CN117645853A - Adhesive for nanocrystalline magnetic core and preparation method thereof - Google Patents
Adhesive for nanocrystalline magnetic core and preparation method thereof Download PDFInfo
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- CN117645853A CN117645853A CN202311534646.3A CN202311534646A CN117645853A CN 117645853 A CN117645853 A CN 117645853A CN 202311534646 A CN202311534646 A CN 202311534646A CN 117645853 A CN117645853 A CN 117645853A
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- epoxy acrylate
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- 239000000853 adhesive Substances 0.000 title claims abstract description 43
- 230000001070 adhesive effect Effects 0.000 title claims abstract description 43
- 238000002360 preparation method Methods 0.000 title claims abstract description 36
- KCTAWXVAICEBSD-UHFFFAOYSA-N prop-2-enoyloxy prop-2-eneperoxoate Chemical class C=CC(=O)OOOC(=O)C=C KCTAWXVAICEBSD-UHFFFAOYSA-N 0.000 claims abstract description 72
- 238000004132 cross linking Methods 0.000 claims abstract description 38
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000002131 composite material Substances 0.000 claims abstract description 26
- 239000000945 filler Substances 0.000 claims abstract description 15
- 239000013589 supplement Substances 0.000 claims abstract description 13
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 12
- 239000000203 mixture Substances 0.000 claims description 95
- 238000003756 stirring Methods 0.000 claims description 65
- 238000006243 chemical reaction Methods 0.000 claims description 42
- 239000011230 binding agent Substances 0.000 claims description 35
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 31
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 30
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 30
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 27
- 238000005303 weighing Methods 0.000 claims description 23
- 238000010438 heat treatment Methods 0.000 claims description 22
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 21
- 239000002904 solvent Substances 0.000 claims description 21
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 20
- 239000008367 deionised water Substances 0.000 claims description 20
- 229910021641 deionized water Inorganic materials 0.000 claims description 20
- AEMRFAOFKBGASW-UHFFFAOYSA-N Glycolic acid Chemical compound OCC(O)=O AEMRFAOFKBGASW-UHFFFAOYSA-N 0.000 claims description 18
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 18
- BAPJBEWLBFYGME-UHFFFAOYSA-N Methyl acrylate Chemical compound COC(=O)C=C BAPJBEWLBFYGME-UHFFFAOYSA-N 0.000 claims description 18
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 18
- WGYKZJWCGVVSQN-UHFFFAOYSA-N propylamine Chemical compound CCCN WGYKZJWCGVVSQN-UHFFFAOYSA-N 0.000 claims description 18
- 238000001035 drying Methods 0.000 claims description 16
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 14
- 238000001816 cooling Methods 0.000 claims description 14
- 238000001914 filtration Methods 0.000 claims description 14
- 239000011259 mixed solution Substances 0.000 claims description 14
- 239000000243 solution Substances 0.000 claims description 13
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 12
- -1 polytetrafluoroethylene Polymers 0.000 claims description 12
- 239000000758 substrate Substances 0.000 claims description 12
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 11
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 11
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 11
- 239000003822 epoxy resin Substances 0.000 claims description 10
- 229920000647 polyepoxide Polymers 0.000 claims description 10
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 10
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 10
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 claims description 9
- MQIUGAXCHLFZKX-UHFFFAOYSA-N Di-n-octyl phthalate Natural products CCCCCCCCOC(=O)C1=CC=CC=C1C(=O)OCCCCCCCC MQIUGAXCHLFZKX-UHFFFAOYSA-N 0.000 claims description 9
- 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 9
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 claims description 9
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 9
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 9
- BJQHLKABXJIVAM-UHFFFAOYSA-N bis(2-ethylhexyl) phthalate Chemical compound CCCCC(CC)COC(=O)C1=CC=CC=C1C(=O)OCC(CC)CCCC BJQHLKABXJIVAM-UHFFFAOYSA-N 0.000 claims description 9
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 claims description 9
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical compound CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 claims description 9
- 239000004202 carbamide Substances 0.000 claims description 9
- 239000008103 glucose Substances 0.000 claims description 9
- IWDCLRJOBJJRNH-UHFFFAOYSA-N p-cresol Chemical compound CC1=CC=C(O)C=C1 IWDCLRJOBJJRNH-UHFFFAOYSA-N 0.000 claims description 9
- 239000000244 polyoxyethylene sorbitan monooleate Substances 0.000 claims description 9
- 235000010482 polyoxyethylene sorbitan monooleate Nutrition 0.000 claims description 9
- 229940068968 polysorbate 80 Drugs 0.000 claims description 9
- 229920000053 polysorbate 80 Polymers 0.000 claims description 9
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 9
- 239000012498 ultrapure water Substances 0.000 claims description 9
- 239000004593 Epoxy Substances 0.000 claims description 8
- 239000007864 aqueous solution Substances 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 8
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 7
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 7
- 230000006837 decompression Effects 0.000 claims description 7
- 230000018044 dehydration Effects 0.000 claims description 7
- 238000006297 dehydration reaction Methods 0.000 claims description 7
- 238000001704 evaporation Methods 0.000 claims description 7
- 238000004108 freeze drying Methods 0.000 claims description 7
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 7
- 239000002244 precipitate Substances 0.000 claims description 7
- 238000002390 rotary evaporation Methods 0.000 claims description 7
- 239000006228 supernatant Substances 0.000 claims description 7
- 238000009210 therapy by ultrasound Methods 0.000 claims description 7
- 238000002604 ultrasonography Methods 0.000 claims description 7
- 238000005406 washing Methods 0.000 claims description 7
- 239000003963 antioxidant agent Substances 0.000 claims description 6
- 230000003078 antioxidant effect Effects 0.000 claims description 6
- 239000003999 initiator Substances 0.000 claims description 6
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 4
- NLZUEZXRPGMBCV-UHFFFAOYSA-N Butylhydroxytoluene Chemical compound CC1=CC(C(C)(C)C)=C(O)C(C(C)(C)C)=C1 NLZUEZXRPGMBCV-UHFFFAOYSA-N 0.000 claims description 4
- 235000010354 butylated hydroxytoluene Nutrition 0.000 claims description 4
- XMNIXWIUMCBBBL-UHFFFAOYSA-N 2-(2-phenylpropan-2-ylperoxy)propan-2-ylbenzene Chemical compound C=1C=CC=CC=1C(C)(C)OOC(C)(C)C1=CC=CC=C1 XMNIXWIUMCBBBL-UHFFFAOYSA-N 0.000 claims description 3
- 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 3
- SJECZPVISLOESU-UHFFFAOYSA-N 3-trimethoxysilylpropan-1-amine Chemical compound CO[Si](OC)(OC)CCCN SJECZPVISLOESU-UHFFFAOYSA-N 0.000 claims description 2
- XDLMVUHYZWKMMD-UHFFFAOYSA-N 3-trimethoxysilylpropyl 2-methylprop-2-enoate Chemical compound CO[Si](OC)(OC)CCCOC(=O)C(C)=C XDLMVUHYZWKMMD-UHFFFAOYSA-N 0.000 claims description 2
- 229910021529 ammonia Inorganic materials 0.000 claims description 2
- 150000008064 anhydrides Chemical class 0.000 claims description 2
- 150000002576 ketones Chemical class 0.000 claims description 2
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 claims description 2
- 230000007935 neutral effect Effects 0.000 claims description 2
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 claims description 2
- 229920003169 water-soluble polymer Polymers 0.000 claims description 2
- NKJOXAZJBOMXID-UHFFFAOYSA-N 1,1'-Oxybisoctane Chemical compound CCCCCCCCOCCCCCCCC NKJOXAZJBOMXID-UHFFFAOYSA-N 0.000 claims 1
- YUYCVXFAYWRXLS-UHFFFAOYSA-N trimethoxysilane Chemical compound CO[SiH](OC)OC YUYCVXFAYWRXLS-UHFFFAOYSA-N 0.000 claims 1
- 239000006247 magnetic powder Substances 0.000 abstract description 2
- 230000004048 modification Effects 0.000 abstract description 2
- 238000012986 modification Methods 0.000 abstract description 2
- 238000004806 packaging method and process Methods 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
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- 239000011162 core material Substances 0.000 description 31
- 230000000052 comparative effect Effects 0.000 description 10
- 239000000463 material Substances 0.000 description 10
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 8
