CN118181889A - Low-dielectric low-expansion polytetrafluoroethylene high-frequency copper-clad plate and preparation method thereof - Google Patents
Low-dielectric low-expansion polytetrafluoroethylene high-frequency copper-clad plate and preparation method thereof Download PDFInfo
- Publication number
- CN118181889A CN118181889A CN202410125185.2A CN202410125185A CN118181889A CN 118181889 A CN118181889 A CN 118181889A CN 202410125185 A CN202410125185 A CN 202410125185A CN 118181889 A CN118181889 A CN 118181889A
- Authority
- CN
- China
- Prior art keywords
- blend
- fiber
- low
- polytetrafluoroethylene
- clad plate
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 229920001343 polytetrafluoroethylene Polymers 0.000 title claims abstract description 39
- 239000004810 polytetrafluoroethylene Substances 0.000 title claims abstract description 39
- -1 polytetrafluoroethylene Polymers 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000000835 fiber Substances 0.000 claims abstract description 54
- 239000000203 mixture Substances 0.000 claims abstract description 37
- 238000005245 sintering Methods 0.000 claims abstract description 17
- 238000002156 mixing Methods 0.000 claims abstract description 14
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229920003235 aromatic polyamide Polymers 0.000 claims abstract description 13
- 239000006185 dispersion Substances 0.000 claims abstract description 13
- 239000000839 emulsion Substances 0.000 claims abstract description 13
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims abstract description 12
- 239000011889 copper foil Substances 0.000 claims abstract description 11
- 238000007731 hot pressing Methods 0.000 claims abstract description 11
- 238000004519 manufacturing process Methods 0.000 claims abstract description 11
- 239000010453 quartz Substances 0.000 claims abstract description 11
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000007788 liquid Substances 0.000 claims abstract description 10
- 238000001035 drying Methods 0.000 claims abstract description 9
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 7
- 238000000967 suction filtration Methods 0.000 claims abstract description 6
- 239000000463 material Substances 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 6
- 229920001410 Microfiber Polymers 0.000 claims description 5
- 239000003658 microfiber Substances 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 4
- BPCXHCSZMTWUBW-UHFFFAOYSA-N triethoxy(1,1,2,2,3,3,4,4,5,5,8,8,8-tridecafluorooctyl)silane Chemical compound CCO[Si](OCC)(OCC)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)CCC(F)(F)F BPCXHCSZMTWUBW-UHFFFAOYSA-N 0.000 claims description 2
- 229910052802 copper Inorganic materials 0.000 claims 2
- 239000010949 copper Substances 0.000 claims 2
- 239000000758 substrate Substances 0.000 abstract description 11
- 238000010521 absorption reaction Methods 0.000 abstract description 5
- 239000011347 resin Substances 0.000 abstract description 5
- 229920005989 resin Polymers 0.000 abstract description 5
- 238000005516 engineering process Methods 0.000 abstract description 4
- 238000009827 uniform distribution Methods 0.000 abstract description 2
- 239000003365 glass fiber Substances 0.000 description 8
- 239000000243 solution Substances 0.000 description 8
- 229920006231 aramid fiber Polymers 0.000 description 6
- 239000004744 fabric Substances 0.000 description 4
- 230000004048 modification Effects 0.000 description 4
- 238000012986 modification Methods 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- 239000002131 composite material Substances 0.000 description 3
- 229920006253 high performance fiber Polymers 0.000 description 3
- 238000005470 impregnation Methods 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 239000002585 base Substances 0.000 description 2
- 239000003292 glue Substances 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 238000003825 pressing Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005189 flocculation Methods 0.000 description 1
- 230000016615 flocculation Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000010030 laminating Methods 0.000 description 1
- 238000003475 lamination Methods 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000002557 mineral fiber Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000012779 reinforcing material Substances 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 238000001338 self-assembly Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000009987 spinning Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000001132 ultrasonic dispersion Methods 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
- 238000003828 vacuum filtration Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
-
- 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
- H05K3/02—Apparatus or processes for manufacturing printed circuits in which the conductive material is applied to the surface of the insulating support and is thereafter removed from such areas of the surface which are not intended for current conducting or shielding
- H05K3/022—Processes for manufacturing precursors of printed circuits, i.e. copper-clad substrates
-
- 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
- B32B15/14—Layered products comprising a layer of metal next to a fibrous or filamentary layer
-
- 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
- B32B15/20—Layered products comprising a layer of metal comprising aluminium or copper
-
- 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
- B32B37/06—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the heating method
-
- 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
