CN113306227B - High-frequency ultralow-dielectric-loss microwave ceramic copper-clad plate and preparation method thereof - Google Patents

High-frequency ultralow-dielectric-loss microwave ceramic copper-clad plate and preparation method thereof Download PDF

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CN113306227B
CN113306227B CN202110579176.7A CN202110579176A CN113306227B CN 113306227 B CN113306227 B CN 113306227B CN 202110579176 A CN202110579176 A CN 202110579176A CN 113306227 B CN113306227 B CN 113306227B
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temperature
clad plate
sheet
parts
dielectric loss
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CN113306227A (en
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陈功田
陈建
李海林
彭灿
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Chenzhou Gongtian Electronic Ceramics Technology Co ltd
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Chenzhou Gongtian Electronic Ceramics Technology Co ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
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    • B32B9/00Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00
    • B32B9/005Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00 comprising one layer of ceramic material, e.g. porcelain, ceramic tile
    • BPERFORMING OPERATIONS; TRANSPORTING
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    • B32B15/20Layered products comprising a layer of metal comprising aluminium or copper
    • BPERFORMING OPERATIONS; TRANSPORTING
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Abstract

The invention discloses a high-frequency ultralow dielectric loss microwave ceramic copper-clad plate and a preparation method thereof, wherein the high-frequency ultralow dielectric loss microwave ceramic copper-clad plate comprises the following components in parts by mass: 30-75 parts of ceramic powder, 25-70 parts of polytetrafluoroethylene dispersion resin powder, 15-25 parts of solvent oil and 5-10 parts of absolute ethyl alcohol; the ceramic powder is filled with polytetrafluoroethylene dispersion resin powder, matched with alkane solvent oil and proper amount of absolute ethyl alcohol, and subjected to the working procedures of proportioning, air flow hot mixing, sheet extrusion, rolling and forming, low-temperature baking, high-temperature vacuum forming and the like to obtain the microwave ceramic copper-clad plate with ultralow dielectric loss, stable and adjustable dielectric constant, excellent dimensional stability and weather resistance and capability of meeting the high-frequency and high-frequency ultralow dielectric loss. The invention has simple process, environmental protection and mass industrialized production, and the product has excellent performance, ultra-low dielectric loss, stable dielectric constant, excellent dimensional stability, weather resistance and the like, and is very suitable for being applied to related equipment such as wireless millimeter wave communication and the like.

Description

High-frequency ultralow-dielectric-loss microwave ceramic copper-clad plate and preparation method thereof
Technical Field
The invention relates to the technical field of copper-clad plates, in particular to a high-frequency ultralow dielectric loss microwave ceramic copper-clad plate and a preparation method thereof.
Background
Under the current situation that the demand for 5G communication materials is increasingly strong, the information electronic products are developed towards high frequency, high speed, high precision and high reliability, and the demands for related equipment such as wireless millimeter wave communication are rapidly increased. The polytetrafluoroethylene copper-clad plate mainly takes emulsion and cut film as main materials, and has better electrical performance than the current main current hydrocarbon copper-clad plate, epoxy resin copper-clad plate, PPO copper-clad plate and the like in China. The raw materials and the manufacturing process are high in cost, so that the application of the copper-clad plate is limited, the dielectric constant adjustable range of the manufactured copper-clad plate is narrow and unstable, the dielectric loss is relatively high, the dimensional stability is low, and the weather resistance and the reliability are low. Therefore, a new scheme is needed to be provided for improving the existing copper-clad plate.
Disclosure of Invention
In view of the above, the main purpose of the present invention is to provide a high-frequency ultralow dielectric loss microwave ceramic copper-clad plate and a preparation method thereof, which can effectively solve the problems of high production cost, narrow adjustable range of dielectric constant, instability, relatively high dielectric loss, low dimensional stability, low weather resistance and low reliability of the existing copper-clad plate.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
the preparation method of the high-frequency ultralow-dielectric-loss microwave ceramic copper-clad plate comprises the following components in parts by mass: 30-75 parts of ceramic powder, 25-70 parts of polytetrafluoroethylene dispersion resin powder, 15-25 parts of solvent oil and 5-10 parts of absolute ethyl alcohol; the method comprises the following steps:
(1) And (3) batching: sieving polytetrafluoroethylene dispersion resin powder and ceramic powder respectively, and mixing according to the proportion to obtain a primary mixed material;
(2) And (3) hot mixing of air flow: pouring the primary mixed material obtained in the step (1) into an airflow mixer, adding solvent oil and absolute ethyl alcohol into an oil injection bottle according to the proportion, and circularly mixing for 4 hours at the temperature of 45-65 ℃ to obtain a uniform mixed material, wherein the circulating hot airflow in a sealed cavity is 5-25 kg/time;
(3) Sheet extrusion: sieving the uniformly mixed material obtained in the step (2), pouring the sieved uniformly mixed material into a prepressing forming machine to be prepressed into a cylinder, placing the cylinder in an extruder, extruding a windable film with the width of 10-30cm and the thickness of 1-5mm through a heating cavity and a sheet-shaped basic die opening, wherein the temperature of the heating cavity is 30-50 ℃, and the temperature of the sheet-shaped extrusion die opening is 50-60 ℃;
(4) Rolling and forming into a sheet: rolling the windable film obtained in the step (3) into a sheet for one or more times by an open mill to obtain an adhesive sheet with the width of 45-55cm and the thickness of 0.038-0.75mm, wherein the temperature of the open mill is 60 ℃;
(5) Baking at low temperature: baking the bonding sheet obtained in the step (4) through a degreasing drying oven to remove solvent oil and absolute ethyl alcohol to obtain a baked bonding sheet, wherein the baking temperature is 160-240 ℃/10min/m;
(6) High-temperature vacuum forming: cutting the baked bonding sheet obtained in the step (5), carrying out lamination and double-sided copper coating according to the difference of the thickness of the manufactured copper-clad plate, carrying out hot press molding by an oil pressure vacuum high-temperature press, and completing the preparation under the conditions that the vacuum condition is 90-100Kpa, the material temperature is 380-405 ℃, the pressure is 5-15MPa, and the dwell time is 1 h.
