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CN116811376A - Ti-based 3 C 2 T x High-temperature-resistant broadband wave-absorbing composite material with honeycomb sandwich structure of MXene aerogel and preparation method thereof - Google Patents

Ti-based 3 C 2 T x High-temperature-resistant broadband wave-absorbing composite material with honeycomb sandwich structure of MXene aerogel and preparation method thereof Download PDF

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Publication number
CN116811376A
CN116811376A CN202310775659.3A CN202310775659A CN116811376A CN 116811376 A CN116811376 A CN 116811376A CN 202310775659 A CN202310775659 A CN 202310775659A CN 116811376 A CN116811376 A CN 116811376A
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temperature
composite material
mxene
wave
resistant
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CN116811376B (en
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杨明龙
刘海韬
孙逊
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National University of Defense Technology
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National University of Defense Technology
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Abstract

The invention relates to the technical field of wave-absorbing composite materials, and particularly discloses a composite material based on Ti 3 C 2 T x The honeycomb sandwich structure high-temperature-resistant broadband wave-absorbing composite material of the MXene aerogel comprises a multi-layer structure, a high-temperature-resistant resin matrix composite material wave-transmitting skin, a honeycomb structure wave-absorbing layer and a high-temperature-resistant resin matrix composite material reflecting skin from outside to inside in sequence, wherein the honeycomb structure wave-absorbing layer is a composite material honeycomb structure filled with the high-temperature-resistant MXene composite aerogel material. The invention is based on Ti 3 C 2 T x High-temperature-resistant broadband wave-absorbing composite material with honeycomb sandwich structure of MXene aerogel and MXene composite aerogel material (density is 2 mg/cm) 3 ~15 mg/cm 3 ) The light composite material honeycomb structural carrier overcomes the defect of high density of the traditional wave-absorbing material, has the effective absorption frequency bandwidth of lower than-10 dB and can reach more than 10GHz, and can simultaneously meet the broadband wave-absorbing performance and light-weight requirements of aerospace aircraft equipment on the wave-absorbing material.

Description

Ti-based 3 C 2 T x High-temperature-resistant broadband wave-absorbing composite material with honeycomb sandwich structure of MXene aerogel and preparation method thereof
Technical Field
The invention relates to the technical field of wave-absorbing composite materials, in particular to a composite material based on Ti 3 C 2 T x A high-temperature resistant broadband wave-absorbing composite material with a honeycomb sandwich structure of MXene aerogel and a preparation method thereof.
Background
The new generation of aviation and aerospace craft equipment is subjected to omnibearing single-station and multi-station detection threat in the service process of ground roadbed radar, marine ship-borne radar, air radar pre-alarm and space-borne radar systems. In order to reduce the radar scattering cross section target characteristics, improve radar stealth and outburst prevention capability, besides the external stealth design, the use of high-performance wave-absorbing materials on the surface of the radar has become a necessary choice. Meanwhile, the requirements of light design of equipment, complex force/heat load working conditions such as pneumatic pressure and heating effect to be faced when flying in the atmosphere, and temperature resistance requirements of key scattering parts of an air inlet channel and the like close to an engine heat source are considered, and the stealth materials used by the aerospace equipment must meet the performance requirements of light weight, high temperature resistance, high strength, broadband wave absorption and the like.
Although the radar wave-absorbing material reported at present can obtain good wave-absorbing effect in a specific frequency band (most of the wave-absorbing material is X, ku wave band), the radar wave-absorbing material also has the performance defects of high material density, low mechanical strength, poor temperature resistance, poor broadband wave-absorbing capability and the like, for example, the density of ferrite wave-absorbing material can reach 4.9-7.6 g/cm 3 The effective absorption bandwidth with reflectivity less than-10 dB is generally less than 8GHz; although carbon-based wave-absorbing materials such as carbon powder and ohmic-loss wave-absorbing materials such as conductive polymers have lower material density, the effective wave-absorbing frequency bandwidth is also mostly below 10GHz, the long-term temperature resistance is lower than 200 ℃, and the material does not generally have mechanical bearing capacity; the wave-absorbing metamaterial composed of the periodic structure metal patterns and the high polymer dielectric matrix has the wave-absorbing frequency width reaching more than 10GHz through structural optimization design, but the matching material thickness is large when the wave-absorbing mechanism is caused by the resonance loss based on the structure, the density of the metal patterns and the high polymer dielectric matrix is higher, and the high temperature resistance and the oxidation resistance are poor. Therefore, the existing wave-absorbing material still has obvious defects in the aspects of material density, absorption frequency bandwidth, mechanical strength and temperature resistance, and is difficult to meet the requirements of the aerospace equipment on radar stealth, complex force and thermal service conditions on the multifunctional integrated performance of light weight, high temperature resistance, high strength and broadband wave absorption. In order to solve the problems, the invention discloses a high-temperature resistant resin-based broadband wave-absorbing composite material with a honeycomb sandwich structure based on Ti3C2Tx MXene aerogel and a preparation method thereof, and aims to realize the design and preparation of a light-weight, high-strength, high-temperature resistant and broadband wave-absorbing multifunctional integrated wave-absorbing material.
