CN116769326B - MXene-based wave-absorbing material, preparation method and application - Google Patents
MXene-based wave-absorbing material, preparation method and application Download PDFInfo
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- CN116769326B CN116769326B CN202310626898.2A CN202310626898A CN116769326B CN 116769326 B CN116769326 B CN 116769326B CN 202310626898 A CN202310626898 A CN 202310626898A CN 116769326 B CN116769326 B CN 116769326B
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Abstract
The invention provides an MXene-based wave-absorbing material, a preparation method and application thereof, and relates to the technical field of radar wave-absorbing materials. The wave-absorbing material comprises the following components in percentage by mass: 0.1-0.3% of MXene material, 0.5-1% of Fe 3 O 4 And the balance of photosensitive resin; wherein the MXene material is a material with a two-dimensional structure formed by removing main group elements from MAX phase, and the Fe 3 O 4 Is nano-scale Fe 3 O 4 The method comprises the steps of carrying out a first treatment on the surface of the The wave absorbing member using the wave absorbing material can be used for military stealth, human body wearable electromagnetic shielding, wall or building filler. The wave-absorbing material is prepared from electrically-lossy MXene material and magnetically-lossy nanoscale Fe 3 O 4 The wave-absorbing material has the strong wave-absorbing characteristic of wide frequency by organic combination, and can be integrally formed by using 3D printing equipment, and the shape can be customized, so that the surface integration degree of the wave-absorbing material is improved.
Description
Technical Field
The invention relates to the technical field of radar wave-absorbing materials, in particular to an MXene-based wave-absorbing material, a preparation method and application.
Background
Because the MXene nano-sheet has good interlayer electronic coupling and excellent conductivity (the conductivity can reach 4600S/cm), the electromagnetic wave entering the inside of the material can be effectively attenuated, and the electromagnetic shielding effectiveness of the MXene film with the thickness of 45 mu m can reach 92dB. Therefore, the MXene material is further processed and mixed with materials such as metal, polymer, ceramic and the like by utilizing the wave absorbing characteristic of the MXene material, and then a 3D structure is constructed by printing layer by layer, so that the MXene material becomes a brand new research hot spot. In order to improve the environmental adaptability of various military weapons, the surface of the military weapons has higher and higher requirements on the structural wave absorbing integration. Accordingly, the present application proposes a solution to improve the surface integration problem of the wave-absorbing material.
Disclosure of Invention
The invention aims to provide an MXene-based wave-absorbing material, a preparation method and application thereof, wherein the wave-absorbing material is prepared from an MXene material with electric loss and nano-scale Fe3O with magnetic loss 4 The organic combination is carried out, so that the wave-absorbing material has the broadband strong wave-absorbing characteristic.
In a first aspect, the present invention provides an MXene-based wave absorbing material, including, in mass percentages: 0.1-0.3% of MXene material, 0.5-1% of Fe3O 4 And the balance of photosensitive resin; wherein the MXene material is a material with a two-dimensional structure formed by removing main group elements from MAX phase, and the Fe3O 4 Is nano-scale Fe3O 4 。
The MXene-based wave-absorbing material provided by the invention has the beneficial effects that: MXene material and nanoscale Fe 3 O 4 All have better wave absorbing performance, can effectively attenuate electromagnetic waves in the material, has good electromagnetic shielding effect, and combines MXene material with nano-scale Fe 3 O 4 Dispersing in photosensitive resin to make the whole material have better plasticity and processability, and simultaneously make MXene material and nano Fe 3 O 4 Uniformly mixing the MXene material with electric loss and nano-scale Fe with magnetic loss 3 O 4 The organic combination is carried out, so that the wave-absorbing material has the broadband strong wave-absorbing characteristic.
Optionally, the MXene material is Ti 3 C 2 T x 。Ti 3 C 2 T x Is Ti 3 A1C 2 After hydrogen fluoride etching, the formed substance with a large number of high electronegativity groups such as-O, -OH and-F on the surface has good metal conductivity, hydrophilicity, large specific surface area and abundant surface modification groups, and is convenient for being matched with nanoscale Fe 3 O 4 And (5) compounding.
Optionally, the MXene material is in a thin film sheet. The beneficial effects are that the film structure has folds, and the plurality of films are extruded and deformed, thereby showing a certain flexibility and being beneficial to nano-scaleFe 3 O 4 The material is dispersed and compounded on the surface of the MXene material.
Optionally, the nanoscale Fe 3 O 4 The particle size of (2) is 10-20nm. Thus is beneficial to Fe 3 O 4 Is uniformly dispersed.
