CN117186588A - High heat-resistant resin composition for electronic circuit substrate and preparation method thereof - Google Patents
High heat-resistant resin composition for electronic circuit substrate and preparation method thereof Download PDFInfo
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- CN117186588A CN117186588A CN202311202282.9A CN202311202282A CN117186588A CN 117186588 A CN117186588 A CN 117186588A CN 202311202282 A CN202311202282 A CN 202311202282A CN 117186588 A CN117186588 A CN 117186588A
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- 239000011342 resin composition Substances 0.000 title claims abstract description 76
- 229920006015 heat resistant resin Polymers 0.000 title claims abstract description 47
- 239000000758 substrate Substances 0.000 title claims abstract description 37
- 238000002360 preparation method Methods 0.000 title claims description 41
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 claims abstract description 51
- 239000003063 flame retardant Substances 0.000 claims abstract description 51
- 239000003292 glue Substances 0.000 claims abstract description 36
- 229920005989 resin Polymers 0.000 claims abstract description 32
- 239000011347 resin Substances 0.000 claims abstract description 32
- 238000007654 immersion Methods 0.000 claims abstract description 27
- 239000011159 matrix material Substances 0.000 claims abstract description 18
- 239000000463 material Substances 0.000 claims abstract description 16
- 238000000748 compression moulding Methods 0.000 claims abstract description 10
- 239000000243 solution Substances 0.000 claims description 141
- 239000003795 chemical substances by application Substances 0.000 claims description 137
- 239000003365 glass fiber Substances 0.000 claims description 65
- 239000000440 bentonite Substances 0.000 claims description 58
- 229910000278 bentonite Inorganic materials 0.000 claims description 58
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 claims description 58
- 229910052582 BN Inorganic materials 0.000 claims description 56
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims description 56
- 238000003756 stirring Methods 0.000 claims description 46
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 39
- 238000001035 drying Methods 0.000 claims description 37
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 37
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 36
- 229910052588 hydroxylapatite Inorganic materials 0.000 claims description 34
- XYJRXVWERLGGKC-UHFFFAOYSA-D pentacalcium;hydroxide;triphosphate Chemical compound [OH-].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O XYJRXVWERLGGKC-UHFFFAOYSA-D 0.000 claims description 34
- 238000000498 ball milling Methods 0.000 claims description 30
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 26
- 239000003607 modifier Substances 0.000 claims description 25
- 238000005406 washing Methods 0.000 claims description 25
- 239000003822 epoxy resin Substances 0.000 claims description 22
- 229920000647 polyepoxide Polymers 0.000 claims description 22
- 238000002156 mixing Methods 0.000 claims description 21
- VQEHIYWBGOJJDM-UHFFFAOYSA-H lanthanum(3+);trisulfate Chemical compound [La+3].[La+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O VQEHIYWBGOJJDM-UHFFFAOYSA-H 0.000 claims description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 19
- NGDQQLAVJWUYSF-UHFFFAOYSA-N 4-methyl-2-phenyl-1,3-thiazole-5-sulfonyl chloride Chemical compound S1C(S(Cl)(=O)=O)=C(C)N=C1C1=CC=CC=C1 NGDQQLAVJWUYSF-UHFFFAOYSA-N 0.000 claims description 15
- 229920001661 Chitosan Polymers 0.000 claims description 15
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 15
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 14
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 14
- 238000001816 cooling Methods 0.000 claims description 13
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 13
- 239000001509 sodium citrate Substances 0.000 claims description 13
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 claims description 13
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 13
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 13
- 238000001354 calcination Methods 0.000 claims description 12
- 238000003825 pressing Methods 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 11
- 239000002994 raw material Substances 0.000 claims description 11
- YDEXUEFDPVHGHE-GGMCWBHBSA-L disodium;(2r)-3-(2-hydroxy-3-methoxyphenyl)-2-[2-methoxy-4-(3-sulfonatopropyl)phenoxy]propane-1-sulfonate Chemical compound [Na+].[Na+].COC1=CC=CC(C[C@H](CS([O-])(=O)=O)OC=2C(=CC(CCCS([O-])(=O)=O)=CC=2)OC)=C1O YDEXUEFDPVHGHE-GGMCWBHBSA-L 0.000 claims description 9
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims description 9
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 7
- DPXJVFZANSGRMM-UHFFFAOYSA-N acetic acid;2,3,4,5,6-pentahydroxyhexanal;sodium Chemical compound [Na].CC(O)=O.OCC(O)C(O)C(O)C(O)C=O DPXJVFZANSGRMM-UHFFFAOYSA-N 0.000 claims description 7
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 7
- 239000007853 buffer solution Substances 0.000 claims description 7
- 239000001768 carboxy methyl cellulose Substances 0.000 claims description 7
- 239000012286 potassium permanganate Substances 0.000 claims description 7
- 235000019812 sodium carboxymethyl cellulose Nutrition 0.000 claims description 7
- 229920001027 sodium carboxymethylcellulose Polymers 0.000 claims description 7
- 239000002904 solvent Substances 0.000 claims description 7
- 229920000877 Melamine resin Polymers 0.000 claims description 6
- 239000000805 composite resin Substances 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 claims description 6
- 239000000347 magnesium hydroxide Substances 0.000 claims description 6
- 229910001862 magnesium hydroxide Inorganic materials 0.000 claims description 6
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical group O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 claims description 6
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims description 6
- 238000000465 moulding Methods 0.000 claims description 6
- 238000009210 therapy by ultrasound Methods 0.000 claims description 6
- 239000012856 weighed raw material Substances 0.000 claims description 6
- 238000005303 weighing Methods 0.000 claims description 5
- 238000002386 leaching Methods 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 230000000052 comparative effect Effects 0.000 description 17
- 230000003138 coordinated effect Effects 0.000 description 8
- 230000000694 effects Effects 0.000 description 8
- 238000000034 method Methods 0.000 description 5
- 239000000853 adhesive Substances 0.000 description 4
- 230000001070 adhesive effect Effects 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 2
- 241000276425 Xiphophorus maculatus Species 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
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- 230000010365 information processing Effects 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000008054 signal transmission Effects 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
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Abstract
The invention relates to the technical field of high heat-resistant resin compositions, and particularly discloses a high heat-resistant resin composition for an electronic circuit substrate, which is characterized by comprising a resin substrate plate; wherein the resin matrix board is prepared by adopting an improved resin composition material through compression molding, and the resin matrix board is immersed into the flame-retardant glue solution for immersion treatment, so as to form the high heat-resistant resin composition. The high heat-resistant resin composition is formed by adopting the resin matrix board prepared by compression molding of the improved resin composition material and then immersing the resin matrix board in the flame-retardant glue solution for immersion treatment, and the prepared product has excellent flame retardance and elongation at break performance, and meanwhile, the heat-resistant stability of the product is excellent, and the performance of the product can be improved in a coordinated manner.
