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1.
Additives to MgB2 can improve the superconducting functional characteristics, such as critical current density (J c) and irreversibility field (H irr). Recently, we have shown that repagermanium (C6H10Ge2O7) is an effective additive, enhancing both J c and H irr. To look into details of the processes taking place during the reactive sintering, a thermal analysis study (0.167 K s?1, in Ar) is reported. We used differential scanning calorimetry between 298 and 863 K and simultaneous thermogravimetric—differential thermal analysis between 298 and 1233 K. Samples were mixtures of powders with composition 97 mol% MgB2 and 3 mol% C6H10Ge2O7. Up to 863 K, repagermanium decomposes by multiple steps and forms amorphous phases. A reaction with MgB2 is not observed. Above this temperature, partial decomposition of MgB2 occurs. Crystalline Ge and MgO are detected before formation of Mg2Ge and MgB4, when temperature approaches the melting point of Ge (1211 K). Carbon substitution for boron in the crystal lattice of MgB2 is observed for samples heated above 863 K. The amount of substitutional C does not significantly change with temperature.  相似文献   

2.
A novel photocatalytic material (Pt,Cd0.8Zn0.2S)/HLaNb2O7 was fabricated by successive intercalation and exchange reactions. The (Pt,Cd0.8Zn0.2S)/HLaNb2O7 possessed a gallery height less than 0.5 nm and showed a broad absorption with wavelength over 370-500 nm. Using (Pt,Cd0.8Zn0.2S)/HLaNb2O7 as catalyst, the photocatalytic H2 evolution was more than 160 cm3·h-1·g-1 in the presence of Na2S as a sacrificial agent under irradiation with wavelength more than 290 nm from a 100-W mercury lamp. Furthermore, the catalyst showed photocatalytic activity even under visible light irradiation.  相似文献   

3.
A H3PW12O40/ZrO2 catalyst for effective dimethyl carbonate (DMC) formation via methanol carbonation was prepared using the sol–gel method. X-ray photoelectron spectra showed that reactive and dominant (63%) W(VI) species, in WO3 or H2WO4, enhanced the catalytic performances of the supported ZrO2. The mesoporous structure of H3PW12O40/ZrO2 was identified by nitrogen adsorption–desorption isotherms. In particular, partial sintering of catalyst particles in the duration of methanol carbonation caused a decrease in the Brunauer–Emmett–Teller surface area of the catalyst from 39 to 19 m2/g. The strong acidity of H3PW12O40/ZrO2 was confirmed by the desorption peak observed at 415 °C in NH3 temperature-programmed desorption curve. At various reaction temperatures (T?=?110, 170, and 220 °C) and CO2/N2 volumetric flow rate ratios (CO2/N2?=?1/4, 1/7, and 1/9), the calculated catalytic performances showed that the optimal methanol conversion, DMC selectivity, and DMC yield were 4.45, 89.93, and 4.00%, respectively, when T?=?170 °C and CO2/N2?=?1/7. Furthermore, linear regression of the pseudo-first-order model and Arrhenius equation deduced the optimal rate constant (4.24?×?10?3 min?1) and activation energy (Ea?=?15.54 kJ/mol) at 170 °C with CO2/N2?=?1/7 which were favorable for DMC formation.  相似文献   

4.
In this study, an ionic complex of V(V) was synthesized by using ultrasonic method, and it was used as a precursor for production of a new catalyst for selective preparation of methylal or dimethoxymethane (DMM). By reaction between an ionic ligand [pyda.H2]2+[pydc]2? (LH2), (pyda.H2 = 2,6-pyridine diammonium and pydc = 2,6-pyridinedicarboxylate) and ammonium vanadate, the five coordinated V(V) complex, [pyda.H][V(pydc)O2], {2,6- diaminopyridinum 2,6-pyridinedicarboxylatodioxovanadate(V)}, VLH2 was synthesized. The prepared complex VLH2 was characterized by SEM, thermal analysis TGA/DTA, FT-IR spectroscopy and X-ray diffraction studies. The results showed that the yield of the reaction was increased up to 64%. The average particle sizes of the obtained complex VLH2 were about 50–60 nm. Also, the nano-catalyst of V2O5/Al2O3 was synthesized by impregnation method and was prepared as a nano-catalyst with average particles sizes of 50–60 nm, and its characterization was performed by XRD, EDX and SEM methods. Finally, the prepared catalyst was used to converting of methanol to methylal at different process conditions.  相似文献   

