CN113306227A - 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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CN113306227A
CN113306227A CN202110579176.7A CN202110579176A CN113306227A CN 113306227 A CN113306227 A CN 113306227A CN 202110579176 A CN202110579176 A CN 202110579176A CN 113306227 A CN113306227 A CN 113306227A
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temperature
clad plate
dielectric loss
sheet
parts
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CN113306227B (en
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陈功田
陈建
李海林
彭灿
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Chenzhou Gongtian Electronic Ceramic Technology Co ltd
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Chenzhou Gongtian Electronic Ceramic Technology Co ltd
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    • Y02P20/10—Process efficiency

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 dispersed resin powder, 15-25 parts of solvent oil and 5-10 parts of absolute ethyl alcohol; the high-frequency ultralow dielectric loss microwave ceramic copper-clad plate which has ultralow dielectric loss, stable and adjustable dielectric constant, excellent dimensional stability and weather resistance and can meet the requirement of high frequency is obtained by filling ceramic powder with polytetrafluoroethylene dispersed resin powder, matching with alkane solvent oil and a proper amount of absolute ethyl alcohol, and performing the procedures of material preparation, airflow hot mixing, sheet extrusion, mold rolling, low-temperature baking, high-temperature vacuum forming and the like. The invention has simple process, environmental protection and large-scale industrial production, has excellent product 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 condition that the demand of 5G communication materials is more and more intense at present, information electronic products develop towards the direction of high frequency, high speed, high precision and high reliability, and the demand of related equipment such as wireless millimeter wave communication and the like is rapidly increased. The polytetrafluoroethylene copper-clad plate mainly takes emulsion and cutting film as main materials, and has better electrical performance than the current domestic mainstream hydrocarbon copper-clad plate, epoxy resin copper-clad plate, PPO copper-clad plate and the like. The raw materials and the manufacturing process have high cost, so that the application of the copper clad laminate is limited, and the manufactured copper clad laminate has narrow and unstable adjustable range of dielectric constant, relatively high dielectric loss, low dimensional stability, low weather resistance and low reliability. Therefore, there is a need to provide a new solution to improve the existing copper-clad plate.
Disclosure of Invention
In view of the above, the present invention provides a high-frequency microwave ceramic copper-clad plate with ultra-low dielectric loss and a preparation method thereof, which can effectively solve the problems of high production cost, narrow and unstable adjustable range of dielectric constant, relatively high dielectric loss, low dimensional stability, low weather resistance and low reliability of the existing copper-clad plate.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a 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 dispersed resin powder, 15-25 parts of solvent oil and 5-10 parts of absolute ethyl alcohol; the method comprises the following steps:
(1) preparing materials: respectively sieving polytetrafluoroethylene dispersed resin powder and ceramic powder, and mixing according to the proportion to obtain a primary mixed material;
(2) airflow hot mixing: 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, circularly mixing for 4 hours at the temperature of 45-65 ℃ to obtain uniformly mixed material, and circulating hot airflow in a sealed cavity for 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 pre-pressing forming machine, pre-pressing the uniformly mixed material into a cylinder, placing the cylinder in an extruder, and extruding a reelable rubber sheet 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 molding into sheets: rolling the reelable rubber sheet obtained in the step (3) into a mold sheet for one time or more times by using 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) and (3) low-temperature baking: baking the bonding sheet obtained in the step (4) in a degreasing drying oven to remove solvent oil and absolute ethyl alcohol to obtain a baked bonding sheet, wherein the baking temperature is 160-;
(6) high-temperature vacuum forming: and (3) cutting the baked bonding sheet obtained in the step (5), laminating and coating copper on two sides according to the difference of the thicknesses of the manufactured copper clad plates, and performing hot press molding by using an oil-pressure vacuum high-temperature press under the vacuum condition of 90-100Kpa, wherein the baking bonding sheet is prepared under the conditions that the material temperature is 380-405 ℃, the pressure is 5-15MPa and the pressure maintaining time is 1 h.
As a preferable scheme, the structure of the ceramic powder is spherical, spherical aggregate or hollow spherical, the sphericity of the ceramic powder is more than or equal to 90%, and the particle size is 0.5-40 μm.
As a preferred scheme, the ceramic powder is one or a mixture of more 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 more of odorless kerosene, white oil and isoparaffin.
