The preparation of poly(methylsilsesquioxane) network-polyimide hybrid materials by the sol-gel process and their properties

1994 ◽  
Vol 6 (1) ◽  
pp. 43-52 ◽  
Author(s):  
Yoshitake Iyoku ◽  
Masa-aki Kakimoto ◽  
Yoshio Imai
Keyword(s):  
Hybrid Materials ◽  
Sol Gel ◽  
Tensile Modulus ◽  
Hybrid Films ◽  
Elongation At Break ◽  
Dimethyl Acetamide ◽  
Flexible Films ◽  
Sol Gel Process ◽  
Heating Up ◽  
Silicone Content

Poly(methylsilsesquixoane) network (silicone)-polyimide hybrid materials were successfully prepared by the sol-gel reaction of methyltriethoxysilane (MTES). The ethoxysilyl group in MTES was hydrolyzed and polycondensed in the solution of the polyamic acid, derived from pyromellitic dianhydride and bis(4-aminophenyl)ether, in N,N-dimethyl-acetamide (DMAc). The hybrid films were obtained by casting the reaction mixture, followed by heating up to 300°C. The hybrid materials containing 0-60wt% of silicone afforded flexible films. The films containing less than 7 wt% silicone were yellow and transparent, whereas the films with higher silicone content were yellow and opaque. Silicone particles with a diameter of around 1-10 μm were observed in the fracture surface of the hybrid films by scanning electron microscopy. Although the tensile strength and tensile modulus of the films obtained decreased with increasing silicone content. the value of the elongation at break remained at 60% up to 30% silicone content.

The preparation of new poly(phenylsilsesquioxane)-polyimide hybrid films by the sol-gel process and their properties

1994 ◽  
Vol 6 (1) ◽  
pp. 53-62 ◽  
Author(s):  
Yoshitake Iyoku ◽  
Masa-aki Kakimoto ◽  
Yoshio Imai
Keyword(s):  
Nmr Spectra ◽  
Sol Gel ◽  
Tensile Modulus ◽  
Heating Process ◽  
Hybrid Films ◽  
Polyamic Acid ◽  
Sol Gel Process ◽  
Polyimide Matrix ◽  
Polyimide Precursor ◽  
Silicone Content

The preparation of poly(phenylsilsesquioxane)-polyimide hybrid films was successfully performed with phenyltriethoxysilane (PhTES) and the polyamic acid (polyimide precursor) prepared from 4.4'-oxydianiline (ODA) and pyromellitic dianhydride (PMDA). During the heating process at 300 C, the imidization of the polyamic acid and the sol-gel reaction, hydrolysis and condensation of PhTES, proceeded simultaneously. The IR spectrum and the t3C-NMR and 29Si-NmR spectra showed that the sol-gel reaction of PhTES proceeded in the polymer matrix with high conversion. The hybrid films with a silsesquioxane content up to 75 wt% were obtained as the self-standing form. The hybrid films having a silsesquioxane content of 45 wt% were yellow and transparent, and those having more silicone content were yellow and translucent. The therma] properties of the hybrid films were improved to some extent by the introduction of the silsesquioxane component into the polyimide matrix. With respect to the tensile properties. the tensile strength remained around 85 MPa up to a silicone content of 45 wt%. This value was twice that of the hybrid films based on methyltriethoxysilane. The tensile modulus decreased with increasing silsesquioxane content.

Preparation Of Polyimide-Silica Hybrid Films

1991 ◽  
Vol 227 ◽  
Author(s):  
Masa-aki Kakimoto ◽  
Atsushi Morikawa ◽  
Yoshitake Iyoku ◽  
Yoshio Imai
Keyword(s):  
Linear Thermal Expansion Coefficient ◽  
Sol Gel ◽  
Linear Thermal Expansion ◽  
Tensile Modulus ◽  
Decomposition Temperature ◽  
Silica Content ◽  
Hybrid Films ◽  
Elongation At Break ◽  
Flexible Films ◽  
Silica Hybrid

