CN112077332A - Carbon-coated magnetic metal simple substance composite material and preparation method and application thereof - Google Patents
Carbon-coated magnetic metal simple substance composite material and preparation method and application thereof Download PDFInfo
- Publication number
- CN112077332A CN112077332A CN202010952848.XA CN202010952848A CN112077332A CN 112077332 A CN112077332 A CN 112077332A CN 202010952848 A CN202010952848 A CN 202010952848A CN 112077332 A CN112077332 A CN 112077332A
- Authority
- CN
- China
- Prior art keywords
- carbon
- composite material
- preparation
- coated magnetic
- carbon source
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 60
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 60
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 55
- 239000002184 metal Substances 0.000 title claims abstract description 55
- 239000002131 composite material Substances 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- 239000000126 substance Substances 0.000 title claims abstract description 25
- 239000004793 Polystyrene Substances 0.000 claims abstract description 30
- 229920002223 polystyrene Polymers 0.000 claims abstract description 30
- 150000003839 salts Chemical class 0.000 claims abstract description 24
- 238000003763 carbonization Methods 0.000 claims abstract description 14
- 238000003756 stirring Methods 0.000 claims abstract description 14
- 238000010521 absorption reaction Methods 0.000 claims abstract description 8
- 239000000203 mixture Substances 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims abstract description 6
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 40
- 229910052759 nickel Inorganic materials 0.000 claims description 20
- 238000000034 method Methods 0.000 claims description 12
- 239000000843 powder Substances 0.000 claims description 10
- 239000002033 PVDF binder Substances 0.000 claims description 8
- 239000007789 gas Substances 0.000 claims description 8
- 229920002981 polyvinylidene fluoride Polymers 0.000 claims description 8
- 239000012298 atmosphere Substances 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 7
- 238000010000 carbonizing Methods 0.000 claims description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 4
- 239000011261 inert gas Substances 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 3
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 2
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 claims description 2
- 229910017052 cobalt Inorganic materials 0.000 claims description 2
- 239000010941 cobalt Substances 0.000 claims description 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 2
- 239000008103 glucose Substances 0.000 claims description 2
- 239000001257 hydrogen Substances 0.000 claims description 2
- 229910052739 hydrogen Inorganic materials 0.000 claims description 2
- 229910052742 iron Inorganic materials 0.000 claims description 2
- 239000002905 metal composite material Substances 0.000 claims 4
- 239000011358 absorbing material Substances 0.000 abstract description 8
- 239000003575 carbonaceous material Substances 0.000 abstract description 5
- 238000011068 loading method Methods 0.000 abstract description 3
- 239000000243 solution Substances 0.000 description 16
- 239000004005 microsphere Substances 0.000 description 9
- 238000010438 heat treatment Methods 0.000 description 7
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 6
- 239000012188 paraffin wax Substances 0.000 description 6
- 230000008569 process Effects 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- MYRTYDVEIRVNKP-UHFFFAOYSA-N 1,2-Divinylbenzene Chemical group C=CC1=CC=CC=C1C=C MYRTYDVEIRVNKP-UHFFFAOYSA-N 0.000 description 4
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical group C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- YFKIWUQBRSMPMZ-UHFFFAOYSA-N methane;nickel Chemical class C.[Ni] YFKIWUQBRSMPMZ-UHFFFAOYSA-N 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 230000035699 permeability Effects 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 239000003431 cross linking reagent Substances 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 description 3
- 239000003995 emulsifying agent Substances 0.000 description 3
- 239000000839 emulsion Substances 0.000 description 3
- ZSWFCLXCOIISFI-UHFFFAOYSA-N endo-cyclopentadiene Natural products C1C=CC=C1 ZSWFCLXCOIISFI-UHFFFAOYSA-N 0.000 description 3
- 239000003999 initiator Substances 0.000 description 3
- 230000007246 mechanism Effects 0.000 description 3
- 239000011259 mixed solution Substances 0.000 description 3
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 description 3
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- KZPXREABEBSAQM-UHFFFAOYSA-N cyclopenta-1,3-diene;nickel(2+) Chemical compound [Ni+2].C=1C=C[CH-]C=1.C=1C=C[CH-]C=1 KZPXREABEBSAQM-UHFFFAOYSA-N 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 239000002159 nanocrystal Substances 0.000 description 2
- 239000012299 nitrogen atmosphere Substances 0.000 description 2
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical group [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 description 2
- 238000002310 reflectometry Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- 239000004698 Polyethylene Substances 0.000 description 1
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical group [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004027 cell Anatomy 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005670 electromagnetic radiation Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 231100000405 induce cancer Toxicity 0.000 description 1
