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Abstract

The kaolin sand containing 36 wt% of kaolinite was thermally transformed at 650 °C/L h to the burnt kaolin sand (BKS) with relevant content of metakaolinite. Thermal behaviour of composites with substitution of Portland cement (PC) by the BKS containing 0, 5, 10 and 15 wt% of metakaolinite and water-to-solid ratio of 0.5 kept for 90 days in 20 ± 1 °C water was studied by thermal analysis. TG/DTA/DTG studies concerned calciumsilicate hydrate and calciumaluminate hydrate formation, portlandite dehydroxylation and calcite decarbonation. The influence of curing time and metakaolinite content were estimated. The reduction in portlandite content was observed in PC–BKS composites opposite to that found in the reference PC system. Compressive strength uptakes were observed in PC–BKS composites relative to that of reference PC system. BKS is characterized as effective pozzolanic material giving cement composites of high performance. The above findings were confirmed by X-ray diffraction analysis (XRD) and scanning electron microscopy (SEM) results.

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The mixed zirconium, titanium, hafnium and first-row transition metal oxides (containing phosphorous oxide) were prepared using ion exchange method followed by calcinations at 1020 K during 12 h. The resulted mixed oxides were identified by XRPD method and studied their thermal behaviour by TG-DTA analysis. As a result of thermal analysis there were found one exothermic (with a peak at about 950 K), and one endothermic (with a peak at about 1300 K) processes, both without mass loss. The observation was valid for all investigated samples. The analysis of XRPD patterns of the investigated samples showed well-defined crystal phases characteristic of each oxide. The XRPD analysis also verified the phase transition of tetravalent metal oxides from orthorhombic to tetragonal, observed by DTA analysis.

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Thermal behaviour of the glass series (100-x)[50ZnO-10B2O3-40P2O5xSb2O3 (x=0-42 mol%) and (100-y)[60ZnO-10B2O3-30P2O5ySb2O3 (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.

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The thermal behavior of Cu—Al alloys with 17, 19 and 21 at.%Al was examined by differential thermal analysis (DTA), differential scanning calorimetry (DSC), X-ray diffractometry (XRD), optical microscopy (OM) and scanning electron microscopy (SEM). The presence of the gamma phase (Al4Cu9)was clearly detected for the Cu—19 at.%Al alloy and caused the 2 phase disordering process in two stages. The tendency to increase the 2 dissolution precipitates with the increase in the Al content seems to be reverted for compositions at about 21 at.%Al and the heating/cooling ratio seems to influence the thermal response of this process. The presence of the endothermic peak corresponding to the 1 transformation depends on an incomplete decomposition reaction. The variation of the heating rate showed that the 1 (+ 1) decomposition is the dominant reaction for alloys containing 19 and 21 at.%Al.

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A microcomposite powder in the system TiO2—ZrO2 as a precursor of zirconium titanate (ZT) materials has been studied by thermal methods (DTA-TG) and X-ray diffraction (XRD). The microcomposite powder has been prepared by chemical processing of crystalline TiO2 (rutile, 10 mass% anatase),as inner core, coated with in situ precipitated amorphous hydrated zirconia gel, asouter core. The morphology and chemical composition of the resultant powders has been examined by SEM-EDX (Scanning electron microscopy-energy dispersive X-ray spectroscopy). Thermal behaviour of the microcomposite powder was reported, showing the dehydration and dehydroxylation of the zirconia gel, the crystallization into metastable cubic/tetragonal zirconia at temperatures 400—470°C, and the feasibility of preparing ZT powder materials by progressive reaction of TiO2 and ZrO2 at higher temperatures (1400°C).

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The thermal behaviour of kaolinites intercalated with formamide, dimethyl sulphoxide and hydrazine has been studied by simultaneous TG-DTG-DTA-EGA and TG-MS techniques. The complexes can be decomposed completely without dehydroxylating the mineral. It was found that the amount of intercalated guest molecules per inner surface OH-group is close to unity for the formamide and dimethyl sulphoxide intercalates. For the intercalation of hydrazine it was found that hydrazine is locked in the expanded mineral as hydrazine hydrate and its amount is somewhat higher than that obtained for the other two reagents. The thermal evolution patterns of the guest molecules revealed that all the three reagents are bonded at least in two different ways in the interlayer space.

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Two different samples of amorphous calcium carbonate (ACC) hydrates were prepared respectively by mixing aqueous solutions of CaCl2 and Na2CO3-NaOH and by allowing the diffusion of (NH4)2CO3 sublimate into ethanol solution of CaCl2. Thermal behaviors of the synthetic ACCs were investigated comparatively by means of thermoanalytical techniques complimented by powder X-ray diffraction, FTIR spectrometry and microscopic observations. The anhydrous ACCs produced by the thermal dehydration of the respective samples were crystallized to calcite in different ways. The sample prepared in aqueous medium was crystallized at around 600 K in a single step. Crystallization in two separated steps at around 600 and 825 K was observed for the sample prepared in ethanol medium. Characteristics of the crystallization processes were discussed from thermodynamic and kinetic points of view.

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Synthesis, characterization and thermal behavior of four compounds that have the general formula [Cu{Pd(CN)4}(L)x]n, in which en=1,2-diaminoethane and pn=1,3-diaminopropane (L=en, x=1 (I); L=pn, x=1 (II); L=en, x=2 (III); L=pn, x=2 (IV)) were described in this work. The complexes were studied by elemental analysis, infrared spectroscopy (IR), differential thermal analysis (DTA) and thermogravimetry (TG) and the residues of the thermal decomposition were characterized by X-ray powder diffraction and found as a mixture of CuO and PdO. The stoichiometry of the compounds was established via thermogravimetric and elemental analyses and their structures were proposed as coordination polymers based on their infrared spectra. The following thermal stability sequence was found: IV<I=II<III.

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The effect of CuO on the thermal behaviour of Zr/KClO4 primer mixtures was studied by thermoanalytical techniques, and the Bruceton method and its related calculation. It was found that the CuO catalytically promoted the decomposition of Zr/KClO4 primer mixtures and shifted the exothermic peak of DSC curves to lower temperatures. In addition, the Zr/KClO4 primer mixture containing CuO had a significant effect on the firing characteristics of electro-explosive devices.

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