CN111849003B - Preparation method of rubber sheet for filling holes in slotted holes of metal substrate - Google Patents
Preparation method of rubber sheet for filling holes in slotted holes of metal substrate Download PDFInfo
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- CN111849003B CN111849003B CN202010785344.3A CN202010785344A CN111849003B CN 111849003 B CN111849003 B CN 111849003B CN 202010785344 A CN202010785344 A CN 202010785344A CN 111849003 B CN111849003 B CN 111849003B
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- solid
- heating
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- mixed solution
- molybdenum disulfide
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- 238000002360 preparation method Methods 0.000 title claims abstract description 41
- 238000011049 filling Methods 0.000 title claims abstract description 30
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 29
- 239000002184 metal Substances 0.000 title claims abstract description 29
- 239000000758 substrate Substances 0.000 title claims abstract description 20
- 239000003292 glue Substances 0.000 claims abstract description 49
- 239000003822 epoxy resin Substances 0.000 claims abstract description 44
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 44
- 238000005303 weighing Methods 0.000 claims abstract description 42
- 238000001035 drying Methods 0.000 claims abstract description 37
- 229920005989 resin Polymers 0.000 claims abstract description 35
- 239000011347 resin Substances 0.000 claims abstract description 35
- 239000000945 filler Substances 0.000 claims abstract description 22
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 21
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 19
- 239000011248 coating agent Substances 0.000 claims abstract description 19
- 238000000576 coating method Methods 0.000 claims abstract description 19
- 238000000227 grinding Methods 0.000 claims abstract description 19
- 229920000139 polyethylene terephthalate Polymers 0.000 claims abstract description 14
- 239000005020 polyethylene terephthalate Substances 0.000 claims abstract description 14
- 238000002156 mixing Methods 0.000 claims abstract description 12
- -1 polyethylene terephthalate Polymers 0.000 claims abstract description 9
- 238000010438 heat treatment Methods 0.000 claims description 73
- 239000007787 solid Substances 0.000 claims description 70
- 239000011259 mixed solution Substances 0.000 claims description 65
- 238000003756 stirring Methods 0.000 claims description 60
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 claims description 59
- 239000004005 microsphere Substances 0.000 claims description 54
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 50
- 238000006243 chemical reaction Methods 0.000 claims description 49
- 239000000243 solution Substances 0.000 claims description 49
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 48
- 239000008367 deionised water Substances 0.000 claims description 45
- 229910021641 deionized water Inorganic materials 0.000 claims description 45
- 239000000203 mixture Substances 0.000 claims description 43
- 229910052982 molybdenum disulfide Inorganic materials 0.000 claims description 43
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 claims description 40
- 229910001981 cobalt nitrate Inorganic materials 0.000 claims description 40
- 238000005406 washing Methods 0.000 claims description 35
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 33
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 30
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 30
- 238000001816 cooling Methods 0.000 claims description 30
- NRTOMJZYCJJWKI-UHFFFAOYSA-N Titanium nitride Chemical compound [Ti]#N NRTOMJZYCJJWKI-UHFFFAOYSA-N 0.000 claims description 29
- 239000004696 Poly ether ether ketone Substances 0.000 claims description 28
- 229920002530 polyetherether ketone Polymers 0.000 claims description 28
- VKTGMGGBYBQLGR-UHFFFAOYSA-N [Si].[V].[V].[V] Chemical compound [Si].[V].[V].[V] VKTGMGGBYBQLGR-UHFFFAOYSA-N 0.000 claims description 27
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 26
- 239000002131 composite material Substances 0.000 claims description 26
- 239000010936 titanium Substances 0.000 claims description 26
- 229910052719 titanium Inorganic materials 0.000 claims description 26
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 22
- 239000012295 chemical reaction liquid Substances 0.000 claims description 21
- 238000001914 filtration Methods 0.000 claims description 20
- LXBGSDVWAMZHDD-UHFFFAOYSA-N 2-methyl-1h-imidazole Chemical compound CC1=NC=CN1 LXBGSDVWAMZHDD-UHFFFAOYSA-N 0.000 claims description 16
- 239000011261 inert gas Substances 0.000 claims description 15
- 239000007788 liquid Substances 0.000 claims description 15
- 239000005543 nano-size silicon particle Substances 0.000 claims description 15
- 235000012239 silicon dioxide Nutrition 0.000 claims description 15
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 15
- 239000002270 dispersing agent Substances 0.000 claims description 12
- 229920002545 silicone oil Polymers 0.000 claims description 12
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 11
- LLJNTLUXOZPFQB-UHFFFAOYSA-N [4-(4-fluorobenzoyl)phenyl]-(4-fluorophenyl)methanone Chemical compound C1=CC(F)=CC=C1C(=O)C1=CC=C(C(=O)C=2C=CC(F)=CC=2)C=C1 LLJNTLUXOZPFQB-UHFFFAOYSA-N 0.000 claims description 11
- ZFVMWEVVKGLCIJ-UHFFFAOYSA-N bisphenol AF Chemical compound C1=CC(O)=CC=C1C(C(F)(F)F)(C(F)(F)F)C1=CC=C(O)C=C1 ZFVMWEVVKGLCIJ-UHFFFAOYSA-N 0.000 claims description 11
- 229910000027 potassium carbonate Inorganic materials 0.000 claims description 11
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 10
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 10
- 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 10
- 239000004202 carbamide Substances 0.000 claims description 10
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 10
- DDXLVDQZPFLQMZ-UHFFFAOYSA-M dodecyl(trimethyl)azanium;chloride Chemical compound [Cl-].CCCCCCCCCCCC[N+](C)(C)C DDXLVDQZPFLQMZ-UHFFFAOYSA-M 0.000 claims description 10
- 229910002804 graphite Inorganic materials 0.000 claims description 10
- 239000010439 graphite Substances 0.000 claims description 10
- 238000010992 reflux Methods 0.000 claims description 10
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 8
- 229920002799 BoPET Polymers 0.000 claims description 7
- WZCQRUWWHSTZEM-UHFFFAOYSA-N 1,3-phenylenediamine Chemical compound NC1=CC=CC(N)=C1 WZCQRUWWHSTZEM-UHFFFAOYSA-N 0.000 claims description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 5
- 239000007789 gas Substances 0.000 claims description 5
- 239000001257 hydrogen Substances 0.000 claims description 5
- 229910052739 hydrogen Inorganic materials 0.000 claims description 5
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims description 5
- 230000007935 neutral effect Effects 0.000 claims description 5
- 230000001681 protective effect Effects 0.000 claims description 5
- 238000004062 sedimentation Methods 0.000 claims description 5
- 239000011863 silicon-based powder Substances 0.000 claims description 5
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 claims description 5
- 230000032683 aging Effects 0.000 abstract description 6
- 230000017525 heat dissipation Effects 0.000 abstract description 5
- 238000003754 machining Methods 0.000 abstract description 2
- 239000002861 polymer material Substances 0.000 abstract description 2
- 239000000463 material Substances 0.000 description 16
- 238000005336 cracking Methods 0.000 description 6
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 4
- RAXXELZNTBOGNW-UHFFFAOYSA-N imidazole Natural products C1=CNC=N1 RAXXELZNTBOGNW-UHFFFAOYSA-N 0.000 description 4
- 239000002904 solvent Substances 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- 239000004020 conductor Substances 0.000 description 3
- MHABMANUFPZXEB-UHFFFAOYSA-N O-demethyl-aloesaponarin I Natural products O=C1C2=CC=CC(O)=C2C(=O)C2=C1C=C(O)C(C(O)=O)=C2C MHABMANUFPZXEB-UHFFFAOYSA-N 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 238000007711 solidification Methods 0.000 description 2
