CN101838431B - Fluororesin mixture, copper-clad plate prepared therefrom and manufacturing method thereof - Google Patents
Fluororesin mixture, copper-clad plate prepared therefrom and manufacturing method thereof Download PDFInfo
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Abstract
The invention relates to a fluororesin mixture, a copper-clad plate prepared therefrom and a manufacturing method thereof. The fluororesin mixture contains the following two substances as necessary components in 100 parts by weight of an organic solid substance: 90-99 parts of polytetrafluoroethylene (PTFE) emulsions and 1-10 parts of polytetrafluoroethylene perfluoroalkyl vinyl ether (PFA) emulsions. The copper-clad plate prepared from the fluororesin mixture comprises a plurality of superimposed varnished cloths and copper foil coating one or two surfaces of the varnished cloths, and each varnished cloth comprises a glass fiber cloth and the fluororesin mixture attached to the dipped and dried glass fiber cloth. The fluororesin mixture is prepared by using the PTFE emulsions as main resins and can dip the glass fiber cloths many times under the condition that the PTFE sintering temperature is330 DEG C to prepare the vanished cloths, and the vanished cloths prepared from the fluororesin mixture has the advantages of good gum dipping quality, level surface, flexibility and easy operation; and besides, the copper-clad plate made from the fluororesin mixture has excellent dielectric performance which meets the dielectric performance requirement of the high-frequency communication field for a base plate material, and has simple making method and process and is beneficial to industrial continuous production.
Description
Technical field
The present invention relates to a kind of fluoro-resin mixture, relate in particular to a kind of fluoro-resin mixture, use copper-clad plate of its making and preparation method thereof.
Background technology
Polytetrafluoroethylene (PTFE) is since 1945 are produced by the E.I.Du Pont Company commercialization; Because physicals and chemical property that this material is unique; People just constantly open up the application of this material in every field; Wherein to utilize the outstanding dielectric properties (low-k and low dielectric loss) of PTFE material to make the copper-clad plate of frequency applications existing historical for many years, introduced the method that fluoro-resin dipping glass cloth is made the glass varnished cloth like USP 2539329; USP 3136680 is patents of introducing the PTFE copper-clad plate the earliest, and it is that one deck perfluoroethylene-propylene (copolymer) film is covered on the surface again by PTFE emulsion dipping glass cloth, and the Copper Foil pressing of handling with NI-G again forms; USP 03556161 has been introduced the method for making sheet material with the PTFE micro mist, is the technical foundation that follow-up filler is filled the copper-clad plate of no glass cloth enhancement type; USP 4335180 has been introduced a kind of fluoropolymer, mineral filler, glass fiber yarn and has been mixed a kind of rubber cement, adds flocculation agent and makes rubber cement flocculate into the dough object, and oven dry is pressed into sheet material then, covers the method that copper forms copper-clad plate again; It is the high-frequency copper-clad plate that stopping composition that main stuffing is made the PTFE emulsion is made low-k and low thermal coefficient of expansion with the silicon powder that USP 4849284 has been introduced; USP 4886699 has been introduced the high-frequency copper-clad plate that glass cloth coating agent which has to be dissolved in alcohol before use and glass yarn sheet material are combined into insulating substrate, and it is higher to have solved conventional P TFE copper-clad plate or specific inductivity, or the problem of poor dimensional stability.
Used PTFE glass cloth coating agent which has to be dissolved in alcohol before use is generally all through repeatedly just meeting the requirements of resin content behind dipping, drying, the sintering in the above-mentioned technology; And the PTFE coating agent which has to be dissolved in alcohol before use smooth surface behind the sintering and, thereby influence follow-up quality of impregnation again and final board quality because of resin shrinkage can produce certain curling; And mentioned in the USP 2539329 PTFE glass cloth coating agent which has to be dissolved in alcohol before use is carried out pre-treatment with 205 ℃; The method of flooding again after rolling is improved " mud crack " phenomenon that the PTFE overweight coating produces; There is former coating caducous phenomenon during impregnation again in this method; Because PTFE only is tight arrangement, do not form as twining the all-in-one-piece film behind the sintering, be not suitable for industrialized continuous production.
Summary of the invention
The object of the present invention is to provide a kind of fluoro-resin mixture, by the varnished cloth that this fluoro-resin mixture dipping makes, gel content is even, the impregnation quality is good, surfacing, soft easy to operate.
