CN112251188B - Heat-conducting adhesive film suitable for bonding optical load structure and preparation method thereof - Google Patents
Heat-conducting adhesive film suitable for bonding optical load structure and preparation method thereof Download PDFInfo
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- CN112251188B CN112251188B CN202011184410.8A CN202011184410A CN112251188B CN 112251188 B CN112251188 B CN 112251188B CN 202011184410 A CN202011184410 A CN 202011184410A CN 112251188 B CN112251188 B CN 112251188B
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J179/00—Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen, with or without oxygen, or carbon only, not provided for in groups C09J161/00 - C09J177/00
- C09J179/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/06—Non-macromolecular additives organic
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J7/00—Adhesives in the form of films or foils
- C09J7/10—Adhesives in the form of films or foils without carriers
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J7/00—Adhesives in the form of films or foils
- C09J7/30—Adhesives in the form of films or foils characterised by the adhesive composition
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
- C09K5/08—Materials not undergoing a change of physical state when used
- C09K5/14—Solid materials, e.g. powdery or granular
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2479/00—Presence of polyamine or polyimide
- C09J2479/08—Presence of polyamine or polyimide polyimide
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- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Combustion & Propulsion (AREA)
- Thermal Sciences (AREA)
- Materials Engineering (AREA)
- Adhesives Or Adhesive Processes (AREA)
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Abstract
A heat-conducting glue film suitable for bonding an optical load structure and a preparation method thereof; belongs to the field of aerospace materials. The invention aims to solve the problems that the conventional modified epoxy adhesive film has high vacuum condensable volatile matter and poor thermal conductivity and cannot meet the bonding requirement of a high-precision and high-resolution satellite optical load structure. The method comprises the following steps: adding dodecylamine modified graphene oxide into an acetone solution of epoxy resin, heating, stirring, reacting, washing with excessive dichloromethane after the reaction is finished, and filtering to obtain DA-GO uniformly coated by the epoxy resin; uniformly mixing cyanate ester resin and polyetherimide, heating and melting, mechanically stirring to be uniform, cooling to 110-130 ℃, then respectively adding DA-GO coated by epoxy resin and a transition metal salt accelerator, and mechanically mixing to be uniform by using a rubber mixing mill; and then pressed into a film. The adhesive film has the advantages of enhanced thermal conductivity, low condensable volatility and good adhesive property.
Description
Technical Field
The invention belongs to the field of aerospace materials; in particular to a heat-conducting adhesive film suitable for bonding an optical load structure and a preparation method thereof.
Background
With the continuous improvement of the functionality and the integration of the spacecraft, higher requirements are put forward on the vacuum gassing characteristic and the thermal conductivity of a spacecraft structure, particularly an optical load structure. The honeycomb sandwich structure is a special composite material for a structure, and is widely applied to a spacecraft structure with special requirements on weight and performance due to the characteristics of high specific strength, high specific rigidity and the like. The honeycomb sandwich structure is formed by clamping a honeycomb-shaped sandwich material between two panels and bonding the two panels by using adhesive films, wherein the performance of the adhesive films directly influences the performance of the bonded structure. However, the existing modified epoxy structural adhesive film has the defects of high vacuum condensable volatile matter, no heat conduction function and incapability of meeting the bonding requirement of a honeycomb sandwich structure of an optical load structure of a high-precision and high-resolution spacecraft. Therefore, it is highly desirable to develop a thermally conductive adhesive film with low volatility.
Disclosure of Invention
Aiming at the problems that the existing modified epoxy adhesive film has high vacuum condensable volatile matter and poor thermal conductivity and cannot meet the bonding requirement of a high-precision and high-resolution satellite optical load structure, the invention provides the thermal conductive adhesive film suitable for bonding the optical load structure and the preparation method thereof, wherein a three-dimensional thermal conductive passage is formed by introducing graphene oxide into main resin, so that the thermal conductive function of the adhesive film is realized; meanwhile, the polyetherimide with low volatility is adopted to modify the main resin, so that the toughness and the shear strength of the adhesive film can be effectively improved, and the adhesive film has low condensable volatility and good bonding performance.