Description
Technical Field
The invention relates to the technical field of electronic circuit resin, in particular to a high heat-resistant resin composition for an electronic circuit substrate and a preparation method thereof.
Background
With the revolution of modern information technology, digital circuits gradually step into the stages of information processing and high speed and signal transmission and high frequency, and on the basis of meeting the requirements of traditional design and manufacture, higher requirements are put on the performance of electronic circuit substrate materials.
In the prior art, most of resin compositions adopted by electronic circuit substrates are epoxy resin compositions, so that the elongation at break and poor flame retardance of products are easily caused for optimizing the heat resistance of epoxy resin composition products, and therefore, the coordinated improvement of the elongation at break, the flame retardance and the heat resistance of the products is difficult to realize, and the use efficiency of the products is limited.
Disclosure of Invention
In view of the drawbacks of the prior art, an object of the present invention is to provide a highly heat-resistant resin composition for electronic circuit substrates and a method for preparing the same, which solve the problems set forth in the background art.
The invention solves the technical problems by adopting the following technical scheme:
the present invention provides a highly heat-resistant resin composition for an electronic circuit substrate, the highly heat-resistant resin composition comprising a resin base plate; wherein the resin matrix board is prepared by adopting an improved resin composition material through compression molding, and is immersed in the flame-retardant glue solution for immersion treatment to form a high heat-resistant resin composition;
the improved resin composition comprises the following raw materials in parts by weight:
80-120 parts of epoxy resin, 3-6 parts of lanthanum sulfate solution, 6-10 parts of bentonite-doped glass fiber agent, 100-110 parts of curing agent, 3-5 parts of sodium dodecyl benzene sulfonate and 4-8 parts of hydroxyapatite modifier;
the preparation method of the hydroxyapatite modifier comprises the following steps:
adding hydroxyapatite into sodium hydroxide solution according to the weight ratio of 1:5, performing ultrasonic dispersion treatment, performing ultrasonic treatment, washing with water, drying, calcining at 310-320 ℃ for 10-20 min, performing calcination, and naturally cooling at room temperature;
the preparation method of the flame-retardant glue solution comprises the following steps:
weighing 5-10 parts of silicon carbide whisker blended boron nitride agent, 3-6 parts of flame retardant, 10-15 parts of epoxy resin glue, 20-25 parts of acetone solvent and 2-5 parts of silane coupling agent KH560; and (5) uniformly stirring and mixing the weighed raw materials to obtain the flame-retardant glue solution.
Preferably, the curing agent is maleic anhydride; the flame retardant is prepared by mixing melamine and magnesium hydroxide according to the weight ratio of 1:2.
Preferably, the mass fraction of the lanthanum sulfate solution is 4-8%; the mass fraction of the sodium hydroxide solution is 6-8%; ultrasonic dispersion treatment is carried out for 1-2 hours, and ultrasonic power is 450-550W.
Preferably, the preparation method of the bentonite-doped glass fiber agent comprises the following steps:
s01: heat-treating bentonite at 220-230 deg.c for 10-15 min, heating to 350-370 deg.c at 2-5 deg.c/min, maintaining for 5-10 min, and cooling to room temperature at 1-3 deg.c/min to obtain heat treated bentonite;
s02: uniformly stirring 8-12 parts of heat-treated bentonite, 2-5 parts of sodium carboxymethyl cellulose, 1-3 parts of chitosan solution, 15-20 parts of sodium citrate solution and 1-2 parts of silica sol to obtain a doped bentonite agent;
s03: 5-10 parts of glass fiber is sent into 10-15 parts of sulfuric acid solution to be stirred uniformly, then washed and dried, and then immersed into yttrium nitrate solution, the immersing treatment is carried out, the immersing pressure is 10-15 MPa, the immersing is carried out for 1-2 h, and then the glass fiber agent is obtained after the immersing is finished, and then the leaching and drying are carried out;
s04: and (5) feeding the glass fiber agent and the doped bentonite agent into a ball mill according to the weight ratio (5-7) 1, ball milling, washing with water and drying after ball milling is finished, so as to obtain the glass fiber agent doped with bentonite.
Preferably, the mass fraction of the sodium citrate solution is 10-15%; the mass fraction of the chitosan solution is 4-8%; the mass fraction of the yttrium nitrate solution is 2-5%; the mass fraction of the sulfuric acid solution is 8-12%.
Preferably, the ball milling rotating speed of the ball milling treatment is 1000-1500 r/min, and the ball milling time is 1-2 h.
