CN113084183B - Cunninghamia lanceolata leaf-shaped cobalt particles and method for preparing magnetic composite material by using same - Google Patents
Cunninghamia lanceolata leaf-shaped cobalt particles and method for preparing magnetic composite material by using same Download PDFInfo
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- CN113084183B CN113084183B CN202110285173.2A CN202110285173A CN113084183B CN 113084183 B CN113084183 B CN 113084183B CN 202110285173 A CN202110285173 A CN 202110285173A CN 113084183 B CN113084183 B CN 113084183B
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- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 title claims abstract description 78
- 239000010941 cobalt Substances 0.000 title claims abstract description 77
- 229910017052 cobalt Inorganic materials 0.000 title claims abstract description 77
- 239000002245 particle Substances 0.000 title claims abstract description 69
- 239000002131 composite material Substances 0.000 title claims abstract description 46
- 238000000034 method Methods 0.000 title claims abstract description 27
- 244000050510 Cunninghamia lanceolata Species 0.000 title description 6
- 239000011259 mixed solution Substances 0.000 claims abstract description 34
- 238000003756 stirring Methods 0.000 claims abstract description 20
- 238000001035 drying Methods 0.000 claims abstract description 17
- 239000000126 substance Substances 0.000 claims abstract description 15
- 239000000243 solution Substances 0.000 claims abstract description 14
- 238000002360 preparation method Methods 0.000 claims abstract description 12
- 238000002156 mixing Methods 0.000 claims abstract description 10
- 238000005406 washing Methods 0.000 claims abstract description 10
- 241000218645 Cedrus Species 0.000 claims abstract description 8
- 238000010438 heat treatment Methods 0.000 claims abstract description 8
- 238000006722 reduction reaction Methods 0.000 claims abstract description 8
- 238000006243 chemical reaction Methods 0.000 claims abstract description 7
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 7
- 150000001868 cobalt Chemical class 0.000 claims abstract description 7
- 239000008139 complexing agent Substances 0.000 claims abstract description 7
- 239000007791 liquid phase Substances 0.000 claims abstract description 7
- 238000004519 manufacturing process Methods 0.000 claims abstract description 7
- 239000002904 solvent Substances 0.000 claims abstract description 7
- 238000010992 reflux Methods 0.000 claims abstract description 6
- 238000009833 condensation Methods 0.000 claims abstract description 3
- 230000005494 condensation Effects 0.000 claims abstract description 3
- 229920000642 polymer Polymers 0.000 claims description 21
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 18
- 239000008367 deionised water Substances 0.000 claims description 11
- 229910021641 deionized water Inorganic materials 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 claims description 8
- KAESVJOAVNADME-UHFFFAOYSA-N Pyrrole Chemical compound C=1C=CNC=1 KAESVJOAVNADME-UHFFFAOYSA-N 0.000 claims description 8
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 8
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 8
- 229920013636 polyphenyl ether polymer Polymers 0.000 claims description 7
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 6
- 230000004048 modification Effects 0.000 claims description 6
- 238000012986 modification Methods 0.000 claims description 6
- 239000000178 monomer Substances 0.000 claims description 6
- 229940011182 cobalt acetate Drugs 0.000 claims description 5
- QAHREYKOYSIQPH-UHFFFAOYSA-L cobalt(II) acetate Chemical compound [Co+2].CC([O-])=O.CC([O-])=O QAHREYKOYSIQPH-UHFFFAOYSA-L 0.000 claims description 5
- KWSLGOVYXMQPPX-UHFFFAOYSA-N 5-[3-(trifluoromethyl)phenyl]-2h-tetrazole Chemical compound FC(F)(F)C1=CC=CC(C2=NNN=N2)=C1 KWSLGOVYXMQPPX-UHFFFAOYSA-N 0.000 claims description 4
- YTPLMLYBLZKORZ-UHFFFAOYSA-N Thiophene Chemical compound C=1C=CSC=1 YTPLMLYBLZKORZ-UHFFFAOYSA-N 0.000 claims description 4
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 4
- 239000003960 organic solvent Substances 0.000 claims description 4
- 239000007800 oxidant agent Substances 0.000 claims description 4
- 230000001590 oxidative effect Effects 0.000 claims description 4
- -1 polyarylethernitrile Polymers 0.000 claims description 4
- 229940057847 polyethylene glycol 600 Drugs 0.000 claims description 4
- 229910001379 sodium hypophosphite Inorganic materials 0.000 claims description 4
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 4
