CN114316742A - Coating for circuit board base plate and preparation method thereof - Google Patents
Coating for circuit board base plate and preparation method thereof Download PDFInfo
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- CN114316742A CN114316742A CN202111605217.1A CN202111605217A CN114316742A CN 114316742 A CN114316742 A CN 114316742A CN 202111605217 A CN202111605217 A CN 202111605217A CN 114316742 A CN114316742 A CN 114316742A
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- 238000000576 coating method Methods 0.000 title claims abstract description 112
- 239000011248 coating agent Substances 0.000 title claims abstract description 108
- 238000002360 preparation method Methods 0.000 title claims abstract description 40
- 239000000945 filler Substances 0.000 claims abstract description 123
- 239000003822 epoxy resin Substances 0.000 claims abstract description 84
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 84
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 61
- 238000005303 weighing Methods 0.000 claims abstract description 35
- 238000003756 stirring Methods 0.000 claims abstract description 28
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 23
- 238000001035 drying Methods 0.000 claims abstract description 17
- 239000002994 raw material Substances 0.000 claims abstract description 17
- 238000002156 mixing Methods 0.000 claims abstract description 16
- 239000000654 additive Substances 0.000 claims abstract description 13
- 230000000996 additive effect Effects 0.000 claims abstract description 13
- 239000000203 mixture Substances 0.000 claims abstract description 9
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 106
- 239000002121 nanofiber Substances 0.000 claims description 59
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 45
- 239000002245 particle Substances 0.000 claims description 26
- ZDXPYRJPNDTMRX-UHFFFAOYSA-N glutamine Natural products OC(=O)C(N)CCC(N)=O ZDXPYRJPNDTMRX-UHFFFAOYSA-N 0.000 claims description 22
- 239000000843 powder Substances 0.000 claims description 21
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 20
- 238000000034 method Methods 0.000 claims description 18
- 238000002791 soaking Methods 0.000 claims description 17
- 239000013078 crystal Substances 0.000 claims description 15
- RAXXELZNTBOGNW-UHFFFAOYSA-N imidazole Natural products C1=CNC=N1 RAXXELZNTBOGNW-UHFFFAOYSA-N 0.000 claims description 14
- 239000002518 antifoaming agent Substances 0.000 claims description 13
- 239000002270 dispersing agent Substances 0.000 claims description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 claims description 8
- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 claims description 7
- 235000010413 sodium alginate Nutrition 0.000 claims description 7
- 229940005550 sodium alginate Drugs 0.000 claims description 7
- 239000000661 sodium alginate Substances 0.000 claims description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 6
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 6
- 239000004202 carbamide Substances 0.000 claims description 6
- QGBSISYHAICWAH-UHFFFAOYSA-N dicyandiamide Chemical compound NC(N)=NC#N QGBSISYHAICWAH-UHFFFAOYSA-N 0.000 claims description 5
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims description 4
- 229920001568 phenolic resin Polymers 0.000 claims description 4
- 229920000877 Melamine resin Polymers 0.000 claims description 3
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims description 3
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 3
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 3
- 239000000377 silicon dioxide Substances 0.000 claims description 3
- 239000005007 epoxy-phenolic resin Substances 0.000 claims description 2
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 2
- 235000012239 silicon dioxide Nutrition 0.000 claims description 2
- 229910001928 zirconium oxide Inorganic materials 0.000 claims description 2
- 239000011247 coating layer Substances 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 claims 1
- 239000002861 polymer material Substances 0.000 abstract description 2
- ZDXPYRJPNDTMRX-VKHMYHEASA-N L-glutamine Chemical compound OC(=O)[C@@H](N)CCC(N)=O ZDXPYRJPNDTMRX-VKHMYHEASA-N 0.000 description 21
- 238000004132 cross linking Methods 0.000 description 16
- 230000000052 comparative effect Effects 0.000 description 15
- 125000003277 amino group Chemical group 0.000 description 9
- 125000003700 epoxy group Chemical group 0.000 description 9
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 9
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 description 7
- 230000000694 effects Effects 0.000 description 7
- 238000005553 drilling Methods 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 5
- -1 polydimethylsiloxane Polymers 0.000 description 5
- 229920005989 resin Polymers 0.000 description 5
- 239000011347 resin Substances 0.000 description 5
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 4
- 239000004205 dimethyl polysiloxane Substances 0.000 description 4
- 238000011049 filling Methods 0.000 description 4
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 4
- 230000010355 oscillation Effects 0.000 description 4
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- 239000004359 castor oil Substances 0.000 description 3
- 235000019438 castor oil Nutrition 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000011094 fiberboard Substances 0.000 description 3
- ZEMPKEQAKRGZGQ-XOQCFJPHSA-N glycerol triricinoleate Natural products CCCCCC[C@@H](O)CC=CCCCCCCCC(=O)OC[C@@H](COC(=O)CCCCCCCC=CC[C@@H](O)CCCCCC)OC(=O)CCCCCCCC=CC[C@H](O)CCCCCC ZEMPKEQAKRGZGQ-XOQCFJPHSA-N 0.000 description 3
- 238000000227 grinding Methods 0.000 description 3
- 230000001050 lubricating effect Effects 0.000 description 3
- 239000003973 paint Substances 0.000 description 3
- 238000011056 performance test Methods 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 229920001187 thermosetting polymer Polymers 0.000 description 3
- 238000001132 ultrasonic dispersion Methods 0.000 description 3
