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1.
2CaO·3B2O3·H2O which has non-linear optical (NLO) property was synthesized under hydrothermal condition and identified by XRD, FTIR and
TG as well as by chemical analysis. The molar enthalpy of solution of 2CaO·3B2O3·H2O in HCl·54.572H2O was determined. From a combination of this result with measured enthalpies of solution of H3BO3 in HCl·54.501H2O and of CaO in (HCl+H3BO3) solution, together with the standard molar enthalpies of formation of CaO(s), H3BO3(s), and H2O(l), the standard molar enthalpy of formation of −(5733.7±5.2) kJ mol−1 of 2CaO·3B2O3·H2O was obtained. Thermodynamic properties of this compound were also calculated by a group contribution method. 相似文献
2.
N. I. Matskevich 《Journal of Thermal Analysis and Calorimetry》2007,90(3):955-958
Enthalpy of formation of the perovskite-related oxide BaCe0.9In0.1O2.95 has been determined at 298.15 K by solution calorimetry. Solution enthalpies of barium cerate doped with indium and mixture
of BaCl2, CeCl3, InCl3 in ratio 1:0.9:0.1 have been measured in 1 M HCl with 0.1 M KI. The standard formation enthalpy of BaCe0.9In0.1O2.95 has been calculated as −1611.7±2.6 kJ mol−1. Room-temperature stability of this compound has been assessed in terms of parent binary oxides. The formation enthalpy of
barium cerate doped by indium from the mixture of binary oxides is Δox
H
0 (298.15 K)=−36.2±3.4 kJ mol−1. 相似文献
3.
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
4.
Summary. Calcium sulfate occurs in nature in form of three different minerals distinguished by the degree of hydration: gypsum (CaSO4·2H2O), hemihydrate (CaSO4·0.5H2O) and anhydrite (CaSO4). On the one hand the conversion of these phases into each other takes place in nature and on the other hand it represents
the basis of gypsum-based building materials. The present paper reviews available phase diagram and crystallization kinetics
information on the formation of calcium sulfate phases, including CaSO4-based double salts and solid solutions.
Uncertainties in the solubility diagram CaSO4–H2O due to slow crystallization kinetics particularly of anhydrite cause uncertainties in the stable branch of crystallization.
Despite several attempts to fix the transition temperatures of gypsum–anhydrite and gypsum–hemihydrate by especially designed
experiments or thermodynamic data analysis, they still vary within a range from 42–60°C and 80–110°C. Electrolyte solutions
decrease the transition temperatures in dependence on water activity.
Dry or wet dehydration of gypsum yields hemihydrates (α-, β-) with different thermal and re-hydration behaviour, the reason
of which is still unclear. However, crystal morphology has a strong influence.
Gypsum forms solid solutions by incorporating the ions HPO4
2−, HAsO4
2−, SeO4
2−, CrO4
2−, as well as ion combinations Na+(H2PO4)− and Ln3+(PO4)3−. The channel structure of calcium sulfate hemihydrate allows for more flexible ion substitutions. Its ion substituted phases
and certain double salts of calcium sulfate seem to play an important role as intermediates in the conversion kinetics of
gypsum into anhydrite or other anhydrous double salts in aqueous solutions. The same is true for the opposite process of anhydrite
hydration to gypsum. Knowledge about stability ranges (temperature, composition) of double salts with alkaline and alkaline
earth sulfates (esp. Na2SO4, K2SO4, MgSO4, SrSO4) under anhydrous and aqueous conditions is still very incomplete, despite some progress made for the systems Na2SO4–CaSO4 and K2SO4–CaSO4–H2O.
Corresponding author. E-mail: daniela.freyer@chemie.tu-freiberg.de
Received December 17, 2002; accepted January 10, 2003
Published online April 3, 2003 相似文献
5.
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
6.
Matthias Weil Franz Werner Frank Kubel 《Monatshefte für Chemie / Chemical Monthly》2002,133(3):267-275
Summary. Single crystals of MgAl2F8(H2O)2 have been obtained under hydrothermal conditions (250°C, 14 d) from a starting mixture of AlF3 and MgAlF5(H2O)2 in a 5% (w/w) HF solution. The crystal structure has been determined and refined from single crystal data (Fmmm (#69), Z = 4, a = 7.2691(7), b = 7.0954(16), c = 12.452(2) ?, 281 structure factors, 27 parameters, R(F
2 > 2σ (F
2)) = 0.0282, wR(F
2 all) = 0.0885). The obtained crystals were systematically twinned according to (010/100/001) as twinning matrix, reflecting
the pseudo-tetragonal metric. The crystal structure is composed of perowskite-type layers built of corner sharing AlF6 octahedra with an overall composition of AlF4
− which are connected via common fluorine atoms of [MgF4/2(H2O)2/1] octahedra. Group-subgroup relations of MgAl2F8(H2O)2 to WO3(H2O)0.33 and to other M(II)M(III)2 F8(H2O)2 structures are briefly discussed. Above 570°C, MgAl2F8(H2O)2 decomposes under elimination of water into α-AlF3, β-AlF3, and MgF2.
