A method for producing a circuit board

By coating the circuit board with an improved layer and a copper foil layer and combining it with a specific treatment liquid, the problem of the difficulty in coordinating the dielectric loss and thermal conductivity of the circuit board is solved, and the stability and efficiency of the product under high heat and high humidity conditions are improved.

CN119893875BActive Publication Date: 2025-10-17JIANGXI LINGDEHUI CIRCUIT CO LTD
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Patent Information

Application Number
CN202510099873.0
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2025-01-22
Publication Date
2025-10-17
Estimated Expiration
2045-01-22

AI Technical Summary

Technical Problem

Existing circuit boards have poor dielectric loss during production, and it is difficult to coordinate thermal conductivity and wear resistance. The products have poor performance stability under high heat and high humidity conditions, which limits the product's efficiency.

Method used

The copper substrate surface is coated with an improved layer and a copper foil layer. The improved layer is composed of epoxy resin, modified filler, nano-titanium dioxide regulator and curing agent. It is formed by hot pressing and combined with a treatment liquid of sodium citrate, chitosan and silane coupling agent to optimize the interface and performance stability.

Benefits of technology

The thermal conductivity, dielectric loss and wear resistance of the circuit board are improved. The product performance is more stable under high heat and high humidity conditions, the performance is balanced and coordinated, and the utilization efficiency is significantly improved.

✦ Generated by Eureka AI based on patent content.

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Abstract

The present application relates to the technical field of circuit board, and particularly relates to a production method of circuit board, which comprises the following steps: sequentially arranging an improved layer and a copper foil layer on the surface of a copper substrate, and then performing hot-pressing treatment on the substrate coated with the improved layer and the copper foil layer, wherein the hot-pressing temperature is 180 DEG C, and the hot-pressing time is 2h. In the production of the circuit board, the surface of the copper substrate is matched with the improved layer and the copper foil layer, the improved layer is obtained by compounding and adjusting epoxy resin, modified filler agent, nano titanium dioxide regulator and curing agent, and is then coated on the surface of the copper substrate to form the improved layer, so that the heat conductivity, dielectric loss and wear resistance of the product are enhanced, the performance balance of the product is improved, and the product performance stability is significantly improved under high heat and high humidity conditions.
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Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of circuit board, and particularly relates to a production method of circuit board. BACKGROUND

[0002] With the rapid development of electronic technology, the manufacturing process of printed circuit board (PCB) which is almost indispensable in electronic products has also been greatly developed. The existing industry has higher and higher requirements for printed circuit board, and the printed circuit board is also developing towards the multi-layer circuit board technology of high-density wiring interconnection (HDI) process, so that more functions can be provided in a smaller space of the PCB.

[0003] The existing circuit board has poor dielectric loss in preparation, and the thermal conductivity of the product is difficult to coordinate with the dielectric loss and wear resistance for improvement. The performance balance technology of the product is the difficulty of the present application, and the product performance stability is poor under high heat and high humidity conditions, which limits the use efficiency of the product. SUMMARY

[0004] In view of the defects of the prior art, the purpose of the present application is to provide a production method of circuit board to solve the problems in the background art.

[0005] The technical problem of the present application is solved by the following technical scheme:

[0006] The present application provides a production method of circuit board, comprising the following steps:

[0007] Step one: sequentially arranging an improvement layer and a copper foil layer on the surface of a copper substrate, and then heat pressing the substrate covered with the improvement layer and the copper foil layer, the heat pressing temperature is 180 DEG C, and the heat pressing time is 2h;

[0008] The improvement layer comprises the following raw materials by weight:

[0009] epoxy resin 50-55 parts, modified filler 5-8 parts, nano-titanium dioxide adjusting agent 4-7 parts, and curing agent 4-7 parts;

[0010] Mixing the epoxy resin, the modified filler, the nano-titanium dioxide adjusting agent and the curing agent to obtain an improvement material, and coating the improvement material on the surface of the copper substrate to form the improvement layer;

[0011] Step two: uniformly blending 3-5 parts of a 5% sodium citrate solution, 2-4 parts of a 2% chitosan solution and 1-3 parts of silane coupling agent KH560 to obtain a treatment liquid;

[0012] Step three: immersing the product of step one in sufficient treatment liquid, the immersion pressure is 10Mpa, and the immersion time is 1h. After the immersion, drying is performed to obtain the circuit board of the present application.

[0013] Preferably, the thickness of the modified layer is 80um; the thickness of the copper foil layer is 20um; the epoxy resin is prepared according to a weight ratio of 2:1 of bisphenol A type epoxy resin and phenolic epoxy resin; and the curing agent is 2-phenylimidazole.

