CN114771050B - High-frequency copper-clad plate and preparation method thereof - Google Patents
High-frequency copper-clad plate and preparation method thereof Download PDFInfo
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- CN114771050B CN114771050B CN202210378334.7A CN202210378334A CN114771050B CN 114771050 B CN114771050 B CN 114771050B CN 202210378334 A CN202210378334 A CN 202210378334A CN 114771050 B CN114771050 B CN 114771050B
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- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B11/00—Making preforms
- B29B11/14—Making preforms characterised by structure or composition
- B29B11/16—Making preforms characterised by structure or composition comprising fillers or reinforcement
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- B32B15/00—Layered products comprising a layer of metal
- B32B15/20—Layered products comprising a layer of metal comprising aluminium or copper
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- 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
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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
- B32B37/10—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
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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
- B32B37/12—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by using adhesives
- B32B37/1284—Application of adhesive
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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
- 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
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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
- B32B7/00—Layered products characterised by the relation between layers; Layered products characterised by the relative orientation of features between layers, or by the relative values of a measurable parameter between layers, i.e. products comprising layers having different physical, chemical or physicochemical properties; Layered products characterised by the interconnection of layers
- B32B7/04—Interconnection of layers
- B32B7/12—Interconnection of layers using interposed adhesives or interposed materials with bonding properties
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H13/00—Pulp or paper, comprising synthetic cellulose or non-cellulose fibres or web-forming material
- D21H13/10—Organic non-cellulose fibres
- D21H13/20—Organic non-cellulose fibres from macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D21H13/26—Polyamides; Polyimides
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H23/00—Processes or apparatus for adding material to the pulp or to the paper
- D21H23/02—Processes or apparatus for adding material to the pulp or to the paper characterised by the manner in which substances are added
- D21H23/22—Addition to the formed paper
- D21H23/32—Addition to the formed paper by contacting paper with an excess of material, e.g. from a reservoir or in a manner necessitating removal of applied excess material from the paper
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K1/00—Printed circuits
- H05K1/02—Details
- H05K1/03—Use of materials for the substrate
- H05K1/0313—Organic insulating material
- H05K1/0353—Organic insulating material consisting of two or more materials, e.g. two or more polymers, polymer + filler, + reinforcement
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K3/00—Apparatus or processes for manufacturing printed circuits
- H05K3/02—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
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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
- B32B2038/0052—Other operations not otherwise provided for
- B32B2038/0076—Curing, vulcanising, cross-linking
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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
- 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
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Abstract
The invention provides a preparation method of a high-frequency copper-clad plate, which comprises the following steps: a) The para-aramid fiber wool paper subjected to high-temperature treatment is subjected to a sizing system to obtain a prepreg; the para-aramid wool paper is prepared from para-aramid chopped fibers and para-nanofibers by wet papermaking; b) The prepreg is assembled according to the structure of copper foil-bonding sheet-prepreg-bonding sheet-copper foil and then is solidified and formed to obtain a copper-clad plate blank; c) And carrying out post-treatment on the copper-clad plate blank to obtain a finished copper-clad plate product. The invention makes full use of the advantages of low dielectric constants of para-aramid and polytetrafluoroethylene resin, and prepares the para-aramid base plate with low dielectric constant by curing polytetrafluoroethylene resin under the conditions of high temperature and high pressure. The middle substrate and the electrolytic copper foils at two sides are welded together through FEP film melting, so that the defect of poor adhesion performance of polytetrafluoroethylene resin is overcome, and the peel strength of the copper-clad plate is improved.
Description
Technical Field
The invention belongs to the technical field of electronic materials, and particularly relates to a high-frequency copper-clad plate and a preparation method thereof.