- 230000002427 irreversible effect Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 210000004698 lymphocyte Anatomy 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- BMGNSKKZFQMGDH-FDGPNNRMSA-L nickel(2+);(z)-4-oxopent-2-en-2-olate Chemical compound [Ni+2].C\C([O-])=C\C(C)=O.C\C([O-])=C\C(C)=O BMGNSKKZFQMGDH-FDGPNNRMSA-L 0.000 description 1
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical group [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- -1 polyethylene Polymers 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/20—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds
- B22F9/22—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds using gaseous reductors
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/16—Metallic particles coated with a non-metal
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/05—Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
-
- 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 relates to the technical field of electromagnetic wave absorbing materials, in particular to a carbon-coated magnetic metal simple substance composite material and a preparation method and application thereof. The invention discloses a preparation method of a carbon-coated magnetic metal simple substance composite material, which comprises the steps of mixing a carbon source solution containing metal salt with polystyrene, immersing the mixture into polystyrene spheres by stirring, loading the metal salt and the carbon source on the polystyrene spheres, removing a template by carbonization, forming a three-dimensional honeycomb structure by the carbon source, and embedding the metal simple substance formed by the carbonization of the metal salt into a honeycomb carbon material. The preparation method simplifies the traditional preparation steps, is simple to operate, and the prepared composite material is thin in thickness, light in weight, high in dielectric loss and magnetic loss capacity, low in density and high in conductivity, enhances the electromagnetic wave absorption performance, and can be used as a wave-absorbing material.
Description
Technical Field
The invention relates to the technical field of electromagnetic wave absorbing materials, in particular to a carbon-coated magnetic metal simple substance composite material and a preparation method and application thereof.
Background
With the rapid development of information technology and the use of various wireless communication tools, more and more electromagnetic waves enter our lives, and thus, the electromagnetic pollution is just a new type of pollution. Research shows that electromagnetic waves not only can interfere the use of precision instruments, but also excessive electromagnetic wave radiation can cause great harm to human health. After long-term exposure to electromagnetic radiation, the cells and tissues in the human body, such as blood, lymphocytes, etc., can be diseased, even induce cancer, and cause irreversible damage to the functions of the human body. The only way to do this is to develop new electromagnetic wave absorbing materials to attenuate unwanted electromagnetic waves. Electromagnetic wave absorbing materials, also known as stealth materials, have also found important applications in strategic military applications. The traditional electromagnetic wave absorbing material preparation method has complicated steps, and various factors such as narrow absorption bandwidth, high density, poor absorption capacity and the like limit the development and application of the material.
Disclosure of Invention
In view of the above, the invention provides a carbon-coated magnetic metal simple substance composite material, and a preparation method and an application thereof.
The specific technical scheme is as follows:
the invention provides a preparation method of a carbon-coated magnetic metal simple substance composite material, which comprises the following steps:
step 1: mixing magnetic metal salt with a carbon source solution to obtain a carbon source solution containing metal salt;
step 2: adding polystyrene sphere powder into the carbon source solution containing the metal salt, stirring, and drying to obtain a mixture;
and step 3: carbonizing the mixture in the atmosphere of reducing gas and inert gas to obtain a carbon-coated magnetic metal simple substance composite material;
the carbon source is selected from polyvinylidene fluoride or glucose.
The preparation method provided by the invention is simple to operate, the polystyrene spheres are used as the template of the carbon-coated magnetic metal simple substance composite material, the carbon source solution containing the metal salt is immersed into the polystyrene spheres in the standing and stirring process, so that the metal salt and the carbon source can be loaded on the polystyrene spheres, the template is removed in the high-temperature carbonization process, the carbon source forms a three-dimensional honeycomb structure due to the decomposition of the polystyrene, and the metal simple substance formed by the carbonization of the metal salt is embedded in the honeycomb carbon material, so that the unique structure not only can form a conductive network and improve the conductivity loss of the material, but also can further improve the loading amount of the magnetic metal among pores, and further improve the magnetic permeability of the carbon-coated magnetic metal simple substance composite material.
