CN115449121B - Polypyrrole coated polyimide hybrid aerogel/phase change material composite film with infrared/electromagnetic double stealth function and preparation method thereof - Google Patents

Polypyrrole coated polyimide hybrid aerogel/phase change material composite film with infrared/electromagnetic double stealth function and preparation method thereof Download PDF

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CN115449121B
CN115449121B CN202211279261.2A CN202211279261A CN115449121B CN 115449121 B CN115449121 B CN 115449121B CN 202211279261 A CN202211279261 A CN 202211279261A CN 115449121 B CN115449121 B CN 115449121B
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phase change
composite film
change material
hybrid aerogel
polyimide hybrid
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CN115449121A (en
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汪晓东
史涛
刘欢
敬建伟
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Beijing University of Chemical Technology
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    • C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
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    • C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/36—After-treatment
    • C08J9/365—Coating
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    • C08J9/36—After-treatment
    • C08J9/40—Impregnation
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F41—WEAPONS
    • F41H—ARMOUR; ARMOURED TURRETS; ARMOURED OR ARMED VEHICLES; MEANS OF ATTACK OR DEFENCE, e.g. CAMOUFLAGE, IN GENERAL
    • F41H3/00—Camouflage, i.e. means or methods for concealment or disguise
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    • C08J2201/00—Foams characterised by the foaming process
    • C08J2201/04—Foams characterised by the foaming process characterised by the elimination of a liquid or solid component, e.g. precipitation, leaching out, evaporation
    • C08J2201/048—Elimination of a frozen liquid phase
    • C08J2201/0484—Elimination of a frozen liquid phase the liquid phase being aqueous
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    • C08J2205/02—Foams characterised by their properties the finished foam itself being a gel or a gel being temporarily formed when processing the foamable composition
    • C08J2205/026—Aerogel, i.e. a supercritically dried gel
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    • 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
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    • C08J2479/00—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 C08J2461/00 - C08J2477/00
    • C08J2479/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
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    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/14—Thermal energy storage

Abstract

The invention discloses a polypyrrole coated polyimide hybrid aerogel/phase change material composite film with infrared/electromagnetic double stealth and a preparation method thereof. The composite film is synthesized by taking a phase change material as a core material, taking a polyimide hybrid aerogel film as a porous framework and taking polypyrrole as a coating layer, taking polyamic acid salt as a matrix and taking a metal organic framework material and a carbon material as doping fillers, and the latent heat capacity of the composite film exceeds 150J/g, so that effective heat buffering and heat isolation can be realized on a target object. The preparation method of the composite film comprises the following steps: polymerizing, hybridizing, freeze drying and thermal imidizing the monomer to obtain polyimide hybridized aerogel film, and then dipping and surface spraying. The flexible composite film prepared by the invention is foldable, adjustable in shape, good in dynamic temperature regulation and control capability and microwave absorption performance, and capable of realizing infrared and electromagnetic double stealth function effects.

Description

Polypyrrole coated polyimide hybrid aerogel/phase change material composite film with infrared/electromagnetic double stealth function and preparation method thereof
Technical Field
The invention relates to the technical field of novel military equipment and electronic devices, in particular to a polyimide hybrid aerogel/phase change material composite film with infrared/electromagnetic double stealth and a preparation method thereof.
Background
With the rapid development of advanced composite detection technology, the multi-physical field stealth technology is receiving a great deal of attention. Currently, radar detection and infrared detection are two mainstream detection techniques. In most cases, the two detection technologies are required to be used simultaneously in military practice, so that the stealth materials of the compatible infrared and electromagnetic integration technology can be developed to effectively reduce the probability of detecting military targets and better realize the electromagnetic and infrared stealth functions.
The infrared stealth material exhibits the characteristics of high reflectivity and low absorption, and the total radiant heat energy of the unit surface area of the radiant target is proportional to the fourth power of the emissivity and the temperature of all the wavelengths according to the Stefan-Boltzmann law. In order to reduce the infrared characteristics of the target object, on one hand, infrared stealth can be achieved by reducing the thermal emissivity of the target object; on the other hand, controlling the target surface temperature through heat flow control and thermal barrier is another effective measure to achieve thermal infrared camouflage and thermal camouflage.
However, radar stealth materials generally exhibit low reflectivity and high absorption characteristics, and although many conventional electromagnetic wave absorption materials cannot meet the requirements of light weight, thin matching thickness, effective absorption bandwidth and strong absorption capacity. Therefore, how to effectively absorb electromagnetic radiation and meet the requirements of electromagnetic wave absorbing materials can reduce detected infrared signals while realizing electromagnetic stealth, and the method has important research significance for the application fields of military stealth and electromagnetic stealth.
