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Method for preparing polyimide/silicon dioxide nanometer hybridized film

A technology of silica and polyimide, which is applied in the field of synthesis and preparation of organic-inorganic hybrid materials, can solve problems such as poor dispersion, unsatisfactory improvement in mechanical and optical properties of hybrid films, and large particles. Achieve the effects of improving compatibility, improving optical transmission performance, and increasing the degree of dispersion

Inactive Publication Date: 2006-09-13
TECHNICAL INST OF PHYSICS & CHEMISTRY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The purpose of the present invention is to overcome prior art when preparing polyimide / silicon dioxide nano-hybrid film, when silicon dioxide content is higher, the dispersibility of silicon dioxide particle in matrix is ​​poor, and the particle that forms is bigger , so that the mechanical and optical properties of the hybrid film cannot be ideally improved, thus providing a polyimide with good dispersion of silica particles in the matrix, excellent mechanical and optical properties of the hybrid film / Preparation method of silicon dioxide nano-hybrid film

Method used

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  • Method for preparing polyimide/silicon dioxide nanometer hybridized film
  • Method for preparing polyimide/silicon dioxide nanometer hybridized film
  • Method for preparing polyimide/silicon dioxide nanometer hybridized film

Examples

Experimental program
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Effect test

Embodiment 1

[0039] in N 2(purity is 99.999%) under protection, in a clean three-necked flask, add 7.0084g 4,4'-diaminodiphenyl ether (ODA) (0.035mol) and 83.0gN, N'-dimethylacetamide (DMAC ), stirred for 10 min, and the mixture became clear; 4.04 g of tetraethyl orthosilicate (TEOS) (0.0194 mol) was added to 12.8 g of ethanol, and stirred evenly. 0.078 mol of deionized water, 0.0008 mol of concentrated hydrochloric acid and 0.002 mol of γ-aminopropyltriethoxysilane (GOTMS) were added dropwise, and stirred for 30 min. Form sol; Add this sol slowly in the DMAc solution of ODA, stir 2h, form uniform solution; Get 0.035mol pyromellitic dianhydride (PMDA), be divided into 3 parts, every 30min join in the above-mentioned solution, in After stirring at room temperature for 4 h, a homogeneous solution was obtained. Then apply a film on a glass plate by scraping, and carry out imidization treatment by gradually increasing the temperature—baking at 80, 100, 120, 150, 180, 240, and 270°C for 1 hou...

Embodiment 2

[0044] in N 2 (purity is 99.999%) under protection, in a clean three-necked flask, add 7.0084g 4,4'-diaminodiphenyl ether (ODA) (0.035mol) and 83.0g N, N'-dimethylacetamide ( DMAC), stirred for 10 min, and the mixture became clear; 1.44 g of tetraethyl orthosilicate (TEOS) (0.0069 mol) was added to 4.58 g of ethanol, and stirred evenly. Add 0.0276mol of deionized water, 0.00028mol of concentrated hydrochloric acid and 0.0007mol of γ-aminopropyltriethoxysilane (GOTMS) dropwise, and stir for 30min to form a sol; slowly add the sol to the DMAc solution of ODA, and stir for 2h , to form a homogeneous solution; take 0.035mol pyromellitic dianhydride (PMDA), divide it into 3 parts, add it to the above solution every 30min, and stir at room temperature for 4h to obtain a homogeneous solution. Then apply a film on a glass plate by scraping, and carry out imidization treatment by gradually increasing the temperature—baking at 80, 100, 120, 150, 180, 240, and 270°C for 1 hour to obtain...

Embodiment 3

[0048] in N 2 (purity is 99.999%) under protection, in a clean three-necked flask, add 7.0084g 4,4'-diaminodiphenyl ether (ODA) (0.035mol) and 83.0g N, N'-dimethylacetamide ( DMAC), stirred for 10 min, and the mixture became clear; 2.45 g of tetraethyl orthosilicate (TEOS) (0.0118 mol) was added to 7.74 g of ethanol, and stirred evenly. Add 0.047mol of deionized water, 0.00047mol of concentrated hydrochloric acid and 0.0012mol of γ-aminopropyltriethoxysilane (GOTMS) dropwise, and stir for 30min to form a sol; slowly add the sol to the DMAc solution of ODA, and stir for 2h , to form a homogeneous solution; take 0.035mol pyromellitic dianhydride (PMDA), divide it into 3 parts, add it to the above solution every 30min, and stir at room temperature for 4h to obtain a homogeneous solution. Then apply a film on a glass plate by scraping, and carry out imidization treatment by gradually increasing the temperature—baking at 80, 100, 120, 150, 180, 240, and 270°C for 1 hour to obtain ...

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Abstract

The invention relates to a producing process of the polyimide / silicon dioxide nm hybridization film. The method improves the existing sol-gel method; the positive silicate sol solution is added in before the forming of the polyamic acid to carry the hydrolytic condensation of the sol-gel and the macromolecule polyreaction of the polyamic acid synchronously; finally, it can be gained by the hot imine treatment of the composite composed by the polyamic and the positive silicic acid. Using the producing process of the polyimide / silicon dioxide nm hybridization film provided by the invention, the polyimide / silicon dioxide nm hybridization film stuff of separating evenly and having the physiofacies of which the size reached to the order of magnitude of 5nm-1um. Comparing with the existing technic, the method can avoid the problem of the silicon dioxide grain is difficult to be separated in the basal body because of the high solution viscosity of the polyamic acid; so it can improve the compatibility of the two phase; the ability of the mechanics and the optics of the hybirgization film is improved highly.

Description

technical field [0001] The invention belongs to the field of synthesis and preparation of organic-inorganic hybrid materials, in particular to a preparation method of polyimide / silicon dioxide nano-hybrid film. Background technique [0002] Polyimide is one of the most high-temperature-resistant and high-strength polymers at present. It can maintain the main physical properties at 550°C for a short period of time, and can be used for a long time at close to 330°C. At the same time, polyimide is also It can withstand extremely low temperature and will not be brittle in liquid nitrogen. In addition, it also has excellent dimensional and oxidation stability, chemical resistance, radiation resistance, as well as excellent toughness and flexibility, and is widely used in aerospace, electronics, precision instruments, automobile manufacturing and other fields. [0003] However, with the development of science and technology, higher requirements are put forward for the performance...

Claims

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Application Information

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IPC IPC(8): C08J5/18C08L79/08C08G73/10C08K3/22
Inventor 付绍云李元庆李艳
Owner TECHNICAL INST OF PHYSICS & CHEMISTRY - CHINESE ACAD OF SCI
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