CN111154206A - Modified PTFE composite medium material, preparation method and application thereof - Google Patents
Modified PTFE composite medium material, preparation method and application thereof Download PDFInfo
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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Abstract
The invention relates to a ceramic modified low-dielectric-constant low-thermal-expansion PTFE composite medium material, which comprises PTFE and non-solid ceramic particles, wherein the consumption of the non-solid ceramic particles is 1-60% of the whole volume fraction of the composite material, the dielectric constant of the modified PTFE composite medium material is 2.0-2.5, the thermal expansion coefficient is 40-120 ppm/DEG C, and the ceramic modified low-dielectric-constant low-thermal-expansion PTFE composite medium material has a lower dielectric constant and a lower thermal expansion coefficient.
Description
Technical Field
The invention relates to a modified PTFE composite material, in particular to a ceramic modified low-dielectric-constant low-thermal-expansion PTFE composite dielectric material and a preparation method thereof, which are applied to the manufacture of circuit boards, especially 5G high-frequency circuit boards.
Background
With the increasing maturity and continuous popularization of 5G mobile communication technology, mobile terminals such as smart phones, smart watches, tablet computers and the like as electronic products supporting 5G enter a new high-speed development period, and Printed Circuit Boards (PCBs) used by the mobile terminals also enter a new development opportunity period. This requires a circuit board having high density, high frequency, high speed, high heat generation, and the like.
The dielectric constant determines the speed of the electric signal propagating in the medium, and the lower the dielectric constant, the faster the signal transmission speed, so the high frequency PCB needs to select a dielectric material with a low dielectric constant, and meanwhile, in order to meet the requirement of high heat dissipation caused by high heat generation, a material with good thermal conductivity is usually added into the dielectric material. Commonly used low dielectric constant dielectric materials include Polytetrafluoroethylene (PTFE), polyimide (MPI), or Liquid Crystal Polymer (LCP). These materials have high and low dielectric constants (Dk < 4), low dissipation factors (Df < 0.005), good dimensional stability and processability. Commonly used heat conductive materials include ceramic powders such as alumina and silica, but the addition of too much heat conductive material increases the dielectric constant.
Polytetrafluoroethylene, which is currently the best choice as a hard low dielectric constant dielectric material, is not hygroscopic, nonflammable, and very stable to oxygen and ultraviolet light compared to epoxy resins, and therefore has excellent weatherability. The dielectric constant and dielectric loss are low in a wide frequency range, and the breakdown voltage, volume resistivity and arc resistance are high.
Although the performance of the polytetrafluoroethylene material is stable, the disadvantages are also obvious. Because the polytetrafluoroethylene has low thermal conductivity, poor thermal conductivity and overlarge linear thermal expansion coefficient which is 10-20 times of that of copper foil, the application of PTFE in the copper-clad plate is limited to a certain extent.
CN103435946A discloses a preparation method of a polytetrafluoroethylene composite microwave ceramic substrate, wherein Zr-Ti based ceramic powder is added into polytetrafluoroethylene, the powder has low thermal expansion coefficient, the formed substrate has good absolute value of dielectric constant temperature coefficient, however, the dielectric constant is high, and the dielectric constant of the final substrate is 6.40-7.80.
CN102260378B uses a porous ePTFE film as a carrier material, and provides a prepreg and a high-frequency circuit board with isotropic dielectric constant in the X, Y direction, which can reduce the dielectric constant and dielectric loss tangent of the high-frequency circuit board. But no improvement in the coefficient of thermal expansion is made.
CN1165575C provides a fluorine-containing polymer substrate and at least one ceramic particle filler dispersed in the polymer substrate, wherein the ceramic particle filler is added for the purpose of reinforcing the composite material plate, and controlling the thermal expansion coefficient of the composite material plate. However, the control of the thermal expansion coefficient is not shown, and the dielectric constant is increased by the addition of the ceramic particles.
Therefore, how to obtain the PTFE medium material with low dielectric constant and low thermal expansion coefficient simultaneously is a problem to be solved in the field.