- 230000007797 corrosion Effects 0.000 description 8
- 238000005260 corrosion Methods 0.000 description 8
- 238000012360 testing method Methods 0.000 description 7
- 230000008859 change Effects 0.000 description 6
- 235000019441 ethanol Nutrition 0.000 description 6
- PKHMTIRCAFTBDS-UHFFFAOYSA-N hexanoyl hexanoate Chemical compound CCCCCC(=O)OC(=O)CCCCC PKHMTIRCAFTBDS-UHFFFAOYSA-N 0.000 description 5
- 229910000077 silane Inorganic materials 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 239000000843 powder Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 230000006872 improvement Effects 0.000 description 3
- YLZOPXRUQYQQID-UHFFFAOYSA-N 3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)-1-[4-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidin-5-yl]piperazin-1-yl]propan-1-one Chemical compound N1N=NC=2CN(CCC=21)CCC(=O)N1CCN(CC1)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F YLZOPXRUQYQQID-UHFFFAOYSA-N 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- 238000007596 consolidation process Methods 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000002845 discoloration Methods 0.000 description 2
- 238000005187 foaming Methods 0.000 description 2
- 230000006870 function Effects 0.000 description 2
- 239000003292 glue Substances 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 229910017604 nitric acid Inorganic materials 0.000 description 2
- 238000007719 peel strength test Methods 0.000 description 2
- 229920001721 polyimide Polymers 0.000 description 2
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- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 239000004925 Acrylic resin Substances 0.000 description 1
- 239000004642 Polyimide Substances 0.000 description 1
- 239000002313 adhesive film Substances 0.000 description 1
- 239000012790 adhesive layer Substances 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
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- 239000012535 impurity Substances 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000012212 insulator Substances 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
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- 238000011056 performance test Methods 0.000 description 1
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J151/00—Adhesives based on graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Adhesives based on derivatives of such polymers
- C09J151/08—Adhesives based on graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Adhesives based on derivatives of such polymers grafted on to macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/10—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polymers containing more than one epoxy radical per molecule
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/06—Non-macromolecular additives organic
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Inorganic Chemistry (AREA)
- Epoxy Resins (AREA)
Abstract
The invention relates to the technical field of electronic device packaging, in particular to an adhesive for a nanocrystalline magnetic core and a preparation method thereof, wherein the adhesive comprises the following components in parts by weight: 80 to 100 parts of modified epoxy acrylate crosslinking system, 23 to 35 parts of filler, 3.5 to 5 parts of photoinitiator, 7 to 8.5 parts of nano supplement, 3 to 6 parts of silane coupling agent and 1.5 to 5 parts of surfactant. The adhesive takes the epoxy acrylate as a basic raw material, has good biocompatibility, and improves the viscosity and the insulativity through specific modification and crosslinking; the composite carbon quantum dots are added, so that the toughness of the composite carbon quantum dots is enhanced, the affinity between the composite carbon quantum dots and magnetic powder is improved according to the dispersibility of the carbon quantum dots, the microstructure of the nanocrystalline magnetic core is further improved, and the magnetic property of the magnetic core is improved.
Description
Technical Field
The invention belongs to the technical field of electronic device packaging, and particularly relates to an adhesive for a nanocrystalline magnetic core and a preparation method thereof.
Background
The nanocrystalline magnetic core is a composite soft magnetic material which is prepared by selecting metal elements with good soft magnetic performance and utilizing a chemical or physical synthesis method to prepare nanocrystalline alloy powder. The preparation process includes mixing the prepared nanometer crystal alloy powder with insulator, adhesive and other matters, molding the mixture in mold at proper temperature and pressure, and heat treatment to obtain the final nanometer crystal magnetic core product. The nanocrystalline magnetic core has a series of excellent magnetic properties, such as higher saturation induction intensity, low hysteresis, low loss and the like. The properties enable the nanocrystalline magnetic core to be widely applied to the fields of power transformers, inductors and the like. The binder is an important component for preparing the nanocrystalline magnetic core, and the main functions of the binder include consolidation of powder, improvement of forming property, promotion of bonding and improvement of heat resistance.
Currently available binders are mainly classified into organic binders and inorganic binders. The organic adhesive is an adhesive made of organic polymer materials, and common organic adhesives comprise epoxy resin, polyimide and the like. The organic adhesives have good plasticity and bonding performance, and are very suitable for bonding nanocrystalline magnetic cores. However, it should be noted that the organic glue material may fail or decompose in a high temperature environment, resulting in loosening or breaking of the adhesive layer. In contrast, inorganic adhesives such as glass and ceramic glues are generally inferior in mechanical properties and are prone to cracking and failure under high loads.
In summary, in the preparation process of the nanocrystalline magnetic core, the binder plays an important role, and the consolidation of the powder and the improvement of the forming performance can be realized through an organic binder or an inorganic binder. The organic adhesive has good plasticity and bonding performance, but can fail or decompose in a high-temperature environment; while inorganic adhesives are generally inferior in mechanical properties. Therefore, in specific applications, the selection needs to be performed according to actual requirements, and the performance of the binder and the influence on the nanocrystalline magnetic core are balanced.
Based on the above problems, it is important to develop an adhesive having high adhesive strength, high insulation and high stability.
Disclosure of Invention
Based on the above problems, an object of the present invention is to provide a binder for a nanocrystalline magnetic core and a method for preparing the same.
In a first aspect of the present invention, there is provided a binder for a nanocrystalline magnetic core, comprising the following components in parts by weight: 80-100 parts of modified epoxy acrylate crosslinking system, 23-35 parts of filler, 3.5-5 parts of photoinitiator, 7-8.5 parts of nano supplement and 3-6 parts of silane coupling agent.
Preferably, the silane coupling agent is one of gamma-propyl methacrylate trimethoxysilane, gamma-aminopropyl trimethoxysilane and gamma-methacryloxypropyl trimethoxysilane, preferably gamma-propyl methacrylate trimethoxysilane.
Preferably, the photoinitiator is one of N-methyldibenzoyl ketone, 1-hydroxycyclopentanone and phenylhydrazone-4-nickel sulfate.
Preferably, the filler is a modified alumina comprising the following preparation steps:
1. weighing Al in a certain proportion 2 O 3 Adding polyvinylpyrrolidone into the flask, sequentially adding ammonia water, ultrapure water and absolute ethanol, and performing microwave ultrasonic treatment for 10min; stirring at 1200rpm for 30min at room temperature; rapidly injecting tetrabutyl titanate, and continuing the stirring reaction for 8 hours; centrifuging at 8000rpm with centrifuge to obtain precipitate, washing with ethanol, and drying in vacuum oven at 120deg.C for 24 hr to obtain Al 2 O 3 @TiO 2 ；
2. Weighing a proper amount of Al 2 O 3 @TiO 2 Adding ethyl orthosilicate, n-propylamine and cyclohexane into a flask according to a certain proportion, performing microwave ultrasound for 10min, and stirring at 1600rpm at room temperature for 30min; raising the temperature to 60 ℃, continuing to stir for 30min, controlling the temperature to 85 ℃ and the time to 80min, removing the solvent by rotary evaporation, and drying in a vacuum oven at 80 ℃ for 18h to obtain the modified Al 2 O 3 @TiO 2 I.e. modified alumina.
