CN1533886A - Polyimide composite aluminium foil and its prepearation method - Google Patents
Polyimide composite aluminium foil and its prepearation method Download PDFInfo
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- CN1533886A CN1533886A CNA031160328A CN03116032A CN1533886A CN 1533886 A CN1533886 A CN 1533886A CN A031160328 A CNA031160328 A CN A031160328A CN 03116032 A CN03116032 A CN 03116032A CN 1533886 A CN1533886 A CN 1533886A
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Abstract
A refractory composite polyimide-aluminium foil is composed of two surficial polyimide film layers as sealing layers and an aluminium foil as carrier between said polyimide film layers. It is prepared through preparing resin, dipping films and imination of polyamide acid. Its advantages are high mechanical and sealing performance at -260-260 deg.C, high strength and size stability at low-temp, and high resistance to radiation.
Description
Technical field
The present invention relates to a kind of composite of high-low temperature resistant, relate in particular to composite of a kind of polyimides and aluminium foil formation and preparation method thereof.
Background technology
Along with rapid development of science and technology, the especially development of space flight and aviation technology has proposed more and more higher requirement to resistant to elevated temperatures encapsulant.At present the encapsulant of industrial widely used high-low temperature resistant all can not meet the demands as poly-polyester film, nylon film etc., and the therefore new resistant to elevated temperatures encapsulant of developmental research as early as possible is to satisfy the needs of relevant department.
Summary of the invention
The technical issues that need to address of the present invention are to disclose a kind of polyimides clad aluminum foil, to overcome the defective that resistance to elevated temperatures that prior art exists can not be desirable, satisfy the needs of space flight and aviation technical development;
Two of the technical issues that need to address of the present invention provide the preparation method of above-mentioned polyimides clad aluminum foil.
Composite of the present invention is by constituting as the aluminium foil of carrier with as the Kapton of sealant, and said aluminium foil is clipped between the two layers of polyimide film.
According to the present invention, said aluminium foil adopts soft aluminium foil, and for suitable, the thickness of said Kapton is suitable with 0.03～0.04mm to its thickness with 0.01～0.02mm.
The preparation method of polyimides clad aluminum foil of the present invention comprises the steps:
(1) preparation of resin: pyromellitic acid anhydride is dropped into dimethylacetylamide, 4 in batches, react in 4 '-diamines yl diphenyl ether and the solvent, acquisition viscosity (Qie Shi) is 20～30 seconds polyamide.Reaction temperature is 20～60 ℃, and the reaction time is 5～9 hours, and in optimized technical scheme of the present invention, pyromellitic acid anhydride can divide 2～5 batches of inputs.
Said solvent comprises a kind of and composition thereof in the compound fragrant hydrocarbons such as dimethylacetylamide or benzene.
Take the dianhydride feeding mode to be progressively batch charging, polymerisation is tended towards stability, and resin viscosity was controlled at Qie Shi 20～30 seconds, and the polyamide solids content after dilution can reach 10～20%, as 15%, be convenient to the control of thickness in the polyamide aluminium foil immersing glue process.
The parts by weight that feed intake of material are:
100 parts of dimethylacetylamides
10～20 parts of pyromellitic acid anhydrides
4,8～18 parts of 4 '-diamines yl diphenyl ethers
40～60 parts of solvents.
(2) dipping of film: the polyamide that step (1) is obtained dilutes with solvent, and making its solid content is 10～20wt%, is that the soft aluminium foil of 0.01～0.02mm floods in the multilayer vertical gluing machine with thickness.
The multilayer vertical gluing machine of being addressed is a kind of equipment of routine.
The solvent of being addressed comprises a kind of and composition thereof in the compound fragrant hydrocarbons such as dimethylacetylamide, benzene or toluene, preferably dimethylacetylamide, benzene or toluene.