Disclosure of Invention
Aiming at the contradiction that the dielectric constant is increased due to the fact that the PTFE has high thermal expansion coefficient and ceramic filling is introduced, and a PTFE composite medium plate containing ceramic filler and having low dielectric constant and low thermal expansion coefficient cannot be obtained at the same time, the invention provides a modified PTFE composite medium material, which is formed by filling non-solid ceramic particles with modified PTFE to form a composite medium material and can solve the problem.
It was found that when non-solid ceramic particles containing a large amount of air are used, the introduction of air can effectively lower the dielectric constant of the composite material because air has a very low dielectric constant (e ═ 1). Therefore, the filling modification using non-solid ceramic particles containing a large amount of air can achieve a low dielectric constant while reducing the coefficient of thermal expansion of the PTFE composite system.
The non-solid ceramic particles are further non-solid SiO2The particles preferably have a silicon oxygen content of 99 wt% or more, and more preferably have a silicon oxygen content of 99.5 wt% or more. If so, since there is no metal element impurity, the low dielectric property thereof can be effectively improved.
The non-solid ceramic particles comprising: hollow SiO2Ceramic particle and mesoporous SiO2Ceramic particles, and combinations thereof. The particle diameter of the hollow ceramic particles is 1-10 μm, preferably 2-5 μm, the sphere is a hollow structure, and the hole wallIs 0.1 to 2 μm, preferably 0.5 to 1 μm. The particle size of the mesoporous ceramic particles is 1-10 μm, preferably 2-5 μm, the mesoporous ceramic particles have a plurality of pore channels with ordered structures and single pore diameters, and the pore diameter range is 2-50nm, preferably 10-30 nm.
The hollow ceramic particles may be prepared by any method known at present, for example, ion exchange resin template method, inorganic particle template method, emulsion droplet template method, vesicle template method, etc., preferably according to the contents described in Cheng X, Liu SQ, et al.
The mesoporous ceramic particles can be prepared by any currently known method, such as a CTAB template method, an emulsion method, an induced polymerization agglomeration method (PICA), and the like. Preferably, a hydrothermal method is adopted, a homogeneous reactor is utilized, polyethylene glycol is used as a template agent, sodium silicate is used as a silicon source, and the mesoporous SiO with high purity and regular sphericity is prepared2And (3) microspheres.
In view of the balance between low dielectric property and low thermal expansion coefficient, the hollow ceramic particles are used in an amount of 1 to 60% by volume of the entire volume fraction of the composite material, preferably 10 to 50% by volume of the entire volume fraction of the composite material, and more preferably 20 to 40% by volume of the entire volume fraction of the composite material; the mesoporous ceramic particles are used in an amount of 1 to 40% of the entire volume fraction of the composite material, preferably 10 to 30% of the entire volume fraction of the composite material, and more preferably 15 to 25% of the entire volume fraction of the composite material. For the combination of the two particles, the volume fraction adjustment foreseen in the art is made within the above range according to the specific mixture ratio.
The specific steps of filling and modifying PTFE by non-solid ceramic comprise:
(1) preparing an emulsion: mixing the non-solid ceramic particles and the PTFE emulsion, and carrying out double-center stirring, wherein the ceramic particles account for 1-60% of the total volume, the double-center stirring speed is 1500-3500r/min, and the stirring time is 20-150 s, so as to obtain the emulsion for the PTFE composite dielectric plate containing the ceramic filler;
(2) preparing a mud pie: adding anhydrous ethanol with the emulsion mass of 30-70 wt% into the mixed emulsion to carry out double-center stirring demulsification, controlling the double-center stirring rotation speed to be 500-1500r/min, and controlling the double-center stirring time to be 20-120s to obtain a mud mass for the composite dielectric slab containing the ceramic filler;
(3) and (3) calendering and forming: pressing the composite dielectric slab containing the ceramic filler obtained by demulsification into a sheet shape by a rolling machine, wherein the rotating speed of an upper roll shaft and a lower roll shaft is controlled to be 0.5-2m/min in the rolling process, and the smooth, flat and compact composite dielectric slab pre-pressing sheet containing the ceramic filler is obtained by rolling, and the thickness of the pre-pressing sheet is controlled to be 1.2-1.8 mm;
(4) and (3) solvent removal: placing the rolled composite dielectric plate prepressed sheet containing the ceramic filler in a drying oven, and drying for 8-12 hours at 80-90 ℃ to remove alcohol in the prepressed sheet; then, controlling the temperature of the oven to be 150-200 ℃, and drying for 8-12 h to remove the water in the pre-tabletting; finally, controlling the temperature of the oven to be 260-265 ℃, and drying for 60-80 h to remove organic matter micromolecules in the preforming sheet;
(5) and (3) final forming: and pressing and flattening the dried pre-pressed sheet by using a rolling machine, eliminating bending caused in the high-temperature sheet drying process, and controlling the thickness of the sheet to be 0.8-1.2mm to obtain the finally-formed non-solid ceramic modified PTFE composite dielectric material.
