CN111674007A - Liquid crystal polymer film for 5G communication and preparation method thereof - Google Patents
Liquid crystal polymer film for 5G communication and preparation method thereof Download PDFInfo
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- CN111674007A CN111674007A CN202010376604.1A CN202010376604A CN111674007A CN 111674007 A CN111674007 A CN 111674007A CN 202010376604 A CN202010376604 A CN 202010376604A CN 111674007 A CN111674007 A CN 111674007A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/001—Combinations of extrusion moulding with other shaping operations
- B29C48/0018—Combinations of extrusion moulding with other shaping operations combined with shaping by orienting, stretching or shrinking, e.g. film blowing
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/25—Component parts, details or accessories; Auxiliary operations
- B29C48/30—Extrusion nozzles or dies
- B29C48/32—Extrusion nozzles or dies with annular openings, e.g. for forming tubular articles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C55/00—Shaping by stretching, e.g. drawing through a die; Apparatus therefor
- B29C55/02—Shaping by stretching, e.g. drawing through a die; Apparatus therefor of plates or sheets
- B29C55/10—Shaping by stretching, e.g. drawing through a die; Apparatus therefor of plates or sheets multiaxial
- B29C55/12—Shaping by stretching, e.g. drawing through a die; Apparatus therefor of plates or sheets multiaxial biaxial
- B29C55/14—Shaping by stretching, e.g. drawing through a die; Apparatus therefor of plates or sheets multiaxial biaxial successively
- B29C55/146—Shaping by stretching, e.g. drawing through a die; Apparatus therefor of plates or sheets multiaxial biaxial successively firstly transversely to the direction of feed and then parallel thereto
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C55/00—Shaping by stretching, e.g. drawing through a die; Apparatus therefor
- B29C55/28—Shaping by stretching, e.g. drawing through a die; Apparatus therefor of blown tubular films, e.g. by inflation
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2300/00—Characterised by the use of unspecified polymers
- C08J2300/12—Polymers characterised by physical features, e.g. anisotropy, viscosity or electrical conductivity
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2367/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
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- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Shaping By String And By Release Of Stress In Plastics And The Like (AREA)
- Manufacture Of Macromolecular Shaped Articles (AREA)
- Extrusion Moulding Of Plastics Or The Like (AREA)
Abstract
The invention discloses a liquid crystal polymer film for 5G communication and a preparation method thereof, wherein the preparation method comprises the following steps: extruding the melt of the liquid crystal polymer resin through a die head with an annular gap to obtain an extrudate; cooling the extrudate to below the glass transition temperature, and then winding at a first draw ratio to obtain a pre-oriented tubular film; heating the pre-oriented tubular film to a temperature between the glass transition temperature and the heat distortion temperature, then winding at a second drawing ratio, and expanding the pre-oriented tubular film at a preset blow-up ratio to obtain the liquid crystal polymer film. The invention can obtain the liquid crystal polymer film with good mechanical properties and excellent dimensional stability in TD and MD directions.
Description
Technical Field
The invention relates to the technical field of high polymer materials, in particular to a liquid crystal polymer film for 5G communication and a preparation method thereof.
Background
Since 1965 Kevlar, the first liquid crystal polymer product, was introduced to DuPont, its superior properties were valued. After the liquid crystal polymer is heated and melted or dissolved by a solvent, the rigidity of a solid substance is lost, the fluidity of a liquid crystal substance is obtained, the ordered arrangement of crystalline substance molecules is still kept, and therefore, the liquid crystal polymer is anisotropic in physical properties and forms a transition state with partial properties of crystals and liquid. Due to the unique chain structure and the ordered arrangement among molecules, the liquid crystal polymer has excellent comprehensive physical and mechanical properties, such as high thermal deformation temperature, dimensional stability, excellent mechanical property, electrical property, irradiation resistance, chemical resistance, aging resistance, self-flame retardance, low permeability and the like, and is widely applied to the fields of electronics, electricity, automobile industry and the like.
Since electromagnetic waves have the characteristics that the higher the frequency, the shorter the wavelength, and the easier the attenuation in a propagation medium, the higher the frequency, the smaller the loss of the antenna material is required. PI films (polyimides) are used as antenna manufacturing materials in the 4G era, and PI materials have excellent advantages of high temperature resistance, low temperature resistance, high electrical insulation, corrosion resistance and the like, and are mainly used as insulating materials in FPCs. However, PI has a large loss at a frequency of 2.4GHz or more, cannot be used at a frequency of 10GHz or more, has a large moisture absorption, is not reliable enough, and is gradually replaced in the high-frequency 5G era. The Liquid Crystal Polymer (LCP) has excellent electrical properties, can keep the dielectric constant even at extremely high frequency and has consistency; the dielectric loss and the conductor loss are small, and the method can be applied to millimeter wave treatment; the thermoplastic property is strong, and the multilayer lamination is easy to realize. With the advent of the 5G era with high frequency and high speed, the excellent properties of LCP films will replace PI as a new flexible board material. Therefore, the Liquid Crystal Polymer (LCP) film has bright application prospect and huge market value in the age of 5G.
