CN113060734B - Infrared low-emissivity MXene film and preparation method thereof - Google Patents
Infrared low-emissivity MXene film and preparation method thereof Download PDFInfo
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Abstract
The invention relates to the field of functional materials, in particular to an infrared low-emissivity MXene film for infrared stealth and thermal camouflage and a preparation method thereof. The preparation method of the infrared low-emissivity MXene film comprises the following steps: pouring the MXene solution into a suction filtration bottle with a filter membrane, uniformly loading the MXene on the surface of the filter membrane through vacuum suction filtration, and forming a MXene thin layer on the surface of the filter membrane; and then separating the dried MXene thin layer from the filter membrane to obtain the MXene thin film. The emissivity of the MXene film prepared by the invention in the infrared band of 7-14 um is 0.05-0.5; the preparation method has the advantages of stable reaction, simplicity, easy operation, safe, convenient and environment-friendly process and good uniformity of the obtained product; the raw materials are widely available, can be used in large scale, and are beneficial to popularization.
Description
Technical Field
The invention relates to the field of functional materials, in particular to an infrared low-emissivity MXene film for the fields of infrared stealth and thermal camouflage and a preparation method thereof.
Background
With the rapid development of electronic countermeasure technology, the acquisition and inverse acquisition of information are becoming the focus. Infrared detection is one of the technologies mainly employed therein. The infrared stealth technology is an important reconnaissance and anti-reconnaissance means, and the application of the infrared stealth technology can reduce the possibility that a target is reconnaissance and found by the thermal infrared imager, so that exposure can be effectively prevented. The use and development of low infrared radiation materials has prompted the achievement of infrared stealth.
The infrared detector collects infrared signals of the targets in the wave bands of 3-5 um and 7-14 um, and then the infrared radiation energy difference between the targets and the background is utilized to identify the targets through imaging. According to Stefan-Boltzmann law (Stefan-Boltzmann law), the infrared radiation energy W=εσT of an object 4 (where ε is the infrared emissivity of the object surface, σ is the Boltzmann constant, and T is the thermodynamic temperature of the object surface). Thus, technical approaches to achieving infrared stealth include reducing the infrared emissivity of an object and reducing the surface temperature of the object.
Reducing the infrared emissivity of the surface of an object is one of the most dominant methods of thermal infrared stealth at present. The metal good conductor (such as Al, cu, ag and the like) has higher infrared reflectivity and low infrared emissivity, is suitable for being used as a filler in infrared stealth materials, and mainly comprises Al powder and Cu powder which have excellent performance, are low in cost and are easy to obtain in practical application. In addition, factors such as particle size, morphology and the like of the metal filler play an important role in reducing the infrared emissivity of the infrared stealth coating. However, the high gloss and readily oxidizable nature of the metal filler is detrimental to its durability, and the metal article is dense and difficult to shape and process.
Journal of Solid State Chemistry,2004,177 (10): 3849-3852 disclose the use of polyimide with string-like nano BaTiO 3 The particles are used as raw materials to prepare polyimide/BaTiO 3 Nanocomposite films, when BaTiO 3 When the addition amount is 14.7% (w), the emissivity of the film in the wave band of 8-14 μm can reach 0.574 at the minimum.
Teachings of Yury go tsi, university of us Lei Saier, et al, found that MXene materials, i.e., two-dimensional transition metal carbides/nitrides/carbonitrides, could be prepared by wet-chemical etching of the MAX phase. MXene is a novel two-dimensional crystal material, and the chemical formula of MXene can be represented by M n+1 X n T x And wherein M is a transition metal, X is carbon or nitrogen, and T represents a surface group (= O, -OH, -F). The MXene surface group is adjustable, has excellent conductivity and can be used for energy storage and electromagnetic shielding; while MXene has nearly one hundred percent photo-thermal conversion efficiency.
Currently, research on an MXene material is mainly focused on electromagnetic shielding, but no report on the infrared emission performance of the MXene is available. Therefore, the development of the MXene material with low infrared emissivity has important significance and application value for promoting the development of infrared stealth and thermal camouflage materials.