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 claims description 3
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims description 3
- 239000004696 Poly ether ether ketone Substances 0.000 claims description 3
- 239000004642 Polyimide Substances 0.000 claims description 3
- 150000001412 amines Chemical class 0.000 claims description 3
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims description 3
- 229920001568 phenolic resin Polymers 0.000 claims description 3
- 239000005011 phenolic resin Substances 0.000 claims description 3
- 229920002530 polyetherether ketone Polymers 0.000 claims description 3
- 229940068918 polyethylene glycol 400 Drugs 0.000 claims description 3
- 229920001721 polyimide Polymers 0.000 claims description 3
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 3
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 3
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 2
- 239000004280 Sodium formate Substances 0.000 claims description 2
- 150000001413 amino acids Chemical class 0.000 claims description 2
- SRSXLGNVWSONIS-UHFFFAOYSA-N benzenesulfonic acid Chemical compound OS(=O)(=O)C1=CC=CC=C1 SRSXLGNVWSONIS-UHFFFAOYSA-N 0.000 claims description 2
- 229940092714 benzenesulfonic acid Drugs 0.000 claims description 2
- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 claims description 2
- 229910000361 cobalt sulfate Inorganic materials 0.000 claims description 2
- 229940044175 cobalt sulfate Drugs 0.000 claims description 2
- KTVIXTQDYHMGHF-UHFFFAOYSA-L cobalt(2+) sulfate Chemical compound [Co+2].[O-]S([O-])(=O)=O KTVIXTQDYHMGHF-UHFFFAOYSA-L 0.000 claims description 2
- WLQXLCXXAPYDIU-UHFFFAOYSA-L cobalt(2+);disulfamate Chemical compound [Co+2].NS([O-])(=O)=O.NS([O-])(=O)=O WLQXLCXXAPYDIU-UHFFFAOYSA-L 0.000 claims description 2
- 229940113115 polyethylene glycol 200 Drugs 0.000 claims description 2
- HLBBKKJFGFRGMU-UHFFFAOYSA-M sodium formate Chemical compound [Na+].[O-]C=O HLBBKKJFGFRGMU-UHFFFAOYSA-M 0.000 claims description 2
- 235000019254 sodium formate Nutrition 0.000 claims description 2
- 229930192474 thiophene Natural products 0.000 claims description 2
- 229940024606 amino acid Drugs 0.000 claims 1
- 150000008107 benzenesulfonic acids Chemical class 0.000 claims 1
- 239000007787 solid Substances 0.000 abstract description 10
- 239000011256 inorganic filler Substances 0.000 abstract description 5
- 229910003475 inorganic filler Inorganic materials 0.000 abstract description 5
- 229910052751 metal Inorganic materials 0.000 abstract description 5
- 239000002184 metal Substances 0.000 abstract description 5
- 239000002202 Polyethylene glycol Substances 0.000 abstract description 2
- 238000009835 boiling Methods 0.000 abstract description 2
- 239000000696 magnetic material Substances 0.000 abstract description 2
- 229920001223 polyethylene glycol Polymers 0.000 abstract description 2
- 239000004094 surface-active agent Substances 0.000 abstract description 2
- 229910000859 α-Fe Inorganic materials 0.000 abstract description 2
- 239000003822 epoxy resin Substances 0.000 description 12
- 229920000647 polyepoxide Polymers 0.000 description 12
- 239000000758 substrate Substances 0.000 description 6
- JOXIMZWYDAKGHI-UHFFFAOYSA-N toluene-4-sulfonic acid Chemical compound CC1=CC=C(S(O)(=O)=O)C=C1 JOXIMZWYDAKGHI-UHFFFAOYSA-N 0.000 description 6
- 230000008569 process Effects 0.000 description 5
- 239000013078 crystal Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000011159 matrix material Substances 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 238000003760 magnetic stirring Methods 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- 238000002791 soaking Methods 0.000 description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 229910000365 copper sulfate Inorganic materials 0.000 description 2
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 description 2
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 239000010954 inorganic particle Substances 0.000 description 2
- 150000002825 nitriles Chemical class 0.000 description 2
- 229920000620 organic polymer Polymers 0.000 description 2
- 238000007747 plating Methods 0.000 description 2
- 229920000090 poly(aryl ether) Polymers 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 230000002194 synthesizing effect Effects 0.000 description 2
- GDDNTTHUKVNJRA-UHFFFAOYSA-N 3-bromo-3,3-difluoroprop-1-ene Chemical group FC(F)(Br)C=C GDDNTTHUKVNJRA-UHFFFAOYSA-N 0.000 description 1
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 239000003109 Disodium ethylene diamine tetraacetate Substances 0.000 description 1
