Ternary composites by an in situ hydrolytic polymerization process.

Polyamide 6/modified silica composite materials have been prepared by a coupled polymerization procedure. For this purpose, the three-component-system we presented in a previous publication, consisting of ε-aminocaproic acid (ε-ACA), ε-caprolactam (ε-CL), and 1,1',1'',1'''-silanetetrayltetrakis-(azepan-2-one) (Si(ε-CL)4), has been combined with other silicon monomers with one or two methyl groups (MeSi(ε-CL)3 and Me2Si(ε-CL)2). The simultaneous polymerization of ε-CL and silicon monomers leads to the in situ formation of silica/polysiloxane particles and the surrounding polyamide 6 matrix in one step. Moreover, 3-aminopropyltriethoxysilane has been added to the three-component-system to achieve covalent bonding between organic and inorganic phases and to inhibit agglomeration of the silica particles. Chemical structures and morphologies of the composites have been investigated by solid-state NMR and FTIR spectroscopy as well as electron microscopy and SEC measurements. Structural effects on thermal properties have been studied by DSC and TGA measurements.

Design of nanostructured hybrid materials: twin polymerization of urethane-based twin prepolymers.

Organic-inorganic hybrid materials with urethane functionalities were obtained by simultaneous twin polymerization of twin prepolymers in combination with the ideal twin monomer 2,2'-spirobi[4H-1,3,2-benzodioxasiline]. The twin prepolymers consist of a urethane-based prepolymer with reactive terminal groups which can react during the twin polymerization process. Nanostructured hybrid materials with integrated dialkylsiloxane crosslinked urethane structures, phenolic resin and SiO2 are obtained in a one pot process. The effects of the polymerization temperature as well as those of various catalysts and reagent ratios on the polymerization behavior were investigated. The molecular structures of the obtained materials were determined by 13C- and 29Si-{1H}-CP-MAS NMR spectroscopies. HAADF-STEM-measurements were performed to prove the distribution of silicon in the hybrid material.

A non-aqueous procedure to synthesize amino group bearing nanostructured organic-inorganic hybrid materials.

Amino-functionalized organic-inorganic hybrid materials with a narrow distributed nanostructure of 2-4 nm in size were obtained by means of a template-free and non-aqueous procedure. Simultaneous twin polymerization of novel amino group containing twin monomers with 2,2'-spirobi[4H-1,3,2-benzodioxasiline] has been applied for this purpose. The amino groups of the organic-inorganic hybrid material are useful for post derivatization.

XPS studies of chemically modified banana fibers.

Banana fibers obtained from the sheath of the banana plant (Musa Sapientum) whose major constituent is cellulose were modified using various chemical agents in order to improve their compatibility with the polymer matrix. The change in the surface composition of the raw and chemically modified fiber was investigated using various techniques such as solvatochromism, electrokinetic measurements, and XPS. Surface characterization by XPS showed the presence of numerous elements on the surface of the fiber. Investigation of the surface after alkali treatment on the other hand showed the removal of most of the elements. Silane treatment was found to introduce a considerable amount of silicon on the surface of the fiber. The [O]/[C] ratio was found to decrease in all cases except for the fluorinated and vinyl silane treated fibers. Detailed investigation of the deconvoluted C 1s spectra revealed the change in the percentage atomic concentration of the various elements on the fiber surface. The dissolution of the various surface components by alkali treatment, which was earlier revealed by SEM, was further confirmed by XPS. The XPS results were found to perfectly agree with the solvatochromic and electrokinetic measurements.

Cationic host-guest polymerization of N-vinylcarbazole and vinyl ethers in MCM-41, MCM-48, and nanoporous glasses.

The synthesis of poly(vinyl ether)s or polyvinylcarbazole under the conditions of constricted geometry can be achieved by means of cationic host-guest polymerisation of the corresponding monomers in the pores of MCM-41 (pore diameter 3.6 nm), MCM-48 (pore diameter 2.4 nm) and in nanoporous glasses (Gelsil with a pore diameter of 5 nm) with bis(4-methoxyphenyl)methyl chloride (BMCC) or triphenylmethyl chloride as the internal surface initiator. The reaction products are new polymer/ MCM-41, polymer/MCM-48 etc., host-guest hybrid materials. The molecular mass of the enclosed polymer and the degree of loading of the host compounds can be adjusted within certain limits. The molecular dynamics were investigated by using broad-band dielectric spectroscopy. Under the conditions of constricted geometry, molecular fluctuation is observed as well as a secondary beta-relaxation, which is hardly affected (in comparison with the free melt) and which corresponds to the relaxation between structural substates (dynamic glass transition). This process is several orders of magnitude faster in its relaxation rate than in the free melt and thus follows a confinement effect. This is already well known in lower molecular weight systems with constricted geometry.