- LLPKQRMDOFYSGZ-UHFFFAOYSA-N 2,5-dimethyl-1h-imidazole Chemical group CC1=CN=C(C)N1 LLPKQRMDOFYSGZ-UHFFFAOYSA-N 0.000 description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 2
- 238000007792 addition Methods 0.000 description 2
- 238000010382 chemical cross-linking Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012856 packing Methods 0.000 description 2
- 239000005011 phenolic resin Substances 0.000 description 2
- 229910052698 phosphorus Inorganic materials 0.000 description 2
- 239000011574 phosphorus Substances 0.000 description 2
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 1
- 229930182816 L-glutamine Natural products 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- 229910052581 Si3N4 Inorganic materials 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000004841 bisphenol A epoxy resin Substances 0.000 description 1
- VPKDCDLSJZCGKE-UHFFFAOYSA-N carbodiimide group Chemical group N=C=N VPKDCDLSJZCGKE-UHFFFAOYSA-N 0.000 description 1
- 150000001718 carbodiimides Chemical class 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 229920001971 elastomer Polymers 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000006266 etherification reaction Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 125000002883 imidazolyl group Chemical group 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
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000011087 paperboard Substances 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
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Abstract
The application relates to the field of high polymer materials, and particularly discloses a coating for a circuit board base plate and a preparation method thereof; a coating for a circuit board base plate is prepared by curing a coating; the coating is prepared from the following raw materials in parts by weight: 30-50 parts of epoxy resin, 6-10 parts of curing agent, 3-5 parts of cross-linking agent, 1-3 parts of additive, 40-60 parts of filler and 3-5 parts of toner; the preparation method comprises the following steps: weighing epoxy resin and filler, stirring and mixing uniformly to prepare a mixture; weighing a curing agent, a cross-linking agent, a toner, an additive and a mixture, mixing and stirring uniformly, and performing vacuum defoaming to prepare a coating; drying and curing the coating to form a coating; so that the coating has higher surface hardness.
Description
Technical Field
The application relates to the field of high polymer materials, in particular to a coating for a circuit board base plate and a preparation method thereof.
Background
The circuit board backing board is prepared by taking a high-density fiberboard as a substrate and coating a coating on the surface of the high-density fiberboard.
The circuit board base plate needs to have better hardness, and burrs on the upper surface of a drilled hole are prevented and reduced; the traditional medium-density and high-density fiber board can not meet the quality requirement of drilling and has relatively low surface hardness; the traditional resin coating can partially improve the hardness of the wire board, but cannot reach the hardness of the phenolic paper board, and still has certain influence on the drilling quality.
Therefore, it is highly desirable to produce a coating having a higher hardness to reduce the edge roughness and burrs resulting from drilling.
Disclosure of Invention
In order to prepare a coating with higher surface hardness, the application provides a coating for a circuit board base plate and a preparation method thereof.
In a first aspect, the present application provides a coating for a circuit board backing plate, which adopts the following technical scheme:
a coating for a circuit board base plate is prepared by curing a coating; the coating is prepared from the following raw materials in parts by weight: 30-50 parts of epoxy resin, 6-10 parts of curing agent, 3-5 parts of cross-linking agent, 1-3 parts of additive, 40-60 parts of filler and 3-5 parts of toner.
By adopting the technical scheme, the epoxy resin, the curing agent and the cross-linking agent are matched, so that the epoxy resin forms a network structure with better cross-linking density, the structural density of the epoxy resin is improved, and the hardness of the cured epoxy resin is improved; meanwhile, the filler with higher content is matched, and the better filling effect of the filler in the cross-linked structure is utilized, so that the structural density of the coating is further improved, and the lubricating effect of the coating is improved, so that the prepared coating has higher surface hardness.
Preferably, the epoxy resin is selected from one or more of bisphenol A type epoxy resin, phenolic resin and multifunctional epoxy resin.
By adopting the technical scheme, the bisphenol A type epoxy resin, the phenolic resin and the multifunctional epoxy resin have longer molecular chains, and are easy to form a compact cross-linked network structure, so that the surface hardness of the coating is improved.
Preferably, the curing agent is one or more of imidazole curing agent, dicyandiamide, melamine and urea curing agent.
By adopting the technical scheme, the imidazole curing agent, dicyandiamide, melamine and urea curing agent can promote the crosslinking of the epoxy resin to form a compact network structure, so that the crosslinking density of the epoxy resin is improved, and the surface hardness of the coating is improved.
Preferably, the additive consists of a leveling agent, an anti-settling agent, a defoaming agent and a dispersing agent.
By adopting the technical scheme, the leveling agent enables the surface of the coating to be smooth, the anti-settling agent improves the uniformity of the coating, the defoaming agent can remove air bubbles in the coating, the density and the apparent effect of the coating are improved, and the dispersing agent promotes substances such as fillers and toner to be uniformly dispersed in the epoxy resin cross-linked structure, so that the fillers and the toner are conveniently filled, the cross-linked density of the epoxy resin structure is improved, and the surface hardness of the coating is improved.
