共查询到20条相似文献,搜索用时 125 毫秒
1.
M. Arshad A. H. Qureshi K. Masud N. K. Qazi 《Journal of Thermal Analysis and Calorimetry》2007,89(2):595-600
The production of bulk high T
c superconducting phase (2223) by EDTA-gel (ethylenediaminetetraacetic acid) techniques has been investigated. It is shown
that close control of pH is necessary for the production of a well-complexed precursor which allows subsequent decomposition
in two stages at 300 and 800°C. The problem of carbonate formation was investigated experimentally and solved. Precursors
are characterised by Fourier transform infrared (FTIR) spectroscopy and X-ray diffraction (XRD) and the sintering behaviour
was monitored by dilatometry. At least three different phases Bi2Sr2Cax−1CuxO8+y (BSCCO); where x=1, 2, 3 were identified within superconducting pellets using XRD, named as Bi2Sr2CuO7 (2201), Bi2Sr2CaCu2O9 (2212) and Bi2Sr2Ca3O10 (2223). The superconducting properties of the sintered samples were studied by vibrating sample magnetometer (VSM). Transition
to a superconducting state around 80 K appeared in samples (sintered at 845°C) containing the Bi2Sr2Ca1Cu2Oy (2212) phase. Liquid phase sintering of the samples aided the formation of Bi2Sr2Ca2Cu3Ox (2223) phase at high temperature (860°C), which showed a superconducting transition temperature of 108 K. 相似文献
2.
Žaneta Dohnalová Petra Šulcová Miroslav Trojan 《Journal of Thermal Analysis and Calorimetry》2010,101(3):973-978
The main aim of this work was to synthesize the magnesium orthostannate doped by terbium cations and tested whether these
materials can be used for colouring of the different materials, e.g. organic binder and ceramic glazes. Initial composition
of pigments was counted according the general formula 2MgO(1 − x)SnO2–xTbO2, where values of x varied from 0.1 to 0.5 in 0.1 steps. The simultaneous TG/DTA measurements of mixture containing tin oxide, magnesium carbonate
hydroxide and terbium oxide showed that the formation of a new compound started at temperature 1,029 °C, but single-phase
system was not prepared. Granulometric compositions of samples that were prepared by calcining at temperatures 1,300–1,400 °C
are characterized by values of median (d
50) in range 4–8 μm. The calcining temperature 1,500 °C caused the increase of the particle sizes at around 12 μm. The composition
of sample 2MgO–1.5SnO2–0.5TbO2 and heating temperature 1,500 °C are the most suitable conditions for preparation of colourfully interesting pigment that
can be recommended also for colouring of ceramic glazes. Especially, for colouring of decorative lead containing glaze G 07091
containing 5 wt% of PbO and 8 wt% of Al2O3. 相似文献
3.
M. Boča V. Danielik Z. Ivanová E. Mikšíková B. Kubíková 《Journal of Thermal Analysis and Calorimetry》2007,90(1):159-165
The phase diagrams of the systems KF-K2TaF7 and KF-Ta2O5 were determined using the thermal analysis method. The phase diagrams were described by suitable thermodynamic model. In
the system KF-K2TaF7 eutectic points at x
KF=0.716 and t=725.4°C and at x
KF=0.214 and t=712.2°C has been calculated. It was suggested that K2TaF7 melts incongruently at around 743°C forming two immiscible liquids. The system KF-Ta2O5 have been measured up to 8 mol% of Ta2O5. The eutectic point was estimated to be at x
KF∼0.9 and t∼816°C. The formation of KTaO3 and K3TaO2F4 compounds has been observed in the solidified samples. 相似文献
4.
The effect of fluorine doping on the electrochemical performance of LiFePO4/C cathode material is investigated. The stoichiometric proportion of LiFe(PO4)1−x
F3x
/C (x = 0.01, 0.05, 0.1, 0.2) materials was synthesized by a solid-state carbothermal reduction route at 650 °C using NH4F as dopant. X-ray diffraction, scanning electron microscope, energy-dispersive X-ray, and X-ray photoelectron spectroscopy
analyses demonstrate that fluorine can be incorporated into LiFePO4/C without altering the olivine structure, but slightly changing the lattice parameters and having little effect on the particle
sizes. However, heavy fluorine doping can bring in impurities. Fluorine doping in LiFePO4/C results in good reversible capacity and rate capability. LiFe(PO4)0.95 F0.15/C exhibits highest initial capacity and best rate performance. Its discharge capacities at 0.1 and 5 C rates are 156.1 and
119.1 mAh g−1, respectively. LiFe(PO4)0.95 F0.15/C also presents an obviously better cycle life than the other samples. We attribute the improvement of the electrochemical
performance to the smaller charge transfer resistance (R
ct) and influence of fluorine on the PO43− polyanion in LiFePO4/C. 相似文献
5.