At present, the main methods for producing liquid crystal polymer films are extrusion blow molding and extrusion casting. Since the liquid crystal polymer has a high degree of orientation under the action of a shearing force, there is a significant disadvantage of mechanical anisotropy, that is, a film prepared by a conventional method has high mechanical properties in the MD Direction (Machine Direction) and poor tensile strength in the TD Direction (perpendicular to the Machine Direction). Therefore, the anisotropy of liquid crystal polymer films limits their application in high frequency transmission applications.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: provided are a liquid crystal polymer film for 5G communication and a method for manufacturing the same, which can obtain a liquid crystal polymer film having good mechanical properties in TD and MD directions and excellent dimensional stability.
In order to solve the technical problems, the invention adopts the technical scheme that:
a preparation method of a liquid crystal polymer film for 5G communication comprises the steps of extruding a melt of liquid crystal polymer resin through a die head with an annular gap to obtain an extrudate; cooling the extrudate to below the glass transition temperature, and then winding at a first draw ratio to obtain a pre-oriented tubular film; heating the pre-oriented tubular film to a temperature between the glass transition temperature and the heat distortion temperature, then winding at a second drawing ratio, and expanding the pre-oriented tubular film at a preset blow-up ratio to obtain the liquid crystal polymer film.
The invention adopts another technical scheme that:
a liquid crystal polymer film for 5G communication is prepared according to the preparation method of the liquid crystal polymer film for 5G communication.
The invention has the beneficial effects that: the melt is extruded and then wound at a certain draw ratio to obtain a pre-oriented tubular film, and the pre-oriented tubular film is simultaneously blown and stretched to enable the film to be biaxially oriented in the TD direction and the MD direction, so that the liquid crystal polymer film with good mechanical properties and excellent dimensional stability in the TD direction and the MD direction can be obtained.
Detailed Description
In order to explain the technical content, the objects and the effects of the present invention in detail, the following description will be given with reference to the embodiments.
The most key concept of the invention is as follows: the pre-oriented tubular film is simultaneously blown and stretched to enable the film to be subjected to biaxial orientation in the TD direction and the MD direction, so that the liquid crystal polymer film with good mechanical property and good dimensional stability is obtained.
A preparation method of a liquid crystal polymer film for 5G communication comprises the steps of extruding a melt of liquid crystal polymer resin through a die head with an annular gap to obtain an extrudate; cooling the extrudate to below the glass transition temperature, and then winding at a first draw ratio to obtain a pre-oriented tubular film; heating the pre-oriented tubular film to a temperature between the glass transition temperature and the heat distortion temperature, then winding at a second drawing ratio, and expanding the pre-oriented tubular film at a preset blow-up ratio to obtain the liquid crystal polymer film.
From the above description, the beneficial effects of the present invention are: the melt is extruded and then wound at a certain draw ratio to obtain a pre-oriented tubular film, and the pre-oriented tubular film is simultaneously blown and stretched to enable the film to be biaxially oriented in the TD direction and the MD direction, so that the liquid crystal polymer film with good mechanical properties and excellent dimensional stability in the TD direction and the MD direction can be obtained. The tensile strength of the prepared liquid crystal polymer film in TM and MD directions is about 160-180 MPa, and the linear expansion coefficient is about 12-19 ppm/DEG C.
Furthermore, the shape of annular gap is the rectangle, the length of annular gap is 10 ~ 20 times of width, the width of annular gap is 0.5 ~ 5 mm.
As can be seen from the above description, the extrudate has some orientation in the MD after extrusion through the annular gap.
Further, the first stretching ratio is 1-2.5.
Further, the second stretching ratio is 1-4.
Further, the preset blow-up ratio is at least twice the second draw ratio.
Further, before extruding the melt of the liquid crystal polymer resin through a die having an annular gap, the method further comprises: drying the liquid crystal polymer resin at 150-170 ℃ for 4-6 h.
As can be seen from the above description, drying the liquid crystal polymer resin can remove small molecular substances such as moisture, and improve the quality of the final liquid crystal polymer film.
Further, the temperature at the time of extrusion is from (Tm-10 ℃) to (Tm +50 ℃), and Tm represents the melting point of the liquid crystal polymer.
As can be seen from the above description, the extrusion temperature should not be too high or too low, too low a viscosity is too high to facilitate molding, and too high a viscosity may cause degradation of the liquid crystal polymer.
The invention relates to another technical scheme which is as follows:
a liquid crystal polymer film for 5G communication is prepared according to the preparation method of the liquid crystal polymer film for 5G communication.