Disclosure of Invention
(one) solving the technical problems
Aiming at the defects of the prior art, the invention aims to provide an infrared low-emissivity MXene film used in the fields of infrared stealth and thermal camouflage and a preparation method thereof.
(II) technical scheme
In order to achieve the above purpose, the invention is realized by the following technical scheme:
the preparation method of the infrared low-emissivity MXene film comprises the following steps:
pouring the MXene solution into a suction filtration bottle with a filter membrane, uniformly loading the MXene on the surface of the filter membrane through vacuum suction filtration, and forming a MXene thin layer on the surface of the filter membrane; and then separating the dried MXene thin layer from the filter membrane to obtain the MXene thin film.
Preferably, the concentration of the MXene solution is 0.1-25 mg/mL.
Preferably, the thickness of the MXene film is 0.1-100 um, and the emissivity of the MXene film in the infrared band of 7-14 um is 0.05-0.5.
Preferably, the MXene film is annealed in vacuum or air or oxygen or inert gas at 20-500 ℃ to produce an annealed modified MXene film.
Preferably, MXene is Ti 3 C 2 T x 、Ti 2 CT x 、Ti 3 CNT x 、Nb 2 CT x 、V 2 CT x At least one of the solutions is prepared by the following steps:
(1) 1-100 g LiF is dissolved in 20-2000 mL 5-12 mol/L HCl solution to prepare etching solution; at 35-40 ℃, 1-100 g Ti is added 3 AlC 2 Adding the solution into the etching solution for etching for 18-36 h, firstly cleaning with deionized water, centrifuging at 3500-5000 rpm till pH=6-7, and pouring out supernatant to obtain Ti 3 C 2 T x Precipitating; the Ti is mixed with 3 C 2 T x Adding the precipitate into 50-3000 mL deionized water, vibrating, centrifuging at 3500-5000 rpm, and collecting supernatant to obtain Ti 3 C 2 T x A solution;
(2) Uniformly mixing 12-1200 mL of 5-12 mol/L HCL solution, 2-200 mL of 15-30 mol/L HF solution and 6-600 mL of deionized water to prepare etching solution; at room temperature, 1 to 100g of Ti 2 AlC is added into the etching liquid to be etched for 18 to 36 hours, deionized water is firstly used for cleaning, then the solution is centrifuged at 3500 to 5000rpm until the pH value is=6 to 7, and supernatant fluid is poured out to prepare Ti 2 CT x Precipitating; the Ti is mixed with 2 CT x Adding the precipitate into 50-3000 mL deionized water, and vibrating at 3500-5000 rpmCentrifuging, collecting supernatant to obtain Ti 2 CT x A solution;
(3) 1-100 g LiF is dissolved in 20-2000 mL 5-12 mol/L HCl solution to prepare etching solution; at 25-40 ℃, 1-100 g Ti 3 AlCN is added into the etching liquid for etching for 18 to 36 hours, firstly deionized water is used for cleaning, then centrifugation is carried out at 3500 to 5000rpm to pH=6 to 7, and supernatant fluid is poured out to prepare Ti 3 CNT x Precipitating; the Ti is mixed with 3 CNT x Adding the precipitate into 50-3000 mL deionized water, vibrating, centrifuging at 3500-5000 rpm, and collecting supernatant to obtain Ti 3 CNT x A solution;
(4) At 35-40 ℃, 1-100 g Nb 2 Adding 20-2000 mL of 15-30 mol/L hydrofluoric acid etching solution into AlC for etching for 48-72 h, firstly cleaning with deionized water, centrifuging at 3500-5000 rpm till pH=6-7, and pouring out supernatant to obtain Nb 2 CT x Precipitating; by adding Nb to 2 CT x Adding the precipitate into 50-3000 mL deionized water, oscillating, centrifuging at 3500-5000 rpm, collecting supernatant to obtain Nb 2 CT x A solution;
(5) At the temperature of 35-40 ℃, 1-100 g V 2 Adding 20-2000 mL of 15-30 mol/L hydrofluoric acid etching solution into AlC for etching for 48-72 h, firstly cleaning with deionized water, centrifuging at 3500-5000 rpm until pH=6-7, and pouring out supernatant to obtain V 2 CT x Precipitating; the V is set up above 2 CT x Adding the precipitate into 50-3000 mL deionized water, oscillating, centrifuging at 3500-5000 rpm, collecting supernatant to obtain V 2 CT x A solution.