Aerogels and hybrid materials thereof are considered to be ideal thermal insulation and promising infrared stealth materials due to their unique porous properties. At present, polyimide aerogel has great application potential in the aspects of infrared stealth and thermal camouflage, and research can form a composite/hybrid state by introducing various inorganic nano-sized fillers so as to improve the heat insulation stealth effect. Furthermore, in recent years, phase change materials have received a great deal of attention in infrared stealth and thermal camouflage applications by virtue of their ability to regulate infrared emissions through passive thermal management. In addition, the phase change material is a latent heat storage material, can store and release a large amount of heat energy through the reversible phase change of a physical state at almost constant temperature, has simple and reliable structure and wide phase change temperature selection range, can efficiently and economically store heat energy and regulate temperature, and has wide application prospect in an energy management system. Therefore, the phase change material is expected to adjust the target heat emissivity through controllable latent heat absorption and release in the phase change temperature process of different backgrounds, and good infrared stealth performance is realized.
Therefore, how to adopt the combination of aerogel and the hybrid material thereof and the phase change material to effectively realize infrared/electromagnetic stealth, and simultaneously, the requirements of light weight, thin matching thickness, effective absorption bandwidth and strong absorption capacity of the material can be met, which are the current research hot spot and difficult point.
Disclosure of Invention
Aiming at the prior art, the invention aims to provide a polypyrrole coated polyimide hybrid aerogel/phase change material composite film with infrared/electromagnetic double stealth and a preparation method thereof.
In order to achieve the above purpose, the invention adopts the following technical scheme:
in a first aspect of the invention, a polypyrrole coated polyimide hybrid aerogel/phase change material composite film is provided.
The polyimide hybrid aerogel/phase change material composite film coated by polypyrrole takes a phase change material as a core material, the polyimide hybrid aerogel film as a porous framework and the polypyrrole as a coating layer.
Preferably, the polyimide hybrid aerogel has a porosity of 95% or more and a tensile strength of 0.5 to 3.0MPa.
Further preferably, the polyimide hybrid aerogel has a porosity of 98% or more and a tensile strength of 1.0 to 2.5MPa
Preferably, the polyimide hybrid aerogel is synthesized by taking polyamic acid salt as a matrix and taking a metal organic framework material and a carbon material as doping fillers.
Preferably, the metal organic framework material is UiO series.
Preferably, the carbon material is one or more of graphene, carbon nano-tube and new transition metal carbon-containing material MXene.
Preferably, the phase change material is one or more of polyethylene glycol, fatty acid and sugar alcohol.
Preferably, the thickness of the polypyrrole coated polyimide hybrid aerogel/phase change material composite film is 50-1000 mu m.
Further preferably, the thickness of the polypyrrole coated polyimide hybrid aerogel/phase change material composite film is 400-800 mu m.
The invention provides a preparation method of a polyimide hybrid aerogel/phase change material composite film coated by polypyrrole, which comprises the following steps:
(1) Adding dibasic acid anhydride, diamine and aminated metal organic frame material into an organic solvent, performing polycondensation reaction to obtain a metal organic frame material hybridized polyamic acid solution, adding organic base into the metal organic frame material hybridized polyamic acid solution, separating out solid in an acetone solvent, filtering and drying to obtain metal organic frame material hybridized polyamic acid salt solid;
(2) Adding the metal organic framework material hybridized polyamic acid salt solid into a dispersion solution containing organic alkali, stirring, adding a carbon material, stirring, and performing freeze drying and thermal imidization treatment to obtain a polyimide hybridized aerogel film;
(3) Soaking the polyimide hybrid aerogel film into a molten phase change material to obtain a polyimide hybrid aerogel/phase change material composite film;
(4) And spraying an pyrrole solution on the surface of the polyimide hybrid aerogel/phase change material composite film, and oxidizing the polyimide hybrid aerogel/phase change material composite film by an oxidant to prepare the polypyrrole-coated polyimide hybrid aerogel/phase change material composite film.
Preferably, in the step (1), the dibasic acid anhydride is one or more of pyromellitic dianhydride, biphenyl tetracarboxylic dianhydride and benzophenone tetracarboxylic dianhydride.
Preferably, in the step (1), the diamine is one or more of diaminodiphenyl ether, 4' diaminodiphenyl methane and p-phenylenediamine.
Preferably, in step (1), the metal organic framework material is UiO series.
Preferably, in the step (1), the mass ratio of the dibasic acid anhydride to the diamine is (1.00-1.02): 1.
Further preferably, in the step (1), the mass ratio of the dibasic acid anhydride to the diamine is 1.01:1.
Preferably, in the step (1), the mass ratio of the total mass of the diamine and the diamine to the aminated organometallic frame is 100: (1-5).
Preferably, in the step (1), the organic solvent is one or more of N, N-dimethylacetamide, N-dimethylformamide and N-methylpyrrolidone.
Preferably, in step (1), the solid content of polyamic acid in the polyamic acid solution hybridized with the metal organic frame material is 10 to 30wt%.
Preferably, in step (1), the organic base is one of triethanolamine, triethylamine and tripropylamine.