Further, the Al 2 O 3 The mass ratio of the polyvinyl pyrrolidone to the polyvinyl pyrrolidone is 1:0.1-0.12; the Al is 2 O 3 With ammonia waterThe ratio of the dosage of the ultrapure water to the dosage of the absolute ethanol is 2.5g to 0.4mL to 1mL to 50mL; the tetrabutyl titanate and Al 2 O 3 The dosage ratio of the components is 0.2-0.24 mL to 1g; the Al is 2 O 3 @TiO 2 The dosage ratio of the water-soluble polymer to the ethyl orthosilicate, the n-propylamine and the cyclohexane is 1 g:0.12-0.15 mL:0.04-0.06 mL:20mL.
Preferably, the nano supplement is a composite carbon quantum dot comprising the following preparation steps:
1) Dissolving glucose and urea in deionized water to form transparent solution, and placing in a closed magnetic stirrer, stirring and mixing uniformly at 300-500 rpm to obtain a mixture; adding the mixture into a reaction kettle filled with polytetrafluoroethylene, controlling the temperature to 160 ℃, heating at constant temperature for reaction for 12 hours, cooling to room temperature, filtering by a 0.22-0.3 mu m filter head, purifying in a centrifuge at a speed of 10000-12000 rpm for 15 minutes, taking supernatant, and freeze-drying to obtain the composite carbon quantum dot;
preferably, the dosage ratio of glucose, urea and deionized water is 1g to 1.2g to 12mL;
preferably, the polytetrafluoroethylene is used in an amount of 5 times that of deionized water.
Preferably, the preparation of the modified epoxy acrylate crosslinking system comprises the following preparation steps:
(1) Adding a proper amount of epoxy resin and p-methylphenol into the triangular flask, controlling the rotating speed to be 400-650 rpm and the temperature to be 95 ℃, and fully stirring and dissolving to obtain a mixture A; adding a proper amount of deionized water into a reaction kettle, sequentially adding methyl methacrylate, methyl acrylate and butyl acrylate, controlling the temperature to be 60 ℃, and fully stirring for 30-45 min to obtain a mixture B;
(2) Heating the mixture in the step (1) to 80 ℃, adding an antioxidant and polysorbate-80, keeping the temperature at 80 ℃, continuing the rotating speed, reacting for 1-1.5 h to obtain a mixed solution C, slowly dripping the mixed solution C into the mixture A, adding dioctyl phthalate and an initiator, keeping the temperature at 105 ℃, continuing the rotating speed, stirring, evaporating, concentrating, and removing the solvent to obtain epoxy acrylate;
(3) Weighing the epoxy acrylate prepared in the step (2) and a proper amount of butanol, adding into a three-necked flask, fully stirring, and adding 8wt% of sodium hydroxide to adjust the pH to 8.2 to obtain a mixture; adding 10 times of 8.2% glycol aqueous solution into the mixture, adding glycolic acid, heating in water bath to control the temperature to 65-80 ℃ for 8 hours, adding 5wt% hydrochloric acid to neutralize pH to neutral, and removing solvent by decompression and dehydration under the vacuum condition of minus 0.091MPa to minus 0.096MPa to obtain modified epoxy acrylate;
(4) Weighing a proper amount of dimethylcarbonamide and the modified epoxy acrylate prepared in the step (3), adding the mixture into ethyl acetate, controlling the temperature to be 80 ℃, slowly adding epoxy maleic anhydride into the mixture at 1mL/s, stirring the mixture at 300-500 rpm for reaction for 30-60 min, cooling the mixture to room temperature, filtering the mixture, defoaming the mixture under vacuum of-0.08 MPa to-0.1 MPa, and standing the mixture for 12h to obtain the modified epoxy acrylate crosslinking system.
Preferably, the mass ratio of the epoxy resin to the p-methylphenol in the step (1) is 1:0.002.
Preferably, the mass ratio of the methyl methacrylate, the methyl acrylate and the butyl acrylate in the step (1) is 0.16-0.25:0.8:0.4-0.6, and the ratio of deionized water to substrate dosage is 12-18 mL:1g.
Preferably, the antioxidant in the step (2) is one of 2, 6-di-tert-butyl-p-cresol and dimercaptodioctyl ether, and the amount of the antioxidant is 0.5% of the mass of the substrate.
Preferably, the polysorbate-80 is used in step (2) in an amount of 2% of the substrate mass.
Preferably, the dioctyl phthalate in step (2) is used in an amount of 1.2% of the substrate mass.
Preferably, the initiator in the step (2) is one of dicumyl peroxide and hydrogen peroxide, and the amount of the initiator is 1.5% of the mass of the substrate.
Preferably, the ratio of butanol to epoxyacrylate in step (3) is 12.5mL to 1g.
Preferably, the mass ratio of the glycolic acid to the epoxyacrylate in the step (3) is 0.15-0.2:1.
Preferably, the ratio of ethyl acetate, epoxyhexanoic anhydride and epoxyacrylate in step (4) is 14.5mL:0.76mL:1g.
Preferably, the dimethylcarbonamide used in the step (4) is 0.5 to 2% of the mass of the substrate.
Preferably, in another aspect of the present invention, there is provided a method for preparing a binder for a nanocrystalline magnetic core, including the steps of:
s1: placing the modified epoxy acrylate crosslinking system in a reaction kettle, controlling the temperature to be 80-98 ℃, adding a silane coupling agent and a filler, controlling the rotating speed to be 800-2200 rpm, and reacting for 1.5h to obtain a mixture a;
s2: gradually adding nano supplement and photoinitiator into the mixture a, controlling the temperature to be 85 ℃, controlling the rotating speed to be 500-800 rpm, and reacting for 5.5 hours to obtain the adhesive.
The method used in the invention is a conventional method unless otherwise specified.
It should be noted that the preparation of the adhesive is carried out within one hour after the preparation of the modified epoxy acrylate crosslinking system is completed.
The invention has the following beneficial effects:
the basic raw material used by the invention is epoxy acrylate, and the epoxy acrylate has the advantages of high hardness, high glossiness, excellent chemical resistance and the like in conventional cognition, and has the characteristics of high viscosity and poor toughness. The invention utilizes the characteristic of large viscosity in epoxy acrylate, enhances the viscosity by modifying and crosslinking the system in a specific proportion, improves the mechanical strength, heat resistance and vibration resistance, and greatly improves the insulativity and ageing resistance under a crosslinking network structure; in addition, the composite carbon quantum dot nano material prepared by the invention is added into an adhesive, so that the internal thermal stress can be effectively reduced, the heat shock performance is improved, the crack generation and delamination caused by temperature change are further reduced, and the toughness of the material is enhanced; in addition, the composite carbon quantum dot nano material has relatively high surface activity and good dispersibility, and can improve the affinity between magnetic powder and a binder, so that the microstructure of the nanocrystalline magnetic core is improved, and the magnetic property of the magnetic core is improved.
The preparation of the inventionIs surface-modified to Al 2 O 3 @TiO 2 The nano-crystalline magnetic core has excellent insulating performance as an adhesive filler, and can form an insulating layer in the nano-crystalline magnetic core to isolate the current of the chip and reduce the wire transfer loss, thereby improving the overall electrical performance; in addition, al 2 O 3 @TiO 2 The material has good thermal stability, can keep the structure and performance of the material unaffected under the high temperature condition, and can effectively resist thermal expansion and thermal shock under the high temperature environment; by surface modification, al 2 O 3 @TiO 2 And the modified epoxy acrylate crosslinking system can form strong interfacial force, so that higher curing degree and stronger bonding strength can be achieved under lower curing conditions, and meanwhile, because of Al 2 O 3 @TiO 2 And the compatibility between the modified epoxy acrylate crosslinking system can effectively improve the thermal property, corrosion resistance and insulativity of the material.