Preferably, the preparation method of the silicon carbide whisker blended boron nitride agent comprises the following steps:
s101: feeding the flaky boron nitride into a potassium permanganate solution with the total amount of 4-5 times of the flaky boron nitride, stirring and dispersing uniformly, and then washing and drying to obtain a pretreated flaky boron nitride agent;
s102: adding 4-6 parts of silicon carbide whisker and 6-10 parts of pretreated flaky boron nitride agent into 10-15 parts of deionized water, then adding 2-3 parts of phosphoric acid buffer solution with the pH value of 5.0, 1-2 parts of sodium lignin sulfonate and 0.55-0.75 part of sodium dodecyl sulfate solution, stirring and reacting for 1-2 hours at the temperature of 45-50 ℃, stirring at the speed of 550-650 r/min, washing with water and drying to obtain the silicon carbide whisker blended boron nitride agent.
Preferably, the mass fraction of the sodium dodecyl sulfate solution is 8-12%.
The invention also provides a preparation method of the high heat-resistant resin composition for the electronic circuit substrate, which comprises the following steps:
uniformly stirring and mixing epoxy resin, 5% by mass of lanthanum sulfate solution, bentonite-doped glass fiber agent, sodium dodecyl benzene sulfonate and hydroxyapatite modifier, adding a curing agent into the uniformly mixed product, and fully stirring to obtain an improved resin composite material;
injecting the improved resin composition into a pressing mold, and performing pressing molding to obtain a resin matrix board; and immersing the resin substrate plate into the flame-retardant glue solution for immersing treatment, and then taking out and drying to form the high heat-resistant resin composition.
Preferably, the immersion pressure of the immersion treatment is 10-15 MPa, and the immersion time is 20-30 min.
Compared with the prior art, the invention has the following beneficial effects:
1. the high heat-resistant resin composition is formed by adopting the resin matrix board prepared by compression molding of the improved resin composition material and then immersing the resin matrix board in the flame-retardant glue solution for immersion treatment, and the prepared product has excellent flame retardance and elongation at break performance, and meanwhile, the heat-resistant stability of the product is excellent, and the performance of the product can be improved in a coordinated manner;
2. the improved resin composition adopts epoxy resin, lanthanum sulfate solution and sodium dodecyl benzene sulfonate to prepare and match with bentonite-doped glass fiber agent and hydroxyapatite modifier, and then is subjected to curing injection compression molding by a curing agent, and excellent heat resistance and elongation at break performance are provided for the substrate body by the coordinated and synergistic effect of the bentonite-doped glass fiber agent and the hydroxyapatite modifier;
3. the silicon carbide whisker blended boron nitride agent, the flame retardant, the epoxy resin adhesive, the acetone solvent and the silane coupling agent KH560 are matched to form a flame-retardant adhesive solution, the flame-retardant adhesive solution is immersed in the improved substrate, the obtained product has excellent flame-retardant performance, the silicon carbide whisker blended boron nitride agent adopts flaky boron nitride to be treated by potassium permanganate solution, the activity of the silicon carbide whisker blended boron nitride agent is optimized, and then the silicon carbide whisker, phosphoric acid buffer solution, sodium lignin sulfonate and sodium dodecyl sulfate solution are mutually blended to coordinate flaky boron nitride together, so that the flame retardant can be better distributed into the adhesive solution base solution, stable flame-retardant environment can be provided for the product, and the flame-retardant efficiency is improved;
4. the glass fiber agent doped with bentonite is prepared by adopting bentonite to perform heat treatment for 10-15 min at 220-230 ℃, then heating to 350-370 ℃ at the rate of 2-5 ℃/min, preserving heat for 5-10 min, finally cooling to room temperature at the rate of 1-3 ℃/min, optimizing the layer-by-layer spacing of bentonite sheets, facilitating distribution in a substrate system, and better improving the heat-resistant stability of the system, while the heat-treated bentonite, sodium carboxymethyl cellulose, chitosan solution, sodium citrate solution and silica sol are matched to obtain the doped bentonite agent which can be ball-milled to improve the glass fiber agent, so that the prepared glass fiber agent doped with bentonite has better elongation at break performance and heat-resistant stability of the system;
5. the glass fiber agent is treated by sulfuric acid solution, and then is immersed and improved by yttrium nitrate, the improved glass fiber agent better coordinates and coordinates with the doped bentonite agent, the performance effect of the system is improved, meanwhile, the hydroxyapatite is subjected to ultrasonic dispersion treatment by sodium hydroxide solution, and is calcined for 10-20 min at 310-320 ℃, the activity and the dispersity of the hydroxyapatite are optimized, so that the coordination effect of the hydroxyapatite modifier and the glass fiber agent doped with bentonite is further improved, the coordination of heat resistance and elongation at break of the system is improved, the flame retardant performance of the product is excellent, and the performance of the product can realize coordinated integral improvement.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and fully with reference to the accompanying drawings, in which it is evident that the embodiments described are only some, but not all embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
A highly heat-resistant resin composition for an electronic circuit substrate of the present embodiment, the highly heat-resistant resin composition comprising a resin base plate; wherein the resin matrix board is prepared by adopting an improved resin composition material through compression molding, and is immersed in the flame-retardant glue solution for immersion treatment to form a high heat-resistant resin composition;
the improved resin composition comprises the following raw materials in parts by weight:
80-120 parts of epoxy resin, 3-6 parts of lanthanum sulfate solution, 6-10 parts of bentonite-doped glass fiber agent, 100-110 parts of curing agent, 3-5 parts of sodium dodecyl benzene sulfonate and 4-8 parts of hydroxyapatite modifier;
the preparation method of the hydroxyapatite modifier comprises the following steps:
adding hydroxyapatite into sodium hydroxide solution according to the weight ratio of 1:5, performing ultrasonic dispersion treatment, performing ultrasonic treatment, washing with water, drying, calcining at 310-320 ℃ for 10-20 min, performing calcination, and naturally cooling at room temperature;
the preparation method of the flame-retardant glue solution comprises the following steps:
weighing 5-10 parts of silicon carbide whisker blended boron nitride agent, 3-6 parts of flame retardant, 10-15 parts of epoxy resin glue, 20-25 parts of acetone solvent and 2-5 parts of silane coupling agent KH560; and (5) uniformly stirring and mixing the weighed raw materials to obtain the flame-retardant glue solution.
