CN106220847A - A kind of Kapton of high heat conduction and preparation method thereof - Google Patents
A kind of Kapton of high heat conduction and preparation method thereof Download PDFInfo
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- CN106220847A CN106220847A CN201610260990.1A CN201610260990A CN106220847A CN 106220847 A CN106220847 A CN 106220847A CN 201610260990 A CN201610260990 A CN 201610260990A CN 106220847 A CN106220847 A CN 106220847A
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- kapton
- methyl pyrrolidone
- aluminium nitride
- heat conduction
- high heat
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/06—Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
- C08G73/10—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
- C08G73/1003—Preparatory processes
- C08G73/1007—Preparatory processes from tetracarboxylic acids or derivatives and diamines
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/06—Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
- C08G73/10—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
- C08G73/1046—Polyimides containing oxygen in the form of ether bonds in the main chain
- C08G73/1053—Polyimides containing oxygen in the form of ether bonds in the main chain with oxygen only in the tetracarboxylic moiety
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/06—Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
- C08G73/10—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
- C08G73/1067—Wholly aromatic polyimides, i.e. having both tetracarboxylic and diamino moieties aromatically bound
- C08G73/1071—Wholly aromatic polyimides containing oxygen in the form of ether bonds in the main chain
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/28—Nitrogen-containing compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2379/00—Characterised by the use of 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 C08J2361/00 - C08J2377/00
- C08J2379/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
- C08J2379/08—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/28—Nitrogen-containing compounds
- C08K2003/282—Binary compounds of nitrogen with aluminium
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/16—Applications used for films
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/20—Applications use in electrical or conductive gadgets
Abstract
The invention discloses Kapton of a kind of high heat conduction and preparation method thereof, according to mass percent, including following components: diphenyl ether dianhydride 5 20%, MDA 5 30%, N methyl pyrrolidone 60 90%, aluminium nitride 0.05 0.8%, preparation method is: for obtaining emulsus aluminium nitride suspension pretreatment fluid, remaining N methyl pyrrolidone is joined in stirred tank, again MDA is joined in stirred tank, stirring, add diphenyl ether dianhydride, stirring, finally the emulsus aluminium nitride suspension pretreatment fluid of preparation is joined in stirred tank, stirring, prepare glue；Glue is prepared as gel film by casting machine；Prepare Kapton；Prepared Kapton is cooled to 20 DEG C 50 DEG C, rolling.The present invention has the advantages such as high thermal conductivity.
Description
Technical field
The present invention relates to Kapton production and processing field, the Kapton of a kind of high heat conduction
And preparation method thereof.
Background technology
Kapton is a kind of novel organic polymer thin film, because Kapton has excellent electrical
Energy, radiation resistance and the high temperature resistant and resistance to low temperature of excellence, be widely used in aviation, navigation, atomic energy and liquid
The fields such as crystalline substance.
Traditional Kapton is at diformazan by pyromellitic acid anhydride (PMDA) and diaminodiphenyl ether (ODA)
Yl acetamide (DMAC) solvent is cast and forms, the most again through biaxial tension, cut molding, but existing Kapton
Thermal conductivity low, therefore some are required that thin film has the field of high-termal conductivity, existing Kapton is the most inapplicable,
It is thus desirable to be further improved.
Summary of the invention
The invention aims to solve the defect that Kapton thermal conductivity of the prior art is low, it is provided that a kind of
Kapton of high heat conduction and preparation method thereof solves the problems referred to above.
The invention discloses the Kapton of a kind of high heat conduction, according to mass percent, including following components: hexichol
Ether dianhydride 5-20%, MDA 5-30%, N-Methyl pyrrolidone 60-90%, aluminium nitride 0.05-0.8%.
As preferably, the invention discloses the Kapton of a kind of high heat conduction, according to mass percent, including following
Component: diphenyl ether dianhydride 18.29%, MDA 11.91%, N-Methyl pyrrolidone 69.65%, aluminium nitride 0.15%.
As preferably, the invention discloses the Kapton of a kind of high heat conduction, according to mass percent, including following
Component: diphenyl ether dianhydride 18.29%, MDA 11.91%, N-Methyl pyrrolidone 69.5%, aluminium nitride 0.3%.
As preferably, the invention discloses the Kapton of a kind of high heat conduction, according to mass percent, including following
Component: diphenyl ether dianhydride 18.29%, MDA 11.91%, N-Methyl pyrrolidone 69.35%, aluminium nitride 0.45%.