The invention can alleviate the problems of stress and thermal mismatch possibly occurring when the temperature of the magnetic core changes through the use of the modified epoxy acrylate crosslinking system, and improve the matching degree with the magnetic core material, thereby reducing the risk of stress concentration and material fatigue. On one hand, the good chemical resistance of the modified epoxy acrylate resin crosslinking system can protect the magnetic core from being damaged by corrosive media, and the stability of the magnetic core in the chemical treatment process is improved; the magnetic core has excellent vibration resistance and heat resistance, so that the magnetic core has better structural stability and durability in a vibration environment; on the other hand, the acrylic ester is generally used as a nontoxic and environment-friendly material, meets the requirements of the adhesive on product safety and environment friendliness, and the modified epoxy acrylic ester crosslinking system has the characteristics of no toxicity and environment friendliness.
Drawings
FIG. 1 is a graph showing the viscosity of the nanocrystalline core binder prepared according to the present invention as a function of time for placement;
FIG. 2 is a graph of peel strength of nanocrystalline core binders made in accordance with the present invention;
FIG. 3 is a schematic diagram of peel strength testing according to the present invention.
Detailed Description
In order that the manner in which the above recited features, objects and advantages of the present invention are obtained will become readily apparent, a more particular description of the invention will be rendered by reference to specific embodiments thereof which are illustrated in the appended drawings. Based on the examples in the embodiments, those skilled in the art can obtain other examples without making any inventive effort, which fall within the scope of the invention. The experimental methods in the following examples are conventional methods unless otherwise specified, and materials, reagents, etc. used in the following examples are commercially available unless otherwise specified.
Example 1: the binder for the nanocrystalline magnetic core comprises the following components in parts by weight: 80 parts of modified epoxy acrylate crosslinking system, 23 parts of filler, 3.5 parts of photoinitiator, 7 parts of nano supplement and 3 parts of silane coupling agent.
1. Preparation of modified alumina:
1): weigh 5g of Al 2 O 3 And 0.5g polyvinylpyrrolidone is added into the flask, and then 0.8mL ammonia water, 2mL ultrapure water and 100mL absolute ethanol are sequentially added, and the microwave ultrasonic treatment is carried out for 10min; stirring at 1200rpm for 30min at room temperature; rapidly injecting 1mL of tetrabutyl titanate, and continuing the stirring reaction for 8 hours; centrifuging at 8000rpm with centrifuge to obtain precipitate, washing with ethanol, and drying in vacuum oven at 120deg.C for 24 hr to obtain Al 2 O 3 @TiO 2 ；
2): weighing a proper amount of 5g of Al 2 O 3 @TiO 2 Adding into a flask, adding 0.6mL of tetraethoxysilane, 0.2mL of n-propylamine and 100mL of cyclohexane, performing microwave ultrasound for 10min, and stirring at 1600rpm at room temperature for 30min; raising the temperature to 60 ℃, continuing to stir for 30min, controlling the temperature to 85 ℃ and the time to 80min, removing the solvent by rotary evaporation, and drying in a vacuum oven at 80 ℃ for 18h to obtain the modified Al 2 O 3 @TiO 2 I.e. modified alumina.
2. Preparation of composite carbon quantum dots: dissolving 10g of glucose and 12g of urea in 120mL of deionized water to form a transparent solution, placing the solution in a closed magnetic stirrer, and stirring and mixing uniformly at 300rpm to obtain a mixture; adding the mixture into a reaction kettle with 5 times volume of polytetrafluoroethylene, controlling the temperature to 160 ℃, heating at constant temperature for reaction for 12 hours, cooling to room temperature, filtering by a 0.3 mu m filter head, purifying in a centrifuge at 10000rpm for 15 minutes, taking supernatant, and freeze-drying to obtain the composite carbon quantum dot.
3. Preparation of modified epoxy acrylate crosslinking system:
(1) Adding 30g of epoxy resin and 0.06g of p-methylphenol into an Erlenmeyer flask, controlling the rotating speed to 400rpm and the temperature to 95 ℃, and fully stirring and dissolving to obtain a mixture A; 816mL of deionized water is added into a reaction kettle, 8g of methyl methacrylate, 40g of methyl acrylate and 20g of butyl acrylate are sequentially added, the temperature is controlled at 60 ℃, and the mixture is fully stirred for 30min to obtain a mixture B;
(2) Heating the mixture B in the step (1) to 80 ℃, adding 0.34g of 2, 6-di-tert-butyl-p-cresol and 1.36g of polysorbate-80, keeping the temperature at 80 ℃, continuing the rotating speed, reacting for 1h to obtain a mixed solution C, slowly dropwise adding the mixed solution C into the mixture A, adding 0.82g of dioctyl phthalate and 1g of dicumyl peroxide, keeping the temperature at 105 ℃, continuing the rotating speed, stirring, evaporating, concentrating and removing the solvent after 4h to obtain epoxy acrylate;
(3) Weighing 10g of the epoxy acrylate prepared in the step (2) and 125mL of butanol, adding into a three-necked flask, fully stirring, and adding 8wt% of sodium hydroxide to adjust the pH to 8.2 to obtain a mixture; adding 10 times of 8.2% glycol aqueous solution into the mixture, adding 1.5g glycolic acid, heating in water bath to control the temperature to 65 ℃ for 8 hours, adding 5wt% hydrochloric acid to neutralize pH to neutrality, and removing solvent by decompression dehydration under vacuum condition of-0.091 MPa to obtain modified epoxy acrylate;
(4) Weighing a proper amount of 0.017g of dimethylcarbonamide and the modified epoxy acrylate prepared in the step (3), adding the mixture into 145mL of ethyl acetate, controlling the temperature to 80 ℃, slowly adding 7mL of epoxy hexanoic anhydride into 1mL/s, stirring at 300rpm for reaction for 30min, cooling to room temperature, filtering, defoaming under vacuum of-0.08 MPa, and standing for 12h to obtain a modified epoxy acrylate crosslinking system.
4. Preparation of the adhesive:
s1: placing the modified epoxy acrylate crosslinking system in a reaction kettle, controlling the temperature to be 80 ℃, adding gamma-propyl methacrylate trimethoxy silane and modified alumina, controlling the rotating speed to be 800rpm, and reacting for 1.5 hours to obtain a mixture a;
s2: and gradually adding the composite carbon quantum dots and the N-methyl dibenzoyl ketone into the mixture a, controlling the temperature to be 85 ℃, controlling the rotating speed to be 500rpm, and reacting for 5.5 hours to obtain the adhesive.
Example 2: the binder for the nanocrystalline magnetic core comprises the following components in parts by weight: 85 parts of modified epoxy acrylate crosslinking system, 25 parts of filler, 4 parts of photoinitiator, 7.5 parts of nano supplement and 4 parts of silane coupling agent.
1. Preparation of modified alumina:
1): weigh 5g of Al 2 O 3 And 0.54g polyvinylpyrrolidone is added into the flask, and then 0.8mL ammonia water, 2mL ultrapure water and 100mL absolute ethanol are sequentially added, and the microwave ultrasonic treatment is carried out for 10min; stirring at 1200rpm for 30min at room temperature; rapidly injecting 1.05mL of tetrabutyl titanate, and continuing the stirring reaction for 8 hours; centrifuging at 8000rpm with centrifuge to obtain precipitate, washing with ethanol, and drying in vacuum oven at 120deg.C for 24 hr to obtain Al 2 O 3 @TiO 2 ；
2): weighing a proper amount of 5g of Al 2 O 3 @TiO 2 Adding into a flask, adding 0.65mL of tetraethoxysilane, 0.22mL of n-propylamine and 100mL of cyclohexane, performing microwave ultrasound for 10min, and stirring at 1600rpm at room temperature for 30min; raising the temperature to 60 ℃, continuing to stir for 30min, controlling the temperature to 85 ℃ and the time to 80min, removing the solvent by rotary evaporation, and drying in a vacuum oven at 80 ℃ for 18h to obtain the modified Al 2 O 3 @TiO 2 I.e. modified alumina.