The curing agent of the embodiment is maleic anhydride; the flame retardant is prepared by mixing melamine and magnesium hydroxide according to the weight ratio of 1:2.
Preferably, the mass fraction of the lanthanum sulfate solution is 4-8%; the mass fraction of the sodium hydroxide solution is 6-8%; ultrasonic dispersion treatment is carried out for 1-2 hours, and ultrasonic power is 450-550W.
The preparation method of the bentonite-doped glass fiber agent comprises the following steps:
s01: heat-treating bentonite at 220-230 deg.c for 10-15 min, heating to 350-370 deg.c at 2-5 deg.c/min, maintaining for 5-10 min, and cooling to room temperature at 1-3 deg.c/min to obtain heat treated bentonite;
s02: uniformly stirring 8-12 parts of heat-treated bentonite, 2-5 parts of sodium carboxymethyl cellulose, 1-3 parts of chitosan solution, 15-20 parts of sodium citrate solution and 1-2 parts of silica sol to obtain a doped bentonite agent;
s03: 5-10 parts of glass fiber is sent into 10-15 parts of sulfuric acid solution to be stirred uniformly, then washed and dried, and then immersed into yttrium nitrate solution, the immersing treatment is carried out, the immersing pressure is 10-15 MPa, the immersing is carried out for 1-2 h, and then the glass fiber agent is obtained after the immersing is finished, and then the leaching and drying are carried out;
s04: and (5) feeding the glass fiber agent and the doped bentonite agent into a ball mill according to the weight ratio (5-7) 1, ball milling, washing with water and drying after ball milling is finished, so as to obtain the glass fiber agent doped with bentonite.
The mass fraction of the sodium citrate solution in the embodiment is 10-15%; the mass fraction of the chitosan solution is 4-8%; the mass fraction of the yttrium nitrate solution is 2-5%; the mass fraction of the sulfuric acid solution is 8-12%.
The ball milling speed of the ball milling treatment in the embodiment is 1000-1500 r/min, and the ball milling time is 1-2 h.
The preparation method of the silicon carbide whisker blended boron nitride agent comprises the following steps:
s101: feeding the flaky boron nitride into a potassium permanganate solution with the total amount of 4-5 times of the flaky boron nitride, stirring and dispersing uniformly, and then washing and drying to obtain a pretreated flaky boron nitride agent;
s102: adding 4-6 parts of silicon carbide whisker and 6-10 parts of pretreated flaky boron nitride agent into 10-15 parts of deionized water, then adding 2-3 parts of phosphoric acid buffer solution with the pH value of 5.0, 1-2 parts of sodium lignin sulfonate and 0.55-0.75 part of sodium dodecyl sulfate solution, stirring and reacting for 1-2 hours at the temperature of 45-50 ℃, stirring at the speed of 550-650 r/min, washing with water and drying to obtain the silicon carbide whisker blended boron nitride agent.
The mass fraction of the sodium dodecyl sulfate solution of this example was 8 to 12%.
The preparation method of the high heat-resistant resin composition for the electronic circuit substrate comprises the following steps:
uniformly stirring and mixing epoxy resin, 5% by mass of lanthanum sulfate solution, bentonite-doped glass fiber agent, sodium dodecyl benzene sulfonate and hydroxyapatite modifier, adding a curing agent into the uniformly mixed product, and fully stirring to obtain an improved resin composite material;
injecting the improved resin composition into a pressing mold, and performing pressing molding to obtain a resin matrix board; and immersing the resin substrate plate into the flame-retardant glue solution for immersing treatment, and then taking out and drying to form the high heat-resistant resin composition.
The immersion pressure of the immersion treatment of this example was 10 to 15MPa, and the immersion time was 20 to 30 minutes.
Example 1.
A highly heat-resistant resin composition for an electronic circuit substrate of the present embodiment, the highly heat-resistant resin composition comprising a resin base plate; wherein the resin matrix board is prepared by adopting an improved resin composition material through compression molding, and is immersed in the flame-retardant glue solution for immersion treatment to form a high heat-resistant resin composition;
the improved resin composition comprises the following raw materials in parts by weight:
80 parts of epoxy resin, 3 parts of lanthanum sulfate solution, 6 parts of bentonite-doped glass fiber agent, 100 parts of curing agent, 3 parts of sodium dodecyl benzene sulfonate and 4 parts of hydroxyapatite modifier;
the preparation method of the hydroxyapatite modifier comprises the following steps:
adding hydroxyapatite into sodium hydroxide solution according to the weight ratio of 1:5, performing ultrasonic dispersion treatment, performing ultrasonic treatment, washing with water, drying, calcining at 310 ℃ for 10min, performing calcination, and naturally cooling at room temperature;
the preparation method of the flame-retardant glue solution comprises the following steps:
weighing 5 parts of silicon carbide whisker blended boron nitride agent, 3 parts of flame retardant, 10 parts of epoxy resin glue, 20 parts of acetone solvent and 2 parts of silane coupling agent KH560; and (5) uniformly stirring and mixing the weighed raw materials to obtain the flame-retardant glue solution.
The curing agent of the embodiment is maleic anhydride; the flame retardant is prepared by mixing melamine and magnesium hydroxide according to the weight ratio of 1:2.
The mass fraction of the lanthanum sulfate solution is 4%; the mass fraction of the sodium hydroxide solution is 6%; ultrasonic dispersion treatment is carried out for 1h, and ultrasonic power is 450W.