As a preferable scheme, the ceramic powder has a spherical structure, a spherical aggregate structure or a hollow sphere structure, the sphericity of the ceramic powder is more than or equal to 90 percent, and the particle size is 0.5-40 mu m.
As a preferable scheme, the ceramic powder is one or a mixture of more than one of titanium dioxide, silicon dioxide, barium titanate, strontium titanate, aluminum oxide and rare earth.
As a preferable scheme, the solvent oil is one or a mixture of a plurality of odorless kerosene, white oil and isoparaffin.
As a preferable scheme, the temperature of the material in the step (6) is 400 ℃.
As a preferable mode, the extrusion opening of the sheet-shaped extrusion die of the step (3) is 20cm wide.
As a preferable scheme, the open mill in the step (4) is a multi-roll open mill.
The high-frequency ultralow-dielectric-loss microwave ceramic copper-clad plate is prepared by the preparation method of the high-frequency ultralow-dielectric-loss microwave ceramic copper-clad plate.
Compared with the prior art, the invention has obvious advantages and beneficial effects, and in particular, the technical scheme can be as follows:
the ceramic powder is filled with polytetrafluoroethylene dispersion resin powder, matched with alkane solvent oil and proper amount of absolute ethyl alcohol, and subjected to the working procedures of proportioning, air flow hot mixing, sheet extrusion, rolling and sheet forming, low-temperature baking, high-temperature vacuum forming and the like to obtain the microwave ceramic copper-clad plate with ultralow dielectric loss, stable and adjustable dielectric constant, excellent dimensional stability and weather resistance and capability of meeting the high-frequency and high-frequency ultralow dielectric loss; in addition, the invention has simple process, environmental protection and mass industrialized production, and the product has excellent performance, ultra-low dielectric loss, stable dielectric constant, excellent dimensional stability, weather resistance and the like, and is very suitable for being applied to related equipment such as wireless millimeter wave communication and the like.
Drawings
FIG. 1 is a graph showing the dielectric constant 3.0 versus frequency for the preferred embodiment 2 of the present invention;
FIG. 2 is a graph showing the dielectric constant 3.0 versus temperature for the preferred embodiment 2 of the present invention.
Detailed Description
The invention discloses a preparation method of a high-frequency ultralow dielectric loss microwave ceramic copper-clad plate, which comprises the following components in parts by mass: 30-75 parts of ceramic powder, 25-70 parts of polytetrafluoroethylene dispersion resin powder, 15-25 parts of solvent oil and 5-10 parts of absolute ethyl alcohol; the method comprises the following steps:
(1) And (3) batching: and respectively sieving polytetrafluoroethylene dispersion resin powder and ceramic powder, and mixing according to the proportion to obtain a primary mixed material.
(2) And (3) hot mixing of air flow: pouring the primary mixed material obtained in the step (1) into an airflow mixer, adding solvent oil and absolute ethyl alcohol into an oil injection bottle according to the proportion, and circularly mixing for 4 hours at the temperature of 45-65 ℃ to obtain a uniform mixed material, wherein the circulating hot airflow in a sealed cavity is 5-25 kg/time; the oil spraying bottle has the function of controlling the oil filling precision and spraying, so that the mixing is more uniform; the spray is regularly and quantitatively sprayed under circulating hot air, the purpose of the hot air is to prepare the preparation for the next step of fully lubricating and uniformly mixing solvent oil, polytetrafluoroethylene dispersion resin powder and ceramic powder molecules, and meanwhile, the mixing and curing time is shortened due to the addition of absolute ethyl alcohol, so that the obtained uniformly mixed material is more uniform and more sufficient.
(3) Sheet extrusion: sieving the uniformly mixed material obtained in the step (2), pouring the sieved uniformly mixed material into a prepressing forming machine to be prepressed into a cylinder, placing the cylinder in an extruder, extruding a windable film with the width of 10-30cm and the thickness of 1-5mm through a heating cavity and a sheet-shaped basic die opening, wherein the temperature of the heating cavity is 30-50 ℃, and the temperature of the sheet-shaped extrusion die opening is 50-60 ℃.