Alternatively, the photosensitive resin is a resin material usable for a 3D printing apparatus. The beneficial effects are that: the method is favorable for customizable plasticity of the wave-absorbing material, and improves convenience in plasticity.
In a second aspect, the present invention also provides a method for preparing an MXene-based wave-absorbing material, comprising the steps of: MXene material and Fe 3 O 4 After being uniformly dispersed, the mixture is added into photosensitive resin and uniformly mixed, thus obtaining the MXene-based wave-absorbing material.
In a third aspect, the present invention also provides a wave-absorbing member of an MXene wave-absorbing material prepared by applying any one of the foregoing MXene wave-absorbing materials or the foregoing method for preparing an MXene-based wave-absorbing material, where the wave-absorbing member may be used in military stealth, human body wearable electromagnetic shielding, wall or building filler.
Optionally, the wave absorbing member is honeycomb-shaped. The beneficial effects are that: the honeycomb structure has better structural strength and higher specific surface area, and is beneficial to wave absorption.
In a fourth aspect, the present invention also provides a method for preparing a wave-absorbing member of an MXene wave-absorbing material prepared by using any one of the above-mentioned MXene wave-absorbing materials or the above-mentioned MXene-based wave-absorbing material preparation method, comprising the steps of: modeling to obtain a wave-absorbing member model; and (3) taking the MXene wave-absorbing material as a raw material, printing the wave-absorbing member model by using 3D printing equipment, and cooling to obtain the wave-absorbing member. The beneficial effects are that: the wave-absorbing member can be customized in specific form and specific size, and meanwhile, the 3D printing equipment is adopted to ensure the structural accuracy and the molding convenience of the wave-absorbing member.
Drawings
FIG. 1 is a diagram of Ti in an embodiment of the invention 3 C 2 T x SEM images of the material;
FIG. 2 is a nano-scale F in an embodiment of the inventione 3 O 4 SEM images of (a);
FIG. 3 is a flowchart of a method for manufacturing a honeycomb-shaped wave-absorbing member according to an embodiment of the present invention;
FIG. 4 is a test result of the wave-absorbing member of example 1 of the present invention when it was subjected to a reflectance test;
FIG. 5 is a test result of the wave-absorbing member of example 2 of the present invention when it was subjected to a reflectance test;
fig. 6 is a test result when the wave-absorbing member of comparative example 1 of the present invention was subjected to a reflectance test.
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 below, 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. Unless otherwise defined, technical or scientific terms used herein should be given the ordinary meaning as understood by one of ordinary skill in the art to which this invention belongs. As used herein, the word "comprising" and the like means that elements or items preceding the word are included in the element or item listed after the word and equivalents thereof without precluding other elements or items.
It should be noted that MXene is a two-dimensional compound of no compound, which is composed of transition metal carbides, nitrides or carbonitrides of several atomic layer thicknesses. Is generally formed by dividing the main group element by a MAX phase, wherein MAX is M n+1 AX n M is a transition metal element, A is a main group element, X is a carbon element, a nitrogen element or a carbon nitrogen element, n is any one of 1, 2 and 3, and the chemical property of A is active because of strong bond energy between M and X, so that the A can be removed from the MAX phase, and a graphene-like two-dimensional structure can be obtained.
The embodiment of the invention provides an MXene-based wave-absorbing material which is prepared from the following components in massThe percentages include: 0.1-0.3% of MXene material, 0.5-1% of Fe 3 O 4 And the balance of photosensitive resin, in particular, fe 3 O 4 Is nano-scale Fe 3 O 4 。
In some embodiments, the MXene material is Ti 3 C 2 T x . Specifically, ti 3 C 2 T x Is Ti 3 AlC 2 After the MAX precursor is etched by hydrofluoric acid, the MXene material with a large number of high electronegativity groups such as-O, -OH, and-F on the surface is formed.
In some embodiments, ti may be 3 AlC 2 Adding MAX precursor into 1-3M hydrofluoric acid to react for 10-20min, taking out and drying to obtain Ti 3 C 2 T x . When the reaction is carried out by using hydrofluoric acid with lower concentration, the safety in preparation and production can be improved.