Preferably, in step (1), the amount of the organic base is 2 to 4 times the amount of the terminal-COOH substance of the polyamic acid hybridized with the metal organic frame material.
It is further preferred that in step (1), the amount of the organic base is 1.5 to 3 times the amount of the terminal-COOH substance of the polyamic acid hybridized with the metal organic frame material.
Preferably, in the step (2), the organic base is one of triethanolamine, triethylamine and tripropylamine.
Preferably, in the step (2), the dispersing agent of the dispersing solution containing the organic base is deionized water or tertiary butanol.
Preferably, in step (2), the metal organic framework material hybridized polyamic acid salt solid is contained in an organic base dispersion solution in an amount of 1 to 10wt%.
It is further preferred that in step (2) the content of the metal organic framework material hybridized polyamic acid salt solid in the organic base dispersion solution is 4 to 8wt%.
Preferably, in the step (2), the mass ratio of the metal organic framework material hybridized polyamic acid salt solid to the carbon material is 100: (1-10).
Preferably, the carbon material is one or more of graphene, carbon nano-tube and new transition metal carbon-containing material MXene.
Further preferably, the mass ratio of the metal organic framework material hybridized polyamic acid salt solid to the carbon material is 100: (5-8).
Preferably, in the step (2), the freezing method is one of unidirectional freezing, bidirectional freezing and random freezing.
Preferably, in the step (2), the freeze-drying temperature is-70-80 ℃ and the vacuum pressure is 0.5-5Pa.
Preferably, in step (2), the freeze-drying time is 8-16 hours.
Preferably, in the step (2), the temperature rising condition of the thermal imidization treatment is: preserving heat for 1h at 0-150 ℃; preserving heat for 2h at 150-300 ℃ and heating up rate of 1.25 ℃/min.
Preferably, in the step (2), the environment required for the thermal imidization is nitrogen or argon.
Preferably, in the step (3), the phase change material is one or more of polyethylene glycol, fatty acid and sugar alcohol.
Preferably, in the step (4), the oxidant is one or two of ferric trichloride solution and ammonium persulfate solution.
Preferably, in the step (4), the mass ratio of the pyrrole solution to the oxidant is 1: (2-4).
Preferably, in the step (4), the amount of the pyrrole solution is 5-10mL.
In a third aspect of the invention, the application of the polypyrrole coated polyimide hybrid aerogel/phase change material composite film in preparing electromagnetic and infrared double stealth materials is provided.
The invention has the beneficial effects that:
the polyimide hybrid aerogel film prepared by the organic component and inorganic component compounding and freeze drying technology has good flexibility, and the polypyrrole coated polyimide hybrid aerogel/phase change material composite film is prepared by a vacuum impregnation method and a spraying technology, has a simple preparation process, is easy to obtain raw materials, and is suitable for expanded production.
The polyimide hybrid aerogel/phase change material composite film coated by the flexible polypyrrole prepared by the invention is flexible and foldable, has good mechanical property, fatigue resistance, excellent heat regulation capability and heat cycle stability, and good heat management capability, can realize temperature regulation and control, has higher thermal shock property and good heat cycle stability, and can meet the long-term use requirements of stealth and electromagnetic double stealth applications.
The invention can reduce the surface temperature of the target by utilizing the thermal regulation capability of the phase-change material, thereby effectively inhibiting the infrared radiation of the target and meeting the requirements of the target in high-efficiency infrared stealth and thermal camouflage application. And meanwhile, the carbon material and the polypyrrole which is an electric loss type wave absorbing material are combined, so that the electromagnetic loss can be enhanced, the impedance matching characteristic of the material is improved, the magnetic energy dissipation capacity and the electromagnetic microwave absorption capacity are enhanced, and the electromagnetic stealth effect is further realized.
Because the polyimide aerogel film has the heat insulation effect of low heat conduction and a three-dimensional porous structure, the heat conduction of a solid phase is reduced, so that the static regulation and control of the surface temperature of a high-temperature target are realized, in addition, the metal organic framework material and the carbon material can enhance the internal photo-thermal conversion of the aerogel, the rapid thermal response of the phase change material loaded in the aerogel on a heat source is effectively promoted, the heat buffering is provided for a system through the latent heat absorption in the phase change process, the surface temperature is effectively reduced, the detected time is prolonged, and the surface temperature of an object is dynamically controlled to realize the stealth effect. Therefore, the polyimide hybrid aerogel/phase change material composite film coated by polypyrrole can effectively realize infrared stealth and thermal camouflage of targets in a wide temperature range.
The effective bandwidth (R) of the polypyrrole coated polyimide hybrid aerogel/phase change material composite film prepared by the invention L < -10 dB) covers the entire X-band, and the minimum reflection loss peak can reach-56.8 dB, which is very attractive for military radars and direct broadcast satellites. The prepared polyimide hybrid aerogel/phase change material composite film coated by polypyrrole has wider broadband absorption capacity, and the carbon material and the polypyrrole material have synergistic enhancement, so that the electromagnetic wave absorption capacity is improved, the electromagnetic stealth of a target in a wide temperature and wide electromagnetic frequency band range is realized, and the polyimide hybrid aerogel/phase change material composite film is applicable to electromagnetic stealth application scenes.