- B32B37/10—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the pressing technique, e.g. using action of vacuum or fluid pressure
-
- 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
- B32B37/10—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the pressing technique, e.g. using action of vacuum or fluid pressure
- B32B37/1018—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the pressing technique, e.g. using action of vacuum or fluid pressure using only vacuum
-
- 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
-
- 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
- B32B5/00—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts
- B32B5/02—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by structural features of a fibrous or filamentary layer
- B32B5/08—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by structural features of a fibrous or filamentary layer the fibres or filaments of a layer being of different substances, e.g. conjugate fibres, mixture of different fibres
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L27/00—Compositions 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; Compositions of derivatives of such polymers
- C08L27/02—Compositions 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; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L27/12—Compositions 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; Compositions of derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
- C08L27/18—Homopolymers or copolymers or tetrafluoroethene
-
- 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
- H05K1/03—Use of materials for the substrate
-
- 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
- H05K1/03—Use of materials for the substrate
- H05K1/05—Insulated conductive substrates, e.g. insulated metal substrate
-
- 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
- B32B2260/02—Composition of the impregnated, bonded or embedded layer
- B32B2260/021—Fibrous or filamentary layer
-
- 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
-
- 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
- B32B2262/00—Composition or structural features of fibres which form a fibrous or filamentary layer or are present as additives
- B32B2262/02—Synthetic macromolecular fibres
- B32B2262/0261—Polyamide fibres
- B32B2262/0269—Aromatic polyamide fibres
-
- 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
- B32B2262/00—Composition or structural features of fibres which form a fibrous or filamentary layer or are present as additives
- B32B2262/10—Inorganic fibres
-
- 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
- B32B2307/00—Properties of the layers or laminate
- B32B2307/20—Properties of the layers or laminate having particular electrical or magnetic properties, e.g. piezoelectric
- B32B2307/204—Di-electric
-
- 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
- B32B2307/00—Properties of the layers or laminate
- B32B2307/30—Properties of the layers or laminate having particular thermal properties
- B32B2307/308—Heat stability
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/14—Polymer mixtures characterised by other features containing polymeric additives characterised by shape
- C08L2205/16—Fibres; Fibrils
Landscapes
- Engineering & Computer Science (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Chemical & Material Sciences (AREA)
- Physics & Mathematics (AREA)
- Fluid Mechanics (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Reinforced Plastic Materials (AREA)
- Laminated Bodies (AREA)
Abstract
The invention discloses a preparation method of a low-dielectric low-expansion polytetrafluoroethylene high-frequency copper-clad plate, which comprises the following steps: a) Pretreating para-aramid fiber and quartz fiber by using a silane coupling agent to obtain surface modified blend fiber; b) Mixing the blend fiber obtained in the step a) with a polyethylene oxide solution to obtain a dispersion liquid of the blend fiber; c) Mixing the dispersion liquid of the blend fiber obtained in the step b) with polytetrafluoroethylene emulsion to obtain a blend; d) Sequentially carrying out suction filtration and drying on the blend obtained in the step c), and sintering at a high temperature to obtain a prepreg; e) And d), stacking the prepreg obtained in the step d) with copper foil, and then performing vacuum hot-pressing sintering to obtain the polytetrafluoroethylene high-frequency copper-clad plate. The wet forming technology is adopted to realize uniform distribution of fibers in a resin medium, and the prepared substrate has good dielectric property, high copper foil peeling strength, good thermal stability and low moisture absorption rate, and simultaneously simplifies the manufacturing process and reduces the manufacturing cost.
Description
Technical Field
The invention belongs to the field of high-frequency circuit board materials, and relates to a low-dielectric low-expansion polytetrafluoroethylene high-frequency copper-clad plate and a preparation method thereof.
Background
Because the development demands of high frequency, high speed and high capacity are put forward by the modern electronic information technology, the working frequency of electronic equipment is higher and higher, and the working frequency is increased to the microwave frequency range, so that the influence of the dielectric substrate material on the high-frequency signal is more remarkable. Polytetrafluoroethylene (PTFE) has good dielectric properties, low moisture absorption, good chemical stability, etc., and can be used as a resin material for a substrate, but Glass Fiber (GF) is often used as a reinforcing material for preparing a PTFE/GF reinforced composite substrate because of its poor rigidity and large thermal expansion coefficient.