Received October 29, 2001. Accepted (revised) December 6, 2001 相似文献
7.
Ji-min Yang Yan Yao Run-zhi Zhang Ai-de Sun Bao-hui Li Hong-zhi Lu Qi-ying Xia 《Journal of solution chemistry》2009,38(4):429-439
Osmotic coefficients and water activities for the Li2B4O7+LiCl+H2O system have been measured at T=273.15 K by the isopiestic method, using an improved apparatus. Two types of osmotic coefficients, φ
S and φ
E, were determined. φ
S is based on the stoichiometric molalities of the solute Li2B4O7(aq), and φ
E is based on equilibrium molalities from consideration of the equilibrium speciation into H3BO3,B(OH)4− and B3O3(OH)4−. The stoichiometric equilibrium constants K
m
for the aqueous speciation reactions were estimated. Two types of representations of the osmotic coefficients for the Li2B4O7+LiCl+H2O system are presented with ion-interaction models based on Pitzer’s equations with minor modifications: model (I) represents
the φ
S data with six parameters based on considering the ion-interactions between three ionic species of Li+, Cl−, and B4O72−, and model (II) for represents the φ
E data based on considering the equilibrium speciation. The parameters of models (I) and (II) are presented. The standard deviations
for the two models are 0.0152 and 0.0298, respectively. Model (I) was more satisfactory than model (II) for representing the
isopiestic data. 相似文献
8.
Nano-structured spinel Li2Mn4O9 powder was prepared via a combustion method with hydrated lithium acetate (LiAc·2H2O), manganese acetate (MnAc2·4H2O), and oxalic acid (C2H2O4·2H2O) as raw materials, followed by calcination of the precursor at 300 °C. The sample was characterized by X-ray diffraction,
scanning electron microscope, and energy-dispersive X-ray spectroscopy techniques. Electrochemical performance of the nano-Li2Mn4O9 material was studied using cyclic voltammetry, ac impedance, and galvanostatic charge/discharge methods in 2 mol L−1 LiNO3 aqueous electrolyte. The results indicated that the nano-Li2Mn4O9 material exhibited excellent electrochemical performance in terms of specific capacity, cycle life, and charge/discharge
stability, as evidenced by the charge/discharge results. For example, specific capacitance of the single Li2Mn4O9 electrode reached 407 F g−1 at the scan rates of 5 mV s−1. The capacitor, which is composed of activated carbon negative electrode and Li2Mn4O9 positive electrode, also exhibits an excellent cycling performance in potential range of 0–1.6 V and keeps over 98% of the
maximum capacitance even after 4,000 cycles. 相似文献
9.
A. D. Chervonnyi 《Russian Journal of Inorganic Chemistry》2010,55(4):556-559
The A1, O, AlO, A12O, Al2O2, WO2, and WO3, partial pressures in the vapor over Al2O3 in a tungsten Knudsen effusion cell between 2300 and 2600 K were derived from A1+, O+, AlO+, A12O+, Al2O2+, WO2+, and WO3+, ion intensities. The mass spectrometer was calibrated against the equilibrium constant of the WO3(g) = WO2(g) + O(g) reaction. Refined values of the ionization cross sections of AlO and A12O2 were used in the partial pressure calculations. The enthalpies of atomization of aluminum suboxides were determined to be
Δat
H
o(AlO, g, 0) = 510.7 ± 3.3 kJ mol−1, Δat
H
o(Al2O, g, 0) = 1067.2 ± 6.9 kJ mol−1, and Δat
H
o(Al2O2, g, 0) = 1556.7 ± 9.9 kJ mol−1. 相似文献
10.
I. E. Animitsa E. N. Dogodaeva S. S. Nokhrin O. A. Kosareva A. Ya. Neiman 《Russian Journal of Electrochemistry》2010,46(7):734-740
Perovskite phases Ba3In2ZrO8 and Ba4In2Zr2O11 with the nominal concentration of structural oxygen vacancies 1/9 and 1/12, respectively, were synthesized by solid-phase
and solution methods. X-ray diffraction showed cubic symmetry of both phases with the unit cell parameter a = 0.4193(2) and 0.4204(3) nm, respectively. The absence of superstructural lines resulted in the conclusion on statistical
arrangement of oxygen vacancies. Thermogravimetry and mass spectrometry proved that both phases can reversibly absorb water
from gas phase (pH2O = 2 × 10−2 atm) with observed correlation between the concentration of oxygen vacancies and amount of absorbed water. The total water
amount was up to 0.9 mol per formula unit or, if recalculated for perovskite unit ABO3, 0.3 and 0.23 mol H2O, respectively. The temperature curves of coductivity in the atmosphere with various partial water vapor pressures (pH2O = 3 × 10−5 and 2 × 10−2 atm) showed significantly higher conductivity and lower activation energy (0.52 eV) in humid atmosphere due to proton transfer.
