CN110039851B - Preparation method of polytetrafluoroethylene copper-clad plate - Google Patents
Preparation method of polytetrafluoroethylene copper-clad plate Download PDFInfo
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Abstract
The invention discloses a preparation method of a polytetrafluoroethylene copper-clad plate. The method comprises the following steps: 1. uniformly mixing the raw material components including polytetrafluoroethylene powder, a lubricant, ceramic powder and short glass fibers, and curing; 2. molding to obtain a preform; 3. obtaining a raw substrate through calendering, and then drying; 4. covering copper foils on two sides of the raw substrate, sintering, and cooling to room temperature after pressure maintaining to obtain the polytetrafluoroethylene copper-clad plate. The invention replaces the preparation method of sizing and dipping by PTFE dispersion liquid, avoids the harm of toxic fluoride, nitrogen oxide and the like, and has good filler dispersion effect, uniform mixing and good product size stability. Through reasonable proportioning, the prepared PTFE copper-clad plate has different dielectric constants of 2.6-8.6MHz, a dielectric loss factor less than or equal to 0.003, a peel strength more than or equal to 1.7kN/m, and comprehensive performance meeting the use requirement. The invention has simple process and meets the requirement of industrialized mass production.
Description
Technical Field
The invention relates to a preparation process of a copper-clad plate, in particular to a preparation method of a polytetrafluoroethylene copper-clad plate, namely a high-frequency microwave copper-clad plate, wherein the prepared polytetrafluoroethylene copper-clad plate meets the use requirement of a high-frequency microwave circuit board.
Background
The polytetrafluoroethylene (PTFE for short) material has excellent dielectric properties (lower dielectric constant, dielectric loss and the like), and good chemical stability and thermal stability. With the development of communication and electronic products towards high frequency and high speed, the market demand of the PTFE copper-clad plate is rapidly increased, and the PTFE copper-clad plate is widely applied to the manufacturing industries of communication equipment, computers, automotive electronics, household appliances and the like. In the high-frequency substrate industry, the dielectric constant, dielectric loss, water absorption and frequency characteristics of the PTFE copper-clad plate are all the best.
The traditional preparation method of the PTFE copper-clad plate comprises the steps of soaking glass fiber cloth with PTFE emulsion, drying the glass fiber cloth at the temperature of about 100 ℃, stacking a plurality of pieces of PTFE soaked cloth, and sintering a copper-clad foil to obtain the PTFE copper-clad plate. Due to the characteristics of PTFE resin, such as insolubility, self-lubrication, inadhesion and the like, the PTFE varnished cloth with proper resin content can be prepared by repeating the steps for many times, so that flow marks formed by vertical flow of different dipping times exist on the surface of the rubberized cloth, the local characteristic uniformity fluctuation of the plate is large, and the PTFE varnished plate with excellent comprehensive performance is very unfavorable for preparing the PTFE copper-clad plate. The production method has high energy consumption and low efficiency, and the prepared PTFE copper-clad plate has large thermal expansion coefficient, high dielectric loss and poor mechanical property, and a large amount of toxic substances exist in the preparation process, thereby causing serious damage to the environment.
Chinese patent application publication No. CN106494036A proposes a method for manufacturing a PTFE copper-clad plate by directly laminating a PTFE film and glass cloth, but in the method, the fluorine resin does not flow basically and cannot fill the gaps of the glass cloth, so that the performance and the uniformity of the plate are influenced; in addition, the glass cloth is easy to deform during operation and lamination, which affects the dimensional stability of the plate.
Disclosure of Invention
In view of the problems and defects in the prior art, the invention aims to provide a method for manufacturing a PTFE copper-clad plate, the comprehensive performance of the manufactured PTFE copper-clad plate meets the use requirement, the product has good dimensional stability, and toxic and harmful substances are avoided in the production process. The invention has simple process and is easy for continuous large-scale production.
