High Kapton of a kind of peel strength and preparation method thereof
Technical field
The present invention relates to Kapton production and processing field, specifically the high polyimides of a kind of peel strength
Film and preparation method thereof.
Background technology
Kapton is the novel high polymer composite that a kind of heat resistance is good, radiation resistance is strong, aviation,
The aspects such as space flight, electric, machinery, microelectronics, chemical industry are widely used, polyimides stable chemical nature, and polyamides is sub-
Amine do not need add fire retardant prevent from burning, general polyimides all anti-chemical solvent such as hydro carbons, esters, ethers,
Alcohols and dichlorodifluoromethan.
But the peel strength using the Kapton prepared by existing method is low, especially using polyamides sub-
When the method that amine film and Copper Foil bind manufactures polyimide copper clad lamination, it is necessary to use on Copper Foil or Kapton or
Person's surface both applies adhesive, and hot repressing makes both be combined together, qualified products its peel strength of 90 ° 10N/ to be reached
Cm or higher, but due to existing Kapton, laminating middle peel strength is low with Copper Foil or acrylic resin glue
Defect, is therefore unfavorable for field prepared by FPC, needs the stripping improving existing Kapton further strong
Degree.
Content of the invention
The invention aims to solve the low defect of Kapton peel strength of the prior art, provide one
Plant high Kapton of peel strength and preparation method thereof and solve the problems referred to above.
To achieve these goals, technical scheme is as follows:The invention discloses high the gathering of a kind of peel strength
Imide membrane, according to mass percent, composed of the following components:Pyromellitic acid anhydride 5-20%, diaminodiphenyl ether 5-
20%th, dimethylacetylamide 60-90%.
As preferably, the invention discloses the high Kapton of a kind of peel strength, according to mass percent, by with
Lower component forms:Pyromellitic acid anhydride the 10.4%th, diaminodiphenyl ether the 9.5%th, dimethylacetylamide 80.1%.
As preferably, the present invention also provides the preparation method of the high Kapton of a kind of above-mentioned peel strength, specifically
Step is as follows:
Step one:The preparation of glue:According to above-mentioned mass percent, dimethylacetylamide and diaminodiphenyl ether are joined instead
In answering kettle, stirring 30-60min, then joining pyromellitic acid anhydride in reactor, stir 60min-90min, stirring completes
After prepare glue;
Step 2:The preparation of gel mould:The glue preparing step one is through the minute surface steel band table of spraying die drool to casting machine
On face, under conditions of 160 DEG C, glue is prepared as gel mould by casting machine;
Step 3:The stretching of gel mould:Gel mould is peeled off from the minute surface steel strip surface of casting machine, under conditions of 400 DEG C,
First using longitudinal stretching machine to carry out longitudinal stretching to gel mould, the draw ratio of longitudinal stretching is 1.2, re-uses transverse drawing mill pair
Gel mould carries out cross directional stretch, and the draw ratio of cross directional stretch is 1.3, prepares Kapton;
Step 4:Surface treatment is carried out to Kapton:The Kapton that step 3 prepares is cooled to 20 DEG C-50
DEG C, after cooling completes, Kapton is used methanol extraction 1-10min, then use Surface Treatment with Plasma machine to polyamides
Imines film carries out oxygen plasma treatment 1-9min, and wherein the DC voltage of Surface Treatment with Plasma machine is 100-325V, electrode
Distance is 2-7.8cm, gas pressure is 0.07-0.5mmHg, is then exposed to the Kapton after oxygen plasma treatment
1-5min in air, is then sent to Kapton in the aqueous solution, according to mass percent, contains 10% in the aqueous solution
Acrylamide, meanwhile, under conditions of 50-70 DEG C, with near ultraviolet ray irradiation 3-10min, then that polyimides is thin
Film takes out from the aqueous solution, cleans the surface of Kapton with pure water, then uses dryer to dry under the conditions of 105 DEG C
Dry 1-5min, then uses winder rolling.
The present invention has the following advantages compared to existing technology:Kapton obtained by the present invention is entered by step 4
Row oxygen plasma treatment, therefore the thrust on Kapton surface can increase, and specific surface area also will increase, and due to
Kapton uses near ultraviolet radiation 3-10min in the aqueous solution containing acrylamide, therefore Kapton
Surface can graft acrylamide, also increase film laminating with Copper Foil during epoxy or acrylic resin colloid bonding
Property, therefore improve the peel strength of Kapton greatly.
Detailed description of the invention
Embodiment 1
Step one:The preparation of glue:According to mass percent, dimethylacetylamide 80.1% and diaminodiphenyl ether 9.5% are added
Enter in reactor, stir 45min, then pyromellitic acid anhydride 10.4% is joined in reactor, stir 45min, stirred
Glue is prepared after one-tenth;
Step 2:The preparation of gel mould:The glue preparing step one is through the minute surface steel band table of spraying die drool to casting machine
On face, under conditions of 160 DEG C, glue is prepared as gel mould by casting machine;
Step 3:The stretching of gel mould:Gel mould is peeled off from the minute surface steel strip surface of casting machine, under conditions of 400 DEG C,
First using longitudinal stretching machine to carry out longitudinal stretching to gel mould, the draw ratio of longitudinal stretching is 1.2, re-uses transverse drawing mill pair
Gel mould carries out cross directional stretch, and the draw ratio of cross directional stretch is 1.3, prepares Kapton;
Step 4:Surface treatment is carried out to Kapton:The Kapton that step 3 prepares is cooled to 30 DEG C, cold
But after completing, Kapton is used methanol extraction 4min, then use Surface Treatment with Plasma machine to Kapton
Carry out oxygen plasma treatment 5min, wherein the DC voltage of Surface Treatment with Plasma machine be 200V, electrode distance be 6cm, gas
Pressure is 0.08mmHg, then the Kapton after oxygen plasma treatment is exposed 5min in atmosphere, then by polyamides
Imines film is sent in the aqueous solution, according to mass percent, contains the acrylamide of 10%, meanwhile, 60 in the aqueous solution
DEG C under conditions of, with near ultraviolet ray irradiation 4min, then Kapton is taken out from the aqueous solution, cleans poly-with pure water
The surface of imide membrane, then uses dryer to dry 5min under the conditions of 105 DEG C, then uses winder rolling.