Background
As human society has entered an informatization age, modern information technologies such as computers, networks, and mobile communications are filling people's lives. Printed circuit boards (Printed Circuit Board, PCBs) as substrates for electronic information products are increasingly being used in electronic products, which are channels for connecting various electronic components, serve as a skeleton for supporting components and a bridge for transmitting electrical signals, and provide mechanical assembly support and electrical connection for various electronic components thereon, so that the components are designed in advance to form a printed circuit, and almost all electronic products use PCBs, thus being called as parents of electronic products. The copper-clad plate serving as the PCB substrate accounts for 40% of the production cost of the PCB, plays the roles of conducting, insulating and supporting 3 in the PCB, and determines the performance, quality and reliability of the PCB in the processing process to a great extent.
The copper-clad plate is a plate-like material which is prepared by impregnating a reinforcing material with resin, coating copper foil on one or both sides, and hot-pressing. After being exposed, etched, drilled, green oil coated and the like, the copper-clad plate can be manufactured into a Printed Circuit Board (PCB) commonly used in the electronic industry. With the rapid development of the electronic information industry, PCBs as substrates for electronic information products face many new challenges, and in the trend of development of 5G communication technology, signals are required to have faster propagation speeds and better propagation qualities. In general, the transmission rate of a signal is inversely proportional to the square root of the dielectric constant of a material, the signal transmission delay is easily caused by a high dielectric constant, the smaller the dielectric constant of a copper-clad plate is, the more stable the transmission is, the loss in the signal transmission process is mainly influenced by the dielectric loss of the material, the smaller the dielectric loss is, the smaller the loss is in the signal transmission, and the better the signal transmission quality is.
The general working frequency is above 5GHz, the ultra-high frequency copper-clad plate is suitable for the ultra-high frequency field, has ultra-low loss characteristic (ultra-low signal transmission loss), can be applied to the microwave/millimeter wave field and is called as a high-frequency copper-clad plate, and the low loss of the high-frequency copper-clad plate is generally represented by Dk (dielectric constant) and Df (dielectric loss < 0.005), and the lower the index is, the better the performance is. Therefore, how to reduce the dielectric constant and low dielectric loss of the copper-clad plate for use in the communication field can make signal propagation obtain a faster propagation speed and a more stable propagation quality is a problem to be solved at present.
Disclosure of Invention
In view of the above, the technical problem to be solved by the invention is to provide a high-frequency copper-clad plate and a preparation method thereof.
The invention provides a preparation method of a high-frequency copper-clad plate, which comprises the following steps:
a) The para-aramid fiber wool paper subjected to high-temperature treatment is subjected to a sizing system to obtain a prepreg;
the para-aramid wool paper is prepared from para-aramid chopped fibers and para-nanofibers by wet papermaking;
b) The prepreg is assembled according to the structure of copper foil-bonding sheet-prepreg-bonding sheet-copper foil and then is solidified and formed to obtain a copper-clad plate blank;
c) And carrying out post-treatment on the copper-clad plate blank to obtain a finished copper-clad plate product.
Preferably, the ratio of the chopped fiber to the nanofiber in the para-aramid wool paper is 60:40-75: 25, a step of selecting a specific type of material;
the para-aramid paper is paper which is not subjected to high-temperature calendaring after wet papermaking.
Preferably, in the step A), the temperature of the high-temperature treatment is 350-400 ℃ and the time is 50-60 min, and the treatment process needs nitrogen protection.
Preferably, the method for passing the para-aramid wool paper through the sizing system comprises the following steps:
and immersing the para-aramid wool paper in the glue solution, and then taking out the para-aramid wool paper to obtain the prepreg after drying, baking and sintering in sequence.
Preferably, the glue solution is polytetrafluoroethylene resin, and the solid content of the polytetrafluoroethylene resin is 30% -45%;
the times of the dipping are 3 to 5 times;
the drying temperature is 80-90 ℃ and the drying time is 6-8 min;
the baking temperature is 130-150 ℃ and the baking time is 3-5 min;
the sintering temperature is 380-400 ℃ and the sintering time is 15-30 min;
the sizing amount of the prepreg is 50% -60%.
Preferably, the adhesive sheet is selected from FEP adhesive sheets.
Preferably, the copper foil is selected from electrolytic copper foil, and has a thickness of 20 to 50 μm.
