CN110461137A - A kind of three-dimensional foam type composite wave-suction material and preparation method thereof - Google Patents

A kind of three-dimensional foam type composite wave-suction material and preparation method thereof Download PDF

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Publication number
CN110461137A
CN110461137A CN201910697871.6A CN201910697871A CN110461137A CN 110461137 A CN110461137 A CN 110461137A CN 201910697871 A CN201910697871 A CN 201910697871A CN 110461137 A CN110461137 A CN 110461137A
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foam
metal
type composite
composite wave
sulfide
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CN201910697871.6A
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CN110461137B (en
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王汝敏
郑远
雷博
张卫东
朱庆
齐暑华
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Northwest University of Technology
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Northwest University of Technology
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    • HELECTRICITY
    • H05ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05KPRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
    • H05K9/00Screening of apparatus or components against electric or magnetic fields
    • H05K9/0073Shielding materials
    • H05K9/0081Electromagnetic shielding materials, e.g. EMI, RFI shielding

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  • Physics & Mathematics (AREA)
  • Electromagnetism (AREA)
  • Engineering & Computer Science (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)
  • Laminated Bodies (AREA)

Abstract

A kind of three-dimensional composite wave-suction material prepared by single step reaction proposed by the present invention and preparation method, the magnetic Ni@Ni of three dimensional skeletal structure is prepared for by one-step method3S2Composite material regulates and controls surface topography and the electromagnetic parameter of composite material by adjusting the ratio of foam metal and transient metal sulfide to adapt to the microwave absorption of different-waveband.The present invention solves the disadvantages of big traditional magnetic component density for showing in inhaling wave, narrow frequency range, impedance matching is poor, take full advantage of that foam metal is porous, lightweight is high, the structural advantage of specific surface area, the regulatable transient metal sulfide dielectric loss profile material in surface improves the impedance matching of foam metal, and there is huge practical application values in terms of electromagnetic wave absorbent material production.