(4) Rolling and forming into a sheet: rolling the windable film obtained in the step (3) into a sheet for one or more times by an open mill to obtain an adhesive sheet with the width of 45-55cm and the thickness of 0.038-0.75mm, wherein the temperature of the open mill is 60 ℃; in the industry, the maximum width of the high-performance film material is 30cm by using pure polytetrafluoroethylene extrusion calendaring, the calendaring width is limited by circular extrusion into a bar shape, and the bottleneck of the ceramic filled polytetrafluoroethylene copper-clad plate by using extrusion calendaring is wide-width improvement and how ceramic powder is completely mixed, uniformly dispersed and extruded; the purpose of the broad width promotion is to match the subsequent circuit board processing plant process, and the small size caused by the too small width will increase the mass production and subsequent processing cost.
(5) Baking at low temperature: baking the bonding sheet obtained in the step (4) through a degreasing drying oven to remove solvent oil and absolute ethyl alcohol to obtain a baked bonding sheet, wherein the baking temperature is 160-240 ℃/10min/m; according to the dielectric constants of the copper-clad plates, the bonding sheets are required to be longitudinally pulled up for shaping in the baking process, the speed is not too high, the film is too dry due to the too high temperature, so that the defect of holes is formed after the lamination is carried out, the solvent oil is not completely volatilized due to the too low temperature, and lamination bubbles or the situation that dielectric loss is increased and peeled off is caused.
(6) High-temperature vacuum forming: cutting the baked bonding sheet obtained in the step (5), carrying out lamination and double-sided copper coating according to the difference of the thickness of the manufactured copper-clad plate, carrying out hot press molding by an oil pressure vacuum high-temperature press, and completing the preparation under the conditions that the material temperature is 380-405 ℃, the pressure is 5-15MPa and the dwell time is 1 h; typically 18um electrolytic copper foil is selected.
The ceramic powder has a spherical structure, a spherical aggregate structure or a hollow sphere structure, the sphericity of the ceramic powder is more than or equal to 90 percent, and the particle size is 0.5-40 mu m; the spherical filler can provide higher filling proportion and excellent dimensional stability, the highest 80% filler ratio of the polytetrafluoroethylene dispersion resin powder with high density and high tensile strength is matched, and the filler ratio and electrical performance are further improved by using different filler compound particle sizes; taking the distribution of 10 μm as an example, the typical compounding is 4:2:3:1, namely the particle size below 10 μm accounts for 40%, the particle size of 10-20 μm accounts for 20%, the particle size of 20-30 μm accounts for 30%, and the particle size of 30-40 μm accounts for 10%. Polytetrafluoroethylene dispersion resin powder with different densities and tensile strengths is selected according to different dielectric constants. A typical relative density is 2.2g/cm and the pull-up strength is 24MPa.
The ceramic powder is one or a mixture of more of titanium dioxide, silicon dioxide, barium titanate, strontium titanate, aluminum oxide and rare earth.
The solvent oil is one or more of odorless kerosene, white oil and isoparaffin.
The temperature of the material in the step (6) is 400 ℃, the temperature of the oil pressure vacuum press with the temperature of 400 ℃ is more uniform than the temperature of the hot plate of the electric heating press, the performance of the plate is more stable to a certain extent, and the mass production is easier to control.
And (3) the extrusion opening of the sheet extrusion die in the step (3) is 20cm wide.
The open mill in the step (4) is a multi-roller open mill, which is beneficial to wide-width lifting.
The invention also discloses a high-frequency ultralow dielectric loss microwave ceramic copper-clad plate which is prepared by the preparation method of the high-frequency ultralow dielectric loss microwave ceramic copper-clad plate.
The invention is described in further detail below in a number of examples:
example 1:
(1) And (3) batching: 50 parts of polytetrafluoroethylene dispersion resin powder and 30 parts of ceramic powder are respectively sieved and mixed according to the proportion to obtain a primary mixed material.
(2) And (3) hot mixing of air flow: pouring the primary mixed material obtained in the step (1) into an airflow mixer, adding 22 parts of odorless kerosene and 5 parts of absolute ethyl alcohol into an oil injection bottle according to the proportion, and circularly mixing for 4 hours at the temperature of 45 ℃ to obtain a uniform mixed material, wherein the circulating hot airflow in a sealed cavity is 15 kg/time.
(3) Sheet extrusion: sieving the uniformly mixed material obtained in the step (2), pouring the sieved uniformly mixed material into a prepressing forming machine to be prepressed into a cylinder, placing the cylinder in an extruder, extruding a windable film with the width of 10-30cm and the thickness of 1-5mm through a heating cavity and a sheet-shaped basic die opening, wherein the temperature of the heating cavity is 40 ℃, and the temperature of the sheet-shaped extrusion die opening is 56 ℃.