Disclosure of Invention
The invention aims to provide a Ti-based alloy 3 C 2 T x A high-temperature-resistant broadband wave-absorbing composite material with a honeycomb sandwich structure of MXene aerogel and a preparation method thereof solve the defects of narrow wave-absorbing frequency, high material density and the like of the existing wave-absorbing material.
To achieve the above object, the present invention provides a Ti-based alloy 3 C 2 T x The high-temperature-resistant broadband wave-absorbing composite material with the honeycomb sandwich structure of the MXene aerogel is of a multi-layer structure, and sequentially comprises a high-temperature-resistant resin matrix composite wave-transmitting skin, a honeycomb structure wave-absorbing layer and a high-temperature-resistant resin matrix composite reflecting skin from outside to inside, wherein the honeycomb structure wave-absorbing layer is of a composite honeycomb structure filled with the high-temperature-resistant MXene composite aerogel material.
Preferably, the above is based on Ti 3 C 2 T x In the high-temperature-resistant broadband wave-absorbing composite material with the honeycomb sandwich structure of the MXene aerogel, the high-temperature-resistant MXene composite aerogel material is Ti 3 C 2 T x MXene/SiO 2 Composite aerogel material with density of 5-15 mg/cm 3 ，Ti 3 C 2 T x MXene and SiO 2 The mass ratio is 1:4-4:1.
Preferably, the above is based on Ti 3 C 2 T x In the high-temperature-resistant broadband wave-absorbing composite material with the honeycomb sandwich structure of the MXene aerogel, the honeycomb structure of the composite material is a quartz fiber or aramid fiber reinforced polyimide composite material honeycomb, the thickness of the honeycomb structure of the composite material is 5-10 mm, the shape of honeycomb holes is hexagonal, rectangular or triangular, the honeycomb Kong Bianchang is 2-10 mm, and the thickness of the hole wall is 0.2-0.5 mm. The composite material honeycomb structure provides mechanical bearing function for the composite material, is used as a carrier framework to protect the MXene composite aerogel wave-absorbing material structure from being damaged, simultaneously inhibits induced vortex current, and optimizes Ti 3 C 2 T x MXene/SiO 2 The impedance matching characteristic of the composite aerogel material enhances electromagnetic wave absorption, and the wave absorbing layer with the honeycomb structure formed by combining the composite aerogel material with the high-temperature-resistant MXene composite aerogel material can improve the wave absorption of the composite materialPerformance.
Preferably, the above is based on Ti 3 C 2 T x In the high-temperature-resistant broadband wave-absorbing composite material with the honeycomb sandwich structure of the MXene aerogel, the wave-transmitting skin of the high-temperature-resistant resin-based composite material is a quartz fiber or aramid fiber reinforced polyimide resin-based composite material, and the thickness is 0.5-2 mm. The high-temperature-resistant resin-based composite material wave-transparent skin provides the composite material with the functions of surface packaging protection, improving the surface impedance matching effect and enhancing the incidence of electromagnetic waves.
Preferably, the above is based on Ti 3 C 2 T x In the high-temperature-resistant broadband wave-absorbing composite material with the honeycomb sandwich structure of the MXene aerogel, the high-temperature-resistant resin-based composite material reflection skin is a carbon fiber reinforced polyimide resin-based composite material or a carbon fiber reinforced bismaleimide resin-based composite material, and the thickness is 0.5-2 mm. The high-temperature-resistant resin-based composite material reflection skin provides a mechanical bearing function for the composite material and reflects electromagnetic waves back into the composite material for secondary absorption.