[0014] Preferably, the preparation method of the modified filler agent is as follows:

[0015] S01: uniformly mix silane coupling agent KH550, ethanol and water according to a weight ratio of 2:5:1 to obtain a silane solution; uniformly blend 2-4 parts of modified boron nitride whisker, 3-5 parts of the silane solution and 1-3 parts of urea solution to obtain a modified solution;

[0016] S02: preheat the nano-palygorskite at 62-66℃ for 1h, then stir and modify the preheated nano-palygorskite in the modified solution at 3-5 times the total amount of the preheated nano-palygorskite, and after the stirring is completed, the modified nano-palygorskite is obtained;

[0017] S03: uniformly stir and mix 3-5 parts of glass fiber, 2-3 parts of cerium oxide and 4-7 parts of sodium silicate solution, then perform suction filtration and drying, and then calcine at 150-170℃ for 1h, and after the calcination is completed, the filler aid is obtained;

[0018] S04: uniformly mix and ball mill the modified nano-palygorskite and the filler aid according to a weight ratio of 5:3, perform suction filtration and drying after the ball milling is completed, and the modified filler agent is obtained.

[0019] Preferably, the mass fraction of the urea solution is 2-5%; the stirring speed of the stirring modification treatment is 450-550r / min, and the stirring time is 1h.

[0020] Preferably, the mass fraction of the sodium silicate solution is 3-6%.

[0021] Preferably, the preparation method of the modified boron nitride whisker is as follows:

[0022] Add 4-7 parts of boron nitride whisker, 1-3 parts of nano-silica sol to 5-8 parts of sodium lignosulfonate solution, then add 2-3 parts of silicon carbide powder and 1-3 parts of lanthanum oxide, and then uniformly mix and ball mill, and after the ball milling is completed, perform suction filtration and drying to obtain the modified boron nitride whisker.

[0023] Preferably, the mass fraction of the sodium lignosulfonate solution is 2-5%; the ball milling speed of the uniform ball milling treatment is 1050-1150r / min, and the ball milling time is 1h.

[0024] Preferably, the preparation method of the nano-titanium dioxide regulator is as follows:

[0025] S101: stirring the nano-titanium dioxide in sufficient potassium permanganate solution, then washing with water, filtering and drying;

[0026] S102: stirring and adjusting the dried nano-titanium dioxide and the adjusting liquid according to a weight ratio of 2:5, filtering and drying after the stirring, to obtain a nano-titanium dioxide adjusting agent;

[0027] The adjusting liquid is prepared by stirring 2-4 parts of hydroxyapatite, 1-3 parts of alginic acid and 1-2 parts of calcium stearate in 3-6 parts of a 5% mass fraction sodium dodecylbenzenesulfonate solution.

[0028] Preferably, the stirring speed of the stirring and adjusting treatment is 550-750 r / min, and the stirring time is 1 h.

[0029] Preferably, the mass fraction of the potassium permanganate solution is 5-7%.

[0030] Compared with the prior art, the present application has the following beneficial effects:

[0031] The circuit board is produced by using a copper substrate surface with an improved layer and a copper foil layer, and the improved layer is obtained by mixing and adjusting an improved material of epoxy resin, modified filler agent, nano-titanium dioxide regulator and curing agent, and then coated on the surface of the copper substrate to form the improved layer, thereby enhancing the product's thermal conductivity, dielectric loss and wear resistance, improving the balanced and coordinated performance of the product, and significantly improving the product's performance stability under high heat and high humidity conditions; the modified filler agent is preheated at 62-66 DEG C for 1 h, then modified by stirring in a modified liquid, and the modified liquid is obtained by mixing silane coupling agent KH550, ethanol and water in a weight ratio of 2:5:1; then the modified boron nitride whisker, silane liquid and urea solution are uniformly blended, the interface of the raw materials of the optimized system is improved by the silane liquid, the modified boron nitride whisker is distributed in the system, and the urea solution is used to enhance the coordination effect between the raw materials, and the modified boron nitride whisker is further treated by ball milling after being mixed and uniformly ground with boron nitride whisker, nano-silica sol and sodium lignosulfonate solution, silicon carbide powder and lanthanum oxide, and then the raw materials such as silicon carbide powder and lanthanum oxide are used to improve the effect of the whisker in the system with the nano-attapulgite and the filler agent, thereby further improving the performance of the product; the filler agent is stirred and mixed uniformly with glass fiber, cerium oxide and sodium silicate solution, then filtered and dried, and then calcined at 150-170 DEG C for 1 h to obtain the filler agent, which is used to supplement the system and improve the performance stability and coordination of the system, thereby further improving the performance of the product; the nano-titanium dioxide regulator is stirred uniformly in potassium permanganate solution to optimize its activity, and then improved by adjusting liquid, and the hydroxyapatite, alginic acid, calcium stearate and 5% sodium dodecylbenzenesulfonate solution in the adjusting liquid are mixed and adjusted to improve the coordination effect between the raw materials, thereby further improving the performance of the product; and the product of step one is treated by a treatment liquid obtained by mixing sodium citrate solution, 2% chitosan solution and silane coupling agent KH560, thereby further improving the interface of the copper foil layer, the improved layer and the copper substrate, and further improving the performance stability of the circuit board. DETAILED DESCRIPTION