Preferably, the filler consists of a powder filler and a modified filler in a weight ratio of 3-5: 1; the powder filler comprises a filler A with the particle size of 1-20 mu m, a filler B with the particle size of 0.1-0.5 mu m and a filler C with the particle size of 5-50nm, and the mass ratio of the filler A to the filler B to the filler C is 1:0.5-2: 1-2.
By adopting the technical scheme, the powder fillers with different particle sizes are conveniently and uniformly dispersed in the epoxy resin cross-linked network structure, and the fillers with small particle sizes are dispersed among the filler structures with larger particle sizes, so that the structural density of the epoxy resin is improved, and the surface hardness of the coating is improved.
Preferably, the filler A, the filler B and the filler C are selected from one or more of silica, silicon carbide, alumina and zirconia.
By adopting the technical scheme, the high hardness of silicon dioxide, silicon nitride, aluminum oxide and zirconium oxide is utilized to be filled in the epoxy resin structure, so that the coating has high density, and the surface hardness of the coating is improved.
Preferably, the modified filler consists of modified alumina nano fibers and modified alumina whiskers in a weight ratio of 1: 0.25-1;
the preparation method of the modified alumina nanofiber comprises the following steps:
soaking the alumina nano fiber in an ethylenediamine solution, wherein the weight ratio of the alumina nano fiber to the ethylenediamine solution is 1:1-2, and performing post-treatment to obtain the modified alumina nano fiber.
By adopting the technical scheme, the modified alumina nano fiber is matched with the modified alumina whisker, the long strip-shaped fiber structure is convenient to insert into the epoxy resin cross-linked structure, and the higher strength of the alumina nano fiber and the alumina whisker is utilized to further improve the density of the epoxy resin cross-linked structure, thereby improving the hardness of the coating.
The aluminum oxide nano fiber and the ethylenediamine solution are matched, the larger specific surface area of the aluminum oxide nano fiber is utilized, the amino group loaded on the surface of the aluminum oxide nano fiber is matched, the reaction of the amino group and the epoxy group is promoted, meanwhile, the aluminum oxide nano fiber is columnar, and more amino groups loaded on the surface are easy to contact and react with the epoxy group, so that the crosslinking density of the epoxy resin is improved, the three-dimensional network structure formed by the epoxy resin is tightly connected, the density of the cured epoxy resin structure is integrally improved, and the coating has higher hardness.
Preferably, the ethylenediamine solution is prepared by the following method:
weighing ethylenediamine, placing the ethylenediamine in water, stirring and dissolving to obtain a solution with the mass fraction of 5-12%; weighing the dissolving solution and 1% of sodium alginate solution according to the weight ratio of 8-12:1, and uniformly mixing and stirring to obtain the ethylenediamine solution.
By adopting the technical scheme, active hydrogen atoms in amine react with epoxy groups in epoxy resin to open the epoxy groups to generate hydroxyl groups, and the generated hydroxyl groups and the epoxy groups are subjected to etherification reaction to generate a network polymer; the ethylene diamine and the sodium alginate are matched, and the density of the epoxy resin network polymer is further improved by improving the amount of reactive hydroxyl groups, so that the coating has better structural density, and the surface hardness of the coating is improved.
Preferably, the preparation method of the modified alumina whisker comprises the following steps:
weighing and placing the alumina crystal whisker into a glutamine solution for soaking, wherein the weight ratio of the alumina crystal whisker to the glutamine solution is 1:1-1.5, and drying after soaking to prepare the modified alumina crystal whisker.
By adopting the technical scheme, the aluminum oxide whisker and the glutamine are matched, and the contact area between the modified aluminum oxide whisker and the epoxy resin and between the modified aluminum oxide whisker and the curing agent is improved by utilizing the needle-punched structure on the surface of the whisker, so that the glutamine on the surface of the modified aluminum oxide whisker is promoted to be contacted with the epoxy resin and the curing agent; the glutamine contains carbonyl and amino, the curing connection is realized by utilizing the action of the carbonyl and the amino in the curing agent, meanwhile, the amino in the glutamine acts with the epoxy resin to further promote the crosslinking of the epoxy resin, and the structural density of the epoxy resin is further improved through the curing connection and the chemical crosslinking so as to improve the structural density of the coating and further improve the surface hardness of the coating.
In a second aspect, the present application provides a method for preparing a coating for a circuit board backing plate, which adopts the following technical scheme: a preparation method of a coating for a circuit board base plate comprises the following steps:
s1, weighing epoxy resin and filler, and stirring and mixing uniformly to obtain a mixture;
s2, weighing the curing agent, the cross-linking agent, the toner, the admixture and the mixture, mixing and stirring uniformly, and performing vacuum defoaming to prepare the coating;
and S3, drying and curing the coating to form a coating.
By adopting the technical scheme, the epoxy resin and the filler are firstly mixed, so that the filler is preliminarily dispersed in the epoxy resin, then the curing agent and the cross-linking agent are added, the filler is promoted to be uniformly dispersed in an epoxy resin cross-linking structure in the curing and cross-linking process, a compact cross-linking network is formed, and the surface hardness of the coating is improved.