- ZGTMUACCHSMWAC-UHFFFAOYSA-L EDTA disodium salt (anhydrous) Chemical compound [Na+].[Na+].OC(=O)CN(CC([O-])=O)CCN(CC(O)=O)CC([O-])=O ZGTMUACCHSMWAC-UHFFFAOYSA-L 0.000 description 1
- 239000004952 Polyamide Substances 0.000 description 1
- 239000004721 Polyphenylene oxide Substances 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000000295 complement effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 229920001940 conductive polymer Polymers 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 235000019301 disodium ethylene diamine tetraacetate Nutrition 0.000 description 1
- 238000012377 drug delivery Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000009713 electroplating Methods 0.000 description 1
- 229920006351 engineering plastic Polymers 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 239000002085 irritant Substances 0.000 description 1
- 231100000021 irritant Toxicity 0.000 description 1
- 239000006249 magnetic particle Substances 0.000 description 1
- 230000005415 magnetization Effects 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 239000002923 metal particle Substances 0.000 description 1
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 1
- 239000013081 microcrystal Substances 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000002135 nanosheet Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- PIBWKRNGBLPSSY-UHFFFAOYSA-L palladium(II) chloride Chemical compound Cl[Pd]Cl PIBWKRNGBLPSSY-UHFFFAOYSA-L 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 238000005191 phase separation Methods 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
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- 229920002647 polyamide Polymers 0.000 description 1
- 229920000767 polyaniline Polymers 0.000 description 1
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- 238000006116 polymerization reaction Methods 0.000 description 1
- 229920006380 polyphenylene oxide Polymers 0.000 description 1
- 229920000128 polypyrrole Polymers 0.000 description 1
- LJCNRYVRMXRIQR-OLXYHTOASA-L potassium sodium L-tartrate Chemical compound [Na+].[K+].[O-]C(=O)[C@H](O)[C@@H](O)C([O-])=O LJCNRYVRMXRIQR-OLXYHTOASA-L 0.000 description 1
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- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
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- 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
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
-
- B22F1/0007—
-
- 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
- B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
- B22F1/102—Metallic powder coated with organic material
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
- H01F1/04—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
- H01F1/06—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys in the form of particles, e.g. powder
- H01F1/068—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys in the form of particles, e.g. powder having a L10 crystallographic structure, e.g. [Co,Fe][Pt,Pd] (nano)particles
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
- H01F41/0253—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets
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- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
A folium cedar leaf-shaped cobalt particle and a method for preparing a magnetic composite material by using the same, belonging to the technical field of composite material preparation. The method comprises the following steps: 1) adding cobalt salt, an alkaline substance, a complexing agent and a reducing agent into a solvent, and uniformly stirring and mixing to obtain a mixed solution A; 2) and transferring the mixed solution A into a round-bottom flask connected with a condensation reflux device, heating to 250 ℃, keeping the solution boiling for carrying out high-temperature liquid-phase reduction reaction, and after the reaction is finished, separating, washing and drying solid substances in a system to obtain the fir leaf-shaped cobalt particles. According to the invention, polyethylene glycol is used as a solvent, and the cobalt particles with uniform dispersity and good shape control can be obtained without a surfactant and special experimental equipment; the metal cobalt particles are adopted to replace conventional magnetic materials such as ferrite and the like as inorganic fillers, and the prepared magnetic composite material has the advantages of low mass density and high magnetic conductivity and can be used for manufacturing electromagnetic shielding layers of embedded inductance magnetic cores and electronic components in printed circuit boards.
