CN112172210B - Preparation method of liquid crystal polymer film with low dielectric constant and low dielectric loss - Google Patents
Preparation method of liquid crystal polymer film with low dielectric constant and low dielectric loss Download PDFInfo
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Abstract
The invention discloses a preparation method of a liquid crystal polymer film with low dielectric constant and low dielectric loss, which comprises the following steps: s1, dissolving a liquid crystal polymer in a solvent to obtain a liquid crystal polymer solution; s2, adding fluororesin powder into the liquid crystal polymer solution, and dispersing the mixed material; s3, coating the mixed material obtained in the step S2 on the surface of a release base material, and forming a film on a coating layer through drying and melting treatment; and S4, separating the film layer from the release substrate to obtain the liquid crystal polymer film. The preparation method of the liquid crystal polymer film material with low dielectric constant and low dielectric loss sequentially comprises four steps of dissolving the liquid crystal polymer, dispersing fluororesin powder, coating and drying mixed materials and forming a film to be separated from a release substrate, and a liquid mixing mode is adopted, so that more fluororesin can be added into the liquid crystal polymer film material conveniently; fluororesin powder in the liquid crystal polymer film is dispersed more uniformly; the invention also discloses a liquid crystal polymer film and a mobile phone antenna based on the liquid crystal polymer film.
Description
Technical Field
The invention relates to the technical field of liquid crystal polymer film material manufacturing, in particular to a preparation method of a liquid crystal polymer film material with low dielectric constant and low dielectric loss, the liquid crystal polymer film material and a mobile phone antenna.
Background
Liquid Crystal Polymer (LCP) materials have high strength, high modulus, outstanding heat resistance, very low linear expansion coefficient, excellent flame resistance, electrical insulation, chemical resistance, weathering resistance, and microwave transparency, and excellent molding processability, etc., and are desirable high frequency (millimeter wave) materials. With the development of the 5G industry, the transmission loss requirement of materials under the high-frequency condition in the industry is lower, and the dielectric loss of the existing LCP film is relatively large and cannot meet the use requirement under the higher frequency, so that the LCP film with lower dielectric loss needs to be developed.
CN111497173A discloses a preparation method of a liquid crystal polymer film, which comprises the steps of firstly extruding polytetrafluoroethylene and a liquid crystal polymer mixed material to prepare granules, then simultaneously extruding the mixed granules and a pure liquid crystal polymer to obtain a three-layer co-extruded melt, and carrying out setting and transverse stretching treatment to obtain a three-layer composite liquid crystal polymer film, wherein the core layer material of the liquid crystal polymer film is 100% of the liquid crystal polymer, and the surface layer material is a polytetrafluoroethylene and liquid crystal polymer blended material.
In the process, the polytetrafluoroethylene and the liquid crystal polymer are mixed and firstly prepared into granules, and then the granules are extruded to obtain a blending surface layer, and the production process has the following defects: firstly, the production process based on pellet blending has low content of polytetrafluoroethylene, and the mass percentage of the polytetrafluoroethylene pellets is 5-25% based on the sum of the mass of the liquid crystal polymer and the mass of the polytetrafluoroethylene being 100%; secondly, the dispersion uniformity of polytetrafluoroethylene in the liquid crystal polymer film obtained by co-extrusion is poor; thirdly, the stretching treatment may adversely affect the consistency of the dielectric constant of the liquid crystal polymer film; fourth, the maximum width of the liquid crystal polymer film is constant, limited by the extrusion equipment.
Disclosure of Invention
The present invention is directed to overcoming the drawbacks of the prior art and providing a method for preparing a liquid crystal polymer film with low dielectric constant and low dielectric loss.
The technical scheme of the invention is as follows: a preparation method of a liquid crystal polymer film with low dielectric constant and low dielectric loss comprises the following steps:
s1, dissolving a liquid crystal polymer in a solvent to obtain a liquid crystal polymer solution;
s2, adding fluororesin powder into the liquid crystal polymer solution, and dispersing the mixed material;
s3, coating the mixed material obtained in the step S2 on the surface of a release base material, and forming a film on a coating layer through drying and melting treatment;
and S4, separating the film layer from the release substrate to obtain the liquid crystal polymer film.