Another object of the present invention is to provide a kind of copper-clad plate of using above-mentioned fluoro-resin mixture to make, this copper-clad plate over-all properties is good, and dielectric properties are excellent, satisfy the dielectric properties requirement of high-frequency communication field to baseplate material.
Another purpose of the present invention is to provide the making method of above-mentioned copper-clad plate, and this procedure is simple, helps industrialized continuous production.
For realizing above-mentioned purpose; The present invention provides a kind of fluoro-resin mixture; Contain following two kinds of materials as necessary component, in organic solid substance by 100 weight parts, wherein: polytetrafluoroethylene (PTFE) emulsion 90-99 part, tetrafluoroethylene perfluoroalkyl vinyl ether (PFA) emulsion 1-10 part.
Also comprise mineral filler and thinner, this mineral filler is silicon powder, kaolin or white titanium pigment, and thinner is non-ionics or zero(ppm) water.
The solids content of this fluoro-resin mixture is 35-60%, and viscosity is 15～40mPas (20 ℃).
Further; A kind of copper-clad plate of using above-mentioned fluoro-resin mixture to make is provided; This copper-clad plate is the PTFE copper-clad plate; It comprises: several superimposed varnished cloths, and be overlaid on the Copper Foil on the varnished cloth one or both sides, each varnished cloth comprises glass cloth and passes through impregnation drying postadhesion fluoro-resin mixture above that.
Glass cloth adopts the alkali-free glass fiber cloth of 106,1080 or 2116 electronic-grades.
In addition, the present invention also provides the making method of above-mentioned copper-clad plate, comprises that step is following:
Step 1 provides Copper Foil, glass cloth, and the preparation fluoro-resin mixture;
Step 2 uses the fluoro-resin mixture of above-mentioned preparation to flood glass cloth, and baking is dry; Baking comprises that two stages, fs storing temperature are 50-100 ℃, and the time is 2-5min, with transpiring moisture; The subordinate phase storing temperature is 200-320 ℃, and the time is 3-5min, to remove the volatilizable thing of low temperature.Repeat this step, obtain varnished cloth;
Step 3 is joined the above-mentioned varnished cloth that obtains is folded, and the two sides is covered with Copper Foil, carries out lamination, obtains copper-clad plate.Lamination is 360-380 ℃/2-5h, and pressure is 50-100kg/cm
2
Beneficial effect of the present invention: fluoro-resin mixture of the present invention is that matrix resin makes with the PTFE emulsion; This mixture can repeatedly flood glass cloth under PTFE sintering temperature (330 ℃) condition and make varnished cloth being lower than, the varnished cloth impregnation quality that is made by this fluoro-resin mixture is good, gel content evenly, surfacing, soft easy to operate; In addition, good by the copper-clad plate over-all properties that this fluorin resin composition is made, dielectric properties are excellent, satisfy the dielectric properties requirement of high-frequency communication field to baseplate material, and the making method process are simple, helps industrialized continuous production.
Embodiment
The present invention provides a kind of fluoro-resin mixture; This fluoro-resin mixture contains following two kinds of materials as necessary component; In organic solid substance by 100 weight parts, wherein: polytetrafluoroethylene (PTFE) emulsion 90-99 part, tetrafluoroethylene perfluoroalkyl vinyl ether (PFA) emulsion 1-10 part.Also comprise mineral filler and thinner, this mineral filler is silicon powder, kaolin or white titanium pigment, and thinner is non-ionics or zero(ppm) water.Also can comprise auxiliary agent, like emulsifying agent, dispersion agent etc.
Said fluoro-resin mixture can be regulated solids content and viscosity through thinner, and the solids content of this fluoro-resin mixture is 35-60%, and viscosity is 15～40mPas (20 ℃).
Said fluoro-resin mixture is a matrix resin with the PTFE emulsion; Add the PFA of an amount of melt-flowable; Regulate the solids content and the viscosity of emulsion with non-ionics or zero(ppm) water, can also optionally add mineral filler, like silicon powder, kaolin, white titanium pigment etc.FEP is prone to fusion and flows and film forming about 310 ℃; In fluoro-resin mixture of the present invention in organic solid substance by 100 weight parts; The PFA addition is 1-10 part, and this scope addition makes and can adhere on the glass cloth at matrix resin PTFE under the lower temperature, and difficult drop-off; Simultaneously, the good fluidity of PFA has remedied the not molten characteristic of PTFE, and there is good filling effect in the space among glass cloth and the PTFE.The PFA addition very little, then mobile deviation, and follow-up impregnation is prone to come off; The PFA addition is too many, then can have gummosis phenomenon bigger than normal during the higher and glass cloth of emulsion cost stack lamination.
