CN118213114A - High-performance wave-absorbing cable - Google Patents

High-performance wave-absorbing cable Download PDF

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Publication number
CN118213114A
CN118213114A CN202410611283.7A CN202410611283A CN118213114A CN 118213114 A CN118213114 A CN 118213114A CN 202410611283 A CN202410611283 A CN 202410611283A CN 118213114 A CN118213114 A CN 118213114A
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China
Prior art keywords
wave
silicon carbide
titanium silicon
absorbing
laminated
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CN202410611283.7A
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Inventor
刘明
张朝阳
舒金表
王雷
陈阿龙
孔阳
郜春山
邓志吉
孔维生
吴望哲
王玮
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Zhejiang Dahua Technology Co Ltd
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Zhejiang Dahua Technology Co Ltd
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Priority to CN202410611283.7A priority Critical patent/CN118213114A/en
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Abstract

The application discloses a high-performance wave-absorbing cable. The high-performance wave absorbing cable includes: a circuit layer; the circuit comprises two wave-absorbing material layers, wherein the two wave-absorbing material layers are respectively arranged on two opposite sides of the circuit layer, the wave-absorbing material layers are prepared from wave-absorbing materials, the wave-absorbing materials are of laminated structures, a plurality of pore channels are formed between two adjacent layers in the laminated layers of the wave-absorbing materials, and the pore channels in the laminated layers are orderly arranged. The application solves the problem of radiation disturbance on the cable by doping the wave-absorbing material.

Description

High-performance wave-absorbing cable
Technical Field
The application relates to the technical field of electromagnetic compatibility, in particular to a high-performance wave-absorbing cable.
Background
Cables are elements and modules that connect the interior of an electronic device and are an essential component of an electronic device. In some cables, such as FFC and FPC cables, multi-track high-speed clock signals are used for transmitting differential signals such as RGB and MIPI, and these high-speed clock signals and other high-speed signals can transmit radiation disturbance inside the electronic device through the cables, which causes unstable operation inside the device and affects normal operation of the electronic device.
The statements made above merely serve to provide background information related to the present disclosure and may not necessarily constitute prior art.
Disclosure of Invention
The application mainly solves the technical problem of providing the high-performance wave-absorbing cable, which can solve the problem of radiation disturbance existing on the cable by doping the wave-absorbing material.
In order to solve the technical problems, the application adopts a technical scheme that: provided is a high-performance wave absorbing cable including: a circuit layer; the circuit comprises two wave-absorbing material layers, wherein the two wave-absorbing material layers are respectively arranged on two opposite sides of the circuit layer, the wave-absorbing material layers are prepared from wave-absorbing materials, the wave-absorbing materials are of laminated structures, a plurality of pore channels are formed between two adjacent layers in the laminated layers of the wave-absorbing materials, and the pore channels in the laminated layers are orderly arranged.
In order to solve the technical problems, the application adopts a technical scheme that: the preparation method of the high-performance wave-absorbing cable comprises the following steps: providing a wave-absorbing material and a circuit layer, wherein the wave-absorbing material is of a laminated structure, a plurality of pore channels are formed between two adjacent layers in the laminated structure of the wave-absorbing material, and the pore channels in the laminated structure are orderly arranged; and two wave-absorbing material layers are respectively prepared on two opposite sides of the circuit layer through the wave-absorbing material.
In order to solve the technical problems, the application adopts another technical scheme that: there is provided a device comprising the high performance wave absorbing cable described above.
The high-performance wave-absorbing cable provided by the application comprises a circuit layer and two wave-absorbing material layers, wherein the two wave-absorbing material layers are respectively arranged on two opposite sides of the circuit layer, the wave-absorbing material layers are prepared from wave-absorbing materials, the wave-absorbing materials are of laminated structures, a plurality of pore channels are formed between two adjacent layers in the laminated layers of the wave-absorbing materials, and the pore channels in the laminated layers are orderly arranged, namely the wave-absorbing material provided by the application has a laminated orderly pore channel structure. The wave-absorbing material is subjected to layering treatment (such as etching treatment) to form a laminated structure, a plurality of pore channels (namely cavities) are formed between two adjacent layers in the wave-absorbing material laminated layer, and the pore channels in the laminated layer are orderly arranged, so that electromagnetic waves are reflected and absorbed for a plurality of times in the laminated ordered pore channel structure, when the electromagnetic waves are injected into the wave-absorbing material layers made of the wave-absorbing material of the even laminated ordered pore channel structure, part of the electromagnetic waves are reflected back by the wave-absorbing material layers on the surface, so that the quantity of the electromagnetic waves entering the interior of an object is reduced, and two wave-absorbing material layers made of the wave-absorbing material of the even laminated ordered pore channel structure are respectively arranged on two opposite sides of a circuit layer, so that the electromagnetic waves radiated by the circuit layer can be subjected to wave-absorbing shielding, and the influence of the electromagnetic waves radiated by the circuit layer on electronic equipment is reduced, and the problem of radiation disturbance on a cable is solved; the electromagnetic compatibility stability inside the electronic equipment is improved, and the equipment abnormality problem caused by the electromagnetic compatibility problem of the equipment is reduced.
The foregoing description is only an overview of the present application, and is intended to be implemented in accordance with the teachings of the present application in order that the same may be more clearly understood and to make the same and other objects, features and advantages of the present application more readily apparent.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present application, the following description will briefly explain the drawings needed in the description of the embodiments, which are merely examples of the present application, and other drawings can be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic diagram of a high performance wave absorbing cable according to an embodiment of the present application;
FIG. 2 is a schematic view of the microstructure of a wave-absorbing material;
FIG. 3 is a schematic diagram of an ideal structure of a wave-absorbing material;
FIG. 4 is a schematic diagram of another embodiment of a high performance wave absorbing cable of the present application;
FIG. 5 is a schematic view of the microstructure of a uniformly laminated titanium silicon carbide of the present application;
FIG. 6 is a schematic representation of the puffed titanium silicon carbide of the present application;
FIG. 7 is a comparative schematic illustration of the shielding properties of a titanium silicon carbide modified material of the present application and a conventional titanium silicon carbide material;
FIG. 8 is a graph showing a comparison of the thermal conductivity of the titanium silicon carbide modified material of the present application and a conventional titanium silicon carbide material;
FIG. 9 is an electron microscope schematic of a titanium silicon carbide modified material prepared by the method of comparative example 1;
FIG. 10 is an electron microscope schematic of a titanium silicon carbide modified material made by the method of example 3;
FIG. 11 is a schematic view of the cable structure in comparative example 2;
FIG. 12 is a graphical representation of far field electromagnetic radiation test results of comparative example 2;
FIG. 13 is a schematic view of a high performance wave absorbing cable according to another embodiment of the present application;
FIG. 14 is a graphical representation of far field electromagnetic radiation test results of comparative example 3;
Fig. 15 is a schematic diagram of far field electromagnetic radiation test results of example 13.
Detailed Description
In order to make the objects, technical solutions and effects of the present application clearer and more specific, embodiments of the technical solutions of the present application will be described in detail below with reference to the accompanying drawings. The following examples are only for more clearly illustrating the technical aspects of the present application, and thus are merely examples, and are not intended to limit the scope of the present application.
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; the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the application; the terms "comprising" and "having" and any variations thereof in the description of the application and the claims and the description of the drawings above are intended to cover a non-exclusive inclusion.
In the description of embodiments of the present application, the technical terms "first," "second," and the like are used merely to distinguish between different objects and are not to be construed as indicating or implying a relative importance or implicitly indicating the number of technical features indicated, a particular order or a primary or secondary relationship. In the description of the embodiments of the present application, the term "plurality" means two or more (including two), and similarly, "plural sets" means two or more (including two), and "plural sheets" means two or more (including two), unless otherwise specifically defined.
Reference herein to "an embodiment" means that a particular feature, structure, or characteristic described in connection with the embodiment may be included in at least one embodiment of the application. The appearances of such phrases in various places in the specification are not necessarily all referring to the same embodiment, nor are separate or alternative embodiments mutually exclusive of other embodiments. Those of skill in the art will explicitly and implicitly appreciate that the embodiments described herein may be combined with other embodiments.