Preferably, the MXene solution is prepared using the following steps: freeze-drying MXene precipitation at-40 ℃ and 10pa to obtain MXene powder; and (3) mixing and stirring the MXene powder, alkyl chain acyl chloride and triethylamine with DMF, washing with absolute ethyl alcohol, centrifuging to pH=6-7, adding deionized water and carrying out ultrasonic treatment to obtain the alkyl chain modified MXene solution.
Preferably, the MXene solution is prepared using the following steps: freeze-drying MXene precipitation at-40 ℃ and 10pa to obtain MXene powder; mixing the MXene powder with an alkali solution or an acid solution, washing with deionized water, centrifuging to pH=6-8, adding deionized water, and performing ultrasonic treatment to obtain the alkali-modified or acid-modified MXene solution.
Preferably, the MXene solution is prepared using the following steps: freeze-drying MXene precipitation at-40 ℃ and 10pa to obtain MXene powder; mixing MXene powder, a silane coupling agent and an ethanol solution, washing with ethanol, centrifuging, and removing unreacted silane coupling agent to obtain a suspension, namely the silane coupling agent modified MXene solution.
An MXene film prepared by the method for preparing the infrared low-emissivity MXene film.
The application of the infrared low-emissivity MXene film is applied to the fields of infrared stealth and thermal camouflage.
(III) beneficial effects
The invention provides an infrared low-emissivity MXene film and a preparation method thereof, and the infrared low-emissivity MXene film has the following beneficial effects:
the emissivity of the MXene film/modified MXene film prepared by the invention in the infrared band range of 7-14 um is 0.05-0.5; the preparation method has the advantages of stable reaction, simplicity, easy operation, safe, convenient and environment-friendly process and good uniformity of the obtained product; the raw materials are widely available, can be used in large scale, and are beneficial to popularization.
Drawings
FIG. 1 is a schematic view of the MXene film prepared in example 1 and its thickness and bending;
FIG. 2 is a graph of the infrared camouflage and thermal camouflage effects of the MXene film prepared in example 1;
FIG. 3 is a graph of the infrared camouflage and thermal camouflage effects of the MXene film prepared in example 2;
FIG. 4 is a graph of the infrared camouflage and thermal camouflage effect of the MXene film of example 3 after annealing at 200℃under vacuum;
FIG. 5 is a graph of the infrared camouflage and thermal camouflage effect of the MXene film after annealing at 500 ℃ in the air atmosphere of example 4;
FIG. 6 is a graph of the infrared camouflage and thermal camouflage effect of the MXene film modified with octadecanoyl chloride of example 5;
FIG. 7 is a graph showing the infrared camouflage and thermal camouflage effects of the MXene film modified with the NaOH solution of example 6;
FIG. 8 is a graph showing the comparison of infrared camouflage and thermal camouflage effects of the MXene film/modified MXene film of examples 1-10 on a 120℃hot plate;
FIG. 9 is an infrared emissivity spectrum of 7 to 14um for the infrared low emissivity film of example 1;
FIG. 10 is a graph of the infrared camouflage and thermal camouflage effects of the MXene film prepared in example 11;
FIG. 11 is a graph of the infrared camouflage and thermal camouflage effects of the MXene film prepared in example 12;
FIG. 12 is a graph of the infrared camouflage and thermal camouflage effects of the MXene film prepared in example 13;
FIG. 13 is a graph of the infrared camouflage and thermal camouflage effects of the MXene film prepared in example 14;
FIG. 14 is a graph of infrared emissivity of 7-14 um for stainless steel films.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments.
