CN104553224A - Manufacturing method of viscous varnished cloth, viscous varnished cloth manufactured with method and copper-clad plate - Google Patents
Manufacturing method of viscous varnished cloth, viscous varnished cloth manufactured with method and copper-clad plate Download PDFInfo
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- CN104553224A CN104553224A CN201410839915.1A CN201410839915A CN104553224A CN 104553224 A CN104553224 A CN 104553224A CN 201410839915 A CN201410839915 A CN 201410839915A CN 104553224 A CN104553224 A CN 104553224A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B17/00—Layered products essentially comprising sheet glass, or glass, slag, or like fibres
- B32B17/02—Layered products essentially comprising sheet glass, or glass, slag, or like fibres in the form of fibres or filaments
- B32B17/04—Layered products essentially comprising sheet glass, or glass, slag, or like fibres in the form of fibres or filaments bonded with or embedded in a plastic substance
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B15/00—Layered products comprising a layer of metal
- B32B15/04—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material
- B32B15/08—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
- B32B37/02—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by a sequence of laminating steps, e.g. by adding new layers at consecutive laminating stations
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
- B32B37/14—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the properties of the layers
- B32B37/15—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the properties of the layers with at least one layer being manufactured and immediately laminated before reaching its stable state, e.g. in which a layer is extruded and laminated while in semi-molten state
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B38/00—Ancillary operations in connection with laminating processes
- B32B38/0036—Heat treatment
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B38/00—Ancillary operations in connection with laminating processes
- B32B38/16—Drying; Softening; Cleaning
- B32B38/164—Drying
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2260/00—Layered product comprising an impregnated, embedded, or bonded layer wherein the layer comprises an impregnation, embedding, or binder material
- B32B2260/04—Impregnation, embedding, or binder material
- B32B2260/046—Synthetic resin
Abstract
The invention discloses a manufacturing method of viscous varnished cloth. The manufacturing method comprises steps as follows: steeping of glass fiber fabric, drying of the glass fiber fabric, high-temperature sintering, forming of middle varnished cloth, glue coating of the middle varnished cloth, drying of the middle varnished cloth, forming of the viscous varnished cloth and the like. The invention further discloses the viscous varnished cloth manufactured with the method and a copper-clad plate. The copper-clad plate comprises a varnished cloth layer and copper foil covering the varnished cloth layer, wherein the varnished cloth layer is formed by stacking pieces of middle varnished cloth and pieces of the viscous varnished cloth, and the viscous varnished cloth is arranged in the position, contacted with the copper foil, of the varnished cloth layer. The bonding capacity of the viscous varnished cloth manufactured with the manufacturing method and the copper foil is high, the bonding force of the varnished cloth and the copper foil is effectively improved, the peel strength of the varnished cloth and the copper foil can be improved if the viscous varnished cloth is used for manufacturing the copper-clad plate, and the problem of difficult bonding of the varnished cloth and the copper foil is solved.
Description
Technical field
The present invention relates to varnished cloth and copper-clad plate technical field, particularly relate to a kind of viscosity varnished cloth preparation method, the application viscosity varnished cloth made of the method and copper-clad plate.
Background technology
Polytetrafluoroethylene (PTFE) (PTFE) from 1945 by since E.I.Du Pont Company's merchandized handling, due to physical property and the chemical property of this material uniqueness, people just constantly open up the application of this material in every field, wherein utilize the outstanding dielectric properties of PTFE material (low-k and low dielectric loss) to make the existing history for many years of copper-clad plate of frequency applications.
The preparation method of traditional PTFE copper-clad plate is with PTFE emulsion impregnated glass fiber cloth, makes PTFE varnished cloth, then by superimposed for several PTFE varnished cloths, and covers Copper Foil on two sides, finally carry out high temperature lamination, make PTFE copper-clad plate.But because the molecular structure surface after PTFE sintering is inert condition, it is more difficult that direct and Copper Foil bonds, is therefore generally adopt fluorine resin film (as polyfluorinated ethylene membrane) PTFE varnished cloth and Copper Foil to be bonded as binding agent at present.Performance and the PTFE of fluorine resin film are close, but fusing point is lower, better than the PTFE varnished cloth after sintering with the bond effect of Copper Foil, but this production technology is more complicated at present, and cost is higher.
Chinese patent literature CN201010181737 describes the copper-clad plate that a kind of fluoro-resin mixture makes, the program mainly adds a certain proportion of perfluoroethylene-propylene (FEP) in PTFE emulsion, this PTFE emulsion mixture can repeatedly flood glass-fiber-fabric under lower than PTFE sintering temperature (330 DEG C) condition and obtain varnished cloth, the copper-clad plate combination property of being suppressed by above-mentioned varnished cloth is good, and preparation method process is simple.But because the sintering temperature of PTFE is higher, if the ratio of perfluoroethylene-propylene is lower, varnished cloth is after shaping lower than PTFE sintering temperature (330 DEG C), and have coming unstuck to a certain degree, this phenomenon is especially obvious in lower one immersing glue process; If improve the ratio of perfluoroethylene-propylene, degumming phenomenon makes moderate progress, but material cost can be higher.