Further; The present invention also provides a kind of copper-clad plate of adopting above-mentioned fluorin resin composition to make; This copper-clad plate is the PTFE copper-clad plate; It comprises: the varnished cloth that several are superimposed, and be overlaid on the Copper Foil on the varnished cloth one or both sides, each varnished cloth comprises glass cloth and passes through impregnation drying postadhesion fluoro-resin mixture above that.
Glass cloth adopts the alkali-free glass fiber cloth of 106,1080 or 2116 electronic-grades.Use above-mentioned fluoro-resin mixture dipping glass cloth; Under being lower than PTFE sintering temperature (330 ℃), carry out drying, can satisfy once more the requirement of impregnation after curing, degumming phenomenon can not occur, through the repeatedly prepared varnished cloth surfacing of impregnation; Do not contain the volatilizable thing of low temperature, soft easy to operate.
In addition, the present invention also provides the making method of above-mentioned copper-clad plate, and it comprises that step is following:
Step 1 provides Copper Foil, glass cloth, and the preparation fluoro-resin mixture.Wherein, Glass cloth adopts the alkali-free glass fiber cloth of 106,1080 or 2116 electronic-grades; Fluoro-resin mixture contains following two kinds of materials as necessary component; In organic solid substance by 100 weight parts, wherein: polytetrafluoroethylene (PTFE) emulsion 90-99 part, tetrafluoroethylene perfluoroalkyl vinyl ether (PFA) emulsion 1-10 part.Also can comprise mineral filler and thinner; This mineral filler is silicon powder, kaolin or white titanium pigment; Thinner is non-ionics or zero(ppm) water; Regulate solids content and viscosity through thinner, the solids content of this fluoro-resin mixture is 35-60%, and viscosity is 15～40mPas (20 ℃).
Step 2 uses the fluoro-resin mixture of above-mentioned preparation to flood glass cloth, and baking is dry.Baking comprises two stages, and the fs storing temperature is 50-100 ℃, and the time is 2-5min, with transpiring moisture; The subordinate phase storing temperature is 200-320 ℃, and the time is 3-5min, to remove the volatilizable thing of low temperature (like auxiliary agent).Repeat this step, up to the varnished cloth that obtains requiring resin content.The storing temperature of this step is low than conventional art, but save energy is enhanced productivity.
Step 3 is joined the above-mentioned varnished cloth that obtains is folded, and both sides are covered with Copper Foil, carry out lamination, obtain copper-clad plate.Lamination is 360-380 ℃/2-5h, and pressure is 50-100kg/cm
2It is fixed that varnished cloth quantity is come according to the thickness demand.
As a kind of embodiment that uses above-mentioned fluoro-resin mixture to make copper-clad plate; The copper-clad plate of this enforcement is 1.01/1 copper-clad plate; Adopt above-mentioned 1080 glass cloth; In above-mentioned fluoro-resin mixture, carry out impregnation, baking, repeat to obtain after five times the varnished cloth of required resin content, varnished cloth substance 130-140g/m
2, thickness is 0.07-0.08 μ m.Get varnished cloth 13-15 and open together range upon range ofly, the two sides is covered with Copper Foil respectively, and the Copper Foil of this embodiment is the Copper Foil of 1oz, at pressure 50-100kg/cm
2, temperature 360-380 ℃, carry out lamination under the condition of time 2-5h, make the copper-clad plate of this embodiment.Its performance is seen table 1.
The copper-clad plate performance that table 1 the foregoing description is made
| PS(N/mm) | Anti-immersed solder property (288 ℃) | Dk(1GHz) | Df(1GHz) |
| 1.8N/mm | ＞5min | 2.65 | 0.001 |
In sum; Fluoro-resin mixture of the present invention is that matrix resin makes with the PTFE emulsion; This mixture can repeatedly flood glass cloth under PTFE sintering temperature (330 ℃) condition and make varnished cloth being lower than, the varnished cloth impregnation quality that is made by this fluoro-resin mixture is good, gel content evenly, surfacing, soft easy to operate; In addition, good by the copper-clad plate over-all properties that this fluorin resin composition is made, dielectric properties are excellent, satisfy the dielectric properties requirement of high-frequency communication field to baseplate material, and the making method process are simple, helps industrialized continuous production.