The preparation method of the bentonite-doped glass fiber agent comprises the following steps:
s01: placing bentonite at 220 ℃ for heat treatment for 10min, then heating to 350 ℃ at the rate of 2 ℃/min, preserving heat for 5min, and finally cooling to room temperature at the rate of 1 ℃/min to obtain the heat-treated bentonite;
s02: uniformly stirring and mixing 8 parts of heat-treated bentonite, 2 parts of sodium carboxymethyl cellulose, 1 part of chitosan solution, 15 parts of sodium citrate solution and 1 part of silica sol to obtain a doped bentonite agent;
s03: 5 parts of glass fiber is sent into 10 parts of sulfuric acid solution to be stirred uniformly, then washed and dried, and then immersed into yttrium nitrate solution, the immersing treatment is carried out, the immersing pressure is 10MPa, the immersing is carried out for 1h, and then the glass fiber agent is obtained after the leaching and drying;
s04: and (3) feeding the glass fiber agent and the doped bentonite agent into a ball mill according to a weight ratio of 5:1 for ball milling treatment, and after ball milling, washing and drying to obtain the glass fiber agent doped with bentonite.
The mass fraction of the sodium citrate solution of this example was 10%; the mass fraction of the chitosan solution is 4%; the mass fraction of the yttrium nitrate solution is 2%; the mass fraction of the sulfuric acid solution was 8%.
The ball milling speed of the ball milling treatment in this example was 1000r/min and the ball milling time was 1h.
The preparation method of the silicon carbide whisker blended boron nitride agent comprises the following steps:
s101: sending the flaky boron nitride into a potassium permanganate solution with the total amount of 4 times of the flaky boron nitride, stirring and dispersing uniformly, and then washing and drying to obtain a pretreated flaky boron nitride agent;
s102: adding 4 parts of silicon carbide whisker and 6 parts of pretreated flaky boron nitride agent into 10 parts of deionized water, then adding 2 parts of phosphoric acid buffer solution with the pH value of 5.0, 1 part of sodium lignin sulfonate and 0.55 part of sodium dodecyl sulfate solution, stirring at 45 ℃ for reaction for 1h, wherein the stirring speed is 550r/min, and after the stirring is finished, washing and drying, thus obtaining the silicon carbide whisker blended boron nitride agent.
The mass fraction of the sodium dodecyl sulfate solution of this example was 8%.
The preparation method of the high heat-resistant resin composition for the electronic circuit substrate comprises the following steps:
uniformly stirring and mixing epoxy resin, 5% by mass of lanthanum sulfate solution, bentonite-doped glass fiber agent, sodium dodecyl benzene sulfonate and hydroxyapatite modifier, adding a curing agent into the uniformly mixed product, and fully stirring to obtain an improved resin composite material;
injecting the improved resin composition into a pressing mold, and performing pressing molding to obtain a resin matrix board; and immersing the resin substrate plate into the flame-retardant glue solution for immersing treatment, and then taking out and drying to form the high heat-resistant resin composition.
The immersion pressure of the immersion treatment of this example was 10MPa, and the immersion time was 20 minutes.
Example 2.
A highly heat-resistant resin composition for an electronic circuit substrate of the present embodiment, the highly heat-resistant resin composition comprising a resin base plate; wherein the resin matrix board is prepared by adopting an improved resin composition material through compression molding, and is immersed in the flame-retardant glue solution for immersion treatment to form a high heat-resistant resin composition;
the improved resin composition comprises the following raw materials in parts by weight:
120 parts of epoxy resin, 6 parts of lanthanum sulfate solution, 10 parts of bentonite-doped glass fiber agent, 110 parts of curing agent, 5 parts of sodium dodecyl benzene sulfonate and 8 parts of hydroxyapatite modifier;
the preparation method of the hydroxyapatite modifier comprises the following steps:
adding hydroxyapatite into sodium hydroxide solution according to the weight ratio of 1:5, performing ultrasonic dispersion treatment, performing ultrasonic treatment, washing with water, drying, calcining at 320 ℃ for 20min, performing calcination, and naturally cooling at room temperature;
the preparation method of the flame-retardant glue solution comprises the following steps:
weighing 10 parts of silicon carbide whisker blended boron nitride agent, 6 parts of flame retardant, 15 parts of epoxy resin glue, 25 parts of acetone solvent and 5 parts of silane coupling agent KH560; and (5) uniformly stirring and mixing the weighed raw materials to obtain the flame-retardant glue solution.
The curing agent of the embodiment is maleic anhydride; the flame retardant is prepared by mixing melamine and magnesium hydroxide according to the weight ratio of 1:2.
The mass fraction of the lanthanum sulfate solution is 8%; the mass fraction of the sodium hydroxide solution is 8%; ultrasonic dispersion treatment is carried out for 2 hours, and ultrasonic power is 550W.
The preparation method of the bentonite-doped glass fiber agent comprises the following steps:
s01: heat-treating bentonite at 230deg.C for 15min, heating to 370deg.C at a rate of 5deg.C/min, maintaining for 10min, and cooling to room temperature at a rate of 3deg.C/min to obtain heat-treated bentonite;
s02: uniformly stirring and mixing 12 parts of heat-treated bentonite, 5 parts of sodium carboxymethyl cellulose, 3 parts of chitosan solution, 20 parts of sodium citrate solution and 2 parts of silica sol to obtain a doped bentonite agent;
s03: 10 parts of glass fiber is sent into 15 parts of sulfuric acid solution to be stirred uniformly, then washed and dried, and then immersed into yttrium nitrate solution, the immersing treatment is carried out, the immersing pressure is 15MPa, the immersing is finished for 2 hours, and then the glass fiber agent is obtained through suction filtration and drying;
s04: and (3) feeding the glass fiber agent and the doped bentonite agent into a ball mill according to the weight ratio of 7:1 for ball milling treatment, and after ball milling, washing and drying to obtain the glass fiber agent doped with bentonite.
