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1.

The process of shrinkage of calcium silicate hydrate was investigated by dilatometry up to 350 °C. The properties of this material are based on the formation of C–S–H phases during the reaction at temperatures between 180 and 205 °C and water vapor pressure lower than 16 bars. The main C–S–H phases are 11.3 Å tobermorite and xonotlite. 11.3 Å tobermorite converts to 9.3 Å tobermorite on air at temperatures around 300 °C. The hydrosilicate materials were prepared from quicklime and finely ground sand with different CaO/SiO2 ratios under different hydrothermal conditions. The reaction time was 24 h. Materials based on xonotlite and tobermorite were produced, and the calcium silicate phases were characterized by XRD and TG/DTA methods. Dilatometry measurements were used to study the effect of heating conditions on sample shrinkage. Dehydration of hydrated calcium silicate minerals occurred during heating. The results show that sample shrinkage is dependent on the type and amount of C–S–H phases, the amount of bound water and formation of 9.3 Å tobermorite. All samples showed shrinkage after heating up to 350 °C, but this change was not irreversible for all samples after cooling to room temperature.

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2.
A transparent silicon polymer gel was prepared by sol–gel technology to serve as the base in the preparation of highly disperse SiO2–C composites at various temperatures (400, 600, 800, and 1000°C) and various exposure times (1, 3, and 6 h) via pyrolysis under a dynamic vacuum (at residual pressures of ~1 × 10–1 to 1 × 10–2 mmHg). These composites were X-ray amorphous; their thermal behavior in flowing air in the range 20–1200°C was studied. The encapsulation of nascent carbon, which kept it from oxidizing in air and reduced the reactivity of the system in SiC synthesis, was enhanced as the carbonization temperature and exposure time increased. How xerogel carbonization conditions affect the micro- and mesostructure of the xerogel was studied by ultra-small-angle neutron scattering (USANS). Both the carbonization temperature and the exposure time were found to considerably influence structure formation in highly disperse SiO2–C composites. Dynamic DSC/DTA/TG experiments in an inert gas flow showed that the increasing xerogel pyrolysis temperatures significantly reduced silicon carbide yields upon subsequent heating of SiO2–C systems to 1500°C, from 35–39 (400°C) to 10–21% (1000°C).  相似文献   

3.
High-efficiency peroxidase-like catalysts that can be easily recycled are desperately needed for the rapid and accurate detection of H2O2. Herein, a novel flexible membrane composed of vanadium/cobalt oxides–anchored carbon (VCoO/C) nanofibers has been purposely designed and fabricated by electrospinning and subsequent carbonization, where there are processing temperature-dependent morphology, composition, and versatile properties. As the carbonization temperature increases from 600°C to 900°C, the saturation magnetization of the as-prepared VCoO/C nanofibers rises gradually. When treated at 750°C under Ar protection, the resultant VCoO/C-750 nanofibers yield superior peroxidase-like catalytic activity toward H2O2 with a low limit of detection of 0.44 μM (signal-to-noise ratio = 3). The combination of magnetic behavior and flexibility enables the effective recovery of catalysts. It is believed that our results will open a new avenue for the controlled preparation of flexible nanofiber materials, which are endowed with multiple functions.  相似文献   

4.
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)SnO2xTbO2, 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   

5.
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[H2W12O40nH2O] 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   

6.
Effects of the anion type on the structure, thermal stability, and catalytic performance of La-doped Cu-Mn catalysts prepared by co-precipitation were characterized by X-ray diffraction, Brunauer-Emmett-Teller, temperature-programmed reduction, temperature-programmed reduction of oxidized surfaces, and temperature-programmed desorption. The Cu-Mn catalyst was tested for the water-gas shift (WGS) reaction. The main crystalline phase of samples prepared with sulfate, acetate, chloride, and nitrate as the starting materials was a Cu1.5Mn1.5O4 spinel structure, following the WGS reaction, the main crystalline phases were transformed into Cu and MnO. The sample prepared with acetate as the starting material showed the most obvious MnCO3 characteristic diffraction peaks, with better synergistic effects of Cu and MnO, increased adsorption of CO2 and improved dispersion of Cu on the catalyst surface; also, the best thermal stability and the highest low temperature catalytic activity were observed. The sample prepared with nitrate as the starting material maintained high thermal stability and catalytic performance in the range of 400°C to 450°C, but CO conversion decreased below 350°C. Catalytic performance of the sample prepared with sulfate and chloride as the starting materials was poor, ranging from 200°C to 450°C.  相似文献   