As a preferable scheme, the material temperature in the step (6) is 400 ℃.
As a preferable scheme, the width of the extrusion port of the sheet-like extrusion die of the step (3) is 20 cm.
As a preferable scheme, the open mill in the step (4) is a multi-roller open mill.
A 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 specifically, the technical scheme includes that:
the high-frequency ultralow dielectric loss microwave ceramic copper-clad plate which has ultralow dielectric loss, stable and adjustable dielectric constant, excellent dimensional stability and weather resistance and can meet the requirement of high frequency is obtained by filling ceramic powder with polytetrafluoroethylene dispersed resin powder, matching with alkane solvent oil and a proper amount of absolute ethyl alcohol, and performing the working procedures of material preparation, airflow hot mixing, sheet extrusion, mold rolling, low-temperature baking, high-temperature vacuum forming and the like; in addition, the invention has simple process, environmental protection and large-scale industrial production, has excellent product 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 of the dielectric constant 3.0 versus frequency characteristic of the preferred embodiment 2 of the present invention;
FIG. 2 is a graph showing the temperature dependence of the dielectric constant of 3.0 in accordance with 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 dispersed resin powder, 15-25 parts of solvent oil and 5-10 parts of absolute ethyl alcohol; the method comprises the following steps:
(1) preparing materials: and respectively sieving the polytetrafluoroethylene dispersed resin powder and the ceramic powder, and mixing according to the proportion to obtain a primary mixed material.
(2) Airflow hot mixing: 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, circularly mixing for 4 hours at the temperature of 45-65 ℃ to obtain uniformly mixed material, and circulating hot airflow in a sealed cavity for 5-25 kg/time; the oil spray bottle is used for controlling the oil filling precision and spraying to ensure that the mixing is more uniform; spraying regularly and quantitatively under circulating hot air, wherein the hot air aims to fully lubricate and uniformly mix solvent oil, polytetrafluoroethylene dispersed resin powder and ceramic powder molecules for the next step, and meanwhile, the mixing and curing time is shortened by adding absolute ethyl alcohol, so that the obtained uniformly mixed material is more uniform and sufficient.
(3) Sheet extrusion: sieving the uniformly mixed material obtained in the step (2), pouring the uniformly mixed material into a pre-pressing forming machine, pre-pressing the uniformly mixed material into a cylinder, placing the cylinder into an extruder, and extruding a reelable 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 molding into sheets: rolling the reelable rubber sheet obtained in the step (3) into a mold sheet for one time or more times by using 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 a high-performance membrane material manufactured by pure polytetrafluoroethylene extrusion rolling is 30cm, the rolling width is limited because the circular extrusion is in a rod shape, and the bottleneck of manufacturing a ceramic-filled polytetrafluoroethylene copper-clad plate by extrusion rolling is width improvement and how to mix ceramic powder and extrude the ceramic powder completely and uniformly; the purpose of the width increase is to match the subsequent circuit board processing factory process, and the small size caused by the too small width will increase the cost of batch production and subsequent processing.
(5) And (3) low-temperature baking: baking the bonding sheet obtained in the step (4) in a degreasing drying oven to remove solvent oil and absolute ethyl alcohol to obtain a baked bonding sheet, wherein the baking temperature is 160-; according to the difference of the dielectric constant of the manufactured copper-clad plate, the bonding sheet needs to be longitudinally pulled up and shaped in the baking process, the speed is not too high, and the film is too dry due to too high temperature, so that the defect of holes is caused after the next step of lamination, and the solvent oil is incompletely volatilized due to too low temperature, so that the condition of reduction of lamination bubbles or medium loss increase stripping is caused.
(6) High-temperature vacuum forming: cutting the baked bonding sheet obtained in the step (5), laminating and coating copper on two sides according to the different thicknesses of the manufactured copper clad plates, and performing hot press molding by using an oil-pressure vacuum high-temperature press under the vacuum condition of 90-100Kpa, wherein the baking bonding sheet is manufactured under the conditions that the material temperature is 380-405 ℃, the pressure is 5-15MPa and the pressure maintaining time is 1 h; typically 18um electrolytic copper foil is selected.