Embodiment 2
Step one:The preparation of glue:According to mass percent, dimethylacetylamide 80.1% and diaminodiphenyl ether 9.5% are added
Enter in reactor, stir 45min, then pyromellitic acid anhydride 10.4% is joined in reactor, stir 45min, stirred
Glue is prepared after one-tenth;
Step 2:The preparation of gel mould:The glue preparing step one is through the minute surface steel band table of spraying die drool to casting machine
On face, under conditions of 160 DEG C, glue is prepared as gel mould by casting machine;
Step 3:The stretching of gel mould:Gel mould is peeled off from the minute surface steel strip surface of casting machine, under conditions of 400 DEG C,
First using longitudinal stretching machine to carry out longitudinal stretching to gel mould, the draw ratio of longitudinal stretching is 1.2, re-uses transverse drawing mill pair
Gel mould carries out cross directional stretch, and the draw ratio of cross directional stretch is 1.3, prepares Kapton;
Step 4:Surface treatment is carried out to Kapton:The Kapton that step 3 prepares is cooled to 25 DEG C, cold
But after completing, Kapton is used methanol extraction 4min, then use Surface Treatment with Plasma machine to Kapton
Carry out oxygen plasma treatment 6min, wherein the DC voltage of Surface Treatment with Plasma machine be 270V, electrode distance be 7cm, gas
Pressure is 0.07mmHg, then the Kapton after oxygen plasma treatment is exposed 5min in atmosphere, then by polyamides
Imines film is sent in the aqueous solution, according to mass percent, contains the acrylamide of 10%, meanwhile, 60 in the aqueous solution
DEG C under conditions of, with near ultraviolet ray irradiation 7min, then Kapton is taken out from the aqueous solution, cleans poly-with pure water
The surface of imide membrane, then uses dryer to dry 3min under the conditions of 105 DEG C, then uses winder rolling.
Embodiment 3
Step one:The preparation of glue:According to mass percent, dimethylacetylamide 80.1% and diaminodiphenyl ether 9.5% are added
Enter in reactor, stir 45min, then pyromellitic acid anhydride 10.4% is joined in reactor, stir 45min, stirred
Glue is prepared after one-tenth;
Step 2:The preparation of gel mould:The glue preparing step one is through the minute surface steel band table of spraying die drool to casting machine
On face, under conditions of 160 DEG C, glue is prepared as gel mould by casting machine;
Step 3:The stretching of gel mould:Gel mould is peeled off from the minute surface steel strip surface of casting machine, under conditions of 400 DEG C,
First using longitudinal stretching machine to carry out longitudinal stretching to gel mould, the draw ratio of longitudinal stretching is 1.2, re-uses transverse drawing mill pair
Gel mould carries out cross directional stretch, and the draw ratio of cross directional stretch is 1.3, prepares Kapton;
Step 4:Surface treatment is carried out to Kapton:The Kapton that step 3 prepares is cooled to 20 DEG C, cold
But after completing, Kapton is used methanol extraction 1-10min, then use Surface Treatment with Plasma machine thin to polyimides
Film carries out oxygen plasma treatment 9min, wherein the DC voltage of Surface Treatment with Plasma machine be 325V, electrode distance be 7cm, gas
Body pressure is 0.5mmHg, then the Kapton after oxygen plasma treatment is exposed 3min in atmosphere, then by polyamides
Imines film is sent in the aqueous solution, according to mass percent, contains the acrylamide of 10%, meanwhile, 68 in the aqueous solution
DEG C under conditions of, with near ultraviolet ray irradiation 9min, then Kapton is taken out from the aqueous solution, cleans poly-with pure water
The surface of imide membrane, then uses dryer to dry 4min under the conditions of 105 DEG C, then uses winder rolling.
By Kapton high for the peel strength preparing according to embodiment 1 to 3 and conventional polyamides in the market
Imines film carries out Performance comparision, result such as table 1 below:
Table 1
|
Embodiment 1 |
Embodiment 2 |
Embodiment 3 |
Conventional polyimide film |
Peel strength(N/cm) |
10.32 |
11.89 |
13.68 |
8.75 |
Mechanical strength (MPa) |
220 |
223 |
218 |
170 |
Electrical strength(MV/m) |
235 |
240 |
234 |
180 |
The high Kapton of peel strength obtained by the present invention is thin relative to conventional polyimide on market as shown in Table 1
Film has the advantage that peel strength is high, mechanical strength is good, electrical strength is good, and as shown in Table 1, embodiment 3 is that the present invention is a kind of
The optimum selection of the high Kapton of peel strength and preparation method thereof.
General principle, principal character and the advantages of the present invention of the present invention have more than been shown and described.The technology of the industry
The simply present invention it should be appreciated that the present invention is not restricted to the described embodiments, described in above-described embodiment and specification for the personnel
Principle, the present invention also has various changes and modifications without departing from the spirit and scope of the present invention, these change and
In the range of improvement both falls within claimed invention.The protection domain of application claims by appending claims and
Equivalent defines.