Preferably, the curing and molding process comprises the following steps: the hot pressing temperature is 370-380 ℃, the hot pressing pressure is 3-5 MPa, the hot pressing time is 15-30 min, and the vacuum degree is-0.1 MPa.
Preferably, the post-treatment method comprises the following steps:
in order to cool down the copper-clad plate in the process of keeping the pressure of 3-5 MPa, the cooling rate is 3-5 ℃ per minute, and the temperature is reduced to below 50 ℃ for die opening and plate taking.
The invention also provides the high-frequency copper-clad plate prepared by the preparation method, wherein the thickness of the high-frequency copper-clad plate is 0.5-2.0 mm, and the density is 1.3-1.5 g/cm 3 。
Compared with the prior art, the invention provides a preparation method of a high-frequency copper-clad plate, which comprises the following steps: a) The para-aramid fiber wool paper subjected to high-temperature treatment is subjected to a sizing system to obtain a prepreg; the para-aramid wool paper is prepared from para-aramid chopped fibers and para-nanofibers by wet papermaking; b) The prepreg is assembled according to the structure of copper foil-bonding sheet-prepreg-bonding sheet-copper foil and then is solidified and formed to obtain a copper-clad plate blank; c) And carrying out post-treatment on the copper-clad plate blank to obtain a finished copper-clad plate product. The invention makes full use of the advantages of low dielectric constants of para-aramid and polytetrafluoroethylene resin, and prepares the para-aramid base plate with low dielectric constant by curing polytetrafluoroethylene resin under the conditions of high temperature and high pressure. The middle substrate and the electrolytic copper foils at two sides are welded together through FEP film melting, so that the defect of poor adhesion performance of polytetrafluoroethylene resin is overcome, and the peel strength of the copper-clad plate is improved. The invention produces the copper-clad plate with low dielectric constant, and can lead the electric signal to have faster propagation speed in the printed circuit board processed by the copper-clad plate.
Detailed Description
The invention provides a preparation method of a high-frequency copper-clad plate, which comprises the following steps:
a) The para-aramid fiber wool paper subjected to high-temperature treatment is subjected to a sizing system to obtain a prepreg;
the para-aramid wool paper is prepared from para-aramid chopped fibers and para-nanofibers by wet papermaking;
b) The prepreg is assembled according to the structure of copper foil-bonding sheet-prepreg-bonding sheet-copper foil and then is solidified and formed to obtain a copper-clad plate blank;
c) And carrying out post-treatment on the copper-clad plate blank to obtain a finished copper-clad plate product.
The preparation method selects para-aramid fiber wool paper as a preparation raw material, wherein the para-aramid fiber wool paper is prepared from para-aramid chopped fibers and para-nanofibers by wet papermaking; the ratio of the chopped fiber to the nanofiber in the para-aramid wool paper is 60:40-75: 25, preferably 60:40, 65:35, 70:30, 75:25, or 60:40-75: any value between 25;
the para-aramid paper is paper which is not subjected to high-temperature calendaring after wet papermaking.
The invention firstly carries out high-temperature treatment on para-aramid Mao Zhi to remove the impurities easy to decompose in the paper. Wherein the temperature of the high temperature treatment is 350-400 ℃, preferably 350, 360, 370, 380, 390, 400, or any value between 350-400 ℃, the time is 50-60 min, preferably 50, 52, 54, 56, 58, 60, or any value between 50-60 min, and the treatment process needs nitrogen protection.
And then, the para-aramid wool paper subjected to high-temperature treatment is subjected to a sizing system to obtain the prepreg.
The method for making para-aramid wool paper pass through the sizing system comprises the following steps:
and immersing the para-aramid wool paper in the glue solution, and then taking out the para-aramid wool paper to obtain the prepreg after drying, baking and sintering in sequence.
