CN115216047B - Preparation method and application of multifunctional visible light transparent low-infrared emission polymer composite film - Google Patents
Preparation method and application of multifunctional visible light transparent low-infrared emission polymer composite film Download PDFInfo
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- CN115216047B CN115216047B CN202211047419.3A CN202211047419A CN115216047B CN 115216047 B CN115216047 B CN 115216047B CN 202211047419 A CN202211047419 A CN 202211047419A CN 115216047 B CN115216047 B CN 115216047B
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- 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
- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
- C08J7/04—Coating
- C08J7/06—Coating with compositions not containing macromolecular substances
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D1/00—Coating compositions, e.g. paints, varnishes or lacquers, based on inorganic substances
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- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/32—Radiation-absorbing paints
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
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- C23C14/086—Oxides of zinc, germanium, cadmium, indium, tin, thallium or bismuth
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- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
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- C08J2333/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
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- C08J2333/06—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers esters of esters containing only carbon, hydrogen, and oxygen, the oxygen atom being present only as part of the carboxyl radical
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Abstract
A preparation method and application of a multifunctional visible light transparent low-infrared emission polymer composite film comprise the following steps: (1) pre-treating the transparent polymer film; (2) preparing an MXene solution; (3) Performing magnetron sputtering on the surface of the pretreated transparent polymer film in the step (1) to obtain an ITO conductive layer with a certain thickness, and performing annealing treatment; and then, circularly spraying MXene solution with a certain concentration, and obtaining the transparent low-infrared emission polymer composite film with a certain infrared emission rate and visible light transmittance by controlling the spraying times. The preparation method has the advantages of simple preparation process, low preparation cost and strong controllability, and can be used for batch preparation; the prepared transparent low-infrared emission polymer film can easily regulate and control visible light transmittance, infrared emissivity and conductivity, and can be applied to the fields of infrared stealth, thermal camouflage, radiation heating, photo-thermal, electric heating and the like.
Description
Technical Field
The invention belongs to the technical field of new materials, and particularly relates to a preparation method and application of a multifunctional visible light transparent low-infrared emission polymer composite film.
Background
The material with transparent visible light and low infrared emission has important application in the fields of infrared stealth, building energy conservation, radiant heating, electrothermal conversion, photothermal conversion and the like. Such materials are rare in nature but have great demands in production and living. Common low-emission materials are mainly metals, but the metals are usually opaque, and have the problems of easy corrosion, high density, difficult processing and the like. Some metal nanowires and optical metamaterials have been used for preparing visible light transparent low-infrared emission materials, but the method often has the problems of high cost, difficult preparation and the like. Many polymers have the advantages of high transparency, light weight, corrosion resistance, easy processing and the like, but have higher emissivity. Therefore, doping low-infrared emission fillers in polymers is an effective strategy for preparing low-infrared emission polymer composites.
MXene is a novel two-dimensional crystal material with the general formula of M n+1 X n T X Wherein M is a transition metal, X is carbon or nitrogen, T is a terminal group, O, F, H or the like. MXene has the characteristic of intrinsic low emissivity, which can reduce the loss of infrared radiation and realize the capability of passive radiation heating, and in addition, MXene has excellent sunlight absorption capability in solar spectrum, so that the MXene has excellent photo-thermal conversion capability, and simultaneously, MXene also has excellent conductivity, so that certain conductivity can be given to the film. ITO is a nano indium tin metal oxide with excellent conductivity and transmittance, and is an ideal material for preparing transparent conductive films.
Disclosure of Invention
The invention aims to solve the defects in the prior art, and provides a preparation method and application of a polymer film for preparing visible light transparent low-infrared emission by a method for applying a coating on the surface of a polymer, so that the polymer composite film for visible light transparent low-infrared emission has the capabilities of infrared stealth, passive radiation heating with zero energy consumption and photo-thermal/electric-thermal conversion.
In order to solve the technical problems, the invention adopts the following technical scheme: the preparation method of the multifunctional visible light transparent low-infrared emission polymer composite film comprises the following steps:
(1) Pretreating a transparent polymer film;
(2) Preparing an MXene solution;
(3) Performing magnetron sputtering on the surface of the pretreated transparent polymer film in the step (1) to obtain an ITO conductive layer with a certain thickness, and performing annealing treatment; and then, circularly spraying MXene solution with a certain concentration, and obtaining the transparent low-infrared emission polymer composite film with a certain infrared emission rate and visible light transmittance by controlling the spraying times.