2. Preparation of composite carbon quantum dots: dissolving 10g of glucose and 12g of urea in 120mL of deionized water to form a transparent solution, placing the solution in a closed magnetic stirrer, and stirring and uniformly mixing at 350rpm to obtain a mixture; adding the mixture into a reaction kettle with 5 times volume of polytetrafluoroethylene, controlling the temperature to 160 ℃, heating at constant temperature for reaction for 12 hours, cooling to room temperature, filtering by a 0.28 mu m filter head, purifying in a centrifuge at 10500rpm for 15 minutes, taking supernatant, and freeze-drying to obtain the composite carbon quantum dot.
3. Preparation of modified epoxy acrylate crosslinking system:
(1) Adding 30g of epoxy resin and 0.06g of p-methylphenol into an Erlenmeyer flask, controlling the rotating speed to be 500rpm and the temperature to be 95 ℃, and fully stirring and dissolving to obtain a mixture A; 970mL of deionized water is added into a reaction kettle, 9g of methyl methacrylate, 40g of methyl acrylate and 20g of butyl acrylate are sequentially added, the temperature is controlled at 60 ℃, and the mixture is fully stirred for 35min to obtain a mixture B;
(2) Heating the mixture B in the step (1) to 80 ℃, adding 0.35g of dimercaptodioctyl ether and 1.38g of polysorbate-80, keeping the temperature at 80 ℃, continuing the rotating speed, reacting for 1.2 hours to obtain a mixed solution C, slowly dropwise adding the mixed solution C into the mixture A, adding 0.83g of dioctyl phthalate and 1g of hydrogen peroxide, keeping the temperature at 105 ℃, continuing the rotating speed, stirring, evaporating and concentrating to remove the solvent after 4 hours to obtain the epoxy acrylate;
(3) Weighing 10g of the epoxy acrylate prepared in the step (2) and 125mL of butanol, adding into a three-necked flask, fully stirring, and adding 8wt% of sodium hydroxide to adjust the pH to 8.2 to obtain a mixture; adding 10 times of 8.2% glycol aqueous solution into the mixture, adding 1.6g glycolic acid, heating in water bath to control the temperature to 70 ℃ for 8 hours, adding 5wt% hydrochloric acid to neutralize pH to neutrality, and removing solvent by decompression dehydration under vacuum condition of-0.093 MPa to obtain modified epoxy acrylate;
(4) Weighing a proper amount of 0.11g of dimethylcarbonamide and the modified epoxy acrylate prepared in the step (3), adding the mixture into 145mL of ethyl acetate, controlling the temperature to 80 ℃, slowly adding 7.6mL of epoxy hexanoic anhydride into 1mL/s, stirring at 350rpm for reaction for 40min, cooling to room temperature, filtering, defoaming under vacuum of-0.085 MPa, and standing for 12h to obtain a modified epoxy acrylate crosslinking system.
4. Preparation of the adhesive:
s1: placing the modified epoxy acrylate crosslinking system in a reaction kettle, controlling the temperature to be 95 ℃, adding gamma-propyl methacrylate trimethoxy silane and modified alumina, controlling the rotating speed to be 1600rpm, and reacting for 1.5 hours to obtain a mixture a;
s2: and gradually adding the composite carbon quantum dots and the N-methyl dibenzoyl ketone into the mixture a, controlling the temperature to be 85 ℃, controlling the rotating speed to be 650rpm, and reacting for 5.5 hours to obtain the adhesive.
Example 3: the binder for the nanocrystalline magnetic core comprises the following components in parts by weight: 90 parts of modified epoxy acrylate crosslinking system, 29 parts of filler, 4.5 parts of photoinitiator, 7.8 parts of nano supplement and 4.5 parts of silane coupling agent.
1. Preparation of modified alumina:
1): weigh 5g of Al 2 O 3 And 0.57g polyvinylpyrrolidone is added into the flask, and then 0.8mL ammonia water, 2mL ultrapure water and 100mL absolute ethanol are sequentially added, and the microwave ultrasonic treatment is carried out for 10min; stirring at 1200rpm for 30min at room temperature; rapidly injecting 1.1mL of tetrabutyl titanate, and continuing the stirring reaction for 8 hours; centrifuging at 8000rpm with centrifuge to obtain precipitate, washing with ethanol, and drying in vacuum oven at 120deg.C for 24 hr to obtain Al 2 O 3 @TiO 2 ；
2): weighing a proper amount of 5g of Al 2 O 3 @TiO 2 Adding into a flask, adding 0.65mL of tetraethoxysilane, 0.25mL of n-propylamine and 100mL of cyclohexane, performing microwave ultrasound for 10min, and stirring at 1600rpm at room temperature for 30min; raising the temperature to 60 ℃, continuing to stir for 30min, controlling the temperature to 85 ℃ and the time to 80min, removing the solvent by rotary evaporation, and drying in a vacuum oven at 80 ℃ for 18h to obtain the modified Al 2 O 3 @TiO 2 I.e. modified alumina.
2. Preparation of composite carbon quantum dots: dissolving 10g of glucose and 12g of urea in 120mL of deionized water to form a transparent solution, placing the solution in a closed magnetic stirrer, and stirring and uniformly mixing at 400rpm to obtain a mixture; adding the mixture into a reaction kettle with 5 times volume of polytetrafluoroethylene, controlling the temperature to 160 ℃, heating at constant temperature for reaction for 12 hours, cooling to room temperature, filtering by a 0.26 mu m filter head, purifying in a centrifuge at 11000rpm for 15 minutes, taking supernatant, and freeze-drying to obtain the composite carbon quantum dot.
3. Preparation of modified epoxy acrylate crosslinking system:
(1) Adding 30g of epoxy resin and 0.06g of p-methylphenol into an Erlenmeyer flask, controlling the rotating speed to be 550rpm and the temperature to be 95 ℃, and fully stirring and dissolving to obtain a mixture A; 1130mL of deionized water is added into a reaction kettle, 10g of methyl methacrylate, 40g of methyl acrylate and 25g of butyl acrylate are sequentially added, the temperature is controlled at 60 ℃, and the mixture is fully stirred for 40min to obtain a mixture B;
(2) Heating the mixture B in the step (1) to 80 ℃, adding 0.38g of 2, 6-di-tert-butyl-p-cresol and 1.5g of polysorbate-80, keeping the temperature at 80 ℃, continuing the rotating speed, reacting for 1.2h to obtain a mixed solution C, slowly dropwise adding the mixed solution C into the mixture A, adding 0.9g of dioctyl phthalate and 1.13g of hydrogen peroxide, keeping the temperature at 105 ℃, continuing the rotating speed, stirring, evaporating, concentrating and removing the solvent after 4h to obtain epoxy acrylate;
(3) Weighing 10g of the epoxy acrylate prepared in the step (2) and 125mL of butanol, adding into a three-necked flask, fully stirring, and adding 8wt% of sodium hydroxide to adjust the pH to 8.2 to obtain a mixture; adding 10 times of 8.2% glycol aqueous solution into the mixture, adding 1.7g glycolic acid, heating in water bath to control the temperature to 70 ℃ for 8 hours, adding 5wt% hydrochloric acid to neutralize pH to neutrality, and removing solvent by decompression dehydration under vacuum condition of-0.096 MPa to obtain modified epoxy acrylate;
(4) Weighing a proper amount of 0.14g of dimethylcarbonamide and the modified epoxy acrylate prepared in the step (3), adding the mixture into 145mL of ethyl acetate, controlling the temperature to 80 ℃, slowly adding 7.6mL of epoxy hexanoic anhydride into 1mL/s, stirring at 400rpm for reaction for 50min, cooling to room temperature, filtering, defoaming under vacuum of-0.092 MPa, and standing for 12h to obtain the modified epoxy acrylate crosslinking system.