K. Suryakala K. R. Marikkannu G. Paruthimal Kalaignan T. Vasudevan 《Journal of Solid State Electrochemistry》2007,11(12):1671-1677
LiMn2O4-based spinels are of great interest as positive electrode materials for lithium ion batteries. LiCo
x
Mn2−x
O4 (x = 0.0, 0.1, 0.2, 0.3, and 0.4) spinel phases have been synthesized by novel citric acid-modified microwave-assisted sol–gel
method. The structural properties of the synthesized products have been investigated by X-ray powder diffraction and scanning
electron microscopy. To improve the recharge capacity of Li/LiCo
x
Mn2−x
O4 cells, the electrochemical features of LiCo
x
Mn2−x
O4 compounds have been evaluated as positive electrode materials. The structural properties of Co-doped oxides are very similar
to LiMn2O4 electrode. Techniques like cyclic voltammetry, charge–discharge and cycle life are also used to characterize the LiCo
x
Mn2−x
O4 (x = 0.0, 0.1, 0.2, 0.3, and 0.4) electrodes. 相似文献
6.
Tatiana Nedoseykina Pavel Plyusnin Yuri Shubin Sergey Korenev 《Journal of Thermal Analysis and Calorimetry》2010,102(2):703-708
Thermolysis of double complex salt [Pd(NH3)4][AuCl4]2 has been studied in helium atmosphere from ambient to 350 °C. The XAFS of Pd K and Au L3 edges and thermogravimetry measurements have been carried out to characterize the intermediates and the final product. In
the temperature range 115–160 °C the complex is decomposed to form Pd(NH3)2Cl2 and AuCl4−x
N
x
species with x ranging from 2 to 3. Subsequent heating of the intermediate up to 300 °C leads to the total loss of NH3. The Au–Cl and Au–Au bonds form the local environment of Au at the stage of decomposition while only four chlorine atoms
are around Pd. At the temperature of 330 °C the Au and Pd nanoparticles as well as residues of palladium chloride are detected.
The final product consists of separated Au and Pd nanoparticles. 相似文献
7.
T. I. Krasnenko M. V. Rotermel’ S. A. Petrova R. G. Zakharov O. V. Sivtsova A. N. Chvanova 《Russian Journal of Inorganic Chemistry》2008,53(10):1641-1647
Phase relations in the Zn2V2O7-Cu2V2O7 system were studied by high-temperature X-ray diffraction and differential thermal analysis. The major phase constituents
of the system are solid solutions based on Zn2V2O7 and Cu2V2O7 polymorphs and their coexistence regions. The generation of α-Zn2 − 2x
Cu2x
V2O7 solid solution, where 0 ≤ x ≤ 0.30, leaves almost unchanged the stabilization temperature of the high-temperature zinc pyrovanadate phase. The α-Cu2 − 2x
Zn2x
V2O7 homogeneity range is 5 mol % Zn2V2O7. In the range 0.050 ≤ x ≤ 0.09 from 20 to ∼ 620°C, there is the two-phase field of α-Cu2V2O7 and β-Cu2V2O7 base solid solutions. At still higher temperatures, β-Zn2 − 2x
Cu2x
V2O7 and α-Cu2 − 2x
Zn2x
V2O7 coexist in the mixed-phase region. β-Zn2 − 2x
Cu2x
V2O7 solid solution, where 0 ≤ x ≤ 0.30, exists above 610 ± 5°C. The extent of the β′-Cu2V2O7-base solid solution is 9 to 65 mol % Zn2V2O7 at 615 ± 5°C, expanding to 0 mol % Zn2V2O7 with rising temperature.
Original Russian Text ¢ T.I. Krasnenko, M.V. Rotermel’, S.A. Petrova, R.G. Zakharov, O.V. Sivtsova, A.N. Chvanova, 2008, published
in Zhurnal Neorganicheskoi Khimii, 2008, Vol. 53, No. 10, pp. 1755–1762. 相似文献
8.
