CN102166852A - Preparation method of PTFE (polytetrafluoroethylene) copper-clad plate with high elastic modulus - Google Patents
Preparation method of PTFE (polytetrafluoroethylene) copper-clad plate with high elastic modulus Download PDFInfo
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Abstract
The invention provides a preparation method of a PTFE (polytetrafluoroethylene) copper-clad plate with a high elastic modulus, which comprises the following steps of: preparing copper foil and glass fiber cloth with a low dielectric constant, and preparing a fluororesin mixture; soaking the glass fiber cloth with the prepared fluororesin mixture, transferring the soaked glass fiber cloth into a baking oven for baking and drying, and repeating the steps to enable the glass fiber cloth to be soaked, baked and dried many times, thereby obtaining soaking pieces the resin content of which is about 60-70%; and superposing the soaking pieces, coating the copper foil on two sides, and laminating to obtain the PTFE copper-clad plate. The baking and drying process comprises three stages, wherein the temperature of the baking oven in the first stage is 50-100 DEG C, the temperature of the baking oven in the second stage is 200-320 DEG C, and the temperature of the baking oven in the third stage is 380-400 DEG C. The plate prepared by the method provided by the invention not only has a lower dielectric constant but also has a higher elastic modulus, and the plate has the advantages of consistent internal structure and good dimensional stability.
Description
Technical field
The present invention relates to the preparation method of a kind of preparation method's of copper-clad plate, particularly a kind of high elastic modulus PTFE copper-clad plate.
Background technology
Polytetrafluoroethylene (PTFE) is since 1945 are produced by the E.I.Du Pont Company commercialization, because the physical property and the chemical property of this material uniqueness, people just constantly open up the application of this material in every field, it is existing historical for many years wherein to utilize the good dielectric properties (low-k and low dielectric loss) of PTFE material to make the copper-clad plate of frequency applications, the most traditional manufacture method is a PTFE emulsion impregnated glass fiber cloth, several PTFE impregnated cloths stack up then, copper foil covered pressure promptly obtains the PTFE copper-clad plate, but this manufacture method is to rely on the resin content that increases sheet material to obtain low dielectric constant, and resin content is high more, and the elastic modelling quantity of sheet material just descends.Adding PTFE is thermoplastic resin, its elastic modelling quantity is very low, so the elastic modelling quantity of the PTFE copper-clad plate that the employing conventional method makes is more much lower than isostructural common copper-clad plate (FR-4), elastic modelling quantity is too low will to have a strong impact on its machinability and reliability.How to obtain modulus and dielectric constant has concurrently, people have also carried out some trials, as United States Patent (USP) 4895752/1990 utilization have than low-k organic fiber---aramid fiber floods the PTFE copper-clad plate that the PTFE emulsion is made the low-k high-modulus, but there is the shortcoming of aramid fiber price height, hear resistance relative mistake in this technology and does not apply; United States Patent (USP) 6417459/2002 has been invented a kind of method that the PFA film improves the sheet material resin content of placing between PTFE/ glass cloth dipstick and Copper Foil, because PFA has high relatively elastic modelling quantity than PTFE, so realized also having higher modulus of elasticity when sheet material has lower dielectric constant, influenced problems such as sheet metal thickness uniformity but this technology exists the inconsistent and PFA film of internal structure easily to flow when lamination.
Summary of the invention
The objective of the invention is at above-mentioned existing problems and deficiency, a kind of sheet material internal structure unanimity that makes is provided, elastic modelling quantity improves greatly, has simultaneously than low-k again and has improved the preparation method of PTFE copper-clad plate of the reliability of machinability and electronic product.And the method for the invention process is simple, helps industrialized continuous production.
Technical scheme of the present invention is achieved in that
The preparation method of the PTFE copper-clad plate of high elastic modulus of the present invention may further comprise the steps:
(1), prepares the glass cloth of Copper Foil, low dielectric constant and preparation fluoro-resin mixture;
(2), the fluoro-resin mixture with preparation in the step () floods glass cloth, glass cloth behind the dipping is sent into baking oven and is toasted drying, and repeat this step glass cloth is repeatedly flooded and toast dry, thereby obtain the dipstick that resin content is about 60-70%;
(3), the above-mentioned dipstick that will obtain is folded joins, and is covered with Copper Foil on the two sides, carries out lamination, promptly obtains PTFE copper-clad plate of the present invention.