In some examples, 1.65g of LiF powder was weighed beforehand using an electronic balance and slowly added to 25mL of 6mol/L hydrochloric acid to obtain a hydrofluoric acid solution after sufficient reaction, and then Ti was added 3 AlC 2 Adding MAX precursor into the prepared hydrofluoric acid solution for reaction, taking out and drying to obtain Ti 3 C 2 T x 。
In some embodiments, 1.25g of Ti is weighed using an electronic balance 3 AlC 2 Slowly adding MAX precursor into hydrofluoric acid solution until completely adding, placing in a constant-temperature water bath at 35 ℃, stirring at 350rpm, fully reacting for 48h, filtering out the product, repeatedly washing and centrifuging the product by using deionized water until the pH value of the product is approximately equal to 6, vacuum-filtering, and drying in a drying oven to obtain Ti 3 C 2 Tx。
In some embodiments, see FIG. 1, ti 3 C 2 T x The film is sheet-shaped, folds exist on the film, extrusion deformation exists between the films, and certain flexibility is shown.
In some embodiments, the film is in the form of Ti 3 C 2 Tx has a size of 40-50 μm.
In some embodiments of the present invention,referring to FIG. 2, nanoscale Fe 3 O 4 Is of a spheroid structure, has a particle size of 10-20nm, and is nano-scale Fe 3 O 4 Has ferromagnetism.
In some embodiments, the photosensitive resin used is any resin material that can be applied to a 3D printing apparatus, and other characteristics of the resin material, such as a rigid resin, a high temperature resistant resin, a marking resin, a performance resin, a flexible resin, a transparent resin, and a ductile resin, may also be adjusted depending on actual needs.
The invention also provides a preparation method of the MXene-based wave-absorbing material in any embodiment, which comprises the following steps: ti is mixed with 3 C 2 T x With Fe 3 O 4 After being uniformly dispersed, the mixture is added into photosensitive resin and uniformly mixed, thus obtaining the MXene-based wave-absorbing material.
In some embodiments, ti is pre-applied to the preparation of the MXene-based wave-absorbing material using an electric stirrer 3 C 2 T x Flake and Fe 3 O 4 After the nano particles are uniformly dispersed, the dispersed mixture is added into photosensitive resin and uniformly mixed to prepare the MXene-based wave-absorbing material.
In some embodiments, in preparing the MXene-based wave-absorbing material, an electric stirrer is used for the Ti 3 C 2 T x Flake and Fe 3 O 4 Stirring and dispersing the nano particles for 15-60 min.
In some embodiments, in the preparation of the MXene-based wave-absorbing material, the dispersed mixture is added into photosensitive resin and stirred for 15-20min to be uniformly mixed, so as to prepare the MXene-based wave-absorbing material.
The invention also provides a wave-absorbing member of the MXene-based wave-absorbing material applied to any embodiment or the MXene-based wave-absorbing material prepared by the preparation method in any embodiment, and the wave-absorbing member has good wave-absorbing shielding function and larger wave-absorbing frequency band, and can be used for military stealth, human body wearable electromagnetic shielding, walls or building fillers.
In some embodiments, the wave absorbing member is honeycomb shaped.
The invention also provides a method for preparing a wave-absorbing member by applying the MXene-based wave-absorbing material in any embodiment or the MXene-based wave-absorbing material prepared by the preparation method in any embodiment, which comprises the following steps: modeling to obtain a wave-absorbing member model; and (3) taking the MXene wave-absorbing material as a raw material, printing the wave-absorbing member model by using 3D printing equipment, and cooling to obtain the wave-absorbing member.
In some embodiments, the wave absorbing member is set to a honeycomb shape when modeling. Specifically, the dimension of the wave absorbing member was set to be 2.98mm in side length, 1mm in wall thickness and 11.84mm in height.
In some embodiments, the wave-absorbing member is obtained by cooling at room temperature, hardening and demolding after printing the wave-absorbing member model by using 3D printing equipment.
Example 1
Referring to fig. 3, embodiment 1 provides a honeycomb-shaped wave-absorbing member, which is prepared by the following steps:
s1, material preparation: respectively weighing 0.1% of Ti by mass percent 3 C 2 T x Flake, 0.5% Fe 3 O 4 And 99.4% of a photosensitive resin, wherein Ti 3 C 2 T x The flake size is 40-50um, fe 3 O 4 The particle size of the resin is 10-20nm, and the photosensitive resin is rigid resin produced by the company of creating three-dimensional science and technology;
s2, mixing and dispersing: ti is mixed with 3 C 2 T x Flake and Fe 3 O 4 After uniformly stirring by using an electric stirrer, adding the mixture into photosensitive resin, and stirring until the three materials are uniformly mixed to obtain an MXene-based wave-absorbing material;
s3, modeling and forming: building a component model with a single honeycomb unit side length of 2.98mm, a wall thickness of 1mm, a height of 11.84mm and an overall size of 180×180mm, printing the component model by using a MXene-based wave absorbing material as a base material by using 3D printing equipment, cooling to hardening at room temperature after printing, and demoulding to obtain the wave absorbing component.