[0032] The technical solutions in the embodiments of the present application will be clearly and completely described in connection with specific embodiments. Obviously, the described embodiments are only part of the embodiments of the present application, rather than all the embodiments. Based on the embodiments in the present application, all other embodiments obtained by those skilled in the art without creative labor fall within the scope of the present application.

[0033] The production method of the circuit board of the present embodiment comprises the following steps:

[0034] Step one: the copper substrate surface is sequentially provided with an improved layer and a copper foil layer, and then the substrate covered with the improved layer and the copper foil layer is heat-pressed, the heat-pressing temperature is 180℃, and the heat-pressing time is 2h;

[0035] The improved layer comprises the following raw materials by weight:

[0036] Epoxy resin 50-55 parts, modified filler agent 5-8 parts, nano titanium dioxide adjusting agent 4-7 parts, and curing agent 4-7 parts;

[0037] The epoxy resin, the modified filler agent, the nano titanium dioxide adjusting agent, and the curing agent are mixed uniformly to obtain an improved material, and the improved material is coated on the surface of the copper substrate to form the improved layer;

[0038] Step two: 3-5 parts of a 5% sodium citrate solution, 2-4 parts of a 2% chitosan solution, and 1-3 parts of silane coupling agent KH560 are uniformly blended to obtain a treatment liquid;

[0039] Step three: the product of step one is immersed in sufficient treatment liquid, the immersion pressure is 10Mpa, the immersion time is 1h, after the immersion is completed, drying is performed, and a circuit board of the present application is obtained.

[0040] The thickness of the improved layer of the present embodiment is 80um; the thickness of the copper foil layer is 20um; the epoxy resin is prepared from bisphenol A type epoxy resin and phenolic epoxy resin at a weight ratio of 2:1; and the curing agent is 2-phenylimidazole.

[0041] The preparation method of the modified filler agent of the present embodiment is as follows:

[0042] S01: the silane coupling agent KH550, ethanol, and water are uniformly mixed at a weight ratio of 2:5:1 to obtain a silane solution; 2-4 parts of modified boron nitride whisker, 3-5 parts of the silane solution, and 1-3 parts of urea solution are uniformly blended to obtain a modified solution;

[0043] S02: the nano attapulgite is preheated at 62-66℃ for 1h, and then the preheated nano attapulgite is stirred in the modified solution at 3-5 times the total amount of the preheated nano attapulgite to perform a modification treatment, after the stirring is completed, a modified nano attapulgite is obtained;

[0044] S03: 3-5 parts of glass fiber, 2-3 parts of cerium oxide, and 4-7 parts of sodium silicate solution are uniformly stirred and mixed, then filtered, dried, and calcined at 150-170℃ for 1h, after the calcination is completed, a filler aid is obtained;

[0045] S04: the modified nano attapulgite and the filler aid are uniformly mixed at a weight ratio of 5:3, ball-milled, filtered, and dried to obtain a modified filler agent.

[0046] The mass fraction of the urea solution of the embodiment is 2-5%; the stirring speed of the stirring modification treatment is 450-550 r / min, and the stirring time is 1 h.

[0047] The mass fraction of the sodium silicate solution of the embodiment is 3-6%.

[0048] The preparation method of the modified boron nitride whisker of the embodiment is as follows:

[0049] 4-7 parts of boron nitride whisker, 1-3 parts of nano silicon sol, 5-8 parts of sodium lignosulfonate solution, 2-3 parts of silicon carbide powder, and 1-3 parts of lanthanum oxide are added into a ball mill, and then uniformly mixed and ball milled, and after the ball milling is completed, the mixture is extracted, filtered, and dried to obtain the modified boron nitride whisker.

[0050] The mass fraction of the sodium lignosulfonate solution of the embodiment is 2-5%; the ball milling speed of the uniform ball milling treatment is 1050-1150 r / min, and the ball milling time is 1 h.

[0051] The preparation method of the nano titanium dioxide regulator of the embodiment is as follows:

[0052] S101: uniformly stirring the nano titanium dioxide in a sufficient amount of potassium permanganate solution, and then washing with water, extracting, filtering, and drying;

[0053] S102: stirring and adjusting the dried nano titanium dioxide and the adjusting liquid according to a weight ratio of 2:5, extracting, filtering, and drying after the stirring is completed to obtain the nano titanium dioxide regulator.