Further, the invention discloses a method for preparing a copper-clad plate by using the obtained non-solid ceramic modified PTFE composite medium material, which comprises the following steps:
(6) copper-clad hot pressing: and (3) placing the composite dielectric material obtained in the step (5) in a hot press, setting pressure according to the area of the prepressed sheet, pasting copper foil on two sides, controlling the maximum pressure to be 15-17 MPa, and controlling the maximum hot pressing temperature to be 330-385 ℃.
Furthermore, the invention also discloses a performance test method for the composite dielectric material after the copper foil is removed, which comprises the following steps:
(7) copper foil corrosion and test: and corroding copper foils on the upper surface and the lower surface of the medium sheet obtained by hot pressing in a ferric trichloride solution, and washing the surface by pure water to ensure that the surface is clean and has no copper foil and ferric chloride solution residues. And (3) placing the sample in an oven at the temperature of 100-120 ℃ for drying for more than 3h to remove moisture, obtaining the non-solid ceramic filled modified PTFE dielectric plate after copper removal, and carrying out dielectric constant and thermal expansion coefficient tests, wherein the dielectric constant test is carried out by adopting a network analyzer ET8722, and the thermal expansion coefficient test is carried out by adopting a thermomechanical analyzer TMA 202.
In the present invention, the non-solid ceramic particle-filled modified PTFE media prepared according to the method of the present invention has a dielectric constant of 2.0 to 2.4, preferably 2.1 to 2.35, and more preferably 2.1 to 2.3, for the hollow ceramic particle-filled modified PTFE media; a coefficient of thermal expansion of between 70 and 120 ppm/DEG C, preferably between 75 and 110-ppm/DEG C, and more preferably between 80 and 90 ppm/DEG C; for the mesoporous ceramic particle filled modified PTFE medium material, the dielectric constant is between 2.0 and 2.5, preferably between 2.1 and 2.4, and more preferably between 2.15 and 2.3; the coefficient of thermal expansion is between 40 and 120 ppm/DEG C, preferably between 30 and 85 ppm/DEG C, and more preferably between 60 and 80 ppm/DEG C.
According to the method for filling and modifying PTFE by non-solid ceramic, the PTFE latex particles are wrapped by the PTFE latex particles in the process of high-speed mixing and stirring in a double-center stirring demulsification mode, so that the interface performance is improved.
The invention has the beneficial effects that: according to the invention, the non-solid ceramic is filled with the modified PTFE, on the premise of utilizing the advantage of low dielectric constant of the PTFE, the non-solid ceramic has low dielectric constant and low thermal expansion coefficient, the condition of poor thermal expansion coefficient of the PTFE can be effectively improved after the non-solid ceramic is added, the uniformity of the composite material is improved by a double-center stirring demulsification mode, the consumption of the modifier is reduced, the interface binding property is ensured, and the performance of low dielectric constant and thermal expansion coefficient is not influenced. Therefore, the modified PTFE composite dielectric material can be widely applied to 5G high-frequency circuit boards and meets corresponding requirements.