The invention also provides a Ti-based alloy 3 C 2 T x The preparation method of the high-temperature-resistant broadband wave-absorbing composite material with the honeycomb sandwich structure of the MXene aerogel comprises the following steps:
(1) Preparing a high-temperature-resistant resin matrix composite wave-transmitting skin;
(2) Ti is mixed with 3 C 2 T x Uniformly stirring an aqueous phase dispersion liquid of the MXene two-dimensional nano material and aqueous phase silica sol to obtain a mixed solution, placing a fiber reinforced polyimide composite honeycomb in a mold, pouring the mixed solution until the honeycomb is just immersed, and obtaining a composite honeycomb structure filled with a high-temperature-resistant MXene composite aerogel material through freezing and vacuum freeze drying;
(3) Preparing a high-temperature-resistant resin-based composite material reflection skin;
(4) The high-temperature resistant resin-based composite material reflection skin, the composite material honeycomb structure filled with the high-temperature resistant MXene composite aerogel material and the high-temperature resistant resin-based composite material wave-transparent skin are sequentially stacked from bottom to top, a high-temperature adhesive film is used between layers, and a die is adoptedBonding molding is carried out by a pressure heating curing bonding method, and Ti-based is obtained 3 C 2 T x High-temperature-resistant broadband wave-absorbing composite material with honeycomb sandwich structure of MXene aerogel.
Preferably, in the above preparation method, ti in the mixed solution 3 C 2 T x MXene and SiO 2 The total concentration is 5-15 mg/mL, ti 3 C 2 T x MXene and SiO 2 The concentration ratio of (2) is 1:4-4:1.
Preferably, in the above preparation method, in the step (1), the preparation of the high temperature resistant resin matrix composite wave-transparent skin specifically includes: and (3) regularly layering the fiber cloth according to a specific angle until the number of layers is set, wherein the fiber cloth is unidirectional fiber cloth or plain fiber cloth, and finishing polyimide resin dipping by adopting a vacuum bag assisted RTM method, and performing compression molding, heating, curing and forming.
Preferably, in the above preparation method, in the step (1), the fiber cloth is unidirectional fiber cloth or plain fiber cloth, the specific angle regular ply is 0 ° and 90 ° alternate orthogonal ply, and the number of layers is 2-10.
Preferably, in the above preparation method, in the step (1), the curing molding temperature is 280-300 ℃ and the curing time is 5-10 hours.
Preferably, in the above preparation method, in the step (2), ti 3 C 2 T x The preparation method of the MXene two-dimensional nanomaterial aqueous dispersion liquid comprises the following steps: tiAlC of MAX phase etched by chemical etchant 2 Ceramic particles, obtaining layered structure Ti 3 C 2 T x MXene, and then cleaning and stripping to obtain Ti 3 C 2 T x An aqueous phase dispersion of an MXene two-dimensional nanomaterial; the chemical etchant is a mixed solution of acid and lithium fluoride, the ratio of the acid to the lithium fluoride is 10 mL:1-5 g, and the acid is hydrochloric acid or hydrofluoric acid.
Preferably, in the above preparation method, in the step (2), the freezing and compacting method is to freeze by liquid nitrogen or freeze on a semiconductor refrigeration plate with controllable temperature or directly freeze in a refrigerator freezing environment.
Preferably, in the above preparation method, in the step (3), the preparation of the high temperature resistant resin matrix composite reflective skin specifically includes: and (3) regularly layering carbon fiber cloth according to a specific angle until the number of layers is set, wherein the carbon fiber cloth is unidirectional fiber cloth or plain fiber cloth, and finishing polyimide resin impregnation by adopting a vacuum bag assisted RTM method, and performing compression molding, heating, curing and forming.
Preferably, in the above preparation method, in the step (3), the carbon fiber cloth is unidirectional fiber cloth or plain fiber cloth, the layering angles are alternately orthogonal layering at 0 ° and 90 °, and the layering layers are 5-10 layers.
Preferably, in the above preparation method, in the step (3), the curing molding temperature is 280-300 ℃ and the curing time is 5-10 hours.
Preferably, in the above preparation method, in the step (4), the high temperature adhesive film is a polyimide high temperature adhesive film with a temperature resistance of 300 ℃, a curing adhesive temperature of 280-300 ℃ and a curing time of 5-10 h.