Therefore, the polyimide hybrid aerogel/phase change material composite film coated by polypyrrole and provided by the invention provides a new strategy for designing and developing a high-performance and lightweight infrared/electromagnetic dual-function stealth material, and further has a wide application prospect.
The polypyrrole coated polyimide hybrid aerogel/phase change material composite film prepared by the invention has wider broadband absorption capacity, and the carbon material and the resistance loss type material have synergistic enhancement effect, so that the electromagnetic wave absorption capacity is improved, the electromagnetic stealth of a target in a wide temperature and wide electromagnetic frequency band range is realized, and the polyimide hybrid aerogel/phase change material composite film can be suitable for electromagnetic stealth application scenes.
Drawings
Fig. 1: (a) a scanning electron micrograph of the polyimide hybrid aerogel film of example 3, (b) a scanning electron micrograph of the polyimide hybrid aerogel/phase change material composite film of example 3, and (c) a scanning electron micrograph of the polypyrrole-coated polyimide hybrid aerogel/phase change material composite film of example 3;
fig. 2: differential scanning calorimeter map of polypyrrole coated polyimide hybrid aerogel/phase change material composite film in example 3;
fig. 3: thermal infrared imaging contrast plots of polypyrrole coated polyimide aerogel/phase change material composite films in example 3 versus composite films in comparative examples 1-3;
fig. 4: a graph comparing electromagnetic microwave absorption capacity of polypyrrole coated polyimide aerogel/phase change material composite film in example 3 with that of the composite films in comparative examples 1-3;
fig. 5: electromagnetic microwave absorption capacity comparison graphs of polypyrrole coated polyimide aerogel/phase change material composite films in examples 3-7.
Detailed Description
It should be noted that the following detailed description is illustrative and is intended to provide further explanation of the present application. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs.
In order to enable those skilled in the art to more clearly understand the technical solutions of the present application, the technical solutions of the present application will be described in detail below with reference to specific embodiments.
The test materials used in the examples of the present invention are all conventional in the art and are commercially available.
Example 1
(1) 5.49g of p-phenylenediamine and 0.39g of UiO-66-NH were taken 2 50.0mL of N-methylpyrrolidone solvent is added into the particles, 16.5g of benzophenone tetracarboxylic dianhydride is added in batches after stirring for 30min, the mixture is vigorously stirred in an ice-water bath for 3h to obtain a polyamic acid solution hybridized by a metal organic framework material, wherein the solid content of polyamic acid in the solution is 30wt%, 78.1mL of tripropylamine is slowly dripped into the flask, the mixture is stirred for 5h to obtain a polyamic acid solution hybridized by the metal organic framework, and then the polyamic acid solution is precipitated in acetone, filtered and washed to obtain a precipitated filiform substance, and finally the precipitated filiform substance is dried in a vacuum oven at 65 ℃ for 24h to obtain a polyamic acid salt solid hybridized by the metal organic framework.
Wherein the amino-functionalized metal organic framework UiO-66-NH 2 Is prepared from the following steps: taking 5.044g of acetic acid and 0.12g of 2-amino terephthalic acid, adding 30mL of N, N-dimethylformamide solvent, and performing ultrasonic treatment until the mixture is completely dissolved to form solution A; then 0.14g of zirconium chloride is dissolved in 20mL of N, N-dimethylformamide and is subjected to ultrasonic treatment to form a solution B, A, B parts of the solution are stirred and mixed, and the solution B is placed into a vacuum drying oven and heated for 12 hours at 120 ℃; finally, the diluted white precipitate solution was removed from the oven and centrifuged in a centrifuge at 9000r/min for 15min. Finally washing with ethanol once, and vacuum drying to obtain UiO-66-NH 2 And (3) particles.
(2) 2.0g of the metal organic framework hybridized polyamic acid salt solid was added to a dispersion solution of tripropylamine, wherein 1.0mL of tripropylamine and 46.9mL of deionized water were uniformly mixed to obtain a dispersion solution of tripropylamine. Adding 0.06g of MXene into the solution, stirring for 6 hours at room temperature, coating to form a film, performing bidirectional freeze drying for 8 hours, wherein the freezing temperature is-70 ℃, the vacuum pressure is 0.5Pa, obtaining a polyimide hybrid aerogel film containing the MXene, and then performing high-temperature thermal imidization in a nitrogen environment, thus obtaining the polyimide hybrid aerogel film.
Wherein, the heating conditions of the thermal imidization treatment are as follows: preserving heat for 1h at 0-150 ℃; preserving heat for 2h at 150-300 ℃ and heating up rate of 1.25 ℃/min.
