CN112877685A - Micro-laminated film with high infrared reflectivity and preparation method thereof - Google Patents

Micro-laminated film with high infrared reflectivity and preparation method thereof Download PDF

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CN112877685A
CN112877685A CN202110050023.3A CN202110050023A CN112877685A CN 112877685 A CN112877685 A CN 112877685A CN 202110050023 A CN202110050023 A CN 202110050023A CN 112877685 A CN112877685 A CN 112877685A
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film
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laminated film
slurry
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CN112877685B (en
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王冉
邓建新
张志慧
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Shandong University
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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
    • C23C24/00—Coating starting from inorganic powder
    • C23C24/08—Coating starting from inorganic powder by application of heat or pressure and heat
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F7/00—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression
    • B22F7/02—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite layers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • B22F2009/043—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling

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  • Chemical Kinetics & Catalysis (AREA)
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Abstract

The present disclosure provides a micro-laminated film with high infrared reflectivity and a preparation method thereof, the steps include: sequentially depositing an intermetallic compound-carbide composite film and a metal oxide film on the surface of the pretreated substrate by adopting an electric jet method to form a micro-laminated film with a multilayer structure; the multilayer micro laminated film is deposited by adopting an electric jet method, the equipment is simple, the controllability is strong, the deposition rate is high, the density of the prepared micro laminated film is high, the number of pores and microcracks on the surface of the film is small, and the film has higher infrared reflectivity; the problems that the spin-coating method has high requirements on experimental environment, the prepared film is uneven, laser cladding equipment of the laser cladding method is expensive, and the obtained coating has more internal pores and uneven coating tissues, so that the coating has lower infrared reflectivity are solved.

Description

Micro-laminated film with high infrared reflectivity and preparation method thereof
Technical Field
The disclosure relates to a micro-laminated film with high infrared reflectivity based on electro-jet deposition and a preparation method thereof.
Background
The statements in this section merely provide background information related to the present disclosure and may not necessarily constitute prior art.
For a long time, some natural composite materials in nature such as bamboo, wood, bones, shells and the like have excellent mechanical properties; especially, the shell pearl layer achieves the best matching of strength and toughness in the long-term evolution process, and people gradually perform structural bionics during the preparation of new materials according to the structural principle. Especially, since Clegg et al creatively prepared a composite material of an alternate laminated structure of SiC flakes and graphite flakes by imitating the structure of a biomaterial in 1990, a method of structural toughening by lamination has been widely used for preparing a high-performance composite material. The intermetallic compound and the ceramic material have excellent high strength and high temperature properties, and can be applied to various fields. Their own physical properties, such as low temperature brittleness and susceptibility to environmental degradation, limit their use. Thus, the lack of inherent properties of these materials should be compensated for by lamination with other materials.
Solar energy is used as an inexhaustible clean renewable energy source, and has a wide development prospect in replacing the traditional fossil energy source to relieve environmental pollution and energy crisis. In order to realize higher photothermal conversion efficiency, the solar thin film is used as a core component in a solar heat collector and has higher infrared reflectivity in a medium-long wave band (2.5-25 μm). Metal-ceramic type solar thin films have been a hot research focus in recent years due to their excellent optical properties. The metal-ceramic based solar thin films are usually composed of transition metals and transition metal oxides, carbides or nitrides, such as Cr-Cr2O3Co-WC, TiC-Ni/Mo, Ti-AlN, etc. However, Cr3C2The wear-resistant and corrosion-resistant performance of the alloy is excellent, the high-temperature resistance (stability at 1100 ℃) of the alloy is better than that of WC (stability at 500 ℃), and the cost is lower; ni3The particular crystal structure of the Al intermetallic compound also gives it the desirable property characteristics of excellent high temperature materials. Due to Cr3C2And Ni3Better physical and chemical compatibility of Al, and the existing Ni3Al-Cr3C2Some work has been done in the research of composite materials. In addition, dense Al2O3The anti-reflection film can play a good hole sealing role and improve the surface defects, so that Ni can be added3Al-Cr3C2Composite film and Al2O3The film forms a micro laminated film to improve the infrared reflectivity of the film, so that the optical performance and the service performance of the micro laminated film are improved.
At present, Al is prepared at home and abroad2O3The main methods of the thin film include spin coating, sol-gel method, ion plating, and the like. Relating to the preparation of Ni3Al-Cr3C2The main methods of the composite material include laser cladding, surface overlaying and the like.
