CN111850432B - Preparation method and application of composite material - Google Patents
Preparation method and application of composite material Download PDFInfo
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- CN111850432B CN111850432B CN201910348379.8A CN201910348379A CN111850432B CN 111850432 B CN111850432 B CN 111850432B CN 201910348379 A CN201910348379 A CN 201910348379A CN 111850432 B CN111850432 B CN 111850432B
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C47/00—Making alloys containing metallic or non-metallic fibres or filaments
- C22C47/02—Pretreatment of the fibres or filaments
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C47/00—Making alloys containing metallic or non-metallic fibres or filaments
- C22C47/14—Making alloys containing metallic or non-metallic fibres or filaments by powder metallurgy, i.e. by processing mixtures of metal powder and fibres or filaments
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C49/00—Alloys containing metallic or non-metallic fibres or filaments
- C22C49/02—Alloys containing metallic or non-metallic fibres or filaments characterised by the matrix material
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C49/00—Alloys containing metallic or non-metallic fibres or filaments
- C22C49/14—Alloys containing metallic or non-metallic fibres or filaments characterised by the fibres or filaments
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- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K9/00—Screening of apparatus or components against electric or magnetic fields
- H05K9/0073—Shielding materials
- H05K9/0081—Electromagnetic shielding materials, e.g. EMI, RFI shielding
Abstract
The invention discloses a preparation method of a composite material, which comprises the following steps: s1, preparing a loofah sponge carbon basic template; s2, preparing a graphene oxide dispersion liquid, and respectively adding a cationic polymer and FeSiAl alloy powder into the graphene oxide dispersion liquid to obtain a composite solution; s3, carrying out solvothermal reaction on the loofah sponge carbon basic template and the composite solution to obtain the composite material hydrogel, and cleaning and drying to obtain the composite material. The composite material is particularly suitable for the design of high-performance wave-absorbing materials, and has the remarkable characteristics of light weight, small density, good electromagnetic wave absorption performance and the like.
Description
[ technical field ] A method for producing a semiconductor device
The invention relates to the field of composite materials, in particular to a preparation method and application of a loofah sponge carbon/three-dimensional graphene/FeSiAl composite material.
[ background of the invention ]
Graphene has the remarkable characteristics of high temperature resistance, good flexibility, light weight, wide wave-absorbing frequency band, high thermal conductivity, multiple pores and the like, and has been widely applied to the fields of energy, electronics, electric power, heat conduction, communication and the like. The application research of graphene is a great hot spot at present, in the prior art, the graphene is used for an electromagnetic wave absorption or stealth structural member, and the wave-absorbing composite material is mainly prepared by blending the graphene, a wave-absorbing agent and matrix resin, but the wave-absorbing effect is not very ideal.
The three-dimensional graphene has many advantages of graphene, but the mechanical property is poor, the problem that the three-dimensional graphene prepared by the prior art is easy to crack is solved, the three-dimensional graphene material with a larger size is difficult to prepare, and the three-dimensional graphene is used for an electromagnetic wave absorption or stealth structural member, especially for high-end weaponry, and needs to have certain strength and size, so that the application of the three-dimensional graphene on the electromagnetic wave absorption or stealth structural member is limited.
[ summary of the invention ]
In order to solve the technical problem, the preparation method of the composite material comprises the following steps: s1, preparing a loofah sponge carbon basic template; s2, preparing a graphene oxide dispersion liquid, and respectively adding a cationic polymer and FeSiAl alloy powder into the graphene oxide dispersion liquid to obtain a composite solution; s3, carrying out solvothermal reaction on the loofah sponge carbon basic template and the composite solution to obtain loofah sponge carbon/three-dimensional graphene/FeSiAl composite material hydrogel, and cleaning and drying to obtain the composite material. According to the invention, firstly, a three-dimensional framework structure of the loofah sponge carbon is prepared, then, the three-dimensional framework structure is used as a basic template, and graphene adsorbed with FeSiAl alloy powder is subjected to self-loading reaction on the loofah sponge carbon three-dimensional framework by a hydrothermal reaction method to generate the loofah sponge carbon/three-dimensional graphene/FeSiAl composite material, so that the technical problem that the large-size graphene is easy to crack in the prior art is effectively solved; through the ultra-large specific surface area and the ultra-strong adsorption effect of the graphene oxide, the FeSiAl alloy powder is uniformly dispersed in the graphene oxide dispersion liquid, so that the uniform dispersion of the FeSiAl alloy powder in the composite material is facilitated. The composite material is particularly suitable for the design of high-performance wave-absorbing materials, and has the remarkable characteristics of light weight, small density and good microwave absorption performance.