The traditional glass fiber cloth-based copper-clad plate has complicated preparation process steps, the glass fibers cannot be randomly distributed in the composite material by adopting the traditional E-glass fibers, the resin impregnation at the alternate positions of the fiber cloth warp and weft yarn tissue points is less, and finally the dielectric property of the thermally extruded substrate is not good enough.
Chinese patent publication No. CN108570877a discloses a method for manufacturing para-aramid-based prepreg for high-frequency high-speed circuit board, which comprises pretreating para-aramid fiber with acid or alkali, papermaking with para-aramid pulp and glass fiber, and pre-curing with glue solution to obtain prepreg; according to the technical scheme, although the wettability of the surface of the para-aramid fiber is improved and the combination property with the glue solution is improved through acid-base pretreatment, the performance of the aramid fiber is damaged through acid-base pretreatment, so that the performance of the aramid fiber is unstable, and the industrial production difficulty is high.
Accordingly, there is a need for improvements in the art that overcome the shortcomings of the prior art.
Disclosure of Invention
The invention aims to provide a preparation method of a low-dielectric low-expansion polytetrafluoroethylene high-frequency copper-clad plate, which overcomes the defects and the shortcomings of the traditional impregnation method for preparing a glass fiber cloth reinforced PTFE composite material, such as complicated steps, less resin impregnation at alternate positions of fiber cloth warp and weft tissue points, and the like, which cause the dielectric property of a substrate finally extruded by heat.
The invention aims at realizing the following technical scheme:
a preparation method of a low-dielectric low-expansion polytetrafluoroethylene high-frequency copper-clad plate comprises the following steps:
a) Pretreating para-aramid fiber and quartz fiber by using a silane coupling agent to obtain surface modified blend fiber;
b) Mixing the blend fiber modified in the step a) with a polyethylene oxide solution to obtain a dispersion liquid of the blend fiber;
c) Mixing the dispersion liquid of the blend fiber obtained in the step b) with polytetrafluoroethylene emulsion to obtain a blend;
d) Sequentially carrying out suction filtration and drying on the blend obtained in the step c), and sintering at a high temperature to obtain a prepreg;
e) And d), stacking the prepreg obtained in the step d) with copper foil, and then performing vacuum hot-pressing sintering to obtain the polytetrafluoroethylene high-frequency copper-clad plate.
Further, the average length of the para-aramid microfibers in the step a) is 800-1000 um, and the average length of the quartz fiber is 500-900 um.
Further, the silane coupling agent in the step a) is tridecafluorooctyl triethoxysilane (F8261).
Further, the concentration of polyethylene oxide in the polyethylene oxide solution in step b) is 0.03 to 0.05wt%.
Further, the polytetrafluoroethylene emulsion in the step c) has a solid content of 55 to 65wt% and an average particle diameter of 0.1 to 0.3 μm.
Further, the mixing of the dispersion of the blend fiber and the polytetrafluoroethylene emulsion in step c) is performed under ultrasonic conditions.
Further, the content of fibers in the blend in step c) is 5 to 15wt%.
Further, the drying mode in the step d) is that the material is dried for 0.5 to 2 hours at the temperature of 85 to 105 ℃, then baked for 10 to 15 minutes at the low temperature of 260 to 300 ℃ and sintered for 5 to 10 minutes at the high temperature of 360 to 380 ℃.
Further, the pressure of the vacuum hot-pressing sintering in the step e) is 1-10 MPa, the time of the vacuum hot-pressing sintering is 6-8 h, and the temperature of the vacuum hot-pressing sintering is 380-400 ℃.
The invention also provides a low-dielectric low-expansion polytetrafluoroethylene high-frequency copper-clad plate which is prepared by adopting the preparation method of the technical scheme.
The invention provides a preparation method of a low-dielectric low-expansion polytetrafluoroethylene high-frequency copper-clad plate, which comprises the steps of firstly carrying out modification pretreatment on high-performance fibers (para-aramid microfibers and/or quartz fibers) with unique length-diameter ratio structures. And then mixing the blended fiber with a polyethylene oxide solution, and using polyethylene oxide as a dispersing agent to avoid the flocculation phenomenon of the fiber and improve the dispersion characteristic of the fiber in a medium. And then adding polytetrafluoroethylene emulsion to obtain a blend, sequentially carrying out vacuum filtration, drying and low-temperature baking on the blend, and sintering at a high temperature to obtain the prepreg. In view of the steric hindrance effect of PTFE particles, the fibers keep their orientation during sedimentation, and a three-dimensional framework structure is synchronously constructed during self-assembly forming, which is helpful for the PTFE particles to enter the inner space of the fiber framework. By constructing an isotropic network structure in the PTFE matrix, the thermal expansion of the dielectric substrate material in the z-axis direction can be significantly reduced, and the dielectric substrate material can have a low thermal expansion coefficient. Finally, the medium layer and the copper foil are subjected to vacuum high-temperature pressing to prepare the polytetrafluoroethylene high-frequency copper-clad plate, and the substrate has the characteristics of low dielectric constant, good mechanical property, light weight, low expansion and the like due to the design of a three-dimensional framework structure and the intrinsic advantages of high-performance fibers.