(1) Spin coating method: the glue is quickly and uniformly spread by means of centrifugal acceleration, then the redundant glue is thrown away from the substrate, and a layer of uniform film is formed on the whole substrate. CN 201710705087.6 discloses high-performance Al2O3/WO3A method for preparing a nano composite electrochromic film, in particular to Al with a mosaic structure2O3/WO3A nano composite electrochromic film and a preparation method thereof. The specific steps are 1) mixing Al2O3The nano-particle powder is dissolved in water by ultrasonic dispersion to form Al2O3An aqueous nanoparticle solution; 2) to Al2O3Adding ammonium metatungstate into the nanoparticle aqueous solution, and performing ultrasonic treatment to form a precursor composite solution; 3) adding ethanol and polyethylene glycol into the precursor composite solution and carrying out ultrasonic treatment to adjust the viscosity and surface tension of the solution; 4) preparing a wet film on a conductive substrate by adopting a spin coating method, and 5) carrying out heat treatment on the wet film in air to obtain Al2O3/WO3A nano composite electrochromic film. However, this method has high requirements for experimental environment and produces a thin film which is not uniform.
(2) A laser cladding method: the method is characterized in that a selected coating material is placed on the surface of a coated substrate in different filling modes, a thin layer of the selected coating material and the surface of the substrate are simultaneously melted through laser irradiation, and the selected coating material and the thin layer of the substrate are rapidly solidified to form a surface coating which has extremely low dilution and is metallurgically bonded with the substrate material. CN201410822105.5 discloses a method for preparing Ni on the surface of a steel matrix by adopting a laser cladding technology3Al-Cr3C2A method for composite coating. The method of the present disclosure comprises the steps of: firstly, the surface of the steel material is pretreated to remove oil stains and impurities attached to the surface of the steel material. Then adding Cr3C2Addition of powder to Ni3Al powder is added and mixed evenly to obtain Ni3Al and Cr3C2Wherein Cr is contained in the mixture3C2The content of (A) is 10 wt% -50 wt%. Finally, cladding the mixture on the surface of the steel material by using a laser cladding technology so that the mixture forms Ni on the surface of the steel material3Al-Cr3C2And (4) composite coating. The coating prepared by laser cladding has excellent wear resistance and high temperature resistance, but laser cladding equipment is expensive, and the obtained coating has more internal pores and uneven coating tissues, so that the coating has lower infrared reflectivity.
Disclosure of Invention
In order to solve the above problems, the present disclosure proposes to provide an electrodeposition-based Ni having high infrared reflectivity3Al-Cr3C2-Al2O3A micro-laminated film and a method for preparing the same. Firstly, Ni is mixed by a high-energy ball mill3Al powder and Cr3C2Ni of powder composition3Al-Cr3C2The composite powder, a certain proportion of dispersant, binder and organic solvent are mixed into Ni3Al-Cr3C2And (4) compounding the slurry. Then mixing Al by a high-energy ball mill according to the same proportion2O3And (3) slurry. Finally, sequentially depositing Ni on the surface of the pretreated metal matrix by adopting an electric jet method3Al-Cr3C2Composite film and Al2O3Thin film, finally forming Ni with multi-layer structure3Al-Cr3C2-Al2O3A microlaminate film. The invention adopts the electric jet method to deposit the multilayer micro-laminated film, and has simple equipment, strong controllability and high deposition rate. Meanwhile, the prepared micro-laminated film has high density, few pores and microcracks on the surface of the film and high infrared reflectivity; the disclosed composite film is easily adaptable to a variety of different shapesThe film is formed on the substrate, the material consumption is less, the cost is low, and the method is suitable for industrial production.
In a first aspect, the present disclosure provides a method for preparing a microlaminate film with high infrared reflectivity, comprising the steps of: and sequentially depositing an intermetallic compound-carbide composite film and a metal oxide film on the surface of the pretreated substrate by adopting an electric jet method to form a micro-laminated film with a multilayer structure.
In a second aspect, the present disclosure provides a microlaminated film with high infrared reflectivity, prepared by the method for preparing a microlaminated film with high infrared reflectivity according to the first aspect.