Compared with the prior art, the invention has the beneficial effects that:
1. the invention is based on Ti 3 C 2 T x High-temperature-resistant broadband wave-absorbing composite material with honeycomb sandwich structure of MXene aerogel, and overall density of composite material is 0.3-0.6 g/cm 3 MXene composite aerogel material (density 2mg/cm 3 ～15mg/cm 3 ) The light composite material honeycomb structural carrier overcomes the defect of high density of the traditional wave-absorbing material, has the effective absorption frequency bandwidth of lower than-10 dB and can reach more than 10GHz, and can simultaneously meet the broadband wave-absorbing performance and light-weight requirements of aerospace aircraft equipment on the wave-absorbing material.
2. The invention is based on Ti 3 C 2 T x The honeycomb sandwich structure high-temperature-resistant broadband wave-absorbing composite material of the MXene aerogel has high temperature resistance up to 300 ℃ and good high temperature resistance; at the same time, a low thermal conductivity MXene composite aerogel material (thermal conductivity<0.03W/m.K) and the composite material honeycomb heat insulation structure, has good heat insulation performance, and meets the heat insulation performance requirements of aerospace craft equipment on the multifunctional integrated wave-absorbing material.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are required to be used in the description of the embodiments will be briefly described below. It will be apparent to those of ordinary skill in the art that the drawings in the following description are of some embodiments of the invention and that other drawings may be derived from them without undue effort.
FIG. 1 is a Ti-based alloy of the present invention 3 C 2 T x The structural schematic diagram of the high-temperature-resistant resin-based broadband wave-absorbing composite material with the honeycomb sandwich structure of the MXene aerogel.
FIG. 2 is a multilayer Ti prepared in example 1 of the invention 3 C 2 T x SEM photograph of MXene particles.
FIG. 3 is a single layer of Ti as prepared in example 1 of the invention 3 C 2 T x TEM photograph of MXene nanoplatelets.
FIG. 4 is a Ti-based alloy of example 1 of the present invention 3 C 2 T x The reflectivity curve graph of the high-temperature-resistant resin-based broadband wave-absorbing composite material with the honeycomb sandwich structure of the MXene aerogel.
FIG. 5 is a Ti-based alloy of example 2 of the invention 3 C 2 T x The reflectivity curve graph of the high-temperature-resistant resin-based broadband wave-absorbing composite material with the honeycomb sandwich structure of the MXene aerogel.
The main reference numerals illustrate:
1-high temperature resistant resin matrix composite wave-transmitting skin, 2-high temperature resistant MXene composite aerogel material filling phase, 3-composite honeycomb structure and 4-high temperature resistant resin matrix composite reflecting skin.
Detailed Description
The following detailed description of specific embodiments of the invention is, but it should be understood that the invention is not limited to specific embodiments. Unless defined otherwise, all technical and scientific terms used hereinafter have the same meaning as commonly understood by one of ordinary skill in the art. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the scope of the present invention. Unless otherwise specifically indicated, the various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or may be prepared by existing methods.
Example 1
Ti-based 3 C 2 T x As shown in FIG. 1, the high-temperature-resistant broadband wave-absorbing composite material with the honeycomb sandwich structure of the MXene aerogel is of a multi-layer structure, an electromagnetic wave incident direction is defined as the outer surface of the material, the composite material is sequentially composed of a high-temperature-resistant resin-based composite material wave-transmitting skin, a honeycomb structure wave-absorbing layer and a high-temperature-resistant resin-based composite material reflecting skin from outside to inside, and the high-temperature-resistant resin-based composite material wave-transmitting skin material is a quartz fiber reinforced polyimide resin-based composite material with the thickness of 0.5mm; the wave absorbing layer of the honeycomb structure is a composite material honeycomb structure filled with a high-temperature-resistant MXene composite aerogel material, and the high-temperature-resistant MXene composite aerogel material is Ti 3 C 2 T x MXene/SiO 2 Composite aerogel material with directional pore structure and density of 5mg/cm 3 ，Ti 3 C 2 T x MXene and SiO 2 The mass ratio is 2:3, the composite honeycomb structure is an aramid fiber reinforced polyimide composite honeycomb, the honeycomb holes are hexagonal, the side length is 5mm, the thickness of the hole wall is 0.2mm, and the thickness of the honeycomb is 10mm; the high-temperature resistant resin-based composite material reflection skin is a carbon fiber reinforced polyimide resin-based composite material, and the thickness is 1mm.