In step 1 of the invention, the magnetic metal in the magnetic metal salt is one or more than two of iron, cobalt and nickel; the elementary metal nickel has typical soft magnetic performance and can improve the magnetic permeability of the material to a certain extent; when the metal in the metal salt is preferably nickel, the metal salt is preferably nickel nitrate, nickel acetylacetonate or nickelocene, more preferably nickelocene;
the carbon source is preferably polyvinylidene fluoride; polyvinylidene fluoride can be used as a carbon source with high dielectric loss and also can be used as a binder to connect all dispersed polystyrene spheres, so that structural collapse cannot occur in the carbonization process, and a good three-dimensional honeycomb structure is kept;
the mass ratio of the metal salt to the carbon source is (1-3): (1-3), preferably 2: 1;
the mass concentration of the carbon source solution is 10% to 50%, more preferably 10% to 30%, and still more preferably 10%.
In step 2 of the present invention, the polystyrene sphere powder can be purchased from the market or prepared by the self. The preparation method of the polystyrene sphere powder comprises the following steps:
mixing a styrene monomer, an initiator, an emulsifier and a cross-linking agent, carrying out water bath reaction, and drying to obtain polyethylene powder;
the initiator is preferably potassium persulfate, the emulsifier is preferably sodium dodecyl sulfate, and the crosslinking agent is divinylbenzene;
the dosage ratio of the styrene monomer, the initiator, the emulsifier and the cross-linking agent is (20-50) mL: (1000-1500) mg: (200- > 250) mg: (3-5) mL;
the mixing is preferably carried out under the condition of stirring, the stirring speed is 250-300 rmp, the time is 20-40min, and the stirring is preferably carried out at 250rmp for 30 min;
the temperature of the water bath reaction is 70-80 ℃, the time is 12-36h, preferably 75 ℃, and 24 h;
the drying temperature is 60-90 ℃, the drying time is 10-14 h, preferably 80 ℃, and 12 h;
the water bath reaction is preferably carried out under an atmosphere of nitrogen or an inert gas.
In the step 2 of the invention, the metal salt and the carbon source are loaded in the polystyrene spheres by stirring the carbon source solution containing the metal salt, so that the loading effect is better than that of vacuum-pumping treatment;
the stirring speed is 250-300 rmp, and the stirring time is 30 min;
the particle size of the polystyrene sphere powder is 100-150nm, preferably 100-120 nm;
the mass ratio of the polystyrene spheres to the carbon source is (1-3): (1-3), preferably 1: 1.
In step 3 of the invention, metal salt is carbonized and reduced into a metal simple substance which is embedded in the three-dimensional honeycomb carbon material in the atmosphere of reducing gas;
the reducing gas is hydrogen;
the carbonization temperature is 500-700 ℃, preferably 550-650 ℃, and the time is 2-4 h, preferably 2 h.
The invention also provides the carbon-coated magnetic metal simple substance composite material prepared by the preparation method.
The particle size of the nickel nanocrystalline in the carbon-coated magnetic metal simple substance composite material is 7-10nm, and the mass content of the metal simple substance is 55%.
The carbon material and the magnetic metal simple substance in the carbon-coated magnetic metal simple substance composite material prepared by the method are combined with dielectric loss and magnetic loss respectively, so that the electromagnetic wave absorption performance of the composite material is greatly improved, and the composite material can be used as a wave-absorbing material.
The invention also provides application of the carbon-coated magnetic metal simple substance composite material prepared by the preparation method in the field of electromagnetic wave absorption.
According to the technical scheme, the invention has the following advantages:
the invention provides a preparation method of a carbon-coated magnetic metal simple substance composite material, in the preparation method, a polystyrene ball is used as a template of the carbon-coated magnetic metal simple substance composite material, a carbon source solution containing metal salt is immersed in the polystyrene ball in the standing and stirring process, so that the metal salt and the carbon source can be loaded on the polystyrene ball, in the high-temperature carbonization process, the template is removed due to the decomposition of polystyrene, the carbon source forms a three-dimensional honeycomb structure, and the metal simple substance formed by the carbonization of the metal salt is embedded in a honeycomb carbon material. The preparation method provided by the invention simplifies the traditional preparation steps, is simple to operate, improves the production efficiency, and the prepared carbon-coated magnetic metal simple substance composite material is thin in thickness, light in weight, high in dielectric loss and magnetic loss capacity, low in density and high in conductivity, so that the electromagnetic wave absorption performance of the composite material is enhanced, and the composite material can be used as a wave-absorbing material. Compared with other inorganic non-metallic materials, the composite material has simpler carbon preparation and lower cost.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without inventive exercise.
