CN114133613B - Surface activation treatment method for PTFE (polytetrafluoroethylene) substrate - Google Patents
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- C08J7/123—Treatment by wave energy or particle radiation
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K1/00—Printed circuits
- H05K1/02—Details
- H05K1/0296—Conductive pattern lay-out details not covered by sub groups H05K1/02 - H05K1/0295
- H05K1/0298—Multilayer circuits
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K3/00—Apparatus or processes for manufacturing printed circuits
- H05K3/46—Manufacturing multilayer circuits
- H05K3/4611—Manufacturing multilayer circuits by laminating two or more circuit boards
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- C08J2327/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers
- C08J2327/02—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment
- C08J2327/12—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
- C08J2327/18—Homopolymers or copolymers of tetrafluoroethylene
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Abstract
The invention relates to a surface activation treatment method of a PTFE substrate, which comprises the following two steps: firstly, carrying out corona activation treatment on a PTFE substrate, ionizing air between two electrodes by utilizing corona discharge generated by a gap between a high-frequency high-voltage discharge knife rest and a knife blade to generate ozone, oxidizing surface molecules of the PTFE substrate, increasing surface energy, increasing surface roughness of the PTFE substrate after being impacted by electrons, and further primarily improving wettability of the PTFE substrate; and secondly, carrying out sodium naphthalene solution treatment on the PTFE substrate subjected to corona activation treatment to enable part of fluorine atoms on the surface of the PTFE substrate to be lost, and then introducing polar groups such as hydroxyl, carbonyl, unsaturated bonds and the like into the surface of the PTFE substrate to increase the surface energy and efficiently and uniformly improve the wettability. The invention can realize the surface activation treatment effect of the PTFE substrate with high hydrophilicity and is beneficial to continuously producing the interlayer bonding sheet for the multilayer board.
Description
Technical Field
The invention belongs to the technical field of microwave composite medium substrates, and particularly relates to a surface activation treatment method of a PTFE (polytetrafluoroethylene) substrate with high hydrophilicity and continuous production.
Background
With the continuous development of modern communication technology, the demands of electronic products are continuously increased, electronic components are developed towards miniaturization, light weight and integration, the demands of high-frequency circuits are increasingly increased, a single-layer microwave composite dielectric plate cannot meet the use requirements, and research on a multi-layer microwave composite dielectric substrate consisting of a microwave substrate bonding sheet material and a single-layer microwave composite dielectric substrate becomes a hot spot.
Polytetrafluoroethylene (PTFE) resin has low dielectric constant, low loss factor, good chemical resistance and heat resistance, and is the preferred base material for the microwave composite dielectric substrate at present, but PTFE resin has low surface energy, extremely poor fluidity and adhesiveness, and is difficult to be used as an adhesive material between multilayer boards. Therefore, the interlayer bonding material for the multilayer board with excellent comprehensive performance is developed, and the interlayer bonding material has great significance for the development of the circuit substrate industry.
Chinese patent applications CN112442202a and CN112538184A, CN112538186a respectively provide a PTFE-based surface activation treatment method, and combine with a dielectric resin layer on both sides to form an adhesive sheet having a strong adhesive property. The method of surface treatment of PTFE substrate in patent CN112442202A is to soak PTFE substrate in naphthalene sodium solution, then wash with acetone and distilled water and dry, although the method can improve the surface energy of PTFE substrate and improve the adhesion with resin layer, the surface hydrophilicity of PTFE substrate is poor, the surface hydrophilicity of PTFE substrate after treatment is directly treated with naphthalene sodium, the surface hydrophilicity of PTFE substrate after treatment is not greatly improved, the adhesion performance of core layer and surface layer of adhesive sheet material is insufficient, so that delamination of adhesive sheet material itself easily occurs under extreme use condition, and the subsequent use is affected. In the patent CN112538184a and CN112538186a, the surface treatment is performed on the PTFE substrate by using plasma, and the PTFE substrate to be treated needs to be placed in a vacuum cavity in a low-temperature vacuum environment for the plasma treatment, so that the method can treat the PTFE sheet, but the PTFE coiled material cannot be treated, which is not beneficial to the continuous production of the subsequent bonding sheet material.
Disclosure of Invention
Aiming at the defects of the prior art, the invention develops a surface activation treatment method of a PTFE substrate, which is used for efficiently and uniformly improving the hydrophilic property of the surface of the PTFE substrate, realizing the high bonding quality of an interlayer bonding sheet material for a multi-layer board, being beneficial to the industrial production of the bonding sheet material and being the research focus in the field.
The method aims at realizing the surface activation treatment effect of the PTFE substrate with high hydrophilicity and is beneficial to continuously producing the interlayer bonding sheet for the multilayer board.