The mixed material is coated on the surface of the release substrate by known liquid continuous coating methods such as blade coating, slit coating and the like; the manner of separating the film layer from the release substrate includes peeling, or removing the release substrate by etching with a suitable etching manner, and etching the metal release substrate, such as chemical etching.
The fluororesin powder is at least one selected from Polytetrafluoroethylene (PTFE) powder, copolymer (PFA) powder of a small amount of perfluoropropyl perfluorovinyl ether and polytetrafluoroethylene, and perfluorinated ethylene propylene (FEP) powder, namely the fluororesin powder is one of the three powders, or is a mixture of any two of the three powders or a mixture of the three powders.
Further, the fineness of the slurry of the mixed material subjected to the S2 dispersion treatment is not more than 15 mu m. The fineness of the slurry is more than 15 mu m, and the fluororesin is easy to agglomerate, which also causes the reduction of dielectric property and the inconsistency of dielectric constant distribution.
The preferable technical proposal is that the mass ratio of the fluororesin powder is 10 to 40 percent, preferably 20 to 40 percent, and more preferably 30 to 40 percent, based on 100 percent of the sum of the mass of the fluororesin powder and the liquid crystal polymer;
preferably, the fluororesin powder has an average particle diameter of 2 to 10 μm.
The mass ratio of the polytetrafluoroethylene powder is, for example, 10%, 12%, 15%, 17%, 20%, 23%, 25%, 28%, 30%, 31%, 32%, 33%, 34%, 35%, 36%, 37%, 38%, 39%, 40% or an interval value in which any two of them are end points, based on 100% of the sum of the mass of the fluororesin powder and the liquid crystal polymer. The mass ratio of the fluororesin powder is more than 40%, the dispersion difficulty of the fluororesin powder in the liquid crystal polymer solution is improved, and the flexural modulus of the prepared liquid crystal polymer film is greatly reduced.
The preferable technical scheme is that the fluororesin powder is polytetrafluoroethylene powder, and the molecular weight of the polytetrafluoroethylene powder is 5 to 50 ten thousand, preferably 5 to 20 ten thousand; for example, the molecular weight of the polytetrafluoroethylene powder is one point value or any two point values of 5 ten thousand, 10 ten thousand, 15 ten thousand, 20 ten thousand, 25 ten thousand, 30 ten thousand, 35 ten thousand, 40 ten thousand, 45 ten thousand and 50 ten thousand as an endpoint interval value.
The preferable technical scheme is that the solvent is an organic solvent, preferably at least one of methyl pyrrolidone and N, N-dimethylacetamide, and further preferably methyl pyrrolidone; the N-methyl pyrrolidone has stronger polarity, lower viscosity and strong dissolving capacity, and the low viscosity is beneficial to the dissolution of the liquid crystal polymer and the dispersion of the fluorine resin powder; and relatively little toxic.
Preferably, the mass percentage of the liquid crystal polymer in the liquid crystal polymer solution is 5 to 20%, preferably 5 to 10%. The mass percentage of the liquid crystal polymer in the liquid crystal polymer solution is 5%, 6.5%, 8%, 10.5%, 12%, 14.5%, 15%, 16.5%, 18%, 20% or an interval value taking any two values as endpoints. If the mass percentage of the solute in the liquid crystal polymer solution is too large, the viscosity of the solution is continuously increased, which is not beneficial to the dispersion of the fluororesin powder; if the mass percentage is too small, the viscosity of the solution is too small, and the technical defect of uneven thickness can occur when the solution is coated on the surface of the release base material at the later stage.
The preferable technical scheme is that the drying temperature is 100 to 200 ℃, and preferably 180 to 200 ℃;
typically, the drying time is 20 to 30 min. The temperature and time of drying depend on the boiling point of the solvent and the evaporation rate of the solvent at the drying temperature.
The preferable technical scheme is that the temperature of the melting treatment is 200 to 330 ℃, preferably 250 to 330 ℃, and further preferably 280 ℃;
the time for the melting treatment is preferably 5 to 15min, more preferably 8 to 13min, and still more preferably 9 to 11min. The temperature of the melting treatment is lower than 200 ℃, so that the solvent is slowly volatilized; n-methyl pyrrolidone can be accelerated at 280 ℃, and the liquid crystal state can be quickly achieved when the critical concentration is reached; when the temperature is too high, the melting point of the fluororesin is reached, the crystal morphology is changed, internal stress is generated, and the Coefficient of Thermal Expansion (CTE) is increased.