In the description of the embodiments of the present application, the term "and/or" is merely an association relationship describing an association object, and indicates that three relationships may exist, for example, a and/or B may indicate: a exists alone, A and B exist together, and B exists alone. In addition, the character "/" herein generally indicates that the front and rear associated objects are an "or" relationship.
Amounts, ratios, and other numerical values are presented herein in a range format. It is to be understood that such range format is used for convenience and brevity and should be interpreted flexibly to include not only the numerical values explicitly recited as the limits of the range, but also to include all the individual numerical values or sub-ranges encompassed within that range as if each numerical value and sub-range is explicitly recited.
All the steps of the present application may be performed sequentially, randomly, or in parallel, preferably sequentially, unless otherwise specified. For example, the method comprises steps (a) and (b), meaning that the method may comprise steps (a) and (b) performed sequentially, may comprise steps (b) and (a) performed sequentially, and may be performed simultaneously. For example, the method may further comprise step (c), meaning that step (c) may be added to the method in any order, e.g., the method may comprise steps (a), (b) and (c), may also comprise steps (a), (c) and (b), may also comprise steps (c), (a) and (b), etc.
Taking the cable as an FPC and an FFC cable as examples, the FPC and the FFC cable are made of flexible base materials, have good flexibility and bending performance, and can be used for connecting and transmitting signals. The FPC mainly refers to a flexible printed circuit having a double-layer structure and a multi-layer structure, and can be designed into various shapes, and the FFC refers to a planar flexible cable. PFC and FFC are elements and modules connected inside an electronic device, and are essential components of the electronic device.
The FFC and the FPC cable are used for transmitting differential signals such as RGB and MIPI, and the high-speed clock signals and other high-speed signals can transmit radiation disturbance through the FFC and the FPC cable in the electronic equipment, so that unstable operation in the equipment is caused, and normal operation of the electronic equipment is affected. The radiation disturbance problem existing on the cable can be directly solved by solving the shielding wave-absorbing problem of the FFC and FPC cable.
However, the traditional FFC and FPC cables basically have no shielding performance, and when the electromagnetic compatibility problem (namely the radiation disturbance problem) of transmission signals in the FFC and FPC cables is found, the radiation disturbance suppression of the cables is realized only by adding flat magnetic rings on the cables. And the FFC and FPC cables which are normally used at present can easily generate signal coupling in equipment, so that other signals which normally work are influenced, and the normal operation of electronic equipment is influenced.
Based on this, as shown in fig. 1, the present application proposes a high performance wave-absorbing cable 10, where the high performance wave-absorbing cable 10 includes a circuit layer 11 and two wave-absorbing material layers 12, the two wave-absorbing material layers 12 are respectively disposed on opposite sides of the circuit layer 11, where the raw materials for preparing the wave-absorbing material layers 12 include wave-absorbing materials, the wave-absorbing materials are in a laminated structure, a plurality of channels are formed between two adjacent layers in the laminated layer of the wave-absorbing materials, and the channels in the laminated layer are orderly arranged, that is, the wave-absorbing material of the present application has a laminated orderly channel structure. The wave-absorbing material is subjected to layering treatment (such as etching treatment) to form a laminated structure, and a plurality of pore channels (i.e. cavities) are formed between two adjacent layers in the laminated layer of the wave-absorbing material, as shown in fig. 2, the pore channels in the laminated layer are orderly arranged, so that electromagnetic waves are reflected and absorbed for a plurality of times in the laminated ordered pore channel structure, as shown in fig. 3, when the electromagnetic waves are injected into the wave-absorbing material layers 12 made of the wave-absorbing material of the even laminated ordered pore channel structure, part of the electromagnetic waves are reflected back by the surface wave-absorbing material layers 12, so that the quantity of the electromagnetic waves entering the inside of an object is reduced, and thus the two wave-absorbing material layers 12 made of the wave-absorbing material of the even laminated ordered pore channel structure are respectively arranged on two opposite sides of the circuit layer 11, and the electromagnetic waves radiated by the circuit layer 11 can be subjected to wave-absorbing shielding, so that the electromagnetic waves radiated by the circuit layer 11 can be reduced from affecting electronic equipment, and the radiation disturbance problem existing on the cable can be solved; the electromagnetic compatibility stability inside the electronic equipment is improved, and the equipment abnormality problem caused by the electromagnetic compatibility problem of the equipment is reduced.
The wave absorbing material may be MAX phase material or mxnes material with laminated ordered pore structure.
Illustratively, the wave-absorbing material may be Ti 3SiC2、Ti3AlC2、Ti2AlC、Ti2AlN、Zr2 SnC or Cr 2 GaN or the like having a stacked ordered pore structure.
Preferably, the wave absorbing material is Ti 3SiC2 with laminated ordered pore structure, wherein Ti 3SiC2 has the characteristics of metal, good heat conduction performance and electric conduction performance at normal temperature, relatively low vickers hardness and high elastic modulus; the alloy has ductility at normal temperature, can be processed like metal, and has plasticity at high temperature; meanwhile, the ceramic material has the properties of ceramic material, high yield strength, high melting point, high thermal stability and good oxidation resistance, and can keep high strength at high temperature, so that the wave-absorbing material has good heat dissipation performance and wave-absorbing performance, has good electromagnetic wave-absorbing shielding effect on different frequency bands, has excellent electromagnetic wave absorption performance at 30 Mhz-18 Ghz, and the Ti 3SiC2 wave-absorbing material with laminated ordered pore channel structure is improved by nearly 30dB compared with the conventional wave-absorbing performance.
More preferably, the pore canal in the laminated ordered pore canal structure is elliptical, the long axis of the pore canal is 200 nm-400 nm, and the short axis of the elliptical is 130 nm-210 nm, so that the size of the pore canal in the laminated ordered pore canal structure is relatively large, and the wave absorbing material can better reflect and absorb electromagnetic waves. Of course, in other embodiments, the cells in the stacked ordered cell structure may have other shapes such as circular, tapered, or cylindrical.
Optionally, the bending part in the laminated ordered pore canal structure is covalently bonded, so that the wave-absorbing material can form effective connection at the bending part, and can maintain good ordered pore canal form, so that the interface thermal resistance of the joint part is relatively smaller, the heat transfer effect is enhanced, and the good heat dissipation effect can be maintained.
In addition, the wave-absorbing material and/or the heat-dissipating material can be filled in the pore canal in the laminated ordered pore canal structure of the wave-absorbing material, so that the wave-absorbing performance and the heat-dissipating performance of the wave-absorbing material are improved.
In one implementation, as shown in fig. 4, the high performance wave-absorbing cable 10 may include a cable body a and a wave-absorbing material layer 12, wherein the cable body a is provided with a circuit layer 11 therein, the wave-absorbing material layer 12 is laminated on a surface of the cable body a, and thus the wave-absorbing material layers 12 laminated on the surface of the cable body a are respectively disposed on opposite sides of the circuit layer 11 in the cable body a.
Alternatively, the cable body a may be a flexible cable such as an FFC cable or an FPC cable. To ensure the flexibility of the wave-absorbing cable 10, the thickness of the wave-absorbing material layer 12 may be controlled to avoid the deterioration of the flexibility of the wave-absorbing cable 10 caused by the provision of the excessively thick wave-absorbing material layer 12, thereby affecting the normal use of the wave-absorbing cable 10, and alternatively, the thickness of the wave-absorbing material layer 12 may be 0.05mm to 0.10mm.
In this implementation, an insulating layer 13 may be disposed on a side of the wave-absorbing material layer 12 remote from the cable body a, so as to improve the security of the electronic device.
In another implementation, as shown in fig. 1, a high performance wave absorbing cable 10 may include a wire layer 11 and a wave absorbing material layer 12 to embed wave absorbing material within the cable.
Alternatively, the wave absorbing cable 10 may be flexible cable such as FFC cable or FPC cable, and the wave absorbing material layer 12 may be prepared by using the wave absorbing material of the present application and pressed on one side of the circuit layer 11 when the flexible cable such as FFC cable or FPC cable is prepared, so that the wave absorbing material may be built in the flexible cable such as FFC cable or FPC cable.
Alternatively, to ensure the safety of the wave-absorbing cable 10, the high-performance wave-absorbing cable 10 may include an insulating layer 13, and the insulating layer 13 may be disposed between the line layer 11 and the wave-absorbing material layer 12, or may be disposed on a side of the wave-absorbing material layer 12 away from the line layer 11.