Description

A kind of three-dimensional foam type composite wave-suction material and preparation method thereof
Technical field
The invention belongs to composite materials and technical field of fine, and it is multiple to be related to a kind of foam type prepared by one-step method Close absorbing material and preparation method.
Background technique
The rapid development of modern electronic technology is provided a great convenience to people's lives, while also being brought serious Electromagnetic pollution.It not only endangers the health of people, also to the system stability of the information security of electronic equipment and surrounding devices It constitutes a threat to, therefore, developing high performance electromagnetic absorber is the effective way to solve the above problems.
For adapt to electromagnetic absorption device gas permeability and electronic component it is integrated, vapor-permeable type electromagnetic wave absorption absorbing material by Gradually become new research hotspot.And the domestic research for porous foam metal for electromagnetic-wave absorbent at present more lacks, It is necessary to the functional application research of system is carried out to it.Foam metal not only inherits the excellent electric conductivity of Traditional bulk metal Or it is magnetic, and due to there are a large amount of hole, the advantages that but also with lightweight, large specific surface area and good permeability, and three The porous structure of dimension connection make electromagnetic wave incident into hole when generate multiple reflections and scattering loss, have in certain wave band There is excellent absorbing property.
Transient metal sulfide (TMDs) has 3d valence electron shell structurre, there is visible-range band gap, possesses and graphite Two-dimensional layered structure as alkenes results in their anisotropy on electricity, chemistry, mechanics and thermal property.And it is current Less applied to electromagnetic wave absorbent material research for transient metal sulfide, researcher mainly concentrates transient metal sulfide Electro-catalysis, photocatalysis, in terms of application.
Summary of the invention
Technical problem solved by the present invention is in order to avoid the shortcomings of the prior art, the present invention proposes that one kind passes through The three-dimensional composite wave-suction material and preparation method of single step reaction preparation.
The technical scheme is that a kind of three-dimensional foam type composite wave-suction material, including foam metal and transition metal, Wherein foam metal can be deployed as substrate, transient metal sulfide as load, the two by different proportion;Foam Metal quality score is 5-25%;The mass fraction of transient metal sulfide is 75-95%.
A further technical solution of the present invention is: the foam metal and transient metal sulfide can pass through 1:2 respectively, The molal weight ratio of 1:2.5,1:3,1:3.5 are deployed.
A further technical solution of the present invention is: the foam metal be three-dimensional netted skeleton, aperture be 200-400 μm it Between.
A further technical solution of the present invention is: the foam metal is nickel foam, foam cobalt or foam copper.
A further technical solution of the present invention is: the transient metal sulfide be cobalt disulfide, copper sulfide, nickel sulfide or Vulcanize three nickel.
A further technical solution of the present invention is: the molal weight ratio of the foam metal and transient metal sulfide is 1:2,1:2.5,1:3,1:3.5, while needing satisfaction to add up mass fraction is absolutely.
A further technical solution of the present invention is: a kind of prepare three-dimensional foam type composite wave-suction material described in claim 1 Method, comprising the following steps:
Step 1: the dehydrated alcohol for being 99.9% using volumetric concentration is that 99.9% ethyl acetate is first respectively with volumetric concentration It alternately rinses afterwards, is cleaned by ultrasonic foam metal material in deionized water, remove surface impurity;
Step 2: in deionized water by transient metal sulfide dissolution, metal sulfide solution is obtained;
Step 3: the mixed liquor for going deimpurity foam metal material and step 2 to obtain in step 1 is successively transferred to In hydrothermal reaction kettle, kettle is sealed, hydrothermal reaction kettle is put into baking oven and is kept for 200-240 DEG C, is reacted 18-24 hours, natural cooling To room temperature, kettle, filtration washing are opened several times, until the transition gold that is colorless and transparent, being dried to obtain foam metal load that filtrate becomes Belong to sulfide.
Invention effect
The technical effects of the invention are that: a kind of three-dimensional composite wave-absorbing material prepared by single step reaction proposed by the present invention Material and preparation method, the magnetic Ni@Ni of three dimensional skeletal structure is prepared for by one-step method3S2Composite material, by adjusting foam gold Belong to the ratio with transient metal sulfide, regulates and controls the surface topography and electromagnetic parameter of composite material, to adapt to the micro- of different-waveband Wave absorbs.The present invention solves big traditional magnetic component density for showing in inhaling wave, narrow frequency range, impedance matching difference etc. Disadvantage, takes full advantage of that foam metal is porous, lightweight is high, the structural advantage of specific surface area, the regulatable Transition Metal Sulfur in surface Compound dielectric loss profile material improves the electromagnetic parameter of foam metal, and there is huge in terms of electromagnetic wave absorbent material production Practical application value.
The purpose of the present invention is preparing foam type composite wave-suction material by one-step method, with the traditional two step method of simplification, gram The shortcomings that taking conventional method simplifies operation, improves production efficiency, reduces production cost, eliminates waste liquid, is absorbing material Industrialization lays the foundation.