Summary of the invention
One object of the present invention is: provide a kind of viscosity varnished cloth preparation method, make the viscosity varnished cloth stronger with the cementitiousness of Copper Foil, effectively improves the bonding force of varnished cloth and Copper Foil, solves the problem of varnished cloth and Copper Foil bond difficult.
Another object of the present invention is: provide the viscosity varnished cloth be made up of above-mentioned viscosity varnished cloth preparation method.
Another object of the present invention is: provide a kind of copper-clad plate, by arranging viscosity varnished cloth, effectively improves the peel strength of varnished cloth and Copper Foil.
For reaching this object, the present invention by the following technical solutions:
On the one hand, a kind of viscosity varnished cloth preparation method is provided, at least comprises the following steps:
S10, make in the middle of varnished cloth: carry out drying after glass fabric being flooded fluoro-resin emulsion, cure, high temperature sintering process, and repeat dry, cure, high temperature sintering process obtains middle varnished cloth for 3-10 time;
S20, middle varnished cloth cover glue: by middle varnished cloth dipping or fluororesin-coated emulsion, ensure that at least one side is covered with fluoro-resin emulsion;
S30, middle varnished cloth are dried: the middle varnished cloth after dipping or fluororesin-coated emulsion is carried out to drying and cures process, remove moisture and each analog assistant;
S40, viscosity varnished cloth are shaping: the middle varnished cloth after order oven dry processes 1-10min under low-temperature sintering temperature environment, described low-temperature sintering temperature is lower than high temperature sintering temperature 0-80 DEG C, make the fluoro-resin emulsion of dipping or coating in step S20 be in slight sintering or non-sintering state, make viscosity varnished cloth.
Further, described low-temperature sintering temperature is lower than high temperature sintering temperature 20-60 DEG C.
Further, step S10 specifically comprises the following steps:
S11, glass-fiber-fabric flood: provide glass fabric and fluoro-resin emulsion, glass fabric is flooded fluoro-resin emulsion;
S12, glass-fiber-fabric are dried: by the glass fabric dry 1-10min under 50 DEG C of-150 DEG C of conditions after dipping fluoro-resin emulsion, remove moisture, then under 200 DEG C of-320 DEG C of conditions, cure 1-10min, remove each analog assistant;
S13, high temperature sintering: process 1-10min under making the glass fabric after oven dry be in 350 DEG C of-400 DEG C of conditions, by fluoro-resin emulsion sinter molding, make transition varnished cloth;
S14, intermediate coat molding with cloth: transition varnished cloth is replaced glass fabric, repeat S11, S12, S13 step 3-10 time, make middle varnished cloth;
Further, a kind of viscosity varnished cloth preparation method, comprises the following steps:
S11, glass-fiber-fabric flood: provide glass fabric and fluoro-resin emulsion, glass fabric is flooded fluoro-resin emulsion;
S12, glass-fiber-fabric are dried: by the glass fabric dry 1-10min under 50 DEG C of-150 DEG C of conditions after dipping fluoro-resin emulsion, remove moisture, then under 200 DEG C of-320 DEG C of conditions, cure 1-10min, remove each analog assistant;
S13, high temperature sintering: process 1-10min under making the glass fabric after oven dry be in 350 DEG C of-400 DEG C of conditions, by fluoro-resin emulsion sinter molding, make transition varnished cloth;
S14, intermediate coat molding with cloth: transition varnished cloth is replaced glass fabric, repeat S11, S12, S13 step 3-10 time, make middle varnished cloth;
S20, middle varnished cloth cover glue: by middle varnished cloth dipping or fluororesin-coated emulsion, ensure that at least one side is covered with fluoro-resin emulsion;
S30, middle varnished cloth are dried: by the middle varnished cloth dry 1-10min under 50 DEG C of-150 DEG C of conditions after dipping or fluororesin-coated emulsion, remove moisture, then under 200 DEG C of-320 DEG C of conditions, cure 1-10min, remove each analog assistant;
S40, viscosity varnished cloth are shaping: process 1-10min under the middle varnished cloth after order oven dry is in 320-350 DEG C of condition, make the fluoro-resin emulsion of dipping or coating in step S20 be in slight sintering or non-sintering state, make viscosity varnished cloth.
Particularly, transition varnished cloth, a kind of intermediateness of middle varnished cloth representative products in processing procedure, viscosity varnished cloth represents a kind of varnished cloth stronger with Copper Foil adhesive power.
Particularly, cure under 200 DEG C of-300 DEG C of conditions in step S12 and step S30 and remove each analog assistant, contribute to the process based prediction model stability improving fluororesin layer.
Particularly, repeat step S11, the number of times of S12, S13 determines according to the thickness requirement of different varnished cloth in step S14, namely the number of times of transition varnished cloth dipping fluoro-resin emulsion is determined for the requirement of thickness according to different varnished cloth.