Compared with the prior art, this disclosure possesses following beneficial effect:
1. according to the method, the multilayer micro-laminated film is deposited by adopting an electric jet method, the equipment is simple, the controllability is strong, the deposition rate is high, meanwhile, the prepared micro-laminated film has high density, few pores and few microcracks on the surface of the film are formed, and the film has higher infrared reflectivity; the problems that the spin-coating method has high requirements on experimental environment, the prepared film is uneven, laser cladding equipment of the laser cladding method is expensive, and the obtained coating has more internal pores and uneven coating tissues, so that the coating has lower infrared reflectivity are solved.
2. The disclosure relates to the production of Ni by high-energy ball milling3Al powder and Cr3C2Ni of powder composition3Al-Cr3C2The composite powder, a certain proportion of dispersant, binder and organic solvent are mixed into Ni3Al-Cr3C2And (4) compounding the slurry. Then mixing Al by a high-energy ball mill according to the same proportion2O3And (3) slurry. Finally, sequentially depositing Ni on the surface of the pretreated metal matrix by adopting an electric jet method3Al-Cr3C2Composite film and Al2O3Thin film, finally forming Ni with multi-layer structure3Al-Cr3C2-Al2O3The micro-laminated film and the composite film are easy to form films on substrates with different shapes, have less materials and low cost and are suitable for industrial production.
Advantages of additional aspects of the disclosure will be set forth in part in the description which follows, and in part will be obvious from the description, or may be learned by practice of the disclosure.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this application, illustrate embodiments of the application and, together with the description, serve to explain the application and are not intended to limit the application.
FIG. 1 is a flow chart of a method of making a microlaminate film with high infrared reflectance of example 1;
FIG. 2 shows Ni prepared in example 13Al-Cr3C2/Al2O3SEM surface topography of microlayer films.
FIG. 3 shows Ni prepared in example 13Al-Cr3C2/Al2O3SEM cross-sectional topography of microlayer films.
FIG. 4 shows Ni prepared in example 13Al-Cr3C2/Al2O3An infrared reflectance spectrum of the microlaminate film.
The specific implementation mode is as follows:
the present disclosure is further described with reference to the following drawings and examples.
It should be noted that the following detailed description is exemplary and is intended to provide further explanation of the disclosure. 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.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of example embodiments according to the present application. As used herein, the singular forms "a", "an" and "the" are intended to include the plural forms as well, and it should be understood that when the terms "comprises" and/or "comprising" are used in this specification, they specify the presence of stated features, steps, operations, devices, components, and/or combinations thereof, unless the context clearly indicates otherwise.
Example one
As shown in fig. 1, a method for preparing a micro-laminated film with high infrared reflectivity comprises the following steps: and sequentially depositing an intermetallic compound-carbide composite film and a metal oxide film on the surface of the pretreated substrate by adopting an electric jet method to form a micro-laminated film with a multilayer structure.
Further, the intermetallic-carbide includes, but is not limited to, Co-WC, TiC-Ni/Mo or Ni3Al-Cr3C2In a preferred embodiment, the intermetallic compound-carbide is Ni3Al-Cr3C2(ii) a The metal oxide includes, but is not limited to, iron sesquioxide or aluminum sesquioxide, and as a preferred embodiment the metal oxide is Al2O3；
Further, the method specifically comprises the following steps:
preparation of Ni3Al-Cr3C2Slurry and Al2O3Sizing agent;
pretreating the surface of the substrate, wherein the pretreatment step comprises polishing and cleaning; specifically, after grinding and polishing the metal matrix, cleaning the metal matrix in an alcohol solution for 15min to finish the pretreatment of the surface of the matrix;
sequentially depositing an intermetallic compound-carbide composite film and a metal oxide film to form a micro-laminated film with a multilayer structure; specifically, an electric jet method is adopted to move and spray Ni on the surface of a pretreated substrate along the X direction through a metal spray needle3Al-Cr3C2Slurry to deposit Ni3Al-Cr3C2Layer, then moving in Y direction and spraying Al2O3Slurry to deposit Al2O3Layers, in turn alternating to realize Ni3Al-Cr3C2Composite film and Al2O3Layer-by-layer deposition of thin film to prepare Ni3Al-Cr3C2-Al2O3A microlaminate film;
wherein, after one layer of intermetallic compound-carbide composite film or metal oxide film deposition is finished, drying and pyrolyzing treatment are carried out; specifically, in order to remove the organic solvent in the deposited micro-laminated film and release stress, after one layer of film deposition is finished, the film is sequentially placed on preheating platforms at 200 ℃ and 300 ℃ for 120s of drying pyrolysis treatment;
and (3) carrying out vacuum high-temperature sintering on the micro-laminated film deposited by the electric jet. Further, electro-jet deposited Ni3Al-Cr3C2-Al2O3The micro-laminated film is placed in a vacuum sintering furnace for high-temperature sintering, and the vacuum degree is 10-3Pa-1Pa, temperature of 1100-;
further, the preparation of Ni3Al-Cr3C2The slurry step comprises adding Ni3Al powder and Cr3C2Mixing the powder to form mixed powder, and then adding a dispersing agent, a binder and an organic solvent; obtaining Ni after ball milling for a set time by adopting a high-energy ball mill3Al-Cr3C2Compounding the slurry; the setting time is 20 to 40 hours, specifically 20 hours, 30 hours or 40 hours.