- 230000008023 solidification Effects 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 229920001887 crystalline plastic Polymers 0.000 description 1
- 229940113088 dimethylacetamide Drugs 0.000 description 1
- 238000010292 electrical insulation Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
- C08J7/04—Coating
- C08J7/0427—Coating with only one layer of a composition containing a polymer binder
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D163/00—Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
- C09D7/62—Additives non-macromolecular inorganic modified by treatment with other compounds
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/65—Additives macromolecular
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/70—Additives characterised by shape, e.g. fibres, flakes or microspheres
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K3/00—Apparatus or processes for manufacturing printed circuits
- H05K3/0094—Filling or covering plated through-holes or blind plated vias, e.g. for masking or for mechanical reinforcement
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K3/00—Apparatus or processes for manufacturing printed circuits
- H05K3/40—Forming printed elements for providing electric connections to or between printed circuits
- H05K3/42—Plated through-holes or plated via connections
- H05K3/422—Plated through-holes or plated via connections characterised by electroless plating method; pretreatment therefor
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K3/00—Apparatus or processes for manufacturing printed circuits
- H05K3/44—Manufacturing insulated metal core circuits or other insulated electrically conductive core circuits
- H05K3/445—Manufacturing insulated metal core circuits or other insulated electrically conductive core circuits having insulated holes or insulated via connections through the metal core
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2367/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
- C08J2367/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2463/00—Characterised by the use of epoxy resins; Derivatives of epoxy resins
-
- 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
- C08K3/30—Sulfur-, selenium- or tellurium-containing compounds
- C08K2003/3009—Sulfides
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Manufacturing & Machinery (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Inorganic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention relates to the field of high polymer materials, in particular to a preparation method of a slotted hole filling film for a metal substrate, which comprises the following steps: s1, preparation of resin glue solution: weighing modified epoxy resin according to the weight, mixing the modified epoxy resin with a heat-conducting filler, dispersing, grinding and curing for 0.5-1 h, adding a curing agent and an auxiliary agent, dispersing and grinding for 2-8 h again, and standing for 2-12 h to obtain a resin glue solution; s2, preparation of a film: and (3) coating the resin glue solution on a PET (polyethylene terephthalate) glue film surface by using a precision coating machine, and drying to obtain the hole filling glue sheet. The hole-filling rubber sheet prepared by the invention has stronger voltage resistance, machining performance, heat conduction performance and high-temperature aging resistance, and can better meet the requirements of high voltage resistance and high heat dissipation.
Description
Technical Field
The invention relates to the field of high polymer materials, in particular to a preparation method of a rubber sheet for filling holes in slotted holes of a metal substrate.
Background
In recent years, the lighting and backlighting technology of the led has been developed and its related products have become popular. It is known that the light emitting diode generates a large amount of heat energy while generating bright light, and the heat energy cannot be effectively discharged by the light emitting diode, which will reduce the light emitting efficiency of the light emitting diode. In contrast, the conventional printed circuit board has not been coated with the substrate of the light emitting diode with high heat dissipation requirement due to low thermal conductivity, so that it is preferable to use a metal substrate or a metal core substrate with high heat dissipation efficiency.
The copper-clad plate is generally selected as the metal substrate, when the electronic component is installed on the copper-clad plate, holes need to be formed in the copper-clad plate, and meanwhile, because the conducting layer and the metal base layer are made of metal, in order to prevent short circuit, insulating fillers need to be filled in the hole walls after the holes are formed, and the conducting layer and the metal base layer are prevented from being conducted when the electronic component is arranged on the copper-clad plate. However, the existing hole-filling film for the slotted holes of the substrate has the following defects: the voltage resistance, the heat conduction performance and the high temperature and aging resistance are poor, and the requirements of high voltage resistance and high heat dissipation cannot be well met.
Disclosure of Invention
Aiming at the problems, the invention provides a preparation method of a metal substrate slotted hole filling film, which comprises the following steps:
s1, preparation of resin glue solution:
weighing modified epoxy resin according to the weight, mixing the modified epoxy resin with a heat-conducting filler, dispersing, grinding and curing for 0.5-1 h, adding a curing agent and an auxiliary agent, dispersing and grinding for 2-8 h again, and standing for 2-12 h to obtain a resin glue solution;
s2, preparation of a film:
and (3) coating the resin glue solution on a PET (polyethylene terephthalate) glue film surface by using a precision coating machine, and drying to obtain the hole filling glue sheet.
Preferably, the thickness of the PET film in the step S2 is 30-50 μm, and the coating thickness of the resin glue solution is 50-200 μm.
Preferably, seven sections of ovens are used for drying in the step S2, and the temperatures of the seven sections of ovens are set to be 70-80 ℃, 100-110 ℃, 120-130 ℃, 140-150 ℃, 160 ℃ and 160 ℃ in sequence.
Preferably, the resin glue solution comprises the following components in parts by weight:
60-80 parts of modified epoxy resin, 1-10 parts of heat-conducting filler, 0.5-5 parts of auxiliary agent and 10-30 parts of curing agent.
Preferably, the preparation method of the modified epoxy resin comprises the following steps:
s1, weighing nano molybdenum disulfide, adding the nano molybdenum disulfide into ethanol, and ultrasonically dispersing until the nano molybdenum disulfide is uniform to obtain a molybdenum disulfide mixed solution; weighing cobalt nitrate, adding the cobalt nitrate into ethanol, and performing ultrasonic dispersion until the cobalt nitrate is uniform to obtain a cobalt nitrate mixed solution;
wherein in the molybdenum disulfide mixed solution, the mass ratio of nano molybdenum disulfide to ethanol is 1: 3-10; in the cobalt nitrate mixed solution, the mass ratio of cobalt nitrate to ethanol is 1: 5-8;
s2, weighing 2-methylimidazole, adding the 2-methylimidazole into the molybdenum disulfide mixed solution, stirring the mixture uniformly, heating the mixture to 40-50 ℃, dropwise adding the cobalt nitrate mixed solution while stirring, performing reflux reaction for 2-3 hours after dropwise adding, cooling the mixture to room temperature, filtering the mixture to obtain a solid, washing the solid with deionized water for three times, then washing the solid with acetone for three times, and drying the solid under reduced pressure to obtain modified molybdenum disulfide;
wherein the mass ratio of the 2-methylimidazole to the molybdenum disulfide mixed liquid to the cobalt nitrate mixed liquid is 1: 6-8: 5-10;
s3, adding the modified molybdenum disulfide into epoxy resin, heating to 40-60 ℃, and stirring and dispersing uniformly to obtain modified epoxy resin;
the mass ratio of the modified molybdenum disulfide to the epoxy resin is 1: 5-10.
