Preparation method of high-thermal-conductivity FR4 copper-clad plate

Abstract

The application relates to a preparation method of a high-thermal-conductivity FR4 copper-clad plate, and belongs to the technical field of copper-clad plate preparation. Raw materials include resin, curing agent, coupling agent, catalyst, filler and solvent; the resin includes naphthalene type epoxy resin and benzocyclobutene resin; the application uses naphthalene type epoxy resin as the main body resin, adds benzocyclobutene resin, increases the thermal conductivity of the copper-clad plate by increasing the proportion of the resin and reducing the proportion of the filler, the copper-clad plate prepared by the application has the properties of heat resistance of 288 DEG C for 10 min or more, thermal conductivity of 3 W / m*K or more, water absorption of 0.15% or less, peeling strength of 1.0 N / mm or more and flame-retardant level of FV-0 grade.

Description

TECHNICAL FIELD

[0001] The application relates to a preparation method of a high-thermal-conductivity FR4 copper-clad plate and belongs to the technical field of copper-clad plate preparation. BACKGROUND

[0002] With the rapid development of the information age, the development of industrial technology and the improvement of people's living standards, the market has higher requirements for higher performance and miniaturization of industrial electronic power products and consumer products, and the requirement for the thermal conductivity of the copper-clad plate is higher and higher. Due to overexploitation, the global energy shortage and global environmental changes are threatening, and a new type of LED light source with energy-saving function becomes a new topic. The most important problem of LED is the heat dissipation problem, and a PCB with good thermal conductivity is required, and then a copper-clad plate with high thermal conductivity is required. SUMMARY

[0003] The purpose of the application is to provide a new technical solution to improve or solve the technical problems existing in the prior art as described above.

[0004] The technical scheme provided by the application is as follows: a preparation method of a high-thermal-conductivity FR4 copper-clad plate, raw materials including resin, curing agent, coupling agent, catalyst, filler and solvent; the resin includes naphthalene type epoxy resin and benzocyclobutene resin.

[0005] On the basis of the above technical scheme, the application can also be improved as follows.

[0006] Further, the curing agent is dicyandiamide; the coupling agent is a titanate coupling agent; the catalyst is a platinum catalyst; the filler includes spherical zinc oxide, silicon carbide and hexagonal boron nitride nanosheet; and the solvent includes any one or a combination of two or more of acetone, butanone and dimethylformamide.

[0007] Further, the method comprises the following steps:

[0008] (1) 2-4 parts of the curing agent dicyandiamide, 8-13 parts of the acetone solvent and 8-13 parts of the butanone solvent are added to a container in parts by weight and stirred to make them fully dissolved;

[0009] (2) 0.06-0.12 parts of the platinum catalyst, 70-89 parts of the naphthalene type epoxy resin, 28-30 parts of the benzocyclobutene resin and 0.2-0.26 parts of the titanate coupling agent are added to the mixed solution of step (1) in parts by weight and stirred to make them fully dissolved;

[0010] (3) 15-20 parts of the hexagonal boron nitride nanosheet, 5-10 parts of the spherical zinc oxide and 3-5 parts of the silicon carbide filler are added to the mixed solution of step (2) in parts by weight and stirred uniformly to make them fully emulsified;

[0011] (4) adding 10-13 parts of dimethylformamide solvent into the mixture of step (3) to adjust the viscosity to 18-21 s, and obtaining the glue solution after gelation;

[0012] (5) completely and uniformly infiltrating the glass fiber cloth with the glue solution obtained in step (4) to obtain a prepreg;

[0013] (6) laminating the copper foil on the prepreg obtained in step (5) to obtain a high-thermal-conductivity FR4 copper-clad plate.

[0014] Further, in step (4), the gelation time is 260-280 s.

[0015] Further, in step (5), the prepreg is baked in an oven at 170-190 DEG C for 3-5 min.

[0016] Further, the gelation time of the prepreg is 100-115 s, and the glue content is 47-52%.

[0017] Further, in step (6), the obtained prepreg is laminated, and the copper foil is laminated on both sides of the prepreg, and the prepreg is hot-pressed in a vacuum press under the conditions of a pressure of 7-20 MPa and a temperature of 160-210 DEG C for 2-3 h, and the temperature is kept for 1.5-2.5 h to obtain a high-thermal-conductivity FR4 copper-clad plate.