Further, said Ni3The powder particle size of Al is 1-10 μm, Cr3C2The powder particle size of (A) is 0.1 μm-1 μm; in the mixed powder, Cr3C2The powder accounts for 30 wt% of the total volume fraction of the composite powder; the mass ratio of the dispersing agent is mixed powder: castor oil 10: 1; the mass ratio of the binder is mixed powder: ethyl cellulose 5: 1; the mass ratio of the organic solvent is mixed powder: anhydrous ethanol ═ 1: 5.
Further, the preparation of Al2O3The slurry is prepared by mixing Al2O3Adding a dispersing agent, a binder and an organic solvent into the powder; al is obtained by adopting a high-energy ball mill to ball-mill for a set time2O3Sizing agent; the setting time is 20 to 40 hours, specifically 20 hours, 30 hours or 40 hours.
Further, Al2O3The powder particle size of (A) is 0.1 μm-1 μm; the mass ratio of the dispersing agent is mixed powder: castor oil 10: 1; the mass ratio of the binder is mixed powder: ethyl cellulose 5: 1; organic compoundsThe mass ratio of the solvent is mixed powder: anhydrous ethanol ═ 1: 5.
Further, the parameters of the electro-jet deposition are as follows: the height of the metal spray needle from the surface of the cutter base body is 5-15mm, and the height is 15mm as one embodiment; the movement speed of the metal spray needle is 20-50mm/s, the movement speed is 30mm/s as one embodiment, the direct current voltage is 5kV, and Ni is adopted3Al/Cr3C2Flow rate of composite slurry and Al2O3The flow rates of the slurries were the same, and as one embodiment the flow rates were 20. mu.l/min.
Further, the dispersing agent is castor oil, the binder is ethyl cellulose, and the organic solvent is absolute ethyl alcohol. The metal material substrate is 316L stainless steel.
Example two
The disclosure also provides a method for preparing a microlaminated film with high infrared reflectivity, compared to example 1, Ni3Al-Cr3C2The step of formulating the slurry comprises the step of incorporating Ni3Al powder and Cr3C2Mixing of the powders into Ni3Al-Cr3C2Compounding powder, and then adding a dispersant, a binder and an organic solvent; ball milling for 30 hours by adopting a high-energy ball mill to obtain Ni3Al-Cr3C2Compounding the slurry; wherein Ni3The powder particle size of Al is 1-10 μm, Cr3C2The powder particle size of (A) is 0.1 μm-1 μm; in the mixed powder, Cr3C2Powder of Ni3Al-Cr3C215 wt% of the total volume fraction of the composite powder; the mass ratio of the dispersing agent is mixed powder: castor oil 10: 1; the mass ratio of the binder is mixed powder: ethyl cellulose 5: 1; the mass ratio of the organic solvent is mixed powder: anhydrous ethanol is 1: 5;
Al2O3the preparation of the slurry comprises the steps of preparing Al2O3Adding a dispersing agent, a binder and an organic solvent into the powder; ball milling for 30 hours by adopting a high-energy ball mill to obtain Al2O3Sizing agent; wherein, Al2O3The powder particle size of (A) is 0.1 μm-1 μm; the mass ratio of the dispersant is Al2O3Powder lot: castor oil 10: 1; the mass ratio of the binder is Al2O3Powder lot: ethyl cellulose 5: 1; the mass ratio of the organic solvent is Al2O3Powder lot: anhydrous ethanol is 1: 5;
grinding and polishing the metal substrate, and then cleaning the metal substrate in an alcohol solution for 15min to finish the pretreatment of the surface of the substrate;
sequentially depositing Ni on the surface of the pretreated substrate by adopting an electric jet method3Al-Cr3C2Composite film and Al2O3Film, metal needle first moved in X direction to deposit Ni3Al-Cr3C2Layer, then moving in Y direction to deposit Al2O3Layers, in turn alternating to realize Ni3Al-Cr3C2Composite film and Al2O3Layer-by-layer deposition of thin film to prepare Ni3Al-Cr3C2-Al2O3A microlaminate film. The parameters of the electrojet deposition were: the height of the metal spray needle from the surface of the cutter base body is 10mm, the movement speed of the metal spray needle is 20mm/s, the direct current voltage is 4kV, and Ni is3Al-Cr3C2Flow rate of composite slurry and Al2O3The flow rate of the slurry was 15. mu.l/min.