7.
Bismuth silicon oxide (Bi12SiO20, BSO) nano crystalline powder was prepared by sol–gel technique using bismuth nitrate and tetraethyl orthosilicate as starting materials. The prepared samples were sintered at various temperatures (750 °C maximum) and characteristic sillenite single cubic phase with crystallite size ~38 nm (calculated from room temperature powder XRD measurements) was realized at 750 °C sintering temperature. SEM analysis showed that the powder contains the nano-sized particles with almost spherical morphology. The observed frequencies in room temperature FTIR spectrum could be assigned to Bi–O, Si–O and Bi–O–Si bonds. The FWHM (full width at half maximum) of the diffraction peaks decreased while the intensity of FTIR absorption lines increased with the increase in the sintering temperature indicating better bond formation and crystallization. The thermograph of the samples recorded in the temperature range 50–1,000 °C showed almost no weight loss after ~575 °C further confirmed the conclusion arrived at from XRD and FTIR analysis. The samples sintered at 750 °C showed about 50% absorbance in 400–600 nm region which was consistent with the pale yellow color of the sample. Broad blue emission centered ~478 nm was observed when excited by 350 nm radiation from a Xe-lamp. The intensity of this broad emission band increased while its FWHM decreased with the increase in sintering temperature. Self-trapped excitons could be responsible for this emission.  相似文献   

8.
By thermoanalytical methods TG, DTG, DTA there have been investigated the processes occurring during the formation of ceramic materials on the basis of Al2O3, ZrO2, Si3N4, SiC,and inorganic binder. IR spectroscopy has been an additional research method. It's been determined that with the use of H3PO4 as the binder for ceramic materials, the mechanisms of thermal decomposition are connected with the following processes: 1. removal of weakly tied and crystallized water in the temperature range of120–230°C, the removal being characterized by the endothermic effect, 2. interaction of the initial powder components of the ceramic materials with orthophosphoric acid conditioned by a strong exothermic effect on the DTA curve in the range of 230–530°C, 3. overlapping of endo- and exo-effects, testifying to a complex mechanism of thermal transformations, 4.oxidizing of the non-reacted silicon at the temperature of 720(760)°C, an increase of mass is observed on the TG curve as a result of the formation of SiO2 – crystoballite. This revised version was published online in July 2006 with corrections to the Cover Date.  相似文献   

9.
Chromite Spinel materials were synthesized in this study by the citrate precursor method using four divalent cations (Ni2+, Co2+, Zn2+, and Cu2+). Citrate precursors consisting of mixed chromium citrates were first subjected to a thermogravimetric (TG) analysis for determining optimum temperatures for annealing. TG of coprecipitated chromium(III) citrate–zinc citrate gel has been carried out separately in N2 and O2 atmospheres. In both the cases, dehydration is followed by a four-step decomposition. The TG data were subjected to kinetic/mechanistic analysis, and the values of activation energy and Arrhenius factor were approximated. TG curves of various powders which were obtained on annealing at the two temperatures did exhibit thermal instability when carried out in N2 atmosphere. A large coercivity of 2701.01 Oe was observed for NiCr2O4 at 650 °C. On the basis of the results, 450 °C has been chosen for annealing treatment of the four gels. The samples were accordingly annealed at two different temperatures (450 and 650 °C) in a muffle furnace for 1 h in each case. The annealed powders were characterized using X-ray diffraction (XRD), SEM, and vibrating sample magnetometer (VSM). The XRD patterns show that annealing of CuCr2O4, NiCr2O4, and CoCr2O4 at 450 °C yields very small crystallites with poor Bragg reflections, although ZnCr2O4 samples show better peaks in XRD data. Annealing at 650 °C resulted in particle size range of 8–89 nm in the four cases. In the case of ZnCr2O4, the particle size was 8 nm.  相似文献   

