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 PDFInfo
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- 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
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- type composite
- composite wave
- sulfide
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- 239000006260 foam Substances 0.000 title claims abstract description 79
- 239000000463 material Substances 0.000 title claims abstract description 25
- 239000002131 composite material Substances 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title abstract description 9
- 229910052751 metal Inorganic materials 0.000 claims abstract description 34
- 239000002184 metal Substances 0.000 claims abstract description 34
- 229910052976 metal sulfide Inorganic materials 0.000 claims abstract description 28
- 230000001052 transient effect Effects 0.000 claims abstract description 23
- 238000000034 method Methods 0.000 claims abstract description 10
- 238000006243 chemical reaction Methods 0.000 claims abstract description 7
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 35
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 17
- 229910052759 nickel Inorganic materials 0.000 claims description 16
- 239000008367 deionised water Substances 0.000 claims description 11
- 229910021641 deionized water Inorganic materials 0.000 claims description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 7
- 229910052723 transition metal Inorganic materials 0.000 claims description 7
- 239000007769 metal material Substances 0.000 claims description 6
- 150000003624 transition metals Chemical class 0.000 claims description 6
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 5
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 4
- XUKVMZJGMBEQDE-UHFFFAOYSA-N [Co](=S)=S Chemical group [Co](=S)=S XUKVMZJGMBEQDE-UHFFFAOYSA-N 0.000 claims description 4
- 229910017052 cobalt Inorganic materials 0.000 claims description 4
- 239000010941 cobalt Substances 0.000 claims description 4
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 4
- 229910052802 copper Inorganic materials 0.000 claims description 4
- 239000010949 copper Substances 0.000 claims description 4
- OMZSGWSJDCOLKM-UHFFFAOYSA-N copper(II) sulfide Chemical compound [S-2].[Cu+2] OMZSGWSJDCOLKM-UHFFFAOYSA-N 0.000 claims description 4
- 239000012535 impurity Substances 0.000 claims description 4
- WWNBZGLDODTKEM-UHFFFAOYSA-N sulfanylidenenickel Chemical compound [Ni]=S WWNBZGLDODTKEM-UHFFFAOYSA-N 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- 238000004090 dissolution Methods 0.000 claims description 3
- 239000000706 filtrate Substances 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
- 239000000758 substrate Substances 0.000 claims description 3
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 2
- 150000001875 compounds Chemical class 0.000 claims description 2
- 229910052717 sulfur Inorganic materials 0.000 claims description 2
- 239000011593 sulfur Substances 0.000 claims description 2
- 238000004073 vulcanization Methods 0.000 claims 2
- 238000011010 flushing procedure Methods 0.000 claims 1
- 230000008901 benefit Effects 0.000 abstract description 5
- 230000002745 absorbent Effects 0.000 abstract description 4
- 239000002250 absorbent Substances 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 239000011165 3D composite Substances 0.000 abstract description 3
- 238000010521 absorption reaction Methods 0.000 abstract description 3
- 238000012876 topography Methods 0.000 abstract description 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 6
- 239000004810 polytetrafluoroethylene Substances 0.000 description 6
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 description 6
- -1 Transition Metal Sulfur Compound Chemical class 0.000 description 4
- 239000011358 absorbing material Substances 0.000 description 4
- 238000011160 research Methods 0.000 description 4
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 3
- 239000007795 chemical reaction product Substances 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 3
- 239000010931 gold Substances 0.000 description 3
- 229910052737 gold Inorganic materials 0.000 description 3
- 230000004044 response Effects 0.000 description 3
- 238000004506 ultrasonic cleaning Methods 0.000 description 3
- 150000001336 alkenes Chemical class 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000035699 permeability Effects 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 230000007704 transition Effects 0.000 description 2
- 239000003643 water by type Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 239000006096 absorbing agent Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000005202 decontamination Methods 0.000 description 1
- 230000003588 decontaminative effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000006262 metallic foam Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- YUKQRDCYNOVPGJ-UHFFFAOYSA-N thioacetamide Chemical compound CC(N)=S YUKQRDCYNOVPGJ-UHFFFAOYSA-N 0.000 description 1
- DLFVBJFMPXGRIB-UHFFFAOYSA-N thioacetamide Natural products CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- 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
Landscapes
- 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
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.
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Cited By (3)
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---|---|---|---|---|
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 |
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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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WO2018125641A1 (en) * | 2016-12-28 | 2018-07-05 | Nanotek Instruments, Inc. | Flexible and shape-conformal rope-shape alkali metal batteries |
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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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