Example 1
An infrared low emissivity MXene film and a preparation method thereof, comprising the following steps:
(1) Adding 10g LiF into 200mL 12mol/L HCl solution, magnetically stirring in water bath for 30min until the LiF is completely dissolved, and preparing etching solution; at 35 ℃, 10g of Ti 3 AlC 2 Adding into etching solution, stirring for 24 hr, cleaning with deionized water, centrifuging at 3500rpm for 5min until pH reaches 6, and removing supernatant to obtain Ti 3 C 2 T x Precipitating;
(2) The Ti is mixed with 3 C 2 T x Adding 200mL deionized water into the precipitate, shaking for 7min, centrifuging at 3500rpm for 5min, and collecting supernatant to obtain Ti with concentration of 3mg/mL 3 C 2 T x A solution;
(3) 30mL of Ti 3 C 2 T x Pouring the solution into a suction filtration bottle with a cellulose acetate filter membrane, and vacuum-filtering Ti 3 C 2 T x Uniformly loaded on the surface of the cellulose acetate filter membrane to form Ti on the surface of the filter membrane 3 C 2 T x Thin layer, then, dry the Ti 3 C 2 T x Separating the thin layer from the filter membrane to obtain Ti 3 C 2 T x A film.
Example 2
An infrared low emissivity MXene film and a preparation method thereof, comprising the following steps:
reference example 1, ti was prepared 3 C 2 T x A solution; 1mL of Ti 3 C 2 T x Pouring the solution into a suction filtration bottle with a filter membrane, and filtering Ti by vacuum 3 C 2 T x Uniformly load on the surface of the filter membrane and form Ti on the surface of the filter membrane 3 C 2 T x Thin layer, then, dry the Ti 3 C 2 T x Separating the thin layer from the filter membrane to obtain Ti 3 C 2 T x A film.
Example 3
An infrared low emissivity MXene film and a preparation method thereof, comprising the following steps:
reference example 1, ti was prepared 3 C 2 T x A solution; 6mL of Ti 3 C 2 T x Pouring the solution into a suction filtration bottle with a filter membrane, and filtering Ti by vacuum 3 C 2 T x Uniformly load on the surface of the filter membrane and form Ti on the surface of the filter membrane 3 C 2 T x Thin layer, then, dry the Ti 3 C 2 T x Separating the thin layer from the filter membrane to obtain Ti 3 C 2 T x A film; ti is mixed with 3 C 2 T x Annealing the film for 2 hours under the vacuum condition of 200 ℃ to prepare the annealed modified Ti 3 C 2 T x A film.
Example 4
An infrared low emissivity MXene film and a preparation method thereof, comprising the following steps:
reference example 1, ti was prepared 3 C 2 T x A solution; 18mL of Ti 3 C 2 T x Pouring the solution into a suction filtration bottle with a filter membrane, and filtering Ti by vacuum 3 C 2 T x Uniformly load on the surface of the filter membrane and form Ti on the surface of the filter membrane 3 C 2 T x Thin layer, then, dry the Ti 3 C 2 T x Separating the thin layer from the filter membrane to obtain Ti 3 C 2 T x A film; the Ti is treated with 3 C 2 T x Annealing the film in 500 ℃ air atmosphere for 2 hours to obtain annealed modified Ti 3 C 2 T x A film.
Example 5
An infrared low emissivity MXene film and a preparation method thereof, comprising the following steps:
reference example 1, ti was prepared 3 C 2 T x A solution; 20mL of Ti 3 C 2 T x Pouring the solution into a suction filtration bottle with a filter membrane, and filtering Ti by vacuum 3 C 2 T x Uniformly load on the surface of the filter membrane and form Ti on the surface of the filter membrane 3 C 2 T x Thin layer, then, dry the Ti 3 C 2 T x Separating the thin layer from the filter membrane to obtain Ti 3 C 2 T x A film; the Ti is treated with 3 C 2 T x Annealing the film for 1h in nitrogen atmosphere at 100 ℃ to prepare the annealed modified Ti 3 C 2 T x A film.
Example 6
The preparation method of the infrared low-emissivity MXene film comprises the following steps:
reference example 1, ti was prepared 3 C 2 T x A solution; 22mL of Ti 3 C 2 T x Pouring the solution into a suction filtration bottle with a filter membrane, and filtering Ti by vacuum 3 C 2 T x Uniformly load on the surface of the filter membrane and form Ti on the surface of the filter membrane 3 C 2 T x Thin layer, then, dry the Ti 3 C 2 T x Separating the thin layer from the filter membrane to obtain Ti 3 C 2 T x A film; the Ti is treated with 3 C 2 T x Annealing the film in 300 ℃ oxygen atmosphere for 4 hours to obtain annealed modified Ti 3 C 2 T x A film.