In summary, the present application has the following beneficial effects:
1. the epoxy resin, the curing agent, the cross-linking agent and the filler are matched, the filler is dispersed in a three-dimensional cross-linked network structure formed by the epoxy resin, the curing agent and the cross-linking agent by utilizing higher filler amount, the compactness of the coating structure is further improved by utilizing better filling effect, and the lubricating effect of the coating is improved, so that the prepared coating has higher surface hardness after being cured.
2. The powder fillers with different grain diameters are dispersed in the epoxy resin cross-linked network structure, and the fillers with small grain diameters are dispersed among the filler structures with larger grain diameters, so that the structural density of the powder fillers is improved, and the surface hardness of the coating is improved.
3. The epoxy resin, the modified alumina nano fiber and the modified alumina whisker are matched, the better heat insulation and high temperature resistance effects of the alumina nano fiber and the alumina whisker are utilized to endow the epoxy resin with better high temperature resistance, and the better heat resistance and strength of the epoxy resin are endowed by utilizing the high strength and high modulus of the alumina nano fiber and the alumina whisker, so that the finished coating has higher surface hardness and the melting and adhesion of a resin coating on a hole wall during drilling of a circuit board are avoided as much as possible.
4. The aluminum oxide nano fiber and the ethylenediamine are matched, the larger specific surface area of the aluminum oxide nano fiber is utilized, the amino group loaded on the surface of the aluminum oxide nano fiber is matched, the reaction of the amino group and the epoxy group is promoted, meanwhile, the aluminum oxide nano fiber is columnar, and more amino groups loaded on the surface are easy to contact and react with the epoxy group, so that the crosslinking density of the epoxy resin is improved, the three-dimensional network structure formed by the epoxy resin is tightly connected, the density of the cured epoxy resin structure is integrally improved, the epoxy resin has better heat resistance, and the resin coating is prevented from being fused and adhered on the hole wall when a circuit board is drilled while the finished coating has higher surface hardness.
5. The aluminum oxide whisker and the glutamine are matched, the contact area between the modified aluminum oxide whisker and the epoxy resin and between the modified aluminum oxide whisker and the curing agent is improved by utilizing a needle-punched structure on the surface of the whisker, the glutamine contains carbonyl and amino, the curing connection is realized by utilizing the action of the carbonyl and the amino in the curing agent, the amino in the glutamine acts on the epoxy resin to further promote the crosslinking of the epoxy resin, and the structural density of the epoxy resin is further improved by the curing connection and the chemical crosslinking, so that the epoxy resin has better heat resistance, the resin coating is prevented from being fused and adhered on a hole wall when a circuit board is drilled while the finished coating has higher surface hardness.
Detailed Description
The present application will be described in further detail with reference to examples.
Preparation example of ethylene diamine solution
The following raw materials are all commercially available.
Preparation example 1: the ethylenediamine solution is prepared by the following method:
weighing ethylenediamine, placing the ethylenediamine in water, stirring and dissolving to obtain a solution with the mass fraction of 10%; weighing the dissolving solution and a sodium alginate solution with the mass fraction of 1% according to the weight ratio of 10:1, mixing and stirring, and stirring uniformly to obtain the ethylenediamine solution.
Preparation example 2: the ethylenediamine solution is prepared by the following method:
weighing ethylenediamine, placing the ethylenediamine in water, stirring and dissolving to obtain a solution with the mass fraction of 5%; weighing the dissolving solution and a sodium alginate solution with the mass fraction of 1% according to the weight ratio of 8:1, mixing and stirring, and stirring uniformly to obtain the ethylenediamine solution.
Preparation example 3: the ethylenediamine solution is prepared by the following method:
weighing ethylenediamine, placing the ethylenediamine in water, stirring and dissolving to obtain a solution with the mass fraction of 12%; weighing the dissolving solution and a sodium alginate solution with the mass fraction of 1% according to the weight ratio of 12:1, mixing and stirring, and stirring uniformly to obtain the ethylenediamine solution.
Preparation example of modified alumina nanofiber
The alumina nano-fiber in the following raw materials is purchased from Jiangsu Xiancheng nano-material science and technology limited; other raw materials and equipment are all sold in the market.
Preparation example 4: the modified alumina nano fiber is prepared by the following method:
weighing 1kg of alumina nano fiber, soaking in 1.5kg of the ethylenediamine solution prepared in the preparation example 1, performing ultrasonic dispersion for 10min under the condition of 20kHz, drying, and grinding to obtain the modified alumina nano fiber, wherein the diameter of the modified alumina nano fiber is 4nm, and the length of the modified alumina nano fiber is 10 nm.
Preparation example 5: the modified alumina nano fiber is prepared by the following method:
weighing 1kg of alumina nanofiber, soaking in 1kg of the ethylenediamine solution prepared in the preparation example 2, performing ultrasonic dispersion for 10min under the condition of 20kHz, and then drying and grinding to obtain the modified alumina nanofiber, wherein the diameter of the modified alumina nanofiber is 4nm, and the length of the modified alumina nanofiber is 10 nm.
