CN110461137B - Three-dimensional foam type composite wave-absorbing material and preparation method thereof - Google Patents
Three-dimensional foam type composite wave-absorbing material and preparation method thereof Download PDFInfo
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- CN110461137B CN110461137B CN201910697871.6A CN201910697871A CN110461137B CN 110461137 B CN110461137 B CN 110461137B CN 201910697871 A CN201910697871 A CN 201910697871A CN 110461137 B CN110461137 B CN 110461137B
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- 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 provides a three-dimensional composite wave-absorbing material prepared through one-step reaction and a preparation method thereof, and magnetic Ni @ Ni with a three-dimensional skeleton structure is prepared through a one-step method3S2The composite material adjusts the ratio of the foam metal to the transition metal sulfide, and adjusts and controls the surface appearance and the electromagnetic parameters of the composite material to adapt to microwave absorption of different wave bands. The invention solves the defects of large density, narrow frequency band, poor impedance matching and the like of the traditional magnetic component in wave absorption, fully utilizes the structural advantages of porosity, light weight, high specific surface area of the foam metal, improves the impedance matching of the foam metal by the transition metal sulfide dielectric loss type material with adjustable and controllable surface, and has great practical application value in the production aspect of the electromagnetic wave absorbing material.
Description
Technical Field
The invention belongs to the technical field of composite materials and fine chemical engineering, and relates to a foam type composite wave-absorbing material prepared by a one-step method and a preparation method thereof.
Background
The rapid development of modern electronic technology provides great convenience for people's life and brings serious electromagnetic pollution. It is not only harmful to the health of people, but also poses a threat to the information security of electronic devices and the system stability of surrounding devices, and therefore, the development of high-performance electromagnetic absorbing materials is an effective way to solve the above problems.
In order to adapt to the integration of the air permeability and electronic components of the electromagnetic absorption device, the air permeable electromagnetic wave absorption material gradually becomes a new research hotspot. At present, the research on the use of porous foam metal for electromagnetic wave-absorbing materials is lacked, and the research on the functional application of the porous foam metal is necessary. The foam metal not only inherits the excellent conductivity or magnetism of the traditional blocky metal, but also has the advantages of light weight, large specific surface area, good air permeability and the like due to the existence of a large number of holes, and the three-dimensional communicated porous structure enables electromagnetic waves to generate multiple reflection and scattering loss when the electromagnetic waves enter the holes, so that the foam metal has excellent wave-absorbing performance within a certain wave band.
Transition Metal Sulfides (TMDs) have a 3 d-valent electron shell structure, have a band gap in the visible light range, and possess a two-dimensional layered structure similar to graphene, resulting in their anisotropy in electrical, chemical, mechanical, and thermal properties. At present, the research on the application of the transition metal sulfide to the electromagnetic wave absorption material is less, and researchers mainly concentrate on the application of the transition metal sulfide in the aspects of electro-catalysis, photocatalysis, lithium ion batteries and the like.
Disclosure of Invention
The technical problem solved by the invention is as follows: in order to avoid the defects of the prior art, the invention provides a three-dimensional composite wave-absorbing material prepared by one-step reaction and a preparation method thereof.
The technical scheme of the invention is as follows: a three-dimensional foam type composite wave-absorbing material comprises foam metal and transition metal, wherein the foam metal is used as a substrate, a transition metal sulfide is used as a load, and the foam metal and the transition metal sulfide can be prepared in different proportions; the mass fraction of the foam metal is 5-25%; the mass fraction of the transition metal sulfide is 75-95%.
The further technical scheme of the invention is as follows: the foam metal and the transition metal sulfide can be prepared according to molar mass ratios of 1:2, 1:2.5, 1:3 and 1:3.5 respectively.
The further technical scheme of the invention is as follows: the foam metal is a three-dimensional reticular framework with the pore diameter of between 200 and 400 mu m.
The further technical scheme of the invention is as follows: the foam metal is nickel foam, cobalt foam or copper foam.