Preferably, the transparent polymer film in the step (1) is made of polyethylene terephthalate (PET), polycarbonate (PC), polymethyl methacrylate (PMMA), polydimethylsiloxane (PDMS), polypropylene (PP), polyethylene (PE) or polyvinyl chloride (PVC);
the specific pretreatment process of the step (1) is as follows: ultrasonic cleaning transparent polymer film with alcohol for 5-10 min, and treating with plasma cleaner for 0.5-2 min.
Preferably, the specific preparation process of the step (2) is as follows: adding LiF powder of 10-200-g into HCl solution of 5-20 mol/L at 20-60 ℃ and stirring for 20-60 min to prepare HF etching solution; adding MAX phase powder of 10-200 and g into etching liquid, stirring at 20-60 ℃ for reaction for 18-36 h to obtain a reaction product, diluting the obtained reaction product, pouring into a centrifuge tube, centrifuging for 4-8 min at a rotating speed of 2500-4500, separating supernatant, repeatedly centrifuging until the pH is more than or equal to 6 to obtain MXene precipitate, adding deionized water into the precipitate, shaking for 5-10 min, centrifuging for 4-8 min at a rotating speed of 2500-4500, and obtaining the supernatant which is the MXene solution with certain concentration.
Preferably, in the step (3), the ITO conductive layer with a certain thickness is 0-500-nm.
Preferably, in the step (3), the concentration of the MXene solution with a certain concentration is circularly sprayed to be 0.1-20 mg/mL, and the cycle spraying times are 0-100 times.
Preferably, in the step (3), the infrared emissivity of the transparent low emissivity polymer composite film prepared by controlling the thickness of the MXene coating, i.e., controlling the concentration of the MXene solution and the spraying frequency of the MXene solution is 10% to 90%, and the transmittance is 30% to 90%.
Preferably, in the step (3), the radiation heating temperature range of the prepared transparent low-infrared emission polymer composite film is 1-10 ℃, and the sunlight heating temperature range is 5-50 ℃; the range of the applied voltage of the electrothermal conversion of the prepared transparent low-emissivity polymer composite film is 0.1-10V, and the temperature range which can be reached by the electrothermal conversion of the prepared transparent low-emissivity polymer composite film is 5-180 ℃.
Preferably, the light source for photo-thermal conversion of the prepared transparent low-infrared emission polymer composite film is one or more of near infrared light, far infrared light and sunlight.
Preferably, the heating mode of the prepared transparent low-infrared emission polymer composite film comprises one or more of passive radiation heating, photo-thermal and electric heating.
Preferably, applications in the fields of visible thermal camouflage, thin film radiant heating, thin film electrical heating, thin film optical heating and thermal conversion are included.
By adopting the technical scheme, the invention has the following technical effects:
the multifunctional visible light transparent low-infrared emissivity flexible polymer film prepared by the invention has the advantages that when the coating thickness is 300 nm, the polymer transmittance is 53 percent, the emissivity is 24.7 percent, the composite film has certain visible light transmittance and excellent infrared stealth capability, the temperature of a human body can be reduced from 32.0 ℃ to 20.8 ℃ under an infrared camera, meanwhile, the film has excellent zero-energy passive radiation heating capability, the heating temperature of the human body can be simulated to be 5.7 ℃, and in addition, the composite film has higher sunlight absorption capability and conductivity, and the surface of the film can be at 853.8W m -2 The solar energy heating device reaches a saturation temperature of 102.3 ℃ under solar irradiation and reaches a saturation temperature of 106.7 ℃ under a voltage of 6V, and the three heating modes can be used in any combination, can cope with various application scenes, and have important significance in saving energy and reducing energy consumption.
The preparation method has the advantages of simple preparation process, low preparation cost and strong controllability, and can be used for batch preparation; the prepared transparent low-infrared emission polymer film can easily regulate and control visible light transmittance, infrared emissivity and conductivity, and can be applied to the fields of infrared stealth, thermal camouflage, radiation heating, photo-thermal, electric heating and the like.