The preferable technical scheme is that the release substrate is resistant to the drying and melting treatment temperature, preferably made of metal, specifically a strip or foil, and further preferably made of aluminum foil or copper foil.
The preferable technical scheme is that the thickness of the LCP film is 30-100 mu m, the dielectric constant of the LCP film is 2.9-3.2, the dielectric loss is 0.002-0.005, and the flexural modulus is 2.8-3.6 Gpa.
The second purpose of the invention is to provide a liquid crystal polymer film material, which is prepared by the method.
The invention also aims to provide a mobile phone antenna, which is prepared from the liquid crystal polymer film material with low dielectric constant and low dielectric loss.
The invention has the advantages and beneficial effects that:
the preparation method of the liquid crystal polymer film material with low dielectric constant and low dielectric loss sequentially comprises four steps of dissolving the liquid crystal polymer, dispersing fluororesin powder, coating and drying mixed materials and forming a film to be separated from a release substrate, and a liquid mixing mode is adopted, so that more fluororesin can be added into the liquid crystal polymer film material conveniently;
fluororesin powder in the liquid crystal polymer film is dispersed more uniformly;
the coating method has simple and reasonable steps and convenient operation;
the width of the liquid crystal polymer film material prepared by the coating method has no upper limit, and can be set according to production requirements;
the dispersion uniformity of the fluororesin powder is improved, the consistency of the dielectric constant of the mobile phone antenna is correspondingly improved, and the stable high information transmission speed is ensured; meanwhile, the dielectric loss is lower and uniform, and the mobile phone signal can be kept stronger.
Detailed Description
The following further describes embodiments of the present invention with reference to examples. The following examples are only for illustrating the technical solutions of the present invention more clearly, and the protection scope of the present invention is not limited thereby.
PTFE resin powder, average particle size 5 μm, source: large gold with an average molecular weight of 10 to 20 ten thousand;
LCP: sumitomo chemistry;
methyl pyrrolidone: analytically pure, commercially available;
releasing the substrate: copper foil.
Example 1
S1: dissolving a Liquid Crystal Polymer (LCP) in an organic solvent by high-speed stirring to prepare a 5% liquid crystal polymer solution;
s2: adding 10% of polytetrafluoroethylene powder into the mixed solution prepared in the step S1 by taking the sum of the mass of the liquid crystal polymer and the mass of the polytetrafluoroethylene powder as 100%, and grinding and dispersing at a high speed for 2 hours to obtain uniform mixed slurry with the mixed slurry fineness of less than 15 mu m;
s3: uniformly coating the mixed slurry prepared in the step S2 on the surface of a copper foil through a glue spreader, drying at 150 ℃ for 30min, and melting at 280 ℃ for 10min to form a film;
s4: the copper foil was chemically etched to obtain an LCP film having a uniform thickness and a uniform dispersion of PTFE, and the film thickness was 30 μm.
Example 2
Example 2 is based on example 1 with the difference that: the solute content of the liquid crystal polymer solution was 12.5%; the weight percentage of the polytetrafluoroethylene powder is 15% and the film thickness of the LCP film material is 50 μm, based on 100% of the sum of the weight of the liquid crystal polymer and the weight of the polytetrafluoroethylene powder.
Example 3
Example 3 is based on example 1 with the difference that: the solute content of the liquid crystal polymer solution was 18%; the mass percent of the polytetrafluoroethylene powder is 25 percent based on 100 percent of the sum of the mass of the liquid crystal polymer and the mass of the polytetrafluoroethylene powder.
Example 4
Example 4 is based on example 1 with the difference that: the solute content of the liquid crystal polymer solution was 12.5%; the mass percent of the polytetrafluoroethylene powder is 35 percent based on 100 percent of the sum of the mass of the liquid crystal polymer and the mass of the polytetrafluoroethylene powder; in the S3, the drying temperature is 150 ℃, and the drying time is 25 min; the melting temperature is 300 ℃, and the melting time is 10 min.