5.
A new reduced ferrous molybdophosphate composite solid of the formula, [(C10H14N2)H]4[FeII 10MoV 24(H2PO4)4(HPO4)12(PO4)4(H2O)16(OH)16O44]·12H2O, has been synthesized from a reaction mixture of MoO3, FeSO4·7H2O, C2H2O4·2H2O, nicotine, H3PO4, and H2O under hydrothermal conditions. The crystal data: monoclinic, space group C2/m, a = 24.4349(124), b = 12.9935(66), c = 14.7281(74) Å, β = 104.87(1) Å, V = 4520(4) Å3, Z = 2, R 1  = 0.0874, wR 2  = 0.2179. The structure is built from the building blocks of the formula, {FeII[Mo6P4O31]2}, consisting of a network of MO6 (M = Fe, Mo) octahedral and PO4 tetrahedral linked through their vertices. The connectivity of the building blocks with two pairs of face-sharing dinuclear Fe(II) clusters of the formula of [FeII 2(H2O)4O5] on which a phosphate group is hanging gives rise to one-dimensional chains with eight-membered apertures. The remarkable hydrogen bonded interactions between the chains form a unique and interesting framework with three-dimensional intersecting tunnels where the protonated nicotine molecules as structuring templates and crystallization water molecules are situated.  相似文献   

6.
Neodymium(III) peroxotitanate is used as a precursor for obtaining Nd2TiO5. The last one possesses numerous valuable electrophysical properties. TiCl4, Nd(NO3)3·6H2O and H2O2 in mol ratio 1:2:10 were used as starting materials. The reaction ambience was alkalized to pH = 9 with a solution of NH3. The obtained neodymium(III) peroxotitanate and intermediate compounds of the isothermal heating were proved by the help of quantitative analysis and infrared spectroscopy (IRS). It has Nd4[Ti2(O2)4(OH)12]·7H2O composition. The absorption band observed in IRS at 831 cm?1 relates to a triangular bonding of the peroxo group of Ti, at 1062 cm?1—terminal groups Ti–OH and at 1491 and 1384 cm?1—the bridging OH?-groups Ti–O(H)–Ti. Nd2TiO5 was obtained by thermal decomposition of neodymium(III) peroxotitanate. The isothermal conditions for decomposition were determined on the base of differential thermal analysis, thermogravimetric and differential scanning calorimetry results in the temperature range of 20–1000 °C. The mechanism of thermal decomposition of Nd4[Ti2(O2)4(OH)12]·7H2O to Nd2TiO5 was studied. In the temperature range of 20–208 °C, a simultaneous decomposition of the peroxo groups by the separation of oxygen and hydrate water is conducted and Nd4[Ti2O4(OH)12] is obtained. From 208 to 390 °C, the terminal OH?-groups are separated and Nd4[Ti2O7(OH)6] is formed. In the range of 390–824 °C, the bridging OH?-groups are completely decomposed to Nd2TiO5. The optimal conditions for obtaining nanocrystalline Nd2TiO5 are 900 °C for 6 h and 20–80 nm.  相似文献   

7.
The authors report on the preparation of a hollow-structured cobalt ferrite (CoFe2O4) nanocomposite for use in a non-enzymatic sensor for hydrogen peroxide (H2O2). Silica (SiO2) nanoparticles were exploited as template for the deposition of Fe3O4/CoFe2O4 nanosheets, which was followed by the removal of SiO2 template under mild conditions. This leads to the formation of hollow-structured Fe3O4/CoFe2O4 interconnected nanosheets with cubic spinel structure of high crystallinity. The material was placed on a glassy carbon electrode where it acts as a viable sensor for non-enzymatic determination of H2O2. Operated at a potential of ?0.45 V vs. Ag/AgCl in 0.1 M NaOH solution, the modified GCE has a sensitivity of 17 nA μM?1 cm?2, a linear response in the range of 10 to 1200 μM H2O2 concentration range, and a 2.5 μM detection limit. The sensor is reproducible and stable and was applied to the analysis of spiked urine samples, where it provided excellent recoveries.
Graphical abstract Schematic of a cobalt ferrite (CoFe2O4) hollow structure for use in electrochemical determination of H2O2. The sensor shows a low detection limit, a wide linear range, and excellent selectivity for H2O2.
  相似文献   