The mass fraction of the sodium citrate solution of this example was 15%; the mass fraction of the chitosan solution is 8%; the mass fraction of the yttrium nitrate solution is 5%; the mass fraction of the sulfuric acid solution was 12%.
The ball milling speed of the ball milling treatment in this example was 1500r/min and the ball milling time was 2h.
The preparation method of the silicon carbide whisker blended boron nitride agent comprises the following steps:
s101: sending the flaky boron nitride into a potassium permanganate solution with the total amount of 5 times of the flaky boron nitride, stirring and dispersing uniformly, and then washing and drying to obtain a pretreated flaky boron nitride agent;
s102: adding 6 parts of silicon carbide whisker and 10 parts of pretreated flaky boron nitride agent into 15 parts of deionized water, then adding 3 parts of phosphoric acid buffer solution with pH value of 5.0, 2 parts of sodium lignin sulfonate and 0.75 part of sodium dodecyl sulfate solution, stirring at 50 ℃ for reaction for 2 hours, wherein the stirring speed is 650r/min, and after the stirring, washing and drying, thus obtaining the silicon carbide whisker blended boron nitride agent.
The mass fraction of the sodium dodecyl sulfate solution of this example was 12%.
The preparation method of the high heat-resistant resin composition for the electronic circuit substrate comprises the following steps:
uniformly stirring and mixing epoxy resin, 5% by mass of lanthanum sulfate solution, bentonite-doped glass fiber agent, sodium dodecyl benzene sulfonate and hydroxyapatite modifier, adding a curing agent into the uniformly mixed product, and fully stirring to obtain an improved resin composite material;
injecting the improved resin composition into a pressing mold, and performing pressing molding to obtain a resin matrix board; and immersing the resin substrate plate into the flame-retardant glue solution for immersing treatment, and then taking out and drying to form the high heat-resistant resin composition.
The immersion pressure of the immersion treatment of this example was 15MPa, and the immersion time was 30min.
Example 3.
A highly heat-resistant resin composition for an electronic circuit substrate of the present embodiment, the highly heat-resistant resin composition comprising a resin base plate; wherein the resin matrix board is prepared by adopting an improved resin composition material through compression molding, and is immersed in the flame-retardant glue solution for immersion treatment to form a high heat-resistant resin composition;
the improved resin composition comprises the following raw materials in parts by weight:
100 parts of epoxy resin, 4.5 parts of lanthanum sulfate solution, 8 parts of bentonite-doped glass fiber agent, 105 parts of curing agent, 4 parts of sodium dodecyl benzene sulfonate and 6 parts of hydroxyapatite modifier;
the preparation method of the hydroxyapatite modifier comprises the following steps:
adding hydroxyapatite into sodium hydroxide solution according to the weight ratio of 1:5, performing ultrasonic dispersion treatment, performing ultrasonic treatment, washing with water, drying, calcining at 315 ℃ for 15min, performing calcination, and naturally cooling at room temperature;
the preparation method of the flame-retardant glue solution comprises the following steps:
7.5 parts of silicon carbide whisker blended boron nitride agent, 4.5 parts of flame retardant, 12.5 parts of epoxy resin glue, 22.5 parts of acetone solvent and 3.5 parts of silane coupling agent KH560 are weighed; and (5) uniformly stirring and mixing the weighed raw materials to obtain the flame-retardant glue solution.
The curing agent of the embodiment is maleic anhydride; the flame retardant is prepared by mixing melamine and magnesium hydroxide according to the weight ratio of 1:2.
The mass fraction of the lanthanum sulfate solution is 6%; the mass fraction of the sodium hydroxide solution is 7%; ultrasonic dispersion treatment is carried out for 1.5 hours, and ultrasonic power is 500W.
The preparation method of the bentonite-doped glass fiber agent comprises the following steps:
s01: placing bentonite at 225 ℃ for heat treatment for 12min, then heating to 360 ℃ at the speed of 3.5 ℃/min, preserving heat for 7.5min, and finally cooling to room temperature at the speed of 2 ℃/min to obtain the heat-treated bentonite;
s02: uniformly stirring and mixing 10 parts of heat-treated bentonite, 3.5 parts of sodium carboxymethyl cellulose, 2 parts of chitosan solution, 17.5 parts of sodium citrate solution and 1.5 parts of silica sol to obtain a doped bentonite agent;
s03: feeding 7.5 parts of glass fiber into 12.5 parts of sulfuric acid solution, stirring uniformly, washing with water, drying, immersing into yttrium nitrate solution, immersing under the pressure of 12.5MPa for 1.5 hours, filtering, and drying to obtain glass fiber agent;
s04: and (3) feeding the glass fiber agent and the doped bentonite agent into a ball mill according to the weight ratio of 6:1 for ball milling treatment, and after ball milling, washing and drying to obtain the glass fiber agent doped with bentonite.
The mass fraction of the sodium citrate solution of this example was 12.5%; the mass fraction of the chitosan solution is 6%; the mass fraction of the yttrium nitrate solution is 3.5%; the mass fraction of the sulfuric acid solution is 10%.
The ball milling speed of the ball milling treatment in this example was 1250r/min and the ball milling time was 1.5h.
The preparation method of the silicon carbide whisker blended boron nitride agent comprises the following steps:
s101: feeding the flaky boron nitride into a potassium permanganate solution with the total amount of 4.5 times of the flaky boron nitride, stirring and dispersing uniformly, and then washing and drying to obtain a pretreated flaky boron nitride agent;
s102: adding 5 parts of silicon carbide whisker and 8 parts of pretreated flaky boron nitride agent into 12.5 parts of deionized water, then adding 2.5 parts of phosphoric acid buffer solution with the pH value of 5.0, 1.5 parts of sodium lignin sulfonate and 0.60 part of sodium dodecyl sulfate solution, stirring at 47 ℃ for reaction for 1.5 hours, wherein the stirring speed is 600r/min, and after stirring, washing and drying to obtain the silicon carbide whisker blended boron nitride agent.