Example 5
Example 5 is based on example 4 with the difference that the mixed slurry fineness is 20 μm.
Comparative example 1
Comparative example 1 based on example 1, except that the organic polymer solution of S1 was directly applied to the surface of copper foil, dried and melted to obtain an LCP film.
Samples of 200X 200mm were taken and tested for dielectric constant (Dk), dielectric loss (Df) and flexural modulus at a frequency of 10Ghz using a Des-Tech network analyzer in accordance with the IPC-TM-650 2.5.5.5 and ASTM D790, and the dielectric properties of the samples were measured at 10 points and averaged. The results are as follows:
| test specimen | Dk（10Ghz） | Df（10Ghz） | Flexural modulus/Gpa |
| Example 1 | 3.4±0.01 | 0.0035~0.0040 | 3.6 |
| Example 2 | 3.3±0.01 | 0.0033~0.0037 | 3.3 |
| Example 3 | 3.1±0.02 | 0.0030~0.0035 | 2.9 |
| Example 4 | 3.0±0.02 | 0.0030~0.0034 | 2.5 |
| Example 5 | 3.2±0.03 | 0.0040~0.0050 | 2.5 |
| Comparative example 1 | 3.6±0.01 | 0.0045~0.0050 | 3.9 |
Examples 1-5 and comparative example 1 had dielectric constant (Dk) tolerance values of: 0.01, ± 0.02, ± 0.03, ± 0.01; the dielectric loss (Df) tolerance values are: + -0.00025, + -0.0002, + -0.0005, + -0.00025.
Along with the increase of the content of polytetrafluoroethylene in the liquid crystal polymer film material raw material, the dielectric constant, the dielectric loss and the bending modulus value of the sample are reduced, the process can realize the production of the liquid crystal polymer film material with high polytetrafluoroethylene content, and the dielectric property consistency of the liquid crystal polymer film material is high.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the technical principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (8)
1. A preparation method of a liquid crystal polymer film with low dielectric constant and low dielectric loss is characterized by comprising the following steps:
s1, dissolving a liquid crystal polymer in a solvent to obtain a liquid crystal polymer solution;
s2, adding fluororesin powder into the liquid crystal polymer solution, and dispersing the mixed material;
s3, coating the mixed material obtained in the step S2 on the surface of a release base material, and forming a film on a coating layer through drying and melting treatment;
s4, separating the film layer from the release substrate to obtain a liquid crystal polymer film material;
the mass percentage of the fluororesin powder is 10-25% calculated by 100% of the sum of the mass of the fluororesin powder and the mass of the liquid crystal polymer; the average grain diameter of the fluororesin powder is 2-10 mu m; s2, the fineness of the mixed material slurry subjected to dispersion treatment is not more than 15 microns; the thickness of the liquid crystal polymer film is 30-100 mu m, the dielectric constant of the liquid crystal polymer film is 2.9-3.2, the dielectric loss is 0.002-0.005, and the flexural modulus is 2.8-3.6 Gpa.
2. The method of claim 1, wherein the fluororesin powder is polytetrafluoroethylene powder, and the polytetrafluoroethylene powder has a molecular weight of 5 to 50 ten thousand.
3. The method for preparing a liquid crystal polymer film with low dielectric constant and low dielectric loss according to claim 1, wherein the solvent is at least one selected from the group consisting of methylpyrrolidone and N, N-dimethylacetamide; the mass percentage of the liquid crystal polymer in the liquid crystal polymer solution is 5-20%.
4. The method for preparing a liquid crystal polymer film with low dielectric constant and low dielectric loss according to claim 1, wherein the drying temperature is 100 to 200 ℃.
5. The method for preparing a liquid crystal polymer film with low dielectric constant and low dielectric loss according to claim 1, wherein the temperature of the melting treatment is 200 to 330 ℃; the time of the melting treatment is 5-15 min.
6. The method of claim 1 or 5, wherein the release substrate is made of metal.
7. A liquid crystal polymer film, characterized in that it is prepared by the method of any one of claims 1 to 6.
8. A cellular phone antenna, characterized in that it is prepared from the low dielectric constant and low dielectric loss liquid crystal polymer film of claim 7.
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