The technical scheme adopted by the invention is as follows: a preparation method of a polytetrafluoroethylene copper-clad plate is characterized by comprising the following steps:
step (1): putting raw material components including polytetrafluoroethylene powder, a lubricant, ceramic powder and short glass fibers into a V-shaped mixer for uniform mixing; then the evenly mixed powder is put at a certain temperature for curing.
Step (2): and (3) filling the uniformly mixed powder obtained in the step (1) into a die cavity of a die to be pressed to obtain a pre-formed blank.
And (3): and (3) rolling the preform obtained in the step (2) to obtain a green chip with a preset thickness, and drying to remove the lubricant.
And (4): covering copper foils on two sides of the raw substrate dried in the step (3), then sintering, and cooling to room temperature after pressure maintaining to obtain the polytetrafluoroethylene copper-clad plate.
In the step (1), the raw material components are as follows according to the weight portion: 30-50 parts of polytetrafluoroethylene powder, 15-20 parts of lubricant, 40-70 parts of ceramic powder and 1-10 parts of short glass fiber.
In the step (1), the curing temperature of the uniformly mixed powder is 35-50 ℃, and the curing time is 4-8 hours.
In the step (2), the preform is molded to obtain a preform having a pressure of 5 to 35kgf/cm2And maintaining the pressure for 2-15 min.
In the step (4) of sintering, the pressure is maintained in a hot press for 4-8 hours under the conditions that the sintering temperature is set to be 360-400 ℃, the pressure is 5-20 Mpa and the vacuum degree is- (90-100) Kpa, and then the temperature is slowly maintained and cooled to the room temperature at the cooling speed of 1.5-2.5 ℃/min.
In the step (4), copper foils are covered on two sides of the green chip, and the thickness of the copper layers is 10-50 μm.
The lubricant is one of solvent oil, petroleum ether and paraffin oil.
The ceramic powder is one of silicon dioxide, aluminum oxide, aluminum nitride, magnesium oxide, calcium carbonate and titanium dioxide.
The particle size of the ceramic powder is 5-20 microns.
The beneficial effects produced by the invention are as follows:
1. under the condition of excellent electrical property and physical property of PTFE, the ceramic powder and the glass fiber powder are added, so that the dielectric constant and the strength can be increased, the heat resistance is improved, lower dielectric loss is obtained, the defects of large thermal expansion coefficient, soft texture, poor mechanical property and the like of PTFE are made up, and the reliability and the stability of the PTFE copper-clad plate are greatly improved.
2. The invention improves the distribution uniformity of PTFE in the plate, and achieves that the DK value is improved to +/-0.04% from +/-2-3% of the common level in the working process.
3. In the pressing process of the copper-clad plate, parameters such as heating speed, pressure maintaining pressure, pressure maintaining time and the like are reasonably set and controlled, so that the qualified PTFE copper-clad plate is ensured. The slow cooling, pressure maintaining and cooling are used for improving the dimensional stability of the product and the adhesive force between the resin and the composite material.
4. The invention does not adopt a gluing and dipping mode, does not have the harm of toxic fluoride, nitric oxide and the like to the environment in the production process of the PTFE copper-clad plate, and meets the requirement of the production process to the process environment; the product surface defect caused by vertical flow of different dipping times is avoided without adopting a gluing dipping mode, and the requirement of the uniformity of the plate is met.
5. The invention has simple processing process and is beneficial to industrialized continuous production.
Detailed Description
The present invention will be described in detail with reference to specific examples.
Example 1:
step (1): according to the parts by weight, 55 parts of PTFE powder, 20 parts of lubricant petroleum ether and 5 mu m of ceramic powder TiO2Putting 44 parts of titanium dioxide and 1 part of short glass fiber into a V-shaped mixer and uniformly mixing; and curing the uniformly mixed powder at the temperature of 35 ℃ for 8 hours to ensure that the lubricant is fully absorbed by the resin and is uniformly distributed in the whole resin system.
Step (2): filling the uniform powder prepared in the step (1) into a die cavity of a die to be pressed to obtain a preform; set the pressure at 20kgf/cm2And keeping the pressure for 5 min.