FIG. 1 is a scanning electron microscope photograph of polystyrene microspheres prepared in example 1 of the present invention;
FIG. 2 is a scanning electron microscope image of a three-dimensional honeycomb-shaped carbon-coated nickel composite material obtained at a carbonization temperature of 600 ℃ in example 3 of the present invention;
FIG. 3 is an X-ray diffraction pattern of three-dimensional honeycomb-shaped nickel-on-carbon composites obtained in inventive examples 2, 3 and 4 at carbonization temperatures of 550, 600 and 650 ℃, respectively;
FIG. 4 is a graph of the real and imaginary parts of the dielectric constant of an annular sample in the frequency range of 2-18GHz in accordance with example 5 of the present invention;
FIG. 5 is a graph of the real and imaginary parts of permeability for an annular sample in the frequency range of 2-18GHz in accordance with example 5 of the invention;
FIG. 6 is a graph of the dielectric loss and magnetic loss mechanism for the annular sample in the frequency range of 2-18GHz in accordance with example 5 of the invention;
FIG. 7 shows the reflectance values obtained by simulating different thicknesses in the frequency range of 2-18GHz for the ring sample in example 5 of the present invention.
Detailed Description
In order to make the objects, features and advantages of the present invention more obvious and understandable, the technical solutions in the embodiments of the present invention will be clearly and completely described below, and it should be apparent that the embodiments described below are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In the examples of the present invention, polyvinylidene fluoride was purchased from Macklin (P875316-500 g).
Example 1
This example is a specific example of the preparation of polystyrene sphere powder.
Firstly, 240mg of sodium dodecyl benzene sulfonate (SDS) is dissolved in 600mL of deionized water and stirred until the SDS is completely dissolved; then 30mL of styrene and 3.6mL of Divinylbenzene (DVB) were added to the three-necked flask and stirred at room temperature for 30min at a rotation speed of 250rmp under a nitrogen atmosphere; then placing the three-neck flask filled with the solution into a water bath kettle, and adding 1.2g of potassium persulfate when the temperature is raised to 75 ℃; 3.6mL of Divinylbenzene (DVB) was added again after the system had reacted for 3 h. And continuously stirring for 24 hours in the nitrogen atmosphere to obtain the polystyrene microsphere emulsion. And finally, standing 100mL of polystyrene microsphere emulsion in an oven at 80 ℃, drying overnight, evaporating and drying the polystyrene microsphere emulsion to form solid blocks, and finally grinding to obtain polystyrene microsphere powder with the particle size of 100-120 nm.
FIG. 1 is a scanning electron microscope photograph of polystyrene microspheres prepared in example 1 of the present invention. Figure 1 shows that in the dry-state, the polystyrene spheres are well deposited and stacked.
Example 2
This example is a specific example of the preparation of a carbon-coated nickel composite material.
0.15g of the polystyrene microspheres prepared in example 1 was weighed and dispersed in 12.5mL of tetrahydrofuran solution, and 0.3218g of nickel cyclopentadienyl and 0.15g of polyvinylidene fluoride were added and stirred at room temperature to obtain a uniformly mixed solution. The homogeneous system was then dried in an oven at 80 ℃ for 24 h. Finally, carbonizing it in H2Heating to 550 ℃ at a heating rate of 5 ℃/min under the atmosphere of/Ar mixed gas, preserving heat for two hours, and cooling to room temperature to obtain the three-dimensional honeycomb-shaped carbon-coated nickel composite material.
FIG. 3 is an X-ray diffraction pattern of a three-dimensional honeycomb-shaped nickel-on-carbon composite material obtained at different carbonization temperatures. The carbon-coated nickel composite material prepared by the method has 3 sharp diffraction peaks at 44.5 degrees, 51.8 degrees and 76.4 degrees, which respectively correspond to three crystal faces (111), (200) and (220) of Ni of a standard card, and no other diffraction peaks are found, so that the carbon-coated nickel composite material prepared by the method is proved to be successful.
Example 3
This example is a specific example of the preparation of a carbon-coated nickel composite material.