The structure of the ceramic powder is spherical, spherical aggregate or hollow spherical, 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 filling proportion of the spherical filler matched with the high-density high-tensile-strength polytetrafluoroethylene dispersion resin powder can reach 80 percent, and the composite particle size of different fillers is used for further improving the filling proportion and the electrical property; taking the distribution of every 10 μm as an example, the typical compound is 4:2:3:1, namely, the grain diameter below 10 μm accounts for 40%, the grain diameter below 10 μm accounts for 20%, the grain diameter between 20 μm and 20 μm accounts for 30%, and the grain diameter between 30 μm and 40 μm accounts for 10%. Selecting polytetrafluoroethylene dispersion resin powder with different densities and tensile strengths according to different dielectric constants. Typical relative density is 2.2g/cm, tensile strength is 24 MPa.
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 a mixture of more of odorless kerosene, white oil and isoparaffin.
In the step (6), the material temperature is 400 ℃, the temperature of the oil pressure vacuum press with the temperature of 400 ℃ is more uniform than that of a hot plate of an electric heating press, the performance of the plate is more stable to a certain extent, and the batch production is easier to control.
The width of the extrusion opening of the sheet extrusion die in the step (3) is 20 cm.
The open mill in the step (4) is a multi-roller open mill, and is beneficial to wide 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 illustrated in more detail below in the following examples:
example 1:
(1) preparing materials: and respectively sieving 50 parts of polytetrafluoroethylene dispersed resin powder and 30 parts of ceramic powder, and mixing according to the proportion to obtain a primary mixed material.
(2) Airflow hot mixing: 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, circularly mixing for 4 hours at the temperature of 45 ℃ to obtain uniformly mixed material, and circulating hot airflow in a sealed cavity for 15 kg/time.
(3) Sheet extrusion: sieving the uniformly mixed material obtained in the step (2), pouring the uniformly mixed material into a pre-pressing forming machine, pre-pressing the uniformly mixed material into a cylinder, placing the cylinder in an extruder, and extruding a reelable 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 molding into sheets: and (4) carrying out one-time or multiple-time rolling and molding on the reelable rubber sheet obtained in the step (3) to form a sheet by using a multi-roller open mill, so as to obtain an adhesive sheet with the width of 45-55cm and the thickness of 0.038-0.75mm, wherein the temperature of the multi-roller open mill is 60 ℃.
(5) And (3) low-temperature baking: and (4) baking the bonding sheet obtained in the step (4) by a degreasing drying oven to remove odorless kerosene and absolute ethyl alcohol to obtain a baked bonding sheet, wherein the baking temperature is 240 ℃/10 min/m.
(6) High-temperature vacuum forming: and (4) cutting the baked bonding sheet obtained in the step (5), laminating and coating copper on two sides according to the difference of the thicknesses of the manufactured copper clad plates, and performing hot press molding by using an oil-pressure vacuum high-temperature press under the vacuum condition of 90Kpa, at the material temperature of 405 ℃, under the pressure of 10MPa and for the pressure maintaining time of 1h to obtain the finished product.
Example 2:
(1) preparing materials: and respectively sieving 25 parts of polytetrafluoroethylene dispersed resin powder and 50 parts of ceramic powder, and mixing according to the proportion to obtain a primary mixed material.
(2) Airflow hot mixing: 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, circularly mixing for 4 hours at the temperature of 55 ℃ to obtain uniformly mixed material, and circulating hot airflow in a sealed cavity for 25 kg/time.
(3) Sheet extrusion: sieving the uniformly mixed material obtained in the step (2), pouring the uniformly mixed material into a pre-pressing forming machine, pre-pressing the uniformly mixed material into a cylinder, placing the cylinder in an extruder, and extruding a reelable rubber sheet 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 molding into sheets: and (4) carrying out one-time or multiple-time rolling and molding on the reelable rubber sheet obtained in the step (3) to form a sheet by using a multi-roller open mill, so as to obtain an adhesive sheet with the width of 45-55cm and the thickness of 0.038-0.75mm, wherein the temperature of the multi-roller open mill is 60 ℃.
(5) And (3) low-temperature baking: and (4) baking the bonding sheet obtained in the step (4) by a degreasing drying oven to remove odorless kerosene and absolute ethyl alcohol to obtain a baked bonding sheet, wherein the baking temperature is 200 ℃/10 min/m.