ABSTRACTPolyimide-silica hybrid films were successfully prepared by the sol-gel reaction starting from a mixture of tetraethoxysilane (TEOS), a solution ofpolyamic acid in N, N-dimethylacetamide and water of pH 7 and pH 3. The hybrid films were obtained by the hydrolysis-polycondensation of TEOS in the polyamic acid solution, followed by heating at 270°C. Fairly flexible films were obtained for silica contents up to 70 wt%. The films containing less than 8 wt% of silica were yellow and transparent, whereas the films with higher silica contents were yellow and opaque. The density of the silica in the hybrid films was estimated to be 1.65 and 1.69 g/cm3 (pH 7 and pH 3). The29Si nuclear magnetic resonance spectrum indicated that the silica in the films consisted of non-hydroxy, monohydroxy, and dihydroxy siloxane structures. Silica particles with submicron diameter were observed in the hybrid films containing less than 8 wt% silica, whereas larger particle size around 5 μ m in the case of higher silica content. The decomposition temperature of the hybrid films increased with increasing silica content. The glass transition temperature of the hybrid films showed the minimum at 8 wt% of silica content. Tensile properties, such as elongation at break, tensile strength, and tensile modulus also exhibited the same tendency. The linear thermal expansion coefficient of the silica in the hybrid films was estimated to be 1.3 × 10−5 and 0.3 × 10−5 (pH 7 and pH 3), which suggested that the silica had a porous structure.

Study on the Dielectric Properties of Hybrid and Porous Polyimide-Silica Films

2008 ◽  
Vol 47-50 ◽  
pp. 973-976 ◽  
Author(s):  
Yi He Zhang ◽  
Qing Song Su ◽  
Li Yu ◽  
Hong Zheng ◽  
Hai Tao Huang ◽  
...  
Keyword(s):  
Dielectric Constant ◽  
Sol Gel ◽  
Silica Particles ◽  
Low Dielectric Constant ◽  
Hybrid Films ◽  
Porous Films ◽  
Silica Films ◽  
Low Dielectric ◽  
Dimethyl Acetamide ◽  
Sol Gel Process

A sol-gel process was used to prepare polyimide-silica hybrid films from the polyimide precursors and TEOS in N,N- dimethyl acetamide, then the hybrid film was treated with hydrofluoric acid to remove the dispersed silica particles, leaving pores with diameters between 80nm to 1µm, depending on the size of silica particles. The structure and dielectric constant of the hybrid and porous films were characterized by FTIR,SEM. The porous films displayed relatively low dielectric constant compared to the hybrid polyimide-silica films.

scholarly journals Preparation and Performance of Nano-hybrids Synthesized from Polyimide and Silica

2009 ◽  
Vol 2 (1) ◽  
pp. 99-107 ◽  
Author(s):  
S. M. M. Alam
Keyword(s):  
Sol Gel ◽  
Tensile Modulus ◽  
Mechanical Analysis ◽  
Hybrid Films ◽  
Scanning Calorimetry ◽  
Chemical Structures ◽  
Sol Gel Process ◽  
Biphenyltetracarboxylic Dianhydride ◽  
Silica Hybrid

Polyimide (PI)-inorganic like silica hybrid films were successfully prepared to combine the good performances of silica like tensile modulus, thermal stability etc. into organic PI. Polyamic acid (PAA), precursor of PI, was prepared from 3, 3′, 4, 4′-biphenyltetracarboxylic dianhydride (BPDA), p-phenylediamine (PDA) and in-situ formed silica was formed into PAA from tetraethoxysilane (TEOS) through in-situ sol-gel process. The films were transparent and became translucent in presence of up to 10% inorganic contents. The chemical structures were characterized by Fourier transform infrared spectroscopy (FTIR). The morphology of the films was investigated by scanning electronic microscopy (SEM). Differential scanning calorimetry (DSC), thermogravimetry analysis (TGA), stress-strain tests and dynamic mechanical analysis (DMA) were used to evaluate the performances of the films. The results indicated that the glass-transition temperatures (Tg) and decomposition temperatures of the PI-silica hybrid films were higher than those of pristine PI. Tensile modulus, tensile strength of PI increased prominently in presence of small amount (1%) of silica in PI-silica hybrid. Keywords: Polyimide; Hybrid; Sol-gel process. © 2010 JSR Publications. ISSN: 2070-0237 (Print); 2070-0245 (Online). All rights reserved. DOI: 10.3329/jsr.v2i1.2733                 J. Sci. Res. 2 (1), 99-107 (2010)  

UV Curable Organic-Inorganic Hybrid Materials

2000 ◽  
Vol 628 ◽  
Author(s):  
Guang-Way Jang ◽  
Ren-Jye Wu ◽  
Yuung-Ching Sheen ◽  
Ya-Hui Lin ◽  
Chi-Jung Chang
Keyword(s):  
Hybrid Materials ◽  
Colloidal Silica ◽  
Sol Gel ◽  
Solution Ph ◽  
Uv Curable ◽  
Inorganic Hybrid ◽  
Degradation Temperature ◽  
Sol Gel Process ◽  
The Stability ◽  
Thermal Degradation Temperature