Detailed description of the invention
Fig. 1: prepared each material microscopic appearance
Fig. 2: the XRD spectrum of prepared each material
Fig. 3: the reflection loss performance for electromagnetic wave of composite material of the present invention
Specific embodiment
Referring to Fig. 1-Fig. 3, a kind of three-dimensional foam composite wave-suction material prepared by one-step method passes through different ratio shape The metal foam of the adjustable three-dimensional structure of looks, in which: foam metal is that substrate constitutes three-dimensional netted skeleton, the transition gold of load Belong to sulfide, by the allotment (1:2,1:2.5,1:3,1:3.5) of different molal weight ratios, foam metal and Transition Metal Sulfur Compound accounting can regulate and control, and the mass fraction of the foam metal is 5-25%;The mass fraction of the transient metal sulfide For 75-95%.
The foam metal is three-dimensional netted skeleton, and aperture is between 200-400 μm.
The foam metal is nickel foam, foam cobalt or foam copper.
The transient metal sulfide is cobalt disulfide, three nickel of copper sulfide, nickel sulfide or curing.
A kind of preparation method of the composite wave-suction material prepared by one-step method, it is characterised in that steps are as follows:
Step 1: the dehydrated alcohol for being 99.9% using volumetric concentration is that 99.9% ethyl acetate is first respectively with volumetric concentration Foam metal material is alternately cleaned afterwards, is cleaned by ultrasonic 30min in deionized water, removes surface impurity.
Step 2: in deionized water by transient metal sulfide dissolution, obtaining metal sulfide solution.
Step 3: the mixed liquor that the foam metal material of decontamination in step 1 and step 2 obtain successively is transferred to water In thermal response kettle, kettle is sealed, hydrothermal reaction kettle is put into baking oven and is kept for 200-240 DEG C, reacts 18-24 hours, naturally cools to Room temperature opens kettle, filtration washing several times, until filtrate becomes colorless and transparent, is dried to obtain the transition metal of foam metal load Sulfide.
Now in conjunction with embodiment, attached drawing, the invention will be further described:
Three-dimensional foam type composite wave-suction material of the invention, ingredient are the foam metals that mass fraction is 5-25%, then In the transient metal sulfide of four kinds of different-shapes of its area load 75-95%, the mass ratio of two kinds of components passes through raw material Proportion can be adjusted;
Foam metal is nickel foam, foam cobalt or foam copper;
Transient metal sulfide is cobalt disulfide, copper sulfide, nickel sulfide, three nickel of curing;
Transient metal sulfide scale can reach nanometer and micron level respectively;
Using foam metal used as nickel foam, transient metal sulfide Ni3S2Illustrate:
Step 1: foam metal being cut to the pane of 1 × 5cm, is 99.9% dehydrated alcohol and volume with volumetric concentration Concentration is that 99.9% ethyl acetate alternately rinses respectively three times, and each 3min, after removing impurity, deionized water is cleaned by ultrasonic 30min, 2 hours are dried at 100 DEG C for use;
Step 2:0.3g thiocarbamide is dissolved in 160 ml deionized waters, and 30min is stirred by ultrasonic;
Step 3:0.6g nickel foam and above-mentioned solution are transferred to polytetrafluoroethylene (PTFE) water heating kettle, seal kettle, are put into baking oven, 200 Reacted 20 hours at DEG C, open kettle, deionized water washing several times, dried for standby.
Embodiment 1:
After 0.6g nickel foam dehydrated alcohol and ethyl acetate ultrasonic cleaning, dried for standby, 0.3g thiocarbamide is dissolved in 160 millis It rises in deionized water, 30min is stirred by ultrasonic, above-mentioned nickel foam and solution are transferred to 200 milliliters of polytetrafluoroethylene (PTFE) water jointly In thermal response kettle, kettle is sealed, is reacted 20 hours at 200 DEG C;Stop reaction after, cool to room temperature automatically to system, open kettle, go from Sub- water cleans reaction product repeatedly, is sealed after drying at room temperature stand-by.
Embodiment 2:
After 0.6g nickel foam dehydrated alcohol and ethyl acetate ultrasonic cleaning, dried for standby, 0.2g thiocarbamide is dissolved in 160 millis It rises in deionized water, 30min is stirred by ultrasonic, above-mentioned nickel foam and solution are transferred to 200 milliliters of polytetrafluoroethylene (PTFE) water jointly In thermal response kettle, kettle is sealed, is reacted 20 hours at 200 DEG C;Stop reaction after, cool to room temperature automatically to system, open kettle, go from Sub- water cleans reaction product repeatedly, is sealed after drying at room temperature stand-by.
Embodiment 3:
After 0.6g nickel foam dehydrated alcohol and ethyl acetate ultrasonic cleaning, dried for standby, 0.15g thioacetamide is dissolved in In 160 ml deionized waters, 30min is stirred by ultrasonic, above-mentioned nickel foam and solution are transferred to 200 milliliters of polytetrafluoroethyl-ne jointly In alkene hydrothermal reaction kettle, kettle is sealed, is reacted 20 hours at 200 DEG C;After stopping reaction, room temperature is cooled to automatically to system, opens kettle, Deionized water cleans reaction product repeatedly, is sealed after drying at room temperature stand-by.
Embodiment 4:
By the Ni@Ni of above-mentioned preparation3S2Foam immerses in atoleine, and after solidifying, foam/waxy product are trimmed to cylinder Shape sample (Φout=7.0mm, Φin=3.04), the weight ratio of foam and wax is 1:1.Cylindrical standard sample uses vector point Analyzer (HP8753D) carries out the reflection loss test of X-band electromagnetic wave.Test result such as Fig. 3.Four kinds of molal weight ratio difference For 1:2,1:2.5,1:3, the best reflection loss of the transient metal sulfide of the foam metal load of 1:3.5 respectively reaches- 45.2dB、-31.6dB、-50.7dB、-39.9dB。