The application also provides a preparation method of the high-performance wave-absorbing cable, which can comprise the following steps: providing a wave-absorbing material and a circuit layer, wherein the wave-absorbing material is of a laminated structure, a plurality of pore channels are formed between two adjacent layers in the laminated structure of the wave-absorbing material, and the pore channels in the laminated structure are orderly arranged; and two wave-absorbing material layers are respectively prepared on two opposite sides of the circuit layer through the wave-absorbing material.
In one implementation, a cable body may be provided; and preparing wave-absorbing material layers on two opposite sides of the provided cable body through wave-absorbing materials so as to obtain the wave-absorbing cable. The cable body may be a finished cable product provided by a manufacturer, which may include a wire layer and an insulating layer coating the wire layer.
Optionally, the thickness of the wave-absorbing material layer may be controlled to give consideration to both the shielding performance of the wave-absorbing material layer in the manufactured wave-absorbing cable and the flexibility of the wave-absorbing cable. Preferably, the thickness of the wave-absorbing material layer can be controlled within the range of 0.05 mm-0.10 mm, wherein the thicker the thickness is, the more effective the shielding performance of the cable is improved, but the thicker the wave-absorbing material layer is, the lower the flexibility of the cable is, and the smaller the thickness of the wave-absorbing material layer is, the shielding performance of the wave-absorbing material layer to the cable is affected.
In another implementation manner, the circuit layer can be prepared first, and then the wave-absorbing material layer is wrapped and arranged on the periphery of the prepared circuit layer, namely, the wave-absorbing material layers are arranged on the two opposite sides of the circuit layer, so that the wave-absorbing cable is obtained, and the wave-absorbing material layer is added in the process of preparing the cable, namely, the wave-absorbing material layer is built in the cable, so that the miniaturization of the prepared wave-absorbing cable can be facilitated.
Alternatively, the wave-absorbing material layers may be disposed on opposite sides of the radial direction of the line layer, so that the wave-absorbing material layers are disposed on the outer sides of the line layer along the current transmission path of the wave-absorbing cable, so that the radiated electromagnetic waves can be efficiently absorbed by the wave-absorbing material layers to minimize the surface radiation of the cable.
In the above implementation manner, the wave-absorbing material layer may be disposed on two opposite sides of the cable body/circuit layer in a hydraulic press-fit manner. In one embodiment, a wave-absorbing material, a solvent, and a coagulant may be mixed to obtain a wave-absorbing mixture; pressing the wave-absorbing mixture on two opposite sides of the cable body/circuit layer in a hydraulic mode; the wave-absorbing mixture pressed on opposite sides of the cable body/circuit layer is subjected to a solidification treatment, optionally after pressing, a cooling solidification treatment at normal temperature.
Alternatively, the coagulant may include a resin material or the like. For example, the coagulant may include an amino resin and/or a phenolic resin, and the like. Further, the coagulant is a product obtained by mixing phenolic resin, amino resin and water according to a ratio of 1:1:0.5, so that the wave-absorbing material can be effectively bonded by overcoming the brittle characteristic of the wave-absorbing material through the coagulant.
In other embodiments, the wave-absorbing compound may be printed on opposite sides of the cable body/wire layer by screen printing, and then the wave-absorbing compound printed on opposite sides of the cable body/wire layer may be solidified.
Preferably, in order to prevent the wave-absorbing cable from causing equipment damage in the use process, an insulating layer may be disposed on a side of the wave-absorbing material layer away from the circuit layer.
The wave-absorbing material may be provided before the step of providing the wave-absorbing material layers on opposite sides of the provided cable body.
Preferably, the wave-absorbing material is Ti 3SiC2 with a laminated ordered pore structure, has flexibility, light weight and thinness, does not influence the flexibility of FFC and FPC, does not influence the normal use of the wave-absorbing cable, has lower cost and is easy to be introduced in a large scale.
The preparation process of the Ti 3SiC2 with the laminated ordered pore structure can be as follows:
Providing a titanium silicon carbide raw material; etching the titanium silicon carbide raw material to obtain uniform laminated titanium silicon carbide as shown in figure 5; mixing the uniformly laminated titanium silicon carbide and a bulking agent to obtain a uniform mixture; the uniform mixture is placed in a reducing atmosphere and heated to 95-105 ℃ and kept for 0.3-1 h, then heated to 145-155 ℃ and kept for 0.5-1.5 h, and the titanium silicon carbide with a laminated ordered pore structure shown in figure 6 is obtained, wherein the laminated ordered pore structure of the titanium silicon carbide can be shown in figure 2. According to the preparation method, the titanium silicon carbide can be gradually expanded to form a laminated ordered pore structure by controlling the reaction time of the expansion reaction temperature of the uniformly laminated titanium silicon carbide and the temperature time maintained in the rising process, so that the cracking of the structure caused by the excessively high expansion speed of the titanium silicon carbide can be avoided, and the laminated ordered pore network morphology of the titanium silicon carbide can be maintained, so that the titanium silicon carbide with better wave absorbing performance and heat conducting performance can be prepared by the preparation method, and the wave absorbing material is obtained. Specifically, the temperature is kept at 100 ℃ for 30min to gradually expand, so that the phenomenon that the whole network is affected due to the fact that the structure is broken due to the fact that the expansion speed is too high is avoided; reacting for 1h at 150 ℃ to expand the mixture to an optimal state and maintain the morphological structure of the mixture.
In one embodiment, the uniformly laminated titanium silicon carbide can be uniformly dispersed in a solvent to obtain a uniformly laminated titanium silicon carbide solution; then adding a proper amount of bulking agent, stirring for a period of time, and drying at a preset temperature to obtain a uniform mixture. In order to improve the dispersing effect of the uniformly laminated titanium silicon carbide, the uniformly laminated titanium silicon carbide colloid dispersion liquid (namely the uniformly laminated titanium silicon carbide solution) can be obtained by adding the uniformly laminated titanium silicon carbide into a proper amount of solvent, stirring for a period of time at a preset rotating speed, and then performing ultrasonic dispersion for a period of time. In addition, the predetermined temperature is less than the decomposition temperature of the bulking agent, for example sodium bicarbonate, and the predetermined temperature may be less than 50 ℃. In other embodiments, the bulking agent may be n-butylamine, etc., without limitation.
Alternatively, the ratio of the bulking agent to the uniformly layered titanium silicon carbide may be within a range, for example, within the range of "1:1.5-1:3", and the degree of bulking of the titanium silicon carbide may be adjusted by adjusting the ratio of the bulking agent to the uniformly layered titanium silicon carbide so that the titanium silicon carbide has different shielding properties. It is preferable that the mass ratio between the swelling agent and the uniformly laminated titanium silicon carbide is 1:2, and as shown in FIG. 7, the titanium silicon carbide (i.e., uniformly laminated swelled Ti 3SiC2 shown in FIG. 7) prepared according to the ratio has excellent electromagnetic wave absorption performance at 30Mhz to 18Ghz, and the shielding performance of the uniformly laminated swelled Ti 3SiC2 composite magnetic material is improved by nearly 30dB, compared with the titanium silicon carbide in the non-swelled state (i.e., ordinary Ti 3SiC2 shown in FIG. 7) prepared without using the swelling agent.
In one specific example, 10g of the uniformly layered titanium silicon carbide powder may be added to 150ml of a 3:1 water and ethanol mixed solution, and uniformly stirred for 3 hours at 300 r/min. Then, uniformly laminating titanium silicon carbide colloid dispersion liquid is obtained through ultrasonic dispersion for 1 h; then, 5g of sodium bicarbonate was added and stirred uniformly at 300r/min for 1 hour, and dried at room temperature to obtain a uniform mixture of uniformly laminated titanium silicon carbide and sodium bicarbonate.
Alternatively, the reducing atmosphere during the puffing reduction treatment may be a hydrogen atmosphere, a nitrogen atmosphere, or the like, without limitation.
In addition, in order to enhance the puffing effect, the temperature rising rate may be controlled within a certain range, for example, within a temperature rising rate range of more than 2 ℃/min and less than 10 ℃/min. More preferably, the rate of temperature increase is 5℃per minute.
Alternatively, the titanium silicon carbide feedstock may be self-made or commercially available.