(4) Rolling and forming into a sheet: and (3) carrying out one or more times of die rolling and sheeting on the windable film obtained in the step (3) through a multi-roll mill to obtain the adhesive sheet with the width of 45-55cm and the thickness of 0.038-0.75mm, wherein the temperature of the multi-roll mill is 60 ℃.
(5) Baking at low temperature: and (3) baking the bonding sheet obtained in the step (4) through a degreasing drying oven to remove odorless kerosene and absolute ethyl alcohol, so as to obtain a baked bonding sheet, wherein the baking temperature is 240 ℃/10min/m.
(6) High-temperature vacuum forming: and (3) cutting the baked bonding sheet obtained in the step (5), laminating and double-sided copper coating according to the thickness difference of the manufactured copper-clad plate, performing hot press forming through an oil pressure vacuum high-temperature press, wherein the vacuum condition is 90Kpa, and the baking bonding sheet is manufactured at the material temperature of 405 ℃, the pressure of 10MPa and the dwell time of 1 h.
Example 2:
(1) And (3) batching: sieving 25 parts of polytetrafluoroethylene dispersion resin powder and 50 parts of ceramic powder respectively, and mixing according to the proportion to obtain a primary mixed material.
(2) And (3) hot mixing of air flow: pouring the primary mixed material obtained in the step (1) into an airflow mixer, adding 15 parts of odorless kerosene and 8 parts of absolute ethyl alcohol into an oil injection bottle according to the proportion, and circularly mixing for 4 hours at the temperature of 55 ℃ to obtain a uniform mixed material, wherein the circulation hot airflow in a sealed cavity is 25 kg/time.
(3) Sheet extrusion: sieving the uniformly mixed material obtained in the step (2), pouring the sieved uniformly mixed material into a prepressing forming machine to be prepressed into a cylinder, placing the cylinder in an extruder, extruding a windable film with the width of 10-30cm and the thickness of 1-5mm through a heating cavity and a sheet-shaped basic die opening, wherein the temperature of the heating cavity is 45 ℃, and the temperature of the sheet-shaped extrusion die opening is 50 ℃.
(4) Rolling and forming into a sheet: and (3) carrying out one or more times of die rolling and sheeting on the windable film obtained in the step (3) through a multi-roll mill to obtain the adhesive sheet with the width of 45-55cm and the thickness of 0.038-0.75mm, wherein the temperature of the multi-roll mill is 60 ℃.
(5) Baking at low temperature: and (3) baking the bonding sheet obtained in the step (4) through a degreasing drying oven to remove odorless kerosene and absolute ethyl alcohol, so as to obtain a baked bonding sheet, wherein the baking temperature is 200 ℃/10min/m.
(6) High-temperature vacuum forming: and (3) cutting the baked bonding sheet obtained in the step (5), laminating and double-sided copper coating according to the thickness difference of the manufactured copper-clad plate, and performing hot press molding by an oil pressure vacuum high-temperature press under the vacuum condition of 100Kpa, wherein the material temperature is 400 ℃, the pressure is 15MPa, and the dwell time is 1 h.
Example 3:
(1) And (3) batching: 68 parts of polytetrafluoroethylene dispersion resin powder and 75 parts of ceramic powder are respectively sieved and mixed according to the proportion to obtain a primary mixed material.
(2) And (3) hot mixing of air flow: pouring the primary mixed material obtained in the step (1) into an airflow mixer, adding 25 parts of odorless kerosene and 8 parts of absolute ethyl alcohol into an oil injection bottle according to the proportion, and circularly mixing for 4 hours at the temperature of 65 ℃ to obtain a uniform mixed material, wherein the circulating hot airflow in a sealed cavity is 20 kg/time.
(3) Sheet extrusion: sieving the uniformly mixed material obtained in the step (2), pouring the sieved uniformly mixed material into a prepressing forming machine to be prepressed into a cylinder, placing the cylinder in an extruder, extruding a windable film with the width of 10-30cm and the thickness of 1-5mm through a heating cavity and a sheet-shaped basic die opening, wherein the temperature of the heating cavity is 30 ℃, and the temperature of the sheet-shaped extrusion die opening is 52 ℃.
(4) Rolling and forming into a sheet: and (3) carrying out one or more times of die rolling and sheeting on the windable film obtained in the step (3) through a multi-roll mill to obtain the adhesive sheet with the width of 45-55cm and the thickness of 0.038-0.75mm, wherein the temperature of the multi-roll mill is 60 ℃.
(5) Baking at low temperature: and (3) baking the bonding sheet obtained in the step (4) through a degreasing drying oven to remove odorless kerosene and absolute ethyl alcohol, so as to obtain a baked bonding sheet, wherein the baking temperature is 160 ℃/10min/m.
(6) High-temperature vacuum forming: and (3) cutting the baked bonding sheet obtained in the step (5), laminating and double-sided copper coating according to the thickness difference of the manufactured copper-clad plate, performing hot press forming through an oil pressure vacuum high-temperature press, wherein the vacuum condition is 97Kpa, and the baking bonding sheet is manufactured at the material temperature of 380 ℃, the pressure of 12MPa and the dwell time of 1 h.