[0018] Compared with the prior art, the technical scheme provided by the application has the following beneficial effects:

[0019] The application uses naphthalene type epoxy resin as the main resin, adds benzocyclobutene resin, increases the thermal conductivity of the copper-clad plate by increasing the ratio of the resin and reducing the ratio of the filler, the copper-clad plate prepared by the application has a heat resistance of ≥10 min at 288 DEG C, a thermal conductivity of ≥3 W / m·K, a water absorption of ≤0.15%, a peel strength of >1.0 N / mm, and a flame-retardant level of FV-0. DETAILED DESCRIPTION

[0020] The principles and characteristics of the application are described below in combination with examples, and the examples are only used to explain the application and not to limit the scope of the application.

[0021] Example 1

[0022] A preparation method of a high-thermal-conductivity FR4 copper-clad plate includes the following steps:

[0023] (1) at room temperature, 2 parts of dicyandiamide, 8 parts of acetone solvent and 8 parts of butanone solvent are added into a container and stirred to make them fully dissolved;

[0024] (2) At room temperature, 0.06 parts of platinum catalyst, 70 parts of naphthalene type epoxy resin, 28 parts of benzocyclobutene resin, 0.2 parts of titanate coupling agent are added into the mixed solution of step (1) to stir and make it fully dissolved;

[0025] (3) 15 parts of hexagonal boron nitride nanosheet, 5 parts of spherical zinc oxide, 3 parts of silicon carbide are added into the mixed solution of step (2) and stirred uniformly to fully emulsify;

[0026] (4) 10 parts of dimethylformamide solvent are added into the mixed solution of step (3) to stir uniformly, the viscosity is adjusted to 20s, and the glue solution is obtained, the glue solution gelation time is 275s;

[0027] (5) The glue solution obtained in step (4) is completely and uniformly infiltrated into the glass fiber cloth, and the glass fiber cloth is baked in a 180℃ oven for 5min to obtain a PP with uniform appearance, the PP gelation time is controlled to 112s, and the glue content is 51%;

[0028] (6) The PP prepared in step (5) is stacked according to the requirement, 18 microns of copper foil is covered on both sides, and is hot-pressed in a vacuum press under the conditions of pressure 7MPa and temperature 160℃ for 1.5h, and then hot-pressed under the conditions of pressure 20MPa and temperature 210℃ for 1h, and the temperature is kept for 2h to obtain a high thermal conductivity FR4 copper-clad plate.

[0029] Example 2

[0030] A preparation method of a high thermal conductivity FR4 copper-clad plate, comprising the following steps:

[0031] (1) At room temperature, 3 parts of dicyandiamide, 11 parts of acetone solvent and 11 parts of butanone solvent are added into a container to stir and make it fully dissolved;

[0032] (2) At room temperature, 0.10 parts of platinum catalyst, 78 parts of naphthalene type epoxy resin, 29 parts of benzocyclobutene resin, 0.24 parts of titanate coupling agent are added into the mixed solution of step (1) to stir and make it fully dissolved;

[0033] (3) 17 parts of hexagonal boron nitride nanosheet, 7 parts of spherical zinc oxide powder, 4 parts of silicon carbide are added into the mixed solution of step (2) and stirred uniformly to fully emulsify;

[0034] (4) 11 parts of dimethylformamide solvent are added into the mixed solution of step (3) to stir uniformly, the viscosity is adjusted to 20s, and the glue solution is obtained, the glue solution gelation time is 271s;

[0035] (5) The adhesive solution obtained in step (4) is completely and uniformly infiltrated into the glass fiber cloth, and is baked in a 180°C oven for 4.5 min to obtain a PP with uniform appearance, a controlled PP gelation time of 115 s, and a glue content of 50%;

[0036] (6) The PP prepared in step (5) is stacked according to requirements, 6 pieces are obtained, and 18 microns of copper foil is covered on both sides. Hot pressing is carried out in a vacuum press under the conditions of a pressure of 7 MPa and a temperature of 160°C for 1.5 h, and then hot pressing is carried out under the conditions of a pressure of 20 MPa and a temperature of 210°C for 1 h, and the temperature is kept for 2 h to obtain a high-thermal-conductivity FR4 copper-clad plate.