Preferably, the heat conducting filler is compounded by organic silicone oil, titanium nitride-vanadium silicide composite microspheres and soluble polyether ether ketone; wherein the mass ratio of the organic silicone oil to the titanium nitride-vanadium silicide composite microspheres to the soluble polyether-ether-ketone is 10: 0.5-3: 2-5.
Preferably, the preparation method of the titanium nitride-vanadium silicide composite microsphere comprises the following steps:
s1, preparing titanium nitride microspheres:
(1) weighing nano silicon dioxide, adding the nano silicon dioxide into deionized water, stirring the mixture evenly, sequentially adding tetrabutyl titanate and urea, and performing ultrasonic dispersion on the mixture evenly to obtain a mixed solution X;
wherein the mass ratio of the nano silicon dioxide to the tetrabutyl titanate to the urea to the deionized water is 1: 1.2-1.8: 1.4-3: 5-10;
(2) adding sodium dodecyl benzene sulfonate into the mixed solution X, stirring the mixed solution X uniformly, pouring the mixed solution into a reaction kettle, heating the mixed solution to 180-200 ℃, carrying out sealed reaction for 2-5 hours, cooling the mixed solution to room temperature, filtering the mixed solution to obtain a solid, washing the solid with deionized water for three times, and drying the solid under reduced pressure to obtain a solid Y;
wherein the mass ratio of the sodium dodecyl benzene sulfonate to the mixed liquid X is 1: 20-50;
(3) adding the solid Y into a high-temperature graphite furnace, heating to 700-1000 ℃ under the protection of inert gas, carrying out heat treatment for 1-3 h, and cooling to room temperature along with the furnace to obtain a solid Z;
(4) adding the solid Z into a sodium hydroxide solution with the mass concentration of 10-40%, slowly stirring for 8-12 h, filtering to obtain a solid, washing with deionized water until a washing solution is neutral, and drying under reduced pressure to obtain titanium nitride microspheres;
wherein the mass ratio of the solid Z to the sodium hydroxide solution is 1: 5-10;
s2, preparing vanadium silicide:
weighing metal vanadium powder and elemental silicon powder, uniformly mixing, adding into a high-temperature graphite furnace, introducing inert gas as protective gas, heating to 900-1100 ℃, reacting for 2-3 h, introducing hydrogen, heating to 1300-1500 ℃, reacting for 3-10 h, cooling to room temperature along with the furnace, and grinding to obtain vanadium silicide;
s3, preparing titanium nitride-vanadium silicide composite microspheres:
weighing the titanium nitride microspheres and the vanadium silicide, adding the titanium nitride microspheres and the vanadium silicide into deionized water, adding dodecyl trimethyl ammonium chloride, performing ultrasonic dispersion until the mixture is uniform, pouring the mixture into a reaction kettle, heating to 200-220 ℃, reacting for 6-8 hours, cooling to room temperature, filtering to obtain a solid, washing with deionized water for three times, and drying under reduced pressure to obtain titanium nitride-vanadium silicide composite microspheres;
the mass ratio of the titanium nitride microspheres to the vanadium silicide to the dodecyl trimethyl ammonium chloride to the deionized water is 1: 0.8-1.2: 0.05-0.1: 5-10.
Preferably, the preparation method of the soluble polyether-ether-ketone comprises the following steps:
s1, weighing 1, 4-bis (4' -fluorobenzoyl) benzene and bisphenol AF, adding the weighed materials into N-methylpyrrolidone, stirring the materials uniformly, adding potassium carbonate and toluene, heating the materials to 120-140 ℃ under the protection of inert gas, and carrying out reflux stirring reaction for 1-2 hours to obtain a reaction liquid A;
wherein the mass ratio of 1, 4-bis (4' -fluorobenzoyl) benzene, bisphenol AF, potassium carbonate, toluene and N-methylpyrrolidone is 1: 1.2-1.6: 0.02-0.05: 2-3: 8-10;
s2, heating the reaction liquid A to 170-190 ℃ for the second time, and stirring for reaction for 1-2 hours; heating to 230-250 ℃ for the third time, and stirring for reaction for 1-2 hours; heating to 270-290 ℃ for the fourth time, and stirring for reaction for 1-2 hours; heating to 300-320 ℃ for the fifth time, and stirring for reaction for 2-6 hours; obtaining reaction liquid B;
and S3, cooling the reaction liquid C to room temperature, then using ethanol for sedimentation, then using deionized water for washing for three times, and then drying under reduced pressure to obtain the soluble polyether-ether-ketone.
Preferably, the auxiliary agent is a 912 dispersant and/or a 3781 dispersant.
Preferably, the curing agent is N-hydroxyethyl metaphenylene diamine and/or N-hydroxypropyl metaphenylene diamine.
The invention has the beneficial effects that:
1. the invention provides a preparation method for a metal substrate slotted hole filling film, which is characterized in that a resin glue solution is prepared firstly, and then the resin glue solution is coated on a PET film surface to prepare the filling film. The hole-filling rubber sheet prepared by the invention has stronger voltage resistance, machining performance, heat conduction performance and high-temperature aging resistance, and can better meet the requirements of high voltage resistance and high heat dissipation.
2. Epoxy resin has the characteristics of easy curing, heat resistance, impact resistance, fatigue resistance, electric insulation and the like, is often used for a pore-filling rubber sheet, and has the defect of limiting the application of the pore-filling rubber sheet due to poor toughness. According to the invention, the epoxy resin is modified, so that the finally obtained product has stronger toughness. Specifically, the metal cobalt and 2-methylimidazole can form zeolite-like imidazole ester with high stability, the molybdenum disulfide with a layered structure is used as a carrier, the surface of the molybdenum disulfide is modified and grafted with the zeolite-like imidazole ester, the problem that the molybdenum disulfide is easy to stack and agglomerate is solved, and the modified molybdenum disulfide can improve the crystalline plastic and mechanical properties of the epoxy resin, so that the toughness of the epoxy resin is improved.
3. Even if the surface of the metal is smooth again, the metal surface is difficult to completely adhere to the organic material, in practical situations, the contact area of the pore-filling film and the metal substrate is often provided with a large number of fine gaps, the heat conduction of the gaps is transferred by air, and the heat conductivity coefficient of the air is only 0.023W/m.k in the conventional situation, so the heat conductivity of the film is greatly influenced. The invention solves the problem well by preparing the titanium nitride-vanadium silicide composite microsphere. The heat-conducting filler is prepared by preparing high-temperature-resistant titanium nitride into a microspherical shape with a large specific surface area, preparing vanadium silicide with high temperature resistance and high oxidation resistance, and grafting the vanadium silicide on the surface and pores of the titanium nitride microsphere, so that the heat-conducting property of the heat-conducting filler is improved, the problem of dispersibility of inorganic materials in heat-conducting materials is solved, bubbles in the heat-conducting materials are reduced, and the adhesion between the heat-conducting materials and a metal substrate is stronger and fewer bubbles are generated.