Example 4:
(1) And (3) batching: after 70 parts of polytetrafluoroethylene dispersion resin powder and 68 parts of ceramic powder are respectively sieved, the mixture is mixed according to the proportion to obtain a primary mixed material.
(2) And (3) hot mixing of air flow: pouring the primary mixed material obtained in the step (1) into an airflow mixer, adding 22 parts of odorless kerosene and 10 parts of absolute ethyl alcohol into an oil injection bottle according to the proportion, and circularly mixing for 4 hours at the temperature of 45 ℃ to obtain a uniform mixed material, wherein the circulating hot airflow in a sealed cavity is 5 kg/time.
(3) Sheet extrusion: sieving the uniformly mixed material obtained in the step (2), pouring the sieved uniformly mixed material into a prepressing forming machine to be prepressed into a cylinder, placing the cylinder in an extruder, extruding a windable film with the width of 10-30cm and the thickness of 1-5mm through a heating cavity and a sheet-shaped basic die opening, wherein the temperature of the heating cavity is 47 ℃, and the temperature of the sheet-shaped extrusion die opening is 60 ℃.
(4) Rolling and forming into a sheet: and (3) carrying out one or more times of die rolling and sheeting on the windable film obtained in the step (3) through a multi-roll mill to obtain the adhesive sheet with the width of 45-55cm and the thickness of 0.038-0.75mm, wherein the temperature of the multi-roll mill is 60 ℃.
(5) Baking at low temperature: and (3) baking the bonding sheet obtained in the step (4) through a degreasing drying oven to remove odorless kerosene and absolute ethyl alcohol, so as to obtain a baked bonding sheet, wherein the baking temperature is 200 ℃/10min/m.
(6) High-temperature vacuum forming: and (3) cutting the baked bonding sheet obtained in the step (5), carrying out lamination and double-sided copper coating according to the thickness difference of the manufactured copper-clad plate, carrying out hot press molding by an oil pressure vacuum high-temperature press, and completing the preparation at the material temperature of 390 ℃ under the pressure of 5MPa for 1h under the vacuum condition of 100 Kpa.
Example 5:
(1) And (3) batching: sieving 40 parts of polytetrafluoroethylene dispersion resin powder and 50 parts of ceramic powder respectively, and mixing according to the proportion to obtain a primary mixed material.
(2) And (3) hot mixing of air flow: pouring the primary mixed material obtained in the step (1) into an airflow mixer, adding 18 parts of white oil and 6 parts of absolute ethyl alcohol into an oil injection bottle according to the proportion, and circularly mixing for 4 hours at the temperature of 55 ℃ to obtain a uniform mixed material, wherein the circulating hot airflow in a sealed cavity is 18 kg/time.
(3) Sheet extrusion: sieving the uniformly mixed material obtained in the step (2), pouring the sieved uniformly mixed material into a prepressing forming machine to be prepressed into a cylinder, placing the cylinder in an extruder, extruding a windable film with the width of 10-30cm and the thickness of 1-5mm through a heating cavity and a sheet-shaped basic die opening, wherein the temperature of the heating cavity is 50 ℃, and the temperature of the sheet-shaped extrusion die opening is 52 ℃.
(4) Rolling and forming into a sheet: and (3) carrying out one or more times of die rolling and sheeting on the windable film obtained in the step (3) through a multi-roll mill to obtain the adhesive sheet with the width of 45-55cm and the thickness of 0.038-0.75mm, wherein the temperature of the multi-roll mill is 60 ℃.
(5) Baking at low temperature: and (3) baking the bonding sheet obtained in the step (4) through a degreasing drying oven to remove white oil and absolute ethyl alcohol, so as to obtain a baked bonding sheet, wherein the baking temperature is 180 ℃/10min/m.
(6) High-temperature vacuum forming: and (3) cutting the baked bonding sheet obtained in the step (5), laminating and double-sided copper coating according to the thickness difference of the manufactured copper-clad plate, performing hot press forming through an oil pressure vacuum high-temperature press, and completing the preparation at the material temperature of 388 ℃, the pressure of 6MPa and the pressure maintaining time of 1h under the vacuum condition of 93 Kpa.
Example 6:
(1) And (3) batching: 46 parts of polytetrafluoroethylene dispersion resin powder and 53 parts of ceramic powder are respectively sieved and mixed according to the proportion to obtain a primary mixed material.
(2) And (3) hot mixing of air flow: pouring the primary mixed material obtained in the step (1) into an airflow mixer, adding 16 parts of white oil and 5 parts of absolute ethyl alcohol into an oil injection bottle according to the proportion, and circularly mixing for 4 hours at the temperature of 55 ℃ to obtain a uniform mixed material, wherein the circulation hot airflow in a sealed cavity is 16 kg/time.
(3) Sheet extrusion: sieving the uniformly mixed material obtained in the step (2), pouring the sieved uniformly mixed material into a prepressing forming machine to be prepressed into a cylinder, placing the cylinder in an extruder, extruding a windable film with the width of 10-30cm and the thickness of 1-5mm through a heating cavity and a sheet-shaped basic die opening, wherein the temperature of the heating cavity is 45 ℃, and the temperature of the sheet-shaped extrusion die opening is 56 ℃.