Drawings
FIG. 1 is a diagram showing hollow SiO with a volume fraction of 10% -60%2And is solidSiO2Graph of dielectric constant filler content variation relationship of filled PTFE composite material
FIG. 2 is a diagram showing hollow SiO with a volume fraction of 10% -60%2Graph of thermal expansion coefficient of filled PTFE composite material changing with filler content
FIG. 3 is a diagram of mesoporous SiO with a volume fraction of 10% -40%2And solid SiO2Graph of dielectric constant filler content variation relationship of filled PTFE composite material
FIG. 4 shows mesoporous SiO with a volume fraction of 10% -40%2And solid SiO2Graph of thermal expansion coefficient of filled PTFE composite material changing with filler content
FIG. 5 is a 30 vol% hollow SiO2SEM (scanning Electron microscope) image of PTFE (Polytetrafluoroethylene) filled and modified at 5000 multiplying power
FIG. 6 is a 30 vol% hollow SiO210000 magnification SEM electron micrograph for filling and modifying PTFE
FIG. 7 shows 30 vol% mesoporous SiO2SEM (scanning Electron microscope) image of PTFE (Polytetrafluoroethylene) filled and modified at 5000 multiplying power
FIG. 8 shows 30 vol% mesoporous SiO210000 magnification SEM electron micrograph for filling and modifying PTFE
Detailed Description
The technical solution of the present invention will be further described in detail with reference to specific embodiments. The following examples are merely illustrative and explanatory of the present invention and should not be construed as limiting the scope of the invention. All the technologies realized based on the above-mentioned contents of the present invention are covered in the protection scope of the present invention.
Unless otherwise indicated, the raw materials and reagents used in the following examples are all commercially available products or can be prepared by known methods.
Example 1
(1) Preparing an emulsion: mixing hollow SiO2Mixing the balls and the PTFE emulsion, and carrying out double-center stirring, wherein the ceramic particles account for 10% of the total volume, the double-center stirring speed is 2000r/min, and the stirring time is 60s, so as to obtain the emulsion for the PTFE composite dielectric plate containing the ceramic filler;
(2) preparing a mud pie: adding absolute ethyl alcohol with the emulsion mass of 50 wt% into the mixed emulsion to carry out double-center stirring demulsification, controlling the double-center stirring rotation speed to be 800r/min, and controlling the double-center stirring time to be 50s to obtain a mud mass for the composite dielectric slab containing the ceramic filler;
(3) and (3) calendering and forming: pressing the composite dielectric plate containing the ceramic filler obtained by demulsification into a sheet shape by a rolling machine, controlling the rotating speed of an upper roll shaft and a lower roll shaft to be 1m/min in the rolling process, obtaining a smooth, flat and compact composite dielectric plate pre-pressing sheet containing the ceramic filler by rolling, and controlling the thickness of the pre-pressing sheet to be 1.5 mm;
(4) and (3) solvent removal: placing the rolled composite dielectric plate pre-pressing sheet containing the ceramic filler in a drying oven, and removing ethanol, water and organic matter micromolecules in the pre-pressing sheet by adopting drying processes of 12 hours at 80 ℃, 12 hours at 180 ℃ and 72 hours at 260 ℃ respectively;
(5) and (3) final forming: pressing and flattening the dried pre-pressed sheet by using a rolling machine, eliminating bending caused in the high-temperature sheet drying process, and controlling the thickness of the sheet to be 1.2mm to obtain the finally-formed hollow ceramic modified PTFE composite dielectric material;
(6) copper-clad hot pressing: covering copper foils on the upper surface and the lower surface of the composite dielectric material obtained in the step (5), placing the composite dielectric material in a hot press for double-sided lamination, and controlling the maximum pressure to be 17MPa and the maximum hot-pressing temperature to be 385 ℃;
(7) copper foil corrosion and test: and corroding copper foils on the upper surface and the lower surface of the medium sheet obtained by hot pressing in a ferric trichloride solution, and washing the surface by pure water to ensure that the surface is clean and has no copper foil and ferric chloride solution residues. And (3) placing the sample in a 120 ℃ oven to be dried for more than 3h to remove moisture, obtaining the hollow ceramic filling modified PTFE medium plate after copper removal, and carrying out dielectric constant and thermal expansion coefficient test.
Example 2:
mixing hollow SiO2The ball content was increased to 20% and the other raw materials, process steps and process parameters were the same as in example 1.