By adopting the technical scheme, the method has the following beneficial effects: the wet forming technology is adopted to realize uniform distribution of fibers in a resin medium, and the prepared substrate has good dielectric property, high copper foil peeling strength, good thermal stability and low moisture absorption rate, and simultaneously simplifies the manufacturing process and reduces the manufacturing cost.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below. It will be apparent to those skilled in the art from this disclosure that the drawings described below are merely exemplary and that other embodiments may be derived from the drawings provided without undue effort.
The structures, proportions, sizes, etc. shown in the present specification are shown only for the purposes of illustration and description, and are not intended to limit the scope of the invention, which is defined by the claims, so that any structural modifications, changes in proportions, or adjustments of sizes, which do not affect the efficacy or the achievement of the present invention, should fall within the ambit of the technical disclosure.
Fig. 1 is a schematic flow state structure provided by the present invention.
Detailed Description
The following describes the embodiments of the present invention further with reference to the drawings. The description of these embodiments is provided to assist understanding of the present invention, but is not intended to limit the present invention. In addition, the technical features of the embodiments of the present invention described below may be combined with each other as long as they do not collide with each other.
Quartz fiber is an amorphous fiber composed of high purity SiO 2, which is the best of all mineral fibers so far, and maintains these excellent properties at high frequencies, high speeds and high temperatures. Quartz fiber has low density, low moisture absorption, and excellent mechanical properties, and is considered as the preferred material for low dielectric related applications. The aramid fiber is a high-performance fiber produced by the first high-molecular liquid crystal spinning technology, has excellent dielectric properties (Dk 2.0-4.0) and negative thermal expansion coefficient, and the CTE of a circuit board prepared from the aramid fiber can reach 6-9 ppm/DEG C. In addition, the aramid fiber has the excellent characteristics of high strength, high modulus, high temperature resistance, corrosion resistance, low density and the like. In view of the excellent dielectric property and thermal stability of the aramid fiber and the quartz fiber, the low-dielectric low-expansion high-frequency copper-clad plate substrate material is prepared by the fiber proportion regulation and one-step wet forming process.
Referring to fig. 1, a preparation method of a low dielectric low expansion polytetrafluoroethylene high frequency copper-clad plate comprises the following steps:
a) Pretreating para-aramid fiber and quartz fiber by using a silane coupling agent to obtain surface modified blend fiber;
b) Mixing the blend fiber modified in the step a) with a polyethylene oxide solution to obtain a dispersion liquid of the blend fiber;
c) Mixing the dispersion liquid of the blend fiber obtained in the step b) with polytetrafluoroethylene emulsion to obtain a blend;
d) Sequentially carrying out suction filtration and drying on the blend obtained in the step c), and sintering at a high temperature to obtain a prepreg;
e) And d), stacking the prepreg obtained in the step d) with copper foil, and then performing vacuum hot-pressing sintering to obtain the polytetrafluoroethylene high-frequency copper-clad plate.
Table 1 component parameters of the polytetrafluoroethylene copper-clad plate of each example
The invention discloses a preparation method of a low-dielectric low-expansion polytetrafluoroethylene high-frequency copper-clad plate, which comprises the following steps:
(1) And (3) fiber modification: the blend fiber is modified by a two-step process. First, 0.2wt% of F8261 was hydrolyzed in a mixed solution of absolute ethanol and deionized water (1:1), and rapidly stirred at a temperature of 50 to 70℃for 30 minutes. Then, the mixed fiber was added to the mixed solution and reacted for 10 hours to completely modify it. And (3) carrying out suction filtration on the dispersion liquid after the reaction, washing with ethanol for 2-3 times, and removing unreacted silane coupling agent. And then drying in a vacuum oven at 80 ℃ to constant weight, and removing water and solvent to obtain the modified blend fiber.