4. The polyether-ether-ketone has excellent heat resistance, water resistance, flame retardance and electrical insulation, and is very suitable for being used as a heat conduction material of electronic products, however, the currently prepared polyether-ether-ketone has high crystallinity, is difficult to dissolve in an organic solvent, has high melting temperature, and is difficult to be compounded with other materials. The invention synthesizes the soluble polyether-ether-ketone by using a gradual heating method, can be dissolved in solvents such as DMF, DMAC and the like, and improves the compounding capability of the polyether-ether-ketone and other materials. Specifically, 1, 4-bis (4' -fluorobenzoyl) benzene and bisphenol AF are used as synthesis raw materials, N-methylpyrrolidone is used as a solvent, potassium carbonate is used as a catalyst, and toluene is used as a water-carrying agent; firstly, heating to 120-140 ℃, wherein the solvent is completely fused with the reaction materials in the process; heating to 170-190 ℃ for the second time, carrying out salt forming reaction in the process, heating to 230-250 ℃ for the third time, wherein the salt forming reaction is completely carried out, and the water carrying agent and the water in the reaction liquid are almost completely evaporated; heating to 270-290 ℃ for the fourth time, and carrying out high-temperature prepolymerization reaction; and heating to 300-320 ℃ in the fifth time, and then entering a polymerization reaction stage, and completely performing the polymerization reaction within 2-6 hours. The crystallinity of the polyether-ether-ketone prepared by the preparation method is lower than that of the polyether-ether-ketone prepared by the conventional method to a large extent, and an ordered semi-crystalline solidification form is formed, so that a semi-crystalline solidification structure appears, and finally the obtained product has a small melt index and a large viscosity, and can be dissolved in solvents such as DMF (dimethyl formamide) and DMAC (dimethyl acetamide).
Detailed Description
The invention is further described with reference to the following examples.
Example 1
A preparation method of a slotted hole filling film for a metal substrate comprises the following steps:
s1, preparation of resin glue solution:
weighing modified epoxy resin according to the weight, mixing the modified epoxy resin with a heat-conducting filler, dispersing, grinding and curing for 0.5-1 h, adding a curing agent and an auxiliary agent, dispersing and grinding for 2-8 h again, and standing for 2-12 h to obtain a resin glue solution;
s2, preparation of a film:
and (3) coating the resin glue solution on a PET (polyethylene terephthalate) glue film surface by using a precision coating machine, and drying to obtain the hole filling glue sheet.
In the step S2, the thickness of the PET film is 30-50 μm, and the coating thickness of the resin glue solution is 50-200 μm.
In the step S2, seven sections of ovens are used for drying, and the temperatures of the seven sections of ovens are set to be 70-80 ℃, 100-110 ℃, 120-130 ℃, 140-150 ℃, 160 ℃ and 160 ℃ in sequence.
The resin glue solution comprises the following components in parts by weight:
70 parts of modified epoxy resin, 5 parts of heat-conducting filler, 3 parts of auxiliary agent and 20 parts of curing agent.
The preparation method of the modified epoxy resin comprises the following steps:
s1, weighing nano molybdenum disulfide, adding the nano molybdenum disulfide into ethanol, and ultrasonically dispersing until the nano molybdenum disulfide is uniform to obtain a molybdenum disulfide mixed solution; weighing cobalt nitrate, adding the cobalt nitrate into ethanol, and performing ultrasonic dispersion until the cobalt nitrate is uniform to obtain a cobalt nitrate mixed solution;
wherein in the molybdenum disulfide mixed solution, the mass ratio of nano molybdenum disulfide to ethanol is 1: 3-10; in the cobalt nitrate mixed solution, the mass ratio of cobalt nitrate to ethanol is 1: 5-8;
s2, weighing 2-methylimidazole, adding the 2-methylimidazole into the molybdenum disulfide mixed solution, stirring the mixture uniformly, heating the mixture to 40-50 ℃, dropwise adding the cobalt nitrate mixed solution while stirring, performing reflux reaction for 2-3 hours after dropwise adding, cooling the mixture to room temperature, filtering the mixture to obtain a solid, washing the solid with deionized water for three times, then washing the solid with acetone for three times, and drying the solid under reduced pressure to obtain modified molybdenum disulfide;
wherein the mass ratio of the 2-methylimidazole to the molybdenum disulfide mixed liquid to the cobalt nitrate mixed liquid is 1: 6-8: 5-10;
s3, adding the modified molybdenum disulfide into epoxy resin, heating to 40-60 ℃, and stirring and dispersing uniformly to obtain modified epoxy resin;
the mass ratio of the modified molybdenum disulfide to the epoxy resin is 1: 5-10.
The heat-conducting filler is compounded by organic silicone oil, titanium nitride-vanadium silicide composite microspheres and soluble polyether-ether-ketone; wherein the mass ratio of the organic silicone oil to the titanium nitride-vanadium silicide composite microspheres to the soluble polyether-ether-ketone is 10:2: 3.
The preparation method of the titanium nitride-vanadium silicide composite microsphere comprises the following steps:
s1, preparing titanium nitride microspheres:
(1) weighing nano silicon dioxide, adding the nano silicon dioxide into deionized water, stirring the mixture evenly, sequentially adding tetrabutyl titanate and urea, and performing ultrasonic dispersion on the mixture evenly to obtain a mixed solution X;
wherein the mass ratio of the nano silicon dioxide to the tetrabutyl titanate to the urea to the deionized water is 1: 1.2-1.8: 1.4-3: 5-10;
(2) adding sodium dodecyl benzene sulfonate into the mixed solution X, stirring the mixed solution X uniformly, pouring the mixed solution into a reaction kettle, heating the mixed solution to 180-200 ℃, carrying out sealed reaction for 2-5 hours, cooling the mixed solution to room temperature, filtering the mixed solution to obtain a solid, washing the solid with deionized water for three times, and drying the solid under reduced pressure to obtain a solid Y;
wherein the mass ratio of the sodium dodecyl benzene sulfonate to the mixed liquid X is 1: 20-50;
(3) adding the solid Y into a high-temperature graphite furnace, heating to 700-1000 ℃ under the protection of inert gas, carrying out heat treatment for 1-3 h, and cooling to room temperature along with the furnace to obtain a solid Z;
(4) adding the solid Z into a sodium hydroxide solution with the mass concentration of 10-40%, slowly stirring for 8-12 h, filtering to obtain a solid, washing with deionized water until a washing solution is neutral, and drying under reduced pressure to obtain titanium nitride microspheres;
wherein the mass ratio of the solid Z to the sodium hydroxide solution is 1: 5-10;
s2, preparing vanadium silicide:
weighing metal vanadium powder and elemental silicon powder, uniformly mixing, adding into a high-temperature graphite furnace, introducing inert gas as protective gas, heating to 900-1100 ℃, reacting for 2-3 h, introducing hydrogen, heating to 1300-1500 ℃, reacting for 3-10 h, cooling to room temperature along with the furnace, and grinding to obtain vanadium silicide;
s3, preparing titanium nitride-vanadium silicide composite microspheres:
weighing the titanium nitride microspheres and the vanadium silicide, adding the titanium nitride microspheres and the vanadium silicide into deionized water, adding dodecyl trimethyl ammonium chloride, performing ultrasonic dispersion until the mixture is uniform, pouring the mixture into a reaction kettle, heating to 200-220 ℃, reacting for 6-8 hours, cooling to room temperature, filtering to obtain a solid, washing with deionized water for three times, and drying under reduced pressure to obtain titanium nitride-vanadium silicide composite microspheres;
the mass ratio of the titanium nitride microspheres to the vanadium silicide to the dodecyl trimethyl ammonium chloride to the deionized water is 1: 0.8-1.2: 0.05-0.1: 5-10.