0.15g of the polystyrene microspheres prepared in example 1 was weighed and dispersed in 12.5mL of tetrahydrofuran solution, and 0.3218g of nickel cyclopentadienyl and 0.15g of polyvinylidene fluoride were added and stirred at room temperature to obtain a uniformly mixed solution. The homogeneous system was then dried in an oven at 80 ℃ for 24 h. Finally, carbonizing it in H2Heating to 600 ℃ at a heating rate of 5 ℃/min under the atmosphere of/Ar mixed gas, preserving heat for two hours, and cooling to room temperature to obtain the three-dimensional honeycomb-shaped carbon-coated nickel composite material (Ni @ C composite material), wherein the particle size of the nickel nanocrystal is about 7-10nm, and the content of the nickel nanocrystal is 55%.
Fig. 2 is a scanning electron microscope image of a three-dimensional honeycomb-shaped carbon-coated nickel composite material obtained at a carbonization temperature of 600 ℃. Fig. 2 shows that the three-dimensional honeycomb structure is relatively complete.
As shown in fig. 3, there are 3 sharp diffraction peaks at 44.5 °, 51.8 ° and 76.4 °, which correspond to the three crystal planes (111), (200) and (220) of Ni of the standard card, respectively, and no other diffraction peaks are found, indicating that this example successfully produces the nickel-on-carbon composite material.
Example 4
This example is a specific example of the preparation of a carbon-coated nickel composite material.
0.15g of the polystyrene microspheres prepared in example 1 was weighed and dispersed in 12.5mL of tetrahydrofuran solution, and 0.3218g of nickel cyclopentadienyl and 0.15g of polyvinylidene fluoride were added and stirred at room temperature to obtain a uniformly mixed solution. The homogeneous system was then dried in an oven at 80 ℃ for 24 h. Finally, carbonizing it in H2Heating to 650 ℃ at a heating rate of 5 ℃/min under the atmosphere of/Ar mixed gas, preserving heat for two hours, and cooling to room temperature to obtainTo a three-dimensional honeycomb-shaped carbon-coated nickel composite material.
As shown in fig. 3, there are 3 sharp diffraction peaks at 44.5 °, 51.8 ° and 76.4 °, which correspond to the three crystal planes (111), (200) and (220) of Ni of the standard card, respectively, and no other diffraction peaks are found, indicating that this example successfully produces the nickel-on-carbon composite material.
Example 5
Preparing an annular sample from the three-dimensional honeycomb Ni @ C composite material prepared in the embodiment 3 and paraffin according to the mass content of the sample of 70 wt%, specifically weighing the sample and the paraffin according to the above proportion, and weighing the use amount of the sample and the paraffin by using an electronic balance; heating and melting paraffin at 70 ℃, mixing the weighed sample with the paraffin, and stirring for 3min to uniformly disperse the sample in the paraffin; when the temperature is reduced to room temperature, the mixture changes from a liquid state to a solid state; then, the mixture was ground into fine powder, charged into a special die, pressed for 30 seconds with an oil jack, and the powder was pressed into a ring-shaped sample (inner diameter 3.04mm, outer diameter 7mm, thickness controlled at 2.6-3.3 mm). And finally, the annular sample is loaded into a clamp of an AV3618 network analyzer, electromagnetic parameters within the range of 2-18GHz of the electromagnetic wave frequency are measured by a coaxial method, and then the reflectivity of the sample under different coating thicknesses is simulated by Matlab.
FIG. 4 is a graph of the real and imaginary parts of the dielectric constant of the annular sample of this embodiment in the frequency range of 2-18GHz, with the real and imaginary values decreasing over the frequency range, showing typical frequency dissipation behavior; FIG. 5 is a graph showing the real and imaginary parts of the permeability of the annular sample of this example in the frequency range of 2-18GHz, with the real part increasing from 1.08 to 3.47 and the imaginary part varying from-0.08 to 0.75; FIG. 6 is a graph of dielectric loss and magnetic loss of the ring sample in the frequency range of 2-18GHz, the loss mechanism of the sample in the frequency range of 3.5-9.0GHz is mainly dielectric loss, and the loss mechanism of the sample in the other frequency range is mainly magnetic loss; FIG. 7 is a reflectivity graph obtained by simulating different thicknesses of the ring sample in the frequency range of 2-18GHz, wherein when the thickness is 4.5mm, the minimum RL is-29.3 dB, and the effective absorption frequency bandwidth reaches the ultra-wide bandwidth of 13 GHz.