As preferably, the present invention also provides for the preparation method of the Kapton of a kind of above-mentioned high heat conduction, concrete steps
As follows:
Step one: according to mass percent, is pyrolyzed aluminium nitride 2h under the pure anhydrous ammonia gas that temperature is 1200 DEG C, is gathered
The aluminum nitride particle of collection, the most first takes out the N-Methyl pyrrolidone accounting for N-Methyl pyrrolidone total amount 5%-35%, by assemble
Aluminum nitride particle joins in taken out N-Methyl pyrrolidone, under conditions of 20 DEG C-25 DEG C, with the speed of 5000r/min
Degree stirring 2h-3h, prepares emulsus aluminium nitride suspension pretreatment fluid, is then joined by remaining N-Methyl pyrrolidone and stir
Mix in still, then MDA is joined in stirred tank, stir 20min-90min, add diphenyl ether dianhydride, stirring
30min-120min, finally joins in stirred tank by the emulsus aluminium nitride suspension pretreatment fluid of preparation, stirs 180min-
300min, prepares glue；
Step 2: the glue that step one is prepared through spraying die drool in the minute surface steel strip surface of casting machine, 150 DEG C-
Under conditions of 190 DEG C, glue is prepared as gel film by casting machine；
Step 3: peel off gel film from the minute surface steel strip surface of casting machine, under conditions of 340 DEG C-560 DEG C, first uses vertical
To stretching-machine, gel film being carried out longitudinal stretching, the draw ratio of longitudinal stretching is 1.2, re-uses transverse drawing mill and enters gel film
Row cross directional stretch, the draw ratio of cross directional stretch is 1.3, prepares Kapton；
Step 4: the Kapton that step 3 prepares is cooled to 20 DEG C-50 DEG C, uses winder to carry out after having cooled down
Rolling.
The present invention has the advantage that aluminium nitride is atomic crystal compared to existing technology, belongs to diamond like carbon nitride, the highest
Can be stabilized to 2200 DEG C, room temperature strength is high, and intensity declines relatively slow with the rising of temperature, and heat conductivity is good, and thermal coefficient of expansion is little, is
Good heat shock resistance material, aluminium nitride or electrical insulator, dielectric properties are good, also get a good chance of as electric elements, because of
Aluminium nitride is a kind of ceramics insulator, and thermal conductivity is high (about 200W/m K), close to BeO and SiC, is more than 5 times of Al2O3, makes
Aluminium nitride has a higher heat-transfer capability, thermal coefficient of expansion (4.5 × 10-6 DEG C) and Si (3.5 ~ 4 × 10-6 DEG C) and GaAs (6 ×
10-6 DEG C) coupling, to making aluminium nitride be widely used in microelectronics, the polyimides of high heat conduction the most of the present invention is thin
Film has high heat conduction and the advantage of good electric insulation.
Detailed description of the invention
Below in conjunction with embodiment, the invention will be further described:
Embodiment 1
The Kapton of high heat conduction of the present invention, according to mass percent, including following components: diphenyl ether dianhydride
18.29%, MDA 11.91%, N-Methyl pyrrolidone 69.65%, aluminium nitride 0.15%.
The preparation method of the Kapton of above-mentioned high heat conduction, specifically comprises the following steps that
Step one: according to mass percent, is pyrolyzed 2h under the pure anhydrous ammonia gas that temperature is 1200 DEG C by aluminium nitride 0.15%,
Obtain the aluminum nitride particle assembled, the most first take out N-Methyl pyrrolidone 7.82%, the aluminum nitride particle of gathering is joined institute
In the N-Methyl pyrrolidone taken out, under conditions of 22 DEG C, stir 2.5h with the speed of 5000r/min, prepare emulsus
Aluminium nitride suspension pretreatment fluid, then joins remaining N-Methyl pyrrolidone 61.83% in stirred tank, then by diaminourea
Diphenyl-methane 11.91% joins in stirred tank, stirs 45min, adds diphenyl ether dianhydride 18.29%, stirs 90min, finally
The emulsus aluminium nitride suspension pretreatment fluid of preparation is joined in stirred tank, stirs 200min, prepare glue；
Step 2: glue step one prepared is on spraying die drool to the minute surface steel strip surface of casting machine, at 180 DEG C
Under the conditions of, glue is prepared as gel film by casting machine；
Step 3: peel off gel film from the minute surface steel strip surface of casting machine, under conditions of 400 DEG C, first use longitudinal stretching
Machine carries out longitudinal stretching to gel film, and the draw ratio of longitudinal stretching is 1.2, re-uses transverse drawing mill and carries out gel film laterally
Stretching, the draw ratio of cross directional stretch is 1.3, prepares Kapton；
Step 4: the Kapton that step 3 prepares is cooled to 25 DEG C, uses winder to carry out rolling after having cooled down
?.
Embodiment 2
The Kapton of high heat conduction of the present invention, according to mass percent, including following components: diphenyl ether dianhydride
18.29%, MDA 11.91%, N-Methyl pyrrolidone 69.5%, aluminium nitride 0.3%.