The preparation method of the soluble polyether-ether-ketone comprises the following steps:
s1, weighing 1, 4-bis (4' -fluorobenzoyl) benzene and bisphenol AF, adding the weighed materials into N-methylpyrrolidone, stirring the materials uniformly, adding potassium carbonate and toluene, heating the materials to 120-140 ℃ under the protection of inert gas, and carrying out reflux stirring reaction for 1-2 hours to obtain a reaction liquid A;
wherein the mass ratio of 1, 4-bis (4' -fluorobenzoyl) benzene, bisphenol AF, potassium carbonate, toluene and N-methylpyrrolidone is 1: 1.2-1.6: 0.02-0.05: 2-3: 8-10;
s2, heating the reaction liquid A to 170-190 ℃ for the second time, and stirring for reaction for 1-2 hours; heating to 230-250 ℃ for the third time, and stirring for reaction for 1-2 hours; heating to 270-290 ℃ for the fourth time, and stirring for reaction for 1-2 hours; heating to 300-320 ℃ for the fifth time, and stirring for reaction for 2-6 hours; obtaining reaction liquid B;
and S3, cooling the reaction liquid C to room temperature, then using ethanol for sedimentation, then using deionized water for washing for three times, and then drying under reduced pressure to obtain the soluble polyether-ether-ketone.
The auxiliary agent is 912 dispersing agent and/or 3781 dispersing agent.
The curing agent is N-hydroxyethyl metaphenylene diamine and/or N-hydroxypropyl metaphenylene diamine.
Example 2
A preparation method of a slotted hole filling film for a metal substrate comprises the following steps:
s1, preparation of resin glue solution:
weighing modified epoxy resin according to the weight, mixing the modified epoxy resin with a heat-conducting filler, dispersing, grinding and curing for 0.5-1 h, adding a curing agent and an auxiliary agent, dispersing and grinding for 2-8 h again, and standing for 2-12 h to obtain a resin glue solution;
s2, preparation of a film:
and (3) coating the resin glue solution on a PET (polyethylene terephthalate) glue film surface by using a precision coating machine, and drying to obtain the hole filling glue sheet.
In the step S2, the thickness of the PET film is 30-50 μm, and the coating thickness of the resin glue solution is 50-200 μm.
In the step S2, seven sections of ovens are used for drying, and the temperatures of the seven sections of ovens are set to be 70-80 ℃, 100-110 ℃, 120-130 ℃, 140-150 ℃, 160 ℃ and 160 ℃ in sequence.
The resin glue solution comprises the following components in parts by weight:
60 parts of modified epoxy resin, 1 part of heat-conducting filler, 0.5 part of auxiliary agent and 10 parts of curing agent.
The preparation method of the modified epoxy resin comprises the following steps:
s1, weighing nano molybdenum disulfide, adding the nano molybdenum disulfide into ethanol, and ultrasonically dispersing until the nano molybdenum disulfide is uniform to obtain a molybdenum disulfide mixed solution; weighing cobalt nitrate, adding the cobalt nitrate into ethanol, and performing ultrasonic dispersion until the cobalt nitrate is uniform to obtain a cobalt nitrate mixed solution;
wherein in the molybdenum disulfide mixed solution, the mass ratio of nano molybdenum disulfide to ethanol is 1: 3-10; in the cobalt nitrate mixed solution, the mass ratio of cobalt nitrate to ethanol is 1: 5-8;
s2, weighing 2-methylimidazole, adding the 2-methylimidazole into the molybdenum disulfide mixed solution, stirring the mixture uniformly, heating the mixture to 40-50 ℃, dropwise adding the cobalt nitrate mixed solution while stirring, performing reflux reaction for 2-3 hours after dropwise adding, cooling the mixture to room temperature, filtering the mixture to obtain a solid, washing the solid with deionized water for three times, then washing the solid with acetone for three times, and drying the solid under reduced pressure to obtain modified molybdenum disulfide;
wherein the mass ratio of the 2-methylimidazole to the molybdenum disulfide mixed liquid to the cobalt nitrate mixed liquid is 1: 6-8: 5-10;
s3, adding the modified molybdenum disulfide into epoxy resin, heating to 40-60 ℃, and stirring and dispersing uniformly to obtain modified epoxy resin;
the mass ratio of the modified molybdenum disulfide to the epoxy resin is 1: 5-10.
The heat-conducting filler is compounded by organic silicone oil, titanium nitride-vanadium silicide composite microspheres and soluble polyether-ether-ketone; wherein the mass ratio of the organic silicone oil to the titanium nitride-vanadium silicide composite microspheres to the soluble polyether-ether-ketone is 10:0.5: 2.
The preparation method of the titanium nitride-vanadium silicide composite microsphere comprises the following steps:
s1, preparing titanium nitride microspheres:
(1) weighing nano silicon dioxide, adding the nano silicon dioxide into deionized water, stirring the mixture evenly, sequentially adding tetrabutyl titanate and urea, and performing ultrasonic dispersion on the mixture evenly to obtain a mixed solution X;
wherein the mass ratio of the nano silicon dioxide to the tetrabutyl titanate to the urea to the deionized water is 1: 1.2-1.8: 1.4-3: 5-10;
(2) adding sodium dodecyl benzene sulfonate into the mixed solution X, stirring the mixed solution X uniformly, pouring the mixed solution into a reaction kettle, heating the mixed solution to 180-200 ℃, carrying out sealed reaction for 2-5 hours, cooling the mixed solution to room temperature, filtering the mixed solution to obtain a solid, washing the solid with deionized water for three times, and drying the solid under reduced pressure to obtain a solid Y;
wherein the mass ratio of the sodium dodecyl benzene sulfonate to the mixed liquid X is 1: 20-50;
(3) adding the solid Y into a high-temperature graphite furnace, heating to 700-1000 ℃ under the protection of inert gas, carrying out heat treatment for 1-3 h, and cooling to room temperature along with the furnace to obtain a solid Z;
(4) adding the solid Z into a sodium hydroxide solution with the mass concentration of 10-40%, slowly stirring for 8-12 h, filtering to obtain a solid, washing with deionized water until a washing solution is neutral, and drying under reduced pressure to obtain titanium nitride microspheres;
wherein the mass ratio of the solid Z to the sodium hydroxide solution is 1: 5-10;
s2, preparing vanadium silicide:
weighing metal vanadium powder and elemental silicon powder, uniformly mixing, adding into a high-temperature graphite furnace, introducing inert gas as protective gas, heating to 900-1100 ℃, reacting for 2-3 h, introducing hydrogen, heating to 1300-1500 ℃, reacting for 3-10 h, cooling to room temperature along with the furnace, and grinding to obtain vanadium silicide;
s3, preparing titanium nitride-vanadium silicide composite microspheres:
weighing the titanium nitride microspheres and the vanadium silicide, adding the titanium nitride microspheres and the vanadium silicide into deionized water, adding dodecyl trimethyl ammonium chloride, performing ultrasonic dispersion until the mixture is uniform, pouring the mixture into a reaction kettle, heating to 200-220 ℃, reacting for 6-8 hours, cooling to room temperature, filtering to obtain a solid, washing with deionized water for three times, and drying under reduced pressure to obtain titanium nitride-vanadium silicide composite microspheres;
the mass ratio of the titanium nitride microspheres to the vanadium silicide to the dodecyl trimethyl ammonium chloride to the deionized water is 1: 0.8-1.2: 0.05-0.1: 5-10.