And (3): performing rolling on the preform obtained in the step (2) to obtain a green chip, wherein the rolling pressure is 490N, the roller linear speed is 0.5m/min, and the roller gap is 990 mu m; and then the raw substrate is put into an oven to be dried to remove the lubricant, wherein the temperature of the oven is 310 ℃, and the time is 6 hours.
And (4): and (4) covering copper foils on two sides of the raw substrate dried in the step (3), and sintering to obtain the PTFE copper-clad plate. Wherein the thickness of the copper foil is 38 mu m, the pressure is maintained for 6 hours in a hot press under the conditions that the sintering temperature is 380 ℃, the pressure is 15Mpa and the vacuum degree is-100 Kpa, and then the temperature is reduced at the speed of 2 ℃/min, the pressure is slowly maintained and the temperature is cooled to the room temperature, thus obtaining the polytetrafluoroethylene copper-clad plate.
Through detection, the main performance indexes of the prepared PTFE copper-clad plate are as follows: at normal temperature, the dielectric constant is 6.25 MHz; the peel strength is 2.4 kN/m; water absorption of 0.01%; the copper foil has no phenomena of edge warping and falling off.
Example 2:
step (1): according to the parts by weight, 55 parts of PTFE powder, 20 parts of lubricant petroleum ether and 15 mu m of ceramic powder SiO2Putting 44 parts of (silicon dioxide) and 1 part of short glass fiber into a V-shaped mixer and uniformly mixing; and curing the uniformly mixed powder at the temperature of 40 ℃ for 6 hours to ensure that the lubricant is fully absorbed by the resin and is uniformly distributed in the whole resin system.
Step (2): filling the uniform powder prepared in the step (1) into a die cavity of a die to be pressed to obtain a preform; set the pressure at 20kgf/cm2And keeping the pressure for 5 min.
And (3): performing rolling on the preform obtained in the step (2) to obtain a green chip, wherein the rolling pressure is 490N, the roller linear speed is 0.5m/min, and the roller gap is 990 mu m;
and then the raw substrate is put into an oven to be dried to remove the lubricant, wherein the temperature of the oven is 310 ℃, and the time is 6 hours.
And (4): and (3) covering copper foils on two sides of the dried raw substrate in the step (3), and sintering to obtain the PTFE copper-clad plate. Wherein the thickness of the copper foil is 38 mu m, the pressure is maintained for 6 hours in a hot press under the conditions that the sintering temperature is 380 ℃, the pressure is 15Mpa and the vacuum degree is-100 Kpa, and then the temperature is slowly maintained and cooled to the room temperature at the cooling speed of 2 ℃/min, thus obtaining the polytetrafluoroethylene copper-clad plate.
Through detection, the main performance indexes of the prepared PTFE copper-clad plate are as follows: at normal temperature, the dielectric constant is 2.67 MHz; the peel strength is 2.2 kN/m; water absorption of 0.02%; the copper foil has no phenomena of edge warping and falling off.
Example 3:
step (1): according to the parts by weight, 35 parts of PTFE powder, 20 parts of lubricant paraffin oil and 20 mu m of ceramic powder SiO2Putting 60 parts of (silicon dioxide) and 5 parts of short glass fiber into a V-shaped mixer to be uniformly mixed; and curing the uniformly mixed powder at the temperature of 45 ℃ for 5 hours to ensure that the lubricant is fully absorbed by the resin and is uniformly distributed in the whole resin system.
Step (2): filling the uniform powder prepared in the step (1) into a die cavity of a die to be pressed to obtain a preform; set the pressure at 20kgf/cm2And keeping the pressure for 5 min.
And (3): carrying out rolling on the preform obtained in the step (2) to obtain a green chip, wherein the rolling pressure is 490N, the roll linear speed is 0.5m/min, and the roll gap is 990 mu m;
and then the raw substrate is put into an oven to be dried to remove the lubricant, wherein the temperature of the oven is 310 ℃, and the time is 6 hours.