4. Preparation of the adhesive:
s1: placing the modified epoxy acrylate crosslinking system in a reaction kettle, controlling the temperature to be 95 ℃, adding gamma-propyl methacrylate trimethoxy silane and modified alumina, controlling the rotating speed to be 1600rpm, and reacting for 1.5 hours to obtain a mixture a;
s2: and gradually adding the composite carbon quantum dots and the N-methyl dibenzoyl ketone into the mixture a, controlling the temperature to be 85 ℃, controlling the rotating speed to be 650rpm, and reacting for 5.5 hours to obtain the adhesive.
Example 4: the binder for the nanocrystalline magnetic core comprises the following components in parts by weight: 95 parts of modified epoxy acrylate crosslinking system, 33 parts of filler, 5 parts of photoinitiator, 8.2 parts of nano supplement and 5.5 parts of silane coupling agent.
1. Preparation of modified alumina:
1): weigh 5g of Al 2 O 3 And 0.58g polyvinylpyrrolidone is added into the flask, and then 0.8mL ammonia water, 2mL ultrapure water and 100mL absolute ethanol are sequentially added, and the microwave ultrasonic treatment is carried out for 10min; stirring at 1200rpm for 30min at room temperature; rapidly injecting 1.1mL of tetrabutyl titanate, and continuing the stirring reaction for 8 hours; centrifuging at 8000rpm with centrifuge to obtain precipitate, washing with ethanol, and drying in vacuum oven at 120deg.C for 24 hr to obtain Al 2 O 3 @TiO 2 ；
2): weighing a proper amount of 5g of Al 2 O 3 @TiO 2 Adding into a flask, adding 0.7mL of tetraethoxysilane, 0.3mL of n-propylamine and 100mL of cyclohexane, performing microwave ultrasound for 10min, and stirring at 1600rpm at room temperature for 30min; raising the temperature to 60 ℃, continuing to stir for 30min, controlling the temperature to 85 ℃ and the time to 80min, removing the solvent by rotary evaporation, and drying in a vacuum oven at 80 ℃ for 18h to obtain the modified Al 2 O 3 @TiO 2 I.e. modified alumina.
2. Preparation of composite carbon quantum dots: dissolving 10g of glucose and 12g of urea in 120mL of deionized water to form a transparent solution, placing the solution in a closed magnetic stirrer, and stirring and mixing uniformly at 450rpm to obtain a mixture; adding the mixture into a reaction kettle with 5 times volume of polytetrafluoroethylene, controlling the temperature to 160 ℃, heating at constant temperature for reaction for 12 hours, cooling to room temperature, filtering by a 0.24 mu m filter head, purifying in a centrifuge at 11500rpm for 15 minutes, taking supernatant, and freeze-drying to obtain the composite carbon quantum dot.
3. Preparation of modified epoxy acrylate crosslinking system:
(1) Adding 30g of epoxy resin and 0.06g of p-methylphenol into an Erlenmeyer flask, controlling the rotating speed to 600rpm and the temperature to 95 ℃, and fully stirring and dissolving to obtain a mixture A; 1300mL of deionized water is added into a reaction kettle, 12.5g of methyl methacrylate, 40g of methyl acrylate and 28g of butyl acrylate are sequentially added, the temperature is controlled at 60 ℃, and the mixture is fully stirred for 40min to obtain a mixture B;
(2) Heating the mixture B in the step (1) to 80 ℃, adding 0.4g of dimercaptodioctyl ether and 1.6g of polysorbate-80, keeping the temperature at 80 ℃, continuing the rotating speed, reacting for 1.5h to obtain a mixed solution C, slowly dropwise adding the mixed solution C into the mixture A, adding 0.97g of dioctyl phthalate and 1.21g of hydrogen peroxide, keeping the temperature at 105 ℃, continuing the rotating speed, stirring, evaporating, concentrating and removing the solvent after 4h to obtain epoxy acrylate;
(3) Weighing 10g of the epoxy acrylate prepared in the step (2) and 125mL of butanol, adding into a three-necked flask, fully stirring, and adding 8wt% of sodium hydroxide to adjust the pH to 8.2 to obtain a mixture; adding 10 times of 8.2% glycol aqueous solution into the mixture, adding 1.8g glycolic acid, heating in water bath to control the temperature to 75 ℃ for 8 hours, adding 5wt% hydrochloric acid to neutralize pH to neutrality, and removing solvent by decompression dehydration under vacuum condition of-0.095 MPa to obtain modified epoxy acrylate;
(4) Weighing a proper amount of 0.21g of dimethylcarbonamide and the modified epoxy acrylate prepared in the step (3), adding the mixture into 145mL of ethyl acetate, controlling the temperature to 80 ℃, slowly adding 7.6mL of epoxy hexanoic anhydride into 1mL/s, stirring at 450rpm for reaction for 55min, cooling to room temperature, filtering, defoaming under vacuum of-0.098 MPa, and standing for 12h to obtain the modified epoxy acrylate crosslinking system.
4. Preparation of the adhesive:
s1: placing the modified epoxy acrylate crosslinking system in a reaction kettle, controlling the temperature to be 95 ℃, adding gamma-propyl methacrylate trimethoxy silane and modified alumina, controlling the rotating speed to be 1800rpm, and reacting for 1.5 hours to obtain a mixture a;
s2: and gradually adding the composite carbon quantum dots and the N-methyl dibenzoyl ketone into the mixture a, controlling the temperature to be 85 ℃, controlling the rotating speed to be 700rpm, and reacting for 5.5 hours to obtain the adhesive.
Example 5: the binder for the nanocrystalline magnetic core comprises the following components in parts by weight: 100 parts of modified epoxy acrylate crosslinking system, 35 parts of filler, 5 parts of photoinitiator, 8.5 parts of nano supplement and 6 parts of silane coupling agent.
1. Preparation of modified alumina:
1): weigh 5g of Al 2 O 3 And 0.6g polyvinylpyrrolidone is added into the flask, and then 0.8mL ammonia water, 2mL ultrapure water and 100mL absolute ethanol are sequentially added, and the microwave ultrasonic treatment is carried out for 10min; stirring at 1200rpm for 30min at room temperature; rapidly injecting 1.2mL of tetrabutyl titanate, and continuing the stirring reaction for 8 hours; centrifuging at 8000rpm with centrifuge to obtain precipitate, washing with ethanol, and drying in vacuum oven at 120deg.C for 24 hr to obtain Al 2 O 3 @TiO 2 ；
2): weighing a proper amount of 5g of Al 2 O 3 @TiO 2 Adding into a flask, adding 0.75mL of tetraethoxysilane, 0.3mL of n-propylamine and 100mL of cyclohexane, performing microwave ultrasound for 10min, and stirring at 1600rpm at room temperature for 30min; raising the temperature to 60 ℃, continuing to stir for 30min, controlling the temperature to 85 ℃ and the time to 80min, removing the solvent by rotary evaporation, and drying in a vacuum oven at 80 ℃ for 18h to obtain the modified Al 2 O 3 @TiO 2 I.e. modified alumina.
2. Preparation of composite carbon quantum dots: dissolving 10g of glucose and 12g of urea in 120mL of deionized water to form a transparent solution, placing the solution in a closed magnetic stirrer, and stirring and mixing uniformly at 500rpm to obtain a mixture; adding the mixture into a reaction kettle with 5 times volume of polytetrafluoroethylene, controlling the temperature to 160 ℃, heating at constant temperature for reaction for 12 hours, cooling to room temperature, filtering by a 0.22 mu m filter head, purifying in a centrifuge at 12000rpm for 15 minutes, taking supernatant, and freeze-drying to obtain the composite carbon quantum dot.