Particularly, the molecular structure of the fluororesin layer that high temperature sintering is shaping is in inert condition in step s 13, surface cementitiousness is more weak, and the surperficial cementitiousness being in the fluororesin layer of slight sintering or non-sintering state formed in step s 40 obviously strengthens, the bond effect when boning with Copper Foil is especially obvious.Further, in step s 12, by the glass fabric dry 4-7min under 80-120 DEG C of condition after dipping fluoro-resin emulsion, remove moisture, then under 250-300 DEG C of condition, cure 4-7min, remove each analog assistant.Further, in step s 13, process 4-7min under making the glass fabric after oven dry be in 360-380 DEG C of condition, by fluoro-resin emulsion sinter molding, make transition varnished cloth.
Further, in step s 30, by the middle varnished cloth dry 4-7min under 80-120 DEG C of condition after dipping or fluororesin-coated emulsion, remove moisture, then under 280-320 DEG C of condition, cure 4-7min, remove each analog assistant.Further, in step s 40, under the middle varnished cloth after order oven dry is in 330-340 DEG C of condition, process 4-7min, make the fluoro-resin emulsion of dipping or coating in step S20 be in slight sintering or non-sintering state, make viscosity varnished cloth.
Further, a fluororesin-coated emulsion in side of described middle varnished cloth.
Only in a fluororesin-coated emulsion in side of described middle varnished cloth, namely described viscosity varnished cloth only has a side to have to be in the fluororesin layer of slight sintering or non-sintering state, use during described viscosity varnished cloth and the side and Copper Foil with the fluororesin layer being in slight sintering or non-sintering state are bonded, can to tackify the adhesion reliability of varnished cloth and Copper Foil, the consumption of fluoro-resin emulsion can be saved again, effectively reduce production cost.
Further, whole sides of described middle varnished cloth are flooded or fluororesin-coated emulsion.
As the preferred technical scheme of one, described fluoro-resin emulsion is by 100 parts by weight, comprise the PTFE emulsion of 80-100 part, and copolymer ETFE, the Kynoar PVDF of the perfluoroethylene-propylene emulsion FEP of 0-20 part, polytetrafluoroethylene (PTFE) perfluoroalkyl vinyl ether emulsion PFA, tetrafluoroethene and ethene, one or more any combination in polytrifluorochloroethylene PCTFE.
As the preferred technical scheme of one, described fluoro-resin emulsion also comprises inorganic filler and diluent, wherein said inorganic filler is the mixture of any one or at least two kinds in silica, aluminium oxide, aluminium nitride, boron nitride, titanium dioxide, barium titanate, barium sulfate, talcum powder, aluminium hydroxide, lithopone, calcium carbonate, wollastonite, kaolin, shepardite, diatomite, bentonite, silicon powder, ground pumice, and described diluent is nonionic surface active agent or distilled water.
Further, described inorganic filler is the mixture of any one or at least two kinds in silica, titanium dioxide, barium titanate.Further, described inorganic filler is that silica is or/and titanium dioxide.
Further, the particle diameter of described inorganic filler is within 12 μm.Further, the particle diameter of described inorganic filler is within 8 μm.Again further, the particle diameter of described inorganic filler is within 5 μm.
Further, the surface of described inorganic filler adopts coupling agent to process.Further, described coupling agent is the coupling agent with vinyl.
Further, described fluoro-resin emulsion is the PTFE emulsion of 90 parts and the perfluoroethylene-propylene emulsion FEP of 10 parts.
Further, described fluoro-resin emulsion is PTFE emulsion and the silica of 100 parts.
Further, described fluoro-resin emulsion is PTFE emulsion and the distilled water of 100 parts.
Further, described fluoro-resin emulsion is the PTFE emulsion of 100 parts.
As the preferred technical scheme of one, described high temperature sintering temperature is 350 DEG C-400 DEG C, and described low-temperature sintering temperature is 320 DEG C-350 DEG C.
As the preferred technical scheme of one, in described middle varnished cloth dipping or fluororesin-coated emulsion process, the one side thickness of fluororesin layer after removing moisture and auxiliary agent controlling dipping or coating is 3-20 μm.
Particularly, the one side thickness of fluororesin layer is too small, the adhesive power of described viscosity varnished cloth and Copper Foil will be caused to reduce, but the one side thickness of fluororesin layer is larger, the baking temperature needed in production process, stoving temperature and forming temperature are higher, the drying time simultaneously needed, the time of curing and molding time are longer, and production control difficulty is also larger, thus cause integral production cost to improve.
Further, the one side thickness of outermost layer fluororesin layer after removing moisture and auxiliary agent is 5 ~ 15 μm.
Further, the one side thickness of outermost layer fluororesin layer after removing moisture and auxiliary agent is 10 μm.
On the other hand, a kind of viscosity varnished cloth made by above-mentioned viscosity varnished cloth preparation method, comprise glass fabric and be coated on some layers of fluororesin layer outside glass fabric, the outermost layer fluororesin layer of described viscosity varnished cloth is in slight sintering or non-sintering state.
Further, middle varnished cloth is made up of step S11, S12, S13 and S14, and described middle varnished cloth comprises glass fabric and is coated on some layers of fluororesin layer outside glass fabric, and the fluororesin layer outside described middle varnished cloth is sintering state.