Wherein the baking drying in the step (three) comprises three phases, and the phase I oven temperature is made as 50-100 ℃, and the time is 1-10 minute, is used to evaporate the moisture on the glass cloth; The second stage oven temperature is made as 200-320 ℃, and the time is 2-20 minute, removes the volatilizable thing of low temperature; The phase III oven temperature is made as 380-400 ℃, and the time is 3-20 minute, is used for fluororesin sintering film forming, and itself and glass cloth are combined closely.To be made as the benefit greater than PTFE sintering temperature (330 degree) be to allow the PTFE crystallization reset to the baking temperature of phase III among the present invention, obtains the integral body of uniformity.
The glass cloth of the low dielectric constant in step () is made by following components in portion by weight: the SiO of 50-60%
2, the Al of 10-20%
2O
3, the B of 20-30%
2O
3, the CaO of 0-5%
2, the MgO of 0-4%
2, surplus is LiO, Na
2O, K
2O, ZrO
2, As
2O
3, Sb
2O
3, ZnO, SrO, Fe
2O
3, Cr
2O
3, P
2O
5The combination of one or more in the oxide.
Above-mentioned fluoro-resin mixture comprises the polytetrafluoroethylene (PTFE) emulsion of following components in portion by weight: 90-100%, the fluororesin of 0-10%, described fluororesin comprises the copolymer (ETFE) of perfluoroethylene-propylene emulsion (FEP), polytetrafluoroethylene (PTFE) perfluoroalkyl vinyl ether emulsion (PFA), tetrafluoroethene and ethene, any combination of one or more in Kynoar (PVDF) or the polytrifluorochloroethylene (PCTFE).
Be difficult for that moving walks guarantees the reliable in structure of sheet material when making Copper Foil and dipstick lamination, the present invention also can adopt between above-mentioned Copper Foil and dipstick tack coat is set.Above-mentioned tack coat can be epoxy bonds sheet or PTFE film.
The present invention is because employing is main liquid with the glass cloth (also being Dk cloth) of low-k and with the PTFE emulsion, cooperate an amount of FEP of interpolation or the made fluoro-resin mixture of PFA emulsion to combine simultaneously and make the method for PTFE copper-clad plate, thereby the good melt fluidity that FEP or PFA emulsion had and the characteristics of higher elasticity modulus have been utilized fully, the sheet material that makes is not only had than low-k, also has simultaneously the higher elasticity modulus, and sheet material internal structure unanimity, the dimensional stability of sheet material might as well, help the assembling of processing of PCB processing procedure and follow-up electronic devices and components, improved the reliability of electronic product greatly.Add that process is simple, production cost is lower, help industrialized continuous production.The prepared PTFE copper-clad plate of the present invention at the dielectric constant that obtains to require simultaneously, wanting that the modular ratio conventional method of sheet material is made is high more than 50%, greatly improve the processability and the reliability of PTFE copper-clad plate, solved in the prior art existing dielectric constant effectively and problem such as modulus can not get both and production cost height, internal structure be inconsistent.And because the present invention also adopts branch three different baking temperature stages from low to high the glass cloth that repeatedly flooded fluoro-resin mixture to be toasted the method for drying and sintering, guarantee combining closely of fluororesin and glass cloth, therefore also further strengthened the reliability of plate construction.
The specific embodiment
The preparation method of the PTFE copper-clad plate of high elastic modulus of the present invention may further comprise the steps:
(1), prepares the glass cloth of Copper Foil, low dielectric constant and preparation fluoro-resin mixture;
(2), the fluoro-resin mixture with preparation in the step () floods glass cloth, glass cloth behind the dipping is sent into baking oven and is toasted drying, and repeat this step glass cloth is repeatedly flooded and toast dry, thereby obtain the dipstick that resin content is about 60-70%;
(3), the above-mentioned dipstick that will obtain is folded joins, and is covered with Copper Foil on the two sides, carries out lamination, promptly obtains PTFE copper-clad plate of the present invention.
Wherein said baking drying comprises three phases, and the phase I oven temperature is made as 50-100 ℃, and the time is 1-10 minute, is used to evaporate the moisture on the glass cloth; The second stage oven temperature is made as 200-320 ℃, and the time is 2-20 minute, removes the volatilizable thing of low temperature; The phase III oven temperature is made as 380-400 ℃, and the time is 3-20 minute, is used for fluororesin sintering film forming, and itself and glass cloth are combined closely.
The glass cloth of the low dielectric constant in step () is made by following components in portion by weight: the SiO of 50-60%
2, the Al of 10-20%
2O
3, the B of 20-30%
2O
3, the CaO of 0-5%
2, the MgO of 0-4%
2, surplus is LiO, Na
2O, K
2O, ZrO
2, As
2O
3, Sb
2O
3, ZnO, SrO, Fe
2O
3, Cr
2O
3, P
2O
5The combination of one or more in the oxide.
