CN108822493B - Preparation method of nano-ceramic filled PCB (printed circuit board) copper-clad plate prepreg - Google Patents
Preparation method of nano-ceramic filled PCB (printed circuit board) copper-clad plate prepreg Download PDFInfo
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- CN108822493B CN108822493B CN201810503288.2A CN201810503288A CN108822493B CN 108822493 B CN108822493 B CN 108822493B CN 201810503288 A CN201810503288 A CN 201810503288A CN 108822493 B CN108822493 B CN 108822493B
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/24—Impregnating materials with prepolymers which can be polymerised in situ, e.g. manufacture of prepregs
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2363/00—Characterised by the use of epoxy resins; Derivatives of epoxy resins
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2206—Oxides; Hydroxides of metals of calcium, strontium or barium
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2217—Oxides; Hydroxides of metals of magnesium
- C08K2003/222—Magnesia, i.e. magnesium oxide
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/003—Additives being defined by their diameter
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
Abstract
The invention discloses a preparation method of a nano-ceramic filled PCB (printed circuit board) copper-clad plate prepreg, which comprises the following steps: firstly, uniformly stirring a curing agent, an accelerator and a solvent in a certain proportion to obtain a transparent solution, then adding a resin in a certain proportion, and stirring for a period of time to completely dissolve the resin; adding SiO with the grain diameter of 1-10 nanometers2、MgO、Al2O3And CaO ceramic powder mixture, and then stirring at a high speed, so that the nano ceramic is uniformly distributed in the epoxy resin; and finally, preparing the PTFE-based PCB copper-clad plate prepreg by the steps of glass fiber cloth immersion gluing, drying and the like. According to the invention, the nano ceramic powder with a certain proportion is added into the epoxy resin, and the ceramic particles and the epoxy resin are uniformly mixed, so that the uniformity and the thermal performance of the prepreg of the copper-clad plate are greatly improved, and the prepreg has an important effect on the application of the high-frequency PCB copper-clad plate in the age of 5G.
Description
Technical Field
The invention relates to a method for preparing a nano-ceramic filled PCB (printed circuit board) copper-clad plate prepreg, belonging to the field of preparation of PCB copper-clad plates.
Background
A Printed Circuit Board (PCB) is an important electronic component, a support for an electronic component, and a carrier for electrical connection of the electronic component. With the continuous progress of the development of electronic information technology, the high frequency of electronic equipment is a development trend, and especially with the increasing development of wireless network and satellite communication, information products are continuously going to high speed and high frequency. High-frequency PCB boards are needed for developing new generation products, particularly high-frequency circuit boards are needed for communication products such as satellite systems and mobile phone receiving base stations, and with the rapid development of the applications in the next few years, a great deal of demand is needed for the high-frequency PCB boards.
The nano ceramic particles have the function of improving the thermal performance in the prepreg of the PCB copper-clad plate, and greatly expand the wind mining for the PCB copper-clad plate in the aspect of high-scattering application. In the past, the phenomena that ceramic particles are easy to distribute unevenly with epoxy resin, the ceramic particles are easy to precipitate in the stirring process and the like often exist in some PCB (printed Circuit Board) copper-clad plate prepregs filled with the ceramic particles. Therefore, the technical personnel in the field are dedicated to developing a preparation method of the nano-ceramic filled PCB copper-clad plate prepreg, and ceramic particles and epoxy resin can be uniformly mixed, so that the performance uniformity of the prepreg is greatly improved, and a foundation is laid for the higher requirement of the 5G era on the PCB.
Disclosure of Invention
The purpose of the invention is as follows: in order to overcome the defects in the prior art, the invention provides a preparation method of a nano-ceramic filled PCB (printed Circuit Board) copper-clad plate prepreg, which is characterized in that a certain proportion of nano-ceramic powder is added on the basis of the conventional preparation process of the copper-clad plate prepreg, and ceramic particles are uniformly mixed with epoxy resin, so that the uniformity and the thermal property of the copper-clad plate prepreg are greatly improved, and the foundation is laid for the higher requirement of the 5G era on a PCB.
The technical scheme is as follows: in order to achieve the purpose, the invention adopts the technical scheme that:
a preparation method of a nano-ceramic filled PCB (printed Circuit Board) copper-clad plate prepreg comprises the following steps:
s1: adding dicyandiamide serving as a curing agent and dimethyl imidazole serving as an accelerator into dimethyl amide serving as a solvent, and stirring and dissolving to obtain transparent liquid A;
s2: adding epoxy resin into the transparent liquid A, and stirring to completely dissolve the epoxy resin to obtain uniform and viscous liquid B;
s3: SiO with the grain diameter of 1-10 nanometers2、MgO、Al2O3Adding CaO powder into the liquid B, adding acetone, and stirring to obtain a uniform solution C;
s4: soaking the glass fiber cloth in the solution C for 20-30 minutes, taking out and airing in a place with good ventilation condition;
s5: putting the dried sample into an oven, and drying at 185-210 ℃ for 1-2 hours;
s6: and taking out the dried prepreg, and cutting the edge of the prepreg by using an edge cutting machine to obtain the finished product of the nano ceramic filled PCB (printed circuit board) copper-clad plate prepreg.