(3) Immersing the polyimide hybrid aerogel film in the step (2) into molten sugar alcohol in a vacuum oven at 180 ℃ for 8 hours to obtain the polyimide hybrid aerogel/phase change material composite film.
(4) 13.7g of ammonium persulfate and 5.68g of ferric trichloride are weighed and dissolved in 100mL of distilled water, and named as solution A; 5mL of pyrrole was added to 50mL of isopropanol and mixed thoroughly, designated solution B. And (3) uniformly spraying the A and the B on the surface of the polyimide hybrid aerogel/phase change material composite film prepared in the step (3) to obtain the polypyrrole coated polyimide hybrid aerogel/phase change material composite film.
Example 2
(1) 4.74g of 4,4' diaminodiphenylmethane and 0.39g of UiO-66-NH were taken 2 50.0mL of N, N-dimethylformamide solvent is added into the particles, 7.11g of biphenyl tetracarboxylic dianhydride is added in batches after stirring for 30min, the mixture is vigorously stirred in an ice-water bath for 3h to obtain a polyamic acid solution containing metal organic framework hybridization, wherein the solid content of polyamic acid in the solution is 20wt%, then 22.8mL of triethanolamine is slowly dripped into the flask, the mixture is stirred for 5h to obtain a polyamic acid salt solution containing metal organic framework material hybridization, and then the solution is subjected to precipitation, filtration and washing in acetone to obtain a precipitated filiform substance, and finally the precipitated filiform substance is dried in a vacuum oven at 65 ℃ for 24h to obtain the polyamic acid salt solid containing metal organic framework hybridization.
Wherein UiO-66-NH 2 The preparation of the granules was carried out in the same manner as in example 1.
(2) 4.0g of metal organic framework hybridized polyamic acid salt solid is added into a triethanolamine dispersion solution, wherein 1.0mL of triethanolamine and 45.9mL of tertiary butanol are uniformly mixed, and thus the triethanolamine dispersion solution is obtained. Adding 0.24g of carbon nano tube into the solution, stirring for 6 hours at room temperature, coating to form a film, carrying out unidirectional freeze drying for 12 hours, wherein the freezing temperature is-75 ℃, the vacuum pressure is 2.5Pa, obtaining a polyimide hybrid aerogel film containing carbon nano tubes, and then carrying out high-temperature thermal imidization in a nitrogen environment, thus obtaining the polyimide hybrid aerogel film.
(3) And (3) immersing the polyimide hybrid aerogel film obtained in the step (2) in molten fatty acid for 6 hours in a vacuum oven at 80 ℃ to obtain the polyimide hybrid aerogel/phase change material composite film.
(4) 23.26g of ferric trichloride is weighed and dissolved in 100mL of distilled water, and the solution is named solution A; 8mL of pyrrole was added to 50mL of isopropanol and mixed thoroughly, designated solution B. And (3) uniformly spraying the A and the B on the surface of the polyimide hybrid aerogel/phase change material composite film prepared in the step (3) to obtain the polypyrrole coated polyimide hybrid aerogel/phase change material composite film.
Example 3
(1) 6.12g of diaminodiphenyl ether and 0.39g of UiO-66-NH were taken 2 100.0mL of N, N-dimethylacetamide solvent is added into the particles, 6.87g of pyromellitic dianhydride is added in batches after stirring for 30min, the mixture is vigorously stirred in an ice water bath for 3h to obtain a polyamic acid solution containing metal organic framework material hybridization, wherein the solid content of polyamic acid in the solution is 10wt%, 21.9mL of triethylamine is slowly dripped into the flask, the mixture is stirred for 5h to obtain a polyamic acid salt solution containing metal organic framework material hybridization, and then the polyamic acid salt solution is subjected to precipitation, filtration and washing in acetone to obtain a precipitated filiform substance, and finally the precipitated filiform substance is dried in a vacuum oven at 65 ℃ for 24h to obtain the polyamic acid salt solid containing metal organic framework hybridization.
Wherein UiO-66-NH 2 The preparation of the granules was carried out in the same manner as in example 1.
(2) Adding 3.0g of metal organic framework hybridized polyamic acid salt solid into a triethylamine dispersion solution, uniformly mixing 1.0mL of triethylamine and 44.9mL of deionized water to obtain a triethylamine dispersion solution, adding 0.3g of graphene into the solution, stirring at room temperature for 6h, coating to form a film, randomly freeze-drying for 16h, obtaining a polyimide hybridization aerogel film containing graphene at a freezing temperature of-80 ℃ and a vacuum pressure of 5.0Pa, and performing thermal imidization in a nitrogen environment to obtain the polyimide hybridization aerogel film.
(3) And (3) immersing the polyimide hybrid aerogel film obtained in the step (2) into melted polyethylene glycol in a vacuum oven at the temperature of 100 ℃ for 5 hours to obtain the polyimide hybrid aerogel/phase change material composite film.