Preparation example 6: the modified alumina nano fiber is prepared by the following method:
weighing 1kg of alumina nanofiber, soaking in 2kg of the ethylenediamine solution prepared in preparation example 3, performing ultrasonic dispersion for 10min under the condition of 20kHz, and then drying and grinding to obtain the modified alumina nanofiber, wherein the diameter of the modified alumina nanofiber is 4nm, and the length of the modified alumina nanofiber is 10 nm.
Preparation example of modified alumina whisker the alumina whisker among the following raw materials was purchased from Qinhuang island-one high-new materials development Co., Ltd., diameter 1 μm, length 10 μm; glutamine was purchased from L-glutamine produced by Shanghai-derived leaf Biotech Co., Ltd; other raw materials and equipment are all sold in the market.
Preparation example 7: the modified alumina crystal whisker is prepared by the following method:
weighing aluminum oxide whiskers, placing the aluminum oxide whiskers in a glutamine solution with the mass fraction of 5%, soaking for 10min under the condition of ultrasonic oscillation, wherein the weight ratio of the aluminum oxide whiskers to the glutamine solution is 1:1.2, and drying after soaking to obtain the modified aluminum oxide whiskers.
Preparation example 8: the modified alumina crystal whisker is prepared by the following method:
weighing and placing the alumina whisker into a glutamine solution with the mass fraction of 5% for soaking for 10min under the condition of ultrasonic oscillation, wherein the weight ratio of the alumina whisker to the glutamine solution is 1:1, and drying after the soaking is finished to prepare the modified alumina whisker.
Preparation example 9: the modified alumina crystal whisker is prepared by the following method:
weighing the alumina crystal whisker, soaking the alumina crystal whisker in a glutamine solution with the mass fraction of 5% for 10min under the condition of ultrasonic oscillation, wherein the weight ratio of the alumina crystal whisker to the glutamine solution is 1:1.5, and drying after the soaking is finished to prepare the modified alumina crystal whisker.
Examples
Bisphenol A epoxy resin in the following raw materials was purchased from Nantong star synthetic materials, Inc. of China, under the designation WSR618 (E-51); carbodiimide was purchased from Jiangsu plerian Biotechnology, Inc.; polydimethylsiloxane was purchased from silicon harbor chemical ltd, denna; the acrylic acid antifoaming agent is purchased from Qianzhi chemical Co., Ltd, brand XUHUAC, model AKN-3352; the BYK-110 dispersant is purchased from Qianzyou chemical Co Ltd of Foshan city; the modified hydrogenated castor oil is purchased from Kay chemical company of Shanghai, model number THIXATROL ST; organosilicon is purchased from Tianjin Yunfan Hui technology Co., Ltd; the multifunctional epoxy resin is purchased from Jiangsu New Material Co., Ltd; other raw materials and equipment are all sold in the market.
Example 1: a coating for a circuit board backing plate:
40kg of epoxy resin, 7.5kg of curing agent, 4kg of cross-linking agent, 2kg of additive, 50kg of filler and 4kg of toner; the epoxy resin is bisphenol A type epoxy resin; the curing agent is dicyandiamide; the cross-linking agent is carbodiimide; the additive consists of 0.6kg of flatting agent, 0.4kg of anti-settling agent, 0.2kg of defoaming agent and 0.8kg of dispersing agent, wherein the flatting agent is polydimethylsiloxane, the anti-settling agent is polyethylene wax, the defoaming agent is acrylic defoaming agent, and the dispersing agent is BYK-110 dispersing agent;
the filler consists of 40kg of powder filler and 10kg of modified filler, the powder filler consists of 10kg of filler A, 10kg of filler B and 20kg of filler C, the particle size of the filler A is 10 micrometers, the particle size of the filler B is 0.2 micrometers, the particle size of the filler C is 10nm, and the filler A, the filler B and the filler C are all alumina; the modified filler consisted of 6.25kg of the modified alumina nanofibers prepared in preparative example 4 and 3.75kg of the modified alumina whiskers prepared in preparative example 7;
the preparation method comprises the following steps:
s1, weighing epoxy resin and a filler, stirring and mixing, uniformly stirring at a rotating speed of 300r/min, pre-reacting for 5min at 85 ℃, and then recovering to 40 ℃ to obtain a mixture;
s2, weighing the curing agent, the cross-linking agent, the toner and the admixture, putting the curing agent, the cross-linking agent, the toner and the admixture into the mixture, continuously stirring at the rotating speed of 300r/min in the adding process, uniformly stirring, and performing vacuum defoaming to prepare the coating;
and S3, drying and curing the coating to form a coating.