Particularly, comparatively by force, and the adhesive power that described middle varnished cloth outermost layer is in the fluororesin layer of sintering state and Copper Foil is more weak for the adhesive power of the fluororesin layer that described viscosity varnished cloth outermost layer is in slight sintering or non-sintering state and Copper Foil.But the production process of described middle varnished cloth is simple, and production cost is low, therefore, the basis using described viscosity varnished cloth makes full use of described middle varnished cloth, be conducive to reducing overall use cost.
As the preferred technical scheme of one, the one side thickness of the outermost layer fluororesin layer of described viscosity varnished cloth is 3-20 μm.
Another aspect, a kind of copper-clad plate of being made up of above-mentioned viscosity varnished cloth, comprise varnished cloth layer, and cover the Copper Foil on described varnished cloth layer, the position that described varnished cloth layer contacts with described Copper Foil is that described viscosity varnished cloth outermost layer is in and slightly sinters or the fluororesin layer of non-sintering state.
As the preferred technical scheme of one, described varnished cloth layer is formed by stacking primarily of some middle varnished cloths and viscosity varnished cloth, the side of described varnished cloth layer has covered described Copper Foil, the outermost layer of described varnished cloth layer near described Copper Foil side is viscosity varnished cloth, and the fluororesin layer that this viscosity varnished cloth outermost layer is in slight sintering or non-sintering state directly contacts with described Copper Foil.
Further, the position that described varnished cloth layer does not contact with described Copper Foil is any combination of middle varnished cloth or viscosity varnished cloth or middle varnished cloth and viscosity varnished cloth.
Particularly, although the adhesive power that described middle varnished cloth outermost layer is in the fluororesin layer of sintering state and Copper Foil is more weak, this fluororesin layer being in sintering state can make to realize durable bond between middle varnished cloth and between middle varnished cloth and viscosity varnished cloth.Therefore, the inside of described varnished cloth layer arranges described middle varnished cloth, effectively can reduce the holistic cost of described varnished cloth layer, ensures the bonding effect of described varnished cloth layer inside simultaneously.
As the preferred technical scheme of one, described middle varnished cloth and described viscosity varnished cloth include glass fabric, and described glass fabric adopts electron level alkali-free glass fiber cloth.
Further, described glass fabric adopts 106,1080,2116 or 7628 electron level alkali-free glass fiber cloths.
Beneficial effect of the present invention is: provide a kind of viscosity varnished cloth preparation method, make the viscosity varnished cloth stronger with the cementitiousness of Copper Foil, effectively improves the bonding force of varnished cloth and Copper Foil, solves the problem of varnished cloth and Copper Foil bond difficult.The viscosity varnished cloth be made up of above-mentioned viscosity varnished cloth preparation method is provided simultaneously.The present invention also provides a kind of copper-clad plate, by arranging viscosity varnished cloth, effectively improves the peel strength of varnished cloth and Copper Foil.
Accompanying drawing explanation
According to drawings and embodiments the present invention is described in further detail below.
Fig. 1 is the flow chart of the viscosity varnished cloth preparation method according to one embodiment of the invention;
Fig. 2 is the cross-sectional view of copper-clad plate described according to a first embodiment of the present invention;
Fig. 3 is the cross-sectional view of copper-clad plate described according to a third embodiment of the present invention;
Fig. 4 is the cross-sectional view of copper-clad plate described according to a fourth embodiment of the present invention.
In Fig. 2 to Fig. 4:
1, middle varnished cloth; 2, viscosity varnished cloth; 3, Copper Foil.
Detailed description of the invention
Technical scheme of the present invention is further illustrated by detailed description of the invention below in conjunction with accompanying drawing.
Fig. 1 is the flow chart of the viscosity varnished cloth preparation method provided according to one embodiment of the invention.As shown in Figure 1, in the present embodiment, viscosity varnished cloth preparation method comprises the following steps: S11, glass-fiber-fabric flood: provide glass fabric and fluoro-resin emulsion, glass fabric is flooded fluoro-resin emulsion; S12, glass-fiber-fabric are dried: by the glass fabric dry 1-10min under 50 DEG C of-150 DEG C of conditions after dipping fluoro-resin emulsion, remove moisture, then under 200 DEG C of-320 DEG C of conditions, cure 1-10min, remove each analog assistant; S13, high temperature sintering: process 1-10min under making the glass fabric after oven dry be in 350 DEG C of-400 DEG C of conditions, by fluoro-resin emulsion sinter molding, make transition varnished cloth; S14, intermediate coat molding with cloth: transition varnished cloth is replaced glass fabric, repeat S11, S12, S13 step 3-10 time, make middle varnished cloth; S20, middle varnished cloth cover glue: by middle varnished cloth dipping or fluororesin-coated emulsion, ensure that at least one side is covered with fluoro-resin emulsion; S30, middle varnished cloth are dried: by the middle varnished cloth dry 1-10min under 50 DEG C of-150 DEG C of conditions after dipping or fluororesin-coated emulsion, remove moisture, then under 200 DEG C of-320 DEG C of conditions, cure 1-10min, remove each analog assistant; S40, viscosity varnished cloth are shaping: process 1-10min under the middle varnished cloth after order oven dry is in 320-350 DEG C of condition, make the fluoro-resin emulsion of dipping or coating in step S20 be in slight sintering or non-sintering state, make viscosity varnished cloth.