(6) High-temperature vacuum forming: and (4) cutting the baked bonding sheet obtained in the step (5), laminating and coating copper on two sides according to the difference of the thicknesses of the manufactured copper clad plates, and performing hot press molding by using an oil-pressure vacuum high-temperature press under the vacuum condition of 100Kpa, at the material temperature of 400 ℃, under the pressure of 15MPa and for the pressure maintaining time of 1h to obtain the copper clad plate.
Example 3:
(1) preparing materials: and respectively sieving 68 parts of polytetrafluoroethylene dispersed resin powder and 75 parts of ceramic powder, and mixing according to the proportion to obtain a primary mixed material.
(2) Airflow hot mixing: 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, circularly mixing for 4 hours at the temperature of 65 ℃ to obtain uniformly mixed material, and circulating hot airflow in a sealed cavity for 20 kg/time.
(3) Sheet extrusion: sieving the uniformly mixed material obtained in the step (2), pouring the uniformly mixed material into a pre-pressing forming machine, pre-pressing the uniformly mixed material into a cylinder, placing the cylinder in an extruder, and extruding a reelable rubber sheet 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 molding into sheets: and (4) carrying out one-time or multiple-time rolling and molding on the reelable rubber sheet obtained in the step (3) to form a sheet by using a multi-roller open mill, so as to obtain an adhesive sheet with the width of 45-55cm and the thickness of 0.038-0.75mm, wherein the temperature of the multi-roller open mill is 60 ℃.
(5) And (3) low-temperature baking: and (4) baking the bonding sheet obtained in the step (4) by a degreasing drying oven to remove odorless kerosene and absolute ethyl alcohol to obtain a baked bonding sheet, wherein the baking temperature is 160 ℃/10 min/m.
(6) High-temperature vacuum forming: and (4) cutting the baked bonding sheet obtained in the step (5), laminating and coating copper on two sides according to the difference of the thicknesses of the manufactured copper clad plates, and performing hot press molding by using an oil-pressure vacuum high-temperature press under the vacuum condition of 97Kpa, at the material temperature of 380 ℃, under the pressure of 12MPa and for the pressure maintaining time of 1h to obtain the copper clad plate.
Example 4:
(1) preparing materials: and sieving 70 parts of polytetrafluoroethylene dispersed resin powder and 68 parts of ceramic powder respectively, and mixing according to the proportion to obtain a primary mixed material.
(2) Airflow hot mixing: 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, circularly mixing for 4 hours at the temperature of 45 ℃ to obtain uniformly mixed material, and circulating hot airflow in a sealed cavity for 5 kg/time.
(3) Sheet extrusion: sieving the uniformly mixed material obtained in the step (2), pouring the uniformly mixed material into a pre-pressing forming machine, pre-pressing the uniformly mixed material into a cylinder, placing the cylinder in an extruder, and extruding a reelable 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 molding into sheets: and (4) carrying out one-time or multiple-time rolling and molding on the reelable rubber sheet obtained in the step (3) to form a sheet by using a multi-roller open mill, so as to obtain an adhesive sheet with the width of 45-55cm and the thickness of 0.038-0.75mm, wherein the temperature of the multi-roller open mill is 60 ℃.
(5) And (3) low-temperature baking: and (4) baking the bonding sheet obtained in the step (4) by a degreasing drying oven to remove odorless kerosene and absolute ethyl alcohol to obtain a baked bonding sheet, wherein the baking temperature is 200 ℃/10 min/m.
(6) High-temperature vacuum forming: and (3) cutting the baked bonding sheet obtained in the step (5), laminating and coating copper on two sides according to the difference of the thicknesses of the manufactured copper clad plates, and performing hot press molding by using an oil-pressure vacuum high-temperature press under the vacuum condition of 100Kpa, at the material temperature of 390 ℃, at the pressure of 5MPa and for the pressure maintaining time of 1h to obtain the copper clad plate.
Example 5:
(1) preparing materials: and respectively sieving 40 parts of polytetrafluoroethylene dispersed resin powder and 50 parts of ceramic powder, and mixing according to the proportion to obtain a primary mixed material.
(2) Airflow hot mixing: pouring the initial mixture 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, circularly mixing for 4 hours at the temperature of 55 ℃ to obtain uniformly mixed materials, and circulating hot airflow in a sealed cavity for 18 kg/time.