The titanium silicon carbide raw material can be prepared by taking carbon powder, titanium powder and silicon powder as raw materials through high-temperature sintering. In one embodiment, titanium powder, carbon powder and silicon powder can be placed into vacuum according to the mass fraction ratio of 10:2:3 for high-temperature sintering at 1500 ℃ through vacuum pressureless sintering, and the titanium silicon carbide raw material is obtained.
Optionally, etching is performed on the titanium silicon carbide raw material by adopting etching modes such as hydrofluoric acid etching, molten salt etching, electrochemical etching, ionic liquid etching and the like, so that the titanium silicon carbide is layered, and the etched titanium silicon carbide is of a uniform laminated structure, namely, the laminated structure of the etched titanium silicon carbide is of uniform spacing by controlling etching conditions.
Taking the molten salt method as an example, the etching treatment of the titanium silicon carbide may include: mixing the titanium silicon carbide raw material and halogenated salt, and then placing the mixture in a salt bed of the halogenated salt; and heating the salt bed and the titanium silicon carbide raw material in the salt bed to 1150-1200 ℃ at a heating rate of 150-200 ℃/h in vacuum, preserving heat for 2-4 h, cooling to 590-610 ℃, adding an etchant, reacting for 10 min-1 h, and cooling to room temperature to obtain the uniform laminated titanium silicon carbide. So, silicon atoms in the Ti 3SiC2 compound can not be etched by controlling the rising rate of the reaction temperature and the reaction time, and only three substances of Ti, si and C remained in the reaction are removed, so that the purity of titanium silicon carbide in the etched product is ensured to be about 89% -95%, and a large number of other derivatives can be avoided; and the layering is more obvious by controlling the rising rate of the reaction temperature and the reaction time, and the titanium silicon carbide is uniformly layered, so that the titanium silicon carbide with a uniform laminated structure is obtained by etching.
Wherein the halide salt may be at least one selected from sodium chloride, potassium chloride and the like, without limitation. The etchant may be one of Lewis acids (CuCl2、CoCl2、ZnCl2、FeCl3、NiCl2、AgCl、FeCl2、CdCl2, etc.). Specifically, in one example, etching the titanium silicon carbide may include: uniformly mixing titanium silicon carbide raw materials, sodium chloride and potassium chloride according to the ratio of 1:5:5, and placing the prepared mixed solution into a sodium chloride salt bed; and secondly, gradually increasing the temperature in vacuum, namely increasing the temperature at the speed of 150 ℃/h to 200 ℃/h, changing low-melting sodium chloride and other salts into liquid state along with the temperature increase, gradually layering titanium silicon carbide powder in vacuum, and reacting for 3 hours at 1200 ℃ to generate laminated titanium silicon carbide. And then FeCl 2 is added when the temperature is reduced by 600 ℃, etching reaction is carried out on the mixture and phases generated in molten salt, after 0.5h of reaction, cooling is carried out at normal temperature, after cooling to the room temperature, redundant salts are filtered out, and drying is carried out under vacuum, so that the uniform laminated titanium silicon carbide powder is finally obtained.
Preferably, after the titanium silicon carbide with the laminated ordered pore structure is obtained through the puffing reduction treatment, the following modification treatment can be further performed on the titanium silicon carbide to obtain the final wave-absorbing material. Optionally, polydopamine modification can be performed on the titanium silicon carbide with the laminated ordered pore structure to obtain polydopamine modified titanium silicon carbide, so that polydopamine and titanium silicon carbide are utilized to have similar open pore structures with high surface area and average interlayer spacing, covalent bonding between pore joints can be well maintained through polydopamine modification, covalent bonding at the pore joints of the titanium silicon carbide is not easy to break, stability of the pore joints of the microstructure of the titanium silicon carbide is improved, overall morphology and laminated ordered pore structure of the titanium silicon carbide can be well maintained through polydopamine modification, and influence on the laminated ordered pore structure of the titanium silicon carbide due to temperature and other environmental adjustment in the subsequent preparation process is prevented.
In the embodiment, the polydopamine monomer and the titanium silicon carbide can be mixed into a disperse phase, so that the polydopamine monomer is gradually increased and deposited on the surface of the titanium silicon carbide, and polydopamine modification on the titanium silicon carbide is realized. In one example, polydopamine monomers and titanium silicon carbide can be mixed into a disperse phase according to the mass ratio of 1:1-4:1, polydopamine monomers are gradually increased at 20-30 ℃ and deposited on the surface of the titanium silicon carbide, so that polydopamine modification on the titanium silicon carbide is realized.
The paraffin particles are filled in the pore canal of the titanium silicon carbide with the laminated ordered pore canal structure, and then the heat pressing densification treatment is carried out, so that the titanium silicon carbide modified material is obtained, and the heat conduction property of the titanium silicon carbide can be improved by filling the paraffin wax like heat conduction substances in the pore canal of the titanium silicon carbide, as shown in fig. 8, the heat conduction rate of the titanium silicon carbide modified material (namely the uniformly laminated expanded Ti 3SiC2 in fig. 8) of the embodiment is improved by about 30 percent compared with that of the common Ti 3SiC2, and the heat conduction rate of the titanium silicon carbide modified material is up to 6W/m 2/K; the paraffin particles are embedded in the pore canal, so that the titanium silicon carbide can also maintain the pore canal state under the condition of external pressure, the shrinkage of the pore canal volume during subsequent hot pressing can be avoided, the change of the pore canal state can be avoided, the laminated ordered pore canal structure of the uniform laminated titanium silicon carbide is reserved, the wave absorbing performance and the heat conducting performance of the titanium silicon carbide can be well maintained, and the powder interlayer of the uniform laminated expanded titanium silicon carbide is modified after the paraffin is melted, so that the continuous network structure of the uniform laminated expanded titanium silicon carbide is realized on a long scale.
Preferably, the paraffin particles have a size smaller than the size of the tunnel so that the paraffin particles can meet the requirements for entering the tunnel. Specifically, the length of the paraffin particles may be 400nm or less, and the width and height of the paraffin particles may be 210nm or less.
To increase the uniformity of the paraffin particle packing, the paraffin particles may be spherical particles. Of course, in other embodiments, the paraffin particles may also be conical particles, lamellar particles, or columnar particles, etc.
In a specific example, the steps of filling paraffin particles in the pore canal of the titanium silicon carbide with the laminated ordered pore canal structure, and performing hot pressing densification to obtain the titanium silicon carbide modified material may include: 10g of uniform lamination expanded titanium silicon carbide powder and 1 g-2 g of paraffin microspheres are taken, firstly, 10g of paraffin microspheres are heated to be gelatinous, then the uniform lamination expanded titanium silicon carbide powder is added and stirred continuously, specifically, the uniform lamination expanded titanium silicon carbide powder is self-assembled into polydopamine modified interlayer pore channels of the uniform lamination expanded titanium silicon carbide powder through the paraffin microspheres, the paraffin microspheres are modified among the uniform lamination expanded titanium silicon carbide powder layers after being melted, and finally, hot-pressing densification is carried out, so that the continuous network structure of the uniform lamination expanded titanium silicon carbide is realized on a long scale, and the interconnected porous structure of the uniform lamination titanium silicon carbide powder in the composite material is reserved.
The preparation process of the rest of the wave-absorbing material can refer to the preparation process of titanium silicon carbide, and the description is omitted here.
The advantageous effects of the present application are further illustrated below with reference to examples.
In order to make the technical problems, technical schemes and beneficial effects solved by the embodiments of the present application more clear, the following will be described in further detail with reference to the embodiments and the accompanying drawings. It will be apparent that the described embodiments are only some, but not all, embodiments of the application. The following description of at least one exemplary embodiment is merely illustrative in nature and is in no way intended to limit the application, its application, or uses. All other embodiments, which can be made by a person skilled in the art based on the embodiments of the application without any inventive effort, are intended to fall within the scope of the application.
1. The influence of the preparation method of the wave-absorbing material on the wave-absorbing property and the heat conductive property of the wave-absorbing material is described by comparative example 1 and examples 1 to 12.