And (4): and (4) covering copper foils on two sides of the dried raw substrate in the step (3), and sintering to obtain the PTFE copper-clad plate. Wherein the thickness of the copper foil is 18 μm, the pressure is maintained for 6 hours in a hot press under the conditions that the sintering temperature is 380 ℃, the pressure is 15Mpa and the vacuum degree is-100 Kpa, and then the temperature is reduced at the speed of 2 ℃/min, the pressure is slowly maintained and the temperature is cooled to the room temperature, thus obtaining the polytetrafluoroethylene copper-clad plate.
Through detection, the main performance indexes of the prepared PTFE copper-clad plate are as follows: at normal temperature, the dielectric constant is 3.02 MHz; the peel strength is 1.7 kN/m; water absorption of 0.01%; the copper foil has no phenomena of edge warping and falling off.
Example 4:
step (1): according to the parts by weight, 50 parts of PTFE powder, 20 parts of lubricant paraffin oil and ceramic powder TiO with the particle size of 15 mu m244 parts of titanium dioxide and 6 parts of short glass fiber are put into a V-shaped mixer to be uniformly mixed; and curing the uniformly mixed powder at the temperature of 50 ℃ for 5 hours to ensure that the lubricant is fully absorbed by the resin and is uniformly distributed in the whole resin system.
Step (2): filling the uniform powder prepared in the step (1) into a die cavity of a die to be pressed to obtain a preform; set the pressure at 20kgf/cm2And keeping the pressure for 5 min.
And (3): carrying out rolling on the preform obtained in the step (2) to obtain a green chip, wherein the rolling pressure is 490N, the roll linear speed is 0.5m/min, and the roll gap is 990 mu m;
and then the raw substrate is put into an oven to be dried to remove the lubricant, wherein the temperature of the oven is 310 ℃, and the time is 6 hours.
And (4): and (4) covering copper foils on two sides of the dried raw substrate in the step (3), and sintering to obtain the PTFE copper-clad plate. Wherein the thickness of the copper foil is 24 μm, the pressure is maintained for 6 hours in a hot press under the conditions that the sintering temperature is 380 ℃, the pressure is 15Mpa and the vacuum degree is-100 Kpa, and then the temperature is reduced at the speed of 2 ℃/min, the pressure is slowly maintained and the temperature is cooled to the room temperature, thus obtaining the polytetrafluoroethylene copper-clad plate.
Through detection, the main performance indexes of the prepared PTFE copper-clad plate are as follows: at normal temperature, the dielectric constant is 6.15 MHz; the peel strength is 1.9 kN/m; water absorption of 0.03%; the copper foil has no phenomena of edge warping and falling off.
Compared with the prior art, the invention replaces the traditional PTFE copper-clad plate and adopts a preparation method of sizing and dipping by PTFE dispersion liquid, thereby avoiding the harm of toxic fluoride, nitrogen oxide and the like, having good filler dispersion effect, uniform mixing and good product size stability. Through reasonable proportioning, the PTFE copper-clad plate prepared by the invention has different dielectric constants (2.6-8.6MHz), a dielectric loss factor less than or equal to 0.003, a peel strength more than or equal to 1.7kN/m and comprehensive performance meeting the use requirement. The invention has simple process and meets the requirement of industrialized mass production.
Claims (5)
1. A preparation method of a polytetrafluoroethylene copper-clad plate is characterized by comprising the following steps:
step (1): putting raw material components including polytetrafluoroethylene powder, a lubricant, ceramic powder and short glass fibers into a V-shaped mixer for uniform mixing; then curing the uniformly mixed powder at a certain temperature;
step (2): filling the uniformly mixed powder obtained in the step (1) into a die cavity of a die to be pressed to obtain a preformed blank;
and (3): obtaining a green chip with a preset thickness by rolling the preform obtained in the step (2), and drying to remove the lubricant;
and (4): covering copper foils on two sides of the raw substrate dried in the step (3), then sintering, and cooling to room temperature after pressure maintaining to obtain the polytetrafluoroethylene copper-clad plate;
in the step (1), the raw material components are as follows according to the weight portion: 30-50 parts of polytetrafluoroethylene powder, 15-20 parts of lubricant, 40-70 parts of ceramic powder and 1-10 parts of short glass fiber;
in the step (1), the curing temperature of the uniformly mixed powder is 35-50 ℃, and the curing time is 4-8 hours;
in the step (2), the preform is obtained by die pressing, wherein the pressure is 5 to 35kgf/cm2Maintaining the pressure for 2-15 min;
and (4) in the sintering in the step (4), maintaining the pressure in a hot press for 4-8 hours under the conditions that the sintering temperature is set to be 360-400 ℃, the pressure is 5-20 Mpa and the vacuum degree is- (90-100) Kpa, and then slowly maintaining the pressure and cooling to room temperature at the cooling speed of 1.5-2.5 ℃/min.