The technical scheme adopted by the invention is as follows: the surface activation treatment method of PTFE substrate, the PTFE substrate is an interlayer for preparing interlayer bonding sheets for a multi-layer board, and the interlayer bonding sheets and bonding resin layers bonded on two sides of the PTFE substrate form interlayer bonding sheet materials for the multi-layer board together; the method comprises the following specific steps:
(1) Carrying out corona activation treatment on the PTFE substrate;
placing a PTFE substrate in a feed zone of a corona activation processor;
starting a corona activation processor, generating corona discharge in a gap between a discharge knife rest and a knife blade by using high-frequency high voltage, ionizing air between the two electrodes, and forming a plasma region on the surface of the PTFE substrate, so that the surface of the PTFE substrate becomes a nonpolar surface, and modifying is achieved; in addition, the air is ionized in a high-voltage electric field to generate ozone, so that surface molecules of the PTFE substrate are oxidized, the PTFE substrate is converted from nonpolar to polar, and the surface energy is improved; meanwhile, after electron impact, the surface roughness of the PTFE substrate is increased, and the surface activity is increased, so that the wettability of the PTFE substrate is improved;
the voltage of the corona activation treatment is 1000V-20000V;
the treatment time of the corona activation treatment is 5-600 s;
the discharge gap of the corona activation treatment is 0.5-cm cm;
the corona speed of the corona activation treatment is 0.1-100 m/min;
the power of the corona activation treatment is 200-5000W;
the corona treatment depth of the PTFE substrate is 5-15 nm;
the contact angle of the PTFE substrate after corona treatment is 90-100 degrees;
(2) Carrying out sodium naphthalene solution treatment on the PTFE substrate subjected to corona activation treatment;
immersing the PTFE substrate in a sodium naphthalene solution for treatment, or brushing or spraying the sodium naphthalene solution on the PTFE substrate to form a sodium naphthalene treatment liquid thin layer on the surface of the PTFE substrate; after the treatment is finished, the PTFE substrate is washed by acetone or ethanol solvent and then is washed by water;
the concentration of the sodium naphthalene solution is 0.3 mol/L-10 mol/L;
the treatment time of the sodium naphthalene solution is 5-600 s;
the contact angle of the PTFE substrate after corona treatment is 30-80 degrees.
The thickness of the PTFE substrate is 20-100 μm.
The corona activated air in the step (1) is water vapor and N 2 O、N 2 One of them.
Compared with the prior art, the invention has the following characteristics:
in the surface treatment method provided by the invention, corona activation treatment is used as a PTFE substrate pretreatment process, so that the contact angle of the surface of the PTFE substrate is reduced from 115 degrees to 90 degrees to 100 degrees, the surface wettability of the PTFE substrate is improved to a certain extent, when sodium naphthalene solution treatment is carried out on the PTFE substrate on the basis, the surface energy of the PTFE substrate can be greatly improved, the surface hydrophilicity of the PTFE substrate is in an excellent state, meanwhile, the 'pattern' of the surface of the PTFE substrate caused by simply and directly carrying out sodium naphthalene solution treatment is avoided, the high-uniformity surface treatment effect is obtained, and the PTFE substrate treated by the surface treatment method provided by the invention and a dielectric resin layer are bonded in a high-strength, high-uniformity and stable manner, and the heat resistance and high-temperature reliability of the PTFE substrate can meet the manufacturing process requirement and the subsequent application requirement of a multilayer printed circuit board.
Meanwhile, the corona activation treatment method provided by the invention has the advantages of simple operation, easy control, short treatment time and high speed, can directly carry out on-line treatment on the PTFE base material, has a shallow treatment range, does not influence the mechanical properties of the material, and is beneficial to the continuous production of the subsequent bonding sheet material.
Detailed description of the preferred embodiments
The technical scheme of the invention is further described through a specific implementation method. It will be apparent to those skilled in the art that the examples are merely to aid in understanding the invention and are not to be construed as a specific limitation thereof.
The experimental materials used in the examples and comparative examples of the present invention are as follows:
(1) PTFE substrate I: immersing 106 electronic grade glass cloth in PTFE composite slurry (average grain diameter of PTFE is 0.3-0.5 μm) containing 50wt% spherical silicon dioxide ceramic powder at normal temperature, drying at 180 ℃ and sintering at 300 ℃ for 30min to obtain the final product;
(2) PTFE base material II: continuously coating PTFE composite slurry containing 20wt% of angular silicon dioxide ceramic powder and a polymer base film, drying at 110 ℃ and curing at 220 ℃, and stripping the PTFE composite slurry and the base film on a stripping rotating shaft to obtain the PTFE composite slurry;
(3) Sodium naphthalene solution: 128g (1 mol) of fine naphthalene is added into a clean and dry three-neck flask, tetrahydrofuran is added, and stirring and dissolution are carried out; then, 23g (1 mol) of metallic sodium is gradually added into the three-neck flask, dry argon is introduced, the temperature is controlled between 5 ℃ and 10 ℃, and the sodium naphthalene solution is obtained after stirring for 2 hours.
