Quantitative Evaluation of Hydrolysis Ratio and Content of Silicic Ester on Film Surface by X-ray Photoelectron Spectroscopy

Tomita, Rie; Urano, Satoshi; Kohiki, Shigemi

doi:10.4011/shikizai1937.74.460

Cited by 3 publications

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“…This showed that the SiOCH 3 bond tended to be cleaved. Changes in the spectral intensity and binding energy by unmonochromatized Mg Kα X‐ray irradiation were compared with changes in hydrolysis performed with an XPS spectrometer 42, 43. A reduction of the CO bond intensity in the C 1 s spectrum, increases in the Si and N atomic concentrations calculated from spectral intensities, and an increase in the Si 2 p binding energy were observed when unmonochromatized Mg Kα X rays were irradiated for 8 h to the 2c film surface immediately after preparation.…”

Section: Resultsmentioning

confidence: 99%

“…Changes in the spectral intensity and binding energy by unmonochromatized Mg K␣ X-ray irradiation were compared with changes in hydrolysis performed with an XPS spectrometer. 42,43 A reduction of the COO bond intensity in the C 1s spectrum, increases in the Si and N atomic concentrations calculated from spectral intensities, and an increase in the Si 2p binding energy were observed when unmonochromatized Mg K␣ X rays were irradiated for 8 h to the 2c film surface immediately after preparation. The same four changes were observed for 2c forced to hydrolyze alkoxy groups via soaking in 2.5 wt % dilute sulfuric acid at room temperature for 12 h. In this case, the reduction of the COO bond intensity in the C 1s spectrum and the increase in the Si 2p binding energy were caused by the hydrolysis reaction of methoxy groups.…”

Section: Decomposition Of Polyalkoxysiloxane On the Film Surface By Mmentioning

confidence: 99%

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Characterization of the surface content, hydrolysis ratio, and condensation degree of polyalkoxysiloxane segregated to the surface of a polyurethane crosslinked film by X‐ray photoelectron spectroscopy

Tomita

Urano

Kohiki

2002

J. Polym. Sci. A Polym. Chem.

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We report, using an electron spectrometer equipped with both monochromatized Al Kα and unmonochromatized Mg Kα sources, the quantitative characterization of the surface content, hydrolysis ratio, and condensation degree of polyalkoxysiloxane segregated to the surface of a polyurethane crosslinked film consisting of acryl polyol, polyisocyanate, and polyalkoxysiloxane. Unmonochromatized Mg Kα X‐ray irradiation extremely accelerated the decomposition of alkoxy groups of polyalkoxysiloxane. The surface content and hydrolysis ratio were determined from C 1s, Si 2p, and N 1s spectral intensities measured with monochromatized Al Kα X rays after decomposition by unmonochromatized Mg Kα X‐ray irradiation. The condensation degree was determined by the kinetic energy of the silicon KLL Auger electron after decomposition. We applied the established characterization method for a polyurethane film containing polyalkoxysiloxane. After 20 days, the surface content of polyalkoxysiloxane was greater than 60 wt %, the hydrolysis ratio ranged from 0.8 to 0.95, and the higher hydrolysis ratio resulted in a larger condensation degree. The hydrophilicity of the film surface became higher as the surface content and hydrolysis ratio increased, and the crack density became higher as the condensation degree increased. A method for characterizing the practical properties of coating film surfaces containing polyalkoxysiloxane was established. © 2002 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 40: 2917–2926, 2002

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Section: Resultsmentioning

confidence: 99%

Section: Decomposition Of Polyalkoxysiloxane On the Film Surface By Mmentioning

confidence: 99%

Characterization of the surface content, hydrolysis ratio, and condensation degree of polyalkoxysiloxane segregated to the surface of a polyurethane crosslinked film by X‐ray photoelectron spectroscopy

Tomita

Urano

Kohiki

2002

J. Polym. Sci. A Polym. Chem.

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“…In coating materials for architecture, one of the methods to improve the coating surface relies on an organic–inorganic hybridization using a condensed alkyl silicate of tetra alkoxyl silane 9. Tomita et al reported the additional effect and the morphology of the condensed alkyl silicate of tetra alkoxyl silane in the coating layer 10, 11. This method is effective for the solvent‐based coating of two liquid types, and gives a hydrophilic property to the material because of the hydrolysis of alkyl silicate during film formation.…”