The working principle of the invention is as follows: the main components are epoxy resin and nano ceramic powder, and the PCB copper-clad plate prepreg is prepared by adding the nano ceramic powder into the epoxy resin (glue mixing process). The nano ceramic powder can be SiO2、MgO、Al2O3And CaO. The grain diameter of the nano ceramic powder is 1-10 nanometers.
Firstly, uniformly stirring a certain proportion of curing agent, accelerator and solvent to obtain a transparent solution, then adding a certain proportion of resin, and stirring for a period of time to completely dissolve the resin. Finally, a certain amount of nano ceramic powder is added and stirred at a certain rotating speed until the nano ceramic powder is uniformly dispersed. The invention mainly aims to add nano ceramic powder on the basis of preparing the copper-clad plate, and adjust the thermal property of the copper-clad plate through the nano ceramic powder.
A large amount of experimental data show that the thermal performance of the copper-clad plate can be greatly improved by adding the nano ceramic powder into the epoxy resin.
Further, the ingredients of the components have the following proportions: 100 parts of epoxy resin, 0.5-0.9 part of dicyandiamide curing agent, 0.1-0.6 part of dimethyl imidazole accelerator, 2-3 parts of dimethyl amide solvent and 1-2 parts of SiO2Powder, 0.8-1 part of MgO powder and 0.5-0.7 part of Al2O3Powder, 0.1-0.3 part of CaO powder and 5-7 parts of acetone.
Further, in the step S1, the transparent liquid A is obtained by stirring at a speed of 100-200 rpm for 3-5 minutes.
Further, in the step S2, the liquid B is stirred at a speed of 100-200 rpm for 30-60 minutes to obtain a uniform viscous liquid B.
Further, in the step S3, stirring is performed at a speed of 800-.
Has the advantages that: compared with the prior art, the preparation method of the nano-ceramic filled PCB (printed Circuit Board) copper-clad plate prepreg provided by the invention has the following advantages: (1) the manufacturing process is simple, the cost is low, the operation period is short, the repeatability is good, and the method is suitable for mass production; (2) by adding the ceramic nano powder into the common epoxy copper-clad plate prepreg and uniformly mixing the ceramic particles and the epoxy resin, the uniformity and the thermal performance of the copper-clad plate prepreg are greatly improved, and a foundation is laid for the higher requirement of the 5G era on the PCB.
Detailed Description
The present invention will be further described with reference to the following examples.
Example 1:
the specific implementation steps are as follows:
s1: weighing 100 parts of epoxy resin, then weighing 0.6 part of curing agent dicyandiamide, 0.2 part of accelerator dimethylimidazole, 2 parts of solvent dimethylamide and preparing 5 parts of acetone;
s2: putting the weighed curing agent and the weighed accelerating agent into a solvent, and stirring for 3 minutes at the speed of 150 revolutions per minute to dissolve the curing agent and the accelerating agent into transparent liquid A;
s3: putting the weighed epoxy resin into the transparent liquid A, and stirring for 30 minutes at the speed of 150 revolutions per minute to completely dissolve the epoxy resin to obtain uniform and viscous liquid B;
s4: the grain diameter is 3 nanometers, and the proportion is 1 part of SiO respectively20.8 part of MgO and 0.5 part of Al2O3And 0.1 part of CaO to the liquid B, 5 parts of acetone, and then 800 revolutionsStirring for 2 hours at a speed of every minute to obtain a uniform solution C;
s5: soaking the glass fiber cloth in the solution C for 20 minutes, taking out, and drying in a place with good ventilation condition;
s6: the dried sample was placed in an oven and baked at 185 ℃ for 2 hours.
S7: and taking out the dried prepreg, and cutting the edge of the prepreg by using an edge cutting machine to obtain the finished product of the PCB copper-clad plate prepreg filled with the nano ceramics.
The Z-direction thermal conductivity of the prepreg obtained in example 1 was 2.4W/(mK), the in-plane thermal conductivity was 3.6W/(mK), the glass transition temperature was 175 ℃ and the cracking temperature was 358 ℃. All thermal properties are obviously higher than those of a common FR-4 copper-clad plate.
Example 2:
the specific implementation steps are as follows:
s1: weighing 100 parts of epoxy resin, then weighing 0.9 part of curing agent dicyandiamide, 0.6 part of accelerator dimethylimidazole, 3 parts of solvent dimethylamide and preparing 7 parts of acetone;
s2: putting the weighed curing agent and the weighed accelerating agent into a solvent, and stirring for 4 minutes at the speed of 200 revolutions per minute to dissolve the curing agent and the accelerating agent into transparent liquid A;
s3: putting the weighed epoxy resin into the transparent liquid A, and stirring for 30 minutes at the speed of 200 revolutions per minute to completely dissolve the epoxy resin to obtain uniform and viscous liquid B;
s4: the grain diameter is 5 nanometers, the proportion is 1 part of SiO respectively21 part of MgO and 0.6 part of Al2O3And 0.2 part of CaO is added into the liquid B, 7 parts of acetone is added, and then the mixture is stirred for 3 hours at the speed of 1000 revolutions per minute to obtain a uniform solution C;
s5: soaking the glass fiber cloth in the solution C for 30 minutes, taking out, and drying in a place with good ventilation condition;
s6: the dried sample was placed in an oven and baked at 210 ℃ for 1 hour.