Drawings
FIG. 1 is a surface scanning electron microscope image of a PET-ITO@MXene film prepared in example 3 of the invention;
FIG. 2 is a surface scanning electron microscope image of the PET-ITO film prepared in example 4 of the present invention;
FIG. 3 is a cross-sectional scanning electron microscope of the PET-ITO@MXene film prepared in example 3 of the invention;
FIG. 4 is a graph showing the transmittance of visible light of PET-ITO@MXene films prepared in examples 1 to 5 and comparative example 1 according to the present invention;
FIG. 5 is a graph showing the mid-IR spectrum emissivity of PET-ITO@MXene films prepared in examples 2 to 5 of the present invention and comparative example 1;
FIG. 6 is a graph showing the electrothermal conversion properties of the PET-ITO@MXene film prepared in example 3 of the present invention under different applied voltages;
FIG. 7 is a graph showing the photo-thermal conversion performance of the PET-ITO@MXene films prepared in examples 1 to 5 and comparative example 1 according to the present invention under outdoor sunlight irradiation;
FIG. 8 is a graph of simulated skin passive radiant heating under different film covers for PET-ITO@MXene films prepared in examples 1-5 and comparative example 1 of the present invention.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions in the embodiments of the present invention will be clearly and completely described in the following in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The preparation method of the multifunctional visible light transparent low-infrared emission polymer composite film comprises the following steps:
(1) Pretreating a transparent polymer film: ultrasonically cleaning the transparent polymer film with alcohol for 5-10 min, and treating with a plasma cleaning instrument for 0.5-2 min;
(2) Preparation of MXene solution: adding LiF powder of 10-200-g into HCl solution of 5-20 mol/L at 20-60 ℃ and stirring for 20-60 min to prepare HF etching solution; adding MAX phase powder of 10-200 g into etching liquid, stirring at 20-60 ℃ for reaction for 18-36 h to obtain a reaction product, diluting the obtained reaction product, pouring into a centrifuge tube, centrifuging for 4-8 min at a rotating speed of 2500-4500, separating supernatant, repeatedly centrifuging until the pH is more than or equal to 6 to obtain precipitate MXene, adding deionized water into the precipitate, shaking for 5-10 min, centrifuging for 4-8 min at a rotating speed of 2500-4500, and obtaining the supernatant which is a MXene solution with a certain concentration;
(3) Preparing a transparent low-infrared emission polymer composite film, and performing magnetron sputtering on the pretreated transparent polymer substrate to form an ITO conductive layer with a certain thickness and annealing; and then, circularly spraying MXene solution with certain concentration on the film, and obtaining the polymer film with certain infrared emissivity and visible light transmittance by controlling the spraying times.
Wherein the polymer-based film is one or more of polyethylene terephthalate (PET), polycarbonate (PC), polymethyl methacrylate (PMMA), polydimethylsiloxane (PDMS), polypropylene (PP), polyethylene (PE) and polyvinyl chloride (PVC); the MAX phase powder is Ti 3 AlC 2 、Ti 2 At least one of AlC.
Example 1
The preparation method of the multifunctional visible light transparent low-infrared emission polymer composite film comprises the following steps:
(1) Pretreating a transparent polymer film: ultrasonically cleaning a commercial polymer film (PET) with alcohol for 10 min, and treating with a plasma cleaner for 1.5 min to obtain a pretreated transparent polymer film;
(2) Preparation of MXene solution: the HF etching solution was prepared by placing 10 LiF powder g and 200 mL of 12 mol/L HCl solution in a Teflon beaker at room temperature and stirring for 30 min. 10 g MAX phase powder (MAX phase powder is Ti 3 AlC 2 、Ti 2 At least one of AlC) is added into HF etching solution, and magnetically stirred at 35 ℃ and 500 rpm for 24 h to prepareObtaining a reaction product; the prepared reaction product is repeatedly washed by deionized water and centrifuged for 5 min at 3500 rpm until the pH value is more than or equal to 6, and MXene precipitate is collected; adding deionized water into the precipitate MXene, shaking for 7 min, centrifuging at 3500 rpm for 5 min, and collecting supernatant to obtain a MXene solution with a certain concentration;
(3) Diluting the MXene solution: adding deionized water into the collected MXene solution to dilute the solution to the concentration of 1.5 mg/ml, and carrying out ultrasonic treatment on the diluted solution for 5 min;
(4) Preparing a PET/ITO/MXene composite film, carrying out magnetron sputtering on ITO of 100 nm on the pretreated PET film, and carrying out annealing treatment for later use. Repeatedly spraying MXene solution of 1.5 mg/ml 10 times on the surface of the ITO-sputtered composite film, and drying at room temperature to obtain PET-IM 10 A film.
