CN102418096B - Kapton/Al2O3 surface nanometer composite membrane and application - Google Patents
Kapton/Al2O3 surface nanometer composite membrane and application Download PDFInfo
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- CN102418096B CN102418096B CN 201110404208 CN201110404208A CN102418096B CN 102418096 B CN102418096 B CN 102418096B CN 201110404208 CN201110404208 CN 201110404208 CN 201110404208 A CN201110404208 A CN 201110404208A CN 102418096 B CN102418096 B CN 102418096B
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- kapton
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Abstract
The invention discloses a Kapton/Al2O3 surface nanometer composite membrane, which is prepared by the following steps of: performing ultrasonic cleaning on a Kapton membrane by using acetone and absolute ethanol, steeping in 1 to 5 mol/L KOH aqueous solution at room temperature for 5 to 10 minutes, taking the membrane out, and fully cleaning by using a large amount of deionized water until the membrane is neutral; steeping the membrane in 0.1 to 0.5 mol/L AlCl3 aqueous solution at the room temperature for 60 to 120 minutes, taking the membrane out, cleaning by using a large amount of deionized water, and drying naturally; and performing oxygen-containing heat treatment in a high-temperature controllable tubular furnace, heating to the temperature of between 260 and 400 DEG C from room temperature at a heating speed of between 2 and 4 DEG C/minute, keeping the temperature for 60 to 180 minutes, and cooling with the furnace. The Kapton/Al2O3 surface nanometer composite membrane can be used as a surface part of a spacecraft, and also can promote the further development of the Kapton membrane and a Kapton-based composite membrane in fields of aerospace, electrons and the like.
Description
Technical field
The present invention relates to a kind of polymer-based laminated film, relate in particular to the polymer-based laminated film that use on a kind of spacecraft surface.
Background technology
Usually said polyimide (Polyimide is called for short PI) is the high-temperature polymer that contains imide ring-type structure on the molecule main chain.1961, the PMMI thin-film material that Dupont (DuPont) company produces took the lead in realizing commercialization in the world, and it is named as Kapton.The Kapton thin-film material has following some advantage than other high molecular film materials: (1) thermostability height, but at life-time service more than 300 ℃, but use 400～500 ℃ of short-terms, still can embrittlement in～269 ℃ liquid nitrogen; (2) mechanical property is outstanding, and the tensile strength of Kapton film is 170MPa, has good wear resistant friction reducing and heat-resistant aging; (3) the chemical stability height is insoluble to organic solvent, and is stable to diluted acid (as nitric acid), but hydrolysis under alkaline condition; (4) radiation property such as anti-ultraviolet, electronics, ray are strong, stablize in high temperature, high vacuum, and volatile matter is few; (5) the Kapton film is the electrically insulating material of using always, and dielectric properties are outstanding, and specific inductivity is about 3.4.The Kapton film is widely used in the space material field because of its above-mentioned excellent properties, as flexible space solar cell, spacecraft heat control coating layer on surface, solar mirror etc.Complicated space environment can make performance degradation, the inefficacy of Kapton film, often needs the Kapton film is carried out integral body or surface modification, to increase the space environment adaptability of material.In the Kapton film, add Al
2O
3Composition can improve the oxidation-resistance of material, anti-corona, high thermal resistance etc., is one of emphasis of present Kapton film study on the modification.
The inorganic compounding method of modifying of existing Kapton film mainly contains magnetron sputtering, ion implantation, in-situ method, colloidal sol～gel method etc.In-situ method prepares inorganic particle doped polyimide film, and " impurity " such as tensio-active agent or strongly-acid negatively charged ion is stranded in the matrix, will impel the degraded of polymer materials; In addition than surface modification, bulk modified bigger for the influence of Kapton mechanical properties in films, general material snappiness, tensile property etc. sharply descend, and the compound high-performance that keeps the middle part body material of surface inorganic, visible surface layer matrix material is more promising; Magnetron sputtering, colloidal sol～gel method are coated with the compact inorganic rete at the Kapton film surface, but bonding properties difference and the surface inorganic film at organic/inorganic hardness jumping characteristic interface easily produce defectives such as cracking; For preparation environmental requirement vacuum enhancing or the high-temperature of magnetron sputtering, ion injection method, these all can cause damage to polymer materials.In addition, the cost of above method is higher, needs special equipment and some to have the chemical reagent of specific groups, and for large-area material preparation poor practicability.
