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<p>Structural analysis of Ge straight-chain linear polymer [OGe(OH)CH<sub>2</sub>CH<sub>2</sub>COOH]<sub>n</sub> by single-crystal X-ray diffraction was revisited and reported. The thermal behavior of the linear polygermoxane during heating/cooling in synthetic air or in argon was investigated using TGA–DSC-QMS complemented by powder X-ray diffraction, FT-IR measurements, and DFT calculations. Approximately seven thermal stages, some of them composed of complex overlapping transformations, were identified between 20 and 1200&#xa0;°C in both gases. Below 230&#xa0;°C, on heating, an endothermic effect is observed, and it is accompanied by a dehydroxylation process. On cooling from 230&#xa0;°C, an exothermal peak is observed at ~ 180&#xa0;°C, and it was assigned to lattice rearrangement. Heating up to 600&#xa0;°C leads to multistep transformations from crystalline to amorphous state, and processes are developing with mass loss. In argon, above 840&#xa0;°C, only metallic Ge is detected, and this phase is stable until melting. When heating in air, oxidation of Ge occurs, with inherent mass increase, and, finally, GeO<sub>2</sub> melts at ~ 1120&#xa0;°C.</p>

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Structural and thermal analysis of the linear polygermoxane GeSP

  • 期刊论文

  • 发表日期：

    2025年1月8日

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  • G. Aldica,
  • D. Batalu,
  • T. Nakamura,
  • M. Ferbinteanu,
  • C. Locovei,
  • M. A. Vlaicu,
  • I. Pasuk,
  • P. Badica

摘要

Structural analysis of Ge straight-chain linear polymer [OGe(OH)CH2CH2COOH]n by single-crystal X-ray diffraction was revisited and reported. The thermal behavior of the linear polygermoxane during heating/cooling in synthetic air or in argon was investigated using TGA–DSC-QMS complemented by powder X-ray diffraction, FT-IR measurements, and DFT calculations. Approximately seven thermal stages, some of them composed of complex overlapping transformations, were identified between 20 and 1200 °C in both gases. Below 230 °C, on heating, an endothermic effect is observed, and it is accompanied by a dehydroxylation process. On cooling from 230 °C, an exothermal peak is observed at ~ 180 °C, and it was assigned to lattice rearrangement. Heating up to 600 °C leads to multistep transformations from crystalline to amorphous state, and processes are developing with mass loss. In argon, above 840 °C, only metallic Ge is detected, and this phase is stable until melting. When heating in air, oxidation of Ge occurs, with inherent mass increase, and, finally, GeO2 melts at ~ 1120 °C.