Example 2
Embodiment 2 provides a honeycomb-shaped wave absorbing member and an embodiment1 is different in that in the step S1 of material preparation, 0.3 percent of Ti is respectively weighed 3 C 2 T x Flake, 1% Fe 3 O 4 And 98.7% of a photosensitive resin.
Comparative example 1
The preparation method of the honeycomb wave-absorbing member provided in the comparative example 1 comprises the following steps:
d1, weighing 100 percent of photosensitive resin by taking the example 1 as a reference; .
And D2, constructing a component model with a single honeycomb unit side length of 2.98mm, a wall thickness of 1mm, a height of 11.84mm and an overall size of 180×180mm, printing the component model by using a 3D printing device by using photosensitive resin as a base material, cooling to a hardened state at room temperature after printing, and demoulding to obtain the wave-absorbing component.
Performance detection
Referring to the test method described in GJB 2038A-2011 "method for testing reflectivity of radar absorbing material", reflectivity of the honeycomb-shaped absorbing members in example 1, example 2 and comparative example 1 was tested, and reflectivity at the frequency band of 1-18GHz was obtained as shown in fig. 4, 5 and 6 in order, and it is known that the absorbing members in example 1 and example 2 have good absorbing shielding function and large absorbing frequency band.
While embodiments of the present invention have been described in detail hereinabove, it will be apparent to those skilled in the art that various modifications and variations can be made to these embodiments. It is to be understood that such modifications and variations are within the scope and spirit of the present invention as set forth in the following claims. Moreover, the invention described herein is capable of other embodiments and of being practiced or of being carried out in various ways.
Claims (5)
1. An MXene-based wave absorbing material, characterized by comprising, in mass percent: 0.1-0.3% of MXene material, 0.5-1% of Fe 3 O 4 And the balance of photosensitive resin; wherein the MXene material is a material with a two-dimensional structure formed by removing main group elements from MAX phase, and the Fe 3 O 4 Is nano-scale Fe 3 O 4 And the nano-scale Fe 3 O 4 The particle size of (2) is 10-20nm; the MXene material is Ti 3 C 2 T x And the MXene material is in a film sheet shape; the photosensitive resin is a resin material that can be used for a 3D printing apparatus.
2. A method for preparing the MXene-based wave-absorbing material according to claim 1, comprising the steps of: MXene material and Fe 3 O 4 After being uniformly dispersed, the mixture is added into photosensitive resin and uniformly mixed, thus obtaining the MXene-based wave-absorbing material.
3. A wave-absorbing member using the MXene wave-absorbing material according to claim 1 or the MXene wave-absorbing material prepared by the method for preparing the MXene wave-absorbing material according to claim 2, characterized in that the wave-absorbing member can be used for military stealth, human body wearable electromagnetic shielding, wall or building filler.
4. The wave-absorbing member for applying an MXene wave-absorbing material according to claim 3, wherein the wave-absorbing member is honeycomb-shaped.
5. A method for producing a wave-absorbing member using an MXene wave-absorbing material according to any one of claims 3 to 4, comprising the steps of:
modeling to obtain a wave-absorbing member model;
and (3) taking the MXene wave-absorbing material as a raw material, printing the wave-absorbing member model by using 3D printing equipment, and cooling to obtain the wave-absorbing member.
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| CN108342036A (en) * | 2018-03-26 | 2018-07-31 | 南昌航空大学 | A kind of magnetism Mxenes polymer composite wave-suction materials and preparation method thereof |
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| CN114552231A (en) * | 2022-01-24 | 2022-05-27 | 华南理工大学 | Ferrite-manganese oxide-MXene composite wave-absorbing particle and preparation method and application thereof |
| CN114655957A (en) * | 2022-04-28 | 2022-06-24 | 陕西科技大学 | Magnetic MXene wave-absorbing composite material with corallite structure and preparation method thereof |
| CN115340761A (en) * | 2022-07-08 | 2022-11-15 | 西安电子科技大学 | Light PEO/MXene aerogel wave-absorbing material based on polyethylene oxide and preparation method thereof |
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| CN108342036A (en) * | 2018-03-26 | 2018-07-31 | 南昌航空大学 | A kind of magnetism Mxenes polymer composite wave-suction materials and preparation method thereof |
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