[0037] Example 3

[0038] A preparation method of a high-thermal-conductivity FR4 copper-clad plate comprises the following steps:

[0039] (1) At room temperature, 4 parts of dicyandiamide, 11 parts of acetone solvent, and 11 parts of butanone solvent are added to a container and stirred to make them fully dissolved;

[0040] (2) At room temperature, 0.10 parts of platinum catalyst, 89 parts of naphthalene type epoxy resin, 30 parts of benzocyclobutene, and 0.26 parts of titanate coupling agent are added to the mixed solution of step (1) and stirred to make them fully dissolved;

[0041] (3) 20 parts of hexagonal boron nitride nanosheet, 10 parts of spherical zinc oxide, and 5 parts of silicon carbide are added to the mixed solution of step (2) and stirred uniformly and fully emulsified;

[0042] (4) 13 parts of dimethylformamide solvent are added to the mixed solution of step (3) and stirred uniformly to adjust the viscosity to 20 s to obtain an adhesive solution, and the adhesive solution has a gelation time of 263 s;

[0043] (5) The adhesive solution obtained in step (4) is completely and uniformly infiltrated into the glass fiber cloth, and is baked in a 180°C oven for 4.5 min to obtain a PP with uniform appearance, a controlled PP gelation time of 115 s, and a glue content of 50%;

[0044] (6) The PP prepared in step (5) is stacked according to requirements, 6 pieces are obtained, and 18 microns of copper foil is covered on both sides. Hot pressing is carried out in a vacuum press under the conditions of a pressure of 7 MPa and a temperature of 160°C for 1.5 h, and then hot pressing is carried out under the conditions of a pressure of 20 MPa and a temperature of 210°C for 1 h, and the temperature is kept for 2 h to obtain a high-thermal-conductivity FR4 copper-clad plate.

[0045] Comparative Example 1

[0046] A preparation method of an FR4 copper-clad plate comprises the following steps:

[0047] (1) The components of the glue solution are weighed by weight parts: 89 parts of bisphenol A type epoxy resin, 30 parts of benzocyclobutene resin, 4 parts of dicyandiamide, 11 parts of acetone solvent, 11 parts of acetone solvent, 0.10 parts of platinum catalyst, 20 parts of hexagonal boron nitride nanosheet, 5 parts of silicon carbide, 10 parts of spherical zinc oxide, are fully mixed and stirred uniformly to obtain a glue solution;

[0048] (2) The glue solution obtained in step (1) is completely and uniformly infiltrated into the glass fiber cloth, and is baked in a 200°C oven for 6 min to obtain a PP with a glue content of 60%;

[0049] (3) The PP prepared in step (2) is stacked by 2, and the two sides are covered with 18 micron copper foil. Hot pressing is carried out in a vacuum press under the conditions of pressure 5.5 MPa and temperature 230°C for 3h, and heat preservation for 2h to obtain a copper-clad plate.

[0050] Comparative Example 2

[0051] A preparation method of an FR4 copper-clad plate, comprising the following steps:

[0052] (1) 93 parts of naphthalene type epoxy resin, 25 parts of benzocyclobutene resin, 5 parts of dicyandiamide, 20 parts of acetone solvent, 14 parts of acetone solvent, 0.13 parts of platinum catalyst, 13 parts of hexagonal boron nitride nanosheet, 6 parts of silicon carbide, 11 parts of spherical zinc oxide, are fully mixed and stirred uniformly to obtain a glue solution;

[0053] (2) The glue solution obtained in step (1) is completely and uniformly infiltrated into the glass fiber cloth, and is baked in a 200°C oven for 6 min to obtain a PP with a glue content of 60%;

[0054] (3) The PP prepared in step (2) is stacked by 2, and the two sides are covered with 18 micron copper foil. Hot pressing is carried out in a vacuum press under the conditions of pressure 5.5 MPa and temperature 230°C for 3h, and heat preservation for 2h to obtain a copper-clad plate.