In order to remove the organic solvent in the deposited micro-laminated film and release stress, the film is sequentially placed on a preheating platform at 200 ℃ and 300 ℃ for 120 seconds for drying and pyrolysis treatment after each layer of film deposition is finished.
Electrojet deposited Ni3Al-Cr3C2-Al2O3The micro-laminated film is placed in a vacuum sintering furnace for high-temperature sintering, and the vacuum degree is 10-1Pa, the temperature is 1300 ℃, and the heat preservation time is 60 min.
EXAMPLE III
The present disclosure also provides a method for preparing a micro-laminate film having a high infrared reflectance, which is different from example 1 in that,
Ni3Al-Cr3C2the slurry is prepared by mixing Ni3Al powder and Cr3C2Mixing the powder to form mixed powder, and then adding a dispersing agent, a binder and an organic solvent; ball milling for 40 hours by adopting a high-energy ball mill to obtain Ni3Al-Cr3C2And (4) compounding the slurry. Wherein Ni3The powder particle size of Al is 1-10 μm, Cr3C2The powder particle size of (A) is 0.1 μm-1 μm; in the mixed powder, Cr3C2The powder accounts for 30 wt% of the total volume fraction of the composite powder; the mass ratio of the dispersing agent is mixed powder: castor oil 10: 1; the mass ratio of the binder is mixed powder: ethyl cellulose 5: 1; the mass ratio of the organic solvent is mixed powder: anhydrous ethanol ═ 1: 5.
Al2O3The preparation of the slurry comprises the following steps of2O3Adding a dispersing agent, a binder and an organic solvent into the powder; ball milling for 40 hours by adopting a high-energy ball mill to obtain Al2O3Sizing agent; wherein, Al2O3The powder particle size of (A) is 0.1 μm-1 μm; the mass ratio of the dispersing agent is mixed powder: castor oil 10: 1; the mass ratio of the binder is mixed powder: ethyl cellulose 5: 1; the mass ratio of the organic solvent is mixed powder: anhydrous ethanol ═ 1: 5.
Grinding and polishing the metal substrate, and then cleaning the metal substrate in an alcohol solution for 15min to finish the pretreatment of the surface of the substrate;
sequentially depositing Ni on the surface of the pretreated substrate by adopting an electric jet method3Al-Cr3C2Composite film and Al2O3Film, metal needle first moved in X direction to deposit Ni3Al-Cr3C2Layer, then moving in Y direction to deposit Al2O3Layers, in turn alternating to realize Ni3Al-Cr3C2Composite film and Al2O3Layer-by-layer deposition of thin film to prepare Ni3Al-Cr3C2-Al2O3A microlaminate film. The parameters of the electrojet deposition were: the height of the metal spray needle from the surface of the cutter base body is 15mm, the movement speed of the metal spray needle is 30mm/s, the direct current voltage is 5kV, and Ni is3Al-Cr3C2Flow rate of composite slurry and Al2O3The flow rate of the slurry is 20 mul/min。
In order to remove the organic solvent in the deposited micro-laminated film and release stress, the film is sequentially placed on a preheating platform at 200 ℃ and 300 ℃ for 120 seconds for drying and pyrolysis treatment after each layer of film deposition is finished.
Electrojet deposited Ni3Al-Cr3C2-Al2O3The micro-laminated film is placed in a vacuum sintering furnace for high-temperature sintering, and the vacuum degree is 10-3Pa, the temperature is 1500 ℃, and the heat preservation time is 90 min.