Specifically, the para-aramid wool paper subjected to high-temperature treatment is immersed in polytetrafluoroethylene resin with the solid content of 30% -45% in a gluing system, is dried for 6-8 min at 80-90 ℃ by a three-stage oven, is baked for 3-5 min at 130-150 ℃, is sintered for 15-30 min at 380-400 ℃, and is subjected to 3-5 glue dipping-drying processes to obtain the para-aramid paper/polytetrafluoroethylene prepreg with the glue sizing amount of 50% -60%.
Wherein the glue solution is polytetrafluoroethylene resin, and the solid content of the polytetrafluoroethylene resin is 30% -45%, preferably 30%, 35%, 40%, 45%, or any value between 30% -45%;
the number of times of the impregnation is 3 to 5, preferably 3, 4, 5, or any value between 3 and 5 times;
the drying temperature is 80-90 ℃, preferably 80, 82, 84, 86, 88, 90, or any value between 80-90 ℃, and the drying time is 6-8 min, preferably 6, 7, 8, or any value between 6-8 min;
the baking temperature is 130-150 ℃, preferably 130, 135, 140, 145, 150, or any value between 130-150 ℃, and the baking time is 3-5 min, preferably 3, 4, 5, or any value between 3-5 min;
the sintering temperature is 380-400 ℃, preferably 380, 385, 390, 395, 400 or any value between 380-400 ℃ and the sintering time is 15-30 min, preferably 15, 20, 25, 30 or any value between 15-30 min;
the sizing amount of the prepreg is 50% to 60%, preferably 50%, 55%, 60%, or any value between 50% and 60%.
And assembling the prepreg according to the structure of copper foil-bonding sheet-prepreg-bonding sheet-copper foil, and then curing and forming to obtain the copper-clad plate blank.
Wherein the copper foil is selected from electrolytic copper foil with the thickness of 20-50 mu m. The surface area of the copper foil is increased and the composite strength of the copper foil and the substrate is improved by electroplating on the surface of the copper foil, which is contacted with the prepreg.
The adhesive sheet is selected from FEP adhesive sheets.
The solidification molding process comprises the following steps: the hot pressing temperature is 370-380 ℃, preferably 370, 375, 380, or any value between 370-380 ℃, the hot pressing pressure is 3-5 MPa, preferably 3, 3.5, 4, 4.5, 5, or any value between 3-5 MPa, the hot pressing time is 15-30 min, preferably 15, 20, 25, 30, or any value between 15-30 min, and the vacuum degree is-0.1 MPa.
The specific steps are as follows:
the first step: placing the structural assembly of copper foil, bonding sheet, prepreg, bonding sheet and copper foil into a vacuum hot press;
and a second step of: starting a vacuum pump, and pumping the air pressure in the hot press cabin to-0.1 MPa;
and a third step of: and (3) pressurizing and closing the hot press, pressurizing to 3-5 MPa, heating to 370-380 ℃, and maintaining the pressure for 15-30 min.
And finally, carrying out post-treatment on the copper-clad plate blank to obtain a finished copper-clad plate product.
The post-treatment method comprises the following steps:
in order to cool down in the process of keeping the pressure of the copper-clad plate, the cooling rate is 3-5 ℃ per minute, and the temperature is reduced to below 50 ℃ for die opening and plate taking.
The invention is formed by high-heat pressing an electrolytic copper foil-FEP bonding sheet-para-aramid paper/polytetrafluoroethylene prepreg-FEP bonding sheet-electrolytic copper foil structural assembly under vacuum condition, wherein the electrolytic copper foil plays a role in conducting electricity in the structure, the FEP film plays a role in bonding the copper foil and an aramid/polytetrafluoroethylene substrate together, and the aramid/polytetrafluoroethylene composite board plays a role in supporting and insulating.
According to the invention, the p-aramid wool paper is dipped with polytetrafluoroethylene resin to be solidified into the substrate, and the substrate is bonded with the electrolytic copper foil through the FEP film, so that the copper-clad plate with low dielectric constant and low dielectric loss is obtained.