Example 7
An infrared low emissivity MXene film and a preparation method thereof, comprising the following steps:
preparation of Ti with reference to example 1 3 C 2 T x Precipitating; ti is mixed with 3 C 2 T x Precipitating at-40deg.C<Freeze-drying under 10pa to obtain dry Ti 3 C 2 T x A powder; at 60 ℃, 1g of Ti 3 C 2 T x The powder was dissolved in 250mL of DMF, added with 0.8g of octadecanoyl chloride and 0.5g of triethylamine and magnetically stirred for 18 h; washing the reaction solution with absolute ethanol, centrifuging at 3500rpm for 5min until pH reaches 6, adding deionized water, and ultrasonic treating for 10min to obtain octadecyl modified Ti with concentration of 3.8mg/mL 3 C 2 T x A solution; 40mL of the above octadecane modified Ti 3 C 2 T x Pouring the solution into a suction filtration bottle with a filter membrane, and vacuum-filtering to obtain octadecane modified Ti 3 C 2 T x Uniformly loading the mixture on a filter membrane to obtain the octadecane modified Ti 3 C 2 T x A film.
Example 8
An infrared low emissivity MXene film and a preparation method thereof, comprising the following steps:
reference example 7, preparation of Ti 3 C 2 T x A powder; at 35 ℃, 0.5g of Ti 3 C 2 T x The powder was dissolved in 500mL of 0.1mol/L NaOH solution and stirred for 6h; washing the reaction solution with deionized water, centrifuging at 3500rpm for 5min until pH reaches 8, adding deionized water, and performing ultrasonic treatment for 5min to obtain Ti modified by NaOH with concentration of 3mg/mL 3 C 2 T x A solution; 50mL NaOH modified Ti 3 C 2 T x Pouring the solution into a suction filtration bottle with a filter membrane, and vacuum-filtering to modify the NaOH-modified Ti 3 C 2 T x Uniformly loading the mixture on the surface of the filter membrane to obtain the membrane with Na on the surface + Ti of (2) 3 C 2 T x A film.
Example 9
An infrared low emissivity MXene film and a preparation method thereof, comprising the following steps:
reference example 7, preparation of Ti 3 C 2 T x A powder; at 35 ℃, 1g of Ti 3 C 2 T x The powder was dissolved in 100mL of 1mol/L H 2 SO 4 Stirring the solution for 6 hours; washing the reaction solution with deionized water, centrifuging at 3500rpm for 5min until pH reaches 6, adding deionized water, and performing ultrasonic treatment for 5min to obtain sulfuric acid modified Ti with concentration of 4.7mg/mL 3 C 2 T x A solution; 30mL sulfuric acid modified Ti 3 C 2 T x Pouring the solution into a suction filtration bottle with a filter membrane, and filtering sulfuric acid modified Ti by vacuum 3 C 2 T x Uniformly loading the mixture on the surface of the filter membrane to obtain the product with SO-containing surface 4 2- Ti of (2) 3 C 2 T x A film.
Example 10
An infrared low emissivity MXene film and a preparation method thereof, comprising the following steps:
reference example 7, preparation of Ti 3 C 2 T x A powder; 1g of Ti 3 C 2 T x The powder, 2g of AEAPTMS (aminopropyl trimethoxysilane) was added to the ethanol solution and stirred for 2h; washing the reaction solution with ethanol, centrifuging at 3500rpm, removing unreacted AEAPTMS, and obtaining suspension as Ti modified by silane coupling agent with concentration of 4.3mg/mL 3 C 2 T x A solution; 60mL of silane coupling agent modified Ti 3 C 2 T x Pouring the suspension into a suction filtration bottle with a polypropylene film, and vacuum-filtering to obtain AEAPTMS modified Ti 3 C 2 T x A film.