Deuk Yong Lee Kyong-Ho Lee Myung-Hyun Lee Nam-Ihn Cho Bae-Yeon Kim 《Journal of Sol-Gel Science and Technology》2010,53(1):43-49
Ba1−x
Sr
x
TiO3(x = 0–0.5, BST) nanofibers with diameters of 150–210 nm were prepared by using electrospun BST/polyvinylpyrrolidone (PVP) composite
fibers by calcination for 2 h at temperatures in the range of 650–800 °C in air. The morphology and crystal structure of calcined
BST/PVP nanofibers were characterized as functions of calcination temperature and Sr content with an aid of XRD, FT-IR, and
TEM. Although several unknown XRD peaks were detected when the fibers were calcined at temperatures less than 750 °C, they
disappeared with increasing the temperature (above 750 °C) due to its thermal decomposition and complete reaction in the formation
of BST. In addition, the FT-IR studies of BST/PVP fibers revealed that the intensities of the O–H stretching vibration bands
(at 3430 and 1425 cm−1) became weaker with increasing the calcination temperature and a broad band at 540 cm−1, Ti–O vibration, appeared sharper and narrower after calcination above 750 °C due to the formation of metal oxide bonds.
However, no effect of Sr content on the crystal structure of the composites was detected. 相似文献
9.
YBaCo4O7 compound is capable to intake and release a large amount of oxygen in the temperature range of 200–400°C. In the present
study, the effect of Zn, Ga and Fe substitution for Co on the oxygen adsorption/desorption properties of YBaCo4O7 were investigated by thermogravimetry (TG) method. Due to fixed oxidation state of Zn2+ ions, the substitution of Zn2+ for Co2+ suppresses the oxygen adsorption of YBaCo4−xZnxO7. The substitution of Ga3+ for Co3+ also decreases the oxygen absorption capacity of YBaCo4−xGaxO7. This can be explained by the strong affinity of Ga3+ ions towards the GaO4 tetrahedron. Compared with Zn- and Ga-substituted samples, the drop of oxygen adsorption capacity is smallest for Fe-substituted
samples because of the similar changeability of oxidation states of Co and Fe ions. 相似文献
10.
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
11.
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
12.
L. A. Isupova E. Yu. Gerasimov V. I. Zaikovskii S. V. Tsybulya N. A. Kulikovskaya N. F. Saputina 《Kinetics and Catalysis》2009,50(6):886-891
Homogeneous La1 − x
Ca
x
MnO3 solid solutions have been synthesized by the Pechini method (using polymer-solid compositions). Their microstructure, stability
at high temperatures, and catalytic activity in methane oxidation are reported. A continuous series of solid solutions stable
in air up to 1100°C forms in the system, and the particle surface is enriched with calcium. A distinctive microstructural
feature of the particles is their microporosity. The catalytic activity of all calcium-containing samples (except for x = 0.7) below 700°C is lower than that of lanthanum manganite and decreases under the action of the reaction medium, which
can be due to the decrease in the amount of weakly bound oxygen on the surface because of the enrichment of the surface with
calcium and the formation of strongly bound surface carbonates. The higher activity and stability of the La0.3Ca0.7MnO3 sample (calcined at 1100°C) above 500°C can be due to the formation of nanosized areas with an Mn3O4 structures on the perovskite particle surface in the reaction medium. 相似文献
13.
Thermal behaviour of the glass series (100-x)[50ZnO-10B2O3-40P2O5]·xSb2O3 (x=0-42 mol%) and (100-y)[60ZnO-10B2O3-30P2O5]·ySb2O3 (y=0-28 mol%) was investigated by DSC and TMA. The addition of Sb2O3 results in a decrease of the glass transition temperature and crystallization temperature in both compositional series. All
glasses crystallize on heating in the temperature range of 522–632°C. Thermal expansion coefficient of the glasses monotonously
increases with increasing Sb2O3 content in both series and varies within the range of 6.6–11.7 ppm °C−1. From changes of thermal capacity within the glass transition region it was concluded that with increasing Sb2O3 content the ‘fragility’ of the studied glasses increases. 相似文献
14.
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
15.
Huaibing Sun Yungui Chen Chenghao Xu Ding Zhu Lihong Huang 《Journal of Solid State Electrochemistry》2012,16(3):1247-1254
Spinel powders of LiMn2−x
RE
x
O4 (RE = La, Ce, Nd, Sm; 0 ≤ x ≤ 0.1) have been synthesized by solid-phase reaction. The structure and electrochemical properties of these electrode materials
were characterized by X-ray diffraction (XRD), cyclic voltammetry (CV), electrochemical impedance spectroscopy (EIS) and charge–discharge
experiment. The part substitution of rare-earth element RE for Mn in LiMn2O4 decreases the lattice parameter, resulting in the improvement of structural stability, and decreases the charge transfer
resistance during the electrochemical process of LiMn2O4. As a result, the cycle ability, 55 °C high-temperature and high-rate performances of LiMn2−x
RE
x
O4 electrode materials are significantly improved with increasing RE addition, compared to the pristine LiMn2O4. 相似文献
16.