[0055] Test method explanation:

[0056] (1) Water absorption rate (%) : GB / T 4722-2017-9.2;

[0057] (2) Heat resistance: GB / T 4722-2017-6.11;

[0058] (3) Peel strength (N / mm): GB / T 4722-2017-7.2.1;

[0059] (4) Flame retardancy: GB / T 4722-2017-6.4.1;

[0060] (5) Thermal conductivity: GB / T 4722-2017-7.3

[0061] The test data of the examples and the comparative examples are shown in Table 1.

[0062] Table 1: Test data of the examples and the comparative examples

[0063]

[0064] As can be seen from the test data in Table 1, the copper-clad plate of the examples has heat resistance (288℃) ≥ 10 min, thermal conductivity ≥ 3 W / m·K, water absorption rate (%) ≤ 0.15, peel strength > 1.0 N / mm, and flame retardance reaching FV-0 level.

[0065] Compared with the comparative examples 1-2, the thermal conductivity, heat resistance time and peel strength of the examples 1-3 are obviously increased, the water absorption rate is reduced, the flame retardance reaches FV-0 level, which is higher than the FV-1 level of the comparative examples 1-2. Therefore, the copper-clad plate prepared by the present application has higher thermal conductivity and other performances are not reduced, and the cost is lower, which provides another possibility for the preparation of high-thermal-conductivity FR4 copper-clad plate.

[0066] The above description is only the preferred embodiments of the present application, and is not intended to limit the present application. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present application shall be included in the protection scope of the present application.

Claims

1. A method for preparing a high thermal conductivity FR4 copper-clad plate, characterized in that, The raw materials include resin, curing agent, coupling agent, catalyst, filler and solvent; the resin includes naphthalene type epoxy resin and benzocyclobutene resin; The curing agent is dicyandiamide; the coupling agent is titanate coupling agent; the catalyst is platinum catalyst; the filler includes spherical zinc oxide, silicon carbide and hexagonal boron nitride nanosheet; The preparation method of the high-thermal-conductivity FR4 copper-clad plate comprises the following steps: (1) 2-4 parts of curing agent dicyandiamide, 8-13 parts of acetone solvent and 8-13 parts of butanone solvent are added into a container and stirred to make them fully dissolved, with the parts by weight; (2) 0.06-0.12 parts of platinum catalyst, 70-89 parts of naphthalene type epoxy resin and 28-30 parts of benzocyclobutene resin, 0.2-0.26 parts of titanate coupling agent are added into the mixed solution in step (1) and stirred to make them fully dissolved, with the parts by weight; (3) 15-20 parts of hexagonal boron nitride nanosheet, 5-10 parts of spherical zinc oxide and 3-5 parts of silicon carbide filler are added into the mixed solution in step (2) and stirred uniformly to make them fully emulsified, with the parts by weight; (4) 10-13 parts of dimethylformamide solvent is added into the mixed solution in step (3) to adjust the viscosity to 18-21 s, and the glue solution is obtained after gelation, with the parts by weight; (5) the glue solution obtained in step (4) is completely and uniformly infiltrated into the glass fiber cloth to prepare a prepreg; (6) the prepreg prepared in step (5) is covered with copper foil and pressed to obtain a high-thermal-conductivity FR4 copper-clad plate.

2. The method for preparing a high thermal conductivity FR4 copper-clad laminate according to claim 1, characterized in that, In step (4), the gelation time is 260-280 s.

3. The method for preparing a high thermal conductivity FR4 copper-clad laminate according to claim 1, characterized in that, In step (5), the prepared prepreg is baked in a 170-190℃ oven for 3-5 min.

4. The method for preparing the high thermal conductivity FR4 copper-clad laminate according to claim 3, characterized in that, The glue content of the prepreg is 47-52%.

5. The method for preparing a high thermal conductivity FR4 copper-clad laminate according to claim 1, characterized in that, In step (6), the obtained prepreg is stacked and covered with copper foil on both sides, and is hot-pressed in a vacuum press under the conditions of a pressure of 7-20 MPa and a temperature of 160-210℃ for 2-3 h and heat preservation for 1.5-2.5 h to obtain a high-thermal-conductivity FR4 copper-clad plate.

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