Above-mentioned fluoro-resin mixture comprises the ptfe emulsion of following components in portion by weight: 90-100%, the fluororesin of 0-10%, described fluororesin comprises the copolymer of perfluoroethylene-propylene emulsion, polytetrafluoroethylene (PTFE) perfluoroalkyl vinyl ether emulsion or tetrafluoroethene and ethene, a kind of, both or several any combinations in Kynoar, the polytrifluorochloroethylene.
Be difficult for that moving walks guarantees the reliable in structure of sheet material when making Copper Foil and dipstick lamination, the present invention also can adopt between above-mentioned Copper Foil and dipstick tack coat is set.Above-mentioned tack coat can be epoxy bonds sheet or PTFE film.
The present invention is described in further detail below in conjunction with specific embodiment:
Take by weighing the SiO of following components in portion by weight: 50-60% earlier
2, the Al of 10-20%
2O
3, the B of 20-30%
2O
3, the CaO of 0-5%
2, the MgO of 0-4%
2, surplus is LiO, Na
2O, K
2O, ZrO
2, As
2O
3, Sb
2O
3, ZnO, SrO, Fe
2O
3, Cr
2O
3, P
2O
5The combination of one or more in the oxide, the glass cloth of the low-k described in the processing cost invention then.The thickness of this glass cloth is at 0.05-0.20mm, and dielectric constant values Dk is about 4.4, and dielectric loss factor Df is about 0.0025.
The manufacture method of this glass cloth: above-mentioned material after high-temperature fusion is mixed wire drawing, twist yarn, warping, sizing, weave cotton cloth and post processing promptly makes the glass cloth with low-k.
The glass fabric that utilizes above-mentioned raw materials to make, it has and the same mechanical performance of common E glass cloth, but the common E glass of permittivity ratio cloth is much lower, make the PTFE copper-clad plate with this glass cloth, can make sheet material have higher modulus of elasticity not sacrificing under the dielectric constant condition of sheet material.And glass cloth of the present invention and common E glass cloth are when obtaining the sheet material of identical dielectric constant, and the gel content of glass cloth of the present invention is few relatively, and the impregnation number of times just can reduce, and has saved the energy and production cost.
Embodiment one:The preparation method of the PTFE copper-clad plate of high elastic modulus of the present invention may further comprise the steps:
(1), prepares Copper Foil, the glass cloth of above-mentioned low-k.The about 0.10mm of the thickness of glass cloth, dielectric constant values Dk is about 4.4, and dielectric loss factor Df is about 0.0025, and warp/weft yarn number is the 60X44 root, the about 95g/m of substance
2
The preparation fluoro-resin mixture.The component of this fluoro-resin mixture comprises that 95% ptfe emulsion, 4% perfluoroethylene-propylene (FEP), 1% are used for regulating the nonionic surface active agent or the deionized water of viscosity and solids content.The solids content of mixture can be adjusted between 35 ~ 60%, and viscosity is 15 ~ 40mPas(20 ℃).
(2), with the fluoro-resin mixture dipping glass cloth of preparation in step (), the glass cloth behind the dipping is sent into baking oven and is toasted drying, temperature of oven is divided into three sections, first section temperature is 50-100 ℃, is mainly water evaporates; Second section temperature is 200-320 ℃, it mainly is the removal of the auxiliary agent volatilizable things of low temperature such as (emulsifying agent, dispersants), the 3rd section temperature is 380-400 ℃, with fluororesin sintering film forming, and combine closely with glass cloth, and repeat this step 3 time, make glass cloth carry out three dippings and baking dry, thereby obtain the dipstick (being called for short the PP sheet) of resin content 65%;
(3), the above-mentioned dipstick that will obtain according to above-mentioned steps totally 15 folded joining, and be covered with the 1OZ Copper Foil on the two sides, carry out lamination, lamination is 360-380 ℃/2-5hrs, pressure is 50-100kgf/cm
2, promptly obtain PTFE copper-clad plate of the present invention.