J. Yao K. Konstantinov G. X. Wang H. K. Liu 《Journal of Solid State Electrochemistry》2007,11(2):177-185
A series of lithium iron phosphates was synthesized via the sol–gel route. Iron phosphides, which are electronic conductors, were formed when sintered at 850°C. Magnetic susceptibility measurements on the samples show antiferromagnetic behaviour with T
N=50±2 K for LiFePO4 and Li0.95Mg0.05PO4 sintered at temperatures below 850°C. The LiFePO4 and Li0.95Mg0.05FePO4 cathodes show a stable electrochemical capacity in the range of 150–160 mA h/g on cycling. The cyclability deteriorates with increasing sample sintering temperature due to the increased crystal size and impurities. 相似文献
17.
J. Dailly F. Mauvy M. Marrony M. Pouchard Jean-Claude Grenier 《Journal of Solid State Electrochemistry》2011,15(2):245-251
Three selected materials have been prepared and shaped as cathode of half cells using the proton-conducting electrolyte BaCe0.9Y0.1O3 − δ
(BCY10): two perovskite compounds, Ba0.5Sr0.5Co0.8Fe0.2O3 − δ
(BSCF) and La0.6Sr0.4Fe0.8Co0.2O3 − δ
(LSFC), and the praseodymium nickelate Pr2NiO4 + δ
(PRN) having the K2NiF4-type structure. The electrochemical properties of these compounds have been studied under zero current conditions (two-electrode
cell) and under polarization (three-electrode cell). Their measured area-specific resistances were about 1–2 Ω cm2 at 600 °C. Under direct current polarization, it appears that the three compounds show almost similar values of current densities
at 625 °C; however, at lower temperatures, BSCF appears to be the most efficient cathode material. 相似文献
18.
S. -X. Wang Z. -C. Tan Y. -S. Li L. -X. Sun Y. Li 《Journal of Thermal Analysis and Calorimetry》2008,92(2):483-487
Synthesis, characterization and thermal analysis of polyaniline (PANI)/ZrO2 composite and PANI was reported in our early work. In this present, the kinetic analysis of decomposition process for these
two materials was performed under non-isothermal conditions. The activation energies were calculated through Friedman and
Ozawa-Flynn-Wall methods, and the possible kinetic model functions have been estimated through the multiple linear regression
method. The results show that the kinetic models for the decomposition process of PANI/ZrO2 composite and PANI are all D3, and the corresponding function is ƒ(α)=1.5(1−α)2/3[1−(1-α)1/3]−1. The correlated kinetic parameters are E
a=112.7±9.2 kJ mol−1, lnA=13.9 and E
a=81.8±5.6 kJ mol−1, lnA=8.8 for PANI/ZrO2 composite and PANI, respectively. 相似文献
19.
Ca3Co4O9 powder was prepared by a polyacrylamide gel route in this paper. The effect of the processing on microstructure and thermoelectric
properties of Ca3Co4O9 ceramics via spark plasma sintering were investigated. Electrical measurement shows that the Seebeck coefficient and conductivity
are 170 μV/K and 128 S/cm, respectively, at 700 °C, yielding a power factor value of 3.70 × 10−4 W m−1 K−2 at 700 °C, which is larger than that of Ca3Co4O9 ceramics via solid-state reaction processing. The polyacrylamide gel processing is a fast, cheap, reproducible and easily
scaled up chemical route to improve the thermoelectric properties of Ca3Co4O9 ceramics by preparing the homogeneous and pure Ca3Co4O9 phase. 相似文献
20.
A. N. Mansurova R. I. Gulyaeva V. M. Chumarev V. P. Mar’evich 《Journal of Thermal Analysis and Calorimetry》2010,101(1):45-47
Homogeneous manganocolumbite (MnNb2O6) was synthesized from Nb2O5 and MnO oxides. Powder sample was orthorhombic with unit cell parameters: α = 0.5766 nm, b = 1.4439 nm, c = 0.5085 nm and V = 0.4234 nm3. Heat capacity over the temperature range of 313–1253 K was measured in an inert atmosphere with combined thermogravimetry
and calorimetry using NETZSCH STA 449C Jupiter thermoanalyzer. Melting point was 1767 ± 3 K, enthalpy of melting was 144 ± 4 kJ mol−1. Experimental heat capacity of MnNb2O6 is fitted to polynomial C
pm = 221.46 + 3.03 · 10−3 T + −39.79 · 105 T
−2 + 40.59 · 10−6 T
2. 相似文献