(4) Rolling and forming into a sheet: and (3) carrying out one or more times of die rolling and sheeting on the windable film obtained in the step (3) through a multi-roll mill to obtain the adhesive sheet with the width of 45-55cm and the thickness of 0.038-0.75mm, wherein the temperature of the multi-roll mill is 60 ℃.
(5) Baking at low temperature: and (3) baking the bonding sheet obtained in the step (4) through a degreasing drying oven to remove white oil and absolute ethyl alcohol, so as to obtain a baked bonding sheet, wherein the baking temperature is 186 ℃/10min/m.
(6) High-temperature vacuum forming: and (3) cutting the baked bonding sheet obtained in the step (5), laminating and double-sided copper coating according to the thickness difference of the manufactured copper-clad plate, performing hot press forming through an oil pressure vacuum high-temperature press, wherein the vacuum condition is 93Kpa, and the baking bonding sheet is manufactured at the temperature of 386 ℃, the pressure of 7MPa and the dwell time of 1 h.
Example 7:
(1) And (3) batching: after 48 parts of polytetrafluoroethylene dispersion resin powder and 69 parts of ceramic powder are respectively sieved, the mixture is mixed according to the proportion to obtain a primary mixed material.
(2) And (3) hot mixing of air flow: pouring the primary mixed material obtained in the step (1) into an airflow mixer, adding 23 parts of isoparaffin and 8 parts of absolute ethyl alcohol into an oil injection bottle according to the proportion, and circularly mixing for 4 hours at the temperature of 58 ℃ to obtain a uniform mixed material, wherein the circulating hot airflow in a sealed cavity is 23 kg/time.
(3) Sheet extrusion: sieving the uniformly mixed material obtained in the step (2), pouring the sieved uniformly mixed material into a prepressing forming machine to be prepressed into a cylinder, placing the cylinder in an extruder, extruding a windable film with the width of 10-30cm and the thickness of 1-5mm through a heating cavity and a sheet-shaped basic die opening, wherein the temperature of the heating cavity is 43 ℃, and the temperature of the sheet-shaped extrusion die opening is 54 ℃.
(4) Rolling and forming into a sheet: and (3) carrying out one or more times of die rolling and sheeting on the windable film obtained in the step (3) through a multi-roll mill to obtain the adhesive sheet with the width of 45-55cm and the thickness of 0.038-0.75mm, wherein the temperature of the multi-roll mill is 60 ℃.
(5) Baking at low temperature: and (3) baking the bonding sheet obtained in the step (4) through a degreasing drying oven to remove isoparaffin and absolute ethyl alcohol, so as to obtain a baked bonding sheet, wherein the baking temperature is 198 ℃/10min/m.
(6) High-temperature vacuum forming: and (3) cutting the baked bonding sheet obtained in the step (5), carrying out lamination and double-sided copper coating according to the thickness difference of the manufactured copper-clad plate, carrying out hot press molding by an oil pressure vacuum high-temperature press, and completing the preparation at the material temperature of 396 ℃ under the pressure of 6MPa for 1 h.
Example 8:
(1) And (3) batching: sieving 30 parts of polytetrafluoroethylene dispersion resin powder and 50 parts of ceramic powder respectively, and mixing according to the proportion to obtain a primary mixed material.
(2) And (3) hot mixing of air flow: pouring the primary mixed material obtained in the step (1) into an airflow mixer, adding 15 parts of isoparaffin and 9 parts of absolute ethyl alcohol into an oil injection bottle according to the proportion, and circularly mixing for 4 hours at the temperature of 50 ℃ to obtain a uniform mixed material, wherein the circulating hot airflow in a sealed cavity is 16 kg/time.
(3) Sheet extrusion: sieving the uniformly mixed material obtained in the step (2), pouring the sieved uniformly mixed material into a prepressing forming machine to be prepressed into a cylinder, placing the cylinder in an extruder, extruding a windable film with the width of 10-30cm and the thickness of 1-5mm through a heating cavity and a sheet-shaped basic die opening, wherein the temperature of the heating cavity is 40 ℃, and the temperature of the sheet-shaped extrusion die opening is 58 ℃.
(4) Rolling and forming into a sheet: and (3) carrying out one or more times of die rolling and sheeting on the windable film obtained in the step (3) through a multi-roll mill to obtain the adhesive sheet with the width of 45-55cm and the thickness of 0.038-0.75mm, wherein the temperature of the multi-roll mill is 60 ℃.
(5) Baking at low temperature: and (3) baking the bonding sheet obtained in the step (4) through a degreasing drying oven to remove isoparaffin and absolute ethyl alcohol, so as to obtain a baked bonding sheet, wherein the baking temperature is 235 ℃/10min/m.
(6) High-temperature vacuum forming: and (3) cutting the baked bonding sheet obtained in the step (5), carrying out lamination and double-sided copper coating according to the thickness difference of the manufactured copper-clad plate, carrying out hot press molding by an oil pressure vacuum high-temperature press, and completing the preparation at the material temperature of 398 ℃ under the pressure of 6MPa for 1h under the vacuum condition.