(2) Wet forming: mixing the modified blend fiber and polyethylene oxide solution (0.03-0.05 wt%) according to a weight ratio of 1:1000 by volume and mixing and stirring. The stirring speed is 1200-1700 r/mm, and the stirring time is 4-7 h. Mixing the obtained dispersion liquid of the blend fiber with polytetrafluoroethylene emulsion with the solid content of 50-80 wt% to obtain a blend, wherein the content of the fiber in the blend is 5-15 wt%; and carrying out ultrasonic dispersion treatment on the blend for 4-7 min, and then carrying out vacuum suction filtration to obtain a pre-pressed tablet. Drying the pre-pressed sheet in a blast drying oven (85-105 ℃) for 0.5-2 hours to remove water, then roasting at a low temperature of 260-300 ℃ for 10-15 minutes to decompose the residual polyethylene oxide and the additives in the polytetrafluoroethylene emulsion, and then sintering at a high temperature of 360-380 ℃ for 5-10 minutes to obtain the prepreg.
(3) High temperature lamination: laminating the prepreg and the copper foil, adding a layer of copper foil above and below the prepreg, adding steel plates on the upper surface and the lower surface of the copper foil, and then placing the copper foil into a high-temperature press for pressing. The temperature of vacuum hot-pressing sintering is set to 380-400 ℃, the pressure is 1-10 MPa, and the time is 6-8 h.
In the invention, the average length of the para-aramid microfiber is 800-1000 um, and the average length of the quartz fiber is 500-900 um. The source of the para-aramid microfiber is not particularly limited in the present invention, and commercially available commercial products known to those skilled in the art may be used.
In the present invention, the polytetrafluoroethylene emulsion has a solid content of 55 to 65wt% and an average particle diameter of 0.1 to 0.3. Mu.m. The source of the polytetrafluoroethylene emulsion is not particularly limited, and commercially available products known to those skilled in the art may be used.
The present application will be described in further detail with reference to the following examples, wherein it should be noted that the examples and the proportions of the raw materials in the examples can be combined with each other without conflict. All technical terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which the application pertains. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of example embodiments in accordance with the application.
Experimental performance tests were performed on the above examples, with the following results:
Therefore, the polytetrafluoroethylene high-frequency copper-clad plate obtained by the preparation method has the characteristics of good dielectric property, good thermal stability and low moisture absorption rate.
The embodiments of the present invention have been described in detail above with reference to the accompanying drawings, but the present invention is not limited to the described embodiments. It will be apparent to those skilled in the art that various changes, modifications, substitutions and alterations can be made to these embodiments without departing from the principles and spirit of the invention, and yet fall within the scope of the invention.
Claims (10)
1. The preparation method of the polytetrafluoroethylene high-frequency copper-clad plate with low dielectric and low expansion is characterized by comprising the following steps of:
a) Pretreating para-aramid fiber and quartz fiber by using a silane coupling agent to obtain surface modified blend fiber;
b) Mixing the blend fiber modified in the step a) with a polyethylene oxide solution to obtain a dispersion liquid of the blend fiber;
c) Mixing the dispersion liquid of the blend fiber obtained in the step b) with polytetrafluoroethylene emulsion to obtain a blend;
d) Sequentially carrying out suction filtration and drying on the blend obtained in the step c), and sintering at a high temperature to obtain a prepreg;
e) And d), stacking the prepreg obtained in the step d) with copper foil, and then performing vacuum hot-pressing sintering to obtain the polytetrafluoroethylene high-frequency copper-clad plate.
2. The method of manufacturing according to claim 1, characterized in that: the average length of the para-aramid microfiber in the step a) is 800-1000 um, and the average length of the quartz fiber is 500-900 um.
3. The preparation method according to claim 1 or 2, characterized in that: the silane coupling agent of step a) is tridecafluorooctyltriethoxysilane.
4. The method of manufacturing according to claim 1, characterized in that: the concentration of polyethylene oxide in the polyethylene oxide solution in step b) is 0.03 to 0.05wt%.
5. The method of manufacturing according to claim 1, characterized in that: the solid content of the polytetrafluoroethylene emulsion in the step c) is 55-65wt% and the average particle diameter is 0.1-0.3 mu m.
6. The method of claim 1 or 5, wherein: the mixing of the dispersion of the blend fibers and the polytetrafluoroethylene emulsion in step c) is carried out under ultrasonic conditions.
7. The method of manufacturing according to claim 6, wherein: the content of fibres in the blend in step c) is from 5 to 15% by weight.