3. Preparation of modified epoxy acrylate crosslinking system:
(1) Adding 30g of epoxy resin and 0.06g of p-methylphenol into the triangular flask, controlling the rotating speed to be 650rpm and the temperature to be 95 ℃, and fully stirring and dissolving to obtain a mixture A; 1485mL of deionized water is added into a reaction kettle, 12.5g of methyl methacrylate, 40g of methyl acrylate and 30g of butyl acrylate are sequentially added, the temperature is controlled at 60 ℃, and the mixture is fully stirred for 45min to obtain a mixture B;
(2) Heating the mixture B in the step (1) to 80 ℃, adding 0.41g of dimercaptodioctyl ether and 1.65g of polysorbate-80, keeping the temperature at 80 ℃, continuing the rotating speed, reacting for 1.5 hours to obtain a mixed solution C, slowly dropwise adding the mixed solution C into the mixture A, adding 0.99g of dioctyl phthalate and 1.23g of hydrogen peroxide, keeping the temperature at 105 ℃, continuing the rotating speed, stirring, evaporating, concentrating and removing the solvent after 4 hours to obtain epoxy acrylate;
(3) Weighing 10g of the epoxy acrylate prepared in the step (2) and 125mL of butanol, adding into a three-necked flask, fully stirring, and adding 8wt% of sodium hydroxide to adjust the pH to 8.2 to obtain a mixture; adding 10 times of 8.2% glycol aqueous solution into the mixture, adding 2g of glycolic acid, heating in water bath to control the temperature to 80 ℃ for 8 hours, adding 5wt% hydrochloric acid to neutralize pH to neutrality, and removing solvent by decompression and dehydration under the vacuum condition of-0.096 MPa to obtain modified epoxy acrylate;
(4) Weighing a proper amount of 0.24g of dimethylcarbonamide and the modified epoxy acrylate prepared in the step (3), adding the mixture into 145mL of ethyl acetate, controlling the temperature to 80 ℃, slowly adding 7mL of epoxy hexanoic anhydride into 1mL/s, stirring at 500rpm for reaction for 60min, cooling to room temperature, filtering, defoaming under vacuum of-0.1 MPa, and standing for 12h to obtain a modified epoxy acrylate crosslinking system.
4. Preparation of the adhesive:
s1: placing the modified epoxy acrylate crosslinking system in a reaction kettle, controlling the temperature to 98 ℃, adding gamma-propyl methacrylate trimethoxy silane and modified alumina, controlling the rotating speed to 2200rpm, and reacting for 1.5h to obtain a mixture a;
s2: and gradually adding the composite carbon quantum dots and the N-methyl dibenzoyl ketone into the mixture a, controlling the temperature to be 85 ℃, controlling the rotating speed to be 800rpm, and reacting for 5.5 hours to obtain the adhesive.
Comparative example 1: substantially the same as in example 2, except that no nano supplement was added in comparative example 1.
Comparative example 2: substantially the same as in example 3, except that Al was used in comparative example 2 2 O 3 As a filler.
Performance test:
chemical resistance test:
uniformly coating the nanocrystalline core magnetic binder prepared in the examples 1-5 and the comparative examples 1-2 on glass with the size of 3cm multiplied by 3cm, and after plastic drying, cleaning by using absolute ethyl alcohol to remove surface impurities; drying the cleaned sample, and then placing the dried sample into a soaking device, and respectively adding concentrated sulfuric acid, concentrated nitric acid and concentrated hydrochloric acid for soaking; during the test, the surface change condition of the sample is observed periodically, and the occurrence time and degree of corrosion phenomena, such as corrosion pits, discoloration, foaming and the like on the surface are recorded, and the test results are shown in table 1.
Table 1. Corrosion resistance test.
A. No obvious change exists; B. a slight color change, or a slight weight change; C. is subject to macroscopic changes, such as corrosion pits, discoloration, foaming, etc.; D. the appearance and ductility change significantly.
Peel strength test:
using the adhesive prepared in the invention, polyimide films were cut into strips 25.+ -. 0.5mm wide and bonded to glass slides 25.+ -. 0.5mm wide, and the average peel force at a vehicle speed of 100mm/min was tested using a universal material tester, and peel strength was calculated from the peel force (not less than 5 per pattern).
；
H is the peel force (N), G is the bond width.
Table 2 peel strength test.
Tensile strength test:
the adhesive binder prepared by the invention was poured into a polytetrafluoroethylene strip mold of 0.5mm×150mm×10mm uniformly, and cured into adhesive film solid strips under the same curing process, three strips for each sample, and the tensile strength was measured, and the results are shown in table 3.
Table 3. Tensile strength test.
As can be seen from the results of fig. 1, the adhesive prepared according to the present invention gradually increases in viscosity as it is left at room temperature for a prolonged period of time; as is clear from the results of Table 1, the binders prepared in the present invention exhibited extremely strong corrosion resistance in concentrated sulfuric acid and concentrated hydrochloric acid, the binders prepared in example 1 did not exhibit significant effect in concentrated nitric acid, examples 2 to 5 exhibited relatively strong corrosion resistance, and example 3 showed Al compared to comparative example 2 2 O 3 @TiO 2 When added as filler to a binder the corrosion resistance of the adhesive is obviously improved; as can be seen from the results of fig. 2 and table 2, the adhesive prepared by the present invention has a strong adhesive force, and the addition of the carbon quantum dot material has a certain influence on the adhesive strength compared with the example 2 and the comparative example 1; example 3 compared to comparative example 2, al 2 O 3 @TiO 2 Has a significant effect on the adhesive strength of the adhesive; as is clear from the results of Table 3, the adhesive prepared in the present invention exhibits strong tensile strength after curing, and comparative examples 2 and 3 and comparative examples 1 and 2 show that the carbon quantum dots and Al added in the present invention 2 O 3 @TiO 2 The tensile strength of the adhesive can be effectively improved.
Those of ordinary skill in the art will appreciate that: the discussion of any of the embodiments above is merely exemplary and is not intended to suggest that the scope of the invention (including the claims) is limited to these examples; the technical features of the above embodiments or in the different embodiments may also be combined within the idea of the invention, the steps may be implemented in any order and there are many other variations of the different aspects of the invention as described above, which are not provided in detail for the sake of brevity.
Claims (10)
1. The binder for the nanocrystalline magnetic core is characterized by comprising the following components in parts by weight: 80-100 parts of modified epoxy acrylate crosslinking system, 23-35 parts of filler, 3.5-5 parts of photoinitiator, 7-8.5 parts of nano supplement and 3-6 parts of silane coupling agent.
2. The binder for a nanocrystalline core according to claim 1, wherein the silane coupling agent is one of gamma-propyl methacrylate-based trimethoxysilane, gamma-aminopropyl trimethoxysilane, and gamma-methacryloxypropyl trimethoxysilane.
3. The binder for a nanocrystalline magnetic core according to claim 2, wherein the photoinitiator is one of N-methyldibenzoyl ketone, 1-hydroxycyclopentanone, and phenylhydrazone-4-nickel sulfate.
4. A binder for a nanocrystalline magnetic core according to claim 3, wherein the filler is modified alumina, and the method for preparing the modified alumina comprises the steps of:
a1: weighing Al in a certain proportion 2 O 3 Adding polyvinylpyrrolidone into the flask, sequentially adding ammonia water, ultrapure water and absolute ethanol, and performing microwave ultrasonic treatment for 10min; stirring at 1200rpm for 30min at room temperature; rapidly injecting tetrabutyl titanate, and continuing the stirring reaction for 8 hours; centrifuging at 8000rpm with centrifuge to obtain precipitate, washing with ethanol, and drying in vacuum oven at 120deg.C for 24 hr to obtain Al 2 O 3 @TiO 2 ；
A2: weighing a proper amount of Al 2 O 3 @TiO 2 Adding ethyl orthosilicate, n-propylamine and cyclohexane into a flask according to a certain proportion, performing microwave ultrasound for 10min, and stirring at 1600rpm at room temperature for 30min; raising the temperature to 60 ℃, continuing to stir for 30min, controlling the temperature to 85 ℃ and the time to 80min, removing the solvent by rotary evaporation, and drying in a vacuum oven at 80 ℃ for 18h to obtain the modified Al 2 O 3 @TiO 2 I.e., modified alumina;
the Al is 2 O 3 The mass ratio of the polyvinyl pyrrolidone to the polyvinyl pyrrolidone is 1:0.1-0.12; the Al is 2 O 3 The dosage ratio of the aqueous solution to ammonia, ultrapure water and absolute ethanol is 2.5g to 0.4mL to 1mL to 50mL; the tetrabutyl titanate and Al 2 O 3 The dosage ratio of the components is 0.2-0.24 mL to 1g; the Al is 2 O 3 @TiO 2 The dosage ratio of the water-soluble polymer to the ethyl orthosilicate, the n-propylamine and the cyclohexane is 1 g:0.12-0.15 mL:0.04-0.06 mL:20mL.