Example 9:
(1) And (3) batching: sieving 65 parts of polytetrafluoroethylene dispersion resin powder and 50 parts of ceramic powder respectively, and mixing according to the proportion to obtain a primary mixed material.
(2) And (3) hot mixing of air flow: pouring the primary mixed material obtained in the step (1) into an airflow mixer, adding 16 parts of isoparaffin and 6 parts of absolute ethyl alcohol into an oil injection bottle according to the proportion, and circularly mixing for 4 hours at the temperature of 55 ℃ to obtain a uniform mixed material, wherein the circulating hot airflow in a sealed cavity is 20 kg/time.
(3) Sheet extrusion: sieving the uniformly mixed material obtained in the step (2), pouring the sieved uniformly mixed material into a prepressing forming machine to be prepressed into a cylinder, placing the cylinder in an extruder, extruding a windable film with the width of 10-30cm and the thickness of 1-5mm through a heating cavity and a sheet-shaped basic die opening, wherein the temperature of the heating cavity is 50 ℃, and the temperature of the sheet-shaped extrusion die opening is 55 ℃.
(4) Rolling and forming into a sheet: and (3) carrying out one or more times of die rolling and sheeting on the windable film obtained in the step (3) through a multi-roll mill to obtain the adhesive sheet with the width of 45-55cm and the thickness of 0.038-0.75mm, wherein the temperature of the multi-roll mill is 60 ℃.
(5) Baking at low temperature: and (3) baking the bonding sheet obtained in the step (4) through a degreasing drying oven to remove isoparaffin and absolute ethyl alcohol, so as to obtain a baked bonding sheet, wherein the baking temperature is 180 ℃/10min/m.
(6) High-temperature vacuum forming: and (3) cutting the baked bonding sheet obtained in the step (5), laminating and double-sided copper coating according to the thickness difference of the manufactured copper-clad plate, performing hot press forming through an oil pressure vacuum high-temperature press, wherein the vacuum condition is 93Kpa, and the baking bonding sheet is manufactured at the material temperature of 400 ℃, the pressure of 10MPa and the dwell time of 1 h.
The samples obtained in the above examples were subjected to performance tests, and the test results are shown in table 1.
TABLE 1
The testing method comprises the following steps:
1. the thickness was measured using a thickness detector.
2. The peel strength was measured according to the method prescribed in IPC-TM-650 by 2.4.8.
3. Copper-containing tin bleaches were measured as specified by method 2.6.8 in IPC-TM-650.
4. Dielectric constants were measured at 1GHz and 10GHz by using SPDR (splite post dielectric resonator) method.
5. Dielectric loss was measured at 10GHz by SPDR (splite post dielectric resonator) method.
6. The coefficient of thermal expansion was measured using the method specified in IPC-TM-650 as 2.4.41.
At present, the main flow of the market requires a board to be DK3.0, and the lowest loss of the board is 0.00035 corresponding to DK3.0-0.254mm, so that the test of dielectric constant stability is carried out on the sample obtained in the embodiment 2, the test results are shown in fig. 1 and 2, the stability of the dielectric constant of the board under different frequencies is proved in fig. 1, the inherent stability of the board in the frequency is illustrated, and convenience is provided for circuit design; fig. 2 demonstrates the stability of the dielectric constant of the sheet material at different temperatures, demonstrating that the material maintains stable dielectric constant characteristics over a wide range of temperature variations. The curves of fig. 1 and 2 were both obtained by the stripline test.
According to the results, the copper-clad plate manufactured by the method has high heat resistance, ultralow dielectric loss, stable and adjustable dielectric constant, excellent dimensional stability, weather resistance and the like, and can meet different high requirements of a high-frequency transmission system on a printed circuit board.
The foregoing description is only a preferred embodiment of the present invention, and is not intended to limit the technical scope of the present invention, so any minor modifications, equivalent changes and modifications made to the above embodiments according to the technical principles of the present invention are still within the scope of the technical solutions of the present invention.