Example 2: the present embodiment is different from embodiment 1 in that:
30kg of epoxy resin, 6kg of curing agent, 3kg of cross-linking agent, 1kg of additive, 40kg of filler and 3kg of toner; the epoxy resin is phenolic resin; the curing agent is imidazole curing agent, and the imidazole curing agent is 2, 4-dimethylimidazole; the cross-linking agent is organic phosphorus; the additive consists of 0.5kg of flatting agent, 0.5kg of anti-settling agent, 0.4kg of defoaming agent and 0.6kg of dispersing agent, wherein the flatting agent is polydimethylsiloxane, the anti-settling agent is modified hydrogenated castor oil, the defoaming agent is an organic silicon defoaming agent, and the dispersing agent is BYK-110 dispersing agent;
the filler consists of 30kg of powder filler and 10kg of modified filler, the powder filler consists of 12kg of filler A, 6kg of filler B and 12kg of filler C, the particle size of the filler A is 1 mu m, the particle size of the filler B is 0.1 mu m, the particle size of the filler C is 5nm, and the filler A, the filler B and the filler C are all silicon carbide; the modified filler consisted of 8kg of the modified alumina nanofibers prepared in preparation example 5 and 2kg of the modified alumina whiskers prepared in preparation example 8.
Example 3: the present embodiment is different from embodiment 1 in that:
50kg of epoxy resin, 10kg of curing agent, 5kg of cross-linking agent, 3kg of additive, 60kg of filler and 5kg of toner; the epoxy resin is multifunctional epoxy resin; the curing agent is urea curing agent, and the urea curing agent is dicyandiamide urea accelerator with the model number UR 300; the cross-linking agent is organic phosphorus; the additive consists of 0.8kg of flatting agent, 0.5kg of anti-settling agent, 0.2kg of defoaming agent and 0.5kg of dispersing agent, wherein the flatting agent is polydimethylsiloxane, the anti-settling agent is modified hydrogenated castor oil, the defoaming agent is an organic silicon defoaming agent, and the dispersing agent is BYK-110 dispersing agent;
the filler consists of 50kg of powder filler and 10kg of modified filler, the powder filler consists of 10kg of filler A, 20kg of filler B and 20kg of filler C, the particle size of the filler A is 20 micrometers, the particle size of the filler B is 0.5 micrometer, the particle size of the filler C is 50nm, and the filler A, the filler B and the filler C are all zirconia; the modified filler consisted of 5kg of the modified alumina nanofibers prepared in preparation example 6 and 5kg of the modified alumina whiskers prepared in preparation example 9.
Example 4: the present embodiment is different from embodiment 1 in that:
the filler is a powder filler.
Example 5: the present embodiment is different from embodiment 1 in that:
the particle size of the powder filler was 10 μm.
Example 6: the present embodiment is different from embodiment 1 in that:
the particle size of the powder filler was 0.2. mu.m.
Example 7: the present embodiment is different from embodiment 1 in that:
the modified alumina nano fiber with the same mass is used for replacing the modified alumina whisker in the modified filler raw material.
Example 8: the present embodiment is different from embodiment 1 in that:
the preparation process of the modified alumina nanofiber comprises the following steps: weighing 1kg of alumina nano fiber, washing with water, and drying to obtain the modified alumina nano fiber.
Example 9: the present embodiment is different from embodiment 1 in that:
the preparation process of the ethylene diamine solution comprises the following steps: weighing ethylenediamine, placing the ethylenediamine in water, stirring and dissolving to obtain an ethylenediamine solution with the mass fraction of 10%.
Example 10: the present embodiment is different from embodiment 1 in that:
the modified alumina whisker is prepared by the following steps: weighing the alumina crystal whisker, washing with water, and drying to obtain the modified alumina crystal whisker.
Example 11: the present embodiment is different from embodiment 1 in that:
the modified alumina whisker is prepared by the following steps: weighing aluminum oxide whiskers, placing the aluminum oxide whiskers in an ethylenediamine solution with the mass fraction of 5%, soaking for 10min under the condition of ultrasonic oscillation, wherein the weight ratio of the aluminum oxide whiskers to the ethylenediamine solution is 1:1.2, and drying after soaking to obtain the modified aluminum oxide whiskers.
Example 12: the present embodiment is different from embodiment 1 in that:
the modified filler is composed of 6.25kg of alumina nano-fiber and 3.75kg of alumina whisker.
Example 13: the present embodiment is different from embodiment 1 in that:
in the preparation process of the coating:
s1, weighing the epoxy resin and the filler, stirring, mixing and stirring uniformly to obtain a mixture.
Comparative example
Comparative example 1: this comparative example differs from example 1 in that:
the cross-linking agent is replaced by the curing agent with the same mass in the raw materials.
Comparative example 2: this comparative example differs from example 1 in that:
the amount of filler in the raw materials was 20 kg.
Comparative example 3: this comparative example differs from example 1 in that:
the coating is prepared by the following steps:
s1, weighing epoxy resin, filler, curing agent, cross-linking agent, toner and additive, mixing and stirring uniformly, and then defoaming in vacuum to obtain the coating.
Performance test
1. Hardness Performance test
The finished coatings were prepared by the methods of examples 1 to 13 and comparative examples 1 to 3, respectively, and the dimensions were 50 × 50 × 5mm, and the data were recorded using a shore D rubber durometer pressed vertically, with the data of the position of the durometer pointer being the hardness of the object to be measured.