[0054] The preparation method of the adjusting liquid is as follows: 2-4 parts of hydroxyapatite, 1-3 parts of alginic acid, and 1-2 parts of calcium stearate are added into 3-6 parts of a 5% mass fraction sodium dodecylbenzenesulfonate solution to obtain the adjusting liquid.

[0055] The stirring speed of the stirring adjustment treatment of the embodiment is 550-750 r / min, and the stirring time is 1 h.

[0056] The mass fraction of the potassium permanganate solution of the embodiment is 5-7%.

[0057] Embodiment 1.

[0058] The production method of the circuit board of the embodiment comprises the following steps:

[0059] Step one: sequentially arranging an improvement layer and a copper foil layer on the surface of a copper substrate, and then heat pressing the substrate covered with the improvement layer and the copper foil layer, the heat pressing temperature is 180℃, and the heat pressing time is 2 h.

[0060] The improvement layer comprises the following raw materials by weight:

[0061] Epoxy resin 50 parts, modified filler agent 5 parts, nano titanium dioxide modifier 4 parts, curing agent 4 parts;

[0062] Mixing the epoxy resin, modified filler agent, nano titanium dioxide modifier and curing agent to obtain the improved material, and coating the improved material on the surface of the copper substrate to form the improved layer;

[0063] Step two: uniformly blend 3 parts of a 5% mass fraction sodium citrate solution, 2 parts of a 2% mass fraction chitosan solution and 1 part of silane coupling agent KH560 to obtain a treatment liquid;

[0064] Step three: immerse the product of step one in sufficient treatment liquid, immerse under a pressure of 10Mpa for 1h, dry after the immersion is completed, to obtain the circuit board of the application.

[0065] The thickness of the improved layer of the embodiment is 80um; the thickness of the copper foil layer is 20um; the epoxy resin is prepared from bisphenol A type epoxy resin and phenolic epoxy resin in a weight ratio of 2:1; and the curing agent is 2-phenylimidazole.

[0066] The preparation method of the modified filler agent of the embodiment is as follows:

[0067] S01: uniformly mix silane coupling agent KH550, ethanol and water in a weight ratio of 2:5:1 to obtain a silane solution; and uniformly blend 2 parts of modified boron nitride whisker, 3 parts of the silane solution and 1 part of urea solution to obtain a modified solution;

[0068] S02: preheat the nano attapulgite at 62℃ for 1h, then stir and modify the preheated nano attapulgite in the modified solution at 3 times the total amount of the preheated nano attapulgite, and after the stirring is completed, obtain the modified nano attapulgite;

[0069] S03: uniformly stir and mix 3 parts of glass fiber, 2 parts of cerium oxide and 4 parts of sodium silicate solution, then perform suction filtration and drying, and then calcine at 150℃ for 1h, and after the calcination is completed, obtain the filler aid;

[0070] S04: uniformly mix and ball mill the modified nano attapulgite and the filler aid in a weight ratio of 5:3, perform suction filtration and drying after the ball milling is completed, to obtain the modified filler agent.

[0071] The mass fraction of the urea solution of the embodiment is 2%; the stirring speed of the stirring modification is 450r / min, and the stirring time is 1h.

[0072] The mass fraction of the sodium silicate solution of the embodiment is 3%.

[0073] The preparation method of the modified boron nitride whisker of the embodiment is as follows:

[0074] 4 parts of boron nitride whiskers and 1 part of nano-silica sol are added to 5 parts of sodium lignin sulfonate solution, followed by adding 2 parts of silicon carbide powder and 1 part of lanthanum oxide, and then mixing and ball milling. After the ball milling is completed, the modified boron nitride whiskers are obtained by filtration and drying.

[0075] The mass fraction of the sodium lignin sulfonate solution in this embodiment is 2%; the ball milling speed of the mixing ball milling treatment is 1050 r / min, and the ball milling is performed for 1 hour.

[0076] The preparation method of the nano titanium dioxide regulator of this embodiment is:

[0077] S101: Stir nano-titanium dioxide in a sufficient amount of potassium permanganate solution, then wash with water, filter and dry;

[0078] S102: Stirring and conditioning the dried nano-titanium dioxide and the conditioning solution in a weight ratio of 2:5. After stirring, filtering and drying to obtain the nano-titanium dioxide conditioning agent;

[0079] The preparation method of the regulating solution is as follows: 2 parts of hydroxyapatite, 1 part of alginic acid, and 1 part of calcium stearate are added to 3 parts of 5% by mass sodium dodecylbenzenesulfonate solution and stirred evenly to obtain the regulating solution.

[0080] The stirring speed of the stirring adjustment process in this embodiment is 550 r / min, and the stirring is performed for 1 hour.