The further technical scheme of the invention is as follows: the transition metal sulfide is cobalt disulfide, copper sulfide, nickel sulfide or nickel disulfide.
The further technical scheme of the invention is as follows: the molar mass ratio of the foam metal to the transition metal sulfide is 1:2, 1:2.5, 1:3, 1:3.5, and the sum of the mass fractions is one hundred percent.
The further technical scheme of the invention is as follows: a method for preparing the three-dimensional foam type composite wave-absorbing material of claim 1, comprising the following steps:
the method comprises the following steps: sequentially and alternately washing the foam metal material by using absolute ethyl alcohol with the volume concentration of 99.9% and ethyl acetate with the volume concentration of 99.9%, and ultrasonically cleaning the foam metal material in deionized water to remove surface impurities;
step two: dissolving a transition metal sulfide in deionized water to obtain a metal sulfide solution;
step three: and (3) transferring the foam metal material with impurities removed in the step one and the metal sulfide solution obtained in the step two into a hydrothermal reaction kettle, sealing the kettle, putting the hydrothermal reaction kettle into an oven, keeping the temperature at 240 ℃ for reacting for 18-24 hours, naturally cooling to room temperature, opening the kettle, filtering and washing for a plurality of times until the filtrate becomes colorless and transparent, and drying to obtain the foam metal loaded transition metal sulfide.
Effects of the invention
The invention has the technical effects that: the invention provides a three-dimensional composite wave-absorbing material prepared through one-step reaction and a preparation method thereof, and magnetic Ni @ Ni with a three-dimensional skeleton structure is prepared through a one-step method3S2The composite material adjusts and controls the surface appearance and electromagnetic parameters of the composite material by adjusting the proportion of the foam metal and the transition metal sulfide so as to adapt to microwave absorption of different wave bands. The invention solves the defects of large density, narrow frequency band, poor impedance matching and the like of the traditional magnetic component in wave absorption, fully utilizes the structural advantages of porosity, light weight, high specific surface area of the foam metal, improves the electromagnetic parameters of the foam metal by the transition metal sulfide dielectric loss type material with adjustable and controllable surface, and has great practical application value in the production aspect of the electromagnetic wave absorption material.
The invention aims to prepare the foam type composite wave-absorbing material by a one-step method, so as to simplify the traditional two-step method, overcome the defects of the traditional method, simplify the operation, improve the production efficiency, reduce the production cost, eliminate waste liquid and lay a foundation for the industrialization of the wave-absorbing material.
Drawings
FIG. 1: the prepared material has micro-morphology.
FIG. 2: XRD patterns of the prepared materials.
FIG. 3: the reflection loss performance of the composite material of the invention to electromagnetic waves.
Detailed Description
Referring to fig. 1-3, a three-dimensional foam composite wave-absorbing material prepared by a one-step method, which is prepared by using metal foam with a three-dimensional structure with adjustable morphology and different mixture ratios, wherein: the foam metal is used as a substrate to form a three-dimensional reticular framework, the loaded transition metal sulfide is prepared according to different molar mass ratios (1:2, 1:2.5, 1:3, 1:3.5), the ratio of the foam metal to the transition metal sulfide can be regulated, and the mass fraction of the foam metal is 5-25%; the mass fraction of the transition metal sulfide is 75-95%.
The foam metal is a three-dimensional reticular framework with the pore diameter of between 200 and 400 mu m.
The foam metal is nickel foam, cobalt foam or copper foam.
The transition metal sulfide is cobalt disulfide, copper sulfide, nickel sulfide or nickel disulfide.
A preparation method of a composite wave-absorbing material prepared by a one-step method is characterized by comprising the following steps:
step 1: and (3) respectively and alternately cleaning the foam metal material by using absolute ethyl alcohol with the volume concentration of 99.9% and ethyl acetate with the volume concentration of 99.9%, and ultrasonically cleaning in deionized water for 30min to remove surface impurities.