2. Detection of heat resistance
Respectively adopting the preparation methods of examples 1-3, 7-10 and 12-13 to prepare finished coatings, treating the coatings at 200 ℃ for 16h by referring to the measuring steps of GB/T1735-2009 paint and varnish heat resistance, and then detecting the impact resistance of the coatings according to GB/T1732-1993 paint film impact resistance measuring method; and the impact resistance of the coating was measured using the same impact resistance measuring method as described above for the non-heat-treated paint film, and the data was recorded.
TABLE 1 Performance test Table
By combining the example 1 and the examples 2-3 and combining the table 1, the finished coating prepared by the method has higher hardness, and the impact resistance of the coating after heat treatment is good, which indicates that the coating has better heat resistance; the epoxy resin, the curing agent, the cross-linking agent and the filler with higher content are matched, the better filling effect of the filler in a cross-linked structure is utilized, the density of the coating structure is improved, and the lubricating effect of the coating is improved, so that the prepared coating has higher surface hardness and better heat resistance, and the roughness and burrs of the hole edge formed by drilling can be reduced.
By combining the example 1 and the examples 4 to 13 and combining the table 1, it can be seen that the filler in the example 4 is a powder filler, the particle size of the powder filler in the example 5 is 10 μm, and the particle size of the powder filler in the example 6 is 0.2 μm, and compared with the example 1, the shore hardness of the examples 4, 5 and 6 is smaller than that of the example 1, which indicates that the coating prepared by using the fillers with different particle sizes enables the powder fillers with different particle sizes to be uniformly dispersed in the epoxy resin cross-linked network structure, and the fillers with small particle sizes are dispersed among the filler structures with larger particle sizes, so that the structure of the powder filler is improved, and the surface hardness of the coating is improved; however, the packing of a single size is not sufficient to achieve a denser packing effect, and thus the hardness of the finished coating is easily affected.
Example 7, in the modified filler raw material, the modified alumina nano-fiber with the same mass is used for replacing the modified alumina whisker, compared with example 1, the shore hardness of example 7 is lower than that of example 1, and the impact resistance after being heated is inferior to that of example 1, so the heat resistance is inferior to that of example 1; the matching of the modified alumina nano fiber and the modified alumina whisker is illustrated, and the structural density of the coating is improved by improving the structural crosslinking density of the epoxy resin, so that the coating has higher surface hardness and heat resistance.
Example 8 modified alumina nanofibers during the preparation: weighing 1kg of alumina nanofiber, washing with water, and drying to obtain a modified alumina nanofiber, wherein in comparison with example 1, the Shore hardness of example 8 is lower than that of example 1, and the impact resistance after heating is inferior to that of example 1, so that the heat resistance is inferior to that of example 1; the matching of the alumina nanofibers and the ethylenediamine is illustrated, the larger specific surface area of the alumina nanofibers is utilized, the amine groups loaded on the surfaces of the alumina nanofibers are matched, the reaction of the amine groups and the epoxy groups is promoted, meanwhile, the alumina nanofibers are columnar, and more amine groups loaded on the surfaces are easy to contact and react with the epoxy groups, so that the crosslinking density of the epoxy resin is improved, the three-dimensional network structure formed by the epoxy resin is tightly connected, the density of the cured epoxy resin structure is integrally improved, the epoxy resin has better hardness and heat resistance, the resin coating is prevented from being fused and adhered to hole walls when a circuit board is drilled while the finished coating has higher surface hardness.
Example 9 ethylene diamine solution during the preparation: weighing ethylenediamine, placing the ethylenediamine in water, stirring and dissolving to obtain an ethylenediamine solution with the mass fraction of 10%, wherein compared with example 1, the Shore hardness of example 9 is lower than that of example 1, and the impact resistance after heating is inferior to that of example 1, so that the heat resistance is inferior to that of example 1; the matching of the ethylenediamine and the sodium alginate is shown, and the density of the epoxy resin network polymer is further improved by improving the amount of the reactive hydroxyl groups, so that the coating has better structural density, and the surface hardness and the heat resistance of the coating are improved.
Example 10 modified alumina whiskers during the preparation: weighing the alumina whisker, washing with water, and drying to obtain a modified alumina whisker, wherein compared with example 1, the Shore hardness of example 10 is lower than that of example 1, and the impact resistance after heating is inferior to that of example 1, and the heat resistance is inferior to that of example 1; the matching of the aluminum oxide whisker and glutamine is illustrated, the contact area between the modified aluminum oxide whisker and the epoxy resin and between the modified aluminum oxide whisker and the curing agent is improved by utilizing the needle-punched structure on the surface of the whisker, the glutamine contains carbonyl and amino, the curing connection is realized by utilizing the action of the carbonyl and the amino in the curing agent, and the amino in the glutamine acts on the epoxy resin to further promote the crosslinking of the epoxy resin.
Example 11 the alumina whiskers were treated with an ethylene diamine solution and compared to example 1, example 11 had a lower shore hardness than example 1; the matching of the aluminum oxide whisker and the glutamine is proved to improve the structural density by connecting the epoxy resin and the curing agent, and the ethylene diamine has no carbonyl group, so that the crosslinking density of the finished coating is easily influenced, and the hardness of the coating is influenced.