In some embodiments of the present invention, the step S1 includes (1) soaking the loofah sponge charcoal in an alkaline solution for 2 to 48 hours, washing and drying, and then carbonizing in an inert atmosphere; (2) Soaking the loofah sponge carbon obtained in the step (1) in strong base with the concentration of 3-9 mol/L for 2-24 h, and cleaning and drying to obtain the loofah sponge carbon basic template.
In some embodiments of the present invention, the alkaline solution includes one or more of a sodium hydroxide solution, a potassium hydroxide solution, a calcium hydroxide solution, an ammonia water solution, and a sodium carbonate solution, the mass fraction of the solute in the alkaline solution is 20% to 50%, the solvent is a mixed solvent of deionized water and absolute ethyl alcohol, and the mass ratio of the deionized water to the absolute ethyl alcohol is 100. In the invention, the ethanol can adjust the content of free water in the system, reduce the size of a hydration layer, improve the penetration effect on fibers, improve the speed of alkali cellulose and increase the alkali adsorption quantity of the fibers, thereby leading the loofah sponge fibers to generate more active centers. After the alkali treatment, the lignin of the loofah sponge fiber is removed, so that the surface of the loofah sponge fiber becomes smooth, and meanwhile, a plurality of irregular holes are formed on the surface of the fiber, so that the internal structure of the fiber is exposed. The porous structure of the loofah sponge carbon and the surface structure characteristics (such as an active center and irregular holes) after alkali treatment are favorable for improving the capillary vessel force of the loofah sponge carbon fiber, the mixed solution of FeSiAl alloy and graphene oxide enters the pore channel of the loofah sponge carbon fiber, the mechanical property and the electromagnetic wave absorption property of the composite material are favorable for improving, the active center and the irregular holes in the loofah sponge carbon are favorable for the three-dimensional graphene to perform self-assembly reaction around the active structure, and the three-dimensional graphene is embedded into the pores of the fiber or wraps the active center to form physical winding and/or chemical bond connection, so that the interaction force between the three-dimensional graphene and the loofah sponge carbon is enhanced, and the mechanical property of the loofah sponge carbon/three-dimensional graphene/FeSiAl composite material is further favorable for improving.
In some embodiments of the present invention, the carbonization temperature in step S2 is 200 to 600 ℃, which can remove volatile matters in the loofah sponge, increase the content of fixed carbon, and make the loofah sponge skeleton have good mechanical strength after carbonization.
In some embodiments of the present invention, the concentration of the graphene oxide is 0.1mg/ml to 1mg/ml, the D50 of the graphene oxide in the graphene oxide solution is less than 4um, the monolayer rate of the graphene oxide is >90%, and the solid content is 0.5% to 3%.
In some embodiments of the invention, the graphene oxide: the cationic polymer is 100. For example, the cationic polymer may be one or more of cationic polyacrylamide, polyhexamethylene ammonium bromide, a quaternary ammonium salt of polyhydroxyethyl cellulose ether.
In some embodiments of the invention, the FeSiAl alloy powder has a D50 < 10um and a density of 3.4g/cm 3 The mass fraction of the graphene oxide is as follows: 5-20% of FeSiAl alloy powder: 1.
in some embodiments of the present invention, in step S3, the loofah sponge carbon basic template and the composite solution are subjected to a solvothermal reaction in a reaction kettle, wherein the reaction temperature of the solvothermal reaction is 100 ℃ to 200 ℃, the reaction pressure is 20MPa to 30MPa, and the reaction time is 1h to 24h. The FeSiAl alloy powder is adsorbed to obtain graphene oxide, the graphene oxide can perform self-assembly reaction on and in the loofah sponge carbon framework by virtue of solvothermal reaction in the reaction kettle, and meanwhile, the composite colloidal solution can be promoted to enter the modified loofah sponge fiber pore channel under the action of loofah sponge carbon capillary force by virtue of a high-temperature and high-pressure environment, so that the self-assembly reaction is performed in the fiber pore channel, the three-dimensional graphene is deeply inserted into the fiber pipeline, the physical entanglement of the loofah sponge carbon fiber framework and the three-dimensional graphene is effectively increased, and the mechanical property and the wave-absorbing property of the composite material are further provided.
The invention also discloses the loofah sponge carbon/three-dimensional graphene/FeSiAl composite material prepared by the preparation method or the preparation method.
The invention also discloses an application of the loofah sponge carbon/three-dimensional graphene/FeSiAl composite material in electromagnetic wave absorption or stealth design.