Step 2: and dissolving the transition metal sulfide in deionized water to obtain a metal sulfide solution.
And step 3: and (3) transferring the foam metal material without impurities in the step one and the metal sulfide solution obtained in the step two into a hydrothermal reaction kettle, sealing the kettle, putting the hydrothermal reaction kettle into an oven, keeping the temperature at 240 ℃ for reacting for 18-24 hours, naturally cooling to room temperature, opening the kettle, filtering and washing for a plurality of times until the filtrate becomes colorless and transparent, and drying to obtain the foam metal loaded transition metal sulfide.
The invention will now be further described with reference to the following examples and drawings:
the three-dimensional foam type composite wave-absorbing material comprises 5-25% of foam metal by mass, and then 75-95% of four transition metal sulfides with different shapes are loaded on the surface of the foam metal, and the mass ratio of the two components can be adjusted through the raw material ratio;
the foam metal is nickel foam, foam cobalt or foam copper;
the transition metal sulfide is cobalt disulfide, copper sulfide, nickel disulfide;
the transition metal sulfide size can reach nanometer and micron level respectively;
the foam metal is nickel foam, and the transition metal sulfide is Ni3S2Description of the drawings:
step 1: cutting the foam metal into a rectangular block of 1 × 5cm, alternately washing with 99.9 vol% absolute ethanol and 99.9 vol% ethyl acetate for three times (3 min each time), removing impurities, ultrasonically cleaning with deionized water for 30min, and drying at 100 deg.C for 2 hr;
step 2: dissolving 0.3g of thiourea in 160 ml of deionized water, and ultrasonically stirring for 30 min;
and step 3: and (3) transferring 0.6g of nickel foam and the solution to a polytetrafluoroethylene hydrothermal kettle, sealing the kettle, putting the kettle into an oven, reacting for 20 hours at 200 ℃, opening the kettle, washing with deionized water for several times, and drying for later use.
Example 1:
ultrasonically cleaning 0.6g of nickel foam by using absolute ethyl alcohol and ethyl acetate, drying for later use, dissolving 0.3g of thiourea in 160 ml of deionized water, ultrasonically stirring for 30min, transferring the nickel foam and the solution into a 200 ml of polytetrafluoroethylene hydrothermal reaction kettle, sealing the kettle, and reacting for 20 hours at 200 ℃; after the reaction is stopped, the system is automatically cooled to room temperature, the kettle is opened, the reaction product is repeatedly washed by deionized water, and the product is sealed and stored for later use after being dried at room temperature.
Example 2:
ultrasonically cleaning 0.6g of nickel foam by using absolute ethyl alcohol and ethyl acetate, drying for later use, dissolving 0.2g of thiourea in 160 ml of deionized water, ultrasonically stirring for 30min, transferring the nickel foam and the solution into a 200 ml of polytetrafluoroethylene hydrothermal reaction kettle, sealing the kettle, and reacting for 20 hours at 200 ℃; after the reaction is stopped, the system is automatically cooled to room temperature, the kettle is opened, the reaction product is repeatedly washed by deionized water, and the product is sealed and stored for later use after being dried at room temperature.
Example 3:
ultrasonically cleaning 0.6g of nickel foam by using absolute ethyl alcohol and ethyl acetate, drying for later use, dissolving 0.15g of thioacetamide in 160 ml of deionized water, ultrasonically stirring for 30min, transferring the nickel foam and the solution into a 200 ml of polytetrafluoroethylene hydrothermal reaction kettle, sealing the kettle, and reacting for 20 hours at 200 ℃; after the reaction is stopped, the system is automatically cooled to room temperature, the kettle is opened, the reaction product is repeatedly washed by deionized water, and the product is sealed and stored for later use after being dried at room temperature.