Description
Technical Field
The invention belongs to the technical field of composite material preparation, and particularly relates to a folium cedar leaf-shaped cobalt particle and a method for preparing a magnetic composite material by using the same.
Background
As a typical magnetic metal material, cobalt has high specific saturation magnetization, high Curie temperature and good oxidation resistance, and has wide application value in the fields of catalysis, drug delivery, magnetic recording, permanent magnet materials and the like. Meanwhile, researchers find that the shape, size and crystal structure of the metal cobalt particles have significant influence on the physical and chemical properties of the metal cobalt particles, for example, the electromagnetic performance of cobalt magnetic particles with special shapes (such as chains, sheets, flowers and spikes) is often superior to that of spherical shapes, so that the method has important significance for preparing the cobalt particles with the special shapes. The literature, Solvothermal Synthesis and catalysis of cobalt with simple structures [ Journal of Alloys and Compounds, 513(2012) 245- ] synthesizes a three-dimensional radial cobalt simple substance with leaves as a basic structural unit by adding ethylenediamine as a structure-directing agent in the hydrothermal Synthesis process, but ethylenediamine is a flammable and explosive substance, generates smoke in the air and simultaneously generates an irritant odor, and has potential safety hazard in the preparation process. The literature, "Synthesis and Characterization of Novel Three-Dimensional Co depletion super Reduction Route" Crystal Growth & Design, 8(2008) 1113-. In the literature, "Flower-like cobalt nanoparticles by a complex precusor reaction route" (Materials Chemistry and Physics 91 (2005)) 293-. In the document of simple synthesis of leaf-like cobalt at low temperature [ Micro & Nano Letters, 9(2014) 312-. In documents of research on preparation of nano Co powder by a liquid phase reduction method and catalytic performance thereof [ hi-tech, 12(2016)1004-7344 ] and influence of dendritic nano cobalt microcrystals on thermal decomposition of ammonium perchlorate [ functional materials, 1(2007)148-151 ], micron-scale lamellar leaf-shaped cobalt particles assembled by nanosheets are prepared by a liquid phase reduction method, but the product particle size and the morphology are not uniform, and the dispersibility is poor.
The cobalt metal particles are usually mixed with high molecular polymers to prepare magnetic composite materials so as to expand the application field of the magnetic composite materials, but in the blending and forming process of inorganic/organic composite material systems, the interaction between inorganic particles and organic polymers is weak, so that the phenomena of phase separation and local agglomeration between inorganic fillers and organic matrixes are easily caused. Document "deicing performance of epoxy resin/cobalt powder composite material based on eddy current heating" (synthetic resin and plastic, 6(2019) 23-26) an epoxy resin/cobalt composite material is prepared by using cobalt particles as a magnetic conductive component and epoxy resin as a matrix, but the viscosity of the epoxy resin matrix is too high to uniformly disperse the cobalt particles, and the material is easy to cause an undesirable joule heating effect in the working process, so that a multi-component filler is required to be added to improve the performance of the composite material, and finally the production cost is increased. Documents "preparation and performance of cobalt-based self-repairing polyamide conductive polymer material" (engineering plastic application, 11(2017) 1-6) report that metal cobalt particles are used as inorganic filler to prepare magnetic composite materials, but the problem of interfaces between inorganic particles and organic polymers is not considered in the process, so that the reliability of products made of the composite materials cannot be guaranteed in the working state, and the products are not suitable for being equipped with certain special electronic equipment.
Disclosure of Invention
The invention aims to provide a folium cedar-shaped cobalt particle and a method for manufacturing a magnetic composite material by using the same, aiming at the problems in the background art.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a preparation method of folium cedar leaf-shaped cobalt particles is characterized by comprising the following steps:
and 2, transferring the mixed solution A obtained in the step 1 to a round-bottom flask connected with a condensation reflux device, heating to 220-280 ℃, keeping the solution boiling for high-temperature liquid-phase reduction reaction, and after the reaction is finished, separating, washing and drying solid substances in the system to obtain the fir leaf-shaped cobalt particles.