Comparative example 1
Uniformly mixing titanium silicon carbide raw materials, sodium chloride and potassium chloride according to the ratio of 1:5:5, and placing the prepared mixed solution into a sodium chloride salt bed; and secondly, gradually raising the temperature in vacuum, specifically raising the temperature at a rate of 150 ℃ per hour, enabling low-melting sodium chloride and other salts to become liquid along with the temperature rise, gradually layering titanium silicon carbide powder in vacuum, and reacting for 3 hours at 1200 ℃ to generate laminated titanium silicon carbide. And then FeCl 2 is added when the temperature is reduced by 600 ℃, etching reaction is carried out on the mixture and phases generated in molten salt, after 0.5h of reaction, cooling is carried out at normal temperature, after cooling to the room temperature, redundant salts are filtered out, and drying is carried out under vacuum, so that the uniform laminated titanium silicon carbide powder is finally obtained.
10G of the uniformly laminated titanium silicon carbide powder was added to 150ml of a 3:1 mixed solution of water and ethanol, and stirred uniformly at 300r/min for 3 hours. Then, the uniform laminated titanium silicon carbide colloid dispersion liquid is obtained by ultrasonic dispersion for 1h. Then, 5g of sodium bicarbonate was added, and the mixture was stirred uniformly at 300r/min for 1 hour, and dried at room temperature to obtain a solid mixture of uniformly laminated titanium silicon carbide and sodium bicarbonate. The solid mixture is put into a reducing atmosphere of hydrogen and nitrogen for expansion reduction, and the temperature is gradually increased to 150 ℃ from room temperature during the expansion reduction, the temperature increasing rate is controlled to be 5 ℃ per minute, and the temperature is maintained at 150 ℃ for 1.5h; and (5) removing excessive sodium salt through filtration after subsequent cooling, and finally obtaining the titanium silicon carbide modified material. An electron microscopic image of the titanium silicon carbide modified material prepared by the method of this comparative example is shown in fig. 9.
Example 1
Uniformly mixing titanium silicon carbide raw materials, sodium chloride and potassium chloride according to the ratio of 1:5:5, and placing the prepared mixed solution into a sodium chloride salt bed; and secondly, gradually raising the temperature in vacuum, specifically raising the temperature at a rate of 150 ℃ per hour, enabling low-melting sodium chloride and other salts to become liquid along with the temperature rise, gradually layering titanium silicon carbide powder in vacuum, and reacting for 3 hours at 1200 ℃ to generate laminated titanium silicon carbide. And then FeCl 2 is added when the temperature is reduced by 600 ℃, etching reaction is carried out on the mixture and phases generated in molten salt, after 0.5h of reaction, cooling is carried out at normal temperature, after cooling to the room temperature, redundant salts are filtered out, and drying is carried out under vacuum, so that the uniform laminated titanium silicon carbide powder is finally obtained.
10G of the uniformly laminated titanium silicon carbide powder was added to 150ml of a 3:1 mixed solution of water and ethanol, and stirred uniformly at 300r/min for 3 hours. Then, the uniform laminated titanium silicon carbide colloid dispersion liquid is obtained by ultrasonic dispersion for 1 h. Then, 5g of sodium bicarbonate was added, and the mixture was stirred uniformly at 300r/min for 1 hour, and dried at room temperature to obtain a solid mixture of uniformly laminated titanium silicon carbide and sodium bicarbonate. The solid mixture is put into a reducing atmosphere of hydrogen and nitrogen for expansion reduction, the temperature is gradually increased to 150 ℃ from room temperature during the expansion reduction, the temperature increasing rate is controlled to be 5 ℃ per minute, the temperature is respectively kept at 100 ℃ for 30 minutes, and the temperature is maintained at 150 ℃ for 1h; and (5) removing excessive sodium salt through filtration after subsequent cooling, and finally obtaining the titanium silicon carbide modified material. An electron microscopic image of the titanium silicon carbide modified material prepared by the method of this comparative example is shown in fig. 2.
Example 2
Uniformly mixing titanium silicon carbide raw materials, sodium chloride and potassium chloride according to the ratio of 1:5:5, and placing the prepared mixed solution into a sodium chloride salt bed; and secondly, gradually raising the temperature in vacuum, specifically raising the temperature at a rate of 150 ℃ per hour, enabling low-melting sodium chloride and other salts to become liquid along with the temperature rise, gradually layering titanium silicon carbide powder in vacuum, and reacting for 3 hours at 1200 ℃ to generate laminated titanium silicon carbide. And then FeCl 2 is added when the temperature is reduced by 600 ℃, etching reaction is carried out on the mixture and phases generated in molten salt, after 0.5h of reaction, cooling is carried out at normal temperature, after cooling to the room temperature, redundant salts are filtered out, and drying is carried out under vacuum, so that the uniform laminated titanium silicon carbide powder is finally obtained.
10G of the uniformly laminated titanium silicon carbide powder was added to 150ml of a 3:1 mixed solution of water and ethanol, and stirred uniformly at 300r/min for 3 hours. Then, the uniform laminated titanium silicon carbide colloid dispersion liquid is obtained by ultrasonic dispersion for 1 h. Then, 5g of sodium bicarbonate was added, and the mixture was stirred uniformly at 300r/min for 1 hour, and dried at room temperature to obtain a solid mixture of uniformly laminated titanium silicon carbide and sodium bicarbonate. The solid mixture is put into a reducing atmosphere of hydrogen and nitrogen for expansion reduction, the temperature is gradually increased to 150 ℃ from room temperature during the expansion reduction, the temperature increasing rate is controlled to be 5 ℃ per minute, the temperature is respectively kept at 95 ℃ for 30 minutes, and the temperature is maintained at 150 ℃ for 1h; and (5) removing excessive sodium salt through filtration after subsequent cooling, and finally obtaining the titanium silicon carbide modified material.
Example 3
Uniformly mixing titanium silicon carbide raw materials, sodium chloride and potassium chloride according to the ratio of 1:5:5, and placing the prepared mixed solution into a sodium chloride salt bed; and secondly, gradually raising the temperature in vacuum, specifically raising the temperature at a rate of 150 ℃ per hour, enabling low-melting sodium chloride and other salts to become liquid along with the temperature rise, gradually layering titanium silicon carbide powder in vacuum, and reacting for 3 hours at 1200 ℃ to generate laminated titanium silicon carbide. And then FeCl 2 is added when the temperature is reduced by 600 ℃, etching reaction is carried out on the mixture and phases generated in molten salt, after 0.5h of reaction, cooling is carried out at normal temperature, after cooling to the room temperature, redundant salts are filtered out, and drying is carried out under vacuum, so that the uniform laminated titanium silicon carbide powder is finally obtained.
10G of the uniformly laminated titanium silicon carbide powder was added to 150ml of a 3:1 mixed solution of water and ethanol, and stirred uniformly at 300r/min for 3 hours. Then, the uniform laminated titanium silicon carbide colloid dispersion liquid is obtained by ultrasonic dispersion for 1 h. Then, 5g of sodium bicarbonate was added, and the mixture was stirred uniformly at 300r/min for 1 hour, and dried at room temperature to obtain a solid mixture of uniformly laminated titanium silicon carbide and sodium bicarbonate. The solid mixture is put into a reducing atmosphere of hydrogen and nitrogen for expansion reduction, the temperature is gradually increased to 150 ℃ from room temperature during the expansion reduction, the temperature increasing rate is controlled to be 5 ℃ per minute, the temperature is respectively kept at 100 ℃ for 1h, and the temperature is kept at 145 ℃ for 1h; and (5) removing excessive sodium salt through filtration after subsequent cooling, and finally obtaining the titanium silicon carbide modified material. An electron microscopic image of the titanium silicon carbide modified material prepared by the method of this example is shown in fig. 10.
Example 4
Uniformly mixing titanium silicon carbide raw materials, sodium chloride and potassium chloride according to the ratio of 1:5:5, and placing the prepared mixed solution into a sodium chloride salt bed; and secondly, gradually raising the temperature in vacuum, specifically raising the temperature at a rate of 150 ℃ per hour, enabling low-melting sodium chloride and other salts to become liquid along with the temperature rise, gradually layering titanium silicon carbide powder in vacuum, and reacting for 3 hours at 1200 ℃ to generate laminated titanium silicon carbide. And then FeCl 2 is added when the temperature is reduced by 600 ℃, etching reaction is carried out on the mixture and phases generated in molten salt, after 0.5h of reaction, cooling is carried out at normal temperature, after cooling to the room temperature, redundant salts are filtered out, and drying is carried out under vacuum, so that the uniform laminated titanium silicon carbide powder is finally obtained.