The preparation method of the Kapton of above-mentioned high heat conduction, specifically comprises the following steps that
Step one: according to mass percent, is pyrolyzed 2h under the pure anhydrous ammonia gas that temperature is 1200 DEG C by aluminium nitride 0.3%,
To the aluminum nitride particle assembled, the most first take out N-Methyl pyrrolidone 15.64%, the aluminum nitride particle of gathering is joined institute
In the N-Methyl pyrrolidone taken out, under conditions of 20 DEG C, stir 2h with the speed of 5000r/min, prepare emulsus nitrogen
Change aluminum suspension pretreatment fluid, then remaining N-Methyl pyrrolidone 53.86% is joined in stirred tank, then by diaminourea two
Phenylmethane 11.91% joins in stirred tank, stirs 60min, adds diphenyl ether dianhydride 18.29%, stirs 90min, finally will
The emulsus aluminium nitride suspension pretreatment fluid of preparation joins in stirred tank, stirs 200min, prepares glue；
Step 2: glue step one prepared is on spraying die drool to the minute surface steel strip surface of casting machine, at 190 DEG C
Under the conditions of, glue is prepared as gel film by casting machine；
Step 3: peel off gel film from the minute surface steel strip surface of casting machine, under conditions of 430 DEG C, first use longitudinal stretching
Machine carries out longitudinal stretching to gel film, and the draw ratio of longitudinal stretching is 1.2, re-uses transverse drawing mill and carries out gel film laterally
Stretching, the draw ratio of cross directional stretch is 1.3, prepares Kapton；
Step 4: the Kapton that step 3 prepares is cooled to 25 DEG C, uses winder to carry out rolling after having cooled down
?.
Embodiment 3
The Kapton of high heat conduction of the present invention, according to mass percent, including following components: diphenyl ether dianhydride
18.29%, MDA 11.91%, N-Methyl pyrrolidone 69.35%, aluminium nitride 0.45%.
The preparation method of the Kapton of above-mentioned high heat conduction, specifically comprises the following steps that
Step one: aluminium nitride 0.45% is pyrolyzed under the pure anhydrous ammonia gas that temperature is 1200 DEG C 2h, obtains the aluminium nitride assembled
Particle, the most first takes out N-Methyl pyrrolidone 23.46%, the aluminum nitride particle of gathering joins taken out N-methyl pyrrole
In pyrrolidone, under conditions of 25 DEG C, stir 3h with the speed of 5000r/min, prepare emulsus aluminium nitride suspension pretreatment
Liquid, then joins remaining N-Methyl pyrrolidone 45.89% in stirred tank, then is added by MDA 11.91%
Enter in stirred tank, stir 90min, add diphenyl ether dianhydride 18.29%, stir 80min, finally by the emulsus nitridation of preparation
Aluminum suspension pretreatment fluid joins in stirred tank, stirs 200min, prepares glue；
Step 2: glue step one prepared is on spraying die drool to the minute surface steel strip surface of casting machine, at 180 DEG C
Under the conditions of, glue is prepared as gel film by casting machine；
Step 3: peel off gel film from the minute surface steel strip surface of casting machine, under conditions of 340 DEG C, first use longitudinal stretching
Machine carries out longitudinal stretching to gel film, and the draw ratio of longitudinal stretching is 1.2, re-uses transverse drawing mill and carries out gel film laterally
Stretching, the draw ratio of cross directional stretch is 1.3, prepares Kapton；
Step 4: the Kapton that step 3 prepares is cooled to 25 DEG C, uses winder to carry out rolling after having cooled down
?.
By the low thermal expansion coefficient polyimide thin film prepared according to embodiment 1 to 3 and conventional polyamides in the market
Imines thin film carries out Performance comparision, result such as table 1 below:
Table 1
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Conventional polyimide thin film | |
| Thermal coefficient of expansion (ppm/K) | 37 | 33 | 28 | 46 |
| Mechanical strength (MPa) | 200 | 215 | 225 | 170 |
| Electrical strength (MV/m) | 250 | 275 | 290 | 180 |
| Thermal conductivity/W/m K | 0.85 | 2.1 | 4.3 | 0.15 |
The Kapton of the high heat conduction obtained by the present invention has relative to conventional polyimide thin film on market as shown in Table 1
There is the advantage that thermal conductivity is high, and as shown in Table 1, embodiment 3 is polyimide film and the preparation side thereof of a kind of high heat conduction of the present invention
The optimum selection of method.
The ultimate principle of the present invention, principal character and advantages of the present invention have more than been shown and described.The technology of the industry
The personnel simply present invention it should be appreciated that the present invention is not restricted to the described embodiments, described in above-described embodiment and description
Principle, the present invention also has various changes and modifications without departing from the spirit and scope of the present invention, these change and
Improvement both falls within the range of claimed invention.The protection domain of application claims by appending claims and
Equivalent defines.