Example 2
The preparation method of the multifunctional visible light transparent low-infrared emission polymer composite film comprises the following steps:
(1) Pretreating a transparent polymer film: ultrasonically cleaning a commercial polymer film (PET) with alcohol for 10 min, and treating with a plasma cleaner for 1.5 min to obtain a pretreated transparent polymer film;
(2) Preparation of MXene solution: the HF etching solution was prepared by placing 10 LiF powder g and 200 mL of 12 mol/L HCl solution in a Teflon beaker at room temperature and stirring for 30 min. 10 g MAX phase powder (MAX phase powder is Ti 3 AlC 2 、Ti 2 At least one of AlC) is added into HF etching solution, and magnetic stirring is carried out at 35 ℃ and 500 rpm for 24 h to obtain a reaction product; the prepared reaction product is repeatedly washed by deionized water and centrifuged for 5 min at 3500 rpm until the pH value is more than or equal to 6, and MXene precipitate is collected; adding deionized water into the precipitate MXene, shaking for 7 min, centrifuging at 3500 rpm for 5 min, and collecting supernatant to obtain a MXene solution with a certain concentration;
(3) Diluting the MXene solution: adding deionized water into the collected MXene solution to dilute the solution to the concentration of 1.5 mg/ml, and carrying out ultrasonic treatment on the diluted solution for 5 min;
(4) Preparation of PET/ITO/MXene composite film: and (3) carrying out magnetron sputtering on ITO of 100 nm on the pretreated PET film, and carrying out annealing treatment for standby. Repeatedly spraying MXene solution of 1.5 mg/ml on the surface of the ITO sputtered composite film for 30 times, and drying at room temperature to obtain PET-IM 30 A film.
Example 3
The preparation method of the multifunctional visible light transparent low-infrared emission polymer composite film comprises the following steps:
(1) Pretreating a transparent polymer film: ultrasonically cleaning a commercial polymer film (PET) with alcohol for 10 min, and treating with a plasma cleaner for 1.5 min to obtain a pretreated transparent polymer film;
(2) Preparation of MXene solution: the HF etching solution was prepared by placing 10 LiF powder g and 200 mL of 12 mol/L HCl solution in a Teflon beaker at room temperature and stirring for 30 min. 10 g MAX phase powder (MAX phase powder is Ti 3 AlC 2 、Ti 2 At least one of AlC) is added into HF etching solution, and magnetic stirring is carried out at 35 ℃ and 500 rpm for 24 h to obtain a reaction product; the prepared reaction product is repeatedly washed by deionized water and centrifuged for 5 min at 3500 rpm until the pH value is more than or equal to 6, and MXene precipitate is collected; adding deionized water into the precipitate MXene, shaking for 7 min, centrifuging at 3500 rpm for 5 min, and collecting supernatant to obtain a MXene solution with a certain concentration;
(3) Diluting the MXene solution: adding deionized water into the collected MXene solution to dilute the solution to the concentration of 1.5 mg/ml, and carrying out ultrasonic treatment on the diluted solution for 5 min;
(4) Preparing a PET/ITO/MXene composite film: and (3) carrying out magnetron sputtering on ITO of 100 nm on the pretreated PET film, and carrying out annealing treatment for standby. Repeatedly spraying MXene solution of 1.5 mg/ml on the surface of the ITO sputtered composite film 50 times, and drying at room temperature to obtain PET-IM 50 A film.
Example 4
The preparation method of the multifunctional visible light transparent low-infrared emission polymer composite film comprises the following steps: ultrasonically cleaning a commercial polymer film (PET) with alcohol for 10 min, and treating with a plasma cleaner for 1.5 min to obtain a pretreated transparent polymer film; and (3) carrying out magnetron sputtering on ITO of 100 nm on the pretreated PET film, and carrying out annealing treatment for standby, namely the PET-I film.
Example 5
The preparation method of the multifunctional visible light transparent low-infrared emission polymer composite film comprises the following steps:
(1) Pretreating a transparent polymer film: ultrasonically cleaning a commercial polymer film (PET) with alcohol for 10 min, and treating with a plasma cleaner for 1.5 min to obtain a pretreated transparent polymer film;
(2) Preparation of MXene solution: the HF etching solution was prepared by placing 10 LiF powder g and 200 mL of 12 mol/L HCl solution in a Teflon beaker at room temperature and stirring for 30 min. 10 g MAX phase powder (MAX phase powder is Ti 3 AlC 2 、Ti 2 At least one of AlC) is added into HF etching solution, and magnetic stirring is carried out at 35 ℃ and 500 rpm for 24 h to obtain a reaction product; the prepared reaction product is repeatedly washed by deionized water and centrifuged for 5 min at 3500 rpm until the pH value is more than or equal to 6, and MXene precipitate is collected; adding deionized water into the precipitate MXene, shaking for 7 min, centrifuging for 5 min at 3500 rpm, and collecting supernatant to obtain a MXene solution with a certain concentration;
(3) Diluting the MXene solution: adding deionized water into the collected MXene solution to dilute the solution to the concentration of 1.5 mg/ml, and carrying out ultrasonic treatment on the diluted solution for 5 min;
(4) Preparing a PET/MXene composite film: repeatedly spraying MXene solution of 1.5 mg/ml on the surface of the pretreated PET film for 30 times, and drying at room temperature to obtain PET-M 30 A film.