10G of the uniformly laminated titanium silicon carbide powder was added to 150ml of a 3:1 mixed solution of water and ethanol, and stirred uniformly at 300r/min for 3 hours. Then, the uniform laminated titanium silicon carbide colloid dispersion liquid is obtained by ultrasonic dispersion for 1 h. Then, 5g of sodium bicarbonate was added, and the mixture was stirred uniformly at 300r/min for 1 hour, and dried at room temperature to obtain a solid mixture of uniformly laminated titanium silicon carbide and sodium bicarbonate. The solid mixture is put into a reducing atmosphere of hydrogen and nitrogen for expansion reduction, the temperature is gradually increased to 150 ℃ from room temperature during the expansion reduction, the temperature increasing rate is controlled to be 5 ℃ per minute, the temperature is respectively kept at 105 ℃ for 1h, and the temperature is maintained at 150 ℃ for 1h; and (5) removing excessive sodium salt through filtration after subsequent cooling, and finally obtaining the titanium silicon carbide modified material.
Example 5
Uniformly mixing titanium silicon carbide raw materials, sodium chloride and potassium chloride according to the ratio of 1:5:5, and placing the prepared mixed solution into a sodium chloride salt bed; and secondly, gradually raising the temperature in vacuum, specifically raising the temperature at a rate of 150 ℃ per hour, enabling low-melting sodium chloride and other salts to become liquid along with the temperature rise, gradually layering titanium silicon carbide powder in vacuum, and reacting for 3 hours at 1200 ℃ to generate laminated titanium silicon carbide. And then FeCl 2 is added when the temperature is reduced by 600 ℃, etching reaction is carried out on the mixture and phases generated in molten salt, after 0.5h of reaction, cooling is carried out at normal temperature, after cooling to the room temperature, redundant salts are filtered out, and drying is carried out under vacuum, so that the uniform laminated titanium silicon carbide powder is finally obtained.
10G of the uniformly laminated titanium silicon carbide powder was added to 150ml of a 3:1 mixed solution of water and ethanol, and stirred uniformly at 300r/min for 3 hours. Then, the uniform laminated titanium silicon carbide colloid dispersion liquid is obtained by ultrasonic dispersion for 1 h. Then, 5g of sodium bicarbonate was added, and the mixture was stirred uniformly at 300r/min for 1 hour, and dried at room temperature to obtain a solid mixture of uniformly laminated titanium silicon carbide and sodium bicarbonate. The solid mixture is put into a reducing atmosphere of hydrogen and nitrogen for expansion reduction, the temperature is gradually increased to 150 ℃ from room temperature during the expansion reduction, the temperature increasing rate is controlled to be 5 ℃ per minute, the temperature is respectively kept at 100 ℃ for 1h, and the temperature is maintained at 155 ℃ for 0.5h; and (5) removing excessive sodium salt through filtration after subsequent cooling, and finally obtaining the titanium silicon carbide modified material.
Example 6
Uniformly mixing titanium silicon carbide raw materials, sodium chloride and potassium chloride according to the ratio of 1:5:5, and placing the prepared mixed solution into a sodium chloride salt bed; and secondly, gradually raising the temperature in vacuum, specifically raising the temperature at a rate of 150 ℃ per hour, enabling low-melting sodium chloride and other salts to become liquid along with the temperature rise, gradually layering titanium silicon carbide powder in vacuum, and reacting for 3 hours at 1200 ℃ to generate laminated titanium silicon carbide. And then FeCl 2 is added when the temperature is reduced by 600 ℃, etching reaction is carried out on the mixture and phases generated in molten salt, after 0.5h of reaction, cooling is carried out at normal temperature, after cooling to the room temperature, redundant salts are filtered out, and drying is carried out under vacuum, so that the uniform laminated titanium silicon carbide powder is finally obtained.
10G of the uniformly laminated titanium silicon carbide powder was added to 150ml of a 3:1 mixed solution of water and ethanol, and stirred uniformly at 300r/min for 3 hours. Then, the uniform laminated titanium silicon carbide colloid dispersion liquid is obtained by ultrasonic dispersion for 1 h. Then, 5g of sodium bicarbonate was added, and the mixture was stirred uniformly at 300r/min for 1 hour, and dried at room temperature to obtain a solid mixture of uniformly laminated titanium silicon carbide and sodium bicarbonate. The solid mixture is put into a reducing atmosphere of hydrogen and nitrogen for expansion reduction, the temperature is gradually increased to 150 ℃ from room temperature during the expansion reduction, the temperature increasing rate is controlled to be 10 ℃ per minute, the temperature is respectively kept at 100 ℃ for 30 minutes, and the temperature is maintained at 150 ℃ for 1h; and (5) removing excessive sodium salt through filtration after subsequent cooling, and finally obtaining the titanium silicon carbide modified material.
Example 7
Uniformly mixing titanium silicon carbide raw materials, sodium chloride and potassium chloride according to the ratio of 1:5:5, and placing the prepared mixed solution into a sodium chloride salt bed; and secondly, gradually raising the temperature in vacuum, specifically raising the temperature at the rate of 125 ℃ per hour, enabling low-melting sodium chloride and other salts to become liquid along with the temperature rise, gradually layering titanium silicon carbide powder in vacuum, and reacting for 3 hours at 1200 ℃ to generate laminated titanium silicon carbide. And then FeCl 2 is added when the temperature is reduced to 590 ℃, etching reaction is carried out on the mixture and a phase generated in molten salt, after 0.5h of reaction, cooling is carried out at normal temperature, after cooling to the room temperature, redundant salt is filtered out, and drying is carried out under vacuum, so that the uniform laminated titanium silicon carbide powder is finally obtained.
10G of the uniformly laminated titanium silicon carbide powder was added to 150ml of a 3:1 mixed solution of water and ethanol, and stirred uniformly at 300r/min for 3 hours. Then, the uniform laminated titanium silicon carbide colloid dispersion liquid is obtained by ultrasonic dispersion for 1 h. Then, 5g of sodium bicarbonate was added, and the mixture was stirred uniformly at 300r/min for 1 hour, and dried at room temperature to obtain a solid mixture of uniformly laminated titanium silicon carbide and sodium bicarbonate. The solid mixture is put into a reducing atmosphere of hydrogen and nitrogen for expansion reduction, the temperature is gradually increased to 150 ℃ from room temperature during the expansion reduction, the temperature increasing rate is controlled to be 5 ℃ per minute, the temperature is respectively kept at 100 ℃ for 30 minutes, and the temperature is maintained at 150 ℃ for 1h; and (5) removing excessive sodium salt through filtration after subsequent cooling, and finally obtaining the titanium silicon carbide modified material.
Example 8
Uniformly mixing titanium silicon carbide raw materials, sodium chloride and potassium chloride according to the ratio of 1:5:5, and placing the prepared mixed solution into a sodium chloride salt bed; and secondly, gradually raising the temperature in vacuum, specifically raising the temperature at the rate of 200 ℃ per hour, enabling low-melting sodium chloride and other salts to become liquid along with the temperature rise, gradually layering titanium silicon carbide powder in vacuum, and reacting for 3 hours at 1200 ℃ to generate laminated titanium silicon carbide. And then adding FeCl 2 when the temperature is reduced by 610 ℃, carrying out etching reaction with a phase generated in molten salt, cooling at normal temperature after 0.5h of reaction, filtering out redundant salt after cooling to the room temperature, and drying under vacuum to finally obtain the uniform laminated titanium silicon carbide powder.
10G of the uniformly laminated titanium silicon carbide powder was added to 150ml of a 3:1 mixed solution of water and ethanol, and stirred uniformly at 300r/min for 3 hours. Then, the uniform laminated titanium silicon carbide colloid dispersion liquid is obtained by ultrasonic dispersion for 1 h. Then, 5g of sodium bicarbonate was added, and the mixture was stirred uniformly at 300r/min for 1 hour, and dried at room temperature to obtain a solid mixture of uniformly laminated titanium silicon carbide and sodium bicarbonate. The solid mixture is put into a reducing atmosphere of hydrogen and nitrogen for expansion reduction, the temperature is gradually increased to 150 ℃ from room temperature during the expansion reduction, the temperature increasing rate is controlled to be 5 ℃ per minute, the temperature is respectively kept at 100 ℃ for 30 minutes, and the temperature is maintained at 150 ℃ for 1h; and (5) removing excessive sodium salt through filtration after subsequent cooling, and finally obtaining the titanium silicon carbide modified material.