Example 12 the modified filler consisted of 6.25kg of alumina nanofibers and 3.75kg of alumina whiskers, and compared to example 1, example 12 had a shore hardness less than that of example 1, and had inferior impact resistance after heating to example 1, and then inferior heat resistance to example 1; the results show that the alumina nano-fiber and the alumina whisker which are not subjected to modification treatment only play a filling role in the epoxy resin coating, have small influence on the crosslinking effect of the epoxy resin, and influence the structural density of the coating, so that the hardness and the heat resistance of the finished coating are influenced.
In the preparation process of the coating in the embodiment 13, the epoxy resin and the filler are directly mixed and stirred to prepare a mixed material, compared with the embodiment 1, the Shore hardness of the embodiment 13 is lower than that of the embodiment 1, the impact resistance after being heated is inferior to that of the embodiment 1, and the heat resistance is inferior to that of the embodiment 1; the density of the cross-linked structure of the coating which is directly mixed and not prepared by the preheating treatment is different from that of the coating which is subjected to the preheating treatment, so that the hardness and the heat resistance of the coating are influenced.
Combining example 1 and comparative examples 1-3 and table 1, it can be seen that the shore hardness of comparative example 1 is less than that of example 1 compared to example 1 when the cross-linking agent is replaced by the same mass of curing agent in the raw material of comparative example 1; the matching of the cross-linking agent and the curing agent can promote the epoxy resin to form a compact cross-linking structure, thereby improving the hardness of the coating.
The addition amount of the filler in the raw material of the comparative example 2 is 20kg, and compared with the example 1, the Shore hardness of the comparative example 2 is lower than that of the example 1; illustrating that smaller filler additions affect the hardness of the finished coating.
Comparative example 3 in the preparation process of the coating, all the raw materials are mixed and stirred at one time to prepare the coating, and compared with example 1, the Shore hardness of comparative example 3 is smaller than that of example 1; it is shown that the one-time mixing easily affects the mixing uniformity of the epoxy resin and the filler, and thus the surface hardness of the coating.
The present embodiment is only for explaining the present application, and it is not limited to the present application, and those skilled in the art can make modifications of the present embodiment without inventive contribution as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present application.
Claims (10)
1. The coating for the circuit board base plate is characterized in that the coating is prepared by curing a coating; the coating is prepared from the following raw materials in parts by weight: 30-50 parts of epoxy resin, 6-10 parts of curing agent, 3-5 parts of cross-linking agent, 1-3 parts of additive, 40-60 parts of filler and 3-5 parts of toner.
2. The coating for a circuit board pad according to claim 1, wherein: the epoxy resin is selected from one or more of bisphenol A type epoxy resin, phenolic resin and multifunctional epoxy resin.
3. The coating for a circuit board pad according to claim 1, wherein: the curing agent is one or more of imidazole curing agent, dicyandiamide, melamine and urea curing agent.
4. The coating for a circuit board pad according to claim 1, wherein: the additive is composed of a leveling agent, an anti-settling agent, a defoaming agent and a dispersing agent.
5. The coating for a circuit board pad according to claim 1, wherein: the filler consists of powder filler and modified filler in a weight ratio of 3-5: 1; the powder filler comprises a filler A with the particle size of 1-20 mu m, a filler B with the particle size of 0.1-0.5 mu m and a filler C with the particle size of 5-50nm, and the mass ratio of the filler A to the filler B to the filler C is 1:0.5-2: 1-2.
6. The coating for a circuit board pad according to claim 5, wherein: the filler A, the filler B and the filler C are selected from one or more of silicon dioxide, silicon carbide, aluminum oxide and zirconium oxide.
7. The coating for a circuit board pad according to claim 5, wherein: the modified filler consists of modified alumina nano fibers and modified alumina whiskers in a weight ratio of 1: 0.25-1;
the preparation method of the modified alumina nanofiber comprises the following steps:
soaking the alumina nano fiber in an ethylenediamine solution, wherein the weight ratio of the alumina nano fiber to the ethylenediamine solution is 1:1-2, and performing post-treatment to obtain the modified alumina nano fiber.
8. The coating for a circuit board pad according to claim 7, wherein: the ethylenediamine solution is prepared by the following method:
weighing ethylenediamine, placing the ethylenediamine in water, stirring and dissolving to obtain a solution with the mass fraction of 5-12%; weighing the dissolving solution and 1% of sodium alginate solution according to the weight ratio of 8-12:1, and uniformly mixing and stirring to obtain the ethylenediamine solution.
9. The coating for a circuit board pad according to claim 7, wherein: the preparation method of the modified alumina whisker comprises the following steps:
weighing and placing the alumina crystal whisker into a glutamine solution for soaking, wherein the weight ratio of the alumina crystal whisker to the glutamine solution is 1:1-1.5, and drying after soaking to prepare the modified alumina crystal whisker.
10. A method for producing a coating layer for a circuit board underlay as recited in any one of claims 1 to 9, characterized by comprising the steps of:
s1, weighing epoxy resin and filler, and stirring and mixing uniformly to obtain a mixture;
s2, weighing the curing agent, the cross-linking agent, the toner, the admixture and the mixture, mixing and stirring uniformly, and performing vacuum defoaming to prepare the coating;
and S3, drying and curing the coating to form a coating.
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