(3) Sheet extrusion: sieving the uniformly mixed material obtained in the step (2), pouring the uniformly mixed material into a pre-pressing forming machine, pre-pressing the uniformly mixed material into a cylinder, placing the cylinder in an extruder, and extruding a reelable 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 molding into sheets: and (4) carrying out one-time or multiple-time rolling and molding on the reelable rubber sheet obtained in the step (3) to form a sheet by using a multi-roller open mill, so as to obtain an adhesive sheet with the width of 45-55cm and the thickness of 0.038-0.75mm, wherein the temperature of the multi-roller open mill is 60 ℃.
(5) And (3) low-temperature baking: and (5) baking the bonding sheet obtained in the step (4) in a degreasing drying oven to remove white oil and absolute ethyl alcohol to obtain a baked bonding sheet, wherein the baking temperature is 180 ℃/10 min/m.
(6) High-temperature vacuum forming: and (3) cutting the baked bonding sheet obtained in the step (5), laminating and coating copper on two sides according to the different thicknesses of the manufactured copper clad plates, and performing hot press molding by using an oil-pressure vacuum high-temperature press under the vacuum condition of 93Kpa, at the material temperature of 388 ℃, at the pressure of 6MPa and for the pressure maintaining time of 1h to obtain the finished product.
Example 6:
(1) preparing materials: and respectively sieving 46 parts of polytetrafluoroethylene dispersed resin powder and 53 parts of ceramic powder, and mixing according to the proportion to obtain a primary mixed material.
(2) Airflow hot mixing: pouring the initial mixture 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, circularly mixing for 4 hours at the temperature of 55 ℃ to obtain uniformly mixed materials, and circulating hot airflow in a sealed cavity for 16 kg/time.
(3) Sheet extrusion: sieving the uniformly mixed material obtained in the step (2), pouring the uniformly mixed material into a pre-pressing forming machine, pre-pressing the uniformly mixed material into a cylinder, placing the cylinder in an extruder, and extruding a reelable 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 molding into sheets: and (4) carrying out one-time or multiple-time rolling and molding on the reelable rubber sheet obtained in the step (3) to form a sheet by using a multi-roller open mill, so as to obtain an adhesive sheet with the width of 45-55cm and the thickness of 0.038-0.75mm, wherein the temperature of the multi-roller open mill is 60 ℃.
(5) And (3) low-temperature baking: and (5) baking the bonding sheet obtained in the step (4) by a degreasing drying oven to remove white oil and absolute ethyl alcohol to obtain a baked bonding sheet, wherein the baking temperature is 186 ℃/10 min/m.
(6) High-temperature vacuum forming: and (3) cutting the baked bonding sheet obtained in the step (5), laminating and coating copper on two sides according to the difference of the thicknesses of the manufactured copper clad plates, and performing hot press molding by using an oil-pressure vacuum high-temperature press under the vacuum condition of 93Kpa, at the material temperature of 386 ℃, at the pressure of 7MPa and for the pressure maintaining time of 1h to obtain the copper clad plate.
Example 7:
(1) preparing materials: and respectively sieving 48 parts of polytetrafluoroethylene dispersed resin powder and 69 parts of ceramic powder, and mixing according to the proportion to obtain a primary mixed material.
(2) Airflow hot mixing: pouring the initial mixture obtained in the step (1) into a gas flow mixer, adding 23 parts of isoparaffin and 8 parts of absolute ethyl alcohol into an oil injection bottle according to the proportion, circularly mixing for 4 hours at the temperature of 58 ℃ to obtain uniformly mixed materials, and circulating hot gas flow in a sealed cavity for 23 kg/time.
(3) Sheet extrusion: sieving the uniformly mixed material obtained in the step (2), pouring the uniformly mixed material into a pre-pressing forming machine, pre-pressing the uniformly mixed material into a cylinder, placing the cylinder in an extruder, and extruding a reelable 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 molding into sheets: and (4) carrying out one-time or multiple-time rolling and molding on the reelable rubber sheet obtained in the step (3) to form a sheet by using a multi-roller open mill, so as to obtain an adhesive sheet with the width of 45-55cm and the thickness of 0.038-0.75mm, wherein the temperature of the multi-roller open mill is 60 ℃.
(5) And (3) low-temperature baking: and (5) baking the bonding sheet obtained in the step (4) by a degreasing drying oven to remove isoparaffin and absolute ethyl alcohol to obtain a baked bonding sheet, wherein the baking temperature is 198 ℃/10 min/m.