The invention aims to realize the technical scheme that a heat-conducting adhesive film suitable for bonding an optical load structure is mainly prepared from graphene oxide powder, dodecylamine, epoxy resin, cyanate ester resin and polyetherimide; the preparation method comprises the following steps:
step one, ultrasonically dispersing graphene oxide powder in distilled water, adding a dodecylamine ethanol solution to obtain a mixed solution A, stirring at room temperature for 24 hours, then adding hydrazine monohydrate, carrying out reflux heating, repeatedly washing with a deionized water and absolute ethanol mixed solution for at least 3 times, and carrying out vacuum drying to obtain dodecylamine modified graphene powder;
dissolving a small amount of epoxy resin in a certain volume of acetone, adding a certain mass of dodecylamine modified graphene powder, heating, stirring and reacting for a certain time, and washing and filtering with excessive dichloromethane after the reaction is finished to obtain DA-GO uniformly coated with the epoxy resin;
step three, uniformly mixing cyanate ester resin and polyetherimide, heating and melting, mechanically stirring to be uniform to obtain main resin, cooling to 110-130 ℃, then respectively adding DA-GO coated by epoxy resin and a transition metal salt accelerator, and mechanically mixing to be uniform by using a rubber mixing mill to obtain a rubber material;
and step four, pressing the sizing material obtained in the step three into a film by a film pressing machine under the heating condition to obtain the heat-conducting adhesive film.
Further limiting, the feeding ratio of the graphene oxide and the distilled water in the first step is 1g:100 mL.
Further, in the first step, the dodecylamine ethanol solution is obtained by dissolving dodecylamine in absolute ethanol according to a feed ratio of 3g:100mL of dodecylamine to absolute ethanol.
Further limiting, the usage amount of the hydrazine monohydrate in the step one accounts for 5-10% of the volume of the mixed solution A.
Further limiting, in the step one, the reflux heating is carried out for 18 to 24 hours at the temperature of 70 ℃.
Further defined, in step one, vacuum drying is carried out at 80 ℃ for 24 hours.
Further limiting, the charging ratio of the epoxy resin, the acetone and the dodecylamine modified graphene powder in the second step is 1g:50mL:3 g.
Further limiting, the heating reaction condition in the second step is that the stirring reaction is carried out for 1 to 3 hours under the condition of 60 ℃.
Further limiting, in the third step, the mass ratio of the cyanate ester resin to the polyetherimide resin is 100: (5-20).
Further limiting, in the third step, the heating and melting temperature is 150-170 ℃, and the mechanical stirring time is 60-90 min.
Further limited, in the third step, the accelerant is one or a mixture of several of zinc acetylacetonate, cobalt acetylacetonate and nickel acetylacetonate transition metal salt according to any ratio, and the addition amount accounts for 0.5% -1.0% of the total mass of the main resin.
Further limiting, in the third step, the temperature is reduced to 110-130 ℃, and the addition mass of the DA-GO coated by the epoxy resin accounts for 10% -15% of the total mass of the main resin.
Further limiting, in the fourth step, the film is pressed at the temperature of 60-100 ℃ to form the film, and the thickness of the obtained adhesive film is 0.1-0.5 mm.
According to the invention, graphene oxide is subjected to surface chemical modification and then subjected to chemical bonding reaction with an epoxy group of epoxy resin, so that the epoxy resin is uniformly wrapped on the surface of the graphene oxide, and then the epoxy resin and cyanate are subjected to pre-reaction and are effectively bonded with a main body of cyanate ester resin, so that the graphene oxide is uniformly dispersed in the cyanate ester resin matrix to form a three-dimensional heat-conducting network passage, and the heat-conducting property of a glue film is improved; in addition, the thermoplastic polyetherimide is adopted to toughen and modify the cyanate ester to form a semi-interpenetrating network structure, so that the toughness and the shear strength of the glue film can be effectively improved, the shear strain of the glue film is improved, and the peeling strength of the aluminum honeycomb sandwich material and the composite material structure is increased.
The thermoplastic polyetherimide resin is adopted, and the condensable volatile matter of the thermoplastic polyetherimide resin is less, and the graphene oxide sheet layer structure in the cross-linked network formed after the adhesive film is cured can prevent small molecules from escaping, so that the obtained heat-conducting adhesive film has the characteristic of low condensable volatile.