The proton conductivity is up to 5 × 10−4 Ohm−1 cm−1 at 300°C for Ba3In2ZrO8 specimen. IR spectrometry showed that protons in the structure exist primarily in OH-groups. 相似文献
11.
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
12.
Ben Hui Wang Ji De Wang RuiQuan Liu Ya Hong Xie Zhi Jie Li 《Journal of Solid State Electrochemistry》2007,11(1):27-31
A new type of oxide–salt composite electrolyte, yttrium doped ceria YDC–Ca3(PO4)2–K3PO4, was developed and demonstrated for its promising use for ammonia synthesis. Using this composite electrolyte, ammonia was
synthesized from nitrogen and natural gas at atmospheric pressure in the solid-state proton conducting cell reactor, and the
optimal condition for ammonia production was determined . The evolved rate of ammonia is up to 6.95×10−9 mol s−1 cm−2. 相似文献
13.
Lanthanum chromite LaCrO3, an important catalyst and interconnect material used in solid oxide fuel cell was prepared from lanthanumtrisoxalatochromate(III)
hydrate [LaCr(C2O4)3]·9H2O (LTCR) employing microwave heating technique. The compound LTCR heated in microwave heating system gave pure LaCrO3 at 500°C within one hour. However LTCR heated in silicon carbide furnace yielded LaCrO3 at 900°C. BET surface area of LaCrO3 prepared by microwave and conventional heating techniques were found to be 2.8 and 1.2 m2 g−1, respectively. Thermogravimetry, differential thermal analysis and X-ray diffraction techniques were used to optimize the
conditions for the microwave processing of the precursor. 相似文献
14.
Imre Miklós Szilágyi Eero Santala Mikko Heikkilä Marianna Kemell Timur Nikitin Leonid Khriachtchev Markku Räsänen Mikko Ritala Markku Leskelä 《Journal of Thermal Analysis and Calorimetry》2011,105(1):73-81
This article demonstrates how important it is to find the optimal heating conditions when electrospun organic/inorganic composite
fibers are annealed to get ceramic nanofibers in appropriate quality (crystal structure, composition, and morphology) and
to avoid their disintegration. Polyvinylpyrrolidone [PVP, (C6H9NO)
n
] and ammonium metatungstate [AMT, (NH4)6[H2W12O40]·nH2O] nanofibers were prepared by electrospinning aqueous solutions of PVP and AMT. The as-spun fibers and their annealing were
characterized by TG/DTA-MS, XRD, SEM, Raman, and FTIR measurements. The 400–600 nm thick and tens of micrometer long PVP/AMT
fibers decomposed thermally in air in four steps, and pure monoclinic WO3 nanofibers formed between 500 and 600 °C. When a too high heating rate and heating temperature (10 °C min−1, 600 °C) were used, the WO3 nanofibers completely disintegrated. At lower heating rate but too high temperature (1 °C min−1, 600 °C), the fibers broke into rods. If the heating rate was adequate, but the annealing temperature was too low (1 °C min−1, 500 °C), the nanofiber morphology was excellent, but the sample was less crystalline. When the optimal heating rate and
temperature (1 °C min−1, 550 °C) were applied, WO3 nanofibers with excellent morphology (250 nm thick and tens of micrometer long nanofibers, which consisted of 20–80 nm particles)
and crystallinity (monoclinic WO3) were obtained. The FTIR and Raman measurements confirmed that with these heating parameters the organic matter was effectively
removed from the nanofibers and monoclinic WO3 was present in a highly crystalline and ordered form. 相似文献
15.
Xianru Pei Xiaodong Wang Shunli Zhang Jingwei Zhang Jianjun Yang Zhensheng Jin 《Frontiers of Chemistry in China》2007,2(3):265-269
Nanotube Li-Ti-O compound with high surface (198.6 m2·g−1) was prepared by a method involving the treatment of nanotube Na2Ti2O5·H2O in molten LiNO3 and characterization by means of transmission electron microscopy (TEM), energy-dispersive spectra (EDS), X-ray diffraction
(XRD), X-ray photoelectron spectroscopy (XPS), and thermogravimetry-differential thermal analysis (TG/DTG). Results show that
the nanotube Li-Ti-O compound prepared by this method involves two crystal phases: spinel Li2Ti2O4 and anatase LixTiO2 (x < 0.1). Li+ exhibits different Li1s binding energy in the two crystal phases. In ambient air, the Li-Ti-O compound adsorbs water easily,
and the chemically adsorbed water is difficult to remove below 400°C.