The above-mentioned embodiments are only used for illustrating the technical solutions of the present invention, and not for limiting the same; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (10)
1. A preparation method of a carbon-coated magnetic metal simple substance composite material is characterized by comprising the following steps:
step 1: mixing magnetic metal salt with a carbon source solution to obtain a carbon source solution containing metal salt;
step 2: adding polystyrene sphere powder into the carbon source solution containing the metal salt, stirring, and drying to obtain a mixture;
and step 3: carbonizing the mixture in the atmosphere of reducing gas and inert gas to obtain a carbon-coated magnetic metal simple substance composite material;
the carbon source is selected from polyvinylidene fluoride or glucose.
2. The method according to claim 1, wherein the magnetic metal in the magnetic metal salt is one or more of iron, cobalt, and nickel.
3. The production method according to claim 1, wherein the reducing gas is hydrogen.
4. The production method according to claim 1, wherein the mass ratio of the metal salt to the carbon source is (1-3): (1-3).
5. The method according to claim 1, wherein the stirring is performed at a rate of 250 to 300rmp for 30 min.
6. The method according to claim 1, wherein the carbon source has a mass concentration of 10 to 50%.
7. The preparation method according to claim 1, wherein the carbonization temperature is 500-700 ℃ and the carbonization time is 2-4 h.
8. The carbon-coated magnetic elemental metal composite material prepared by the preparation method of any one of claims 1 to 7.
9. The carbon-coated magnetic elemental metal composite material according to claim 8, wherein the mass content of the elemental metal in the carbon-coated magnetic elemental metal composite material is 55%.
10. The use of the carbon-coated magnetic elemental metal composite material of claim 8 in the field of electromagnetic wave absorption.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010952848.XA CN112077332A (en) | 2020-09-11 | 2020-09-11 | Carbon-coated magnetic metal simple substance composite material and preparation method and application thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010952848.XA CN112077332A (en) | 2020-09-11 | 2020-09-11 | Carbon-coated magnetic metal simple substance composite material and preparation method and application thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN112077332A true CN112077332A (en) | 2020-12-15 |
Family
ID=73736629
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010952848.XA Pending CN112077332A (en) | 2020-09-11 | 2020-09-11 | Carbon-coated magnetic metal simple substance composite material and preparation method and application thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112077332A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115318296A (en) * | 2022-08-19 | 2022-11-11 | 广东工业大学 | High-dispersion film-shaped carbon-coated nickel catalyst and preparation method and application thereof |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20010009118A1 (en) * | 2000-01-21 | 2001-07-26 | Sumitomo Electric Industries, Ltd. And Sumitomo Electric Fine Polymer, Inc. | Method of producing alloy powders, alloy powders obtained by said method, and products applying said powders |
| US20050181202A1 (en) * | 2004-02-18 | 2005-08-18 | Hitachi Metals, Ltd. | Fine composite metal particles and their production method, micro-bodies, and magnetic beads |
| CN1773638A (en) * | 2005-11-10 | 2006-05-17 | 北京科技大学 | Method for producing magnetic powder by form method |
| CN105562005A (en) * | 2016-02-29 | 2016-05-11 | 复旦大学 | Nano composite material with carbon-coated Ni nano crystal particles loaded on graphene and preparation method of nano composite material |
| CN106041124A (en) * | 2016-07-18 | 2016-10-26 | 中北大学 | Preparation method of metal and metal oxide hollow microspheres with adjustable particle sizes |
| CN106180744A (en) * | 2016-08-25 | 2016-12-07 | 董晓 | A kind of preparation method of diamond composition pre-alloyed powder |
| CN110534762A (en) * | 2019-09-05 | 2019-12-03 | 中国科学院新疆理化技术研究所 | A kind of preparation method of cobalt and the 3-D ordered multiporous C catalyst of N doping |
-
2020
- 2020-09-11 CN CN202010952848.XA patent/CN112077332A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20010009118A1 (en) * | 2000-01-21 | 2001-07-26 | Sumitomo Electric Industries, Ltd. And Sumitomo Electric Fine Polymer, Inc. | Method of producing alloy powders, alloy powders obtained by said method, and products applying said powders |