Embodiments of the invention additionally provide viscosity varnished cloth product, and this viscosity varnished cloth combines one or more varnished cloth preparation methods of the present invention to produce.This viscosity varnished cloth be used to make copper-clad plate, this copper-clad plate comprises varnished cloth and Copper Foil, the varnished cloth of the copper-clad plate made thus and the peel strength of copper foil layer high.
Fluoro-resin emulsion of the present invention is by 100 parts by weight, comprise the PTFE emulsion of 80-100 part, and copolymer ETFE, the Kynoar PVDF of the perfluoroethylene-propylene emulsion FEP of 0-20 part, polytetrafluoroethylene (PTFE) perfluoroalkyl vinyl ether emulsion PFA, tetrafluoroethene and ethene, one or more any combination in polytrifluorochloroethylene PCTFE.Described fluoro-resin emulsion also comprises inorganic filler and diluent, wherein said inorganic filler is the mixture of any one or at least two kinds in silica, aluminium oxide, aluminium nitride, boron nitride, titanium dioxide, barium titanate, barium sulfate, talcum powder, aluminium hydroxide, lithopone, calcium carbonate, wollastonite, kaolin, shepardite, diatomite, bentonite, silicon powder, ground pumice, the surface of described inorganic filler adopts the coupling agent with vinyl to process, and the particle diameter of described inorganic filler is within 12 μm.Described diluent is nonionic surface active agent or distilled water.
Fig. 2 is the cross-sectional view of copper-clad plate described according to a first embodiment of the present invention.As shown in Figure 2, in the first embodiment, method for manufacturing cover clad laminate of the present invention is as follows:
1, Copper Foil and glass fabric are provided, and prepare fluoro-resin emulsion
The Copper Foil of the 1oz that Copper Foil adopts Feitian, Suzhou to provide.Glass fabric adopts 1080 electron level alkali-free glass fiber cloths.Fluoro-resin emulsion, by 100 parts by weight, comprises the PTFE emulsion of 95 parts and the perfluoroethylene-propylene emulsion FEP of 5 parts.Fluoro-resin emulsion adopts nonionic surface active agent to regulate solids content and viscosity, and make the solids content of fluoro-resin emulsion be 35-60%, viscosity is 15-40mPas (under 20 DEG C of conditions).
2, varnished cloth in the middle of preparation
Use above-mentioned fluoro-resin emulsion to flood 1080 electron level alkali-free glass fiber cloths, make all surfaces of glass fabric be covered with this fluoro-resin emulsion; Then by the glass fabric dry 3-4min under 80-120 DEG C of condition after dipping fluoro-resin emulsion, remove moisture, under 290-310 DEG C of condition, cure 4-5min, remove the auxiliary agent of all kinds of low temperature volatilization; Then process 3-4min under making the glass fabric after oven dry be in 360-380 DEG C of condition, by fluoro-resin emulsion sinter molding, make transition varnished cloth; Finally transition varnished cloth is replaced glass fabric, repeat above-mentioned steps 5 times, make the middle varnished cloth that thickness is 70-80 μm.
3, viscosity varnished cloth is prepared
Use above-mentioned fluoro-resin emulsion to flood middle varnished cloth, make all surfaces of middle varnished cloth be covered with this fluoro-resin emulsion; Then by the middle varnished cloth dry 3-4min under 80-120 DEG C of condition after dipping fluoro-resin emulsion, remove moisture, under 290-310 DEG C of condition, cure 4-5min, remove the auxiliary agent of all kinds of low temperature volatilization; Process 3-4min under middle varnished cloth after finally order oven dry is in 330-340 DEG C of condition, the fluoro-resin emulsion making this flood is in slight sintering or non-sintering state, and the thickness controlling the fluororesin layer that this is covered with is 5-10 μm, makes viscosity varnished cloth.
4, copper-clad plate is prepared
With reference to the structure for covering copper plate shown in Fig. 2,12 blocks of middle varnished cloths are superimposed together, and one block of viscosity varnished cloth of respectively fitting in the both sides of 12 blocks of middle varnished cloths, form varnished cloth layer, then to fit respectively in the both sides of varnished cloth layer the Copper Foil of one piece of 1oz, at 360-380 DEG C/2-5h, pressure is carry out lamination under the condition of 50-100kg/cm2, makes copper-clad plate.
First comparative example is corresponding with the first embodiment of the present invention, and the copper-clad plate of the first comparative example adopts conventional fabrication method, specific as follows:
1, Copper Foil and glass fabric are provided, and prepare fluoro-resin emulsion.
The Copper Foil of the 1oz that Copper Foil adopts Feitian, Suzhou to provide.Glass fabric adopts 1080 electron level alkali-free glass fiber cloths.Fluoro-resin emulsion, by 100 parts by weight, comprises the PTFE emulsion of 95 parts and the perfluoroethylene-propylene emulsion FEP of 5 parts.Fluoro-resin emulsion adopts nonionic surface active agent to regulate solids content and viscosity, and make the solids content of fluoro-resin emulsion be 35-60%, viscosity is 15-40mPas (under 20 DEG C of conditions).