Summary of the invention
At above-mentioned prior art, the invention provides a kind of Al
2O
3The Kapton/Al that nano particle is grown from inside to outside and formed at the Kapton upper layer
2O
3The nano surface laminated film, low, the no particular surroundings of its production cost or reagent requirement, simple, suitable big area production, Al
2O
3Nano particle and Kapton film associativity are strong, excellent combination property.Kapton/Al of the present invention
2O
3The nano surface laminated film helps to promote the Kapton film, and Kapton based coextruded film further developing in fields such as space flight, electronics.
In order to solve the problems of the technologies described above Kapton/Al of the present invention
2O
3The technical scheme that the nano surface laminated film is achieved is: prepared by following steps:
Step 1, the Kapton film is successively used acetone and dehydrated alcohol ultrasonic cleaning 10min, remove the residual organic pollutant of material surface, clean up back seasoning in air.
Step 2, will be through step 1 surface-treated Kapton film, at room temperature impregnated in concentration is in the KOH aqueous solution of 1～5mol/L, takes out behind 5～10min, fully cleans to neutrality with a large amount of deionized waters;
Step 3, will at room temperature impregnated in the AlCl of 0.1～0.5mol/L through the Kapton of step 2 hydrolysis treatment film
3Take out behind 60～120min in the aqueous solution, fully clean with a large amount of deionized waters, remove surperficial residual metal salts solution, seasoning in air.
Step 4, will after step 3 ion-exchange, contain Al
3+The Kapton film in the controlled tube furnace of high temperature, contain oxygen thermal treatment, be warming up to 260～400 ℃ with 2～4 ℃/min of heat-up rate from room temperature, the insulation 60～180min, cool to room temperature then with the furnace.
Kapton/Al of the present invention
2O
3The nano surface laminated film is applied to the surface elements of spacecraft.
Compared with prior art, the invention has the beneficial effects as follows:
The present invention has used the Kapton film and has issued the unboiled water solution at alkaline condition, makes the polyimide molecule open loop form polyamic acid sylvite; At AlCl
3Al in the solion
3+To break away from Cl
3+Enter modified layer and K separately
+Exchange, the K that is displaced
+With Cl
3+Form ionic linkage.In heat treatment process, the polyamic acid imidization reverts to polyimide, simultaneously Al
3+Under the oxygen effect, form the Al atom, and then be oxidized to Al
2O
3Atom.With the rising of thermal treatment temp, or holding time prolonging, Al
2O
3Elementide forms nano particle and to matrix film surface growth diffusion, forms Al at the Kapton film surface
2O
3The nano particle composite bed.Al among the present invention
2O
3Nano particle and Kapton body material mortise, the whole mechanical property of laminated film, the anti-corona of high-temperature stability significantly improve; Al
2O
3Nanoparticle size unanimity and be uniformly distributed in matrix surface, surfacingization, flawless, and roughness reduces; Preparation technology is simple, and cost is low, does not have " impurity " in the preparation process and adds, and is suitable for big area production.
Description of drawings
Fig. 1 is pure Kapton film 2 * 2 μ m atomic power microstructure figure;
Fig. 2 is Kapton/Al of the present invention
2O
32 * 2 μ m atomic power microstructure figure of nano compound film embodiment 1;
Fig. 3 is Kapton/Al of the present invention
2O
32 * 2 μ m atomic power microstructure figure of nano compound film embodiment 2.
Embodiment
Tell about detailed process of the present invention by the following examples, it is convenience in order to understand that embodiment is provided, and never is restriction the present invention.
Embodiment 1:
The Kapton film is successively used acetone and dehydrated alcohol ultrasonic cleaning 10min, remove the residual organic pollutant of material surface, clean up back seasoning in air; The concentration that Kapton film after cleaning at room temperature be impregnated in is in the KOH aqueous solution of 5mol/L, takes out behind the 5min, fully cleans with a large amount of deionized waters, removes the remaining alkali lye in surface to neutral.The Kapton film of said hydrolyzed processing at room temperature be impregnated in the AlCl of 0.5mol/L
3Take out behind the 120min in the aqueous solution, fully clean with a large amount of deionized waters, remove surperficial residual metal salts solution, seasoning in air; Al will be contained after the ion-exchange
3+The Kapton film in the controlled tube furnace of high temperature, contain oxygen thermal treatment, be warming up to 300 ℃ with 4 ℃/min of heat-up rate from room temperature, the insulation 120min, cool to room temperature then with the furnace; So far, prepare Kapton/Al of the present invention
2O
3The nano surface laminated film.