Example 11
An infrared low emissivity MXene film and a preparation method thereof, comprising the following steps:
(1) Uniformly mixing 12mL of 12mol/L HCL solution, 2mL of 28mol/L HF solution and 6mL of deionized water to prepare etching solution; 1g of Ti at room temperature 2 AlC is added into the etching liquid to be etched for 36 hours, deionized water is firstly used for cleaning, then the centrifugal is carried out at the rotation speed of 4000rpm until the pH value is=6, and the supernatant is poured out to prepare Ti 2 CT x Precipitating;
(2) The Ti is mixed with 2 CT x Adding 200mL deionized water into the precipitate, shaking for 7min, centrifuging at 3500rpm for 5min, and collecting supernatant to obtain Ti with concentration of 2.8mg/mL 3 C 2 T x A solution;
(3) 1mL of Ti 2 CT x Pouring the solution into a suction filtration bottle with a cellulose acetate filter membrane, and vacuum-filtering Ti 3 C 2 T x Uniformly loaded on the surface of the cellulose acetate filter membrane to form Ti on the surface of the filter membrane 2 CT x Thin layer, then, dry the Ti 2 CT x Separating the thin layer from the filter membrane to obtain Ti 2 CT x A film.
Example 12
An infrared low emissivity MXene film and a preparation method thereof, comprising the following steps:
(1) 5g LiF is dissolved in 100mL 12mol/L HCl solution to prepare etching solution; at 30 ℃, 5g of Ti 3 Adding AlCN into the etching solution, etching for 18h, cleaning with deionized water, centrifuging at 3500rpm till pH=6, and removing supernatant to obtain Ti 3 CNT x Precipitating;
(2) The Ti is mixed with 3 CNT x Adding the precipitate into 150mL deionized water, oscillating, centrifuging at 3500-5000 rpm, collecting supernatant to obtain Ti with a concentration of 3.5mg/mL 3 CNT x A solution;
(3) 2mL of Ti 3 CNT x Pouring the solution into a suction filtration bottle with a cellulose acetate filter membrane, and vacuum-filtering Ti 3 CNT x Uniformly loaded on the surface of the cellulose acetate filter membrane to form Ti on the surface of the filter membrane 3 CNT x Thin layer, then, dry the Ti 3 CNT x Separating the thin layer from the filter membrane to obtain Ti 3 CNT x A film.
Example 13
An infrared low emissivity MXene film and a preparation method thereof, comprising the following steps:
(1) At 35 ℃, 1g of Nb 2 Adding AlC into 20mL 28mol/L hydrofluoric acid etching solution, etching for 48h, cleaning with deionized water, centrifuging at 3500rpm till pH=6, and pouring out supernatant to obtain Nb 2 CT x Precipitating;
(2) By adding Nb to 2 Adding CTx precipitate into 100mL deionized water, shaking, centrifuging at 3500rpm, and collecting supernatant to obtain Nb with concentration of 4mg/mL 2 CT x A solution.
(3) 4mL Nb 2 Pouring CTx solution into a suction filtration bottle with a cellulose acetate filter membrane, and vacuum-filtering Nb 2 CTx is uniformly loaded on the surface of cellulose acetate filter membrane to form Nb on the surface of the filter membrane 2 CT x Thin layer, then, dry Nb 2 CT x Separating the thin layer from the filter membrane to obtain Nb 2 CT x A film.
Example 14
An infrared low emissivity MXene film and a preparation method thereof, comprising the following steps:
(1) At 40 ℃, 1g V 2 AlC is added into 20mL 25mol/L hydrofluoric acid etching solution to be etched for 60 hours, deionized water is firstly used for cleaning, then centrifugation is carried out at 3500rpm till pH=6, and supernatant fluid is poured out to prepare V 2 CT x Precipitating;
(2) The V is set up above 2 CT x Adding the precipitate into 100mL deionized water, shaking, centrifuging at 3500rpm, and collecting supernatant to obtain a concentration of 3.8mg/mL V 2 CT x A solution;
(3) Will be 6mLV 2 CT x Pouring the solution into a suction filtration bottle with a cellulose acetate filter membrane, and vacuum-filtering to obtain V 2 CT x Uniformly loaded on the surface of the cellulose acetate filter membrane and V is formed on the surface of the filter membrane 2 CT x Thin layer, then, dry V 2 CT x Separating the thin layer from the filter membrane to obtain V 2 CT x A film.