The invention provides a preparation method of a copper-clad plate, which is characterized by low dielectric constant, low dielectric loss, light weight and easy processing. The method uses para-aramid fiber wool paper, polytetrafluoroethylene resin, an FEP bonding sheet and an electrolytic copper foil as raw materials, fully utilizes the low dielectric properties of the para-aramid fiber paper and the polytetrafluoroethylene resin, has high bonding strength, and can better tightly combine the aramid fiber paper and the aramid fiber paper with the copper foil in the forming process to obtain the copper-clad plate with high peeling strength and low dielectric properties. The copper-clad plate is prepared from para-aramid paper, polytetrafluoroethylene resin, FEP adhesive sheets and electrolytic copper foil, and has the thickness of 0.5-2.0 mm and the density of 1.3-1.5 g/cm 3 The method is suitable for the fields of communication, high-end servers, military and the like.
In order to further understand the present invention, the following examples are provided to illustrate the high-frequency copper-clad plate and the preparation method thereof, and the protection scope of the present invention is not limited by the following examples.
Example 1
Putting para-aramid paper into a muffle furnace, introducing nitrogen, carrying out heat treatment for 50min at 350 ℃, immersing polytetrafluoroethylene resin with 30% of solid content in a horizontal sizing machine, passing through a three-stage oven, drying for 6min at 80 ℃, baking for 3min at 130 ℃, sintering for 1min at 380 ℃, carrying out gum dipping-drying for 3 times to obtain aramid paper/polytetrafluoroethylene prepreg, assembling according to the structure of copper foil-adhesive sheet-prepreg-adhesive sheet-copper foil, starting a vacuum pump, pumping air pressure in a hot press cabin to-0.1 MPa, pressurizing and closing the hot press, pressurizing to 3MPa, heating to 370 ℃, maintaining pressure for 15min, opening a cooling device, cooling at a cooling rate of 3-5 ℃ per minute, opening a die, taking out a copper-clad plate product, and testing results are shown in table 1.
Example 2
Putting para-aramid paper into a muffle furnace, introducing nitrogen, carrying out heat treatment for 50min at 380 ℃, immersing polytetrafluoroethylene resin with the solid content of 35% in a horizontal sizing machine, drying for 6min at 80 ℃ by a three-stage oven, baking for 3min at 150 ℃, sintering for 1min at 400 ℃, carrying out gum dipping-drying for 3 times to obtain aramid paper/polytetrafluoroethylene prepreg, assembling according to the structure of copper foil-adhesive sheet-prepreg-adhesive sheet-copper foil, starting a vacuum pump, pumping air pressure in a hot press cabin to-0.1 MPa, pressurizing and closing the hot press, pressurizing to 5MPa, heating to 370 ℃, maintaining the pressure for 20min, starting a cooling device, cooling at a cooling rate of 3-5 ℃ per minute, opening a die, taking out a copper-clad plate product, and testing results are shown in table 1.
Example 3
Putting para-aramid paper into a muffle furnace, introducing nitrogen, carrying out heat treatment for 60min at 400 ℃, immersing polytetrafluoroethylene resin with the solid content of 45% in a horizontal sizing machine, drying for 8min at 90 ℃ by a three-stage oven, baking for 5min at 150 ℃, sintering for 15min at 380 ℃, carrying out gum dipping-drying for 4 times to obtain aramid paper/polytetrafluoroethylene prepreg, assembling according to the structure of copper foil-adhesive sheet-prepreg-adhesive sheet-copper foil, starting a vacuum pump, pumping air pressure in a hot press cabin to-0.1 MPa, pressurizing and closing the hot press, pressurizing to 3MPa, heating to 380 ℃, maintaining the pressure for 15min, starting a cooling device, cooling at a cooling rate of 3-5 ℃ per minute, opening a die, taking out a copper-clad plate product, and testing results are shown in table 1.