Because the polyamide molecular weight as dipping is less, Qie Shi viscosity was controlled at 20～30 seconds, in case resin sticks to and enters the solvent evaporates zone on the aluminium foil piecemeal, after being heated, strengthens resin the energy of percentage, make between the molecule that has carboxyl and amido in the molecule segment reaction has taken place, accelerated the strand growth, and in propagation process.Followed the part molecule to ask imidization, make the big molecule of linear molecule Zhi Liancheng network-type, make film middle part fractionated molecule structure be transformed into insoluble not molten state. if the solvent evaporates regional temperature is too high, cause the film appearance in thereby the imidization of intramolecule part after separate out in the water of denier and oligomer remain in, in case, cause doing on the Kapton hole bubble and bloat and separate with aluminium foil through the high-temperature sub amination.For this reason, dipping process must be controlled suitable temperature, with the imidization degree of polyamide in the control dipping process, stops repeating of micropore bubble.
According to the present invention, suitable dipping temperature is 80～190 ℃.
(3) imidization of polyamic acid: under 300～350 ℃ temperature, the polyamic acid resin that is immersed on the aluminium foil is carried out imidization, the imidization time is 1～4 hour, and side cut rewinding packing promptly obtains polyimides clad aluminum foil of the present invention.
Said imidization refers to be carried out intramolecular dehydration and is closed into imide ring, because the existence of carboxyl in the polyamic acid molecule makes that the hydrogen atom in the amide groups is comparatively active, protonated easily.At high temperature with carboxyl in hydroxyl form synthetic water and separate out, formed polyimides.In inferior gel process, have rolling length greater than mill run at this product, and film thickness is thin, and has static the polyimides clad aluminum foil.Easy lodging and generation folding line phenomenon, through adjusting heating rate, the too fast heat ageing phenomenon that causes the shade deviation of hot-spot carbonization and upper and lower temperature difference formation of having avoided heating up.
The imidization degree of polyimides is bigger to the influence of product quality, cyclisation rate (being the imidization degree) is bigger, imide ring the more in the macromolecular chain of polyimides, its molecular structure just more is tending towards perfect condition, The comprehensive performance is more good, if imidization is incomplete, remain in carboxyl and the very easily hydrolysis of acid amides chain in the macromolecular chain, make the combination property difference of polyimides and cause material damage, and the cyclisation rate of polyimides, depend primarily on the cyclisation temperature, so strict temperature and the corresponding time of selecting suitable imidization condition and accurately control imidization is the key factor that the Kapton quality is guaranteed.
Kapton of the present invention adopts the GB/13022-92 standard to test, its result shows, under-260～260 ℃ condition, use, higher mechanical properties and excellent sealing performance are arranged, radiation hardness, especially under low-temperature condition, enough intensity and dimensional stability are arranged, can be used as the external heat-insulating material of space rocket etc.
The specific embodiment
Embodiment 1
(1) preparation of resin: divide 3 batches to drop into 230 kilograms of dimethylacetylamides, 30 kilogram 4 32 kilograms of powdery pyromellitic acid anhydrides, react in 4 '-diamines yl diphenyl ether and 130 kilograms of toluene, acquisition viscosity (Qie Shi) is 30 seconds polyamide, reaction temperature is 30 ℃, reaction time is 7 hours
(2) dipping of film: the polyamide that step (1) is obtained dilutes with toluene, and making its solid content is 15wt%, is that the soft aluminium foil of 0.015mm floods in the multilayer vertical gluing machine with thickness.Dipping temperature is 140 ℃.
(3) imidization of polyamic acid: under 320 ℃ temperature, the polyamic acid resin that is immersed on the aluminium foil is carried out imidization, the imidization time is 3 hours, and side cut rewinding packing promptly obtains polyimides clad aluminum foil of the present invention.
Adopt the GB/13022-92 standard to test tensile strength: vertical 75 grams/square metre; Horizontal 73.6 grams/square metre.