The Ti-based alloy of this embodiment 3 C 2 T x The preparation method of the high-temperature-resistant broadband wave-absorbing composite material with the honeycomb sandwich structure of the MXene aerogel comprises the following steps:
(1) Preparing a high-temperature-resistant resin matrix composite wave-transmitting skin: adopting high-temperature resistant low-dielectric unidirectional quartz fiber cloth to be regularly paved into 4 layers according to 0 DEG and 90 DEG alternating paving angles, adopting a vacuum bag assisted RTM method to finish polyimide resin dipping, carrying out mould pressing and heating to 300 ℃ and preserving heat for 5 hours to finish curing and forming, adopting linear cutting to cut a formed composite material flat plate into 300mm multiplied by 300mm transverse dimensions, and adopting a grinding machine or manual grinding to grind the surface of the composite material to be smooth, thus obtaining the 0.5 mm-thick high-temperature resistant resin matrix composite material wave-transparent skin;
(2) Preparing a composite material honeycomb structure filled with a high-temperature-resistant MXene composite aerogel material:
1.5g LiF is dissolved in 30mL of concentrated hydrochloric acid with the concentration of 9mol/L to obtain a mixed etching agent of hydrochloric acid and lithium fluoride, and 1g of MAX phase TiAlC with the particle size of 325 meshes is added 2 The ceramic particles were added to 30mL of etchant, placed in a polytetrafluoroethylene beaker, and stirred at a constant temperature of 3000r/min in a water bath at 30℃for 24h. And then centrifugally collecting the etched solid powder precipitate to obtain the multilayer structure Ti 3 C 2 T x MXene particles, a scanning electron microscope photograph of which is shown in FIG. 2;
dispersing the precipitate into 50mL deionized water, centrifuging at 3000r/min for 5min, collecting again to complete one time cleaning, and repeating the dispersing-centrifuging collecting process to obtain supernatant pH>6, or after centrifugation, the upper layer liquid is not transparent any more, namely, the washing link is completed; dispersing the precipitate into 50mL deionized water, sealing, filling argon protective atmosphere, isolating air, performing ultrasonic treatment for 15min, centrifuging for 30min at 9000r/min, and collecting upper liquid to obtain single-layer Ti 3 C 2 T x MXene nanosheet aqueous dispersion, ti 3 C 2 T x The transmission electron microscope photograph of the MXene nano-sheet is shown in figure 3; adding aqueous phase silica sol, stirring uniformly to obtain Ti with concentration of 5mg/mL 3 C 2 T x MXene nanoplatelets and SiO 2 A mixed solution with a mass ratio of 2:3;
placing 300mm×300mm×10mm aramid fiber/polyimide composite honeycomb in a customized trough mold with metal bottom plate and sealed edge, pouring mixed solution until the honeycomb is just immersed, pouring liquid nitrogen into the mold for freezing until the mixed solution in the honeycomb holes is completely frozen, placing into a cold well at-40deg.C and vacuum degree of 10 -5 Drying in a Pa freeze dryer for 5 days to obtain a composite material honeycomb structure filled with the high-temperature-resistant MXene composite aerogel material;
(3) Preparing a high-temperature-resistant resin-based composite material reflection skin: uniformly layering unidirectional carbon fiber cloth to 5 layers according to 0 DEG and 90 DEG alternating layering angles, finishing dipping polyimide resin by adopting a vacuum bag assisted RTM method, performing compression molding and heating to 300 ℃ and preserving heat for 5 hours to finish curing molding, cutting a molded composite material flat plate into a size of 300mm multiplied by 300mm by adopting linear cutting, grinding the surface of the composite material by adopting a grinding machine or manual grinding to smooth, and obtaining a high-temperature-resistant resin-based composite material reflection skin with the thickness of 1mm;
(4) Integral gluing of honeycomb sandwich structure composite material: the method comprises the steps of stacking a composite material honeycomb structure filled with a high-temperature-resistant resin-based composite material reflection skin, a high-temperature-resistant MXene composite aerogel material and a high-temperature-resistant resin-based composite material wave-transparent skin sequentially from bottom to top, using a 300 ℃ -resistant polyimide high-temperature adhesive film between layers, heating to 300 ℃ by adopting a mould pressing heating curing method, preserving heat for 10 hours to finish the gluing molding of each functional layer of the composite material, and then cutting edges and finishing the dimensions to obtain the Ti-based composite material 3 C 2 T x High-temperature-resistant broadband wave-absorbing composite material with honeycomb sandwich structure of MXene aerogel.