Translated from Chinese Journal of Inorganic Chemistry, 2006, 22(12): 2135–2139 [译自: 无机化学学报] 相似文献
16.
Xin Zhang Suqin Liu Kelong Huang Shuxin Zhuang Jun Guo Tao Wu Ping Cheng 《Journal of Solid State Electrochemistry》2012,16(3):937-944
The macroporous Li3V2(PO4)3/C composite was synthesized by oxalic acid-assisted carbon thermal reaction, and the common Li3V2(PO4)3/C composite was also prepared for comparison. These samples were characterized by X-ray diffraction (XRD), scanning electron
microscope (SEM), and electrochemical performance tests. Based on XRD and SEM results, the sample has monoclinic structure
and macroporous morphology when oxalic acid is introduced. Electrochemical tests show that the macroporous Li3V2(PO4)3/C sample has a high initial discharge capacity (130 mAh g−1 at 0.1 C) and a reversible discharge capacity of 124.9 mAh g−1 over 20 cycles. Moreover, the discharge capacity of the sample is still 91.5 mAh g−1, even at a high rate of 2 C, which is better than that of the sample with common morphology. The improvement in electrochemical
performance should be attributed to its improved lithium ion diffusion coefficient for the macroporous morphology, which was
verfied by cyclic voltammetry and electrochemical impedance spectroscopy. 相似文献
17.
Y. R. Zhao J. X. Dong Y. Liu S. S. Qu 《Journal of Thermal Analysis and Calorimetry》2007,90(2):565-568
The two complexes, [RE(Gly)4(Im)(H2O)](ClO4)3(s)(RE = Eu, Sm), have been synthesized and characterized. The standard molar enthalpies of reaction for the following reactions,
RECl3·6H2O(s)+4Gly(s)+Im(s)+3NaClO4(s) = =[RE(Gly)4(Im)(H2O)](ClO4)3(s)+3NaCl(s)+5H2O(l), were determined by solution-reaction colorimetry. The standard molar enthalpies of formation of the two complexes at
T = 298.15 K were derived as Δf
H
mΘ {Eu(Gly)4(Im)(H2O)}(ClO4)3(s)} = = −(3396.6±2.3) kJ mol−1 and Δf
H
mΘ {Sm(Gly)4(Im)(H2O)}(ClO4)3(s)} = −(3472.7±2.3) kJ mol−1, respectively. 相似文献
18.
R. G. Bulgakov Yu. G. Ponomareva Z. S. Muslimov F. G. Valyamova R. A. Sadykov R. F. Tuktarov 《Russian Chemical Bulletin》2007,56(2):211-219
Fullerenyl radicals (FR) RC60
· and chemiluminescence (CL) are generated in the presence of O2 in C60—R3Al (R = Et, Bui) solutions in toluene (T = 298 K). The FR are formed due to the addition of the R· radical, which is an intermediate of R3Al autooxidation, to C60. Mass spectroscopy and HPLC were used to identify EtnC60Hm (n, m = 1–6), EtpC60 (p = 2–6), and dimer EtC60C60Et as stable products of FR transformations. As found by ESR, the EtC60
· radical (g = 2.0037) is also generated by photolysis of solutions obtained after interaction in the (C60— R3Al)—O2 system. In the presence of dioxygen, the FR is not oxidized but yields complexes with O2, which appear as broadening of the ESR signals. Chemiluminescence arising in the (C60—R3Al)—O2 system is much brighter (I
max = 1.86·108 photon s−1 mL−1) than the known background CL (I
max = 6.0·106 photon s−1 mL−1) for the autooxidation of R3Al and is localized in a longer-wavelength spectral region (λmax = 617 and 664 nm). This CL is generated as a result of energy transfer from the primary emitter 3CH3CHO* to the products of FR transformation: RnC60Hm, RpC60, and EtC60C60Et.
Published in Russian in Izvestiya Akademii Nauk. Seriya Khimicheskaya, No. 2, pp. 205–213, February, 2007. 相似文献
19.
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
20.
采用水合前驱物分解的方法, 以钨酸铵、钼酸铵及硝酸氧锆为原料制备了不同形貌的ZrWMoO8粉体. 对其前驱体进行了热重-差热分析(TG-DSC), 并以X射线粉末衍射(XRD)、扫描电子显微镜(SEM)及X射线荧光光谱仪(XRF)等手段考察了不同胶凝剂(HCl, HClO4, HNO3, H2SO4及H3PO4)对产物结构和形貌的影响. 结果表明, 胶凝剂的选择对ZrWMoO8粉体的形貌有较大影响. 在100—700 ℃范围内, 以HCl为胶凝剂制备出来的立方相ZrWMoO8粉体的热膨胀系数为-3.84×10-6 K-1. 相似文献