The preparation method of the soluble polyether-ether-ketone comprises the following steps:
s1, weighing 1, 4-bis (4' -fluorobenzoyl) benzene and bisphenol AF, adding the weighed materials into N-methylpyrrolidone, stirring the materials uniformly, adding potassium carbonate and toluene, heating the materials to 120-140 ℃ under the protection of inert gas, and carrying out reflux stirring reaction for 1-2 hours to obtain a reaction liquid A;
wherein the mass ratio of 1, 4-bis (4' -fluorobenzoyl) benzene, bisphenol AF, potassium carbonate, toluene and N-methylpyrrolidone is 1: 1.2-1.6: 0.02-0.05: 2-3: 8-10;
s2, heating the reaction liquid A to 170-190 ℃ for the second time, and stirring for reaction for 1-2 hours; heating to 230-250 ℃ for the third time, and stirring for reaction for 1-2 hours; heating to 270-290 ℃ for the fourth time, and stirring for reaction for 1-2 hours; heating to 300-320 ℃ for the fifth time, and stirring for reaction for 2-6 hours; obtaining reaction liquid B;
and S3, cooling the reaction liquid C to room temperature, then using ethanol for sedimentation, then using deionized water for washing for three times, and then drying under reduced pressure to obtain the soluble polyether-ether-ketone.
The auxiliary agent is 912 dispersing agent and/or 3781 dispersing agent.
The curing agent is N-hydroxyethyl metaphenylene diamine and/or N-hydroxypropyl metaphenylene diamine.
Example 3
A preparation method of a slotted hole filling film for a metal substrate comprises the following steps:
s1, preparation of resin glue solution:
weighing modified epoxy resin according to the weight, mixing the modified epoxy resin with a heat-conducting filler, dispersing, grinding and curing for 0.5-1 h, adding a curing agent and an auxiliary agent, dispersing and grinding for 2-8 h again, and standing for 2-12 h to obtain a resin glue solution;
s2, preparation of a film:
and (3) coating the resin glue solution on a PET (polyethylene terephthalate) glue film surface by using a precision coating machine, and drying to obtain the hole filling glue sheet.
In the step S2, the thickness of the PET film is 30-50 μm, and the coating thickness of the resin glue solution is 50-200 μm.
In the step S2, seven sections of ovens are used for drying, and the temperatures of the seven sections of ovens are set to be 70-80 ℃, 100-110 ℃, 120-130 ℃, 140-150 ℃, 160 ℃ and 160 ℃ in sequence.
The resin glue solution comprises the following components in parts by weight:
80 parts of modified epoxy resin, 10 parts of heat-conducting filler, 5 parts of auxiliary agent and 30 parts of curing agent.
The preparation method of the modified epoxy resin comprises the following steps:
s1, weighing nano molybdenum disulfide, adding the nano molybdenum disulfide into ethanol, and ultrasonically dispersing until the nano molybdenum disulfide is uniform to obtain a molybdenum disulfide mixed solution; weighing cobalt nitrate, adding the cobalt nitrate into ethanol, and performing ultrasonic dispersion until the cobalt nitrate is uniform to obtain a cobalt nitrate mixed solution;
wherein in the molybdenum disulfide mixed solution, the mass ratio of nano molybdenum disulfide to ethanol is 1: 3-10; in the cobalt nitrate mixed solution, the mass ratio of cobalt nitrate to ethanol is 1: 5-8;
s2, weighing 2-methylimidazole, adding the 2-methylimidazole into the molybdenum disulfide mixed solution, stirring the mixture uniformly, heating the mixture to 40-50 ℃, dropwise adding the cobalt nitrate mixed solution while stirring, performing reflux reaction for 2-3 hours after dropwise adding, cooling the mixture to room temperature, filtering the mixture to obtain a solid, washing the solid with deionized water for three times, then washing the solid with acetone for three times, and drying the solid under reduced pressure to obtain modified molybdenum disulfide;
wherein the mass ratio of the 2-methylimidazole to the molybdenum disulfide mixed liquid to the cobalt nitrate mixed liquid is 1: 6-8: 5-10;
s3, adding the modified molybdenum disulfide into epoxy resin, heating to 40-60 ℃, and stirring and dispersing uniformly to obtain modified epoxy resin;
the mass ratio of the modified molybdenum disulfide to the epoxy resin is 1: 5-10.
The heat-conducting filler is compounded by organic silicone oil, titanium nitride-vanadium silicide composite microspheres and soluble polyether-ether-ketone; wherein the mass ratio of the organic silicone oil to the titanium nitride-vanadium silicide composite microspheres to the soluble polyether-ether-ketone is 10:3: 5.