10.
Thermogravimetric Analysis of three aquatic materials, i.e. cuttlebone, mussel shell and oyster shell, and other physicochemical characteristics were investigated. The highest decomposition rates of aquatic materials under two surrounding gases, i.e. oxygen and nitrogen, exhibited no significant difference for cuttlebone (3.6×10-5-4.8×10-5 mg s-1 mginitial-1 at heating rate 5 °C/min and 11.8 ×10-5 -12.5×10-5 mg s-1 mginitial-1 at heating rate 15 °C/min) and mussel shell (3.4×10-5- 5.2×10-5 mg s-1 mginitial-1 at heating rate 5 °C/min and 11.9×10-5 – 12.4×10-5 mg s-1 mginitial-1 at heating rate 15 °C/min), while oyster shell provided the higher decomposition rate under nitrogen surrounding gas (7.6×10-4 mg s-1 mginitial-1 at heat rate 5 °C/min and 21.53×10-4 mg s-1 mginitial-1 at heating rate 15 °C/min). This is probably because of the difference in their starting crystalline structures, i.e. aragonite (cuttlebone and mussel shell) and calcite (oyster shell). The cubic calcium oxides were prepared by calcination of three aquatic materials under oxygen and nitrogen surrounding gases at 5 °C/min ramping to 850 °C for 2 hours. All resulting calcium oxides obtained from oxygen atmosphere provided only cubic crystalline phases and the adsorption-desorption isotherms (IUPAC Type III), whereas the calcinations under nitrogen surrounding gas gave a presence of calcium hydroxide crystalline or hydroxyl- contaminate existing with cubic calcium oxide that influences on the strength and the number of carbon dioxide adsorption sites. The specific surface area of all resulting calcium oxides ranged from 0.1 – 1.5 m2/g and the average pore diameter was found in the range of 40-60 nm. The the number of basic sites belonging to CaO derived from Oyster shell or Cuttlebone were improved while firing under oxygen atmosphere. The suitable firing condition is at the low heating rate to develop porous materials.  相似文献   

11.
SrSnO3 was synthesized by the polymeric precursor method with elimination of carbon in oxygen atmosphere at 250 °C for 24 h. The powder precursors were characterized by TG/DTA and high temperature X-ray diffraction (HTXRD). After calcination at 500, 600 and 700 °C for 2 h, samples were evaluated by X-ray diffraction (XRD), infrared spectroscopy (IR) and Rietveld refinement of the XRD patterns for samples calcined at 900, 1,000 and 1,100 °C. During thermal treatment of the powder precursor ester combustion was followed by carbonate decomposition and perovskite crystallization. No phase transition was observed as usually presented in literature for SrSnO3 that had only a rearrangement of SnO6 polyhedra.  相似文献   

12.
The thermal production of 4PbO·PbSO4 was comprehensively studied and characterized for two syntheses routes, i.e. either heating 3PbO·PbSO4·H2O, or a mixture of 4PbO:PbSO4, in air to about 700 °C. In the 3PbO·PbSO4·H2O approach, the formation of an intermediate amorphous phase occurred at around 210 °C with the loss of H2O from the hydrated structure. Formation of 4PbO·PbSO4 initiated at around 270 °C with predominantly 4PbO·PbSO4 and 13% residual PbO·PbSO4 existing at 700 °C. With the synthesis route of mixing a stoichiometric ratio of 4PbO with PbSO4, an intermediate phase of PbO·PbSO4 formed at around 300 °C, before the 4PbO·PbSO4 phase started to form at around 500 °C. Upon further heating, 4PbO·PbSO4 was the predominant phase with 8% of PbO·PbSO4 remaining. Both samples decomposed upon further heating to 850 °C. Powder neutron diffraction studies of the final 4PbO·PbSO4 products from the two different synthesis routes showed similar crystallographic unit cell lattice parameters with slight differences in the PbO:PbSO4 contents. This could possibly be linked to differences observed in the microscopic crystallite shapes from the two synthesis routes.  相似文献   

13.
Thermal behavior of commercial PVC cable insulation both before and after extraction of plasticizers, fillers and other agents were tested by TG/DTG and DSC during heating in the range 20-800°C in air. The ultrasound enhanced hexane extraction and dissolution in THF with subsequent precipitation of PVC were used to prepare 'extracted' and 'precipitated' samples. The total mass loss measured for the 'non-treated', 'extracted' and 'precipitated' PVC samples was 71.6, 66.6 and 97%, respectively. In the temperature range 200-340°C the release of dioctylphthalate, HCl and CO2was observed by simultaneous TG/FTIR. From TG results measured at different heating rates (1.5, 5, 10, 15 K min-1) in the range 200-340°C the non-isothermal kinetics of the PVC samples degradation was determined. Activation energy values of the thermal degradation processes calculated by ASTM E 698 method, for 'non-treated', 'extracted' and 'precipitated' PVC samples were 174.6±17 kJ min-1, 192.8±19 kJ min-1, 217.1±20 kJ min-1, respectively. These kinetic parameters were used for the lifetime simulation of the materials.  相似文献   