2, varnished cloth in the middle of preparation
Use above-mentioned fluoro-resin emulsion to flood 1080 electron level alkali-free glass fiber cloths, make all surfaces of glass fabric be covered with this fluoro-resin emulsion; Then by the glass fabric dry 3-4min under 80-120 DEG C of condition after dipping fluoro-resin emulsion, remove moisture, under 290-310 DEG C of condition, cure 4-5min, remove the auxiliary agent of all kinds of low temperature volatilization; Then process 3-4min under making the glass fabric after oven dry be in 360-380 DEG C of condition, by fluoro-resin emulsion sinter molding, make transition varnished cloth; Finally transition varnished cloth is replaced glass fabric, repeat above-mentioned steps 5 times, make the middle varnished cloth that thickness is 70-80 μm.
3, copper-clad plate is prepared
Be superimposed together by 14 blocks of middle varnished cloths, form varnished cloth layer, the Copper Foil of the one piece of 1oz that then fits respectively in the both sides of varnished cloth layer, at 360-380 DEG C/2-5h, pressure is carry out lamination under the condition of 50-100kg/cm2, makes copper-clad plate.
Two kinds of copper-clad plates of making in the first embodiment and the first comparative example are carried out the contrast experiment of varnished cloth layer and peel strength of copper foil, result is as follows:
The peel strength of copper foil of the copper-clad plate with viscosity varnished cloth of making in the first embodiment in four experiments is respectively 1.72,1.69,1.75,1.8, mean value is 1.74, all be greater than the peel strength of copper foil of the copper-clad plate of making in the first comparative example, as can be seen here, the varnished cloth layer of copper-clad plate that makes of the inventive method and copper foil layer peel strength high.
Copper Foil in first embodiment and the first comparative example is replaced by the Copper Foil of the 1oz that Luxembourg provides by the second embodiment of the present invention and the second comparative example respectively, make two kinds of copper-clad plates respectively, and carry out the contrast experiment of varnished cloth layer and peel strength of copper foil, result is as follows:
The peel strength of copper foil of the copper-clad plate with viscosity varnished cloth of making in the second embodiment in four experiments is respectively 3.2,3.1,3.24,3.27, mean value is 3.2, all be greater than the peel strength of copper foil of the copper-clad plate of making in the second comparative example, as can be seen here, preparation method of the present invention can improve varnished cloth layer and the copper foil layer peel strength of copper-clad plate.
Fig. 3 is the cross-sectional view of copper-clad plate described according to a third embodiment of the present invention.As shown in Figure 3, the preparation method of the copper-clad plate of the present embodiment is as follows:
1, Copper Foil and glass fabric are provided, and prepare fluoro-resin emulsion
The Copper Foil of the 1oz that Copper Foil adopts Feitian, Suzhou to provide.Glass fabric adopts 106 electron level alkali-free glass fiber cloths.Fluoro-resin emulsion, by 100 parts by weight, comprises PTFE emulsion and the silica of 100 parts.Fluoro-resin emulsion adopts nonionic surface active agent to regulate solids content and viscosity, and make the solids content of fluoro-resin emulsion be 40-65%, viscosity is 20-45mPas (under 20 DEG C of conditions).
2, varnished cloth in the middle of preparation
Use above-mentioned fluoro-resin emulsion to flood 106 electron level alkali-free glass fiber cloths, make all surfaces of glass fabric be covered with this fluoro-resin emulsion; Then by the glass fabric dry 1-3min under 50-100 DEG C of condition after dipping fluoro-resin emulsion, remove moisture, under 250-300 DEG C of condition, cure 3-4min, remove the auxiliary agent of all kinds of low temperature volatilization; Then process 1-3min under making the glass fabric after oven dry be in 350-370 DEG C of condition, by fluoro-resin emulsion sinter molding, make transition varnished cloth; Finally transition varnished cloth is replaced glass fabric, repeat above-mentioned steps 5 times, make the middle varnished cloth that thickness is 70-80 μm.
3, viscosity varnished cloth is prepared
Use above-mentioned fluoro-resin emulsion to flood middle varnished cloth, make all surfaces of middle varnished cloth be covered with this fluoro-resin emulsion; Then by the middle varnished cloth dry 1-3min under 50-100 DEG C of condition after dipping fluoro-resin emulsion, remove moisture, under 250-300 DEG C of condition, cure 3-4min, remove the auxiliary agent of all kinds of low temperature volatilization; Process 1-3min under middle varnished cloth after finally order oven dry is in 320-330 DEG C of condition, the fluoro-resin emulsion making this flood is in slight sintering or non-sintering state, and the thickness controlling the fluororesin layer that this is covered with is 3-5 μm, makes viscosity varnished cloth.
4, copper-clad plate is prepared
With reference to the structure for covering copper plate shown in Fig. 3,6 blocks of middle varnished cloths and 5 blocks of viscosity varnished cloths are superimposed and staggered, and one block of viscosity varnished cloth of respectively fitting in the both sides of these 11 blocks of varnished cloths, form varnished cloth layer, then to fit respectively in the both sides of varnished cloth layer the Copper Foil of one piece of 1oz, at 360-380 DEG C/2-5h, pressure is carry out lamination under the condition of 50-100kg/cm2, makes copper-clad plate.
