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Fluorene-containing polyimide adhesive and preparation method thereof

A technology of fluorene polyimide and adhesive is applied in the field of fluorene-containing polyimide adhesive and its preparation, and can solve the problems of reducing bonding strength and the like

Inactive Publication Date: 2009-12-02
BEIHANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

When the adhesive joint is prepared in the form of polyamic acid solution, the volatilization of the solvent during the thermal imidization process will cause a large number of pore defects in the matrix and reduce the bond strength

Method used

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  • Fluorene-containing polyimide adhesive and preparation method thereof
  • Fluorene-containing polyimide adhesive and preparation method thereof
  • Fluorene-containing polyimide adhesive and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Fully dissolve 0.98 mol of 4,4'-diaminodiphenyl ether in the solvent N-methylpyrrolidone, add 1 mol of 3,3',4,4'-diphenylmethyl ether tetracarboxylic anhydride after 15 minutes, and After 12 hours, add 0.05mol end-capping agent α-aminofluorene, and continue to stir for 12 hours to obtain a uniform polyamic acid solution; coat the polyamic acid solution on a glass plate, and heat up in stages in a far-infrared oven to prepare part For the imidized polyimide film, the heating program is 80°C / 2h, 120°C / 1h, 150°C / 1h, 200°C / 1h.

[0028] Fully polish the metal surface with sandpaper, rinse it with acetone, and dry it in an electric blast drying oven; place a 0.04mm thick two-layer film between two metal sheets, and press it on a press according to GB7124-86 standard , the pressure is 1-2MPa, the temperature is 200°C, put it in, raise the temperature to 370°C, keep the constant pressure at this temperature for 2h, and then keep the pressure and cool down to obtain a single lap...

Embodiment 2

[0031] Fully dissolve 0.25mol of 3,3'-diaminodiphenylsulfone and 0.25mol of 9,9'-bis(2-trifluoromethyl, 4-aminophenoxyphenyl)fluorene in the solvent N-methyl In the pyrrolidone, after 15 minutes, 0.5 mol of triphenyl ether tetra-acid dianhydride was added, and stirred at room temperature; after stirring for 24 hours, a homogeneous polyamic acid solution was obtained.

[0032] The treatment mode of metal surface is the same as embodiment 1 operation. Use a glass rod to evenly coat the polyamic acid solution on the area to be bonded, dry at 120°C for 30 minutes, continue to coat the polyamic acid solution, and then dry until the thickness of the adhesive layer reaches about 0.04mm, using the GB7124-86 standard Hot press on the press, the pressure is 1-2MPa, put it in at 200°C, raise the temperature to 350°C, keep the pressure at this temperature for 2h, and then keep the pressure and cool down to get a single lap joint that is firmly bonded .

[0033] The shear strength of the...

Embodiment 3

[0035] Fully dissolve the diamine mixture of 0.04mol 9,9'-bis(4-aminophenyl)fluorene and 0.06mol 1,3-bis(4-aminophenoxy)benzene in the solvent N,N'-dimethyl In acetamide, add 0.98mol of 3,3',4,4'-benzophenone tetracarboxylic anhydride after 15min, and stir at room temperature; add 0.05mol of end-capping agent phthalic anhydride after 12h, and continue stirring for 12h Obtain a uniform polyamic acid solution; add about the same volume of N,N'-dimethylacetamide to the polyamic acid solution to dilute, stir evenly, and slowly add benzoic anhydride and aminopyridine dropwise to it using a dropping funnel After the powder starts to precipitate, continue to stir for 4 hours. After the polyimide powder is completely precipitated, pour it into ethanol, wash and filter it several times, and then vacuum dry it at 80°C for 12 hours to obtain a dry polyimide. imide powder.

[0036] The treatment mode of metal surface is the same as embodiment 1 operation. Soak the polyimide powder with ...

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Abstract

The invention provides a fluorene-containing polyimide adhesive having good adhesivity with metal, which is characterized in that: the adhesive at least comprises a fluorene-containing diamine monomer, a fluorene-containing dianhydride monomer and / or a fluorene-containing end capping agent, and at least one of other fluorene-containing diamine monomers, other fluorene-containing dianhydride monomers and / or other end capping agents. A preparation method for the fluorene-containing polyimide adhesive comprises the following steps: A, dissolving a certain amount of diamine, dianhydride or the end capping agent in organic solvent, stirring at room temperature, and obtaining even polyamic acid solution; B, preparing polyimide powder or a partial imidization polyimide film by a chemical imidization method or a heat imidization method; and C, arranging the powder with certain thickness or the film between two metal sheets, and performing hot pressing on a press for a certain period of time to obtain a single-lap joint bonded part with firm adhesivity. The fluorene-containing polyimide adhesive provided by the invention is applied in the fields of high-tech such as aviation, space flight, microelectronics, etc.

Description

technical field [0001] The invention relates to a fluorene-containing polyimide adhesive and a preparation method thereof. The adhesive contains at least one fluorene-containing diamine monomer, fluorene dianhydride-containing monomer and / or fluorene-containing end-capping agent, and at least one other diamine monomer, other dianhydride monomer and / or other end-capping agent. Background technique [0002] Adhesive is an indispensable material in the national economy, and the bonding technology has also developed maturely, becoming one of the three contemporary connection technologies alongside welding and mechanical connection. With the development of modern science and technology, space vehicles such as launch vehicles and space shuttles are developing in the direction of light weight, good reliability and long life. These new design ideas put forward higher requirements for the high temperature resistance of adhesives. Computers and other electronic equipment increase the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09J179/08
Inventor 詹茂盛安颢瑗王凯
Owner BEIHANG UNIV
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