According to the preparation method of the composite material, the three-dimensional framework structure of the loofah sponge carbon is prepared, then the three-dimensional framework structure is used as a basic template, and the graphene oxide adsorbed with FeSiAl alloy powder is subjected to self-loading reaction on the loofah sponge carbon three-dimensional framework by a hydrothermal reaction method to generate the loofah sponge carbon/three-dimensional graphene/FeSiAl composite material, so that the problem that the large-size graphene is easy to crack in the prior art is effectively solved; the FeSiAl alloy powder is dispersed in the graphene oxide dispersion liquid through the ultra-large specific surface area and the ultra-strong adsorption effect of the graphene oxide, and then the three-dimensional graphene mixed with the FeSiAl alloy powder is obtained through the autonomous reaction of the graphene oxide under certain conditions, so that the uniform dispersion of the FeSiAl alloy powder in the composite material is facilitated. The loofah sponge carbon/three-dimensional graphene/FeSiAl composite material is particularly suitable for designing high-performance wave-absorbing materials, and has the remarkable characteristics of light weight, low density and good microwave absorption performance.
[ description of the drawings ]
FIG. 1 is a process flow diagram of a method of making a composite material of the present invention;
fig. 2 is a graph of the reflection curves of samples 1-3 versus untreated graphene at different frequencies.
[ detailed description ] embodiments
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and do not limit the invention.
Example 1
S1: soaking the loofah sponge in a sodium hydroxide solution for 24 hours, wherein the mass fraction of sodium hydroxide is 20%, the solvent is a mixed solvent of deionized water and absolute ethyl alcohol, the mass ratio of the deionized water to the absolute ethyl alcohol is 100; (2) Soaking the loofah sponge carbon obtained in the step (1) in a sodium hydroxide solution with the concentration of 9mol/L for 8 hours, and cleaning and drying to obtain a loofah sponge carbon basic template; s2, preparing a graphene oxide dispersion liquid by a hummers method, wherein the concentration of graphene oxide is 0.1mg/ml, the D50 of the graphene oxide in the graphene oxide solution is less than 4um, the single-layer rate of the graphene oxide is more than 90%, and the solid content is 0.5% -3%, and then respectively adding a cationic polymer and FeSiAl alloy powder into the graphene oxide dispersion liquid to obtain a composite solution, wherein the mass ratio of the graphene oxide to the cationic polymer is 100: 1; s3, adding the loofah sponge carbon basic template and the composite solution into a reaction kettle, carrying out solvothermal reaction for 6 hours at the temperature of 150 ℃ and under the pressure of 20MPa to obtain loofah sponge carbon/three-dimensional graphene/FeSiAl composite hydrogel, and cleaning and drying to obtain the composite material, namely the sample 1.
Example 2
S1: soaking the loofah sponge in a sodium hydroxide solution for 24 hours, wherein the mass fraction of sodium hydroxide is 50%, the solvent is a mixed solvent of deionized water and absolute ethyl alcohol, the mass ratio of the deionized water to the absolute ethyl alcohol is 100; (2) Soaking the loofah sponge carbon obtained in the step (1) in a sodium hydroxide solution with the concentration of 3mol/L for 8 hours, and cleaning and drying to obtain a loofah sponge carbon basic template; s2, preparing a graphene oxide dispersion liquid by a hummers method, wherein the concentration of graphene oxide is 1mg/ml, the D50 of the graphene oxide in the graphene oxide solution is less than 4um, the single-layer rate of the graphene oxide is greater than 90%, and the solid content is 0.5% -3%, and then respectively adding a cationic polymer and FeSiAl alloy powder into the graphene oxide dispersion liquid to obtain a composite solution, wherein the mass ratio of the graphene oxide to the cationic polymer is 100; s3, adding the loofah sponge carbon basic template and the composite solution into a reaction kettle, carrying out solvothermal reaction for 6 hours at 150 ℃ under the pressure of 25MPa to obtain loofah sponge carbon/three-dimensional graphene/FeSiAl composite hydrogel, and cleaning and drying to obtain the composite material, namely the sample 2, disclosed by the invention.
Example 3
S1: soaking the loofah sponge in a sodium hydroxide solution for 24 hours, wherein the mass fraction of sodium hydroxide is 40%, the solvent is a mixed solvent of deionized water and absolute ethyl alcohol, the mass ratio of the deionized water to the absolute ethyl alcohol is 100; (2) Soaking the loofah sponge carbon obtained in the step (1) in a sodium hydroxide solution with the concentration of 6mol/L for 8 hours, and cleaning and drying to obtain a loofah sponge carbon basic template; s2, preparing a graphene oxide dispersion liquid by a hummers method, wherein the concentration of graphene oxide is 0.6mg/ml, the D50 of the graphene oxide in the graphene oxide solution is less than 4um, the single-layer rate of the graphene oxide is more than 90%, and the solid content is 0.5% -3%, and then respectively adding a cationic polymer and FeSiAl alloy powder into the graphene oxide dispersion liquid to obtain a composite solution, wherein the mass ratio of the graphene oxide to the cationic polymer is 100; s3, adding the loofah sponge carbon basic template and the composite solution into a reaction kettle, carrying out solvothermal reaction for 6 hours at the temperature of 150 ℃ and under the pressure of 28MPa to obtain loofah sponge carbon/three-dimensional graphene/FeSiAl composite hydrogel, and cleaning and drying to obtain the composite material, namely the sample 3.