Embodiment two:The preparation method of the PTFE copper-clad plate of high elastic modulus of the present invention may further comprise the steps:
(1), prepares Copper Foil, the glass cloth of above-mentioned low-k.The about 0.10mm of the thickness of glass cloth, dielectric constant values Dk is about 4.4, and dielectric loss factor Df is about 0.0025, and warp/weft yarn number is the 60X44 root, the about 95g/m of substance
2
The preparation fluoro-resin mixture.The component of this fluoro-resin mixture comprises that 95% ptfe emulsion, 4% polytetrafluoroethylene (PTFE) perfluoroalkyl vinyl ether (PFA) emulsion, 1% are used for regulating the nonionic surface active agent or the deionized water of viscosity and solids content.The solids content of mixture is about 60%, and viscosity is 15 ~ 40mPas(20 ℃).
(2), with the fluoro-resin mixture dipping glass cloth of preparation in step (), the glass cloth behind the dipping is sent into baking oven and is toasted drying, temperature of oven is divided into three sections, first section temperature is 50-100 ℃, is mainly water evaporates; Second section temperature is 200-320 ℃, it mainly is the removal of the volatilizable things of low temperature such as auxiliary agent (generally being the auxiliary agent such as emulsifying agent, dispersant in the PTFE supernatant liquid), the 3rd section temperature is 380-400 ℃, with fluororesin sintering film forming, and combine closely with glass cloth, and repeat this step 3 time, make glass cloth carry out three dippings and baking dry, thereby obtain the dipstick (being called for short the PP sheet) of resin content about 65%;
(3), the above-mentioned dipstick that will obtain totally 15 folded joining, after covering tack coat on the folded dipstick of joining, be covered with the 1OZ Copper Foil at one or both sides again, carry out lamination, lamination is 360-380 ℃/2-5hrs, pressure is 50-100kgf/cm
2, promptly obtain PTFE copper-clad plate of the present invention.
Embodiment three:The preparation method of the PTFE copper-clad plate of high elastic modulus of the present invention may further comprise the steps:
(1), prepares Copper Foil, the glass cloth of above-mentioned low-k.The about 0.10mm of the thickness of glass cloth, dielectric constant values Dk is about 4.4, and dielectric loss factor Df is about 0.0025, and warp/weft yarn number is the 60X44 root, the about 95g/m of substance
2
The preparation fluoro-resin mixture.The component of this fluoro-resin mixture comprises that the emulsion, 1% of the one or more combination in copolymer, Kynoar or the polytrifluorochloroethylene of 90% ptfe emulsion, 9% tetrafluoroethene and ethene is used for regulating the nonionic surface active agent or the deionized water of viscosity and solids content.The solids content of mixture is about 60%, and viscosity is 15 ~ 40mPas(20 ℃).
(2), with the fluoro-resin mixture dipping glass cloth of preparation in step (), the glass cloth behind the dipping is sent into baking oven and is toasted drying, temperature of oven is divided into three sections, first section temperature is 50-100 ℃, is mainly water evaporates; Second section temperature is 200-320 ℃, it mainly is the removal of the volatilizable things of low temperature such as auxiliary agent (generally being the auxiliary agent such as emulsifying agent, dispersant in the PTFE supernatant liquid), the 3rd section temperature is 380-400 ℃, with fluororesin sintering film forming, and combine closely with glass cloth, and repeat this step 3 time, make glass cloth carry out three dippings and baking dry, thereby obtain the dipstick (being called for short the PP sheet) of resin content about 70%;
(3), the above-mentioned dipstick that will obtain totally 15 folded joining, after covering tack coat on the folded dipstick of joining, be covered with the 1OZ Copper Foil at one or both sides again, carry out lamination, lamination is 360-380 ℃/2-5hrs, pressure is 50-100kgf/cm
2, promptly obtain PTFE copper-clad plate of the present invention.
Comparative example 4
Adopting model is that 2116 E glass fabric is replaced the low-k glass cloth among the present invention, the about 0.10mm of E glass fabric thickness, and warp/weft yarn number is the 60X58 root, the about 103g/m of substance
2
With ptfe emulsion dipping E glass fabric.Above-mentioned ptfe emulsion can be regulated viscosity and solids content with nonionic surface active agent or deionized water, and solids content can be adjusted between 35 ~ 60%, and viscosity is 15 ~ 40mPas(20 ℃).
E glass fabric behind the dipping is sent into baking oven baking drying, and temperature of oven is divided into three sections, and first section temperature is 50 ~ 100 ℃, is mainly water evaporates; Second section temperature is 200 ~ 320 ℃, mainly is the removal of the auxiliary agent volatilizable things of low temperature such as (emulsifying agent, dispersants), and the 3rd section temperature is 380 ~ 400 ℃.Repeat this step 5 time, obtain the dipstick (being called for short the PP sheet) of resin content about 75%.