The mass fraction of the sodium dodecyl sulfate solution of this example was 10%.
The preparation method of the high heat-resistant resin composition for the electronic circuit substrate comprises the following steps:
uniformly stirring and mixing epoxy resin, 5% by mass of lanthanum sulfate solution, bentonite-doped glass fiber agent, sodium dodecyl benzene sulfonate and hydroxyapatite modifier, adding a curing agent into the uniformly mixed product, and fully stirring to obtain an improved resin composite material;
injecting the improved resin composition into a pressing mold, and performing pressing molding to obtain a resin matrix board; and immersing the resin substrate plate into the flame-retardant glue solution for immersing treatment, and then taking out and drying to form the high heat-resistant resin composition.
The immersion pressure of the immersion treatment of this example was 12.5MPa, and the immersion time was 25 minutes.
Comparative example 1.
The difference from example 3 is that the modified resin composition is not added with a glass fiber agent doped with bentonite.
Comparative example 2.
The difference from example 3 is that the preparation method of the bentonite-doped glass fiber agent is not added with the bentonite-doped glass fiber agent.
Comparative example 3.
The difference from example 3 is that bentonite is used instead of bentonite in the heat-treated bentonite in the preparation process of the doped bentonite agent.
Comparative example 4.
The difference from example 3 is that no chitosan solution or silica sol was added in the preparation method of the doped bentonite agent.
Comparative example 5.
The difference from example 3 is that the glass fiber agent is directly replaced by glass fiber raw material in the preparation method of the doped bentonite agent.
Comparative example 6.
The difference from example 3 is that no treatment with a solution immersed in yttrium nitrate was used in the preparation of the glass fiber agent.
Comparative example 7.
The difference from example 3 is that the modified resin composition was not added with a hydroxyapatite modifier.
Comparative example 8.
The difference from example 3 is that the hydroxyapatite modifier is directly replaced by a hydroxyapatite raw material.
Comparative example 9.
The difference from example 3 is that silicon carbide whisker and boron nitride agent are not added into the flame-retardant glue solution.
Comparative example 10.
The difference from example 3 is that silicon carbide whiskers were not added in the preparation of the silicon carbide whisker blended boron nitride agent.
Comparative example 11.
The difference from example 3 is that the preparation of the silicon carbide whisker blended boron nitride agent does not add a pretreated platy boron nitride agent.
Comparative example 12.
The difference from example 3 is that no sodium lignin sulfonate or sodium dodecyl sulfate solution was added in the preparation of the silicon carbide whisker blended boron nitride agent.
The test products of examples 1 to 3 and comparative examples 1 to 12 were subjected to performance test, the flame retardance and elongation at break of the test products, and the heat resistance of the test products were tested by placing the products at 65℃for 6 hours;
as can be seen from comparative examples 1 to 12 and examples 1 to 3;
the product of the embodiment 3 has excellent elongation at break and limiting oxygen index, the performance effects of the two can be improved in a coordinated way, and meanwhile, the product has excellent performance stability under heat-resistant conditions;
as shown in comparative examples 1 to 6 and example 3, the modified resin composition is not added with the glass fiber agent doped with bentonite, the breaking elongation and limiting oxygen index performance of the product are obviously reduced, the performance change is more obvious under the heat-resistant condition, the bentonite is not added in the preparation method of the glass fiber agent doped with bentonite, the bentonite subjected to heat treatment is replaced by bentonite, the chitosan solution, silica sol and glass fiber agent are not added in the preparation method of the doped bentonite agent, the glass fiber agent is directly replaced by glass fiber raw materials, the glass fiber agent is not subjected to treatment by immersing in yttrium nitrate solution, the performance of the product is in a poor trend, and the performance effect of the product is most obvious only by adopting the glass fiber agent prepared by the method, the doped bentonite agent and the specific raw material proportion of the invention;
from comparative examples 7 to 8 and example 3, it is seen that the hydroxyapatite modifier and the bentonite-doped glass fiber agent are coordinated with each other and cooperate with each other, the elongation at break and limiting oxygen index of the product can be improved in a coordinated manner, and the heat resistance stability of the product is improved obviously;
as shown in comparative examples 9 to 12 and example 3, the flame retardant performance of the product is obviously degraded without adding silicon carbide whisker and boron nitride agent in the flame retardant glue solution, and the performance of the product is obviously improved only by adopting the silicon carbide whisker and boron nitride agent prepared by the method of the invention without adding silicon carbide whisker, without adding pretreated flaky boron nitride agent, without adding sodium lignin sulfonate and sodium dodecyl sulfate solution.
In summary, the modified resin composition of the invention is added with the bentonite-doped glass fiber agent, the hydroxyapatite modifier and the flame-retardant glue solution, and the silicon carbide whisker and the boron nitride agent are added, so that the elongation at break and limiting oxygen index of the product can be improved in a coordinated manner, the heat-resistant stability of the product is excellent, and the performance effect of the product is most obvious only when the modified resin composition is prepared by adopting the raw material process of the invention, and the effect is not as obvious as when the modified resin composition is replaced by adopting other processes.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential characteristics thereof. The present embodiments are, therefore, to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Furthermore, it should be understood that although the present disclosure describes embodiments, not every embodiment is provided with a separate embodiment, and that this description is provided for clarity only, and that the disclosure is not limited to the embodiments described in detail below, and that the embodiments described in the examples may be combined as appropriate to form other embodiments that will be apparent to those skilled in the art.