Example four
The disclosure also provides a micro-laminated film with high infrared reflectivity, which is prepared by the preparation method of the micro-laminated film with high infrared reflectivity as the embodiment, wherein the micro-laminated film is formed by sequentially depositing an intermetallic compound-carbide composite film and a metal oxide film on the surface of a substrate; the intermetallic compound-carbide is Ni3Al-Cr3C2The metal oxide is Al2O3。
The above description is only a preferred embodiment of the present disclosure and is not intended to limit the present disclosure, and various modifications and changes may be made to the present disclosure by those skilled in the art. Any modification, equivalent replacement, improvement and the like made within the spirit and principle of the present disclosure should be included in the protection scope of the present disclosure.
Although the present disclosure has been described with reference to specific embodiments, it should be understood that the scope of the present disclosure is not limited thereto, and those skilled in the art will appreciate that various modifications and changes can be made without departing from the spirit and scope of the present disclosure.

Claims (10)

1. A method for preparing a micro-laminated film with high infrared reflectivity is characterized by comprising the following steps: and sequentially depositing an intermetallic compound-carbide composite film and a metal oxide film on the surface of the pretreated substrate by adopting an electric jet method to form a micro-laminated film with a multilayer structure.
2. The method of claim 1, wherein the intermetallic-carbide is Ni3Al-Cr3C2(ii) a The metal oxide is Al2O3。
3. The method of claim 2, wherein the step of preparing a high ir reflectivity microlaminate film comprises:
preparation of Ni3Al-Cr3C2Slurry and Al2O3Sizing agent;
pretreating the surface of the substrate, wherein the pretreatment step comprises polishing and cleaning;
sequential deposition of Ni by means of an electrojet process3Al-Cr3C2Composite film and Al2O3A film formed as a micro-laminated film having a multi-layer structure in which each Ni layer is formed3Al-Cr3C2Composite film or Al2O3Drying and pyrolyzing the deposited film;
and (3) carrying out vacuum high-temperature sintering on the micro-laminated film deposited by the electric jet.
4. The method of claim 3, wherein the pretreated substrate surface is moved in the X direction by a metal needle using an electro-jet method and coated with Ni3Al-Cr3C2Slurry to deposit Ni3Al-Cr3C2Layer, moving in Y direction and spraying Al2O3Slurry to deposit Al2O3Layers, in turn alternating to realize Ni3Al-Cr3C2Composite film and Al2O3Layer-by-layer deposition of thin film to prepare Ni3Al-Cr3C2-Al2O3A microlaminate film.
5. The method of claim 3, wherein the dry pyrolysis treatment is performed by sequentially placing the film on a preheating stage at 200 ℃ and 300 ℃ for 120 seconds.
6. The method of claim 3, wherein the vacuum sintering is performed in a vacuum sintering furnace under a vacuum degree of 10-3Pa-1Pa, temperature of 1100-.
7. The method of claim 3, wherein the Ni is prepared3Al-Cr3C2The slurry step comprises adding Ni3Al powder and Cr3C2Mixing the powder to form mixed powder, and then adding a dispersing agent, a binder and an organic solvent; obtaining Ni after ball milling for a set time by adopting a high-energy ball mill3Al-Cr3C2And (4) compounding the slurry.
8. The method of claim 7, wherein the Ni is Ni3The powder particle size of Al is 1-10 μm, Cr3C2The powder particle size of (A) is 0.1 μm-1 μm; in the mixed powder, Cr3C2The powder accounts for 30 wt% of the total volume fraction of the composite powder;
preferably, the mass ratio of the dispersing agent is mixed powder: castor oil 10: 1; the mass ratio of the binder is mixed powder: ethyl cellulose 5: 1; the mass ratio of the organic solvent is mixed powder: anhydrous ethanol ═ 1: 5.
9. The method of claim 3, wherein the Al is prepared by a method comprising preparing a microlaminated film with high IR reflectivity2O3The slurry is prepared by mixing Al2O3Adding a dispersing agent, a binder and an organic solvent into the powder; al is obtained by adopting a high-energy ball mill to ball-mill for a set time2O3Sizing agent;
preferably, Al2O3The powder particle size of (A) is 0.1 μm-1 μm; the mass ratio of the dispersant is Al2O3Powder lot: castor oil 10: 1; the mass ratio of the binder is Al2O3Powder lot: ethyl cellulose 5: 1; the mass ratio of the organic solvent is Al2O3Powder lot: anhydrous ethanol ═ 1: 5.
10. A microlaminated film having a high infrared reflectance, characterized by being produced by the method for producing a microlaminated film having a high infrared reflectance according to any one of claims 1 to 9.
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