Claims (5)
1. the Kapton of a high heat conduction, it is characterised in that: according to mass percent, including following components: diphenyl ether
Dianhydride 5-20%, MDA 5-30%, N-Methyl pyrrolidone 60-90%, aluminium nitride 0.05-0.8%.
The Kapton of a kind of high heat conduction the most according to claim 1, it is characterised in that: according to mass percent,
Including following components: diphenyl ether dianhydride 18.29%, MDA 11.91%, N-Methyl pyrrolidone 69.65%, nitridation
Aluminum 0.15%.
The Kapton of a kind of high heat conduction the most according to claim 1, it is characterised in that: according to mass percent,
Including following components: diphenyl ether dianhydride 18.29%, MDA 11.91%, N-Methyl pyrrolidone 69.5%, aluminium nitride
0.3%。
The Kapton of a kind of high heat conduction the most according to claim 1, it is characterised in that: according to mass percent,
Including following components: diphenyl ether dianhydride 18.29%, MDA 11.91%, N-Methyl pyrrolidone 69.35%, nitridation
Aluminum 0.45%.
5. according to the preparation method of the Kapton of the arbitrary described a kind of high heat conduction of claim 1-4, it is characterised in that:
Specifically comprise the following steps that
Step one: according to mass percent, is pyrolyzed aluminium nitride 2h under the pure anhydrous ammonia gas that temperature is 1200 DEG C, is gathered
The aluminum nitride particle of collection, the most first takes out the N-Methyl pyrrolidone accounting for N-Methyl pyrrolidone total amount 5%-35%, by assemble
Aluminum nitride particle joins in taken out N-Methyl pyrrolidone, under conditions of 20 DEG C-25 DEG C, with the speed of 5000r/min
Degree stirring 2h-3h, prepares emulsus aluminium nitride suspension pretreatment fluid, is then joined by remaining N-Methyl pyrrolidone and stir
Mix in still, then MDA is joined in stirred tank, stir 20min-90min, add diphenyl ether dianhydride, stirring
30min-120min, finally joins in stirred tank by the emulsus aluminium nitride suspension pretreatment fluid of preparation, stirs 180min-
300min, prepares glue；
Step 2: the glue that step one is prepared through spraying die drool in the minute surface steel strip surface of casting machine, 150 DEG C-
Under conditions of 190 DEG C, glue is prepared as gel film by casting machine；
Step 3: peel off gel film from the minute surface steel strip surface of casting machine, under conditions of 340 DEG C-560 DEG C, first uses vertical
To stretching-machine, gel film being carried out longitudinal stretching, the draw ratio of longitudinal stretching is 1.2, re-uses transverse drawing mill and enters gel film
Row cross directional stretch, the draw ratio of cross directional stretch is 1.3, prepares Kapton；
Step 4: the Kapton that step 3 prepares is cooled to 20 DEG C-50 DEG C, uses winder to carry out after having cooled down
Rolling.
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| CN201610260990.1A CN106220847A (en) | 2016-04-26 | 2016-04-26 | A kind of Kapton of high heat conduction and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108997597A (en) * | 2018-06-13 | 2018-12-14 | 安徽统唯新材料科技股份有限公司 | A kind of Kapton of alternating copolymerization and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101168598A (en) * | 2007-10-08 | 2008-04-30 | 江阴市云达电子新材料有限公司 | Method for preparing ultra-thick polyimide film with high heat conductivity and low thermal expansion coefficient |
| CN103194062A (en) * | 2013-03-29 | 2013-07-10 | 株洲时代电气绝缘有限责任公司 | Polyimide film and preparation method thereof |
| US20150198915A1 (en) * | 2014-01-15 | 2015-07-16 | Xerox Corporation | Fuser member compositions |
-
2016
- 2016-04-26 CN CN201610260990.1A patent/CN106220847A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101168598A (en) * | 2007-10-08 | 2008-04-30 | 江阴市云达电子新材料有限公司 | Method for preparing ultra-thick polyimide film with high heat conductivity and low thermal expansion coefficient |
| CN103194062A (en) * | 2013-03-29 | 2013-07-10 | 株洲时代电气绝缘有限责任公司 | Polyimide film and preparation method thereof |
| US20150198915A1 (en) * | 2014-01-15 | 2015-07-16 | Xerox Corporation | Fuser member compositions |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108997597A (en) * | 2018-06-13 | 2018-12-14 | 安徽统唯新材料科技股份有限公司 | A kind of Kapton of alternating copolymerization and preparation method thereof |
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Application publication date: 20161214 |