A thermoanalytical study in non-isothermal conditions was realized on Ga-substituted MBa2Cu3O7-δ superconducting compounds formation (M=Yb, Eu). The presence of different oxides in the reaction mixtures leads to different reactivity of the system. The type
of lanthanoide ion present in the studied compositions determines the reactivity of the system. In the system containing Eu
the solid state reactions start at lower temperature than in the system containing Yb. Ga-substitution does not change evidently
the thermal behavior of the unsubstituted samples. Different reactivities of the studied reaction mixtures led, after similar
thermal treatment in isothermal conditions, to samples with different structure and superconducting properties.
This study reports experimental investigations by DTA/TG analysis of (1−x)SnO2−xCuO compositions, up to 1773 K and at two oxygen partial pressures (i.e. air and argon). In air, DTA/TG results showed thermal
effects due exclusively to CuO presence in the initial mixture. No binary compounds were formed. The reduction process of
CuO to Cu2O over 1273 K as well as the formation over 1373 K of the liquid phase, have been evidenced. In argon atmosphere, CuO to Cu2O reduction reaction is shifted toward 1205 K, while the liquid phase appears in the studied mixtures over 1473 K. The formation
of an eutectic composition between SnO2−Cu2O, melting at 1491 K, coordinates:0.932Cu2O+0.068SnO2, has been experimentally established in argon.
The paper presents a new, nonconventional method, based upon coprecipitation, for the synthesis of niobium oxidic compounds.
The coprecipitation product of niobic acid with calcium oxalate was used as precursor. Calcium metaniobate was obtained by
appropriate thermal treatment of the coprecipitate. The coprecipitation mechanism was studied and the optimal conditions for
quantitative precipitation of niobium and calcium were established. The mechanism of thermal decomposition of the coprecipitate
was investigated by means of differential thermal analysis and X-ray powder diagrams. The final product of thermal decomposition,
calcium metaniobate, is formed at 730°C.
The paper reports a new, nonconventional method for the preparation of oxygen-containing niobium compounds, based upon coprecipitation.
The coprecipitation product of niobic acid with lead oxalate was used as precursor. Lead metaniobate was obtained by proper
thermal treatment of the coprecipitate. The coprecipitate mechanism was studied and the optimal conditions for quantitative
precipitation of niobium and lead were established. The mechanism of thermal decomposition of the coprecipitate was investigated
by differential thermal analysis and X-ray powder diagrams. The final product of thermal decomposition, lead metaniobate,
is formed at 850C.
In order to clarify the effect of PbO addition on the formation steps of the superconducting phases in the system Bi2O3−SrO−CaO−CuO, a study of solid-state reactions under non-isothermal conditions, in the PbO−MO (M=Ca, Sr, Ca+Sr) system has been carried out.
Results suggest that the reactivity of the components in the system containing PbO and CaO is much higher than in the system
containing SrO. The Ca2PbO4 compound is formed first even in the system whereM=Ca+Sr. It is confirmed that Ca2PbO4 systems containing PbO.
Authors:M. Popa, J. Calderon-Moreno, D. Crisan, and M. Zaharescu
This work introduces results obtained during the preparation of a Bi-based material with superconducting properties by oxalate
The influence of Fe presence on the precursors thermal stability and on the superconducting phases formation mechanism are
presented. The thermal decomposition and the stability in air of FeC2O42H2O and also of the components mixture were studied by DTA/TG. It was evidenced that iron oxalate decomposes at the lowest temperature
compared to the decomposition temperatures of the individual oxalates.
XRD, IR and TEM/ED studies were approached to investigate the individual oxalates and the mixture coprecipitates for the high-Tc superconducting material synthesis.
Authors:A. Brăileanu, M. Zaharescu, D. Crişan, and E. Segal
Following our previous research, this work is dedicated to the study of phase formation in the subsolidus domain of the Bi2O3-PbO-CaO system.
Former investigations performed by DTA/TGA and XRD have pointed out that under non-isothermal conditions only the formation
of binary compounds occurs. Under such conditions these compounds could be non-equilibrium phases.
In order to establish the conditions of formation of equilibrium phases, a study of the Bi2O3-PbO-CaO system, in isothermal conditions, was carried out. The results obtained in isothermal conditions have confirmed the
presence of Bi2O3-rich solid solutions and Ca2PbO4 as main equilibrium phases. An attempt to represent the phase relations of the mentioned system at 700C should be equally
Authors:M. Zaharescu, A. Jitianu, A. Braileanu, J. Madarász, and G. Pokol
It is well known that SiO2 -based inorganic-organic hybrid materials present significant differences due to the organic moieties bound to the inorganic
network and to the preparation conditions.
In the present work the ageing effect on the thermal stability of the SiO2 -based inorganic-organic hybrid materials prepared using tetraethoxysilan (TEOS), triethoxymethylsilan (MTEOS), triethoxyvinylsilan
(VTEOS), tetramethoxysilan (TMOS), trimethoxymethylsilan (MTMOS) and trimethoxyvinylsilan (VTMOS) was studied.
TG/DTA-MS was used to study the decomposition process of the materials. The structural modifications of the materials during
ageing were studied using spectral methods.
The gels obtained starting with more reactive alkoxides, of methoxy-type, present more complex structures and are less stable