5. The binder for a nanocrystalline magnetic core according to claim 4, wherein the nano supplement is a composite carbon quantum dot, and the preparation method of the composite carbon quantum dot comprises the following steps:
b1: after glucose and urea are dissolved in deionized water to form transparent solution, placing the transparent solution in a closed magnetic stirrer, and stirring and mixing uniformly at 300-500 rpm to obtain a mixture; adding the mixture into a reaction kettle filled with polytetrafluoroethylene, controlling the temperature to 160 ℃, heating at constant temperature for reaction for 12 hours, cooling to room temperature, filtering by a 0.22-0.3 mu m filter head, purifying in a centrifuge at a speed of 10000-12000 rpm for 15 minutes, taking supernatant, and freeze-drying to obtain the composite carbon quantum dot;
the dosage ratio of the glucose to the urea to the deionized water is 1g to 1.2g to 12mL;
the dosage of polytetrafluoroethylene is 5 times of deionized water.
6. The binder for nanocrystalline magnetic cores according to claim 5, wherein the preparation method of the modified epoxy acrylate crosslinking system comprises the following steps:
(1) Adding epoxy resin and p-methylphenol into the triangular flask, controlling the rotating speed to 400rpm and the temperature to 95 ℃, and fully stirring and dissolving to obtain a mixture A; adding deionized water into a reaction kettle, sequentially adding methyl methacrylate, methyl acrylate and butyl acrylate, controlling the temperature to be 60 ℃, and fully stirring for 30min to obtain a mixture B;
(2) Heating the mixture B in the step (1) to 80 ℃, adding an antioxidant and polysorbate-80, keeping the temperature at 80 ℃, continuing the rotating speed, reacting for 1h to obtain a mixed solution C, slowly dripping the mixed solution C into the mixture A, adding dioctyl phthalate and an initiator, keeping the temperature at 105 ℃, continuing the rotating speed, stirring, evaporating, concentrating and removing the solvent after 4h to obtain epoxy acrylate;
(3) Weighing the epoxy acrylate and butanol prepared in the step (2), adding into a three-necked flask, fully stirring, and adding 8wt% of sodium hydroxide to adjust the pH to 8.2 to obtain a mixture; adding 10 times of 8.2% glycol aqueous solution into the mixture, adding glycolic acid, heating in water bath to control the temperature to 65-80 ℃ for 8 hours, adding 5wt% hydrochloric acid to neutralize pH to neutral, and removing solvent by decompression and dehydration under the vacuum condition of minus 0.091MPa to minus 0.096MPa to obtain modified epoxy acrylate;
(4) Weighing a proper amount of dimethylcarbonamide and the modified epoxy acrylate prepared in the step (3), adding the mixture into ethyl acetate, controlling the temperature to be 80 ℃, slowly adding epoxy maleic anhydride into the mixture at 1mL/s, stirring the mixture at 300-500 rpm for reaction for 30-60 min, cooling the mixture to room temperature, filtering the mixture, defoaming the mixture under vacuum of-0.08 MPa to-0.1 MPa, and standing the mixture for 12h to obtain the modified epoxy acrylate crosslinking system.
7. The binder for nanocrystalline magnetic core according to claim 6, wherein the mass ratio of epoxy resin to p-methylphenol in step (1) is 1:0.002, the ratio of methyl methacrylate, methyl acrylate and butyl acrylate is 0.16-0.25:0.8:0.4-0.6, and the mass ratio of deionized water to substrate is 12-18 ml:1g; the antioxidant in the step (2) is one of 2, 6-di-tert-butyl-p-cresol and dimercapto dioctyl ether, and the dosage of the antioxidant is 0.5% of the mass of the substrate; the consumption of polysorbate-80 is 2% of the mass of the substrate; the dosage of the dioctyl phthalate is 1.2% of the mass of the substrate; the initiator is one of dicumyl peroxide and hydrogen peroxide, and the use amount of the initiator is 1.5% of the mass of the substrate.
8. The binder for nanocrystalline magnetic cores according to claim 7, wherein the ratio of butanol to epoxyacrylate used in step (3) is 12.5ml to 1g; the mass ratio of the glycolic acid to the epoxy acrylate is 0.15-0.2:1.
9. The binder for nanocrystalline magnetic cores according to claim 8, wherein the ratio of ethyl acetate, epoxyhexanoic anhydride, and epoxyacrylate in step (4) is 14.5ml to 0.76ml to 1g; the dosage of the dimethylcarbonamide is 0.5 to 2 percent of the mass of the substrate.
10. A method for preparing the binder for a nanocrystalline magnetic core according to any one of claims 1 to 9, characterized by comprising the following preparation steps:
s1: placing the modified epoxy acrylate crosslinking system in a reaction kettle, controlling the temperature to be 80-98 ℃, adding a silane coupling agent and a filler, controlling the rotating speed to be 800-2200 rpm, and reacting for 1.5h to obtain a mixture a;
s2: gradually adding nano supplement and photoinitiator into the mixture a, controlling the temperature to be 85 ℃, controlling the rotating speed to be 500-800 rpm, and reacting for 5.5 hours to obtain the adhesive.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20180026099A (en) * | 2016-09-02 | 2018-03-12 | 주식회사 제이텍 | Adhesive film including inorganic filler for removing optical clear adhesives, method for preparing the same, and remove method of optical clear adhesives on touch screen panel |
| CN108219730A (en) * | 2018-01-16 | 2018-06-29 | 黑龙江省科学院石油化学研究院 | The preparation method and its conductive adhesive of a kind of conductive adhesive |
| CN108546393A (en) * | 2018-07-19 | 2018-09-18 | 东莞蚂蚁三维科技有限公司 | A kind of resistance to ultralow temperature 3D printing photosensitive nanocomposite and its preparation |
| CN116144307A (en) * | 2023-03-02 | 2023-05-23 | 常州市宝丽胶粘剂有限公司 | High-viscosity acrylic adhesive and preparation method thereof |
-
2023
- 2023-11-17 CN CN202311534646.3A patent/CN117645853B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20180026099A (en) * | 2016-09-02 | 2018-03-12 | 주식회사 제이텍 | Adhesive film including inorganic filler for removing optical clear adhesives, method for preparing the same, and remove method of optical clear adhesives on touch screen panel |
| CN108219730A (en) * | 2018-01-16 | 2018-06-29 | 黑龙江省科学院石油化学研究院 | The preparation method and its conductive adhesive of a kind of conductive adhesive |
| CN108546393A (en) * | 2018-07-19 | 2018-09-18 | 东莞蚂蚁三维科技有限公司 | A kind of resistance to ultralow temperature 3D printing photosensitive nanocomposite and its preparation |
| CN116144307A (en) * | 2023-03-02 | 2023-05-23 | 常州市宝丽胶粘剂有限公司 | High-viscosity acrylic adhesive and preparation method thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN118185563A (en) * | 2024-05-16 | 2024-06-14 | 朗峰新材料启东有限公司 | Nanocrystalline magnetic core packaging organosilicon binder and preparation method thereof |
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