8.
In the current study, a nanophotocatalyst doped with of TiO2 and Fe2O3 nanoparticles supported on Iranian clinoptilolite was synthesized and characterized by XRD, XRF, SEM, and EDX analyses. The results suggested the successful loading of TiO2 and Fe2O3 nanoparticles onto the surface of clinoptilolite. The SEM images confirmed the average size of nanoparticles deposited on zeolite, which was about 20–40 nm. Furthermore, application of the synthesized photocatalyst in photocatalytic degradation of Acid Black 172 dye was studied using the Taguchi method and the chosen parameters were as follows: pH (2–7), dye concentration (50–200 mg/l), irradiation time (30–120 min), and catalyst dosage (0.5–1.5 g/l). The results indicate that dye concentration, pH, and irradiation time are respectively the most effective factors in these experiments while with the minimum dosage of the catalyst (0.5 g/l), up to 90 % removal efficiency could be achieved. The optimum value for each parameter was pH = 2, dye concentration = 50 mg/l, catalyst dosage = 1 g/l and irradiation time = 60 min, and the dye removal efficiency reached up to 100 % at these optimal conditions. Furthermore, after five-times recycling and reusing the catalyst, the efficiency of the photocatalytic degradation was reduced from 91.5 to 65.9 %, which is still an acceptable value.  相似文献   

9.
Ce2Sn2O7 pyrochlore was synthesized by a hydrothermal method. X-ray powder diffraction (XRD) and X-ray photoelectron spectroscopy (XPS) were used to characterize the composition and valence state of the sample. The oxygen exchange property of the Ce2Sn2O7 phase was measured by an oxidation reaction in sealed air atmosphere and a followed reduction reaction in 5% H2-95% N2 atmosphere. Gas chromatography (GC) was used to analyze the oxygen change in the reaction. The results show that Ce2Sn2O7 sample has excellent oxygen absorption capacity at 250°C as Ce3+ ions are oxidized to Ce4+ ions. The oxidized sample can be reduced by 5% H2-95% N2. The refreshed sample remains the capacity of oxygen absorption, while the oxygen exchange capacity degrades with the reduction times.  相似文献   

10.
11.
Fe@Fe2O3 core-shell nanowires were synthesized via the reduction of Fe3+ ions by sodium borohydride in an aqueous solution with a subsequent heat treatment to form Fe2O3 shell and employed as a cathode catalyst for non aqueous Li-air batteries. The synthesized core-shell nanowires with an average diameter of 50–100 nm manifest superior catalytic activity for oxygen evolution reaction (OER) in Li-O2 batteries with the charge voltage plateau reduced to ~3.8 V. An outstanding performance of cycling stability was also achieved with a cutoff specific capacity of 1000 milliampere hour per gram over 40 cycles at a current density of 100 mA g?1. The excellent electrochemical properties of Fe@Fe2O3 as an O2 electrode are ascribed to the high surface area of the nanowires’ structure and high electron conductivity. This study indicates that the resulting iron-containing nanostructures are promising catalyst in Li-O2 batteries.  相似文献   

12.
The removal of hydrogen sulfide and dust simultaneously by the DC corona discharge plasma with a wire-cylinder reactor was studied at atmospheric pressure and room temperature. The outlet gases were analyzed by Fourier Transform Infrared. Chemical compositions of the dust collected from ground electrode were analyzed by X-ray fluorescence. The results showed that the DC corona discharge is effective in removing H2S and dust simultaneously. The best H2S conversion was gained with the 2 cm discharge gap. The lower inlet H2S concentration, the higher conversion efficiency was gained at any specific input energy (SIE), while the energy yield was on the contrary. The removal efficiency of H2S decreased gradually as oxygen concentration increased, which means that the H2S decomposition mainly depends on direct electron collisions or short-living species, such as·O, ·OH radicals in the non-thermal plasma. At the initial stage, the conversion efficiency of H2S increased with the increasing of relative humidity, but later decreased while the relative humidity keep increasing with the same SIE. Existing of dust can not only reduce the energy consumption of H2S conversion and improve the removal efficiency, but also inhibit the yield of SO2 for it can further react with some compounds in the dust. With the discharge gap of 2 cm, inlet H2S concentration of 2400 ppm, O2 Of 0.5 %, relative humidity of 41 %, dust content of 4000 ± 5 % mg/m3 and SIE of 600 J/L, the H2S conversion reached 98.8 %, and the dust removal efficiency was close to 100 %.  相似文献   