Fig. 4 is the cross-sectional view of copper-clad plate described according to a fourth embodiment of the present invention.As shown in Figure 4, the preparation method of the copper-clad plate of the present embodiment is as follows:
1, Copper Foil and glass fabric are provided, and prepare fluoro-resin emulsion
The Copper Foil of the 1oz that Copper Foil adopts Feitian, Suzhou to provide.Glass fabric adopts 7628 electron level alkali-free glass fiber cloths.Fluoro-resin emulsion, by 100 parts by weight, comprises the PTFE emulsion of 100 parts.Fluoro-resin emulsion adopts distilled water to regulate solids content and viscosity, and make the solids content of fluoro-resin emulsion be 35-60%, viscosity is 15-40mPas (under 20 DEG C of conditions).
2, varnished cloth in the middle of preparation
Use above-mentioned fluoro-resin emulsion to flood 7628 electron level alkali-free glass fiber cloths, make all surfaces of glass fabric be covered with this fluoro-resin emulsion; Then by the glass fabric dry 4-6min under 90-130 DEG C of condition after dipping fluoro-resin emulsion, remove moisture, under 290-320 DEG C of condition, cure 6-7min, remove the auxiliary agent of all kinds of low temperature volatilization; Then process 4-6min under making the glass fabric after oven dry be in 370-390 DEG C of condition, by fluoro-resin emulsion sinter molding, make transition varnished cloth; Finally transition varnished cloth is replaced glass fabric, repeat above-mentioned steps 5 times, make the middle varnished cloth that thickness is 70-80 μm.
3, viscosity varnished cloth is prepared
Use above-mentioned fluoro-resin emulsion to flood middle varnished cloth, make all surfaces of middle varnished cloth be covered with this fluoro-resin emulsion; Then by the middle varnished cloth dry 4-6min under 90-130 DEG C of condition after dipping fluoro-resin emulsion, remove moisture, under 290-320 DEG C of condition, cure 6-7min, remove the auxiliary agent of all kinds of low temperature volatilization; Process 4-6min under middle varnished cloth after finally order oven dry is in 330-340 DEG C of condition, the fluoro-resin emulsion making this flood is in slight sintering or non-sintering state, and the thickness controlling the fluororesin layer that this is covered with is 10-15 μm, makes viscosity varnished cloth.
4, copper-clad plate is prepared
With reference to the structure for covering copper plate shown in Fig. 4, varnished cloth in the middle of 7 blocks of viscosity varnished cloths and 6 pieces is superimposed and staggered, forms varnished cloth layer, then to fit in the side of varnished cloth layer the Copper Foil of one piece of 1oz, at 360-380 DEG C/2-5h, pressure is carry out lamination under the condition of 50-100kg/cm2, makes copper-clad plate.
In description of the invention, it is to be appreciated that term " first ", " second ", " the 3rd ", " the 4th " only for being distinguished in description, not special implication.
It is to be understood that; above-mentioned detailed description of the invention is only preferred embodiment of the present invention and institute's application technology principle; in technical scope disclosed in this invention, the change that any those skilled in the art of being familiar with easily expect or replacement, all should be encompassed in protection scope of the present invention.
Claims (10)
1. a viscosity varnished cloth preparation method, is characterized in that, at least comprises the following steps:
S10, make in the middle of varnished cloth: carry out drying after glass fabric being flooded fluoro-resin emulsion, cure, high temperature sintering process, and repeat dry, cure, high temperature sintering process obtains middle varnished cloth for 3-10 time;
S20, middle varnished cloth cover glue: by middle varnished cloth dipping or fluororesin-coated emulsion, ensure that at least one side is covered with fluoro-resin emulsion;
S30, middle varnished cloth are dried: the middle varnished cloth after dipping or fluororesin-coated emulsion is carried out to drying and cures process, remove moisture and each analog assistant;
S40, viscosity varnished cloth are shaping: the middle varnished cloth after order oven dry processes 1-10min under low-temperature sintering temperature environment, described low-temperature sintering temperature is lower than high temperature sintering temperature 0-80 DEG C, make the fluoro-resin emulsion of dipping or coating in step S20 be in slight sintering or non-sintering state, make viscosity varnished cloth.
2. viscosity varnished cloth preparation method according to claim 1, it is characterized in that, described fluoro-resin emulsion is by 100 parts by weight, comprise the PTFE emulsion of 80-100 part, and copolymer ETFE, the Kynoar PVDF of the perfluoroethylene-propylene emulsion FEP of 0-20 part, polytetrafluoroethylene (PTFE) perfluoroalkyl vinyl ether emulsion PFA, tetrafluoroethene and ethene, one or more any combination in polytrifluorochloroethylene PCTFE.
3. viscosity varnished cloth preparation method according to claim 2, it is characterized in that, described fluoro-resin emulsion also comprises inorganic filler and diluent, wherein said inorganic filler is the mixture of any one or at least two kinds in silica, aluminium oxide, aluminium nitride, boron nitride, titanium dioxide, barium titanate, barium sulfate, talcum powder, aluminium hydroxide, lithopone, calcium carbonate, wollastonite, kaolin, shepardite, diatomite, bentonite, silicon powder, ground pumice, and described diluent is nonionic surface active agent or distilled water.