[0081] The mass fraction of the potassium permanganate solution in this embodiment is 5%.

[0082] Example 2.

[0083] A method for producing a circuit board according to this embodiment includes the following steps:

[0084] Step 1: The surface of the copper substrate is sequentially provided with an improved layer and a copper foil layer, and then the substrate covered with the improved layer and the copper foil layer is subjected to hot pressing at a temperature of 180°C for 2 hours;

[0085] The improved layer comprises the following raw materials in parts by weight:

[0086] 55 parts of epoxy resin, 8 parts of modified filler, 7 parts of nano titanium dioxide regulator, and 7 parts of curing agent;

[0087] The epoxy resin, modified filler, nano titanium dioxide regulator and curing agent are mixed thoroughly to obtain an improved material, and the improved material is coated on the surface of the copper substrate to form an improved layer;

[0088] Step 2: 5 parts by mass of 5% sodium citrate solution, 4 parts by mass of 2% chitosan solution and 3 parts by mass of silane coupling agent KH560 were evenly mixed to obtain a treatment solution;

[0089] Step three: the product of step one is immersed in a sufficient amount of treatment solution, the immersion pressure is 10Mpa, the immersion time is 1h, after the immersion, the product is dried, and the circuit board of the application is obtained.

[0090] The thickness of the modified layer of the embodiment is 80um; the thickness of the copper foil layer is 20um; the epoxy resin is prepared from bisphenol A type epoxy resin and phenolic epoxy resin in a weight ratio of 2:1; and the curing agent is 2-phenylimidazole.

[0091] The preparation method of the modified filler agent of the embodiment is as follows:

[0092] S01: uniformly mix silane coupling agent KH550, ethanol and water in a weight ratio of 2:5:1 to obtain a silane solution; uniformly blend 4 parts of modified boron nitride whisker, 5 parts of the silane solution and 3 parts of urea solution to obtain a modified solution;

[0093] S02: preheat the nano-palygorskite at 66℃ for 1h, then stir and modify the preheated nano-palygorskite in the modified solution which is 5 times the total amount of the preheated nano-palygorskite, and after the stirring is completed, the modified nano-palygorskite is obtained;

[0094] S03: uniformly stir and mix 5 parts of glass fiber, 3 parts of cerium oxide and 7 parts of sodium silicate solution, then perform suction filtration and drying, and then calcine at 170℃ for 1h, and after the calcination is completed, the filler aid is obtained;

[0095] S04: uniformly mix and ball mill the modified nano-palygorskite and the filler aid in a weight ratio of 5:3, perform suction filtration and drying after the ball milling is completed, and the modified filler agent is obtained.

[0096] The mass fraction of the urea solution of the embodiment is 5%; the stirring speed of the stirring modification is 550r / min, and the stirring time is 1h.

[0097] The mass fraction of the sodium silicate solution of the embodiment is 6%.

[0098] The preparation method of the modified boron nitride whisker of the embodiment is as follows:

[0099] Add 7 parts of boron nitride whisker and 3 parts of nano-silica sol to 8 parts of sodium lignosulfonate solution, then add 3 parts of silicon carbide powder and 3 parts of lanthanum oxide, and then uniformly mix and ball mill, perform suction filtration and drying after the ball milling is completed, and the modified boron nitride whisker is obtained.

[0100] The mass fraction of the sodium lignosulfonate solution of the embodiment is 5%; the ball milling speed of the uniform ball milling is 1150r / min, and the ball milling time is 1h.

[0101] The preparation method of the nano-titanium dioxide regulator of the embodiment is as follows:

[0102] S101: Stir the nanometer titanium dioxide in a sufficient amount of potassium permanganate solution, then wash with water, filter and dry;

[0103] S102: Stir the dried nanometer titanium dioxide and the adjusting solution according to a weight ratio of 2:5, filter and dry after the stirring is completed, to obtain a nanometer titanium dioxide adjusting agent;

[0104] The adjusting solution is prepared by stirring 4 parts of hydroxyapatite, 3 parts of alginic acid and 2 parts of calcium stearate in 6 parts of a 5% sodium dodecylbenzenesulfonate solution.

[0105] The stirring speed of the stirring and adjusting process of this embodiment is 750 r / min, and the stirring time is 1 h.

[0106] The mass fraction of the potassium permanganate solution of this embodiment is 7%.

[0107] Example 3.