2. The method for preparing the polytetrafluoroethylene copper-clad plate according to claim 1, wherein in the step (4), copper foils are covered on two sides of the raw substrate, and the thickness of the copper layer is 10-50 μm.
3. The method for preparing the polytetrafluoroethylene copper-clad plate according to claim 1, wherein the lubricant is one of solvent oil, petroleum ether and paraffin oil.
4. The method for preparing the polytetrafluoroethylene copper-clad plate according to claim 1, wherein the ceramic powder is one of silica, alumina, aluminum nitride, magnesium oxide, calcium carbonate and titanium dioxide.
5. The preparation method of the polytetrafluoroethylene copper-clad plate according to claim 1, wherein the particle size of the ceramic powder is 5-20 μm.
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| CN110602888A (en) * | 2019-09-18 | 2019-12-20 | 中国电子科技集团公司第四十六研究所 | Preparation method of aluminum-lined high-frequency substrate |
| CN110606698B (en) * | 2019-11-01 | 2021-12-31 | 中国电子科技集团公司第四十六研究所 | Microwave composite dielectric substrate with high uniformity and low thermal expansion coefficient and preparation process thereof |
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| CN111844824A (en) * | 2020-06-24 | 2020-10-30 | 腾辉电子（苏州）有限公司 | Preparation method of PTFE composite material sheet, PTFE composite material sheet and copper-clad plate using PTFE composite material sheet |
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| CN112175216B (en) * | 2020-09-29 | 2022-09-13 | 江苏中际信通讯材料有限公司 | Production method of copper-clad plate with adjustable dielectric constant |
| CN112442243B (en) * | 2020-11-17 | 2022-05-06 | 中国电子科技集团公司第四十六研究所 | Preparation method of polytetrafluoroethylene-based ceramic composite green substrate |
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| CN113061311B (en) * | 2021-04-21 | 2022-08-02 | 山东森荣新材料股份有限公司 | PTFE modified membrane for high-frequency copper-clad plate |
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| CN115850888A (en) * | 2022-12-22 | 2023-03-28 | 广东生益科技股份有限公司 | Fluorine-containing resin-based composition and application thereof |
| CN116373415B (en) * | 2023-06-05 | 2023-07-28 | 山东森荣新材料股份有限公司 | Preparation method of PTFE ceramic filler composite high-frequency copper-clad plate |
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| CN104211320B (en) * | 2014-07-25 | 2016-01-20 | 中国电子科技集团公司第四十六研究所 | A kind of microwave composite medium substrate preparation method |
| CN104647868B (en) * | 2015-02-10 | 2017-09-08 | 郴州功田电子陶瓷技术有限公司 | A kind of preparation method of Copper Clad Laminates Based On Polytetrafluoroethylene |
| CN106751254B (en) * | 2016-12-08 | 2018-12-14 | 中国电子科技集团公司第四十六研究所 | A kind of high dielectric constant covers copper foil microwave-medium plate and preparation method thereof |
| CN107474312B (en) * | 2017-06-12 | 2019-02-26 | 电子科技大学 | The preparation method of ceramic filled polytetrafluoroethylglass microwave composite medium substrate |
| CN108724900B (en) * | 2018-05-29 | 2020-06-16 | 中国电子科技集团公司第三十八研究所 | Preparation method of dry microwave composite dielectric plate |
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