Claims (10)
1. A high heat-resistant resin composition for an electronic circuit substrate, characterized in that the high heat-resistant resin composition comprises a resin base plate; wherein the resin matrix board is prepared by adopting an improved resin composition material through compression molding, and is immersed in the flame-retardant glue solution for immersion treatment to form a high heat-resistant resin composition;
the improved resin composition comprises the following raw materials in parts by weight:
80-120 parts of epoxy resin, 3-6 parts of lanthanum sulfate solution, 6-10 parts of bentonite-doped glass fiber agent, 100-110 parts of curing agent, 3-5 parts of sodium dodecyl benzene sulfonate and 4-8 parts of hydroxyapatite modifier;
the preparation method of the hydroxyapatite modifier comprises the following steps:
adding hydroxyapatite into sodium hydroxide solution according to the weight ratio of 1:5, performing ultrasonic dispersion treatment, performing ultrasonic treatment, washing with water, drying, calcining at 310-320 ℃ for 10-20 min, performing calcination, and naturally cooling at room temperature;
the preparation method of the flame-retardant glue solution comprises the following steps:
weighing 5-10 parts of silicon carbide whisker blended boron nitride agent, 3-6 parts of flame retardant, 10-15 parts of epoxy resin glue, 20-25 parts of acetone solvent and 2-5 parts of silane coupling agent KH560; and (5) uniformly stirring and mixing the weighed raw materials to obtain the flame-retardant glue solution.
2. The highly heat-resistant resin composition for electronic circuit substrates according to claim 1, wherein the curing agent is maleic anhydride; the flame retardant is prepared by mixing melamine and magnesium hydroxide according to the weight ratio of 1:2.
3. The high heat-resistant resin composition for electronic circuit substrates according to claim 1, wherein the lanthanum sulfate solution has a mass fraction of 4 to 8%; the mass fraction of the sodium hydroxide solution is 6-8%; ultrasonic dispersion treatment is carried out for 1-2 hours, and ultrasonic power is 450-550W.
4. The high heat resistant resin composition for electronic circuit substrates according to claim 1, wherein the bentonite-doped glass fiber agent is prepared by the following steps:
s01: heat-treating bentonite at 220-230 deg.c for 10-15 min, heating to 350-370 deg.c at 2-5 deg.c/min, maintaining for 5-10 min, and cooling to room temperature at 1-3 deg.c/min to obtain heat treated bentonite;
s02: uniformly stirring 8-12 parts of heat-treated bentonite, 2-5 parts of sodium carboxymethyl cellulose, 1-3 parts of chitosan solution, 15-20 parts of sodium citrate solution and 1-2 parts of silica sol to obtain a doped bentonite agent;
s03: 5-10 parts of glass fiber is sent into 10-15 parts of sulfuric acid solution to be stirred uniformly, then washed and dried, and then immersed into yttrium nitrate solution, the immersing treatment is carried out, the immersing pressure is 10-15 MPa, the immersing is carried out for 1-2 h, and then the glass fiber agent is obtained after the immersing is finished, and then the leaching and drying are carried out;
s04: and (5) feeding the glass fiber agent and the doped bentonite agent into a ball mill according to the weight ratio (5-7) 1, ball milling, washing with water and drying after ball milling is finished, so as to obtain the glass fiber agent doped with bentonite.
5. The high heat resistant resin composition for electronic circuit substrates according to claim 4, wherein the mass fraction of the sodium citrate solution is 10 to 15%; the mass fraction of the chitosan solution is 4-8%; the mass fraction of the yttrium nitrate solution is 2-5%; the mass fraction of the sulfuric acid solution is 8-12%.
6. The high heat resistant resin composition for electronic circuit substrates according to claim 5, wherein the ball milling speed of the ball milling treatment is 1000 to 1500r/min and the ball milling time is 1 to 2 hours.
7. The high heat resistant resin composition for electronic circuit substrates according to claim 1, wherein the preparation method of the silicon carbide whisker and boron nitride agent is as follows:
s101: feeding the flaky boron nitride into a potassium permanganate solution with the total amount of 4-5 times of the flaky boron nitride, stirring and dispersing uniformly, and then washing and drying to obtain a pretreated flaky boron nitride agent;
s102: adding 4-6 parts of silicon carbide whisker and 6-10 parts of pretreated flaky boron nitride agent into 10-15 parts of deionized water, then adding 2-3 parts of phosphoric acid buffer solution with the pH value of 5.0, 1-2 parts of sodium lignin sulfonate and 0.55-0.75 part of sodium dodecyl sulfate solution, stirring and reacting for 1-2 hours at the temperature of 45-50 ℃, stirring at the speed of 550-650 r/min, washing with water and drying to obtain the silicon carbide whisker blended boron nitride agent.
8. The highly heat-resistant resin composition for electronic circuit substrates according to claim 7, wherein the sodium dodecyl sulfate solution has a mass fraction of 8 to 12%.
9. A method for producing the highly heat-resistant resin composition for electronic circuit substrates according to any one of claims 1 to 8, comprising the steps of:
uniformly stirring and mixing epoxy resin, 5% by mass of lanthanum sulfate solution, bentonite-doped glass fiber agent, sodium dodecyl benzene sulfonate and hydroxyapatite modifier, adding a curing agent into the uniformly mixed product, and fully stirring to obtain an improved resin composite material;
injecting the improved resin composition into a pressing mold, and performing pressing molding to obtain a resin matrix board; and immersing the resin substrate plate into the flame-retardant glue solution for immersing treatment, and then taking out and drying to form the high heat-resistant resin composition.
10. The method for producing a highly heat-resistant resin composition for electronic circuit substrates according to claim 9, wherein the immersion pressure of the immersion treatment is 10 to 15MPa and the immersion time is 20 to 30 minutes.
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