The preparation method of the titanium nitride-vanadium silicide composite microsphere comprises the following steps:
s1, preparing titanium nitride microspheres:
(1) weighing nano silicon dioxide, adding the nano silicon dioxide into deionized water, stirring the mixture evenly, sequentially adding tetrabutyl titanate and urea, and performing ultrasonic dispersion on the mixture evenly to obtain a mixed solution X;
wherein the mass ratio of the nano silicon dioxide to the tetrabutyl titanate to the urea to the deionized water is 1: 1.2-1.8: 1.4-3: 5-10;
(2) adding sodium dodecyl benzene sulfonate into the mixed solution X, stirring the mixed solution X uniformly, pouring the mixed solution into a reaction kettle, heating the mixed solution to 180-200 ℃, carrying out sealed reaction for 2-5 hours, cooling the mixed solution to room temperature, filtering the mixed solution to obtain a solid, washing the solid with deionized water for three times, and drying the solid under reduced pressure to obtain a solid Y;
wherein the mass ratio of the sodium dodecyl benzene sulfonate to the mixed liquid X is 1: 20-50;
(3) adding the solid Y into a high-temperature graphite furnace, heating to 700-1000 ℃ under the protection of inert gas, carrying out heat treatment for 1-3 h, and cooling to room temperature along with the furnace to obtain a solid Z;
(4) adding the solid Z into a sodium hydroxide solution with the mass concentration of 10-40%, slowly stirring for 8-12 h, filtering to obtain a solid, washing with deionized water until a washing solution is neutral, and drying under reduced pressure to obtain titanium nitride microspheres;
wherein the mass ratio of the solid Z to the sodium hydroxide solution is 1: 5-10;
s2, preparing vanadium silicide:
weighing metal vanadium powder and elemental silicon powder, uniformly mixing, adding into a high-temperature graphite furnace, introducing inert gas as protective gas, heating to 900-1100 ℃, reacting for 2-3 h, introducing hydrogen, heating to 1300-1500 ℃, reacting for 3-10 h, cooling to room temperature along with the furnace, and grinding to obtain vanadium silicide;
s3, preparing titanium nitride-vanadium silicide composite microspheres:
weighing the titanium nitride microspheres and the vanadium silicide, adding the titanium nitride microspheres and the vanadium silicide into deionized water, adding dodecyl trimethyl ammonium chloride, performing ultrasonic dispersion until the mixture is uniform, pouring the mixture into a reaction kettle, heating to 200-220 ℃, reacting for 6-8 hours, cooling to room temperature, filtering to obtain a solid, washing with deionized water for three times, and drying under reduced pressure to obtain titanium nitride-vanadium silicide composite microspheres;
the mass ratio of the titanium nitride microspheres to the vanadium silicide to the dodecyl trimethyl ammonium chloride to the deionized water is 1: 0.8-1.2: 0.05-0.1: 5-10.
The preparation method of the soluble polyether-ether-ketone comprises the following steps:
s1, weighing 1, 4-bis (4' -fluorobenzoyl) benzene and bisphenol AF, adding the weighed materials into N-methylpyrrolidone, stirring the materials uniformly, adding potassium carbonate and toluene, heating the materials to 120-140 ℃ under the protection of inert gas, and carrying out reflux stirring reaction for 1-2 hours to obtain a reaction liquid A;
wherein the mass ratio of 1, 4-bis (4' -fluorobenzoyl) benzene, bisphenol AF, potassium carbonate, toluene and N-methylpyrrolidone is 1: 1.2-1.6: 0.02-0.05: 2-3: 8-10;
s2, heating the reaction liquid A to 170-190 ℃ for the second time, and stirring for reaction for 1-2 hours; heating to 230-250 ℃ for the third time, and stirring for reaction for 1-2 hours; heating to 270-290 ℃ for the fourth time, and stirring for reaction for 1-2 hours; heating to 300-320 ℃ for the fifth time, and stirring for reaction for 2-6 hours; obtaining reaction liquid B;
and S3, cooling the reaction liquid C to room temperature, then using ethanol for sedimentation, then using deionized water for washing for three times, and then drying under reduced pressure to obtain the soluble polyether-ether-ketone.
The auxiliary agent is 912 dispersing agent and/or 3781 dispersing agent.
The curing agent is N-hydroxyethyl metaphenylene diamine and/or N-hydroxypropyl metaphenylene diamine.
Comparative example
A preparation method of a slotted hole filling film for a metal substrate comprises the following steps:
s1, preparation of resin glue solution:
weighing modified epoxy resin according to the weight, mixing the modified epoxy resin with a heat-conducting filler, dispersing, grinding and curing for 0.5-1 h, adding a curing agent and an auxiliary agent, dispersing and grinding for 2-8 h again, and standing for 2-12 h to obtain a resin glue solution;
s2, preparation of a film:
and (3) coating the resin glue solution on a PET (polyethylene terephthalate) glue film surface by using a precision coating machine, and drying to obtain the hole filling glue sheet.
In the step S2, the thickness of the PET film is 30-50 μm, and the coating thickness of the resin glue solution is 50-200 μm.
In the step S2, seven sections of ovens are used for drying, and the temperatures of the seven sections of ovens are set to be 70-80 ℃, 100-110 ℃, 120-130 ℃, 140-150 ℃, 160 ℃ and 160 ℃ in sequence.
The resin glue solution comprises the following components in parts by weight:
70 parts of epoxy resin, 5 parts of heat-conducting filler, 3 parts of auxiliary agent and 20 parts of curing agent.
The heat-conducting filler is compounded by organic silicone oil, titanium nitride microspheres and polyether ether ketone; wherein the mass ratio of the organic silicone oil to the titanium nitride microspheres to the polyether-ether-ketone is 10:2: 3.
The auxiliary agent is 912 dispersing agent and/or 3781 dispersing agent.
The curing agent is N-hydroxyethyl metaphenylene diamine and/or N-hydroxypropyl metaphenylene diamine.
To illustrate the present invention more clearly, the slotted hole filling rubber sheets of the metal substrates prepared in examples 1 to 3 of the present invention and comparative examples were prepared in a shape of length × width × height 10mm × 10mm × 5mm, and the results of performance tests were shown in table 1:
wherein, the arc resistance is tested according to the 5.3 th item in GB/T2567-2008, the test temperature is 23 +/-2 ℃, and the bending rate is 10 mm/min;
the dielectric strength is measured by a dielectric strength tester;
the thermal conductivity was measured by the unsteady state hot wire method using an LFA447 type thermal conductivity meter from NETZSCH;
the high-temperature aging resistance is that the pore-filling rubber sheet is placed in an oven at 250 ℃ for heat treatment for 72h, and whether cracking or crazing occurs is detected.