Example 9
Uniformly mixing titanium silicon carbide raw materials, sodium chloride and potassium chloride according to the ratio of 1:5:5, and placing the prepared mixed solution into a sodium chloride salt bed; and secondly, gradually raising the temperature in vacuum, specifically raising the temperature at a rate of 150 ℃ per hour, enabling low-melting sodium chloride and other salts to become liquid along with the temperature rise, gradually layering titanium silicon carbide powder in vacuum, and reacting for 3 hours at 1200 ℃ to generate laminated titanium silicon carbide. And then FeCl 2 is added when the temperature is reduced by 600 ℃, etching reaction is carried out on the mixture and phases generated in molten salt, after 0.5h of reaction, cooling is carried out at normal temperature, after cooling to the room temperature, redundant salts are filtered out, and drying is carried out under vacuum, so that the uniform laminated titanium silicon carbide powder is finally obtained.
10G of the uniformly laminated titanium silicon carbide powder was added to 150ml of a 3:1 mixed solution of water and ethanol, and stirred uniformly at 300r/min for 3 hours. Then, the uniform laminated titanium silicon carbide colloid dispersion liquid is obtained by ultrasonic dispersion for 1 h. Then, 5g of sodium bicarbonate was added, and the mixture was stirred uniformly at 300r/min for 1 hour, and dried at room temperature to obtain a solid mixture of uniformly laminated titanium silicon carbide and sodium bicarbonate. The solid mixture is put into a reducing atmosphere of hydrogen and nitrogen for expansion reduction, the temperature is gradually increased to 150 ℃ from room temperature during the expansion reduction, the temperature increasing rate is controlled to be 5 ℃ per minute, the temperature is respectively kept at 100 ℃ for 30 minutes, and the temperature is maintained at 150 ℃ for 1h; and (5) removing redundant sodium salt through filtration after subsequent cooling, and finally obtaining the uniform lamination puffed titanium silicon carbide powder.
And modifying the titanium silicon carbide with the laminated ordered pore structure by polydopamine to obtain the titanium silicon carbide modified material.
Example 10
Uniformly mixing titanium silicon carbide raw materials, sodium chloride and potassium chloride according to the ratio of 1:5:5, and placing the prepared mixed solution into a sodium chloride salt bed; and secondly, gradually raising the temperature in vacuum, specifically raising the temperature at a rate of 150 ℃ per hour, enabling low-melting sodium chloride and other salts to become liquid along with the temperature rise, gradually layering titanium silicon carbide powder in vacuum, and reacting for 3 hours at 1200 ℃ to generate laminated titanium silicon carbide. And then FeCl 2 is added when the temperature is reduced by 600 ℃, etching reaction is carried out on the mixture and phases generated in molten salt, after 0.5h of reaction, cooling is carried out at normal temperature, after cooling to the room temperature, redundant salts are filtered out, and drying is carried out under vacuum, so that the uniform laminated titanium silicon carbide powder is finally obtained.
10G of the uniformly laminated titanium silicon carbide powder was added to 150ml of a 3:1 mixed solution of water and ethanol, and stirred uniformly at 300r/min for 3 hours. Then, the uniform laminated titanium silicon carbide colloid dispersion liquid is obtained by ultrasonic dispersion for 1 h. Then, 5g of sodium bicarbonate was added, and the mixture was stirred uniformly at 300r/min for 1 hour, and dried at room temperature to obtain a solid mixture of uniformly laminated titanium silicon carbide and sodium bicarbonate. The solid mixture is put into a reducing atmosphere of hydrogen and nitrogen for expansion reduction, the temperature is gradually increased to 150 ℃ from room temperature during the expansion reduction, the temperature increasing rate is controlled to be 5 ℃ per minute, the temperature is respectively kept at 100 ℃ for 30 minutes, and the temperature is maintained at 150 ℃ for 1h; and (5) removing redundant sodium salt through filtration after subsequent cooling, and finally obtaining the uniform lamination puffed titanium silicon carbide powder.
And modifying the polydopamine on the titanium silicon carbide with the laminated ordered pore structure to obtain polydopamine modified titanium silicon carbide.
Filling spherical paraffin particles with the particle size of 100nm into the polydopamine modified titanium silicon carbide, and performing hot-pressing densification treatment to obtain the titanium silicon carbide modified material.
Example 11
Uniformly mixing titanium silicon carbide raw materials, sodium chloride and potassium chloride according to the ratio of 1:5:5, and placing the prepared mixed solution into a sodium chloride salt bed; and secondly, gradually raising the temperature in vacuum, specifically raising the temperature at a rate of 150 ℃ per hour, enabling low-melting sodium chloride and other salts to become liquid along with the temperature rise, gradually layering titanium silicon carbide powder in vacuum, and reacting for 3 hours at 1200 ℃ to generate laminated titanium silicon carbide. And then FeCl 2 is added when the temperature is reduced by 600 ℃, etching reaction is carried out on the mixture and phases generated in molten salt, after 0.5h of reaction, cooling is carried out at normal temperature, after cooling to the room temperature, redundant salts are filtered out, and drying is carried out under vacuum, so that the uniform laminated titanium silicon carbide powder is finally obtained.
10G of the uniformly laminated titanium silicon carbide powder was added to 150ml of a 3:1 mixed solution of water and ethanol, and stirred uniformly at 300r/min for 3 hours. Then, the uniform laminated titanium silicon carbide colloid dispersion liquid is obtained by ultrasonic dispersion for 1 h. Then, 5g of sodium bicarbonate was added, and the mixture was stirred uniformly at 300r/min for 1 hour, and dried at room temperature to obtain a solid mixture of uniformly laminated titanium silicon carbide and sodium bicarbonate. The solid mixture is put into a reducing atmosphere of hydrogen and nitrogen for expansion reduction, the temperature is gradually increased to 150 ℃ from room temperature during the expansion reduction, the temperature increasing rate is controlled to be 5 ℃ per minute, the temperature is respectively kept at 100 ℃ for 30 minutes, and the temperature is maintained at 150 ℃ for 1h; and (5) removing redundant sodium salt through filtration after subsequent cooling, and finally obtaining the uniform lamination puffed titanium silicon carbide powder.
And modifying the polydopamine on the titanium silicon carbide with the laminated ordered pore structure to obtain polydopamine modified titanium silicon carbide.
Filling spherical paraffin particles with the particle size of 300nm into the polydopamine modified titanium silicon carbide, and performing hot-pressing densification treatment to obtain the titanium silicon carbide modified material.
Example 12
Uniformly mixing titanium silicon carbide raw materials, sodium chloride and potassium chloride according to the ratio of 1:5:5, and placing the prepared mixed solution into a sodium chloride salt bed; and secondly, gradually raising the temperature in vacuum, specifically raising the temperature at a rate of 150 ℃ per hour, enabling low-melting sodium chloride and other salts to become liquid along with the temperature rise, gradually layering titanium silicon carbide powder in vacuum, and reacting for 3 hours at 1200 ℃ to generate laminated titanium silicon carbide. And then FeCl 2 is added when the temperature is reduced by 600 ℃, etching reaction is carried out on the mixture and phases generated in molten salt, after 0.5h of reaction, cooling is carried out at normal temperature, after cooling to the room temperature, redundant salts are filtered out, and drying is carried out under vacuum, so that the uniform laminated titanium silicon carbide powder is finally obtained.
10G of the uniformly laminated titanium silicon carbide powder was added to 150ml of a 3:1 mixed solution of water and ethanol, and stirred uniformly at 300r/min for 3 hours. Then, the uniform laminated titanium silicon carbide colloid dispersion liquid is obtained by ultrasonic dispersion for 1 h. Then, 5g of sodium bicarbonate was added, and the mixture was stirred uniformly at 300r/min for 1 hour, and dried at room temperature to obtain a solid mixture of uniformly laminated titanium silicon carbide and sodium bicarbonate. The solid mixture is put into a reducing atmosphere of hydrogen and nitrogen for expansion reduction, the temperature is gradually increased to 150 ℃ from room temperature during the expansion reduction, the temperature increasing rate is controlled to be 5 ℃ per minute, the temperature is respectively kept at 100 ℃ for 30 minutes, and the temperature is maintained at 150 ℃ for 1h; and (5) removing redundant sodium salt through filtration after subsequent cooling, and finally obtaining the uniform lamination puffed titanium silicon carbide powder.