| US20050181202A1 (en) * | 2004-02-18 | 2005-08-18 | Hitachi Metals, Ltd. | Fine composite metal particles and their production method, micro-bodies, and magnetic beads |
| CN1773638A (en) * | 2005-11-10 | 2006-05-17 | 北京科技大学 | Method for producing magnetic powder by form method |
| CN105562005A (en) * | 2016-02-29 | 2016-05-11 | 复旦大学 | Nano composite material with carbon-coated Ni nano crystal particles loaded on graphene and preparation method of nano composite material |
| CN106041124A (en) * | 2016-07-18 | 2016-10-26 | 中北大学 | Preparation method of metal and metal oxide hollow microspheres with adjustable particle sizes |
| CN106180744A (en) * | 2016-08-25 | 2016-12-07 | 董晓 | A kind of preparation method of diamond composition pre-alloyed powder |
| CN110534762A (en) * | 2019-09-05 | 2019-12-03 | 中国科学院新疆理化技术研究所 | A kind of preparation method of cobalt and the 3-D ordered multiporous C catalyst of N doping |
Non-Patent Citations (2)
| Title |
|---|
| CONGAI HAN等: "Ultrafine FeNi3 Nanocrystals Embedded in 3D Honeycomb-Like Carbon Matrix for High-Performance Microwave Absorption", 《NANOMATERIALS》 * |
| 汪旭光, 冶金工业出版社 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115318296A (en) * | 2022-08-19 | 2022-11-11 | 广东工业大学 | High-dispersion film-shaped carbon-coated nickel catalyst and preparation method and application thereof |
| CN115318296B (en) * | 2022-08-19 | 2024-03-19 | 广东工业大学 | High-dispersion film-shaped carbon-coated nickel catalyst and preparation method and application thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107399735B (en) | Preparation method and application of graphene composite aerogel wave-absorbing material | |
| CN112195013B (en) | Method for synthesizing porous magnetic metal oxide/carbon composite wave-absorbing material | |
| CN112961650B (en) | Three-metal organic framework derived iron-nickel alloy/porous carbon ultrathin wave absorber and preparation method thereof | |
| CN107338024B (en) | Co-Fe alloy/carbon sphere composite microwave absorbent and preparation method thereof | |
| CN111138206B (en) | Amorphous carbon modified SiC nanowire continuous three-dimensional network structure wave-absorbing foam and preparation method thereof | |
| CN112077332A (en) | Carbon-coated magnetic metal simple substance composite material and preparation method and application thereof | |
| CN112479179B (en) | Preparation method of composite wave absorber based on biomass material | |
| CN113999651A (en) | Nickel-cobalt dual-ligand metal-organic framework material and preparation method and application thereof | |
| CN113163698A (en) | Honeycomb composite material and preparation method thereof | |
| CN110589797A (en) | Metal oxide three-dimensional honeycomb carbon material and preparation method thereof | |
| CN114980715B (en) | Composite porous microsphere material and preparation method and application thereof | |
| CN113845773B (en) | Sulfonic group doped microporous polyphenyl/polypyrrole composite material, and preparation method and application thereof | |
| CN113423256B (en) | Composite wave-absorbing material and preparation method and application thereof | |
| CN113061421B (en) | ZnO/N doped hollow dielectric wave-absorbing material and preparation method and application thereof | |
| CN114314679A (en) | Polypyrrole-coated ferroferric oxide nanoflower wave-absorbing material, preparation method and application | |
| CN110818950A (en) | Preparation method of magnetic wave-absorbing resin | |
| CN113754911B (en) | Environment-friendly electromagnetic shielding building material and preparation method thereof | |
| CN110723723B (en) | Two-dimensional carbon material loaded Fe 3 N-nanoparticle light wave-absorbing material and preparation method and application thereof | |
| CN114684802B (en) | Magnetic iron-cobalt-nickel alloy/carbon series composite wave-absorbing material and preparation method and application thereof | |
| CN116726816A (en) | Composite aerogel material and preparation method and application thereof | |
| CN113708085B (en) | Preparation method of nano porous carbon coated magnetic nanoparticle compound | |
| CN116605863A (en) | MOF-derived wood-based porous carbon wave-absorbing material and preparation method thereof | |
| CN115491178B (en) | CoFe (CoFe) 2 O 4 Preparation and application of mesoporous carbon core-shell wave-absorbing material | |
| CN112909235B (en) | Battery negative electrode material of binuclear molybdenum cluster compound and preparation method thereof | |
| CN115636443A (en) | Preparation method of magnetic nanoparticle coated microcapsule-shaped carbon-based composite material |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20201215 |