4. viscosity varnished cloth preparation method according to claim 1, is characterized in that, described high temperature sintering temperature is 350 DEG C-400 DEG C, and described low-temperature sintering temperature is 320 DEG C-350 DEG C.
5. the viscosity varnished cloth preparation method according to any one of Claims 1-4, it is characterized in that, in described middle varnished cloth dipping or fluororesin-coated emulsion process, the one side thickness of fluororesin layer after removing moisture and auxiliary agent controlling dipping or coating is 3-20 μm.
6. a viscosity varnished cloth, it is characterized in that, made by the viscosity varnished cloth preparation method described in any one of claim 1 to 5, viscosity varnished cloth comprises glass fabric and is coated on some layers of fluororesin layer outside glass fabric, and the outermost layer fluororesin layer of described viscosity varnished cloth is in slight sintering or non-sintering state.
7. viscosity varnished cloth according to claim 6, is characterized in that, the one side thickness of the outermost layer fluororesin layer of described viscosity varnished cloth is 3-20 μm.
8. a copper-clad plate of being made up of the viscosity varnished cloth described in claim 6 or 7, it is characterized in that, comprise varnished cloth layer, and the Copper Foil covered on described varnished cloth layer, the position that described varnished cloth layer contacts with described Copper Foil is that described viscosity varnished cloth outermost layer is in and slightly sinters or the fluororesin layer of non-sintering state.
9. copper-clad plate according to claim 8, it is characterized in that, described varnished cloth layer is formed by stacking primarily of some middle varnished cloths and viscosity varnished cloth, the side of described varnished cloth layer has covered described Copper Foil, the outermost layer of described varnished cloth layer near described Copper Foil side is viscosity varnished cloth, and the fluororesin layer that this viscosity varnished cloth outermost layer is in slight sintering or non-sintering state directly contacts with described Copper Foil.
10. copper-clad plate according to claim 9, is characterized in that, described middle varnished cloth and described viscosity varnished cloth include glass fabric, and described glass fabric adopts electron level alkali-free glass fiber cloth.
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| CN105862395A (en) * | 2016-04-28 | 2016-08-17 | 江苏富仕德科技发展有限公司 | High-thermal-conductivity-coefficient glass fiber cloth and manufacturing method thereof |
| CN106274007A (en) * | 2016-07-30 | 2017-01-04 | 龙宇电子(梅州)有限公司 | For multilayer printed wiring board and the preparation method of the cushion pad of copper-clad plate process for pressing |
| CN107385936A (en) * | 2017-07-12 | 2017-11-24 | 广东生益科技股份有限公司 | A kind of method for preparing PTFE varnished cloths, the PTFE varnished cloths and metal-clad laminate prepared by this method |
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| CN114179461A (en) * | 2021-11-08 | 2022-03-15 | 安徽鸿海新材料股份有限公司 | Glass fiber cloth reinforced copper-clad plate and preparation method thereof |
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| CN105572947A (en) * | 2016-03-18 | 2016-05-11 | 京东方科技集团股份有限公司 | Array base plate and manufacturing method thereof as well as display device |
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| CN105862395A (en) * | 2016-04-28 | 2016-08-17 | 江苏富仕德科技发展有限公司 | High-thermal-conductivity-coefficient glass fiber cloth and manufacturing method thereof |
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| CN106274007A (en) * | 2016-07-30 | 2017-01-04 | 龙宇电子(梅州)有限公司 | For multilayer printed wiring board and the preparation method of the cushion pad of copper-clad plate process for pressing |
| CN106274007B (en) * | 2016-07-30 | 2018-12-25 | 龙宇电子(梅州)有限公司 | Preparation method for multilayer printed wiring board and the cushion of copper-clad plate process for pressing |
| CN107385936A (en) * | 2017-07-12 | 2017-11-24 | 广东生益科技股份有限公司 | A kind of method for preparing PTFE varnished cloths, the PTFE varnished cloths and metal-clad laminate prepared by this method |
| CN107385936B (en) * | 2017-07-12 | 2019-12-17 | 广东生益科技股份有限公司 | method for preparing PTFE (Polytetrafluoroethylene) varnished cloth, PTFE varnished cloth prepared by method and metal foil-clad laminated board |
| CN112248595A (en) * | 2020-09-22 | 2021-01-22 | 瑞声新能源发展(常州)有限公司科教城分公司 | Insulating plate and preparation method thereof, laminated plate and preparation method and application thereof |
| WO2022061970A1 (en) * | 2020-09-22 | 2022-03-31 | 瑞声声学科技(深圳)有限公司 | Insulation board and preparation method therefor, laminate and preparation method therefor, and application of insulation board or laminate |
| WO2022110389A1 (en) * | 2020-11-30 | 2022-06-02 | 瑞声声学科技(深圳)有限公司 | Method for preparing flexible insulation board and flexible insulation board obtained using same, flexible laminate and method for preparing same, and application |
| CN114179461A (en) * | 2021-11-08 | 2022-03-15 | 安徽鸿海新材料股份有限公司 | Glass fiber cloth reinforced copper-clad plate and preparation method thereof |
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