Testing and analysis
(1) Bending effect of MXene film
As shown in FIG. 1, the thickness of the MXene film prepared in the embodiment 1 of the invention is 29um, and the MXene film can be folded in half without damage, which shows that the MXene film has good bending effect.
(2) Thermal camouflage effect test and analysis
And (3) covering the MXene film prepared in the embodiment on the surface of the heat table by adopting an FLIR E75 type infrared thermal imager for photographing, and observing the infrared stealth and thermal camouflage effects of the MXene film by comparing the temperature difference between the MXene film and the heat table in an infrared photo. As can be seen from FIGS. 3 to 8, the surface functional groups of the annealed MXene film are reduced in the inert gas and vacuum, so that the thermal camouflage effect is improved, compared with the pure MXene film; the heat camouflage effect of the MXene film annealed in the air and oxygen atmosphere is reduced to a different degree compared with that of the pure MXene film which is subjected to surface modification by alkyl chain acyl chloride, sulfuric acid, sodium hydroxide and a silane coupling agent.
The MXene film with different modification methods can be selected according to different required heat camouflage degrees according to the actual temperature of the target object so as to further regulate and control the temperature of the object in the infrared camera.
(3) Infrared emissivity test and analysis
The resulting MXene film/modified MXene film of the above example was tested for infrared emissivity and the results are shown in table 1.
TABLE 1 Infrared emittance of different MXene films
As can be seen from the combination of FIGS. 2 to 14 and Table 1, the MXene film obtained in example 1 of the present invention was subjected to different surface modifications than the modified MXene films obtained in examples 2 to 9The emissivity is smaller than polyimide/BaTiO in the background technology 3 The infrared emissivity of the nano composite film is close to or smaller than that of the stainless steel film.
In conclusion, the pure MXene film and the MXene film subjected to surface modification by different methods are infrared low-emissivity films, and have good heat camouflage effect.
The foregoing is only a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art, who is within the scope of the present invention, should make equivalent substitutions or modifications according to the technical scheme of the present invention and the inventive concept thereof, and should be covered by the scope of the present invention.
Claims (5)
1. An application of an MXene film with the thickness of 0.1-100 um and the emissivity of 0.05-0.5 in the infrared band of 7-14 um in the infrared stealth and thermal camouflage fields;
the preparation method of the MXene film comprises the following steps: pouring the MXene solution into a suction filtration bottle with a filter membrane, uniformly loading the MXene on the surface of the filter membrane through vacuum suction filtration, and forming a MXene thin layer on the surface of the filter membrane; then separating the dried MXene thin layer from the filter membrane to obtain an MXene thin film;
the concentration of the MXene solution is 0.1-25 mg/mL;
the MXene is Ti 3 C 2 T x 、Ti 2 CT x 、Ti 3 CNT x 、Nb 2 CT x 、V 2 CT x At least one of the solutions is prepared by the following steps:
1-100 g LiF is dissolved in 20-2000 mL 5-12 mol/L HCl solution to prepare etching solution; at 35-40 ℃, 1-100 g Ti is added 3 AlC 2 Adding the solution into the etching solution for etching for 18-36 h, firstly cleaning with deionized water, centrifuging at 3500-5000 rpm till pH=6-7, and pouring out supernatant to obtain Ti 3 C2T x Precipitating; the Ti is mixed with 3 C2T x Adding the precipitate into 50-3000 mL deionized water, vibrating, centrifuging at 3500-5000 rpm, collecting supernatantObtaining Ti 3 C2T x A solution;