Example 4
Putting para-aramid paper into a muffle furnace, introducing nitrogen, carrying out heat treatment for 50min at 380 ℃, immersing polytetrafluoroethylene resin with the solid content of 40% in a horizontal sizing machine, drying for 8min at 80 ℃ by a three-stage oven, baking for 5min at 130 ℃, sintering for 15min at 380 ℃, carrying out gum dipping-drying for 5 times to obtain aramid paper/polytetrafluoroethylene prepreg, assembling according to the structure of copper foil-adhesive sheet-prepreg-adhesive sheet-copper foil, starting a vacuum pump, pumping air pressure in a hot press cabin to-0.1 MPa, pressurizing and closing the hot press, pressurizing to 5MPa, heating to 370 ℃, maintaining the pressure for 15min, starting a cooling device, cooling at a cooling rate of 3-5 ℃ per minute, opening a die, taking out a copper-clad plate product, and testing results are shown in table 1.
Example 5
Putting para-aramid paper into a muffle furnace, introducing nitrogen, carrying out heat treatment at 380 ℃ for 60min, immersing polytetrafluoroethylene resin with the solid content of 45% in a horizontal sizing machine, drying at 100 ℃ for 6min, baking at 150 ℃ for 3min, sintering at 400 ℃ for 15min, carrying out gum dipping-drying for 5 times to obtain aramid paper/polytetrafluoroethylene prepreg, assembling according to the structure of copper foil-adhesive sheet-prepreg-adhesive sheet-copper foil, starting a vacuum pump, pumping air pressure in a hot press cabin to-0.1 MPa, pressurizing and closing the hot press, pressurizing to 5MPa, heating to 370 ℃, maintaining the pressure for 15min, opening a cooling device, cooling at a cooling rate of 3-5 ℃ per minute, opening a die, taking out a copper-clad plate product, and testing results are shown in table 1.
Comparative example 1
Putting meta-aramid paper into a muffle furnace, introducing nitrogen, performing heat treatment at 300 ℃ for 60min, soaking polytetrafluoroethylene resin with the solid content of 45% in a horizontal sizing machine, passing through a three-stage oven, drying at 100 ℃ for 6min, baking at 150 ℃ for 3min, and sintering at 400 ℃ for 15min, wherein the meta-aramid paper is seriously decomposed at 400 ℃ and cannot be used for preparing aramid paper/polytetrafluoroethylene prepregs.
Comparative example 2
Putting glass fiber cloth into a muffle furnace, introducing nitrogen, carrying out heat treatment for 50min at 450 ℃, immersing polytetrafluoroethylene resin with the solid content of 40% in a horizontal sizing machine, drying for 8min at 80 ℃ by a three-stage oven, baking for 5min at 130 ℃, sintering for 15min at 380 ℃, carrying out gum dipping-drying for 5 times to obtain glass fiber cloth/polytetrafluoroethylene prepreg, assembling according to the structure of copper foil-bonding sheet-prepreg-bonding sheet-copper foil, starting a vacuum pump, pumping the air pressure in a hot press cabin to-0.1 MPa, pressurizing and closing the hot press, pressurizing to 5MPa, heating to 370 ℃, maintaining the pressure for 15min, starting a cooling device, cooling to 3-5 ℃ per minute, opening a die, taking out a copper-clad plate product, and testing results are shown in table 2.
Comparative example 3
Putting the para-glass fiber cloth into a muffle furnace, introducing nitrogen, carrying out heat treatment for 60min at 450 ℃, immersing polytetrafluoroethylene resin with the solid content of 45% in a horizontal sizing machine, passing through a three-stage oven, drying for 6min at 100 ℃, baking for 3min at 150 ℃, sintering for 15min at 400 ℃, carrying out gum dipping-drying for 5 times to obtain glass fiber cloth/polytetrafluoroethylene prepreg, assembling according to the structure of copper foil-bonding sheet-prepreg-bonding sheet-copper foil, starting a vacuum pump, pumping the air pressure in a hot press cabin to-0.1 MPa, pressurizing and closing the hot press, pressurizing to 5MPa, heating to 370 ℃, maintaining the pressure for 15min, starting a cooling device, cooling at a cooling rate of 3-5 ℃ per minute, opening a die, taking out a copper-clad plate product, and testing results are shown in table 2.