With the PP sheet that obtains totally 13 folded joining, the 1OZ Copper Foil is covered on the two sides, carries out lamination, and lamination is 360 ~ 380 ℃/2 ~ 5hrs., and pressure is 50 ~ 100kgf/cm2.Make 1.6 1/1 samples.
Below be the Performance Detection table of comparisons of prepared sheet material:
| Test event | Embodiment 1 | Embodiment 2 | Comparative example 4 |
| Hot strength (MPa) | 102 | 95 | 87 |
| Elastic modelling quantity (GPa) | 1.8 | 1.5 | 1.0 |
| Dk(1GHz) | 2.60 | 2.60 | 2.60 |
| Df(1GHz) | 0.0008 | 0.0008 | 0.0006 |
| PS(N/mm) | 1.8 | 1.7 | 1.7 |
Can find out from the above-mentioned table of comparisons, utilize the sheet material of the identical dielectric constant that the method for the invention makes, its elastic modelling quantity will be higher than the elastic modelling quantity that utilizes the sheet material that Comparative Examples 4 described methods make out and away.
The present invention describes by embodiment, but the present invention is not construed as limiting, with reference to description of the invention, other variations of the disclosed embodiments, expect easily that as professional person such variation should belong within the claim restricted portion of the present invention for this area.
Claims (7)
1. the preparation method of the PTFE copper-clad plate of a high elastic modulus is characterized in that may further comprise the steps:
(1), prepares the glass cloth of Copper Foil, low dielectric constant and preparation fluoro-resin mixture;
(2), the fluoro-resin mixture with preparation in the step () floods glass cloth, glass cloth behind the dipping is sent into baking oven and is toasted drying, and repeat this step glass cloth is repeatedly flooded and toast dry, thereby obtain the dipstick of resin content 60～70%;
(3), the above-mentioned dipstick that will obtain is folded joins, and is covered with Copper Foil at one or both sides, carries out lamination, promptly obtains PTFE copper-clad plate of the present invention;
Wherein in step (two), described baking drying comprises three phases, and the phase I oven temperature is made as 50-100 ℃, and stoving time is 1～10 minute, is used to evaporate the moisture on the glass cloth; The second stage oven temperature is made as 200-320 ℃, and stoving time is 2～20 minutes, removes the volatilizable thing of low temperature; The phase III oven temperature is made as 380-400 ℃, and stoving time is 3～20 minutes, is used for fluororesin sintering film forming, and itself and glass cloth are combined closely.
2. according to the preparation method of the PTFE copper-clad plate of the described high elastic modulus of claim 1, it is characterized in that: the glass cloth of low dielectric constant is to be made by following components in portion by weight in step (): the SiO of 50-60%
2, the Al of 10-20%
2O
3, the B of 20-30%
2O
3, the CaO of 0-5%
2, the MgO of 0-4%
2, surplus is LiO, Na
2O, K
2O, ZrO
2, As
2O
3, Sb
2O
3, ZnO, SrO, Fe
2O
3, Cr
2O
3, P
2O
5The combination of one or more in the oxide.
3. according to the preparation method of the PTFE copper-clad plate of the described high elastic modulus of claim 1, it is characterized in that above-mentioned fluoro-resin mixture comprises the ptfe emulsion of following components in portion by weight: 90-100%, the fluororesin of 0-10%, wherein said fluororesin comprises one or more the combination in copolymer, Kynoar or the polytrifluorochloroethylene of perfluoroethylene-propylene emulsion, polytetrafluoroethylene (PTFE) perfluoroalkyl vinyl ether emulsion, tetrafluoroethene and ethene.
4. according to the preparation method of the PTFE copper-clad plate of the described high elastic modulus of claim 3, it is characterized in that above-mentioned fluoro-resin mixture also comprises the diluent that is used for regulating viscosity and solids content, this diluent is nonionic surface active agent or deionized water, the solids content of described fluoro-resin mixture is between the 35-60%, and viscosity is 15-40mPas.
5. according to the preparation method of the PTFE copper-clad plate of the described high elastic modulus of claim 1, it is characterized in that: in step (three), want between Copper Foil and dipstick, tack coat is set earlier when on folded dipstick of joining, covering Copper Foil, and then lamination.
6. according to the preparation method of the PTFE copper-clad plate of the described high elastic modulus of claim 5, it is characterized in that above-mentioned tack coat is epoxy bonds sheet or PTFE film.
7. according to the preparation method of the PTFE copper-clad plate of the described high elastic modulus of claim 1, it is characterized in that the lamination in step (three) is 360-380 ℃/2-5hrs, pressure is 50-100kgf/cm
2
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