Table 1 performance testing of hole-filled films
| Example 1 | Example 2 | Example 3 | Comparative example | |
| Arc resistance/s | 232 | 225 | 228 | 142 |
| Dielectric strength/MV · m-1 | 18.6 | 18.1 | 18.3 | 5.3 |
| Thermal conductivity/W (mK)-1 | 8.96 | 8.32 | 8.57 | 3.21 |
| High temperature aging resistance | No cracking and crazing | No cracking and crazing | No cracking and crazing | Cracking in 30% area |
As can be seen from Table 1, the pore-filling rubber sheets prepared in the embodiments 1-3 of the invention have better arc resistance and higher dielectric strength, which indicates that the pore-filling rubber sheets have excellent voltage resistance; the heat conductivity can reach 8.96W/(mK), which shows that the heat conduction and radiation performance is better; after heat treatment for 72 hours in an oven at 250 ℃, cracking and crazing phenomena still do not occur, which indicates that the high-temperature aging resistance is better.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention, and not for limiting the protection scope of the present invention, although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (5)
1. A preparation method of a slotted hole filling film for a metal substrate is characterized by comprising the following steps:
s1, preparation of resin glue solution:
weighing modified epoxy resin according to the weight, mixing the modified epoxy resin with a heat-conducting filler, dispersing, grinding and curing for 0.5-1 h, adding a curing agent and an auxiliary agent, dispersing and grinding for 2-8 h again, and standing for 2-12 h to obtain a resin glue solution;
s2, preparation of a film:
coating the resin glue solution on a PET (polyethylene terephthalate) glue film surface by using a precision coating machine, and drying to obtain a hole filling glue sheet;
the resin glue solution comprises the following components in parts by weight:
60-80 parts of modified epoxy resin, 1-10 parts of heat-conducting filler, 0.5-5 parts of auxiliary agent and 10-30 parts of curing agent;
the preparation method of the modified epoxy resin comprises the following steps:
A1. weighing nano molybdenum disulfide, adding the nano molybdenum disulfide into ethanol, and ultrasonically dispersing until the nano molybdenum disulfide is uniform to obtain a molybdenum disulfide mixed solution; weighing cobalt nitrate, adding the cobalt nitrate into ethanol, and performing ultrasonic dispersion until the cobalt nitrate is uniform to obtain a cobalt nitrate mixed solution;
wherein in the molybdenum disulfide mixed solution, the mass ratio of nano molybdenum disulfide to ethanol is 1: 3-10; in the cobalt nitrate mixed solution, the mass ratio of cobalt nitrate to ethanol is 1: 5-8;
A2. weighing 2-methylimidazole, adding the 2-methylimidazole into the molybdenum disulfide mixed solution, stirring the mixture uniformly, heating the mixture to 40-50 ℃, dropwise adding the cobalt nitrate mixed solution while stirring, performing reflux reaction for 2-3 hours after dropwise adding, cooling the mixture to room temperature, filtering the mixture to obtain a solid, washing the solid with deionized water for three times, then washing the solid with acetone for three times, and drying the solid under reduced pressure to obtain modified molybdenum disulfide;
wherein the mass ratio of the 2-methylimidazole to the molybdenum disulfide mixed liquid to the cobalt nitrate mixed liquid is 1: 6-8: 5-10;
A3. adding the modified molybdenum disulfide into epoxy resin, heating to 40-60 ℃, and stirring and dispersing uniformly to obtain modified epoxy resin;
the mass ratio of the modified molybdenum disulfide to the epoxy resin is 1: 5-10;
the heat-conducting filler comprises organic silicone oil, titanium nitride-vanadium silicide composite microspheres and soluble polyether-ether-ketone; wherein the mass ratio of the organic silicone oil to the titanium nitride-vanadium silicide composite microspheres to the soluble polyether-ether-ketone is 10: 0.5-3: 2-5;
the preparation method of the titanium nitride-vanadium silicide composite microsphere comprises the following steps:
B1. preparing titanium nitride microspheres:
(1) weighing nano silicon dioxide, adding the nano silicon dioxide into deionized water, stirring the mixture evenly, sequentially adding tetrabutyl titanate and urea, and performing ultrasonic dispersion on the mixture evenly to obtain a mixed solution X;
wherein the mass ratio of the nano silicon dioxide to the tetrabutyl titanate to the urea to the deionized water is 1: 1.2-1.8: 1.4-3: 5-10;
(2) adding sodium dodecyl benzene sulfonate into the mixed solution X, stirring the mixed solution X uniformly, pouring the mixed solution into a reaction kettle, heating the mixed solution to 180-200 ℃, carrying out sealed reaction for 2-5 hours, cooling the mixed solution to room temperature, filtering the mixed solution to obtain a solid, washing the solid with deionized water for three times, and drying the solid under reduced pressure to obtain a solid Y;
wherein the mass ratio of the sodium dodecyl benzene sulfonate to the mixed liquid X is 1: 20-50;
(3) adding the solid Y into a high-temperature graphite furnace, heating to 700-1000 ℃ under the protection of inert gas, carrying out heat treatment for 1-3 h, and cooling to room temperature along with the furnace to obtain a solid Z;
(4) adding the solid Z into a sodium hydroxide solution with the mass concentration of 10-40%, slowly stirring for 8-12 h, filtering to obtain a solid, washing with deionized water until a washing solution is neutral, and drying under reduced pressure to obtain titanium nitride microspheres;
wherein the mass ratio of the solid Z to the sodium hydroxide solution is 1: 5-10;
B2. preparing vanadium silicide:
weighing metal vanadium powder and elemental silicon powder, uniformly mixing, adding into a high-temperature graphite furnace, introducing inert gas as protective gas, heating to 900-1100 ℃, reacting for 2-3 h, introducing hydrogen, heating to 1300-1500 ℃, reacting for 3-10 h, cooling to room temperature along with the furnace, and grinding to obtain vanadium silicide;
B3. preparing titanium nitride-vanadium silicide composite microspheres:
weighing the titanium nitride microspheres and the vanadium silicide, adding the titanium nitride microspheres and the vanadium silicide into deionized water, adding dodecyl trimethyl ammonium chloride, performing ultrasonic dispersion until the mixture is uniform, pouring the mixture into a reaction kettle, heating to 200-220 ℃, reacting for 6-8 hours, cooling to room temperature, filtering to obtain a solid, washing with deionized water for three times, and drying under reduced pressure to obtain titanium nitride-vanadium silicide composite microspheres;
wherein the mass ratio of the titanium nitride microspheres to the vanadium silicide to the dodecyl trimethyl ammonium chloride to the deionized water is 1: 0.8-1.2: 0.05-0.1: 5-10;
the preparation method of the soluble polyether-ether-ketone comprises the following steps:
C1. weighing 1, 4-bis (4' -fluorobenzoyl) benzene and bisphenol AF, adding the mixture into N-methylpyrrolidone, stirring the mixture uniformly, adding potassium carbonate and toluene, heating the mixture to 120-140 ℃ under the protection of inert gas, and carrying out reflux stirring reaction for 1-2 hours to obtain a reaction liquid A;
wherein the mass ratio of 1, 4-bis (4' -fluorobenzoyl) benzene, bisphenol AF, potassium carbonate, toluene and N-methylpyrrolidone is 1: 1.2-1.6: 0.02-0.05: 2-3: 8-10;
C2. heating the reaction liquid A to 170-190 ℃ for the second time, and stirring for reaction for 1-2 hours; heating to 230-250 ℃ for the third time, and stirring for reaction for 1-2 hours; heating to 270-290 ℃ for the fourth time, and stirring for reaction for 1-2 hours; heating to 300-320 ℃ for the fifth time, and stirring for reaction for 2-6 hours; obtaining reaction liquid B;
C3. and cooling the reaction liquid B to room temperature, then using ethanol for sedimentation, then using deionized water for washing for three times, and then drying under reduced pressure to obtain the soluble polyether-ether-ketone.
2. A method as claimed in claim 1, wherein the thickness of the PET film in step S2 is 30-50 μm, and the thickness of the resin glue is 50-200 μm.
3. The method as claimed in claim 1, wherein the seven-section oven is used in the step S2, and the temperature of the seven-section oven is set to 70-80 ℃, 100-110 ℃, 120-130 ℃, 140-150 ℃, 160 ℃ and 160 ℃ in sequence.
4. The method for preparing a slotted hole filling film for a metal substrate according to claim 1, wherein the auxiliary agent is 912 dispersant and/or 3781 dispersant.
5. The method as claimed in claim 1, wherein the curing agent is N-hydroxyethyl meta-phenylenediamine and/or N-hydroxypropyl meta-phenylenediamine.
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