Above embodiment; Be not that the content of compsn of the present invention is done any restriction; Every foundation technical spirit of the present invention or compsn composition or content all still belong in the scope of technical scheme of the present invention any trickle modification, equivalent variations and modification that above embodiment did.
Claims (5)
1. a fluoro-resin mixture is characterized in that, it contains following two kinds of materials as necessary component, in organic solid substance by 100 weight parts, wherein: ptfe emulsion 90-99 part, tetrafluoroethylene perfluoroalkyl vinyl ether emulsion 1-10 part; Also comprise mineral filler and thinner, this mineral filler is silicon powder, kaolin or white titanium pigment, and thinner is a non-ionics; The solids content of said fluoro-resin mixture is 35-60%, and in the time of 20 ℃, viscosity is 15～40mPas.
2. copper-clad plate of adopting fluoro-resin mixture as claimed in claim 1 to make; It is characterized in that; This copper-clad plate comprises: several superimposed varnished cloths; And being overlaid on the Copper Foil on the varnished cloth one or both sides, each varnished cloth comprises glass cloth and passes through impregnation drying postadhesion fluoro-resin mixture above that; Said fluoro-resin mixture contains following two kinds of materials as necessary component, in organic solid substance by 100 weight parts, wherein: ptfe emulsion 90-99 part, tetrafluoroethylene perfluoroalkyl vinyl ether emulsion 1-10 part; Also comprise mineral filler and thinner, this mineral filler is silicon powder, kaolin or white titanium pigment, and thinner is a non-ionics; The solids content of said fluoro-resin mixture is 35-60%, and in the time of 20 ℃, viscosity is 15～40mPas.
3. copper-clad plate as claimed in claim 2 is characterized in that, said glass cloth adopts the alkali-free glass fiber cloth of 106,1080 or 2116 electronic-grades.
4. a method of making copper-clad plate as claimed in claim 2 is characterized in that, comprises the steps:
Step 1 provides Copper Foil, glass cloth, and the preparation fluoro-resin mixture;
Step 2 uses the fluoro-resin mixture of above-mentioned preparation to flood glass cloth, and baking is dry; Repeat this step, obtain varnished cloth; The baking drying comprises two stages, and the fs storing temperature is 50-100 ℃, and the time is 2-5min, transpiring moisture; The subordinate phase storing temperature is 200-320 ℃, and the time is 3-5min, removes the volatilizable thing of low temperature;
Step 3 is joined the above-mentioned varnished cloth that obtains is folded, and the two sides is covered with Copper Foil, carries out lamination, obtains copper-clad plate; Lamination is 360-380 ℃/2-5h, and pressure is 50-100kg/cm
2
5. the making method of copper-clad plate as claimed in claim 4; It is characterized in that; Said glass cloth adopts the alkali-free glass fiber cloth of 106,1080 or 2116 electronic-grades; Fluoro-resin mixture contains following two kinds of materials as necessary component, in organic solid substance by 100 weight parts, wherein: ptfe emulsion 90-99 part, tetrafluoroethylene perfluoroalkyl vinyl ether emulsion 1-10 part; The solids content of this fluoro-resin mixture is 35-60%, and in the time of 20 ℃, viscosity is 15～40mPas.
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| CN2010101800345A CN101838431B (en) | 2010-05-21 | 2010-05-21 | Fluororesin mixture, copper-clad plate prepared therefrom and manufacturing method thereof |
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| CN2010101800345A CN101838431B (en) | 2010-05-21 | 2010-05-21 | Fluororesin mixture, copper-clad plate prepared therefrom and manufacturing method thereof |
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| US11818838B2 (en) | 2019-06-21 | 2023-11-14 | Taiwan Union Technology Corporation | Metal-clad laminate and manufacturing method of the same |
| US11840047B2 (en) | 2019-09-04 | 2023-12-12 | Taiwan Union Technology Corporation | Metal-clad laminate, printed circuit board, and method for manufacturing the same |
| US11805600B2 (en) | 2020-07-28 | 2023-10-31 | Saint-Gobain Performance Plastics Corporation | Dielectric substrate and method of forming the same |
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