Example 6
The preparation method of the multifunctional visible light transparent low-infrared emission polymer composite film comprises the following steps:
(1) Pretreating a transparent polymer film: ultrasonically cleaning a commercial polymer film (PC) with alcohol for 10 min, and treating with a plasma cleaner for 1.5 min to obtain a pretreated transparent polymer film;
(2) Preparation of MXene solution: will 1 at room temperatureThe LiF powder of 0 g and the 12 mol/L HCl solution of 200 mL are placed in a polytetrafluoroethylene beaker and stirred for 30 min to prepare the HF etching solution. 10 g MAX phase powder (MAX phase powder is Ti 3 AlC 2 、Ti 2 At least one of AlC) is added into HF etching solution, and magnetic stirring is carried out at 35 ℃ and 500 rpm for 24 h to obtain a reaction product; the prepared reaction product is repeatedly washed by deionized water and centrifuged for 5 min at 3500 rpm until the pH value is more than or equal to 6, and MXene precipitate is collected; adding deionized water into the precipitate MXene, shaking for 7 min, centrifuging at 3500 rpm for 5 min, and collecting supernatant to obtain a MXene solution with a certain concentration;
(3) Diluting the MXene solution: adding deionized water into the collected MXene solution to dilute the solution to the concentration of 1.5 mg/ml, and carrying out ultrasonic treatment on the diluted solution for 5 min;
(4) Preparing a PC/ITO/MXene composite film: and (3) pretreating ITO of the magnetron sputtering 100 nm on the PC film, and carrying out annealing treatment for standby. Repeatedly spraying MXene solution of 1.5 mg/ml on the surface of the ITO sputtered composite film 50 times, and drying at room temperature to obtain PC-IM 50 A film.
Example 7
The preparation method of the multifunctional visible light transparent low-infrared emission polymer composite film comprises the following steps:
(1) Pretreating a transparent polymer film: ultrasonically cleaning a commercial polymer film (PMMA) with alcohol for 10 min, and treating with a plasma cleaner for 1.5 min to obtain a pretreated transparent polymer film;
(2) Preparation of MXene solution: the HF etching solution was prepared by placing 10 LiF powder g and 200 mL of 12 mol/L HCl solution in a Teflon beaker at room temperature and stirring for 30 min. 10 g MAX phase powder (MAX phase powder is Ti 3 AlC 2 、Ti 2 At least one of AlC) is added into HF etching solution, and magnetic stirring is carried out at 35 ℃ and 500 rpm for 24 h to obtain a reaction product; the prepared reaction product is repeatedly washed by deionized water and centrifuged for 5 min at 3500 rpm until the pH value is more than or equal to 6, and MXene precipitate is collected; adding deionized water into the precipitate MXene, shaking for 7 min, and centrifuging at 3500 rpm5 min, collecting supernatant to obtain a MXene solution with a certain concentration;
(3) Diluting the MXene solution: adding deionized water into the collected MXene solution to dilute the solution to the concentration of 1.5 mg/ml, and carrying out ultrasonic treatment on the diluted solution for 5 min;
(4) Preparing a PMMA/ITO/MXene composite film: and (3) carrying out magnetron sputtering on the ITO of 100 nm on the pretreated PMMA film, and carrying out annealing treatment for standby. Repeatedly spraying MXene solution of 1.5 mg/ml on the surface of the ITO-sputtered composite film 50 times, and drying at room temperature to obtain PMMA-IM 50 A film.
Example 8
The preparation method of the multifunctional visible light transparent low-infrared emission polymer composite film comprises the following steps:
(1) Pretreating a transparent polymer film: ultrasonically cleaning a commercial polymer film (PET) with alcohol for 10 min, and treating with a plasma cleaner for 1.5 min to obtain a pretreated transparent polymer film;
(2) Preparation of MXene solution: the HF etching solution was prepared by placing 10 LiF powder g and 200 mL of 12 mol/L HCl solution in a Teflon beaker at room temperature and stirring for 30 min. 10 g MAX phase powder (MAX phase powder is Ti 3 AlC 2 、Ti 2 At least one of AlC) is added into HF etching solution, and magnetic stirring is carried out at 35 ℃ and 500 rpm for 24 h to obtain a reaction product; the prepared reaction product is repeatedly washed by deionized water and centrifuged for 5 min at 3500 rpm until the pH value is more than or equal to 6, and MXene precipitate is collected; adding deionized water into the precipitate MXene, shaking for 7 min, centrifuging at 3500 rpm for 5 min, and collecting supernatant to obtain a MXene solution with a certain concentration;
(3) Diluting the MXene solution: adding deionized water into the collected MXene solution to dilute the solution to the concentration of 10 mg/ml, and carrying out ultrasonic treatment on the diluted solution for 5 min;
(4) Preparing a PET/ITO/MXene composite film: and (3) carrying out magnetron sputtering on ITO of 100 nm on the pretreated PET film, and carrying out annealing treatment for standby. And repeatedly spraying an MXene solution of 10 mg/ml on the surface of the ITO sputtered composite film for 50 times, and drying at room temperature to obtain the PET composite film.