14.
To study the effect of atmospheric type and heating rate on formation mechanism of MoSi2, the Mo + 2Si powder mixture was exposed to simultaneous thermal analysis (STA) in air atmosphere at different heating rates (10, 15, and 20 °C/min). To further study the changes, thermal analyses of molybdenum powders and consumed silicon were also performed separately. An amount of aluminum powder (5 wt.%) was also added to Mo + 2Si powder mixture and exposed to thermal analysis at different heating rates (10, 15, and 20 °C/min) to study the effect of the presence of active elements (like aluminum) on the trend of the performance of changes. To perform phase studies on the products of the thermal analysis at a later stage, each product was separately tested by an X-ray diffraction (XRD) method. Contrary to expectations, the XRD patterns showed that the trends of changes during thermal analysis were not in the direction of MoSi2, and the DTA–TG peaks obtained from these analyses were in fact related to other changes. Ultimately, the results showed that the peaks on the DTA curves resulted from the oxidation of molybdenum particles; and the (MoO3) melt of the product, and in continuation of the reduction of a part of this oxide, it resulted during the silicothermic and aluminothermy reactions. The results of this research also showed that with regard to the presence of intensive oxidation tendency of molybdenum particles, there is no chance for the formation of MoSi2 by heating the powder mixture of Mo + 2Si in air atmosphere and at low heating rates.  相似文献   

15.

Lanthanum ferrite, LaFeO3 (LF), has raised considerable interest since it can be used in many applications such as solid-oxide fuel cell electrode, sensor material (H2O and ethanol) and catalyst. Since the conventional ceramic route of synthesis has some disadvantages, mainly related to an exaggerated grain growth, LF has been prepared by different methods including combustion synthesis, sol–gel, hydrothermal processes, polymerizable complex method and mechanochemistry. As concerns this last method, a problem occurs due to the moisture sensitivity of La2O3. To overcome the problem, we used lanthanum acetate sesquihydrate [La(CH3COO)3·1.5H2O] and iron (II) oxalate dehydrate [FeC2O4·2H2O] as precursors. The mechanism of the solid-state reactions in the mixtures has been studied by TG–DSC and XRPD. Synthesis of LaFeO3 has been realized by annealing the mechanically activated mixtures for 3 h at temperatures between 500 and 800 °C. While LF prepared at 500 °C < T < 600 °C has an amorphous character, LF obtained at T ≥ 600 °C is free from carbonaceous impurities as it is shown by FT-IR and TG measurements. The specific area of the LaFeO3 powders obtained starting from the mechanically activated mixture is decreasing by increasing the annealing temperature. On the contrary, the annealing on samples of physical mixture at temperatures up to 800 °C only yields a mixture of LaFeO3, La2O3 and Fe2O3.

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16.
The thermoanalytical curves (TA), i.e. TG, DTG and DTA for pure cephalexin and its mixtures with talc, magnesium stearate, starch and microcrystalline cellulose, respectively, were drawn up in air and nitrogen at a heating rate of 10 °C min−1. The thermal degradation was discussed on the basis of EGA data obtained for a heating rate of 20 °C min−1. Until 250 °C, the TA curves are similar for all mixtures, up this some peculiarities depending on the additive appears. These certify that between the pure cephalosporin and the excipients do not exists any interaction until 250 °C. A kinetic analysis was performed using the TG/DTG data in air for the first step of cephalexin decomposition at four heating rates: 5, 7, 10 and 12 °C min−1. The data processing strategy was based on a differential method (Friedman), an integral method (Flynn–Wall–Ozawa) and a nonparametric kinetic method (NPK). This last one allowed an intrinsic separation of the temperature, respective conversion dependence on the reaction rate and less speculative discussions on the kinetic model. All there methods had furnished very near values of the activation energy, this being an argument for a single thermooxidative degradation at the beginning (192–200 °C).  相似文献   