(4) 19.4g of ammonium persulfate was weighed and dissolved in 100mL of distilled water and designated as solution A; 10mL of pyrrole was added to 50mL of isopropanol and mixed thoroughly, designated solution B. Uniformly spraying the A and the B on the surface of the polyimide hybrid aerogel/phase change material composite film containing the graphene prepared in the step (3), and obtaining the polyimide hybrid aerogel/phase change material composite film coated by polypyrrole.
The polyimide hybrid aerogel/phase change material composite film coated with polypyrrole prepared in example 3 is subjected to metal spraying treatment and then is characterized by a scanning electron microscope, and the obtained scanning electron microscope pictures are shown in fig. 1, and are respectively (a) a polyimide hybrid aerogel film, (b) a polyimide hybrid aerogel/phase change material composite film and (c) a polyimide hybrid aerogel/phase change material composite film coated with polypyrrole.
The high porosity of the polyimide hybrid aerogel film is observed in fig. 1 (a), the pore size is uniform, the pore wall is thick, a powerful supporting frame is provided for filling the phase change material, and meanwhile, graphene sheets can be uniformly dispersed on the pore wall. As shown in fig. 1 (b), the prepared polyimide hybrid aerogel/phase-change material composite film is impregnated with enough polyethylene glycol, and no gap exists between the polyimide hybrid aerogel/phase-change material composite film and an aerogel framework, and fig. 1 (c) shows that polypyrrole serving as a surface coating layer can more effectively inhibit leakage of the phase-change material, so that the polyimide hybrid aerogel/phase-change material composite film is better used for infrared stealth practical application.
The heat flow-temperature curve of the polyimide hybrid aerogel phase-change composite film coated with polypyrrole prepared in example 3 is shown in fig. 2 after the phase-change composite film is tested by a differential scanning calorimeter.
The melting enthalpy and the crystallization enthalpy of the polyimide hybrid aerogel/phase change material composite film obtained by integrating the curves in the figure 2 are respectively 154.4J/g and 151.8J/g, and the polyimide hybrid aerogel/phase change material composite film has good latent heat storage-release performance and high heat storage capacity, and is suitable for practical application of infrared stealth and heat camouflage.
Example 4
The difference between this example and example 3 is that the mass of graphene is 0.24g, and other technical details are the same as example 3.
Example 5
The difference between this example and example 3 is that the mass of graphene is 0.18g, and other technical details are the same as example 3.
Example 6
The difference between this example and example 3 is that the mass of graphene is 0.12g, and other technical details are the same as example 3.
Example 7
The difference between this embodiment and embodiment 3 is that the mass of graphene is 0.06g, and other technical details are the same as embodiment 3.
Comparative example 1: polyimide aerogel phase-change composite film coated by polypyrrole without graphene
The difference between this embodiment and embodiment 3 is that the mass of graphene is 0g, and other technical details are the same as embodiment 3.
Comparative example 2: polyimide hybrid aerogel/phase change composite film without graphene and polypyrrole coating
(1) 6.12g of diaminodiphenyl ether and 0.39g of UiO-66-NH were taken 2 100.0mL of N, N-dimethylacetamide solvent is added into the particles, 6.87g of pyromellitic dianhydride is added in batches after stirring for 30min, the mixture is vigorously stirred in an ice water bath for 3h to obtain a polyamic acid solution containing metal organic framework material hybridization, wherein the solid content of polyamic acid in the solution is 10wt%, 21.9mL of triethylamine is slowly dripped into the flask, the mixture is stirred for 5h to obtain a polyamic acid salt solution containing metal organic framework material hybridization, and then the polyamic acid salt solution is subjected to precipitation, filtration and washing in acetone to obtain a precipitated filiform substance, and finally the precipitated filiform substance is dried in a vacuum oven at 65 ℃ for 24h to obtain the polyamic acid salt solid containing metal organic framework hybridization.
Wherein UiO-66-NH 2 The preparation of the granules was carried out in the same manner as in example 1.
(2) 3.0g of a metal organic framework hybridized polyamic acid salt solid was added to a dispersion solution of triethylamine, wherein 1.0mL of triethylamine and 44.9mL of deionized water were uniformly mixed to obtain a dispersion solution of triethylamine. Stirring for 6h at room temperature, coating to form a film, randomly freeze-drying for 16h, wherein the freezing temperature is-80 ℃, the vacuum pressure is 5.0Pa, and then obtaining the polyimide hybrid aerogel film, and performing high-temperature thermal imidization in a nitrogen environment to obtain the polyimide hybrid aerogel film.
(3) Immersing the polyimide hybridization aerogel film containing graphene obtained in the step (2) into melted polyethylene glycol in a vacuum oven at the temperature of 100 ℃ for 5 hours, and obtaining a target product.