Comparative example 1
Preparing a graphene oxide aqueous solution with the concentration of 1mg/ml by a hummer method for later use; adding ascorbic acid into a graphene oxide aqueous solution to obtain a reaction solution, wherein the mass ratio of the graphene oxide aqueous solution to the ascorbic acid is 1:5, carrying out self-assembly reaction at 55 ℃ to obtain a three-dimensional graphene hydrogel, cleaning, and freeze-drying to obtain the three-dimensional graphene which is not modified, namely the unprocessed graphene.
The three-dimensional graphene composite materials obtained in examples 1 to 3 and comparative example 1 were cut into flat pieces of sizes 180mm by 10mm, and the cut pieces were placed in a microwave dark room to test reflectivity curves of 2 to 18GHz, and the results are shown in fig. 2. As can be seen from FIG. 2, the loofah sponge carbon/three-dimensional graphene/FeSiA composite material has a large absorption bandwidth in the 2-18GHz wave band range and has broadband wave-absorbing characteristics, wherein the maximum absorption intensity of the sample 1 reaches-18 dB, the maximum absorption intensity of the sample 2 reaches-35.5 dB, and the maximum absorption intensity of the sample 3 reaches-27 dB. According to test data, the composite material has the characteristics of wide absorption frequency band and good wave absorption efficiency.
In the above embodiments, the present invention has been described only exemplarily, but those skilled in the art, after reading the present patent application, can make various modifications to the present invention without departing from the spirit and scope of the present invention.
Claims (8)
1. A method for preparing a composite material, comprising the steps of:
s1, preparing a loofah sponge carbon three-dimensional basic template;
s2, preparing a graphene oxide dispersion liquid, and respectively adding a cationic polymer and FeSiAl alloy powder into the graphene oxide dispersion liquid to obtain a composite solution;
s3, carrying out solvothermal reaction on the loofah sponge carbon three-dimensional base template and the composite solution to obtain loofah sponge carbon/three-dimensional graphene/FeSiAl composite material hydrogel, and cleaning and drying to obtain the composite material;
the step S1 comprises (1) soaking the loofah sponge in an alkaline solution for 2-48 h, cleaning and drying, and then carbonizing in an inert atmosphere; (2) Soaking the loofah sponge carbon obtained in the step (1) in a strong alkali solution with the concentration of 3-9 mol/L for 2-24 h, and cleaning and drying to obtain a loofah sponge carbon basic template;
wherein, by mass fraction, the graphene oxide: the cationic polymer is 100: 5-20% of FeSiAl alloy powder: 1.
2. the preparation method according to claim 1, wherein the alkaline solution comprises one or more of a sodium hydroxide solution, a potassium hydroxide solution and a calcium hydroxide solution, the mass fraction of the solute in the alkaline solution is 20% to 50%, and the solvent is a mixed solution of deionized water and absolute ethyl alcohol, wherein the mass ratio of the deionized water to the absolute ethyl alcohol is 100.
3. The method according to claim 1, wherein the carbonization temperature in the step S1 is 200 to 600 ℃.
4. The preparation method of claim 1, wherein the concentration of the graphene oxide is 0.1mg/ml to 1mg/ml, the D50 of the graphene oxide in the graphene oxide solution is less than 4um, the monolayer rate of the graphene oxide is greater than 90%, and the solid content is 0.5% to 3%.
5. The method according to claim 1, wherein the FeSiAl alloy powder has a D50 of less than 10um and a density of 3.4g/cm 3 。
6. The preparation method of claim 1, wherein the step S3 comprises the steps of reacting at a temperature of 150-200 ℃, at a pressure of 20-30 MPa, and for a period of 1-24 h.
7. The loofah sponge carbon/three-dimensional graphene/FeSiAl composite material obtained by the preparation method according to any one of claims 1 to 6.
8. Use of the composite material of claim 7 for electromagnetic wave absorption or stealth design.
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| CN112911919A (en) * | 2021-02-04 | 2021-06-04 | 四川大学 | Carbonized loofah sponge/nano nickel/rGO electromagnetic shielding material and preparation method thereof |
| CN113340153A (en) * | 2021-05-20 | 2021-09-03 | 西北工业大学 | Infrared-radar compatible stealth material based on raw wood and preparation method |
| CN113278400B (en) * | 2021-07-13 | 2021-09-24 | 信维通信（江苏）有限公司 | Graphene foam composite wave-absorbing material and preparation method thereof |
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| CN108252081B (en) * | 2018-01-03 | 2020-06-16 | 江苏理工学院 | Preparation method and application of loofah sponge/carbon-based nanoparticle synergistically modified polymer conductive composite material |
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