-Cerda J. R. Torres-Lubián O. S. Rodríguez-Fernández 《Journal of Sol-Gel Science and Technology》2007,42(2):181-186
In this work the synthesis of CoFe2O4-SiO2 and NiFe2O4-SiO2 nanocomposites was studied via the sol–gel method, using the polymerized complex route. The polymerized precursors obtained
by the reaction of citric acid, ethylene glycol, tetraethylorthosilicate, ferric nitrate, and cobalt nitrate or nickel chloride
were characterized by nuclear magnetic resonance (NMR) and infrared (IR) spectroscopy. NMR and IR spectra of the precursors,
without and with metallic ions, show the formation of polymeric chains with ester and ether groups and complexes of metal-polymeric
precursor. The nanocomposites were obtained by the thermal decomposition of the organic fraction and characterized by X-ray
diffraction (XRD) and vibrating sample magnetometry (VSM). XRD patterns show the formation of CoFe2O4 and NiFe2O4 in an amorphous silica matrix above 400 °C in both cases. When the calcination temperature was 800 °C the particle size of
the crystalline phases, calculated using the Scherrer equation, reached ∼35 nm for the two oxides. VSM plots show the ferrimagnetic
behavior that is expected for this type of magnetic material; the magnetization at 12.5 KOe of the CoFe2O4-SiO2 and NiFe2O4-SiO2 compounds was 29.5 and 17.4 emu/g, respectively, for samples treated at 800 °C. 相似文献
16.
O. V. Nipruk N. G. Chernorukov E. L. Kostrova G. N. Chernorukov 《Russian Journal of Inorganic Chemistry》2016,61(5):572-574
Sodium triuranate Na2(UO2)3O3(OH)2 was synthesized by the reaction between aqueous uranyl acetate solution and aqueous sodium nitrate solution under hydrothermal conditions at 200°C. The composition and structure of the synthesized compound were determined, and its dehydration and thermal decomposition were studied, by chemical analysis, X-ray diffraction, IR spectroscopy, and thermal analysis. 相似文献
17.
A. L. Gushchin K. A. Kovalenko M. N. Sokolov D. Yu. Naumov E. V. Peresypkina A. V. Virovets V. P. Fedin 《Russian Chemical Bulletin》2007,56(9):1707-1711
The reactions of the oxalate complexes [M3Q7(C2O4)3]2− (M = Mo or W; Q = S or Se) with MnII, CoII, NiII, and CuII aqua and ethylenediamine complexes in aqueous and aqueous ethanolic solutions were studied. The previously unknown heterometallic
complexes [Mo3Se7(C2O4)3Ni(H2O)5]·3.5H2O (1) and K3{[Cu(en)2H2O]([Mo3S7(ox)3]2Br)}·5.5H2O (2) were synthesized. In these complexes, the oxalate clusters serve as monodentate ligands. The K(H2en)2[W3S7(C2O4)3]2Br·4H2O salt (3) was isolated from solutions containing CoII, NiII, or CuII aqua complexes and ethylenediamine. The reaction of [Mo3Se7(C2O4)3]2− with HBr produced the bromide complex [Mo3Se7Br6]2−, which was isolated as (Bu4N)2[Mo3Se7Br6] (4). Complexes 1–3 were characterized by X-ray diffraction, IR spectra, and elemental analysis. The formation of 4 was detected by electrospray mass spectrometry.
Dedicated to Academician G. A. Abakumov on the occasion of his 70th birthday.
Published in Russian in Izvestiya Akademii Nauk. Seriya Khimicheskaya, No. 9, pp. 1645–1649, September, 2007. 相似文献
18.
Among the various positive electrode materials investigated for Li-ion batteries, spinel LiMn2O4 is one of the most important materials. Small particles of the active materials facilitate high-rate capability due to large
surface to mass ratio and small diffusion path length. The present work involves the synthesis of submicron size particles
of LiMn2O4 in a quaternary microemulsion medium. The precursor obtained from the reaction is heated at different temperatures in the
range from 400 to 900 °C. The samples heated at 800 and 900 °C are found to possess pure spinel phase with particle size <200 nm,
as evidenced from XRD, SEM, and TEM studies. The electrochemical characterization studies provide discharge capacity values
of about 100 mAh g−1 at C/5 rate, and there is a moderate decrease in capacity by increasing the rate of charge–discharge cycling. Studies also
include charge–discharge cycling and ac impedance studies in temperature range from −10 to 40 °C. Impedance data are analyzed
with the help of an equivalent circuit and a nonlinear least squares fitting program. From temperature dependence of charge-transfer
resistance, a value of 0.62 eV is obtained for the activation energy of Mn3+/Mn4+ redox process, which accompanies the intercalation/deintercalation of the Li+ ion in LiMn2O4. 相似文献
19.
Eniko Berei Cornelia Muntean Oana Ştefănescu Mircea Niculescu Mircea Ştefănescu 《Journal of Thermal Analysis and Calorimetry》2018,131(1):137-144
CuCr2O4 spinel powders were synthesized starting from different chromium sources, namely (i) chromium oxide (α-Cr2O3) and (ii) ammonium dichromate ((NH4)2Cr2O7). The copper source was a Cu(II) carboxylate-type complex. The Cu(II) carboxylate complex was obtained by the redox reaction between Cu(NO3)2·3H2O and 1,3-propanediol (1,3PG) at 130 °C. In the first case (i), we have started from a mixture of α-Cr2O3, Cu(NO3)2·3H2O and 1,3PG that upon heating formed the copper malonate complex, which decomposed around 220 °C forming an oxide mixture (CuO + α-Cr2O3). In the second case (ii), (NH4)2Cr2O7, Cu(NO3)2·3H2O and 1,3PG were homogenously mixed. Heating this mixture at 130 °C resulted, in situ, in the Cu(II) complex. On controlled temperature increase, the violent decomposition of (NH4)2Cr2O7 took place at 180 °C along with the decomposition of the Cu(II) complex, leading to an amorphous oxide mixture of Cr2O3+x and CuO. By annealing the samples in the temperature range 400–1000 °C, the spinel phase (CuCr2O4) was obtained in both cases: (i) at 800 °C and (ii) at 600 °C as a result of the interactions between the precursors used, when the oxide system was amorphous and highly reactive. The presence of CuCr2O4 was highlighted by XRD and FTIR analyses. 相似文献
20.
L. S. Cavalcante J. C. Sczancoski F. S. De Vicente M. T. Frabbro M. Siu Li J. A. Varela E. Longo 《Journal of Sol-Gel Science and Technology》2009,49(1):35-46
Ba[Zr0.25Ti0.75]O3 (BZT) thin films were synthesized by the complex polymerization method and heat treated at 400 °C for different times and
at 700 °C for 2 h. These thin films were analyzed by X-ray diffraction (XRD), Fourier-transform infrared (FT-IR) spectroscopy,
field emission gun-scanning electron microscopy (FEG-SEM) and atomic force microscopy (AFM), Ultraviolet–visible (UV–vis)
absorption spectroscopy, electrical and photoluminescence (PL) measurements. FEG-SEM and AFM micrographs showed that the microstructure
and thickness of BZT thin films can be influenced by the processing times. Dielectric constant and dielectric loss of BZT
thin films heat treated at 700 °C were approximately 148 and 0.08 at 1 MHz, respectively. UV–vis absorption spectra suggested
the presence of intermediary energy levels (shallow and deep holes) within the band gap of BZT thin films. PL behavior was
explained through the optical band gap values associated to the visible light emission components. 相似文献