The Ti-based alloy of this embodiment 3 C 2 T x High-temperature-resistant broadband wave-absorbing composite material with honeycomb sandwich structure of MXene aerogel, and overall density of composite material is 0.3g/cm 3 As can be seen from the graph of FIG. 4 showing the electromagnetic wave reflectivity at 1-18GHz, the high-temperature-resistant broadband wave-absorbing composite material with the honeycomb sandwich structure of the embodiment has the reflectivity of lower than-10 dB at 7.69-18.00 GHz and the reflectivity at 3.58-7.69 GHz<-9dB, excellent broadband wave-absorbing performance.
Example 2
Ti-based 3 C 2 T x As shown in FIG. 1, the high-temperature-resistant broadband wave-absorbing composite material with the honeycomb sandwich structure of the MXene aerogel is of a multi-layer structure, an electromagnetic wave incident direction is defined as the outer surface of the material, the composite material is sequentially composed of a high-temperature-resistant resin-based composite material wave-transmitting skin, a honeycomb structure wave-absorbing layer and a high-temperature-resistant resin-based composite material reflecting skin from outside to inside, and the high-temperature-resistant resin-based composite material wave-transmitting skin material is a quartz fiber reinforced polyimide resin-based composite material with the thickness of 1mm; the wave absorbing layer of the honeycomb structure is a composite material honeycomb structure filled with a high-temperature-resistant MXene composite aerogel material, and the high-temperature-resistant MXene composite aerogel material is Ti 3 C 2 T x MXene/SiO 2 Composite aerogel material having a directional pore structure and a density of 10mg/cm 3 ，Ti 3 C 2 T x MXene and SiO 2 The mass ratio is 4:1, the composite honeycomb structure is an aramid fiber reinforced polyimide composite honeycomb, the honeycomb holes are rectangular, the length is 10mm, the width is 5mm, the hole wall thickness is 0.5mm, and the honeycomb thickness is 5mm; the high-temperature resistant resin-based composite material reflection skin is a carbon fiber reinforced polyimide resin-based composite material, and the thickness is 2mm.
The Ti-based alloy of this embodiment 3 C 2 T x The preparation method of the high-temperature-resistant broadband wave-absorbing composite material with the honeycomb sandwich structure of the MXene aerogel comprises the following steps:
(1) Preparing a high-temperature-resistant resin matrix composite wave-transmitting skin: adopting high-temperature-resistant low-dielectric quartz fiber plain cloth to be regularly paved into 10 layers according to an alternating paving angle of 0 DEG and 90 DEG, adopting a vacuum bag assisted RTM method to finish polyimide resin dipping, carrying out mould pressing and heating to 300 ℃ and preserving heat for 5 hours to finish curing and forming, adopting linear cutting to cut a formed composite material flat plate into a transverse dimension of 300mm multiplied by 300mm, and adopting a grinding machine or manual grinding to grind the surface of the composite material to be smooth, thus obtaining a high-temperature-resistant resin matrix composite material wave-transparent skin with the thickness of 1mm;
(2) Preparing a composite material honeycomb structure filled with a high-temperature-resistant MXene composite aerogel material:
2.5g LiF is dissolved in 50mL 9mol/L concentrated hydrochloric acid to obtain a mixed etching agent of hydrochloric acid and lithium fluoride, and 2g of MAX phase TiAlC with 325 mesh particle size is added 2 The ceramic particles were added to 50mL of etchant, placed in a polytetrafluoroethylene beaker, and stirred at 3500r/min in a 50℃water bath for 24h. And then centrifugally collecting the etched solid powder precipitate to obtain the multilayer structure Ti 3 C 2 T x MXene particles;
dispersing the precipitate into 50mL deionized water, centrifuging at 3500r/min for 5min, collecting again to complete one time cleaning, and repeating the dispersing-centrifuging collecting process to obtain supernatant pH>6, or after centrifugation, the upper layer liquid is not transparent any more, namely, the washing link is completed; dispersing the precipitate into 50mL deionized water, sealing and isolating air from ultrasonic for 15min, centrifuging at 9000r/min for 1h, and collecting the upper liquid to obtain single-layer Ti 3 C 2 T x MXeneAdding proper amount of aqueous phase silica sol into the aqueous phase dispersion liquid of the nano-sheet, and uniformly stirring to obtain Ti with the concentration of 10mg/mL 3 C 2 T x MXene nanoplatelets and SiO 2 A mixed solution with a mass ratio of 4:1;