[0108] The production method of the circuit board of this embodiment comprises the following steps:

[0109] Step one: sequentially arrange an improvement layer and a copper foil layer on the surface of a copper substrate, and then perform hot pressing treatment on the substrate covered with the improvement layer and the copper foil layer, with a hot pressing temperature of 180℃ and a hot pressing time of 2 h;

[0110] The improvement layer comprises the following raw materials by weight:

[0111] 52.5 parts of epoxy resin, 6.5 parts of modified filler, 5.5 parts of nanometer titanium dioxide adjusting agent and 5.5 parts of curing agent;

[0112] Mix the epoxy resin, the modified filler, the nanometer titanium dioxide adjusting agent and the curing agent to obtain an improvement material, and coat the improvement material on the surface of the copper substrate to form the improvement layer;

[0113] Step two: uniformly blend 4 parts of a 5% sodium citrate solution, 3 parts of a 2% chitosan solution and 2 parts of silane coupling agent KH560 to obtain a treatment solution;

[0114] Step three: immerse the product of step one in a sufficient amount of the treatment solution, with an immersion pressure of 10 Mpa and an immersion time of 1 h, and then dry to obtain the circuit board of the present application.

[0115] The thickness of the improvement layer of this embodiment is 80 um, the thickness of the copper foil layer is 20 um, the epoxy resin is prepared by mixing bisphenol A type epoxy resin and phenolic epoxy resin according to a weight ratio of 2:1, and the curing agent is 2-phenylimidazole.

[0116] The preparation method of the modified filler of this embodiment is as follows:

[0117] S01: mixing silane coupling agent KH550, ethanol and water in a weight ratio of 2:5:1 to obtain a silane solution; mixing 3 parts of modified boron nitride whisker, 4 parts of the silane solution and 2 parts of urea solution to obtain a modification solution;

[0118] S02: preheating the nano-palygorskite at 64℃ for 1h, then stirring and modifying the preheated nano-palygorskite in the modification solution at 4 times the total amount of the preheated nano-palygorskite, and obtaining modified nano-palygorskite after the stirring;

[0119] S03: stirring and mixing 4 parts of glass fiber, 2.5 parts of cerium oxide and 5.5 parts of sodium silicate solution, then filtering and drying, and calcining at 160℃ for 1h to obtain a filler aid;

[0120] S04: mixing and ball-milling the modified nano-palygorskite and the filler aid in a weight ratio of 5:3, then filtering and drying to obtain a modified filler agent.

[0121] The mass fraction of the urea solution in this embodiment is 3.5%; the stirring speed of the stirring modification is 500r / min, and the stirring time is 1h.

[0122] The mass fraction of the sodium silicate solution in this embodiment is 4.5%.

[0123] The preparation method of the modified boron nitride whisker in this embodiment is as follows:

[0124] Adding 5.5 parts of boron nitride whisker, 2 parts of nano-silica sol into 6.5 parts of sodium lignosulfonate solution, then adding 2.5 parts of silicon carbide powder and 2 parts of lanthanum oxide, and then mixing and ball-milling to obtain the modified boron nitride whisker.

[0125] The mass fraction of the sodium lignosulfonate solution in this embodiment is 3.5%; the ball-milling speed of the mixing and ball-milling is 1100r / min, and the ball-milling time is 1h.

[0126] The preparation method of the nano-titanium dioxide regulator in this embodiment is as follows:

[0127] S101: stirring and mixing the nano-titanium dioxide in sufficient potassium permanganate solution, then washing with water, filtering and drying;

[0128] S102: stirring and adjusting the dried nano-titanium dioxide and the adjusting solution in a weight ratio of 2:5, then filtering and drying to obtain the nano-titanium dioxide regulator;

[0129] The preparation method of the adjusting liquid is as follows: 3 parts of hydroxyapatite, 2 parts of alginic acid and 1.5 parts of calcium stearate are added into 4.5 parts of a 5% mass fraction sodium dodecylbenzenesulfonate solution and stirred uniformly to obtain the adjusting liquid.

[0130] The stirring speed of the stirring adjusting treatment in this example is 600 r / min, and the stirring time is 1 h.

[0131] The mass fraction of the potassium permanganate solution in this example is 6%.

[0132] Comparative Example 1.

[0133] The difference between this example and Example 3 is that no modified filler agent is added.

[0134] Comparative Example 2.

[0135] The difference between this example and Example 3 is that no modified nano-palygorskite is added in the preparation of the modified filler agent.

[0136] Comparative Example 3.

[0137] The difference between this example and Example 3 is that no modifying liquid is added in the preparation of the modified nano-palygorskite.

[0138] Comparative Example 4.

[0139] The difference between this example and Example 3 is that no modified boron nitride whisker is added in the modifying liquid.

[0140] Comparative Example 5.

[0141] The difference between this example and Example 3 is that no filler aid is added in the preparation of the modified filler agent.

[0142] Comparative Example 6.

[0143] The difference between this example and Example 3 is that no glass fiber is added in the preparation of the filler aid.

[0144] Comparative Example 7.

[0145] The difference between this example and Example 3 is that no cerium oxide is added in the preparation of the filler aid.