Claims (8)

1. The preparation method of the high-frequency ultralow-dielectric-loss microwave ceramic copper-clad plate is characterized by comprising the following components in parts by mass: 30-75 parts of ceramic powder, 25-70 parts of polytetrafluoroethylene dispersion resin powder, 15-25 parts of solvent oil and 5-10 parts of absolute ethyl alcohol; the method comprises the following steps:
(1) And (3) batching: sieving polytetrafluoroethylene dispersion resin powder and ceramic powder respectively, and mixing according to the proportion to obtain a primary mixed material;
(2) And (3) hot mixing of air flow: pouring the primary mixed material obtained in the step (1) into an airflow mixer, adding solvent oil and absolute ethyl alcohol into an oil injection bottle according to the proportion, and circularly mixing for 4 hours at the temperature of 45-65 ℃ to obtain a uniform mixed material, wherein the circulating hot airflow in a sealed cavity is 5-25 kg/time;
(3) Sheet extrusion: sieving the uniformly mixed material obtained in the step (2), pouring the sieved uniformly mixed material into a prepressing forming machine to be prepressed into a cylinder, placing the cylinder in an extruder, extruding a windable film with the width of 10-30cm and the thickness of 1-5mm through a heating cavity and a sheet-shaped basic die opening, wherein the temperature of the heating cavity is 30-50 ℃, and the temperature of the sheet-shaped extrusion die opening is 50-60 ℃;
(4) Rolling and forming into a sheet: rolling the windable film obtained in the step (3) into a sheet for one or more times by an open mill to obtain an adhesive sheet with the width of 45-55cm and the thickness of 0.038-0.75mm, wherein the temperature of the open mill is 60 ℃;
(5) Baking at low temperature: baking the bonding sheet obtained in the step (4) through a degreasing drying oven to remove solvent oil and absolute ethyl alcohol to obtain a baked bonding sheet, wherein the baking temperature is 160-240 ℃/10min/m;
(6) High-temperature vacuum forming: cutting the baked bonding sheet obtained in the step (5), carrying out lamination and double-sided copper coating according to the difference of the thickness of the manufactured copper-clad plate, carrying out hot press molding by an oil pressure vacuum high-temperature press, and completing the preparation under the conditions that the vacuum condition is 90-100Kpa, the material temperature is 380-405 ℃, the pressure is 5-15MPa, and the dwell time is 1 h.
2. The method for preparing the high-frequency ultralow dielectric loss microwave ceramic copper-clad plate according to claim 1, which is characterized by comprising the following steps: the ceramic powder has a spherical structure, a spherical aggregate structure or a hollow sphere structure, the sphericity of the ceramic powder is more than or equal to 90 percent, and the particle size is 0.5-40 mu m.
3. The method for preparing the high-frequency ultralow dielectric loss microwave ceramic copper-clad plate according to claim 1, which is characterized by comprising the following steps: the ceramic powder is one or a mixture of more of titanium dioxide, silicon dioxide, barium titanate, strontium titanate, aluminum oxide and rare earth.
4. The method for preparing the high-frequency ultralow dielectric loss microwave ceramic copper-clad plate according to claim 1, which is characterized by comprising the following steps: the solvent oil is one or more of odorless kerosene, white oil and isoparaffin.
5. The method for preparing the high-frequency ultralow dielectric loss microwave ceramic copper-clad plate according to claim 1, which is characterized by comprising the following steps: the temperature of the material in the step (6) is 400 ℃.
6. The method for preparing the high-frequency ultralow dielectric loss microwave ceramic copper-clad plate according to claim 1, which is characterized by comprising the following steps: and (3) the extrusion opening of the sheet extrusion die in the step (3) is 20cm wide.
7. The method for preparing the high-frequency ultralow dielectric loss microwave ceramic copper-clad plate according to claim 1, which is characterized by comprising the following steps: the open mill in the step (4) is a multi-roller open mill.
8. A high-frequency ultralow dielectric loss microwave ceramic copper-clad plate is characterized in that: prepared by the preparation method of the high-frequency ultralow dielectric loss microwave ceramic copper-clad plate according to any one of claims 1 to 7.
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CN114509474A (en) * 2022-01-28 2022-05-17 山东国瓷功能材料股份有限公司 Detection method for dielectric property of ceramic powder and application thereof
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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102555349A (en) * 2012-02-22 2012-07-11 珠海国能复合材料科技有限公司 Method for manufacturing ceramic filled polytetrafluoroethylene glass fiber copper-clad substrate
CN104647868A (en) * 2015-02-10 2015-05-27 郴州功田电子陶瓷技术有限公司 Manufacturing method for polytetrafluoroethylene copper-clad plate
CN107474312A (en) * 2017-06-12 2017-12-15 电子科技大学 The preparation method of ceramic filled polytetrafluoroethylglass microwave composite medium substrate
WO2020114419A1 (en) * 2018-12-04 2020-06-11 大金氟化工(中国)有限公司 Preparation method for polytetrafluoroethylene composition, polytetrafluoroethylene composition, forming product, conductive pipe, heat conduction film, and substrate ccl

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US9455064B2 (en) * 2012-12-12 2016-09-27 Centre for Materials for Electronics Technology (C-MET) Ceramic filled fluoropolymer compositions, methods and applications thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102555349A (en) * 2012-02-22 2012-07-11 珠海国能复合材料科技有限公司 Method for manufacturing ceramic filled polytetrafluoroethylene glass fiber copper-clad substrate
CN104647868A (en) * 2015-02-10 2015-05-27 郴州功田电子陶瓷技术有限公司 Manufacturing method for polytetrafluoroethylene copper-clad plate
CN107474312A (en) * 2017-06-12 2017-12-15 电子科技大学 The preparation method of ceramic filled polytetrafluoroethylglass microwave composite medium substrate
WO2020114419A1 (en) * 2018-12-04 2020-06-11 大金氟化工(中国)有限公司 Preparation method for polytetrafluoroethylene composition, polytetrafluoroethylene composition, forming product, conductive pipe, heat conduction film, and substrate ccl

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