placing 300mm×300mm×5mm aramid fiber/polyimide composite honeycomb in a customized trough mold with metal bottom plate and sealed edge, pouring mixed solution until the honeycomb is just immersed, freezing the mold in a refrigerator with constant temperature of-18deg.C until the mixed solution in honeycomb holes is completely frozen, and placing into a cold well with temperature of-50deg.C and vacuum degree of 10 -5 Drying in a Pa freeze dryer for 7 days to obtain a composite material honeycomb structure filled with the high-temperature-resistant MXene composite aerogel material;
(3) Preparing a high-temperature-resistant resin-based composite material reflection skin: adopting carbon fiber plain cloth to be regularly paved into 10 layers according to alternating paving angles of 0 DEG and 90 DEG, adopting a vacuum bag assisted RTM method to finish polyimide resin dipping, carrying out mould pressing and heating to 300 ℃ and preserving heat for 5 hours to finish curing and forming, adopting linear cutting to cut a formed composite material flat plate into a size of 300mm multiplied by 300mm, and adopting a grinding machine or manual grinding to grind the surface of the composite material to be smooth, thus obtaining a 2mm thick high-temperature-resistant resin-based composite material reflection skin;
(4) Integral gluing of honeycomb sandwich structure composite material: the method comprises the steps of stacking a composite material honeycomb structure filled with a high-temperature-resistant resin-based composite material reflection skin, a high-temperature-resistant MXene composite aerogel material and a high-temperature-resistant resin-based composite material wave-transparent skin sequentially from bottom to top, using a 300 ℃ resistant polyimide high-temperature adhesive film between layers, heating to 280 ℃ by adopting a mould pressing heating curing method, preserving heat for 10 hours to finish the gluing molding of each functional layer of the composite material, and then cutting edges and finishing the dimensions to obtain the Ti-based composite material 3 C 2 T x High-temperature-resistant broadband wave-absorbing composite material with honeycomb sandwich structure of MXene aerogel.
The Ti-based alloy of this embodiment 3 C 2 T x High-temperature-resistant broadband wave-absorbing composite material with honeycomb sandwich structure of MXene aerogel, and overall density of composite material is 0.6g/cm 3 As can be seen from FIG. 5, the reflectivity of electromagnetic wave at 1-18GHz is shown in the bee of this embodimentThe high-temperature resistant broadband wave-absorbing composite material with the nest sandwich structure has the reflectivity lower than-10 dB at 6.85-18.00 GHz and excellent broadband wave-absorbing performance.
The foregoing descriptions of specific exemplary embodiments of the present invention are presented for purposes of illustration and description. It is not intended to limit the invention to the precise form disclosed, and obviously many modifications and variations are possible in light of the above teaching. The exemplary embodiments were chosen and described in order to explain the specific principles of the invention and its practical application to thereby enable one skilled in the art to make and utilize the invention in various exemplary embodiments and with various modifications as are suited to the particular use contemplated. It is intended that the scope of the invention be defined by the claims and their equivalents.

Claims (10)

1. Ti-based 3 C 2 T x The high-temperature-resistant broadband wave-absorbing composite material with the honeycomb sandwich structure of the MXene aerogel is characterized in that the high-temperature-resistant broadband wave-absorbing composite material with the honeycomb sandwich structure is of a multi-layer structure and sequentially comprises a high-temperature-resistant resin matrix composite material wave-transmitting skin, a honeycomb structure wave-absorbing layer and a high-temperature-resistant resin matrix composite material reflecting skin from outside to inside, and the honeycomb structure wave-absorbing layer is of a composite material honeycomb structure filled with the high-temperature-resistant MXene composite aerogel material.
2. Ti-based according to claim 1 3 C 2 T x The high-temperature-resistant broadband wave-absorbing composite material with the honeycomb sandwich structure of the MXene aerogel is characterized in that the high-temperature-resistant MXene composite aerogel material is Ti 3 C 2 T x MXene/SiO 2 Composite aerogel material with density of 5-15 mg/cm 3 ，Ti 3 C 2 T x MXene and SiO 2 The mass ratio is 1:4-4:1; the composite honeycomb structure is a quartz fiber or aramid fiber reinforced polyimide composite honeycomb, the thickness of the honeycomb is 5-10 mm, the shape of honeycomb holes is hexagonal, rectangular or triangular, the honeycomb Kong Bianchang is 2-10 mm, and the thickness of the hole wall is 0.2-0.5 mm.