By atomic force microscope to pure Kapton film and the Kapton/Al of the present invention that obtained by above-described embodiment 1
2O
3The nano compound film surface is observed, and pure Kapton film surface is uneven, and surfaceness (Ra) is 2.112nm, and film thickness is 50 μ m, as shown in Figure 1; And embodiment 1 gained Kapton/Al of the present invention
2O
3The nano compound film surface is distribution Al evenly
2O
3Nano particle, material surface area increase, and the surface becomes evenly, smoothly, and surfaceness (Ra) is 1.107nm, and film thickness increases to 52 μ m, as shown in Figure 2.
Embodiment 2:
The Kapton film is successively used acetone and dehydrated alcohol ultrasonic cleaning 10min, remove the residual organic pollutant of material surface, clean up back seasoning in air; The concentration that Kapton film after cleaning at room temperature be impregnated in is in the KOH aqueous solution of 5mol/L, takes out behind the 10min, fully cleans with a large amount of deionized waters, removes the remaining alkali lye in surface to neutral; The Kapton film of hydrolysis treatment at room temperature be impregnated in the AlCl of 0.5mol/L
3Take out behind the 120min in the aqueous solution, fully clean with a large amount of deionized waters, remove surperficial residual metal salts solution, seasoning in air; Al will be contained after the ion-exchange
3+The Kapton film in the controlled tube furnace of high temperature, contain oxygen thermal treatment, be warming up to 340 ℃ with 4 ℃/min of heat-up rate from room temperature, the insulation 120min, cool to room temperature then with the furnace, so far, prepare Kapton/Al of the present invention
2O
3The nano surface laminated film.
By atomic force microscope to pure Kapton film and the Kapton/Al of the present invention that obtained by above-mentioned enforcement 2
2O
3The nano compound film surface is observed, and pure Kapton film surface is uneven, and surfaceness (Ra) is 2.112nm, and film thickness is 50 μ m, as shown in Figure 1; And embodiment 2 gained Kapton/Al of the present invention
2O
3The nano compound film surface is distribution Al evenly
2O
3Nano particle, material surface area increase, and the surface becomes evenly, smoothly, and surfaceness (Ra) is 1.037nm, and film thickness increases to 51 μ m, as shown in Figure 3.
Embodiment 3:
The Kapton film is successively used acetone and dehydrated alcohol ultrasonic cleaning 10min, remove the residual organic pollutant of material surface, clean up back seasoning in air; The concentration that Kapton film after cleaning at room temperature be impregnated in is in the KOH aqueous solution of 4mol/L, takes out behind the 5min, fully cleans with a large amount of deionized waters, removes the remaining alkali lye in surface to neutral; The Kapton film of hydrolysis treatment at room temperature be impregnated in the AlCl of 0.4mol/L
3Take out behind the 60min in the aqueous solution, fully clean with a large amount of deionized waters, remove surperficial residual metal salts solution, seasoning in air; Al will be contained after the ion-exchange
3+The Kapton film in the controlled tube furnace of high temperature, contain oxygen thermal treatment, be warming up to 340 ℃ with 2 ℃/min of heat-up rate from room temperature, the insulation 180min, cool to room temperature then with the furnace; So far, prepare Kapton/Al of the present invention
2O
3The nano surface laminated film.
The Kapton/Al that above-described embodiment 3 is obtained
2O
3Nano surface laminated film, pure Kapton film, and the Kapton/Al that obtains at pure Kapton film and embodiment 3 respectively
2O
3Adopt sol-gel method to be coated with MEMO/SiO on the nano surface laminated film
2Film.Adopt single shaft experiment matrix thin film mechanical performance and laminated film interfacial combined function to estimate according to GB/T 1040.3-2006, the tensile strength of each film (σ) Mpa, unit elongation (ε) % and Young's modulus (E) GPa are as shown in the table, thereby draw Kapton/Al
2O
3The purer Kapton film of nano surface film toughness strengthens, Kapton/Al
2O
3The nano surface particle of nano surface film has increased the interface bonded area, in addition, and at Kapton/Al of the present invention
2O
3The nano surface film surface is coated with MEMO/SiO
2Film helps to form the mechanical bond at interface, and therefore, the bonding properties of laminated film and its surface film increases.