(6) High-temperature vacuum forming: and (3) cutting the baked bonding sheet obtained in the step (5), laminating and coating copper on two sides according to the difference of the thicknesses of the manufactured copper clad plates, and performing hot press molding by using an oil-pressure vacuum high-temperature press under the vacuum condition of 93Kpa, at the material temperature of 396 ℃, under the pressure of 6MPa and for the pressure maintaining time of 1h to obtain the copper clad plate.
Example 8:
(1) preparing materials: and respectively sieving 30 parts of polytetrafluoroethylene dispersed resin powder and 50 parts of ceramic powder, and mixing according to the proportion to obtain a primary mixed material.
(2) Airflow hot mixing: pouring the initial mixture obtained in the step (1) into a gas flow mixer, adding 15 parts of isoparaffin and 9 parts of absolute ethyl alcohol into an oil injection bottle according to the proportion, circularly mixing for 4 hours at the temperature of 50 ℃ to obtain uniformly mixed materials, and circulating hot gas flow in a sealed cavity for 16 kg/time.
(3) Sheet extrusion: sieving the uniformly mixed material obtained in the step (2), pouring the uniformly mixed material into a pre-pressing forming machine, pre-pressing the uniformly mixed material into a cylinder, placing the cylinder in an extruder, and extruding a reelable rubber sheet 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 molding into sheets: and (4) carrying out one-time or multiple-time rolling and molding on the reelable rubber sheet obtained in the step (3) to form a sheet by using a multi-roller open mill, so as to obtain an adhesive sheet with the width of 45-55cm and the thickness of 0.038-0.75mm, wherein the temperature of the multi-roller open mill is 60 ℃.
(5) And (3) low-temperature baking: and (5) baking the bonding sheet obtained in the step (4) by a degreasing drying oven to remove isoparaffin and absolute ethyl alcohol to obtain a baked bonding sheet, wherein the baking temperature is 235 ℃/10 min/m.
(6) High-temperature vacuum forming: and (3) cutting the baked bonding sheet obtained in the step (5), laminating and coating copper on two sides according to the difference of the thicknesses of the manufactured copper clad plates, and performing hot press molding by using an oil-pressure vacuum high-temperature press under the vacuum condition of 93Kpa, at the material temperature of 398 ℃, at the pressure of 6MPa and for the pressure maintaining time of 1h to obtain the copper clad plate.
Example 9:
(1) preparing materials: and respectively sieving 65 parts of polytetrafluoroethylene dispersed resin powder and 50 parts of ceramic powder, and mixing according to the proportion to obtain a primary mixed material.
(2) Airflow hot mixing: pouring the initial mixture obtained in the step (1) into a gas flow mixer, adding 16 parts of isoparaffin and 6 parts of absolute ethyl alcohol into an oil injection bottle according to the proportion, circularly mixing for 4 hours at the temperature of 55 ℃ to obtain uniformly mixed materials, and circulating hot gas flow in a sealed cavity for 20 kg/time.
(3) Sheet extrusion: sieving the uniformly mixed material obtained in the step (2), pouring the uniformly mixed material into a pre-pressing forming machine, pre-pressing the uniformly mixed material into a cylinder, placing the cylinder in an extruder, and extruding a reelable 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 molding into sheets: and (4) carrying out one-time or multiple-time rolling and molding on the reelable rubber sheet obtained in the step (3) to form a sheet by using a multi-roller open mill, so as to obtain an adhesive sheet with the width of 45-55cm and the thickness of 0.038-0.75mm, wherein the temperature of the multi-roller open mill is 60 ℃.
(5) And (3) low-temperature baking: and (5) baking the bonding sheet obtained in the step (4) by a degreasing drying oven to remove isoparaffin and absolute ethyl alcohol to obtain a baked bonding sheet, wherein the baking temperature is 180 ℃/10 min/m.
(6) High-temperature vacuum forming: and (4) cutting the baked bonding sheet obtained in the step (5), laminating and coating copper on two sides according to the difference of the thicknesses of the manufactured copper clad plates, and performing hot press molding by using an oil-pressure vacuum high-temperature press under the vacuum condition of 93Kpa, at the material temperature of 400 ℃, under the pressure of 10MPa and for the pressure maintaining time of 1h to obtain the copper clad plate.
