Authors:P. Pulišová, J. Boháček, J. Šubrt, L. Szatmáry, P. Bezdička, E. Večerníková, and V. Balek
Thermogravimetry-differential thermal analysis, emanation thermal analysis, mass spectrometry detection, Fourier transform
infrared and XRD were used to characterize thermal behaviour of titanium dioxide photocatalyst precursors prepared by precipitation
at various conditions from peroxotitanic acid sols. The transmission electron microscopy HRTEM technique was used to characterize
the surface microstructure. The sols contained TiO2 anatase particles of approximately 10 nm in diameter. During heating of the air dried samples, their chemical degradation
took place giving rise to anatase. On further heating, the crystallization of anatase and formation of rutile phase was observed.
To test the photocatalytic activity of the samples, the decomposition of 4-chlorophenol (4-CP) under ultraviolet and visible
irradiation was monitored. It was shown that photocatalytic activities of the samples are comparable to the Degussa P25 photocatalyst
The thermal behavior for three homologous series of cationic geminis surfactants of the type n-2-n, alkanediyl-α,ω-bis(alkyldimethylammonium bromide), with n = 12, 14, 16, and 18, and sodium alkyl sulfates, SCmS, with m = 12, 14, and 16, is reported here. The cationic/anionic molar ratio is kept at 1:2 (equicharged mixtures), and salt is also
present. Polarizing light microscopy and differential scanning calorimetry show a stepwise fusion for the mixtures with appearance
of several mesophases between the crystalline structures and the isotropic liquid. A main endothermic transition is observed,
associated with partial chain melting and consequent loss of crystalline order, followed by a transition to a smectic liquid
crystal. The phase transition thermodynamics is interpreted in terms of an interplay between van der Waals chain–chain interactions
and ionic head group interactions.
Authors:M. Kuliffayová, L’. Krajči, I. Janotka, and V. Šmatko
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.
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.
Authors:X. Zhang, Y. Ding, Y. Zhang, Y. Hao, G. Meng, and L. Zhang
Highly oriented single crystal antimony nanowire arrays have been synthesized within anodic aluminum oxide (AAO) template
by pulsed electrodeposition. Thermal behavior and oxidation analysis of the antimony nanowires have been investigated by means
of thermogravimetry and differential scanning calorimetry in Ar and air atmosphere, respectively. Compared to bulk antimony,
the antimony nanowires exhibit a lower sublimation temperature at 496.4°C. Evident oxidation of the Sb nanowires occurs at
429.8°C in air atmosphere and α-Sb2O4 nanowires have been obtained as the oxidation product. The results indicate that the sublimation and the oxidation of the
antimony nanowires in the AAO template is a slow multi-step process. The present results are of relevance when processing
antimony nanowries for thermoelectric applications at high temperatures.
Authors:C. Radhakrishnan, A. Sujith, and G. Unnikrishnan
The thermal behaviour of styrene butadiene rubber (SBR)/poly (ethylene-co-vinyl acetate) (EVA) blends was studied by using
thermogravimetry (TG) and differential scanning calorimetry (DSC). The effects of blend ratio, cross-linking systems and compatibilization
on the thermal stability and phase transition of the blends were analyzed. It was found that the mass loss of the blends at
any temperature was lower than that of the components, highlighting the advantage of blending SBR and EVA. The addition of
compatibilizer was also found to improve the thermal stability. DSC studies indicated the thermodynamic immiscibility of SBR/EVA
system even in the presence of the compatibilizer. This is evident from the presence of two different glass transition temperatures,
corresponding to SBR and EVA phases in both compatibilized and uncompatibilized blends.
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.
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
transformation depends on an incomplete decomposition reaction. The variation of the heating rate showed that the
1) decomposition is the dominant reaction for alloys containing 19 and 21 at.%Al.
Authors:G. Colón, M. Avilés, J. Navío, and P. Sánchez-Soto
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).
Authors:J. Kristóf, R. Frost, J. Kloprogge, E. Horváth, and M. Gábor
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