Further, the solvent in step 1 is one or more of polyethylene glycol 200, polyethylene glycol 400 or polyethylene glycol 600.
Further, the cobalt salt in the step 1 is one or more of cobalt sulfate, cobalt acetate, cobalt chloride or cobalt sulfamate; the alkaline substance is one or more of sodium hydroxide, potassium hydroxide or organic amine; the complexing agent is one or more of amino acid, benzenesulfonic acid and derivatives thereof; the reducing agent is one or more of sodium formate, sodium hypophosphite or hydrazine hydrate.
Further, the time of the high-temperature liquid phase reduction reaction in the step 2 is 1-8 h; the drying temperature is 40-100 ℃, and the drying time is 1-24 h.
The magnetic composite material is characterized by comprising 5-80 wt% of folium cedar-like cobalt particles and 20-95 wt% of high polymer, wherein the folium cedar-like cobalt particles are prepared by the method, and the high polymer is one of polyphenyl ether, polyarylether nitrile, phenolic resin, polytetrafluoroethylene, polyimide or polyetheretherketone.
A preparation method of a magnetic composite material is characterized by comprising the following steps;
2.1 adding the folium cedar-like cobalt particles prepared in the step 1 into deionized water to obtain a mixed solution B with the concentration of 1-5 g/L;
2.2 adding a polymer monomer into the mixed solution B obtained in the step 2.1, and uniformly stirring and mixing to obtain a mixed solution C; in the mixed solution C, the concentration of the polymer monomer is 0.1-5 ml/L;
2.3, dropwise adding an oxidant into the mixed solution C obtained in the step 2.2, continuously stirring at room temperature for polymerization reaction for 12 hours, and after the reaction is finished, separating, washing and drying solid matters in a system to obtain modified folium cedar leaf-shaped cobalt particles;
step 3, preparing the magnetic composite material:
3.1 adding the high molecular polymer into an organic solvent, and uniformly stirring and mixing to obtain a polymer solution with the concentration of 10-100 g/L;
3.2 adding the modified folium cedar-like cobalt particles obtained in the step 2 into the polymer solution, and uniformly stirring and mixing to obtain a mixed solution D; in the mixed solution D, the concentration of the modified folium cedar leaf-shaped cobalt particles is 1-200 g/L;
and 3.3, curing the mixed solution D to obtain the magnetic composite material.
Further, the polymer monomer in step 2 is one of thiophene, aniline, and pyrrole.
Further, the oxidant in the step 2 is ammonium persulfate, and the concentration is 1-30 g/L.
Further, in the step 2, the drying temperature is 40-100 ℃, and the drying time is 1-24 hours.
Further, the high molecular polymer in step 3 is one of polyphenylene oxide, polyarylether nitrile, epoxy resin, phenolic resin, polytetrafluoroethylene, polyimide and polyetheretherketone; the organic solvent is one of N-methyl pyrrolidone and tetrahydrofuran; the curing treatment temperature is 25-200 ℃, and the curing time is 1-12 h.
According to the folium cedar-shaped cobalt particles and the method for manufacturing the magnetic composite material by using the folium cedar-shaped cobalt particles, the folium cedar-shaped cobalt particles are subjected to surface modification treatment, so that the cobalt particles can be uniformly dispersed in a high-molecular polymer matrix, a polymer formed by the surface modification treatment can be adsorbed on the surfaces of the cobalt particles in a chemical bond form, and the problem of interface incompatibility between the cobalt particles as an inorganic filler and the high-molecular polymer matrix is finally solved.
Compared with the prior art, the invention has the beneficial effects that:
1. according to the preparation method of the folium cedar-like cobalt particles, polyethylene glycol is used as a solvent, and the cobalt particles with uniform dispersity and good shape control can be obtained without a surfactant and special experimental equipment.
2. The invention adopts the metal cobalt particles to replace the conventional magnetic materials such as ferrite and the like as the inorganic filler, and the prepared magnetic composite material has the advantages of low mass density and high magnetic conductivity, and can be used for manufacturing the electromagnetic shielding layer of the embedded inductance magnetic core and the electronic element in the printed circuit board.