Comparative example 3: polyimide aerogel/phase change material composite film without graphene and metal organic framework and without polypyrrole coating
(1) Taking 6.12g of diaminodiphenyl ether, adding 100.0mL of N, N-dimethylacetamide solvent, stirring for 30min, adding 6.87g of pyromellitic dianhydride in batches, vigorously stirring in an ice water bath for 3h to obtain a polyamic acid solution, wherein the solid content of the polyamic acid in the solution is 10wt%, slowly dropwise adding 21.9mL of triethylamine into a flask, stirring for 5h to obtain a polyamic acid salt solution hybridized by a metal organic framework material, then precipitating in acetone, filtering and washing to obtain a precipitated filiform substance, and finally drying in a vacuum oven at 65 ℃ for 24h to obtain a polyamic acid salt solid.
(2) 3.0g of polyamic acid salt solid was added to a dispersion solution of triethylamine, wherein 1.0mL of triethylamine and 44.9mL of deionized water were uniformly mixed to obtain a dispersion solution of triethylamine. Stirring for 6h at room temperature, coating to form a film, randomly freeze-drying for 16h, wherein the freezing temperature is-80 ℃, and the vacuum pressure is 5.0Pa, so as to obtain the aerogel film containing polyimide, and then carrying out high-temperature thermal imidization in a nitrogen environment, so as to obtain the aerogel film containing polyimide.
(3) And (3) immersing the polyimide aerogel film obtained in the step (2) into melted polyethylene glycol in a vacuum oven at the temperature of 100 ℃ for 5 hours to obtain the polyimide aerogel/phase change material composite film.
Test example 1:
the polypyrrole-coated polyimide hybrid aerogel/phase change material composite film prepared in examples 1 to 3 was pressed into a ring shape with standard outer diameter, inner diameter and thickness to adapt to a sample holder in an instrument, electromagnetic parameters of a sample were measured by using a vector network analyzer by a transmission/reflection method, and the microwave absorption effect of the sample was determined according to the obtained electromagnetic parameters within a certain range (4 to 18 GHz), as shown in table 1.
TABLE 1 electromagnetic microwave absorption Performance parameters of hybrid aerogel/phase change Material composite films in examples 1-3
Figure BDA0003897998960000101
The absorption capacity of a material for electromagnetic waves is generally measured by reflection loss (R L ) Expressed by R L The higher the absolute value, the more powerful the ability to absorb electromagnetic waves, and when the absolute value is greater than 10dB, it is shown that 90% of the electromagnetic wave energy can be absorbed.
Figure BDA0003897998960000102
Figure BDA0003897998960000103
Wherein each represents the meaning: input impedance (Z) in ) Free space impedance (Z) 0 ) Light velocity (c), electromagnetic wave frequency (f), complex permittivity (epsilon), complex permeability (mu), thickness (d) of the composite film.
As can be seen from table 1, the hybrid aerogel/phase change material composite films of examples 1 to 3 all have good electromagnetic microwave absorption effects, wherein the hybrid aerogel/phase change material composite film of example 3 has smaller reflection loss values and wider effective absorption bands than the hybrid aerogel/phase change material composite films of examples 1 and 2, and thus can exhibit better electromagnetic microwave absorption effects.
Test example 2
The polypyrrole-coated polyimide hybrid aerogel phase-change composite film (S1) prepared in example 3, the undoped graphene-coated polyimide hybrid aerogel film (S2) prepared in comparative example 1, the undoped graphene prepared in comparative example 2, and the polyimide hybrid aerogel/phase-change material composite film (S3) not coated with polypyrrole, the undoped graphene prepared in comparative example 3, and the polyimide aerogel/phase-change composite film (S4) not coated with metal organic frames and coated with polypyrrole were placed on a hot bench having a constant temperature of 90 ℃ respectively, and the temperature change process thereof was recorded using a thermal infrared camera, and the thermal infrared stealth performance test results are shown in fig. 3.
As can be seen from fig. 3, the four samples S1, S2, S3, S4 exhibited a significant color change from blue to yellow rapidly after the heating process of 1 minute and 5 minutes. Comparing S1 and S2, the composite film (S1) added with the hybrid filler graphene has a slightly faster temperature change response, which shows that the addition of the graphene can enhance a certain photo-thermal conversion capability, so that the filled phase change material can quickly respond to and convert phases on a heat source, the large latent heat adsorption can cause slow response to background temperature, an additional thermal buffering effect is generated on the composite film, the surface temperature of the composite film is effectively reduced, the detection time of a thermal infrared camera is delayed, and the target and the environmental temperature of the composite film are fused as much as possible. And compared with S1, S2, S3 and S4, the temperature change difference value after 5 minutes is found to fluctuate within the range of 2-4 ℃, so that the influence of thermal infrared imaging of the composite film coated by the graphene, the metal organic frame and the polypyrrole is smaller, better electromagnetic performance is ensured, and meanwhile, a certain temperature control effect is still achieved, and therefore, the thermal infrared imaging device is very beneficial to infrared stealth and thermal camouflage of a heat source for infrared detection.
The microwave absorbing capacities of the composite films prepared in example 3 and comparative examples 1 to 3, respectively, were measured by a vector network analyzer and are shown in fig. 4.