[0146] Comparative Example 8.

[0147] The difference between this example and Example 3 is that no nano-titanium dioxide adjusting agent is added.

[0148] Comparative Example 9.

[0149] The difference between this example and Example 3 is that no adjusting liquid treatment is added in the nano-titanium dioxide adjusting agent.

[0150] Comparative Example 10.

[0151] The difference between this example and Example 3 is that no hydroxyapatite and alginic acid is added in the adjusting liquid.

[0152] The improved layer in the products of Examples 1-3 and Comparative Examples 1-10 is subjected to a conventional performance test, and the thermal conductivity, dielectric loss and wear resistance are tested, and the product stability under high heat and high humidity conditions is tested (the product is placed in a condition of 75 DEG C and humidity of 45% for 48 hours, and the performance stability of the product is tested), and the test results are as follows:

[0153]

[0154] From the Comparative Examples 1-10 and Examples 1-3 and the stability test, it can be seen that

[0155] The product of Example 3 has excellent thermal conductivity, dielectric loss and wear resistance, and the three performances can be improved coordinately, and the product stability under high heat and high humidity conditions is significantly improved, and the performance stability of the product is obviously improved;

[0156] The product performance stability is obviously deteriorated without adding the modified filler agent and the nano-titanium dioxide regulator, and the performance effect of the product is most significant when the two are coordinated and jointly effected;

[0157] The product performance is deteriorated to different degrees without adding the modified nano-attapulgite in the preparation of the modified filler agent, without adding the modified liquid in the preparation of the modified nano-attapulgite, without adding the modified boron nitride whisker in the modified liquid, without adding the filler aid in the preparation of the modified filler agent, without adding the glass fiber in the preparation of the filler aid, and without adding the cerium oxide in the preparation of the filler aid, and the performance effect of the product is most significant when the modified nano-attapulgite obtained by the specific method is used in combination with the specific filler aid, and the effect is not as obvious as that of the present application when other methods are used instead, and the present inventor has also found that the product performance is deteriorated more obviously without adding the modified boron nitride whisker in the modified liquid;

[0158] The product performance is also deteriorated without adding the adjusting liquid treatment in the nano-titanium dioxide regulator and without adding the hydroxyapatite and alginic acid in the adjusting liquid, and the performance effect of the product is most significant when the nano-titanium dioxide regulator prepared by the specific method is used.

[0159] The present application further explores the product performance through the preparation of the modified boron nitride whisker;

[0160] Experimental Example 1.

[0161] The only difference between Example 3 and the present application is that the boron nitride whisker is not added in the preparation of the modified boron nitride whisker.

[0162] Experimental Example 2.

[0163] The only difference from Example 3 is that silicon carbide powder is not added in the preparation of modified boron nitride whiskers.

[0164] Experimental Example 3.

[0165] The only difference from Example 3 is that lanthanum oxide is not added in the preparation of the modified boron nitride whiskers.

[0166] Experimental Example 4.

[0167] The only difference from Example 3 is that no nano-silica sol is added in the preparation of modified boron nitride whiskers.

[0168] Experimental Example 5.

[0169] The only difference from Example 3 is that the sodium lignin sulfonate solution is replaced by water.

[0170] Taking the product under high heat and high humidity conditions as an example, the performance test was conducted and its performance was tested as follows;

[0171]

[0172] It can be seen from Experimental Examples 1-5 that no boron nitride whiskers are added in the preparation of modified boron nitride whiskers, and the performance of the product changes under normal conditions. Among the preparation factors of modified boron nitride whiskers, the performance deterioration is the most obvious. At the same time, no silicon carbide powder is added in the preparation of modified boron nitride whiskers, and the performance of the product deteriorates most significantly under the stability test. Silicon carbide powder and boron nitride whiskers are used to assist each other in the preparation of modified boron nitride whiskers, which enhances the performance effect of the product. At the same time, no lanthanum oxide is added in the preparation of modified boron nitride whiskers, no nano-silica sol is added in the preparation of modified boron nitride whiskers, and water is used instead of sodium lignin sulfonate solution. The performance of the product has a tendency to deteriorate. Only the modified boron nitride whiskers obtained by the method of the present invention have the best product performance effect, and the conditions for adjusting the preparation of boron nitride whiskers of the present invention are unique. Modified boron nitride whiskers prepared by other methods are not as significant as those of the present invention.

[0173] It will be apparent to those skilled in the art that the present invention is not limited to the details of the exemplary embodiments described above and that the invention can be embodied in other specific forms without departing from the spirit or essential characteristics of the invention. Therefore, the embodiments should be considered in all respects as illustrative and non-restrictive, and the scope of the invention is defined by the appended claims rather than the foregoing description, and it is intended that all variations that come within the meaning and range of equivalents of the claims be embraced therein.

