The paper describes the results of differential thermal analysis of the octahedral Fe(III) complexes of the general formula [Fe(HLn)2]Cl and Fe(HL3)L3, as well as of the corresponding ligands H2Ln (H2Ln — tridentate salicylaldehyde semi thiosemi- and S-methylisothiosemi-carabazones with n=1, 2 and 3 respectively). The decomposition of the complexes involving sulphur-containing ligands (H2L2 and H2L3) starts with sulphur elimination. In case of the complexes [Fe(HL2)]Cl and [Fe(HL3)]Cl sulphur evolves independently, whereas with Fe(HL3)L3 it is eliminated within the SCH3 group. In the former case, sulphur elimination takes place at the same temperature for both complexes. The change in the coordination mode, being a consequence of the replacement of O by S, has no essential effect on thermal stability of the coordination polyhedron. The complexes involving ONN coordination, realized with the H2L3 ligand, exhibit a comparatively highest thermal stability of the coordination polyhedron.
The paper describes the results of a study of glasses of the type CuxAs50Se50-xfor x=5, 10 and 15 at.% Cu, by the method of thermomechanical analysis. Values of the thermal coefficients of linear expansion
in solid (αg) and visco-plastic (αω) phase were determined. On the basis of the results obtained using the mentioned methods it was possible to determine the
specific temperature of the beginning of the softening process of the glass (Tg), as well as the temperature of the beginning of the deformation (Tω). It was shown that coefficients of linear expansion decrease with the increase of Cu content. On the other hand, the increase
of Cu content caused the increase of the temperatures. The analytical forms of dependence of four physical parameters αg, αω, Tg, Tωas a function of the Cu content were fitted.
Results of thermal investigations of the amorphous five-component chalcogenide system Ge20As14(SexS1−x)52I14 are presented. Differential thermal analysis (DTA), derivative differential thermal analysis (DDTA), and dilatometry were
employed to determine the temperatures of softening and partial crystallization of the samples. Thermal treatment of the samples
at 1000°C and recording of the corresponding thermogravimetric (TG) and derivative thermogravimetric (DTG) curves allowed
an elucidation of the full mechanism of their decomposition, which proceeds via seven characteristic phase transitions.
Kinetic analysis of the crystallization process in Bi4(As2S3)96 and Bi6(As2S3)94 glasses was performed based on DSC curves recorded under non-isothermal measurement conditions. Samples were thermally treated at different heating rates in the temperature range 300–770 K. The activation energy of crystallization E and the pre-exponential factor K0 are determined by the Kissinger method and the characteristic crystallization parameters m and n of investigated glasses by the Matusita method. For both crystallization processes the glass with 4 at.% of Bi is characterized by the mechanism of volume nucleation, which is manifested in the form of two-dimensional growth at the first crystallization process, and as three-dimensional at the second one. On the other hand, in the sample with 6 at.% Bi, the average value of the parameter m is close to one, which indicates one-dimensional crystal growth. Compatibility of the values of the parameters m and n suggests that this sample has a large number of crystallization centers, which do not increase significantly during the thermal treatment.
The thermal decomposition of tetrahedral cobalt(II) complexes with 3(5)-amino-4-acetyl5(3)-methylpyrazole (HL) of the general formula [Co(HL)2X2] (X=Cl, Br, I, NCO, NCS) and octahedral [Co(HL)2(H2O)4](NO3)2 and [Co(HL)2−N(CN)2}2] complexes was investigated in air atmosphere in the interval from room temperature to 1000°C. Decomposition of the complexes occurred in several successive endothermic and exothermic processes, and the residue was in all cases CoO.
The paper describes results of a study of glasses of the type Cux (AsSe1.4 I0.2 )100–x for x =0, l, 5, 10, 15, 20 and 25 at% Cu, by the methods of thermomechanical analysis. Values of the thermal coefficients of linear
expansion in solid and visco-plastic phase were determined and the dependence of this parameter on copper concentration was
established. The experimental method used enabled the determination of characteristics glass transition temperature and the
temperature of the beginning of deformation, and it was found that these parameters increase with increase in the copper content.
The course and kinetics of free radical polymerization in bulk ofp-alkylphenyl methacrylates with AIBN initiator were studied by DSC, in the temperature range 348–373 K. The enthalpy of polymerization, the residual monomer content, as well as the overall reaction rate constants and the activation energies were determined. The similar values of the overall rate constants indicate that the relatively small alkyl substituents inp-position of the phenyl ring affect the polymerization rate to a very small, if any, extent.