13.
The non-isothermal decomposition kinetics of 4Na2SO4·2H2O2·NaCl have been investigated by simultaneous TG-DSC in nitrogen atmosphere and in air. The decomposition processes undergo a single step reaction. The multivariate nonlinear regression technique is used to distinguish kinetic model of 4Na2SO4·2H2O2·NaCl. Results indicate that the reaction type Cn can well describe the decomposition process, the decomposition mechanism is n-dimensional autocatalysis. The kinetic parameters, n, A and E are obtained via multivariate nonlinear regression. The n th-order with autocatalysis model is used to simulate the thermal decomposition of 4Na2SO4·2H2O2·NaCl under isothermal conditions at various temperatures. The flow rate of gas has little effect on the decomposition of 4Na2SO4·2H2O2·NaCl.  相似文献   

14.
Chemical preparation, crystal structure, and NMR spectroscopy of a new trans-2,5-dimethylpiperazinium monophosphate are given. This new compound crystallizes in the triclinic system, with the space group P-1 and the following parameters: a = 6.5033(3), b = 7.6942(4), c = 8.1473(5) Å, α = 114.997(3), β = 92.341(3), γ = 113.136(3), V = 329.14(3) Å3, Z = 1, and Dx = 1.565 g cm?3. The crystal structure has been determined and refined to R = 0.030 and R w(F 2) = 0.032 using 1558 independent reflections. The structure can be described as infinite [H2PO4] n n? chains with (C6H16N2)2+ organic cations anchored between adjacent polyanions to form columns of anions and cations running along the b axis. This compound has also been investigated by IR, thermal, and solid-state, 13C and 31P MAS NMR spectroscopies and Ab initio calculations.  相似文献   

15.
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   

16.
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   

17.
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   

18.
Li4Ti5O12/Li2TiO3 composite nanofibers with the mean diameter of ca. 60 nm have been synthesized via facile electrospinning. When the molar ratio of Li to Ti is 4.8:5, the Li4Ti5O12/Li2TiO3 composite nanofibers exhibit initial discharge capacity of 216.07 mAh g?1 at 0.1 C, rate capability of 151 mAh g?1 after being cycled at 20 C, and cycling stability of 122.93 mAh g?1 after 1000 cycles at 20 C. Compared with pure Li4Ti5O12 nanofibers and Li2TiO3 nanofibers, Li4Ti5O12/Li2TiO3 composite nanofibers show better performance when used as anode materials for lithium ion batteries. The enhanced electrochemical performances are explained by the incorporation of appropriate Li2TiO3 which could strengthen the structure stability of the hosted materials and has fast Li+-conductor characteristics, and the nanostructure of nanofibers which could offer high specific area between the active materials and electrolyte and shorten diffusion paths for ionic transport and electronic conduction. Our new findings provide an effective synthetic way to produce high-performance Li4Ti5O12 anodes for lithium rechargeable batteries.  相似文献   

19.
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   

20.
Direct hydrocarbon type solid oxide fuel cells are attractive from simple gas feed process and also high energy conversion efficiency. In this study, La0.5Sr0.5MnO3 (LSM55) perovskite oxide was studied as oxide anode for direct hydrocarbon type solid oxide fuel cell (SOFC). Although reasonable power density like 1 W/cm2 and open circuit voltage (OCV) (1.1 V) at 1273 K was exhibited when H2 was used as fuel, the power density as well as OCV of the cell using LSM55 for anode was significantly decreased when dry C3H8 was used for fuel. After power generation measurement, LSM55 phase was decomposed to MnO and La2MnO4. Effects of various dopants to Mn site in LSM55 were studied and it was found that partial substitution of Mn in LSM55 with other cation, especially transition metal, is effective for increasing maximum power density. In particular, reasonable high power density can be achieved on the cell using Ni-doped LSM55 for anode. On the other hand, Al substitution is effective for increasing stability against reduction and so, dopant effects of Al were studied in more details for dry C3H8 fuel. The power density as well as OCV increased with increasing Al content and the highest power density was achieved at x = 0.4 in La0.5Sr0.5Mn1 ? x Al x O3. Among the examined composition, it was found that the cell using La0.5Sr0.5Mn0.6Al0.4O3 anode shows the largest power density (0.2 W/cm2) at 1173 K and high OCV (1.01 V) against dry C3H8 fuel.  相似文献   

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