Example 9
The preparation method of the multifunctional visible light transparent low-infrared emission polymer composite film comprises the following steps:
(1) Pretreating a transparent polymer film: ultrasonically cleaning a commercial polymer film (PET) with alcohol for 10 min, and treating with a plasma cleaner for 1.5 min to obtain a pretreated transparent polymer film;
(2) Preparation of MXene solution: the HF etching solution was prepared by placing 10 LiF powder g and 200 mL of 12 mol/L HCl solution in a Teflon beaker at room temperature and stirring for 30 min. 10 g MAX phase powder (MAX phase powder is Ti 3 AlC 2 、Ti 2 At least one of AlC) is added into HF etching solution, and magnetic stirring is carried out at 35 ℃ and 500 rpm for 24 h to obtain a reaction product; the prepared reaction product is repeatedly washed by deionized water and centrifuged for 5 min at 3500 rpm until the pH value is more than or equal to 6, and MXene precipitate is collected; adding deionized water into the precipitate MXene, shaking for 7 min, centrifuging at 3500 rpm for 5 min, and collecting supernatant to obtain a MXene solution with a certain concentration;
(3) Diluting the MXene solution: adding deionized water into the collected MXene solution to dilute the solution to the concentration of 1.5 mg/ml, and carrying out ultrasonic treatment on the diluted solution for 5 min;
(4) Preparing a PET/ITO/MXene composite film: and (3) carrying out magnetron sputtering on the ITO of 500 nm on the pretreated PET film, and carrying out annealing treatment for standby. And repeatedly spraying MXene solution of 1.5 mg/ml on the surface of the ITO-sputtered composite film for 50 times, and drying at room temperature to obtain the PET composite film.
Example 10
The preparation method of the multifunctional visible light transparent low-infrared emission polymer composite film comprises the following steps:
(1) Pretreating a transparent polymer film: ultrasonically cleaning a commercial polymer film (PET) with alcohol for 5 min, and treating with a plasma cleaner for 1.5 min to obtain a pretreated transparent polymer film;
(2) Preparation of MXene solution: placing 10 g LiF powder and 200 mL HCl solution of 12 mol/L in polytetrafluoroethylene at room temperatureStirring for 30 min in a beaker to obtain the HF etching solution. 10 g MAX phase powder (MAX phase powder is Ti 3 AlC 2 、Ti 2 At least one of AlC) is added into HF etching solution, and magnetic stirring is carried out at 35 ℃ and 500 rpm for 24 h to obtain a reaction product; the prepared reaction product is repeatedly washed by deionized water and centrifuged for 5 min at 3500 rpm until the pH value is more than or equal to 6, and MXene precipitate is collected; adding deionized water into the precipitate MXene, shaking for 7 min, centrifuging at 3500 rpm for 5 min, and collecting supernatant to obtain a MXene solution with a certain concentration;
(3) Diluting the MXene solution: adding deionized water into the collected MXene solution to dilute the solution to the concentration of 1.5 mg/ml, and carrying out ultrasonic treatment on the diluted solution for 5 min;
(4) Preparing a PET/ITO/MXene composite film: and (3) carrying out magnetron sputtering on ITO of 100 nm on the pretreated PET film, and carrying out annealing treatment for standby. And repeatedly spraying MXene solution of 1.5 mg/ml on the surface of the ITO-sputtered composite film for 50 times, and drying at room temperature to obtain the PET composite film.
Comparative example 1
And ultrasonically cleaning the PET film after 10 minutes by alcohol.
Comparative example 2
And ultrasonically cleaning the PC film after 10 min by alcohol.
Comparative example 3
And ultrasonically cleaning the PMMA film after 10 minutes by alcohol.
