Thermal evolution of ladder-like silsesquioxanes during formation of black glasses

Jeleń, Piotr; Szumera, Magdalena; Gawęda, M.; Długoń, E.; Sitarz, Maciej

doi:10.1007/s10973-017-6249-9

Cited by 24 publications

(30 citation statements)

References 44 publications

(84 reference statements)

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“…After 7‐days aging layers and xerogels samples underwent the high‐temperature heat treatment in the atmosphere of argon at the temperature of 800°C achieved at a rate of 5°C per minute. The protective atmosphere of the inert gas is needed to avoid oxidation and the loss of carbon ions from the structure of black glasses . The obtained ceramic layers were of the 1 μm thickness.…”

Section: Methodsmentioning

confidence: 99%

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Bioactive layers based on black glasses on titanium substrates

et al. 2017

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Black glasses are amorphous materials based on silicon oxycarbide. The use of precursors in the form of ladder‐like silsesquioxanes enables the control of the amount of carbon ions in the glass network by adjusting ratios of T to D structural units in precursors. In this study, four different sols precursors of four different layers of black glasses on titanium substrates were prepared. The materials were analyzed with the use of various spectroscopic and microscopic methods. Formation of continuous and hermetic layers resistant to corrosion was proven. The black glasses layers were examined as materials for biomedical applications. Therefore, preliminary tests of their bioactivity and biocompatibility were performed. The best results were obtained for the material of lower contribution of carbon ions.

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Section: Methodsmentioning

confidence: 99%

“…The protective atmosphere of the inert gas is needed to avoid oxidation and the loss of carbon ions from the structure of black glasses. 18,43 The obtained ceramic layers were of the 1 lm thickness.…”

Section: Formation Of Black Glasses Layersmentioning

confidence: 99%

Bioactive layers based on black glasses on titanium substrates

et al. 2017

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“…Depending on the conditions of the thermal processing during the whole procedure (drying, pyrolysis) the porous microstructure of the final product is generated. In this work, these parameters were determined based on our previous results [ 20 , 40 , 48 ]. However, to the best of our knowledge, porous SiOC materials obtained from ladder-like silsesquioxanes have not yet been investigated.…”

Section: Resultsmentioning

confidence: 99%

“…Such an observation is typical for ladder like-structures. The first reflection is due to the limited degree of order of the intermolecular chain distance, while the second one can be the result of the distance between the ladder structure [ 45 , 48 ]. Samples after thermal processing at 800 °C similarly do not show any crystalline peaks, which classify their structure as amorphous.…”

Section: Resultsmentioning

confidence: 99%

Chemical Structure and Microstructure Characterization of Ladder-Like Silsesquioxanes Derived Porous Silicon Oxycarbide Materials

et al. 2021

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The aim of this work was to synthesize porous ceramic materials from the SiOC system by the sol-gel method and the subsequent pyrolysis. The usage of two types of precursors (siloxanes) was determined by Si/C ratio in starting materials. It allows us to control the size of the pores and specific surface area, which are crucial for the potential applications of the final product after thermal processing. Methyltrimethoxysilane and dimethyldiethoxysilane were mixed in three different molar ratios: 4:1, 2:1, and 1:1 to emphasize Si/C ratio impact on silicon oxycarbide glasses properties. Structure and microstructure were examined both for xerogels and obtained silicon oxycarbide materials. Brunauer-Emmett-Teller (BET) analysis was performed to confirm that obtained materials are porous and Si/C ratio in siloxanes precursors affects porosity and specific surface area. This kind of porous ceramics could be potentially applied as gas sensors in high temperatures, catalyst supports, filters, adsorbents, or advanced drug delivery systems.

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“…For Si-O species, the stretching and bending vibrations are expected and seen in the 1060-1080 cm −1 range and at 470 cm −1 , respectively [24,30], whereas potential Si-N stretching and bending modes may be overlapped between 950 and 1000 cm −1 . In addition to these bonding modes, Si-C stretching vibrations are expected between 800-900 cm −1 [31][32][33][34][35] to further complicate the deconvolution of the broad band seen in the 800-1100 cm −1 range. The vertical lines in Figure 4 illustrate the overlap of the discussed peaks and the qualitative nature of their assignments given the broadness/irregularity of the resulting bands.…”

Section: Resultsmentioning

confidence: 99%

Amorphous Silicon Oxynitride-Based Powders Produced by Spray Pyrolysis from Liquid Organosilicon Compounds

et al. 2021

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Silicon oxynitrides (SiOxNy) have many advantageous properties for modern ceramic applications that justify a development of their new and efficient preparation methods. In the paper, we show the possibility of preparing amorphous SiOxNy-based materials from selected liquid organosilicon compounds, methyltrimethoxysilane CH3Si(OCH3)3 and methyltriethoxysilane CH3Si(OC2H5)3, by a convenient spray pyrolysis method. The precursor mist is transported with an inert gas or a mixture of reactive gases through a preheated tube reactor to undergo complex decomposition changes, and the resulting powders are collected in the exhaust filter. The powders are produced in the tube at temperatures of 1200, 1400, and 1600 °C under various gas atmosphere conditions. In the first option, argon Ar gas is used for mist transportation and ammonia NH3 gas serves as a reactive medium, while in the second option nitrogen N2 is exclusively applied. Powder X-Ray Diffraction (XRD) results confirm the highly amorphous nature of all products except those made at 1600 °C in nitrogen. SEM examination shows the spheroidal particle morphology of powders, which is typical for this method. Fourier Transform Infrared (FT-IR) spectroscopy reveals the presence of Si–N and Si–O bonds in the powders prepared under Ar/NH3, whereas those produced under N2 additionally contain Si–C bonds. Raman spectroscopy measurements also support some turbostratic free carbon C in the products prepared under nitrogen. The directly determined O- and N-contents provide additional data linking the process conditions with specific powder composition, especially from the point of view of oxygen replacement in the Si–O moieties formed upon initial precursor decomposition reactions by nitrogen (from NH3 or N2) or carbon (from the carbonization of the organic groups).

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Thermal evolution of ladder-like silsesquioxanes during formation of black glasses

Cited by 24 publications

References 44 publications

Bioactive layers based on black glasses on titanium substrates

Bioactive layers based on black glasses on titanium substrates

Chemical Structure and Microstructure Characterization of Ladder-Like Silsesquioxanes Derived Porous Silicon Oxycarbide Materials

Amorphous Silicon Oxynitride-Based Powders Produced by Spray Pyrolysis from Liquid Organosilicon Compounds

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