Kapton/Al of the present invention
2O
3The nano surface composite membrane can be applied to the surface elements of spacecraft, be matrix with this laminated film, be coated with other space environment protective films on the surface, the nano particle at laminated film interface has not only increased the interface bonded area, and help to form the mechanical bond at interface, so the bonding properties of laminated film and its surfacecti proteon film increases.
Although top invention has been described in conjunction with figure; but the present invention is not limited to above-mentioned embodiment; above-mentioned embodiment only is schematic; rather than it is restrictive; those of ordinary skill in the art is under enlightenment of the present invention; under the situation that does not break away from aim of the present invention, can also make a lot of distortion, these all belong within the protection of the present invention.
Claims (2)
1. Kapton/Al
2O
3The nano surface laminated film is characterized in that, is prepared by following steps:
Step 1, the Kapton film is successively used acetone and dehydrated alcohol ultrasonic cleaning 10min, remove the residual organic pollutant of material surface, clean up back seasoning in air;
Step 2, will be through step 1 surface-treated Kapton film, at room temperature impregnated in concentration is in the KOH aqueous solution of 1～5mol/L, takes out behind 5～10min, fully cleans to neutrality with a large amount of deionized waters;
Step 3, will at room temperature impregnated in the AlCl of 0.1～0.5mol/L through the Kapton of step 2 hydrolysis treatment film
3Take out behind 60～120min in the aqueous solution, fully clean with a large amount of deionized waters, remove surperficial residual metal salts solution, seasoning in air;
Step 4, will after step 3 ion-exchange, contain Al
3+The Kapton film in the controlled tube furnace of high temperature, contain oxygen thermal treatment, be warming up to 260～400 ℃ with 2～4 ℃/min of heat-up rate from room temperature, the insulation 60～180min, cool to room temperature then with the furnace.
2. Kapton/Al according to claim 1
2O
3The application of nano surface laminated film is characterized in that, this nano surface laminated film is used for the surface elements of spacecraft.
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| CN 201110404208 CN102418096B (en) | 2011-12-07 | 2011-12-07 | Kapton/Al2O3 surface nanometer composite membrane and application |
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| CN102418096B true CN102418096B (en) | 2013-08-07 |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1422897A (en) * | 2002-12-19 | 2003-06-11 | 中国科学院兰州化学物理研究所 | Self-lubricating organic-inorganic composite nano film and preparation method thereof |
| CN1979695A (en) * | 2006-11-22 | 2007-06-13 | 鲁东大学 | Flexible composite transparent conductive film and mfg. method |
| CN101812183A (en) * | 2009-07-28 | 2010-08-25 | 哈尔滨理工大学 | Method for preparing polyimide multilayer complex films containing inorganic nanometer powder |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1422897A (en) * | 2002-12-19 | 2003-06-11 | 中国科学院兰州化学物理研究所 | Self-lubricating organic-inorganic composite nano film and preparation method thereof |
| CN1979695A (en) * | 2006-11-22 | 2007-06-13 | 鲁东大学 | Flexible composite transparent conductive film and mfg. method |
| CN101812183A (en) * | 2009-07-28 | 2010-08-25 | 哈尔滨理工大学 | Method for preparing polyimide multilayer complex films containing inorganic nanometer powder |
Non-Patent Citations (2)
| Title |
|---|
| 吴战鹏."具有高反射和高导电特性聚酰亚胺银复合薄膜的制备及其形成机理研究".《中国优秀博硕士学位论文全文数据库（博士） 工程科技Ⅰ辑》.2006, |
| 吴战鹏."具有高反射和高导电特性聚酰亚胺银复合薄膜的制备及其形成机理研究".《中国优秀博硕士学位论文全文数据库(博士) 工程科技Ⅰ辑》.2006, * |
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