Test results and analysis of Polymer/MXene composite fabrics
(1) Scanning electron microscope analysis
As shown in FIG. 1, the surface of the PET/ITO/MXene composite film prepared in example 3 was observed by a scanning electron microscope. As shown in FIG. 2, the surface of the PET/ITO composite film prepared in example 4 was observed by a scanning electron microscope, and it was found that ITO nanoparticles were uniformly distributed on the PET film.
As shown in FIG. 3, the thickness of the ITO and MXene coating on the PET surface was observed by scanning electron microscopy on the cross section of the PET/ITO/MXene composite film prepared in example 3.
(2) Visible light transmittance test
Examples 1 to 5 were characterized by using an ultraviolet-visible spectrophotometer, and comparative example 1 was tested in the visible light band (300-800 nm), and the results are shown in fig. 4, and the examples all have good transmittance. The transmittance at 550 nm of examples 1 to 10 and comparative examples 1 to 3 is shown in table 1.
(3) Mid infrared emissivity test
Examples 2 to 4 were measured using a fourier transform infrared spectrometer with an integrating sphere, and the infrared reflectance of comparative example 1 [ ]ρ) And transmittance [ ]τ) Infrared emissivity [ ]ε) By passing throughThe results of the calculations are shown in FIG. 5, and the emissivity of examples 1-5 is significantly lower than that of comparative example 1. Average emissivity is +.>Performing a calculation in whichE black (λ, T) And epsilon%λ) Respectively represent the spectral radiation of a black body at t=300K, the corresponding infrared emittance at different wavelengths at room temperature. The average emissivity of examples 1 to 10 and comparative examples 1 to 3 in the 7-14 um band is shown in Table 1.
(4) Radiant heating Performance test
The examples 1-10, comparative examples 1-3 and black cotton cloth coated silicone rubber heating plates were subjected to a simulated passive radiant heating test. The silicone rubber heating plate was maintained at about 36 c by applying a dc power to it to simulate the skin temperature of a human body. A type K thermocouple was attached to the heating plate to record the surface temperature of the artificial skin covered with the composite film. The radiation heating temperature curves of examples 2 to 5 and comparative example 1 are shown in fig. 6. The passive radiation heating stabilization temperatures of examples 1 to 10 and comparative examples 1 to 3 are shown in table 1. It can be seen that the passive radiant heating capability of the examples is significantly better than the comparative examples, and the synergistic effect of ITO and MXene results in a composite film exhibiting lower infrared emissions and more excellent radiant heating and stealth properties.
(5) Photothermal performance test
The areas of examples 1 to 10, comparative examples 1 to 3 and black cotton cloth were 3X 3 cm 2 The composite film of (2) was irradiated under outdoor sunlight, a type K thermocouple was attached under the film for recording the temperature change of the film, and at the same time, solar irradiance was recorded using an irradiation meter, as shown in fig. 7, examples 2 to 5 exhibited excellent photothermal conversion effects, and at the same time, the surface temperatures of example 2, example 3, example 4, example 5 reached 96.2, 102.3, 70.1, 92.2 c, which were 38.1, 44.2, 12.0, 34.1 c higher than the surface temperatures of comparative example 1, respectively. The highest photothermal conversion temperatures of examples 1 to 10 and comparative examples 1 to 3 are shown in table 1 under clear weather. Examples 1-10 show excellent photo-thermal conversion effect, which proves that the PET/ITO/MXene composite film with transparent visible light and low infrared emission has great potential in building thermal management by using abundant solar energy.
(6) Electrothermal Performance test
Examples 1 to 10 and comparative examples 1 to 3 were taken to give a surface area of 1X 2 cm 2 The middle of the composite film is stuck with an adhesive tape with high infrared emissivity, and the two sides of the composite film are fixed by copper sheets; the temperature change of the film surface with time is recorded by using a small direct current power box to input different voltages and using a thermal infrared imager (the power is turned off after 90 s is pressurized, and the temperature change of 180 s is recorded). Different voltages are input, as shown in FIG. 8, the temperature of the PET/ITO/MXene composite film increases faster as the voltage increases; when the voltage of the power supply is increased to 6V, the temperature of the PET/ITO/MXene composite film reaches 106 ℃ at most. As shown in table 1, the highest electrothermal conversion temperature of the different films at an input voltage of 6V. Comparative examples 1 to 3 were not conductive, so that there was no electrothermal effect. Examples 1 to 10 all show obvious electrothermal conversion effects, and the synergistic effect of ITO and MXene makes the conductive performance and electrothermal conversion performance of the composite film more excellent.