17.
Na-montmorillonite (Na-MONT) was loaded with hexadecyltrimethylammonium cations (HDTMA) by replacing 41 and 90% of the exchangeable Na with HDTMA, labeled OC-41 and OC-90, respectively. Na-MONT, OC-41, and OC-90 were heated in air up to 900 °C. Unheated and thermally treated organoclays heated at 150, 250, 360, and 420 °C are used in our laboratory as sorbents of different hazardous organic compounds from waste water. In order to get a better knowledge about the composition and nature of the thermally treated organoclays Na-MONT and the two organo-clays were studied by thermogravimetry (TG) in air and under nitrogen. Carbon and hydrogen contents in each of the thermal treated sample were determined and their infrared spectra were recorded. The present results showed that at 150 °C both organoclays lost water but not intercalated HDTMA cations. At 250 °C, many HDTMA cations persisted in OC-41, but in OC-90 significant part of the cations were air-oxidized into H2O and CO2 and the residual carbon formed charcoal. After heating both samples at 360 °C charcoal was present in both organo clays. This charcoal persisted at 420 °C but was gradually oxidized by air with further rise in temperature. TG runs under nitrogen showed stepwise degradation corresponding to interlayer water desorption followed by decomposition of the organic compound, volatilization of small fragments and condensation of non-volatile fragments into quasi-charcoal. After dehydroxylation of the clay the last stages of organic matter pyrolysis and volatilization occurred.  相似文献   

18.
Sol-gel process was employed to synthesize the Pb-BSCCO system having general composition Bi2−xPbxSr2Ca2Cu3O10−δ, where x=0.2, 0.4 and 0.8. Fourier transform infrared (FTIR) spectroscopy, X-ray diffraction (XRD), dilatometry and vibrating sample magnetometer (VSM) were employed to study the materials produced at different stages. Two-stage heating firstly at 300 and then 800°C was adopted in order to avoid the burning of the materials and formation of carbonates. The carbonate formation was avoided by heating the materials firstly at 300°C for 2 h and without intermediate cooling moved to the furnace having temperature 800°C and hold for 2 h. The sintering behaviour of samples was studied by dilatometry and the results revealed that the sample having x=0.4 was stabled up to a temperature of 700°C while samples having x=0.2 and 0.8 to a temperature of 625°C. The maximum shrinkage was observed at 850°C in all the samples. On the basis of dilatometry results, the samples were sintered at 845°C for 60 h to observe the superconducting phases. The highest volume fraction of high superconducting phase (2223) was noticed in the sample containing x=0.4 having onset T c=110 K.  相似文献   

19.
In this study, a strong acid ion-exchange resin, as the starting material of spherical activated carbon contained Zn (Zn-SPAC), was treated by 0.1 N zinc solution. Ion-exchange treatment was performed from one to three times for controlling the zinc content. The ion-exchanged resins were activated under N2/H2O vapor atmosphere at 900°C for 0.5 h, followed by carbonization treatment at 700°C under N2 atmosphere. The Zn-SPAC samples were measured for their physicochemical characteristics, such as X-ray diffraction (XRD) patterns, scanning electron microscope (SEM) images, electron probe micro analyzer (EPMA) images, energy dispersive X-ray spectroscopy (EDXS), Brunauer–Emmett–Teller (BET) specific surface area, strength, and zinc content. Also, the samples were used in order to measure photochemical activities, such as the removal efficiency of humic acid (HA) in a fluidized batch reactor. The XRD patterns appeared as the ZnS type. The Zn-SPAC had a large BET specific surface area and their shape was spherical, with a diameter of about 350–400 μm. When the Zn-SPAC was dosed in a fluidized bed reactor with UV light, the HA removal efficiency increased by up to 60%. On the other hand, the HA removal efficiency by only UV-C (λ max = 254 nm) irradiation was very low, about 15%. Therefore, we infer that Zn-SPAC has good photochemical activity and presented the possibility of being a useful photocatalyst for water purification.  相似文献   

20.
《Comptes Rendus Chimie》2014,17(7-8):785-789
In the context of fuel upgrading by selective ring opening of naphthenes, we have investigated the catalytic conversion of cyclopentane in large hydrogen excess over iridium and platinum single-crystal surfaces. Both (111) and (112) orientations have been considered. The catalytic tests have been performed at 1 kPa and 25–600 °C using a recently developed surface reactor equipped with laser heating and online gas chromatography. Only cyclopentene and C1–C4 cracking products are formed on iridium, while platinum additionally catalyzes the formation of pentane around 200 °C, which dehydrogenates to pentene at 250 °C. Noticeably, on both metals, the surface steps prevent hydrocarbon cracking (up to 400 °C) at the benefit of dehydrogenation. In all cases, a carbon overlayer is formed on the surfaces in the course of the reaction.  相似文献   

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