Claims (7)

1. a kind of three-dimensional foam type composite wave-suction material, which is characterized in that including foam metal and transition metal, wherein foam is golden Belong to and be used as substrate, transient metal sulfide can be deployed as load, the two by different proportion;Foam metal quality point Number is 5-25%;The mass fraction of transient metal sulfide is 75-95%.
2. a kind of three-dimensional foam type composite wave-suction material as described in claim 1, which is characterized in that the foam metal and mistake 1:2,1:2.5,1:3 can be passed through respectively by crossing metal sulfide, and the molal weight ratio of 1:3.5 is deployed.
3. a kind of three-dimensional foam type composite wave-suction material as described in claim 1, which is characterized in that the foam metal is three Mesh skeleton is tieed up, aperture is between 200-400 μm.
4. a kind of three-dimensional foam type composite wave-suction material as described in claim 1, which is characterized in that the foam metal is bubble Foam nickel, foam cobalt or foam copper.
5. a kind of three-dimensional foam type composite wave-suction material as described in claim 1, which is characterized in that the transition metal vulcanization Object is cobalt disulfide, three nickel of copper sulfide, nickel sulfide or vulcanization.
6. a kind of three-dimensional foam type composite wave-suction material as described in claim 1, which is characterized in that the foam metal and mistake The molal weight ratio of metal sulfide is crossed as 1:2,1:2.5,1:3,1:3.5, while needing satisfaction to add up mass fraction to be Absolutely.
7. a kind of method for preparing three-dimensional foam type composite wave-suction material described in claim 1, which is characterized in that including following step It is rapid:
Step 1: the dehydrated alcohol for being 99.9% using volumetric concentration and volumetric concentration are that 99.9% ethyl acetate is taken up in order of priority friendship For flushing, it is cleaned by ultrasonic foam metal material in deionized water, removes surface impurity;
Step 2: in deionized water by transient metal sulfide dissolution, metal sulfide solution is obtained;
Step 3: the mixed liquor for going deimpurity foam metal material and step 2 to obtain in step 1 is successively transferred to hydro-thermal In reaction kettle, kettle is sealed, hydrothermal reaction kettle is put into baking oven and is kept for 200-240 DEG C, reacts 18-24 hours, naturally cools to room Temperature opens kettle, filtration washing several times, until the Transition Metal Sulfur that is colorless and transparent, being dried to obtain foam metal load that filtrate becomes Compound.
CN201910697871.6A 2019-07-31 2019-07-31 Three-dimensional foam type composite wave-absorbing material and preparation method thereof Expired - Fee Related CN110461137B (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111170761A (en) * 2020-01-11 2020-05-19 西安交通大学 Silicon carbide @ metal oxide wave-absorbing foam and preparation method thereof
CN112500832A (en) * 2020-12-11 2021-03-16 西北工业大学 Preparation method of foam nickel-based oxide composite wave-absorbing material
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

Citations (4)

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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
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

Patent Citations (4)

* Cited by examiner, † Cited by third party
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
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

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111170761A (en) * 2020-01-11 2020-05-19 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
CN112500832A (en) * 2020-12-11 2021-03-16 西北工业大学 Preparation method of foam nickel-based oxide composite wave-absorbing material
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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