As can be seen from fig. 4, the composite film prepared in example 3 has smaller minimum reflection loss value and wider effective absorption frequency band compared with comparative examples 1-3, which also illustrates the composite of the metal organic frame material, the carbon material and the resistive loss material, forming dielectric and electromagnetic multistage dissipation, improving the impedance matching characteristics of the material, enhancing the electromagnetic energy dissipation capability, thereby having better microwave absorption capability and more effectively realizing electromagnetic stealth.
Test example 3
The polypyrrole coated polyimide phase-change composite films with different graphene contents prepared in examples 3-7 are tested by a vector network analyzer to obtain the microwave absorption capacity shown in figure 5.
As can be seen from fig. 5, as the content of graphene increases, the minimum reflection loss value becomes smaller, and when the content of example 3 is reached, the minimum reflection loss value can reach-56.8 dB, and the microwave absorption effect is the best.
The foregoing description is only of the preferred embodiments of the present application and is not intended to limit the same, but rather, various modifications and variations may be made by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principles of the present application should be included in the protection scope of the present application.

Claims (2)

1. The polyimide hybrid aerogel/phase change material composite film coated by polypyrrole is characterized in that the polyimide hybrid aerogel/phase change material composite film takes a phase change material as a core material, the polyimide hybrid aerogel film is a porous framework, and the polypyrrole is a surface coating; the polyimide hybrid aerogel is synthesized by taking polyamic acid salt as a matrix and taking a metal organic framework material and a carbon material as doping fillers;
the metal organic framework material is UiO series; the carbon material is one or more of graphene, carbon nano tube and a new transition metal carbon-containing material MXene; the phase change material is one or more of polyethylene glycol, fatty acid and sugar alcohol;
the preparation method of the polypyrrole coated polyimide hybrid aerogel/phase change material composite film comprises the following steps:
(1) Adding dibasic acid anhydride, diamine and aminated metal organic frame material into an organic solvent, performing polycondensation reaction to obtain a metal organic frame material hybridized polyamic acid solution, adding organic base, separating out solid in an acetone solvent, filtering and drying to obtain a metal organic frame material hybridized polyamic acid salt solid;
(2) Adding the metal organic framework material hybridized polyamic acid salt solid into a dispersion solution containing organic alkali, stirring, adding a carbon material, stirring, and performing freeze drying and thermal imidization treatment to obtain a polyimide hybridized aerogel film;
(3) Soaking the polyimide hybrid aerogel film into a molten phase change material to obtain a polyimide hybrid aerogel/phase change material composite film;
(4) Spraying pyrrole solution on the surface of the polyimide hybrid aerogel/phase change material composite film, and oxidizing the polyimide hybrid aerogel/phase change material composite film by using an oxidant to prepare a polypyrrole coated polyimide hybrid aerogel/phase change material composite film;
in the step (1), the dicarboxylic anhydride is one or more of pyromellitic dianhydride, biphenyl tetracarboxylic dianhydride and benzophenone tetracarboxylic dianhydride, the diamine is one or more of diaminodiphenyl ether, 4' -diaminodiphenyl methane and p-phenylenediamine, the organic solvent is one or more of N, N-dimethylacetamide, N-dimethylformamide and N-methylpyrrolidone, and the mass ratio of the dicarboxylic anhydride to the diamine is (1.00-1.02): 1, a step of; the mass ratio of the total mass of the dibasic acid anhydride and the diamine to the metal amide organic framework is 100: (1-5) the solid content of polyamic acid in the polyamic acid solution hybridized by the metal organic frame material is 10-30wt%, the organic base is one or more of triethanolamine, triethylamine and tripropylamine, and the mass ratio of the organic base to the carboxyl at the end of the polyamic acid hybridized by the metal organic frame material is (2-4): 1;
in the step (2), the dispersing agent of the dispersing solution containing the organic base is deionized water or tertiary butyl alcohol, the content of the metal organic framework material hybridized polyamic acid salt solid in the organic base dispersing solution is 1-10wt%, and the mass ratio of the metal organic framework material hybridized polyamic acid salt solid to the carbon material is 100: (1-10), wherein the freezing method is one or more of unidirectional freezing, bidirectional freezing and random freezing, the freezing and drying temperature is-70-80 ℃, the vacuum pressure is 0.5-5Pa, the freezing and drying time is 8-16h, and the heating condition of the thermal imidization treatment is as follows: preserving heat for 1h at 0-150 ℃; preserving heat for 2 hours at the temperature of 150-300 ℃ and the heating rate of 1.25 ℃/min;
in the step (4), the oxidant is ferric trichloride solution or ammonium persulfate solution; the mass ratio of the pyrrole solution to the oxidant is (1-4): (3-12).
2. The use of the polypyrrole coated polyimide hybrid aerogel/phase change material composite film of claim 1 in the preparation of a material with infrared/electromagnetic double stealth.
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