3. The folium cedar-shaped cobalt particles and the method for preparing the magnetic composite material by using the folium cedar-shaped cobalt particles have the advantages of simple preparation process, low equipment dependence, mild condition, environmental friendliness, low cost and easiness in realizing large-scale industrial production.
Drawings
FIG. 1 is a scanning electron microscope photograph of cobalt particles prepared in example 1;
FIG. 2 is an X-ray diffraction peak pattern of cobalt particles prepared in example 1;
FIG. 3 is a scanning electron microscope photograph of cobalt particles prepared in example 2;
FIG. 4 is a diagram showing an embodiment of an air core embedded inductor in example 3;
FIG. 5 is a pictorial representation of the magnetic composite material prepared in example 3 used as a magnetic core for an embedded inductor;
FIG. 6 shows the inductance of the magnetic composite material obtained in example 3 after it is used as an embedded inductor core.
Detailed Description
So that those skilled in the art can better understand the principle and the scheme of the present invention, the following detailed description is given with reference to the accompanying drawings and the specific embodiments.
Example 1
A preparation method of folium Cunninghamiae Lanceolatae leaf-shaped cobalt particles comprises the following steps:
1) dissolving 0.125g of cobalt acetate, 0.1g of p-toluenesulfonic acid and 0.1g of sodium hydroxide in 50ml of polyethylene glycol 400, adding 0.5g of sodium hypophosphite after fully dissolving by magnetic stirring, and continuously stirring to obtain a uniform mixed solution;
2) adding the mixed solution into a 100ml round-bottom flask, heating to 250 ℃, refluxing for 4h, naturally cooling to room temperature, and separating by using a magnet to obtain a product; and washing the product with deionized water and absolute ethyl alcohol for multiple times, and drying in an oven at 60 ℃ for 12h to obtain the magnetic solid particles.
The microscopic morphology of the magnetic solid cobalt particles prepared in the embodiment 1 of the invention is shown in fig. 1, and the result shows that the microscopic morphology of the prepared sample is in a shape of Chinese fir leaves; the X-ray diffraction peak pattern of the prepared magnetic solid cobalt particles is shown in figure 2, and the result shows that the prepared sample is simple substance cobalt with a pure hcp phase structure.
Example 2
A Chinese fir leaf-shaped cobalt particle and a method for preparing a magnetic composite material by using the same are disclosed, and the specific implementation steps are as follows:
1) Dissolving 1.25g of cobalt acetate, 1g of p-toluenesulfonic acid and 0.4g of sodium hydroxide in 50ml of polyethylene glycol 600, adding 2ml of hydrazine hydrate after fully dissolving by magnetic stirring, and continuously stirring to obtain a uniform mixed solution;
2) adding the mixed solution into a 100ml round-bottom flask, heating to 250 ℃, refluxing for 4h, naturally cooling to room temperature, and separating to obtain a product; washing the product with deionized water and absolute ethyl alcohol for multiple times, and drying in an oven at 60 ℃ for 12h to obtain magnetic solid cobalt particles;
1) Dissolving 5g of the magnetic cobalt particles prepared in the step 1 in 2L of deionized water, fully stirring, adding 5ml of aniline to form a uniform mixed solution, adding 15g of ammonium persulfate into the mixed solution, continuously stirring at normal temperature for 12h, filtering and washing the mixed solution, and drying the product in a 60 ℃ drying oven for 12h to obtain magnetic cobalt particles with the polyaniline polymerized on the surface;
2) dissolving 2g of polyphenyl ether resin in 20ml of tetrahydrofuran, violently stirring to prepare a uniform solution system, adding 1g of magnetic cobalt particles with aniline polymerized on the surface into the solution system to prepare a uniform mixed system, pouring the mixed system into a mold, and curing at the normal temperature of 25 ℃ for 6 hours to obtain a solid magnetic composite material;
the micro-topography of the cunninghamia lanceolata leaf-shaped cobalt particles synthesized in the embodiment 2 of the invention is shown in fig. 3.