Example 3:
mixing hollow SiO2The ball content is increased to 30%, and other raw materials, method steps and process parameters are the same as those of the example 1.
Example 4:
mixing hollow SiO2The ball content is increased to 40%, and other raw materials, method steps and process parameters are the same as those of the example 1.
Example 5:
mixing hollow SiO2The ball content was increased to 50% and the other raw materials, process steps and process parameters were the same as in example 1.
Example 6:
mixing hollow SiO2The ball content was increased to 60% and the other raw materials, process steps and process parameters were the same as in example 1.
Example 7:
by mesoporous SiO2Ball substituted hollow SiO2The ball, other raw materials and method steps, and process parameters were the same as in example 1.
Example 8:
by mesoporous SiO2Ball substituted hollow SiO2The ball, other raw materials and method steps, process parameters were the same as in example 2.
Example 9:
by mesoporous SiO2Ball substituted hollow SiO2The ball, other raw materials and method steps, process parameters were the same as in example 3.
Example 10:
by mesoporous SiO2Ball substituted hollow SiO2The ball, other raw materials and method steps, process parameters were the same as in example 4.
Comparative example 1:
mixing hollow SiO2Replacement of balls with solid SiO2The content of the balls is 10 percent, and other raw materials, method steps and process parameters are the same as those of the example 1.
Comparative example 2:
mixing hollow SiO2Replacement of balls with solid SiO2The content of the balls is 20 percent, and other raw materials, method steps and process parameters are the same as those of the example 1.
Comparative example 3:
mixing hollow SiO2Replacement of balls with SiO 230% of balls and other raw materialsThe method steps and the process parameters are the same as those of the example 1.
Comparative example 4:
mixing hollow SiO2Replacement of balls with solid SiO2The content of the balls is 40 percent, and other raw materials, method steps and process parameters are the same as those of the example 1.
Comparative example 5:
mixing hollow SiO2Replacement of balls with solid SiO2The content of the balls is 50 percent, and other raw materials, method steps and process parameters are the same as those of the example 1.
Comparative example 6:
mixing hollow SiO2Replacement of balls with solid SiO2The content of the balls is 60 percent, and other raw materials, method steps and process parameters are the same as those of the example 1.
The test method comprises the following steps:
dielectric constant tests were performed on the PTFE composite media sheet samples of examples 1-10 and comparative examples 1-6, respectively, using a network analyzer ET 8722.
The PTFE composite media sheet samples of examples 1-10 and comparative examples 1-6 were subjected to coefficient of thermal expansion testing using thermomechanical analyzer TMA 202.
As can be seen from fig. 1 and 3, the hollow and mesoporous ceramic filler modification can achieve lower dielectric constant in the range compared to the solid ceramic filler, wherein the dielectric constant performance of the hollow ceramic is better.
It can be seen from FIGS. 2 and 4 that the hollow ceramic filling modification within the range can make the thermal expansion coefficient of the PTFE composite material in the range of 70-120 ppm/DEG C, and the solid SiO2The thermal expansion coefficient of the PTFE composite material is equivalent, the thermal expansion coefficient of the PTFE composite material can be controlled to be 40-120 ppm/DEG C by the mesoporous ceramic filling modification, and the effect of the mesoporous ceramic filling modification on the improvement of the thermal expansion coefficient is better.
From the SEM images of FIGS. 5-8, it can be seen that the hollow and mesoporous ceramics are fully embedded in PTFE, uniformly dispersed, and have small interfacial pores.
In summary, the hollow and mesoporous ceramic-filled modified PTFE prepared in examples 1-10 are superior to the solid ceramic-filled modified PTFE prepared in comparative examples 1-6 in both dielectric constant and thermal expansion coefficient.
The embodiments of the present invention have been described above. However, the present invention is not limited to the above embodiment. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. The modified PTFE composite medium material is characterized by comprising PTFE and hollow ceramic particles, wherein the amount of the hollow ceramic particles is 1-60% of the whole volume fraction of the composite material, the dielectric constant of the modified PTFE composite medium material is 2.0-2.4, and the thermal expansion coefficient is 70-120 ppm/DEG C.