Claims (7)
1. polyimides clad aluminum foil is characterized in that said aluminium foil is clipped between the two layers of polyimide film by constituting as the aluminium foil of carrier with as the Kapton of sealant.
2. polyimides clad aluminum foil according to claim 1 is characterized in that, said aluminium foil is soft aluminium foil.
3. polyimides clad aluminum foil according to claim 2 is characterized in that, its thickness is 0.03～0.04mm, and the thickness of aluminium foil is 0.01～0.02mm.
4. according to the preparation method of claim 1,2 or 3 described polyimides clad aluminum foils, it is characterized in that comprising the steps:
(1) preparation of resin: pyromellitic acid anhydride is dropped into dimethylacetylamide, 4 in batches, react in 4 '-diamines yl diphenyl ether and the solvent, reaction temperature is 20～60 ℃, and the reaction time is 5～9 hours;
(2) dipping of film: the polyamide that step (1) is obtained dilutes with solvent, and soft aluminium foil is flooded in the multilayer vertical gluing machine.
Dipping temperature is 80～190 ℃;
(3) imidization of polyamic acid: under 300～350 ℃ temperature, the polyamic acid resin that is immersed on the aluminium foil is carried out imidization, the imidization time is 1～4 hour, promptly obtains polyimides clad aluminum foil of the present invention.
5. method according to claim 4 is characterized in that, the viscosity of polyamide (Qie Shi) is 20～30 seconds.
6. method according to claim 4 is characterized in that, the parts by weight that feed intake of material are:
100 parts of dimethylacetylamides
10～20 parts of pyromellitic acid anhydrides
4,8～18 parts of 4 '-diamines yl diphenyl ethers
40～60 parts of solvents.
7. method according to claim 4 is characterized in that, the polyamide that step (1) is obtained dilutes with solvent, and making its solid content is 10～20wt%, and the thickness of aluminium foil is 0.01～0.02mm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA031160328A CN1533886A (en) | 2003-03-27 | 2003-03-27 | Polyimide composite aluminium foil and its prepearation method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA031160328A CN1533886A (en) | 2003-03-27 | 2003-03-27 | Polyimide composite aluminium foil and its prepearation method |
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| Publication Number | Publication Date |
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| CN1533886A true CN1533886A (en) | 2004-10-06 |
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| Application Number | Title | Priority Date | Filing Date |
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| CNA031160328A Pending CN1533886A (en) | 2003-03-27 | 2003-03-27 | Polyimide composite aluminium foil and its prepearation method |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114179483A (en) * | 2021-12-24 | 2022-03-15 | 扬州众想科技绝缘材料有限公司 | Polyimide aluminizer and preparation method thereof |
| CN114213896A (en) * | 2021-12-28 | 2022-03-22 | 扬州众想科技绝缘材料有限公司 | Polyimide composite aluminum foil and preparation method thereof |
| CN114724859A (en) * | 2022-06-09 | 2022-07-08 | 南通海星电子股份有限公司 | Preparation process of polyimide-aluminum composite foil |
-
2003
- 2003-03-27 CN CNA031160328A patent/CN1533886A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114179483A (en) * | 2021-12-24 | 2022-03-15 | 扬州众想科技绝缘材料有限公司 | Polyimide aluminizer and preparation method thereof |
| CN114213896A (en) * | 2021-12-28 | 2022-03-22 | 扬州众想科技绝缘材料有限公司 | Polyimide composite aluminum foil and preparation method thereof |
| CN114724859A (en) * | 2022-06-09 | 2022-07-08 | 南通海星电子股份有限公司 | Preparation process of polyimide-aluminum composite foil |
| CN114724859B (en) * | 2022-06-09 | 2022-08-12 | 南通海星电子股份有限公司 | Preparation process of polyimide-aluminum composite foil |
| WO2023236572A1 (en) * | 2022-06-09 | 2023-12-14 | 南通海星电子股份有限公司 | Preparation process for polyimide-aluminum composite foil |
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