Example 4:
mixing the Ni @ Ni prepared above3S2Soaking the foam in liquid paraffin, solidifying, and trimming the foam/wax sample into cylindrical sample (phi)out＝7.0mm,Φin3.04) the foam to wax weight ratio was 1: 1. The cylindrical standard sample was subjected to a reflection loss test of an X-band electromagnetic wave using a vector analyzer (HP 8753D). The test results are shown in FIG. 3. The optimal reflection loss of the four foam metal loaded transition metal sulfides with the molar mass ratios of 1:2, 1:2.5, 1:3 and 1:3.5 respectively reaches-45.2 dB, -31.6dB, -50.7dB and-39.9 dB.
Claims (1)
1. A three-dimensional foam type composite wave-absorbing material is characterized by comprising foam metal and transition metal, wherein the foam metal is used as a substrate, and a transition metal sulfide is used as a load, and the foam metal and the transition metal sulfide can be prepared in different proportions; the mass fraction of the foam metal is 5-25%; the mass fraction of the transition metal sulfide is 75-95%; the foam metal and the transition metal sulfide can be respectively prepared according to the molar mass ratio of any one of 1:2, 1:2.5, 1:3 and 1: 3.5; meanwhile, the mass fraction is required to be one hundred percent; the foam metal is a three-dimensional reticular framework with the aperture of 200-400 mu m; the foam metal is foam nickel, foam cobalt or foam copper; the transition metal sulfide is cobalt disulfide, copper sulfide, nickel sulfide or nickel disulfide; the three-dimensional foam type composite wave-absorbing material is prepared by the following steps:
the method comprises the following steps: alternately washing the foam metal material by using absolute ethyl alcohol with the volume concentration of 99.9% and ethyl acetate with the volume concentration of 99.9%, removing surface impurities, ultrasonically cleaning the foam metal material in deionized water, and drying for later use;
step two: dissolving a transition metal sulfide in deionized water to obtain a transition metal sulfide solution;
step three: and (3) transferring the foam metal material with impurities removed in the step one and the transition metal sulfide solution obtained in the step two into a hydrothermal reaction kettle, sealing the kettle, putting the hydrothermal reaction kettle into an oven, keeping the temperature at 240 ℃ for reacting for 18-24 hours, naturally cooling to room temperature, opening the kettle, filtering and washing for a plurality of times until the filtrate becomes colorless and transparent, and drying to obtain the foam metal loaded transition metal sulfide.
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| CN111170761B (en) * | 2020-01-11 | 2021-12-28 | 西安交通大学 | Silicon carbide @ metal oxide wave-absorbing foam and preparation method thereof |
| CN114619724A (en) * | 2020-12-10 | 2022-06-14 | 南京航空航天大学 | High-temperature-resistant structure wave-absorbing composite material and preparation method thereof |
| CN112500832B (en) * | 2020-12-11 | 2023-04-18 | 西北工业大学 | Preparation method of foam nickel-based oxide composite wave-absorbing material |
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| WO2018125641A1 (en) * | 2016-12-28 | 2018-07-05 | Nanotek Instruments, Inc. | Flexible and shape-conformal rope-shape alkali metal batteries |
| CN108899222A (en) * | 2018-06-26 | 2018-11-27 | 中南大学 | A kind of preparation method of electrode material for super capacitor |
| CN109852344A (en) * | 2019-02-26 | 2019-06-07 | 广东工业大学 | A kind of composite wave-suction material and preparation method thereof |
| CN109943023A (en) * | 2019-04-08 | 2019-06-28 | 深圳先进技术研究院 | A kind of thermally conductive electromagnetic shielding composite material and its preparation method and application |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2018125641A1 (en) * | 2016-12-28 | 2018-07-05 | Nanotek Instruments, Inc. | Flexible and shape-conformal rope-shape alkali metal batteries |
| CN108899222A (en) * | 2018-06-26 | 2018-11-27 | 中南大学 | A kind of preparation method of electrode material for super capacitor |
| CN109852344A (en) * | 2019-02-26 | 2019-06-07 | 广东工业大学 | A kind of composite wave-suction material and preparation method thereof |
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