Section: Introductionmentioning

confidence: 99%

Properties of organic–inorganic composite materials prepared from acrylic resin emulsions and colloidal silicas

Wada

Inui²,

Uragami

2006

J of Applied Polymer Sci

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ABSTRACT:To design an organic-inorganic composite material with colloidal silica as the inorganic component, an acrylic resin emulsion and an organic silane hybridized acrylic resin emulsion were prepared by emulsion polymerization. The organic-inorganic composite films were prepared by blending the emulsion and the colloidal silica. The contact angles for water, gloss at 60°, and the transparencies of those films were measured. The dispersion state of colloidal silica in films was observed with a scanning electron microscope (SEM) and a transmission electron microscope (TEM). From these results, the contact angle for water of the organic-inorganic composite film obtained from the silane hybridized acrylic resin emulsion was lower than that of the organic-inorganic composite film obtained from an acrylic resin emulsion. The contact angles for water in organicinorganic composite films with colloidal silicas were lower than those of the films without the colloidal silicas. The films prepared from silane hybridized acrylic resin emulsion composites with colloidal silicas of less than 100 nm were more hydrophilic. SEM and TEM observations demonstrated that some aggregations of the small colloidal particle silica were densely dispersed on the film surface.

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“…Organicinorganic composite materials have thus been investigated for a variety of applications including medicine, electronics, cosmetics, adhesives, surface coatings, [9][10][11] and separation membranes. [12][13][14][15][16][17] Tomita et al [18][19][20] have reported an additional effect of hydrophilicity and the morphology of the condensed alkyl silicate of tetraalkoxysilane in the coating layer of architectural coating materials. Their method, which is effective for coatings containing two liquids, confers hydrophilicity to the material due to the hydrolysis of alkyl silicate during the film formation.…”

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confidence: 99%

Preparation and characteristics of a waterborne preventive stain coating material with organic-inorganic composites

Wada¹,

Uragami

2006

J Coat. Technol. Res.

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With the goal of developing a waterborne coating material that prevents staining, organic-inorganic composites prepared from colloidal silica and two types of acrylic resin emulsions were investigated as exterior coatings. Conventional acrylic resin emulsion and organic silane hybridized acrylic resin emulsion prepared by emulsion polymerization were mixed with colloidal silica to form organic-inorganic composite films. The addition of colloidal silica to emulsions yielded films with higher hydrophilicities, as indicated by lower water contact angles for these films in comparison to films without colloidal silica. The water contact angles of organic silane hybridized acrylic resin emulsion/colloidal silica films were lower than those of acrylic resin emulsion/colloidal silica films. Composite films containing colloidal silica particles smaller than 100 nm in diameter showed high hydrophilicities. Observations of the dispersed state of colloidal silica particles in organic-inorganic composite films by scanning electron microscopy (SEM) and transmission electron microscopy (TEM) demonstrated that colloidal silica particles were densely aggregated on the film surface. Outdoor exposure tests of the coating materials prepared from organic silane hybridized acrylic resin and colloidal silica particles with diameters of 7.5 nm showed excellent stain resistance.

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Quantitative Evaluation of Hydrolysis Ratio and Content of Silicic Ester on Film Surface by X-ray Photoelectron Spectroscopy

Cited by 3 publications

References 0 publications

Characterization of the surface content, hydrolysis ratio, and condensation degree of polyalkoxysiloxane segregated to the surface of a polyurethane crosslinked film by X‐ray photoelectron spectroscopy

Characterization of the surface content, hydrolysis ratio, and condensation degree of polyalkoxysiloxane segregated to the surface of a polyurethane crosslinked film by X‐ray photoelectron spectroscopy

Properties of organic–inorganic composite materials prepared from acrylic resin emulsions and colloidal silicas

Preparation and characteristics of a waterborne preventive stain coating material with organic-inorganic composites

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