The invention detects performance indexes of the low dielectric constant copper-clad plate, and the detection items and the method are as follows:
dielectric properties: reference to test method of rigid copper-clad laminate for GB/T4722-2017 printed Circuit Board
Table 1 example test results
Table 2 comparative test results
The foregoing is merely a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention, which are intended to be comprehended within the scope of the present invention.
Claims (4)
1. The preparation method of the high-frequency copper-clad plate is characterized by comprising the following steps of:
a) The para-aramid fiber wool paper subjected to high-temperature treatment is subjected to a sizing system to obtain a prepreg;
the para-aramid wool paper is prepared from para-aramid chopped fibers and para-nanofibers by wet papermaking; the mass ratio of the para-aramid chopped fiber to the para-nanofiber in the para-aramid wool paper is 60:40-75: 25, a step of selecting a specific type of material; the para-aramid paper is paper which is manufactured by a wet method and is not subjected to high-temperature calendaring;
the method for making para-aramid wool paper pass through the sizing system comprises the following steps:
immersing the para-aramid wool paper in a glue solution, and then taking out the para-aramid wool paper to obtain a prepreg after drying, baking and sintering in sequence;
the glue solution of the glue coating system is polytetrafluoroethylene resin, and the solid content of the polytetrafluoroethylene resin is 30% -45%;
the sizing amount of the prepreg is 50% -60%;
the temperature of the high-temperature treatment is 350-400 ℃, the time is 50-60 min, and nitrogen protection is needed in the treatment process;
b) The prepreg is assembled according to the structure of copper foil-bonding sheet-prepreg-bonding sheet-copper foil and then is solidified and formed to obtain a copper-clad plate blank;
the adhesive sheet is an FEP adhesive sheet;
the solidification molding process comprises the following steps:
the first step: placing the structural assembly of copper foil, bonding sheet, prepreg, bonding sheet and copper foil into a vacuum hot press;
and a second step of: starting a vacuum pump, and pumping the air pressure in the hot press cabin to-0.1 MPa;
and a third step of: pressurizing and closing the hot press, pressurizing to 3-5 MPa, heating to 370-380 ℃, and maintaining the pressure for 15-30 min;
c) Post-processing the copper-clad plate blank to obtain a finished copper-clad plate product;
the post-treatment method comprises the following steps:
and cooling in the process of keeping the pressure of the copper-clad plate at 3-5 MPa, wherein the cooling rate is 3-5 ℃ per minute, and the temperature is reduced to below 50 ℃ to open the die and take out the plate.
2. The method according to claim 1, wherein the number of times of impregnation is 3 to 5 times;
the drying temperature is 80-90 ℃ and the drying time is 6-8 min;
the baking temperature is 130-150 ℃ and the baking time is 3-5 min;
the sintering temperature is 380-400 ℃, and the sintering time is 15-30 min.
3. The method according to claim 1, wherein the copper foil is an electrolytic copper foil having a thickness of 20 to 50 μm.
4. A high-frequency copper-clad plate prepared by the preparation method according to any one of claims 1 to 3, wherein the high-frequency copper-clad plate has a thickness of 0.5 to 2.0mm and a density of 1.3 to 1.5g/cm 3 。
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| CN115323828A (en) * | 2022-08-11 | 2022-11-11 | 黄河三角洲京博化工研究院有限公司 | Para-aramid paper cyanate ester high-frequency copper-clad plate and preparation method thereof |
| CN115341404B (en) * | 2022-08-15 | 2023-10-13 | 黄河三角洲京博化工研究院有限公司 | Para-aramid nanofiber reinforced copper-clad plate and preparation method thereof |
| CN115339191A (en) * | 2022-08-15 | 2022-11-15 | 黄河三角洲京博化工研究院有限公司 | Para-aramid paper composite base halogen-free low-dielectric copper-clad plate and preparation method thereof |
| CN115418885B (en) * | 2022-09-15 | 2023-09-01 | 黄河三角洲京博化工研究院有限公司 | Low-dielectric-loss aramid paper and preparation method thereof |
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