2. The modified PTFE composite media of claim 1, wherein the hollow ceramic particles are hollow SiO2Fillers, preferably hollow SiO having a silica content of 99 wt.% or more2The filler is more preferably hollow SiO having a silica content of 99.5 wt% or more2And (4) filling.
3. The modified PTFE composite media of claim 1, wherein said hollow ceramic particles have a particle size of 1 to 10 μm, preferably 2 to 5 μm;
the sphere of the hollow ceramic particle is of a hollow structure, and the hole wall is 0.1-2 μm, preferably 0.5-1 μm.
4. The modified PTFE composite media of claim 1, wherein the hollow ceramic particles are from 10 to 50% of the bulk volume fraction of the composite, preferably from 20 to 40% of the bulk volume fraction of the composite.
5. The modified PTFE composite medium material is characterized by comprising PTFE and mesoporous ceramic particles, wherein the consumption of the mesoporous ceramic particles is 1-40% of the whole volume fraction of the composite material, the dielectric constant of the modified PTFE composite medium material is 2.0-2.5, and the thermal expansion coefficient is 40-120 ppm/DEG C.
6. The modified PTFE composite media of claim 5, wherein the mesoporous ceramic particles have a particle size of 1-10 μm, preferably 2-5 μm;
the mesoporous ceramic particles have a plurality of pore passages with ordered structures and single pore diameters, and the pore diameter range is 2-50nm, preferably 10-30 nm.
7. The modified PTFE composite media of claim 5, wherein the mesoporous ceramic particles comprise 10-30% of the overall volume fraction of the composite, preferably 15-25% of the overall volume fraction of the composite.
8. The method for preparing the modified PTFE composite media material of any one of claims 1 to 7, wherein the modified PTFE composite media material is prepared according to the following specific steps:
(1) preparing an emulsion: mixing the hollow ceramic particles and/or the mesoporous ceramic particles with the PTFE emulsion, and carrying out double-center stirring, wherein the ceramic particles account for 1-60% of the total volume, the double-center stirring speed is 1500-3500r/min, and the stirring time is 20-150 s, so as to obtain the emulsion for the PTFE composite dielectric plate containing the ceramic filler;
(2) preparing a mud pie: adding anhydrous ethanol with the emulsion mass of 30-70 wt% into the mixed emulsion to carry out double-center stirring demulsification, controlling the double-center stirring rotation speed to be 500-1500r/min, and controlling the double-center stirring time to be 20-120s to obtain a mud mass for the composite dielectric slab containing the ceramic filler;
(3) and carrying out subsequent solvent removal and final forming steps on the composite dielectric plate containing the ceramic filler by using a mud mass to obtain the hollow ceramic filled modified PTFE dielectric plate.
9. A copper-clad plate, characterized by comprising the modified PTFE composite media material of any one of claims 1 to 7.
10. A5G high frequency circuit board comprising the modified PTFE composite dielectric material according to any one of claims 1 to 7.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112551945A (en) * | 2020-12-09 | 2021-03-26 | 武汉理工大学 | Modified PTFE composite dielectric material with high thermal conductivity and low dielectric constant and preparation method thereof |
| CN113232383A (en) * | 2021-05-25 | 2021-08-10 | 武汉理工大学 | PTFE composite medium substrate and preparation method thereof |
| WO2022007069A1 (en) * | 2020-07-09 | 2022-01-13 | 瑞声声学科技(深圳)有限公司 | Method for preparing composite dielectric copper-clad laminate, and printed circuit board |
| CN114181482A (en) * | 2021-11-29 | 2022-03-15 | 山东东岳高分子材料有限公司 | Filled polytetrafluoroethylene dispersion resin and preparation method thereof |
| WO2023016242A1 (en) * | 2021-08-12 | 2023-02-16 | 广东生益科技股份有限公司 | Fluorine-containing resin-based resin composition and application thereof |
| CN117165215A (en) * | 2023-10-25 | 2023-12-05 | 山东东岳高分子材料有限公司 | Fluororesin bonding sheet core layer for copper-clad plate, bonding sheet and preparation method of bonding sheet |
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