3. Ti-based according to claim 1 3 C 2 T x The high-temperature-resistant broadband wave-absorbing composite material with the honeycomb sandwich structure of the MXene aerogel is characterized in that the wave-transmitting skin of the high-temperature-resistant resin-based composite material is a polyimide resin-based composite material reinforced by quartz fibers or aramid fibers, and the thickness of the composite material is 0.5-2 mm.
4. Ti-based according to claim 1 3 C 2 T x The high-temperature-resistant broadband wave-absorbing composite material with the honeycomb sandwich structure of the MXene aerogel is characterized in that the high-temperature-resistant resin-based composite material reflection skin is a carbon fiber reinforced polyimide resin-based composite material or a carbon fiber reinforced bismaleimide resin-based composite material, and the thickness is 0.5-2 mm.
5. Ti-based alloy according to any one of claims 1 to 4 3 C 2 T x The preparation method of the high-temperature-resistant broadband wave-absorbing composite material with the honeycomb sandwich structure of the MXene aerogel is characterized by comprising the following steps of:
(1) Preparing a high-temperature-resistant resin matrix composite wave-transmitting skin;
(2) Ti is mixed with 3 C 2 T x Uniformly stirring an aqueous phase dispersion liquid of the MXene two-dimensional nano material and aqueous phase silica sol to obtain a mixed solution, placing a fiber reinforced polyimide composite honeycomb in a mold, pouring the mixed solution until the honeycomb is just immersed, and obtaining a composite honeycomb structure filled with a high-temperature-resistant MXene composite aerogel material through freezing and vacuum freeze drying;
(3) Preparing a high-temperature-resistant resin-based composite material reflection skin;
(4) The method comprises the steps of sequentially stacking a high-temperature-resistant resin-based composite material reflection skin, a high-temperature-resistant MXene composite aerogel material filled composite material honeycomb structure and a high-temperature-resistant resin-based composite material wave-transparent skin from bottom to top, using a high-temperature adhesive film between layers, and performing adhesive bonding molding by adopting a compression molding, heating, curing and adhesive bonding method to obtain a Ti-based alloy material 3 C 2 T x MXThe honeycombed sandwich structure of ene aerogel is high temperature resistant and broadband to absorb the composite material.
6. The method according to claim 5, wherein Ti in the mixed solution 3 C 2 T x MXene and SiO 2 The total concentration is 5-15 mg/mL, ti 3 C 2 T x MXene and SiO 2 The concentration ratio of (2) is 1:4-4:1.
7. The method according to claim 5, wherein in the step (1), the preparation of the high-temperature-resistant resin-based composite material wave-transparent skin specifically comprises: and (3) alternately and orthogonally layering the fiber cloth according to 0 DEG and 90 DEG, wherein the fiber cloth is unidirectional fiber cloth or plain fiber cloth, polyimide resin impregnation is completed by adopting a vacuum bag assisted RTM method, and the molding, heating, curing and forming are carried out, wherein the curing and forming temperature is 280-300 ℃, and the curing time is 5-10 h.
8. The method according to claim 5, wherein in the step (2), ti is 3 C 2 T x The preparation method of the MXene two-dimensional nanomaterial aqueous dispersion liquid comprises the following steps: tiAlC of MAX phase etched by chemical etchant 2 Ceramic particles, obtaining layered structure Ti 3 C 2 T x MXene, and then cleaning and stripping to obtain Ti 3 C 2 T x An aqueous phase dispersion of an MXene two-dimensional nanomaterial; the chemical etchant is a mixed solution of acid and lithium fluoride, the ratio of the acid to the lithium fluoride is 10 mL:1-5 g, and the acid is hydrochloric acid or hydrofluoric acid; the freezing and solidifying method is to freeze by adopting liquid nitrogen or placed in a temperature-controllable semiconductor freezing on a refrigeration plate or directly in a refrigerator freezing environment.
9. The method according to claim 5, wherein in the step (3), the preparing of the high temperature resistant resin-based composite reflective skin is specifically: and (3) alternately and orthogonally layering carbon fiber cloth according to 0 DEG and 90 DEG, wherein the carbon fiber cloth is unidirectional fiber cloth or plain fiber cloth, polyimide resin impregnation is completed by adopting a vacuum bag-assisted RTM method, the molding temperature is 280-300 ℃, and the curing time is 5-10 h.
10. The method according to claim 5, wherein in the step (4), the high temperature adhesive film is a polyimide high temperature adhesive film with a temperature resistance of 300 ℃, a curing adhesive temperature of 280-300 ℃ and a curing time of 5-10 h.
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