8. The method of manufacturing according to claim 1, characterized in that: the drying mode in the step d) is that the material is dried for 0.5 to 2 hours at the temperature of 85 to 105 ℃, then baked for 10 to 15 minutes at the low temperature of 260 to 300 ℃ and sintered for 5 to 10 minutes at the high temperature of 360 to 380 ℃.
9. The method of manufacturing according to claim 1, characterized in that: the pressure of the vacuum hot-pressing sintering in the step e) is 1-10 MPa, the time of the vacuum hot-pressing sintering is 6-8 h, and the temperature of the vacuum hot-pressing sintering is 380-400 ℃.
10. A low dielectric low expansion polytetrafluoroethylene high frequency copper clad laminate characterized in that the copper clad laminate is prepared by the preparation method of any one of claims 1 to 9.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202410125185.2A CN118181889A (en) | 2024-01-30 | 2024-01-30 | Low-dielectric low-expansion polytetrafluoroethylene high-frequency copper-clad plate and preparation method thereof |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202410125185.2A CN118181889A (en) | 2024-01-30 | 2024-01-30 | Low-dielectric low-expansion polytetrafluoroethylene high-frequency copper-clad plate and preparation method thereof |
Publications (1)
Publication Number | Publication Date |
---|---|
CN118181889A true CN118181889A (en) | 2024-06-14 |
Family
ID=91393849
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN202410125185.2A Pending CN118181889A (en) | 2024-01-30 | 2024-01-30 | Low-dielectric low-expansion polytetrafluoroethylene high-frequency copper-clad plate and preparation method thereof |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN118181889A (en) |
-
2024
- 2024-01-30 CN CN202410125185.2A patent/CN118181889A/en active Pending
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN108189520B (en) | Manufacturing method of modified polytetrafluoroethylene copper-clad plate | |
KR101819805B1 (en) | Circuit substrate and Process for Preparing the same | |
CN109648935B (en) | Preparation process of PTFE ceramic composite high-frequency copper-clad plate | |
CN110228239B (en) | Low-dielectric poly (perfluoroethylene propylene) copper-clad plate and preparation method thereof | |
CN111993720B (en) | Polytetrafluoroethylene high-frequency copper-clad plate with high thermal conductivity | |
US11802192B2 (en) | Low dielectric resin substrate | |
CN115610044B (en) | Low-loss PTFE-based microwave composite dielectric substrate and preparation method thereof | |
CN113597121B (en) | Manufacturing method of glass fiber cloth reinforced copper-clad plate | |
JP7502218B2 (en) | Resin substrate with dielectric properties that are less dependent on frequency | |
CN114889273B (en) | Glass fiber-free ceramic/hydrocarbon resin-based microwave dielectric substrate and preparation method thereof | |
CN115075057B (en) | Low dielectric loss non-woven fabric and preparation method and application thereof | |
CN111187478A (en) | Composite material and sheet for microwave circuit substrate, microwave circuit substrate and preparation method of microwave circuit substrate | |
KR20170090464A (en) | Circuit substrate and preparation method thereof | |
CN114621543A (en) | High-frequency prepreg, high-frequency copper-clad plate and preparation method thereof | |
CN105347788B (en) | Microwave composite dielectric material with low dielectric loss and preparation method thereof | |
CN111825955B (en) | Prepreg for high frequency, preparation method thereof and copper-clad plate and preparation method thereof | |
CN116284914B (en) | Preparation method and application of composite dielectric substrate | |
CN118181889A (en) | Low-dielectric low-expansion polytetrafluoroethylene high-frequency copper-clad plate and preparation method thereof | |
CN116278233A (en) | Preparation method of PTFE-based copper-clad plate containing mesoporous ceramic powder | |
CN116731456A (en) | Preparation method of polytetrafluoroethylene copper-clad plate with low dielectric constant and low loss | |
CN204887693U (en) | Preimpregnation sandwich body reaches circuit substrate, printed circuit board by its preparation for circuit substrate | |
CN109370497B (en) | Preparation method of glue for producing high-speed copper-clad plate and product thereof | |
CN112812476B (en) | Polytetrafluoroethylene composite material and preparation method and application thereof | |
CN116039186A (en) | Preparation method of liquid crystal polymer fiber cloth-based low-dielectric composite board | |
CN115198564A (en) | Low-dielectric-loss non-woven fabric and preparation method and application thereof |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
PB01 | Publication | ||
PB01 | Publication | ||
SE01 | Entry into force of request for substantive examination |