TABLE 1 test results of Polymer composite films
In conclusion, the visible light transparent low-infrared emission polymer composite film prepared by the method has excellent infrared stealth, passive radiation heating, photo-thermal conversion capability and electric-thermal conversion capability, and has great potential in the fields of military safety, thermal management, building energy conservation and the like.
The above embodiments are only for illustrating the technical solution of the present invention, and are not limiting; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit and scope of the technical solutions of the embodiments of the present invention.
Claims (8)
1. A preparation method of a multifunctional visible light transparent low-infrared emission polymer composite film is characterized by comprising the following steps of: the method comprises the following steps:
(1) Pretreating a transparent polymer film;
(2) Preparing an MXene solution;
(3) Performing magnetron sputtering on the surface of the pretreated transparent polymer film in the step (1) to obtain an ITO conductive layer with a certain thickness, and performing annealing treatment; then, the MXene solution with certain concentration is recycled and sprayed, and a transparent low-infrared emission polymer composite film with certain infrared emission rate and visible light transmittance is obtained by controlling the spraying times;
the specific preparation process of the step (2) comprises the following steps: adding LiF powder of 10-200-g into HCl solution of 5-20 mol/L at 20-60 ℃ and stirring for 20-60 min to prepare HF etching solution; adding MAX phase powder of 10-200 g into etching liquid, stirring at 20-60 ℃ for reaction for 18-36 h to obtain a reaction product, diluting the obtained reaction product, pouring into a centrifuge tube, centrifuging for 4-8 min at a rotating speed of 2500-4500, separating supernatant, repeatedly centrifuging until the pH is more than or equal to 6 to obtain MXene precipitate, adding deionized water into the precipitate, shaking for 5-10 min, centrifuging for 4-8 min at a rotating speed of 2500-4500, and obtaining the supernatant which is a MXene solution with a certain concentration;
in the step (3), the radiation heating temperature range of the prepared transparent low-infrared emission polymer composite film is 1-10 ℃, and the sunlight heating temperature range is 5-50 ℃; the range of the applied voltage of the electrothermal conversion of the prepared transparent low-emissivity polymer composite film is 0.1-10V, and the temperature range which can be reached by the electrothermal conversion of the prepared transparent low-emissivity polymer composite film is 5-180 ℃.
2. The method for preparing the multifunctional visible light transparent low-infrared emission polymer composite film according to claim 1, which is characterized in that: the transparent polymer film in the step (1) is made of polyethylene terephthalate (PET), polycarbonate (PC), polymethyl methacrylate (PMMA), polydimethylsiloxane (PDMS), polypropylene (PP), polyethylene (PE) or polyvinyl chloride (PVC);
the specific pretreatment process of the step (1) is as follows: ultrasonic cleaning transparent polymer film with alcohol for 5-10 min, and treating with plasma cleaner for 0.5-2 min.
3. The method for preparing the multifunctional visible light transparent low-infrared emission polymer composite film according to claim 1, which is characterized in that: in the step (3), the ITO conductive layer with a certain thickness is 0-500 and nm.
4. The method for preparing the multifunctional visible light transparent low-infrared emission polymer composite film according to claim 1, which is characterized in that: in the step (3), the concentration of the MXene solution with certain concentration is circularly sprayed to be 0.1-20 mg/mL, and the times of circularly spraying are 0-100 times.
5. The method for preparing the multifunctional visible light transparent low-infrared emission polymer composite film according to claim 1, which is characterized in that: in the step (3), the infrared emissivity of the transparent low-emissivity polymer composite film prepared by controlling the thickness of the MXene coating, namely controlling the concentration of the MXene solution and the spraying times of the MXene solution is 10% -90%, and the transmittance is 30% -90%.
6. The method for preparing the multifunctional visible light transparent low-infrared emission polymer composite film according to claim 1, which is characterized in that: the light source for photo-thermal conversion of the prepared transparent low-infrared emission polymer composite film is one or more of near infrared light, far infrared light and sunlight.
7. The method for preparing the multifunctional visible light transparent low-infrared emission polymer composite film according to claim 1 or 6, which is characterized in that: the heating mode of the prepared transparent low-infrared emission polymer composite film comprises one or more of passive radiation heating, photo-thermal and electric heating.
8. The use of a multifunctional visible light transparent low emissivity polymer composite film of claim 1, wherein: including applications in the fields of visible-light thermal camouflage, thin film radiant heating, thin film electrical heating, thin film optical heating, and thermal conversion.
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| CN113060734A (en) * | 2021-04-06 | 2021-07-02 | 郑州大学 | Infrared low-emissivity MXene film and preparation method thereof |
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