The samples obtained in the above examples were subjected to performance tests, and the test results are shown in table 1.
TABLE 1
Figure 501370DEST_PATH_IMAGE002
The test method comprises the following steps:
1. thickness, measured using a thickness gauge.
2. The peel strength was measured by the method defined in IPC-TM-650 as 2.4.8.
3. Copper-containing tin oxide was measured by the method defined in IPC-TM-650, 2.6.8.
4. The dielectric constant was measured at 1GHz and 10GHz by the SPDR (split post dielectric resonator) method.
5. The dielectric loss was measured by the SPDR (split post dielectric resonator) method at 10 GHz.
6. The coefficient of thermal expansion was measured by the method defined in IPC-TM-650, 2.4.41.
The plate is required to be DK3.0 in the mainstream of the current market, the lowest loss of the plate corresponding to the substrate with the thickness of DK3.0-0.254mm is 0.00035, so that the dielectric constant stability of the sample obtained in the embodiment 2 is tested, the test result is shown in figures 1 and 2, and the figure 1 proves the stability of the dielectric constant of the plate under different frequencies, so that the inherent stability of the plate in the frequencies is illustrated, and convenience is provided for circuit design; fig. 2 demonstrates the stability of the dielectric constant of the material at different temperatures, illustrating that the material maintains stable dielectric constant characteristics over a wide temperature range. The curves of fig. 1 and 2 were both tested by the stripline method.
According to the results, the copper-clad plate manufactured by the invention 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 above description is only a preferred embodiment of the present invention, and is not intended to limit the technical scope of the present invention, so that any minor modifications, equivalent changes and modifications made to the above embodiment according to the technical spirit of the present invention are within the technical scope 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 dispersed resin powder, 15-25 parts of solvent oil and 5-10 parts of absolute ethyl alcohol; the method comprises the following steps:
(1) preparing materials: respectively sieving polytetrafluoroethylene dispersed resin powder and ceramic powder, and mixing according to the proportion to obtain a primary mixed material;
(2) airflow hot mixing: 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, circularly mixing for 4 hours at the temperature of 45-65 ℃ to obtain uniformly mixed material, and circulating hot airflow in a sealed cavity for 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 pre-pressing forming machine, pre-pressing the uniformly mixed material into a cylinder, placing the cylinder in an extruder, and extruding a reelable rubber sheet 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 molding into sheets: rolling the reelable rubber sheet obtained in the step (3) into a mold sheet for one time or more times by using 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) and (3) low-temperature baking: baking the bonding sheet obtained in the step (4) in a degreasing drying oven to remove solvent oil and absolute ethyl alcohol to obtain a baked bonding sheet, wherein the baking temperature is 160-;
(6) high-temperature vacuum forming: and (3) cutting the baked bonding sheet obtained in the step (5), laminating and coating copper on two sides according to the difference of the thicknesses of the manufactured copper clad plates, and performing hot press molding by using an oil-pressure vacuum high-temperature press under the vacuum condition of 90-100Kpa, wherein the baking bonding sheet is prepared under the conditions that the material temperature is 380-405 ℃, the pressure is 5-15MPa and the pressure maintaining time is 1 h.
2. The preparation method of the high-frequency ultra-low dielectric loss microwave ceramic copper-clad plate according to claim 1, which is characterized by comprising the following steps: the structure of the ceramic powder is spherical, spherical aggregate or hollow spherical, 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 preparation method of the high-frequency ultra-low 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 preparation method of the high-frequency ultra-low 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 a mixture of more of odorless kerosene, white oil and isoparaffin.
5. The preparation method of the high-frequency ultra-low dielectric loss microwave ceramic copper-clad plate according to claim 1, which is characterized by comprising the following steps: the material temperature in the step (6) is 400 ℃.
6. The preparation method of the high-frequency ultra-low dielectric loss microwave ceramic copper-clad plate according to claim 1, which is characterized by comprising the following steps: the width of the extrusion opening of the sheet extrusion die in the step (3) is 20 cm.
7. The preparation method of the high-frequency ultra-low 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: 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 according to any one of claims 1 to 7.
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CN114889273A (en) * 2022-03-23 2022-08-12 电子科技大学 Glass fiber-free ceramic/hydrocarbon resin-based microwave medium substrate and preparation method thereof

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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
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