And modifying the polydopamine on the titanium silicon carbide with the laminated ordered pore structure to obtain polydopamine modified titanium silicon carbide.
Filling flaky paraffin particles with the particle size of 100nm into the polydopamine modified titanium silicon carbide, and performing hot-pressing densification to obtain the titanium silicon carbide modified material.
(1) Insertion loss test: reference GB/T32596, test absorption bandwidth and insertion loss;
(2) And (3) heat conduction rate test: referring to GB/T10294, the heat conduction rate is tested;
(3) The titanium silicon carbide modified materials prepared in the above comparative examples and examples were subjected to heat press treatment, and then the heat-press-treated materials were subjected to post-heat press insertion loss and post-heat press heat conduction rate measurement by using the above insertion loss test method and heat conduction rate test method.
Table 1 test parameter tables for each of examples and comparative examples
As can be seen from the data of table 1, the comparative examples and comparative example 1 can provide the wave-absorbing material with a stacked ordered cavity structure by controlling the appropriate swelling reduction temperature and reaction time; compared with the wave-absorbing material without the laminated ordered hole structure, the wave-absorbing material with the laminated ordered hole structure has excellent wave-absorbing performance and heat dissipation performance.
Further, as is clear from comparative examples 1 and 9, by modifying the wave-absorbing material with polydopamine, the wave-absorbing performance of the wave-absorbing material can be improved, and the influence of hot pressing on the wave-absorbing performance of the wave-absorbing material can be reduced.
As is clear from comparative examples 9 to 12, by filling the polydopamine-modified titanium silicon carbide material with paraffin particles, the heat radiation performance of the wave-absorbing material can be significantly improved, and the influence of hot pressing on the wave-absorbing performance of the wave-absorbing material can be further reduced.
2. The influence of different structures of the cable on the wave-absorbing shielding performance (wave-absorbing shielding bandwidth or insertion loss, etc.) and the heat conducting performance of the cable is demonstrated by comparative example 2, comparative example 3 and a plurality of examples.
Comparative example 2
As shown in fig. 11, the cable 20 includes an insulating layer 22, a wiring layer 21, and an insulating layer 22, which are laminated in this order. The far field electromagnetic radiation test results of the cable 20 are shown in fig. 12.
Comparative example 3
As shown in fig. 13, the wave-absorbing cable 10 includes an insulating layer 13, a wave-absorbing material layer 12, a wiring layer 11, a wave-absorbing material layer 12, and an insulating layer 13, which are laminated in this order. The wave-absorbing material in the wave-absorbing material layer 12 was the wave-absorbing material produced by the method described in comparative example 1. The far field electromagnetic radiation test results of the wave absorbing cable 10 are shown in fig. 14.
Example 13
As shown in fig. 13, the wave-absorbing cable 10 includes an insulating layer 13, a wave-absorbing material layer 12, a wiring layer 11, a wave-absorbing material layer 12, and an insulating layer 13, which are laminated in this order. The wave-absorbing material in the wave-absorbing material layer 12 was different from that in comparative example 3, specifically, the wave-absorbing material of the wave-absorbing material layer 12 was the wave-absorbing material produced by the method described in example 1 above, and the conditions of production methods, dimensions, and the like of the remaining layers were uniform. The test result of far field electromagnetic radiation of the wave absorbing cable 10 is shown in fig. 15. As can be seen from comparison of fig. 15 and fig. 12, and comparison of fig. 14 and fig. 12, by adding the wave-absorbing material layer 12, electromagnetic wave crosstalk inside the electronic device can be effectively suppressed, and electromagnetic radiation disturbance of the electronic device to the outside can be reduced. As can be seen from comparison between fig. 15 and fig. 14, the wave-absorbing cable prepared from the wave-absorbing material having the stacked ordered cavity structure can suppress electromagnetic wave crosstalk inside the electronic device, and can further reduce electromagnetic radiation disturbance of the electronic device to the outside, compared with the wave-absorbing material having no stacked ordered cavity structure.
Example 14
As shown in fig. 13, the wave-absorbing cable 10 includes an insulating layer 13, a wave-absorbing material layer 12, a wiring layer 11, a wave-absorbing material layer 12, and an insulating layer 13, which are laminated in this order. In comparison with example 13, the thickness of the wave-absorbing material layer 12 was different, and the conditions such as the preparation method and the size of the other layers were the same. Specifically, the thickness of the wave-absorbing material layer 12 of example 13 was 0.05mm. The thickness of the wave-absorbing material layer 12 of example 14 was 0.10mm.
The foregoing description is only of embodiments of the present application, and is not intended to limit the scope of the application, and all equivalent structures or equivalent processes using the descriptions and the drawings of the present application or directly or indirectly applied to other related technical fields are included in the scope of the present application.

Claims (10)

1. A high performance wave absorbing cable, the high performance wave absorbing cable comprising:
a circuit layer;
the circuit comprises two wave-absorbing material layers, wherein the two wave-absorbing material layers are respectively arranged on two opposite sides of the circuit layer, the wave-absorbing material layers are prepared from wave-absorbing materials, the wave-absorbing materials are of laminated structures, a plurality of pore channels are formed between two adjacent layers in the laminated layers of the wave-absorbing materials, and the pore channels in the laminated layers are orderly arranged.
2. The high performance wave absorbing cable of claim 1, wherein the channels in the wave absorbing material are elliptical-like;
Optionally, the major axis of the ellipse-like shape is 200 nm-400 nm, and the minor axis of the ellipse-like shape is 130 nm-210 nm.
3. The high performance wave absorbing cable of claim 1, wherein the wave absorbing material is covalently bonded at junctions between the channels.
4. The high performance wave absorbing cable of claim 1, wherein the wave absorbing material is titanium silicon carbide.
5. The high performance wave absorbing cable of claim 1, wherein the high performance wave absorbing cable comprises:
and the insulating layer is formed on one side of the wave-absorbing material layer away from the circuit layer.
6. The preparation method of the high-performance wave-absorbing cable is characterized by comprising the following steps of:
providing a wave-absorbing material and a circuit layer, wherein the wave-absorbing material is of a laminated structure, a plurality of pore channels are formed between two adjacent layers in the laminated structure of the wave-absorbing material, and the pore channels in the laminated structure are orderly arranged;
and two wave-absorbing material layers are respectively prepared on two opposite sides of the circuit layer through the wave-absorbing material.
7. The method of manufacturing according to claim 6, wherein the providing a wave-absorbing material comprises:
Providing a titanium silicon carbide raw material;
etching the titanium silicon carbide raw material to obtain uniform laminated titanium silicon carbide;
mixing the uniformly laminated titanium silicon carbide and a bulking agent to obtain a uniform mixture;
And placing the uniform mixture in a reducing atmosphere, heating to 95-105 ℃ and preserving heat for 0.3-1 h, and then heating to 145-155 ℃ and preserving heat for 0.5-1.5 h to obtain the titanium silicon carbide modified material.
8. The method of preparing according to claim 7, wherein said mixing said homogeneously layered titanium silicon carbide with a bulking agent to obtain a homogeneous mixture comprises:
Dispersing the uniformly laminated titanium silicon carbide in a solution to prepare a colloid dispersion liquid;
Adding sodium bicarbonate into the colloidal dispersion, stirring for a period of time, and drying to obtain the uniform mixture.
9. The method of claim 7, wherein the etching the titanium silicon carbide material to obtain a uniform stack of titanium silicon carbide comprises:
mixing the titanium silicon carbide raw material and halogenated salt, and then placing the mixture in a salt bed of the halogenated salt;
and heating the salt bed and the titanium silicon carbide raw material in the salt bed to 1150-1200 ℃ at a heating rate of 150-200 ℃/h in vacuum, preserving heat for 2-4 h, cooling to 590-610 ℃, adding an etchant, reacting for 10 min-1 h, and cooling to room temperature to obtain the uniform laminated titanium silicon carbide.
10. A device comprising the high performance wave absorbing cable of any one of claims 1 to 5.
CN202410611283.7A 2024-05-16 2024-05-16 High-performance wave-absorbing cable Pending CN118213114A (en)

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