(4) Corona activation processor, corona activation processor is film corona machine or sheet corona machine or corona device connected to PTFE production equipment.
The molding method of the PTFE substrate comprises extrusion, mould pressing, calendaring, turning, casting, coating and dipping, and the PTFE substrate can be filled with reinforcing materials such as inorganic fillers, glass fibers and the like.
Example 1
(1) Cleaning PTFE substrate I with the thickness of 100 mu m by ethanol, removing greasy dirt and drying; then placing the PTFE substrate in a corona treatment machine, setting the voltage to 3000V, setting the corona gap to 1cm, setting the corona speed to 0.5m/min and the power to 1kW, and taking out the PTFE substrate after being treated in air for 60 seconds to obtain a PTFE substrate I after corona activation treatment;
(2) Soaking the PTFE substrate I subjected to corona activation treatment in a sodium naphthalene solution in a dry nitrogen protection atmosphere, wherein the concentration of the sodium naphthalene solution is 0.8 mol/L, taking out after soaking for 300 seconds, and respectively washing and drying with ethanol and distilled water to obtain a PTFE substrate 1 subjected to surface treatment;
(3) The PTFE substrate I after surface treatment is observed, the color is uniform, no pattern exists, four corners and the center of the substrate of 18 '. Times.24' are respectively sampled, the contact angle test results are 65 degrees, 69 degrees, 73 degrees, 61 degrees and 74 degrees, the surface hydrophilicity is good, and the uniformity is general.
Example 2
(1) Cleaning a PTFE substrate II with the thickness of 50 mu m by ethanol, removing greasy dirt, and drying; then placing the PTFE substrate in a corona treatment machine, setting the voltage to 10000V, setting the corona gap to 0.8cm, setting the corona speed to 1.2m/min and the power to 1.3kW, treating the PTFE substrate in water vapor for 300s, and taking out the PTFE substrate to obtain a PTFE substrate II after corona activation treatment;
(2) Soaking the PTFE substrate 2 subjected to corona activation treatment in a sodium naphthalene solution in a dry nitrogen protection atmosphere, wherein the concentration of the sodium naphthalene solution is 4mol/L, taking out after soaking for 120 seconds, and respectively cleaning and drying by using ethanol and distilled water to obtain a PTFE substrate II subjected to surface treatment;
(3) The PTFE substrate II after surface treatment is observed, the color is uniform, no pattern exists, four corners and the center of the substrate of 18 '. Times.24' are respectively sampled, the contact angle test results are 75 degrees, 77 degrees, 73 degrees, 76 degrees and 74 degrees, the surface uniformity is good, and the surface hydrophilicity is general.
Example 3
(1) Cleaning a PTFE substrate I with the thickness of 80 mu m by ethanol, removing greasy dirt, and drying; then placing the PTFE substrate in a corona treatment machine, setting the voltage to 14000V, the corona gap to be 1cm, the corona speed to be 1.5m/min and the power to be 2kW, and taking out the PTFE substrate after being treated in air for 90 seconds to obtain a PTFE substrate I after corona activation treatment;
(2) Soaking the PTFE substrate I subjected to corona activation treatment in a sodium naphthalene solution in a dry nitrogen protection atmosphere, wherein the concentration of the sodium naphthalene solution is 2mol/L, taking out after soaking for 180 seconds, and respectively cleaning and drying by using acetone and distilled water to obtain a PTFE substrate 1 subjected to surface treatment;
(3) The PTFE substrate I after surface treatment is observed, the color is uniform, no pattern exists, four corners and the center of the substrate are respectively sampled at 18 '. Times.24', the contact angle test results are 53 DEG, 57 DEG, 56 DEG, 55 DEG and 54 DEG, and the surface hydrophilicity and the surface uniformity are excellent.
Example 4
(1) Cleaning a PTFE substrate II with the thickness of 70 mu m by ethanol, removing greasy dirt and drying; then placing the PTFE substrate in a corona treatment machine, setting the voltage to 18000V, setting the corona gap to be 2cm, setting the corona speed to be 3m/min and the power to be 1.5kW, and taking out the PTFE substrate after being treated in water vapor for 20s to obtain a PTFE substrate II after corona activation treatment;
(2) Soaking the PTFE substrate II subjected to corona activation treatment in a sodium naphthalene solution in a dry nitrogen protection atmosphere, wherein the concentration of the sodium naphthalene solution is 6mol/L, taking out after soaking for 30 seconds, and respectively cleaning and drying by using acetone and distilled water to obtain a PTFE substrate II subjected to surface treatment;
(3) The PTFE substrate II after surface treatment was observed to be uniform in color and free of patterns, samples were taken at the four corners and the center of a substrate of 18 "x 24", and the contact angle test results were 74 °, 77 °, 79 °, 81 °, 74 °, and the surface hydrophilicity was general.