uniformly mixing 12-1200 mL of 5-12 mol/L HCL solution, 2-200 mL of 15-30 mol/L HF solution and 6-600 mL of deionized water to prepare etching solution; at room temperature, 1 to 100g of Ti 2 AlC is added into the etching liquid to be etched for 18 to 36 hours, deionized water is firstly used for cleaning, then the solution is centrifuged at 3500 to 5000rpm until the pH value is=6 to 7, and supernatant fluid is poured out to prepare Ti 2 CT x Precipitating; the Ti is mixed with 2 CT x Adding the precipitate into 50-3000 mL deionized water, vibrating, centrifuging at 3500-5000 rpm, and collecting supernatant to obtain Ti 2 CT x A solution;
1-100 g LiF is dissolved in 20-2000 mL 5-12 mol/L HCl solution to prepare etching solution; at 25-40 ℃, 1-100 g Ti 3 AlCN is added into the etching liquid for etching for 18 to 36 hours, firstly deionized water is used for cleaning, then centrifugation is carried out at 3500 to 5000rpm to pH=6 to 7, and supernatant fluid is poured out to prepare Ti 3 CNT x Precipitating; the Ti is mixed with 3 CNT x Adding the precipitate into 50-3000 mL deionized water, vibrating, centrifuging at 3500-5000 rpm, and collecting supernatant to obtain Ti 3 CNT x A solution;
at 35-40 ℃, 1-100 g Nb 2 Adding 20-2000 mL of 15-30 mol/L hydrofluoric acid etching solution into AlC for etching for 48-72 h, firstly cleaning with deionized water, centrifuging at 3500-5000 rpm till pH=6-7, and pouring out supernatant to obtain Nb 2 CT x Precipitating; by adding Nb to 2 CT x Adding the precipitate into 50-3000 mL deionized water, oscillating, centrifuging at 3500-5000 rpm, collecting supernatant to obtain Nb 2 CT x A solution;
at the temperature of 35-40 ℃, 1-100 g V 2 Adding 20-2000 mL of 15-30 mol/L hydrofluoric acid etching solution into AlC for etching for 48-72 h, firstly cleaning with deionized water, centrifuging at 3500-5000 rpm until pH=6-7, and pouring out supernatant to obtain V 2 CT x Precipitating; the V is set up above 2 CT x Adding the precipitate into 50-3000 mL deionized water, oscillating, centrifuging at 3500-5000 rpm, collecting supernatant to obtain V 2 CT x A solution.
2. The use according to claim 1, wherein the method for producing an MXene film further comprises the steps of: annealing the MXene film in vacuum or inert gas at 20-200 ℃ to improve infrared stealth and thermal camouflage effects and prepare an annealed modified MXene film; or annealing the MXene film in air or oxygen at 300-500 ℃ to reduce infrared stealth and thermal camouflage effects and prepare the annealed modified MXene film.
3. The use according to claim 1, wherein the step of preparing the MXene solution further comprises:
the MXene is precipitated and freeze-dried at the temperature of minus 40 ℃ and less than 10pa to prepare MXene powder; and (3) mixing and stirring the MXene powder, the alkyl chain acyl chloride and the triethylamine with DMF, washing with absolute ethyl alcohol, centrifuging to pH=6-7, adding deionized water and carrying out ultrasonic treatment to obtain an alkyl chain modified MXene solution, and reducing the infrared stealth and thermal camouflage effects of the MXene film through alkyl chain modification.
4. The use according to claim 1, wherein the step of preparing the MXene solution further comprises:
the MXene is precipitated and freeze-dried at the temperature of minus 40 ℃ and less than 10pa to prepare MXene powder; and (3) mixing the MXene powder with an alkali solution or an acid solution, washing with deionized water, centrifuging to pH=6-8, adding deionized water for ultrasonic treatment to obtain an alkali modified or acid modified MXene solution, and reducing the infrared stealth and thermal camouflage effects of the MXene film through alkali modification or acid modification.
5. The use according to claim 1, wherein the step of preparing the MXene solution further comprises:
the MXene is precipitated and freeze-dried at the temperature of minus 40 ℃ and less than 10pa to prepare MXene powder; after mixing MXene powder, a silane coupling agent and an ethanol solution, washing with ethanol, centrifuging, and removing unreacted silane coupling agent to obtain a suspension, namely the silane coupling agent modified MXene solution, wherein the silane coupling agent is used for modifying to reduce the infrared stealth and thermal camouflage effects of the MXene film.
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