Example 3
A Chinese fir leaf-shaped cobalt particle and a method for preparing a magnetic composite material by using the same are disclosed, and the specific implementation steps are as follows: step 1, synthesizing fir leaf-shaped magnetic cobalt particles
1) Dissolving 1g of cobalt acetate, 1g of p-toluenesulfonic acid and 1g of sodium hydroxide in 50ml of polyethylene glycol 600, adding 0.5g of sodium hypophosphite after fully dissolving by magnetic stirring, and continuously stirring to obtain a uniform mixed solution;
2) adding the mixed solution into a 100ml round-bottom flask, heating and refluxing for 2h, naturally cooling to room temperature, and separating by using a magnet to obtain a product; washing the product with deionized water and absolute ethyl alcohol for multiple times, and drying in a 60 ℃ drying oven for 12h to obtain magnetic solid particles;
1) Dissolving 5g of the magnetic cobalt particles prepared in the step 1 in 2L of deionized water, fully stirring, adding 5ml of pyrrole to form a uniform mixed solution, adding 15g of ammonium persulfate into the mixed solution, continuously stirring at normal temperature for 12h, filtering and washing the mixed solution, and drying the product in a 60 ℃ drying oven for 12h to obtain magnetic cobalt particles with polypyrrole on the surface;
2) dissolving 2g of polyphenyl ether resin in 20ml of tetrahydrofuran, violently stirring to prepare a uniform solution system, adding 1g of magnetic cobalt particles with pyrrole polymerized on the surface into the solution system to prepare a uniform mixed system, pouring the mixed system into a mould, and curing at 100 ℃ for 3 hours to obtain a solid magnetic composite material;
step 3, manufacturing the printed circuit embedded inductor by using the magnetic composite material as the magnetic core
1) Covering a resist of a negative image inductance coil pattern on the surface of the epoxy resin substrate, wherein the inductance coils on the upper surface and the lower surface are complementary in a reverse direction; soaking the epoxy resin substrate covered with the resist in an activation solution consisting of 60mg/L palladium chloride, 5% sulfuric acid by volume percentage concentration and deionized water for 5min, and depositing required catalytic seed crystals on the surface of the substrate; soaking the epoxy resin substrate with the catalytic seed crystal deposited on the surface in a copper plating solution consisting of 25g/L copper chloride, 20g/L copper sulfate, 4g/L formaldehyde, 20g/L disodium ethylenediamine tetraacetate, 10g/L potassium sodium tartrate, 15g/L sodium hydroxide and deionized water at 50 ℃ for 10min to complete a chemical copper plating process, and forming a conductive double-layer spiral coil on the epoxy resin substrate; electroplating the epoxy resin plate in a solution consisting of 75g/L copper sulfate, 240g/L concentrated sulfuric acid, 60mg/L chloride ions and deionized water for 60min, wherein the current density is 2A/dm2Increasing the thickness of the inductance coil; soaking the electroplated epoxy resin substrate in an etching solution consisting of 100g/L copper chloride, 100g/L ammonia chloride, 600g/L ammonia water and deionized water for 1min to remove the resist, thereby obtaining the printed circuit embedded inductance coil;
2) milling an epoxy resin base material in the center of the coil without damaging the inductance coil, and embedding the magnetic composite material prepared in the step 2 at the milled position;
3) solidifying a layer of polyphenyl ether on the surface of the inductor structure embedded with the magnetic composite material, covering the magnetic composite material prepared in the step (2) on the polyphenyl ether by a hot pressing method, and solidifying a layer of polyphenyl ether on the surface of the magnetic composite material to form the printed circuit embedded inductor;
a real image of the air core embedded inductor manufactured in example 3 is shown in fig. 4; the physical diagram of the magnetic composite material used as the embedded inductance core is shown in FIG. 5; the inductance value of the magnetic composite material obtained after being used as the embedded inductor core is shown in fig. 6.
While the preferred embodiments of the present invention have been described and illustrated in the accompanying drawings, the technical scope of the present invention should not be limited to the description, and various modifications thereof by those skilled in the art without departing from the technical spirit of the present invention and the scope of the appended claims should fall within the scope of the present invention, and all modifications made thereto within the scope of the present invention are intended to be protected by the present invention.