Detailed Description
Example 1, the thermally conductive adhesive film suitable for bonding the optical load structure of this example is implemented by the following steps:
firstly, ultrasonically dispersing 0.5g of graphene oxide in 50mL of distilled water, adding an ethanol solution of Dodecylamine (DA), stirring for 24 hours at room temperature, then adding 5mL of hydrazine monohydrate, refluxing and heating for 20 hours at 70 ℃, repeatedly washing an obtained product for 3 times by using a mixed solution of deionized water and absolute ethyl alcohol, and carrying out vacuum drying for 24 hours at 80 ℃ to obtain dodecylamine modified graphene powder (DA-GO);
wherein the ethanol solution of Dodecylamine (DA) is prepared by dissolving 1.5g of Dodecylamine (DA) in 50mL of anhydrous ethanol, and mixing.
And secondly, dissolving 1g of epoxy resin in 50mL of acetone, adding 3g of DA-GO, stirring and reacting at 60 ℃ for 2h, washing and filtering with excessive dichloromethane to obtain the DA-GO uniformly coated by the epoxy resin.
And thirdly, mixing 100g of cyanate ester resin and 20g of polyetherimide, heating and melting at 160 ℃, mechanically stirring for 90min to obtain main resin, cooling to 120 ℃, then respectively adding 15g of epoxy resin-coated DA-GO and 0.5g of zinc acetylacetonate transition metal salt accelerator, and mechanically mixing on a rubber mixing mill until the mixture is in a uniform phase to obtain the sizing material.
Fourthly, preheating the sizing material obtained in the third step for 30min at the temperature of 80 ℃, and pressing the sizing material into a 0.3mm glue film through a film pressing machine to obtain the heat-conducting glue film.
The thermal conductivity of the thermal conductive adhesive film obtained in the embodiment is tested, the longitudinal thermal conductivity coefficient of the thermal conductive adhesive film is 1.05W/m.K, the condensable volatile component of the thermal conductive adhesive film is 0.008% after being cured and is tested in a vacuum environment, the mass loss rate is 0.20 wt%, the shear strength at room temperature is greater than 20MPa, and the peel strength at room temperature of 90 degrees is greater than 20N/cm. Therefore, the heat-conducting adhesive film completely meets the bonding requirement of the satellite optical load structure.
Claims (10)
1. A heat-conducting adhesive film suitable for bonding an optical load structure is characterized in that the heat-conducting adhesive film is mainly made of graphene oxide, dodecylamine, epoxy resin, cyanate ester resin and polyetherimide;
wherein, the preparation method comprises the following steps: step one, ultrasonically dispersing graphene oxide in distilled water, adding a dodecylamine ethanol solution to obtain a mixed solution A, stirring at room temperature for 24 hours, then adding hydrazine monohydrate, carrying out reflux heating, repeatedly washing with a deionized water and absolute ethanol mixed solution for at least 3 times, and carrying out vacuum drying to obtain dodecylamine modified graphene powder;
dissolving epoxy resin in acetone with a certain volume, adding dodecylamine modified graphene powder with a certain mass, heating, stirring, reacting, washing and filtering with excessive dichloromethane after the reaction is finished, and obtaining DA-GO uniformly coated with epoxy resin;
step three, uniformly mixing cyanate ester resin and polyetherimide, heating and melting, mechanically stirring to be uniform to obtain main resin, cooling to 110-130 ℃, respectively adding DA-GO coated by epoxy resin and a transition metal salt accelerator, and mechanically mixing to be uniform by using a rubber mixing mill to obtain a rubber material;
and step four, pressing the sizing material obtained in the step three into a film by a film pressing machine under the heating condition to obtain the heat-conducting adhesive film.