[0174] Furthermore, it should be understood that although the specification is described in terms of embodiments, not every embodiment includes every feature or implementation described herein. The specification can include implicit combinations of explicitly mentioned features and / or implicit combinations of implicitly mentioned features. Such combinations are also expressly included within the scope of the specification and an embodiment.

Claims

1. A method for producing a circuit board, characterized in that: The following steps are involved: Step 1: The surface of the copper substrate is sequentially provided with an improved layer and a copper foil layer, and then the substrate covered with the improved layer and the copper foil layer is subjected to hot pressing at a temperature of 180°C for 2 hours; The improved layer comprises the following raw materials in parts by weight: 50-55 parts of epoxy resin, 5-8 parts of modified filler, 4-7 parts of nano titanium dioxide regulator, and 4-7 parts of curing agent; The epoxy resin, modified filler, nano titanium dioxide regulator and curing agent are mixed thoroughly to obtain an improved material, and the improved material is coated on the surface of the copper substrate to form an improved layer; Step 2: 3-5 parts by mass of 5% sodium citrate solution, 2-4 parts by mass of 2% chitosan solution and 1-3 parts by mass of silane coupling agent KH560 are uniformly blended to obtain a treatment solution; Step 3: The product of step 1 is immersed in a sufficient amount of treatment liquid at a pressure of 10 MPa for 1 hour. After the immersion is completed, it is dried to obtain a circuit board; The preparation method of the modified filler is: S01: Silane coupling agent KH550, ethanol and water are mixed in a weight ratio of 2:5:1 to obtain silane liquid; 2-4 parts of modified boron nitride whiskers, 3-5 parts of silane solution and 1-3 parts of urea solution are uniformly mixed to obtain a modified solution; S02: preheating the nano-attapulgite at 62-66° C. for 1 hour, then stirring the preheated nano-attapulgite in a modifying liquid 3-5 times the total amount of the preheated nano-attapulgite for modification, and completing the stirring to obtain modified nano-attapulgite; S03: 3-5 parts of glass fiber, 2-3 parts of cerium oxide and 4-7 parts of sodium silicate solution are stirred and mixed thoroughly, then filtered and dried, and then calcined at 150-170°C for 1 hour. After calcination, a filler additive is obtained; S04: mixing the modified nano-attapulgite and the filler additive in a weight ratio of 5:3 and subjecting them to ball milling. After the ball milling is completed, filtering and drying are performed to obtain a modified filler; The preparation method of the modified boron nitride whisker is: Add 4-7 parts of boron nitride whiskers and 1-3 parts of nano-silica sol to 5-8 parts of sodium lignin sulfonate solution, then add 2-3 parts of silicon carbide powder and 1-3 parts of lanthanum oxide, mix well and perform ball milling. After the ball milling is completed, filter and dry to obtain modified boron nitride whiskers; The preparation method of the nano titanium dioxide regulator is: S101: Stir nano-titanium dioxide in a sufficient amount of potassium permanganate solution, then wash with water, filter and dry; S102: Stirring and conditioning the dried nano-titanium dioxide and the conditioning solution in a weight ratio of 2:

5. After stirring, filtering and drying to obtain the nano-titanium dioxide conditioning agent; The preparation method of the regulating solution is as follows: 2-4 parts of hydroxyapatite, 1-3 parts of alginic acid, and 1-2 parts of calcium stearate are added to 3-6 parts of 5% by mass sodium dodecylbenzenesulfonate solution and stirred evenly to obtain the regulating solution.

2. The method for producing a circuit board according to claim 1, wherein: The thickness of the improved layer is 80 μm; the thickness of the copper foil layer is 20 μm; the epoxy resin is prepared by mixing bisphenol A epoxy resin and novolac epoxy resin in a weight ratio of 2:1; and the curing agent is 2-phenylimidazole.

3. The method for producing a circuit board according to claim 2, wherein: The mass fraction of the urea solution is 2-5%; the stirring speed of the stirring modification treatment is 450-550 r / min, and the stirring is for 1 hour.

4. A method for producing a circuit board according to claim 3, characterized in that: The mass fraction of the sodium silicate solution is 3-6%.

5. The method for producing a circuit board according to claim 4, wherein: The mass fraction of the sodium lignin sulfonate solution is 2-5%; the ball milling speed of the mixing ball milling treatment is 1050-1150 r / min, and the ball milling is performed for 1 hour.

6. A method for producing a circuit board according to claim 5, characterized in that: The stirring speed of the stirring adjustment treatment is 550-750 r / min, and the stirring is performed for 1 hour.

7. A method for producing a circuit board according to claim 6, characterized in that: The mass fraction of the potassium permanganate solution is 5-7%.

Citation Information

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