The PTFE substrate surface contact angle in example 3 described above is the lowest, and the PTFE substrate surface hydrophilicity and uniformity are the best.
The naphthalene sodium solution is a dark green viscous mixed suspension formed by dissolving or complexing fine naphthalene and metallic sodium in tetrahydrofuran or glycol dimethyl ether active ether solvent.
The principle of sodium naphthalene solution treatment is that the sodium naphthalene solution is subjected to chemical reaction with PTFE to enable partial fluorine atoms on the surface of a PTFE substrate to be lost, and then polar groups such as hydroxyl, carbonyl and unsaturated bonds are introduced into the surface of the PTFE substrate, so that the surface energy of the PTFE substrate is increased, and the wettability of the PTFE substrate is improved.
It should be understood that although the present disclosure describes embodiments in terms of individual implementations, not every implementation is solely comprised of a single implementation, and that such descriptions in the disclosure are for clarity only, and that those skilled in the art will recognize that the implementations may be practiced with other combinations of implementations as appropriate.
The above embodiments are merely specific illustrations of practical methods of the present invention, and they are not intended to limit the scope of the invention, but all equivalent implementation methods or modifications that do not depart from the spirit of the invention are included in the scope of the invention.
Claims (1)
1. A surface activation treatment method for PTFE base material is characterized in that: the PTFE substrate is an intermediate layer for preparing an interlayer bonding sheet for the multilayer board, and the PTFE substrate and bonding resin layers bonded on two sides of the PTFE substrate form an interlayer bonding sheet material for the multilayer board together; the method comprises the following specific steps:
(1) Carrying out corona activation treatment on the PTFE substrate;
placing a PTFE substrate in a feed zone of a corona activation processor;
starting a corona activation processor, generating corona discharge in a gap between a discharge knife rest and a knife blade by using high-frequency high voltage, ionizing air between the two electrodes, and forming a plasma region on the surface of the PTFE substrate, so that the surface of the PTFE substrate becomes a nonpolar surface, and modifying is achieved; in addition, the air is ionized in a high-voltage electric field to generate ozone, so that surface molecules of the PTFE substrate are oxidized, the PTFE substrate is converted from nonpolar to polar, and the surface energy is improved; meanwhile, after electron impact, the surface roughness of the PTFE substrate is increased, and the surface activity is increased, so that the wettability of the PTFE substrate is improved;
the voltage of the corona activation treatment is 1000V-20000V;
the treatment time of the corona activation treatment is 5-600 s;
the discharge gap of the corona activation treatment is 0.5-cm cm;
the corona speed of the corona activation treatment is 0.1-100 m/min;
the power of the corona activation treatment is 200-5000W;
the corona treatment depth of the PTFE substrate is 5-15 nm;
the contact angle of the PTFE substrate after corona treatment is 90-100 degrees;
(2) Carrying out sodium naphthalene solution treatment on the PTFE substrate subjected to corona activation treatment;
immersing the PTFE substrate in a sodium naphthalene solution for treatment, or brushing or spraying the sodium naphthalene solution on the PTFE substrate to form a sodium naphthalene treatment liquid thin layer on the surface of the PTFE substrate; after the treatment is finished, the PTFE substrate is washed by acetone or ethanol solvent and then is washed by water;
the concentration of the sodium naphthalene solution is 0.3 mol/L-10 mol/L;
the treatment time of the sodium naphthalene solution is 5-600 s;
the contact angle of the PTFE substrate after corona treatment and sodium naphthalene solution treatment is 30-80 degrees;
the thickness of the PTFE substrate is 20-100 mu m;
the corona activated air in the step (1) is water vapor and N 2 O、N 2 One of them.
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| CN115042460A (en) * | 2022-07-20 | 2022-09-13 | 上海翊科聚合物科技有限公司 | Continuous etching method of PTFE (polytetrafluoroethylene) tube |
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| GB1345748A (en) * | 1970-10-09 | 1974-02-06 | Du Pont | Surface-patterned surface-activated polymer film |
| CN103236510B (en) * | 2013-04-18 | 2015-08-12 | 中南大学 | A kind of corona treatment process of membrane for polymer of lithium rechargeable battery |
| CN108211814B (en) * | 2018-03-23 | 2020-11-03 | 北京工业大学 | Hydrophilic modification method for polytetrafluoroethylene porous membrane |
| CN112442202B (en) * | 2019-09-04 | 2022-10-18 | 广东生益科技股份有限公司 | Interlayer bonding sheet for multilayer board and preparation method and application thereof |
| CN112044274B (en) * | 2020-08-28 | 2022-09-09 | 盐城工学院 | Preparation method of porous polytetrafluoroethylene filtering membrane |
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