This work successfully prepared an UV curable organic-inorganic hybrid material consisting of organic modified colloidal silica. Applications of UV curable organic-inorganic hybrid materials include abrasion resistant coatings, photo-patternable thin films and waveguides. Colloidal silica containing reactive functional groups were also prepared by reacting organic silane and tetraethyl orthosilicate (TEOS) using sol-gel process. In addition, the efficiency of grafting organic moiety onto silica nanoparticles was investigated by applying TGA and FTIR techniques. Experimental results indicated a strong interdependence between surface modification efficiency and solution pH. Acrylate-SiO2 hybrid formation could result in a shifting of thermal degradation temperature of organic component from about 200°C to near 400°C. In addition, the stability of organic modified colloidal silica in UV curable formula and the physical properties of resulting coatings were discussed. Furthermore, the morphology of organic modified colloidal silica was investigated by performing TEM and SEM studies‥

Synthesis and Intermolecularly Mediated Assembly of Organic Pigment in Hybrid Coating Films

1998 ◽  
Vol 519 ◽  
Author(s):  
Y. Yan ◽  
Z. Duan ◽  
D.-G. Chen ◽  
S. Ray Chaudhuri
Keyword(s):  
Sol Gel ◽  
Hybrid Coating ◽  
Hypsochromic Shift ◽  
Hybrid Films ◽  
Coating Films ◽  
Organic Pigment ◽  
Inorganic Hybrid ◽  
Matrix Interactions ◽  
Sol Gel Process

AbstractThe insoluble, strongly hydrogen bonded organic pigment of 3,6-bis-(4-chlorphenyl)-l,4- diketopyrrolo [3,4-c] pyrrole was transiently blocked by adding carbamate groups, and consequently incorporated into organic-inorganic hybrid matrices by a sol-gel process. The homo- (pigment-pigment) and hetero-intermolecular (pigment-matrix) interactions were found to control both the assembly and dispersion of pigment molecules in the hybrid coating films. A weaker interaction between matrices and pigment molecules results in aggregation of the carbamate pigment in the methyl-silicate films. A stronger interaction forms a homogenous dispersion and coloration of the phenyl-silicate films. The as-prepared methyl- and phenylsilicate films doped with the organic pigment were distinguished by a morphology change and a blue (hypsochromic) shift in absorption from 550 to 460 nm. Thermal treatment can remove the carbamate groups and in-situ form the organic pigment in the hybrid films.

scholarly journals Preparation of Polyimide-Silica Hybrid Films Using Sol-Gel Process.

1992 ◽  
Vol 5 (2) ◽  
pp. 393-396 ◽  
Author(s):  
Atsushi Morikawa ◽  
Hidehiro Yamaguchi ◽  
Yoshitake Iyoku ◽  
Masa-aki Kakimoto ◽  
Yoshio Imai
Keyword(s):  
Sol Gel ◽  
Hybrid Films ◽  
Sol Gel Process ◽  
Silica Hybrid

Synthesis and characterization of hybrid films from hyperbranched polyester using a sol-gel process

2013 ◽  
Vol 131 (3) ◽  
pp. n/a-n/a ◽  
Author(s):  
Amélie Houel ◽  
Jocelyne Galy ◽  
Aurélia Charlot ◽  
Jean-François Gérard
Keyword(s):  
Sol Gel ◽  
Synthesis And Characterization ◽  
Hyperbranched Polyester ◽  
Hybrid Films ◽  
Sol Gel Process

Organic–inorganic hybrids having a talc-like structure as suitable hosts to guest a wide range of species

2018 ◽  
Vol 47 (9) ◽  
pp. 2925-2932 ◽  
Author(s):  
J. Brendlé
Keyword(s):  
Hybrid Materials ◽  
Sol Gel ◽  
Step Method ◽  
Mild Conditions ◽  
Condensation Reactions ◽  
Wide Range ◽  
Sol Gel Process ◽  
Hydrolysis And Condensation ◽  
One Step

The sol–gel process involving hydrolysis and condensation reactions is an attractive way to form siloxane based hybrid materials since it is a one-step method performed under mild conditions.

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