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1.
Growth mechanism and structure of electrochemically synthesized dendritic polymethylsilane molecules
Matjaž Valant, Gregor Mali, Artem V. Badasyan, Andraž Mavrič, 2017, izvirni znanstveni članek

Opis: The study of an electrochemical synthesis of polymethylsilane from trifunctional trichloro- methylsilane monomers identified a single polymerization pathway involving reduction of the monomer to silyl anions and their addition to the growing polymer. The sizes of the synthesized macromolecules, measured with dynamic light scattering, are much larger than the theoretical size estimated for an ideal dendrimer. The reason for this, found by NMR analysis, is in a large number of branching irregularities (defects) contained in the molecular structure, which can be described as a hyperbranched dendritic polymer. Theoretical estimates of sizes for an ideal dendrimer were corrected assuming a branching defect is a cavity with the volume of one monomer. Appropriateness of the theoretical and experimental models was confirmed with a good quantitative agreement between the experimental densities and the theoretically calculated values.
Najdeno v: ključnih besedah
Ključne besede: Polymethylsilane Dendritic polymer Electropolymerization
Objavljeno: 20.03.2017; Ogledov: 982; Prenosov: 0
.pdf Polno besedilo (705,04 KB)

2.
The electrochemical synthesis of dendritic polymethylsilane
Matjaž Valant, Gregor Mali, Artem V. Badasyan, Andraž Mavrič, 2017, objavljeni povzetek znanstvenega prispevka na konferenci

Najdeno v: ključnih besedah
Povzetek najdenega: ... electropolymerization, polysilane, dendrimer...
Ključne besede: electropolymerization, polysilane, dendrimer
Objavljeno: 11.09.2017; Ogledov: 838; Prenosov: 0
.pdf Polno besedilo (152,81 KB)

3.
Amorphous nanocomposite of polycarbosilanes and aluminum oxide
Andraž Mavrič, 2018, doktorska disertacija

Opis: This work presents a paradigm for high temperature stabilization of bulk amorphous aluminium oxide. The thermodynamic stabilization is achieved by preparing a nanocomposite, where polymethylsilane dendritic molecules are dispersed in an aluminium hydroxide gel. Upon heat-treatment the gel transforms to the amorphous aluminium oxide that is stable up to 900°C. The dispersion of the macromolecules and their covalent bonding to the alumina matrix induce homogeneously distributed strain fields that keep the alumina amorphous. The first part of the thesis focuses on the synthesis, characterization and solubility properties of the dendritic polymethylsilane. The polymethylsilane is synthetized by electrochemical polymerization from trichloromethylsilane monomer. The polymerization mechanism, involving a single polymerization pathway, is identified. The polymer growth proceeds through reduction of the monomers to the silyl anions and their addition to the growing polymer. The solubility of three chemically related but topologically different polysilanes (linear, dendritic and network) were studied by dynamic light scattering. At room temperature the agglomerates in a range from 500 to 1300 nm are present. They undergo de-agglomeration at slightly elevated temperatures of around 40°C. The de-agglomeration results in formation of stable solutions, where a hydrodynamic diameter of the individual polymer molecules was measured to be in a range from 20 to 40 nm. The obtained diameters of two dendritic polymethylsilane macromolecules, synthesized under different electrolysis conditions, are much larger than the theoretical size estimated for an ideal dendrimer. We determined by 29Si NMR that the reason for this is in a large number of branching irregularities (defects) contained in the molecular structure. Combining the experimental values obtained by DLS and density measurements with a structural model that considers the branching irregularities, it is shown that the inclusion of the defects allows the dendritic polymer to exceed the sterical limitations and form the hyperbranched dendritic structure. The final size depends on a relative amount of the branching defects. In the second part, the synthetized polymethylsilane molecules were successfully used for the nanocomposite formation. The aluminium hydroxide gel with the dispersed polymethylsilane molecules was prepared as a precursor. Upon heat-treatment it gives the amorphous aluminium oxide stable up to 900°C. The dispersed macromolecules induce homogeneously distributed strain fields that keep the aluminium oxide amorphous during the thermal treatment the dispersed macromolecules covalently bind to the matrix, inducing the interface strain. The amorphous state was confirmed by the presence of penta-coordinated aluminium detected by 27Al NMR and a low bandgap measured by UV-vis absorption spectroscopy.
Najdeno v: ključnih besedah
Povzetek najdenega: ...amorphous aluminium oxide, polymethylsilane, nanocomposite, electropolymerization, solubility, agglomeration, de-agglomeration, dendrimer, hyperbranched dendritic...
Ključne besede: amorphous aluminium oxide, polymethylsilane, nanocomposite, electropolymerization, solubility, agglomeration, de-agglomeration, dendrimer, hyperbranched dendritic structure, dynamic light scattering, thermal analysis, transmission electron microscopy, scanning electron microscopy, X-ray diffraction, infrared spectroscopy, UV-Vis spectroscopy
Objavljeno: 19.07.2018; Ogledov: 1055; Prenosov: 65
.pdf Polno besedilo (5,07 MB)

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