Claims (9)
1. A preparation method of folium cedar leaf-shaped cobalt particles is characterized by comprising the following steps:
step 1, adding cobalt salt, an alkaline substance, a complexing agent and a reducing agent into a solvent, and uniformly stirring and mixing to obtain a mixed solution A; wherein the concentration of the cobalt salt is 0.01-1 mol/L, the concentration of the alkaline substance is 0.01-3 mol/L, the concentration of the complexing agent is 0.01-4 mol/L, and the concentration of the reducing agent is 0.01-4 mol/L; the complexing agent is one or more of amino acid, benzenesulfonic acid and benzenesulfonic acid derivatives, and the solvent is one or more of polyethylene glycol 200, polyethylene glycol 400 or polyethylene glycol 600;
and 2, transferring the mixed solution A obtained in the step 1 to a round-bottom flask connected with a condensation reflux device, heating to 220-280 ℃, carrying out high-temperature liquid-phase reduction reaction, and after the reaction is finished, separating, washing and drying to obtain the fir leaf-shaped cobalt particles.
2. The method for preparing folium Cunninghamiae Lanceolatae leaf-like cobalt particles according to claim 1, wherein the cobalt salt in step 1 is one or more of cobalt sulfate, cobalt acetate, cobalt chloride or cobalt sulfamate; the alkaline substance is one or more of sodium hydroxide, potassium hydroxide or organic amine; the reducing agent is one or more of sodium formate, sodium hypophosphite or hydrazine hydrate.
3. The method for preparing folium Cunninghamiae Lanceolatae leaf-like cobalt particles according to claim 1, wherein the time of the high temperature liquid phase reduction reaction in step 2 is 1-8 h.
4. A magnetic composite material, characterized by comprising 5 wt% -80 wt% of folium cedar-like cobalt particles and 20 wt% -95 wt% of high molecular polymer, wherein the folium cedar-like cobalt particles are prepared by the method of any one of claims 1 to 3, and the high molecular polymer is one of polyphenyl ether, polyarylethernitrile, phenolic resin, polytetrafluoroethylene, polyimide or polyetheretherketone.
5. A method of making a magnetic composite material as claimed in claim 4, comprising the steps of;
step 1, preparing fir leaf-shaped cobalt particles;
step 2, surface modification treatment of the fir leaf-shaped cobalt particles:
2.1 adding the folium cedar-like cobalt particles prepared in the step 1 into deionized water to obtain a mixed solution B with the concentration of 1-5 g/L;
2.2 adding a polymer monomer into the mixed solution B obtained in the step 2.1, and uniformly stirring and mixing to obtain a mixed solution C; in the mixed solution C, the concentration of the polymer monomer is 0.1-5 ml/L;
2.3, adding an oxidant into the mixed solution C obtained in the step 2.2, stirring for reaction, and after the reaction is finished, separating, washing and drying to obtain modified folium cedar leaf-shaped cobalt particles;
step 3, preparing the magnetic composite material:
3.1 adding the high molecular polymer into an organic solvent, and uniformly stirring and mixing to obtain a polymer solution with the concentration of 10-100 g/L;
3.2 adding the modified folium cedar-like cobalt particles obtained in the step 2 into the polymer solution, and uniformly stirring and mixing to obtain a mixed solution D; in the mixed solution D, the concentration of the modified folium cedar leaf-shaped cobalt particles is 1-200 g/L;
and 3.3, curing the mixed solution D to obtain the magnetic composite material.
6. The method for preparing a magnetic composite material according to claim 5, wherein the polymer monomer in step 2 is one of thiophene, aniline and pyrrole.
7. The preparation method of the magnetic composite material according to claim 5, wherein the oxidant in the step 2 is ammonium persulfate, and the concentration is 1-30 g/L.
8. The method for preparing a magnetic composite material according to claim 5, wherein the organic solvent is one of N-methylpyrrolidone and tetrahydrofuran.
9. The method for preparing the magnetic composite material according to claim 5, wherein the curing treatment temperature is 25-200 ℃ and the curing time is 1-12 h.
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