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Abstract  

The volatile scandium-β-diketonates are synthesised using acetylacetone (acac) and tetramethylheptanedione (tmhd) as coordinative ligands for CVD application. The X-ray powder patterns are indexed and analysed and found to be orthorhombic and monoclinic phases for Sc(acac)3(1) and Sc(tmhd)3(2) respectively. The sublimation and evaporation kinetics have been analyzed using three calculating techniques. The non-isothermal based activation energy values are found to be 38 ± 2 and 73 ± 2 kJ mol−1 by Flynn–Wall technique for (1) and (2) respectively. The measured Ea values are close to the value obtained using Kissinger method.

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Journal of Thermal Analysis and Calorimetry
Authors: E. Filatov, S. Sysoev, Ludmila Zelenina, Tamara Chusova, V. Logvinenko, P. Semyannikov, and I. Igumenov

Abstract  

Thermal behaviour of a series of lithium β-diketonates: Li(dpm) (dpm=dipivaloylmethanate (2,2,6,6-tetramethylheptane-3,5- dionate)), Li(pta) (pta=pivaloyltrifluoracetonate (2,2-dimethyl-6,6,6-trifluoro-3,5-hexanedionate)), Li(tfa) (tfa=trifluoracetylacetonate (1,1,1-trifluoro-2,4-pentandionate)), Li(hfa) (hfa=hexafluoracetylacetonate (1,1,1,5,5,5-hexafluoro-2,4-pentandionate)) has been investigated. Gas phase composition of these complexes has been established. Temperature dependences of vapor pressure of lithium compounds were obtained by static and dynamic methods, and thermodynamic parameters were calculated. Dependence of compound volatility on ligand structure is shown. For Li(dpm) detailed investigation has been done by differential scanning calorimetry (DSC).

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Journal of Thermal Analysis and Calorimetry
Authors: Ksenia Zherikova, Natalia Morozova, Ludmila Zelenina, S. Sysoev, Tamara Chusova, and I. Igumenov

Abstract  

Five volatile hafnium(IV) and zirconium(IV) β-diketonates: hafnium(IV) acetylacetonate, hafnium(IV) trifluoroacetylacetonate, hafnium(IV) pivaloyltrifluoroacetonate, hafnium(IV) 2,2,6,6-tetramethylheptane-3,5-dionate and zirconium(IV) 2,2,6,6-tetramethylheptane-3,5-dionate were obtained, purified and identified. Thermal behavior of solid compounds was investigated by thermogravimetry (TG) and differential scanning calorimetry (DSC) in helium atmosphere and in vacuum. DSC method was also used for definition of thermodynamic characteristics of melting processes. Using the static method with quartz membrane zero-manometer and the flow method the temperature dependencies of saturated vapor pressure for hafnium(IV) complexes was obtained. The standard thermodynamic characteristics ΔH T 0 and ΔS T 0 of sublimation and evaporation processes were calculated from the temperature dependences of saturated vapor pressure.

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DSC and vapour pressure measurements are presented on some Be, Al and Cr complexes with 2,4-pentanedione tetramethyl-3,5-heptanedione, 1,1,1-trifluoro-2,4-pentanedione and hexafluoro-2,4-pentanedione. Thermodynamic functions are given for the sublimation, vaporization and melting processes of the substances.

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The standard molar enthalpies of formation of the crystalline lanthanum(III) chelate complexes with pentane-2,4-dione (acetylacetone, Hacac) and 1-phenylbutane-1,3-dione (benzoylacetone, Hbzac) were determined by the solution calorimetry method. The following values ofΔH

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Abstract  

A series of metal -diketonates were irradiated with bremsstrahlung of maximum energy of 50 MeV and the recoil behavior of7Be, formed from12C of ligands through12C(, n)7Be reaction, was investigated.7Be nuclides thus formed were detected partially as central metal atoms of the complexes. Complex yields of7Be were compared and an anomalously high yield was observed in tris-acetylacetonatocobalt(III) [Co(acac)3].

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Abstract  

Trace amounts of lanthanum hexafluoroacetylacetonate and indium acetylacetonate were isolated by combination of methods, which includes synthesis of volatile elements -diketonates by nucleophilic ligands exchange and fractional sublimation. This method is useful for produce isotope generators.

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Abstract  

Volatile hexafluoroacetylacetonates of hafnium, ytterbium, scandium, as well as scandium trifluoroacetylacetonate and acetylacetonate have been obtained by interaction of -diketone vapours with radionuclides formed in a cyclotron in on-line operation. The application of volatile -diketonates for transport and separation of the short-life isotopes of metallic elements has been shown.

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Thermal dissociation processes ofβ-diketonate adducts with the composition ML2 · 2B (L = acetylacetone and its substituted derivatives;M = Ni, Co;B = H2O, BuNH2CH3OH, Py, NH3) were investigated. Kinetics of dissociation were studied in a flow reactor. For dehydration processes a compensation relationship is observed (lgA=E+b), demonstrating analogous mechanisms.

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