S7: and taking out the dried prepreg, and cutting the edge of the prepreg by using an edge cutting machine to obtain the finished product of the PCB copper-clad plate prepreg filled with the nano ceramics.
The Z-direction thermal conductivity of the prepreg obtained in example 2 above can reach 2.5W/(mK), the in-plane thermal conductivity can reach 3.7W/(mK), the glass transition temperature is 170 ℃ and the cracking temperature is 355 ℃. All thermal properties are obviously higher than those of a common FR-4 copper-clad plate.
In addition, a large amount of experimental data show that the thermal performance of the copper-clad plate can be greatly improved by adding the ceramic nano powder into the epoxy resin, and a foundation is laid for the higher requirement of the 5G era on the PCB.
The above description is only of the preferred embodiments of the present invention, and it should be noted that: it will be apparent to those skilled in the art that various modifications and adaptations can be made without departing from the principles of the invention and these are intended to be within the scope of the invention.
Claims (4)
1. A preparation method of a nano-ceramic filled PCB (printed Circuit Board) copper-clad plate prepreg is characterized by comprising the following steps:
s1: adding dicyandiamide serving as a curing agent and dimethyl imidazole serving as an accelerator into dimethyl amide serving as a solvent, and stirring and dissolving to obtain transparent liquid A;
s2: adding epoxy resin into the transparent liquid A, and stirring to completely dissolve the epoxy resin to obtain uniform and viscous liquid B;
s3: SiO with the grain diameter of 1-10 nanometers2、MgO、Al2O3Adding CaO powder into the liquid B, adding acetone, and stirring to obtain a uniform solution C;
s4: soaking the glass fiber cloth in the solution C for 20-30 minutes, taking out and airing in a place with good ventilation condition;
s5: putting the dried sample into an oven, and drying at 185-210 ℃ for 1-2 hours;
s6: taking out the dried prepreg, and cutting the edge of the prepreg by using an edge cutting machine to obtain a finished product of the nano ceramic filled PCB (printed circuit board) copper-clad plate prepreg;
the ingredients of the components are as follows: 100 portions of epoxy resin, 0.5 to 0.9 portion of curing agent dicyandiamide, 0.1 to 0.6 portion2-3 parts of solvent dimethyl amide, 1-2 parts of SiO2Powder, 0.8-1 part of MgO powder and 0.5-0.7 part of Al2O3Powder, 0.1-0.3 part of CaO powder and 5-7 parts of acetone.
2. The method for preparing the nano-ceramic-filled PCB copper-clad plate prepreg according to claim 1, wherein in the step S1, the stirring is carried out at a speed of 100-200 rpm for 3-5 minutes to obtain the transparent liquid A.
3. The method for preparing the nano-ceramic-filled PCB copper-clad plate prepreg according to claim 1, wherein in the step S2, the mixture is stirred at a speed of 100-200 rpm for 30-60 minutes to obtain the uniform viscous liquid B.
4. The method for preparing the nano-ceramic-filled PCB copper-clad plate prepreg according to claim 1, wherein in the step S3, the solution C is stirred at the speed of 800-1000 rpm for 2-5 hours to obtain a uniform solution C.
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| CN201810503288.2A CN108822493B (en) | 2018-05-23 | 2018-05-23 | Preparation method of nano-ceramic filled PCB (printed circuit board) copper-clad plate prepreg |
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| CN108822493B true CN108822493B (en) | 2020-06-16 |
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104363697A (en) * | 2014-10-16 | 2015-02-18 | 金壬海 | Copper-clad plate with aluminum substrate and media filled with ceramics and method for manufacturing copper-clad plate |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104363697A (en) * | 2014-10-16 | 2015-02-18 | 金壬海 | Copper-clad plate with aluminum substrate and media filled with ceramics and method for manufacturing copper-clad plate |
Non-Patent Citations (3)
| Title |
|---|
| "Develop ment of Epoxy-M atrix Composite with Both High-Ther mal Conductivity and Low-Dielectric Constant via Hybrid Filler Systems";K C Yung et al.;《Journal of Applied Polymer Science》;20100405;第116卷(第1期);第518–527页 * |
| "Study on the Properties of the Epoxy-Matrix Composites Filled with Thermally Conductive AlN and BN Ceramic Particles";B. L. Zhu et al.;《Journal of Applied Polymer Science》;20100629;第118卷(第5期);第2754–2764页 * |
| "Thermal Conductivity, Elastic Modulus, and Coefficient of Thermal Expansion of Polymer Composites Filled with Ceramic Particles for Electronic Packaging";C. P. WONG et al.;《Journal of Applied Polymer Science》;19991227;第74卷(第14期);第3396–3403 页 * |
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