2. The method according to claim 1, wherein the method comprises the following steps:
step one, ultrasonically dispersing graphene oxide in distilled water, adding a dodecylamine ethanol solution to obtain a mixed solution A, stirring at room temperature for 24 hours, then adding hydrazine monohydrate, carrying out reflux heating, repeatedly washing with a deionized water and absolute ethanol mixed solution for at least 3 times, and carrying out vacuum drying to obtain dodecylamine modified graphene powder;
dissolving epoxy resin in acetone with a certain volume, adding dodecylamine modified graphene powder with a certain mass, heating, stirring, reacting, washing and filtering with excessive dichloromethane after the reaction is finished, and obtaining DA-GO uniformly coated with epoxy resin;
step three, uniformly mixing cyanate ester resin and polyetherimide, heating and melting, mechanically stirring to be uniform to obtain main resin, cooling to 110-130 ℃, respectively adding DA-GO coated by epoxy resin and a transition metal salt accelerator, and mechanically mixing to be uniform by using a rubber mixing mill to obtain a rubber material;
and step four, pressing the sizing material obtained in the step three into a film by a film pressing machine under the heating condition to obtain the heat-conducting adhesive film.
3. The method according to claim 2, wherein the feeding ratio of graphene oxide to distilled water in the first step is 1g:100mL, and the dodecylamine ethanol solution is obtained by dissolving dodecylamine in anhydrous ethanol at a feeding ratio of 3g:100 mL.
4. The method according to claim 2, wherein the amount of hydrazine monohydrate in step one is 5% to 10% by volume of the mixed solution A.
5. The preparation method according to claim 2, wherein the first step is performed by heating under reflux at 70 ℃ for 18-24 h.
6. The method according to claim 2, wherein the drying step is carried out at 80 ℃ for 24 hours under vacuum.
7. The preparation method according to claim 2, wherein the charge ratio of the epoxy resin, the dodecylamine modified graphene and the acetone in the second step is 1g: 3g: 50mL, and the reaction is carried out for 1 to 3 hours under the condition of 60 ℃ by heating and stirring.
8. The preparation method according to claim 2, wherein the mass ratio of the cyanate ester resin to the polyetherimide resin in step three is 100: (5-20), heating and melting at 150-170 ℃, mechanically stirring for 60-90 min, wherein the accelerant is one or a mixture of several of zinc acetylacetonate, cobalt acetylacetonate and nickel acetylacetonate transition metal salt.
9. The preparation method of claim 2, wherein the temperature is reduced to 110-130 ℃ in the third step, the addition amount of the epoxy resin-coated DA-GO accounts for 10-15% of the total mass of the main resin, and the addition amount of the accelerator accounts for 0.5-1.0% of the total mass of the main resin.
10. The preparation method of claim 2, wherein the film is formed by pressing at 60-100 ℃ in the fourth step, and the thickness of the obtained adhesive film is 0.1-0.5 mm.
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| CN202011184410.8A CN112251188B (en) | 2020-10-28 | 2020-10-28 | Heat-conducting adhesive film suitable for bonding optical load structure and preparation method thereof |
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| CN202011184410.8A CN112251188B (en) | 2020-10-28 | 2020-10-28 | Heat-conducting adhesive film suitable for bonding optical load structure and preparation method thereof |
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| CN112251188B true CN112251188B (en) | 2021-07-20 |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1226350C (en) * | 2003-07-21 | 2005-11-09 | 复旦大学 | Cyanate resin modified by polyether imide |
| CN102876247B (en) * | 2012-10-24 | 2015-04-01 | 黑龙江省科学院石油化学研究院 | Modified cyanate adhesive film and preparation method thereof |
| CN104231624B (en) * | 2014-08-22 | 2016-05-11 | 南京信息职业技术学院 | Modified cyanate ester resin heat-conducting composite material and preparation method thereof |
| CN105368046B (en) * | 2015-11-27 | 2018-06-01 | 北京卫星制造厂 | Cyanate ester resin/heat conduction filler composition, prepreg and its application |
| CN107552055B (en) * | 2017-09-20 | 2020-02-18 | 河南科技大学 | Amido functionalized graphene oxide immobilized non-noble metal nano catalyst and preparation method thereof |
| CN107955577A (en) * | 2017-12-18 | 2018-04-24 | 安徽新立滤清器有限公司 | A kind of preparation method of the resistance to oil rectifier adhesive of high temperature resistant |
| KR102696647B1 (en) * | 2018-11-09 | 2024-08-22 | 삼성디스플레이 주식회사 | Flexible display apparatus and manufacturing method thereof |
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