Example one
The first embodiment of the invention is as follows: a preparation method of a liquid crystal polymer film for 5G communication comprises the following steps:
1. the melt of the liquid crystalline polymer resin is extruded through a die having an annular gap to give an extrudate.
The extruding a melt of liquid crystal polymer resin through a die having an annular gap further comprises: the liquid crystal polymer resin is dried for 4-6 hours at the temperature of 150-170 ℃, so that micromolecular substances such as water and the like can be removed, and the adopted liquid crystal polymer resin is high-melt-viscosity liquid crystal polymer resin. The shape of annular gap is the rectangle, the length of annular gap is 10 ~ 20 times of width, the width of annular gap is 0.5 ~ 5 mm. The processing temperature during extrusion is (Tm-10 ℃) to (Tm +50 ℃), and Tm represents the melting point of the liquid crystal polymer.
2. The extrudate is cooled below the glass transition temperature and then wound at a first draw ratio to provide a pre-oriented tubular film.
After extrusion, the extrudate is rapidly cooled to below the glass transition temperature, in this example, the first draw ratio is 1 to 2.5.
3. Heating the pre-oriented tubular film to a temperature between the glass transition temperature and the heat distortion temperature, then winding at a second drawing ratio, and expanding the pre-oriented tubular film at a preset blow-up ratio to obtain the liquid crystal polymer film.
Heating the pre-oriented tubular film in a heater, wherein the second stretching ratio is 1-4, and the preset blow-up ratio is at least two times of the second stretching ratio.
Example two
The second embodiment of the present invention is a method for preparing a liquid crystal polymer film for 5G communication, which is different from the first embodiment in that:
in step 1, the liquid crystal polymer resin used is a wholly aromatic polyester liquid crystal polymer having a melting point of about 280 ℃, a glass transition temperature of about 200 ℃ and a heat distortion temperature of about 260 ℃. The liquid crystal polymer resin is dried for 4 hours at the temperature of 170 ℃. The width of the annular gap is 2mm, and the length of the annular gap is 15 times of the width, namely 30 mm. The processing temperature during extrusion was 280 ℃.
In step 2, the first draw ratio is 1.
In step 3, the pre-oriented tubular film was heated to 200 ℃ with a second draw ratio of 2.5 and a blow-up ratio of 5.6.
EXAMPLE III
The third embodiment of the present invention is a method for preparing a liquid crystal polymer film for 5G communication, which is different from the first embodiment in that:
in step 1, the liquid crystal polymer resin used is a wholly aromatic polyester liquid crystal polymer having a melting point of about 280 ℃, a glass transition temperature of about 200 ℃ and a heat distortion temperature of about 260 ℃. The liquid crystal polymer resin is dried for 6 hours at the temperature of 150 ℃. The width of the annular gap is 0.5mm, and the length of the annular gap is 20 times of the width, namely 10 mm. The processing temperature during extrusion was 300 ℃.
In step 2, the first draw ratio is 1.
In step 3, the pre-oriented tubular film was heated to 250 ℃, the second draw ratio was 2.7, and the blow-up ratio was 5.6.
Example four
The fourth embodiment of the present invention is a method for preparing a liquid crystal polymer film for 5G communication, which is different from the first embodiment in that:
in step 1, the liquid crystal polymer resin used is a wholly aromatic polyester liquid crystal polymer having a melting point of about 280 ℃, a glass transition temperature of about 200 ℃ and a heat distortion temperature of about 260 ℃. The liquid crystal polymer resin is dried for 6 hours at the temperature of 150 ℃. The width of the annular gap is 0.5mm, and the length of the annular gap is 20 times of the width, namely 10 mm. The processing temperature during extrusion was 300 ℃.
In step 2, the first draw ratio is 1.
In step 3, the pre-oriented tubular film was heated to 250 ℃, the second draw ratio was 2.7, and the blow-up ratio was 8.
EXAMPLE five
The fifth embodiment of the present invention is a method for preparing a liquid crystal polymer film for 5G communication, which is different from the first embodiment in that:
in step 1, the liquid crystal polymer resin used is a wholly aromatic polyester liquid crystal polymer having a melting point of about 280 ℃, a glass transition temperature of about 200 ℃ and a heat distortion temperature of about 260 ℃. The liquid crystal polymer resin is dried for 5 hours at the temperature of 160 ℃. The width of the annular gap is 5mm, and the length of the annular gap is 10 times of the width, namely 50 mm. The processing temperature during extrusion was 270 ℃.
In step 2, the first draw ratio is 1.
In step 3, the pre-oriented tubular film is heated to 230 ℃, the second draw ratio is 3, and the blow-up ratio is 8.
EXAMPLE six
The sixth embodiment of the present invention is a method for preparing a liquid crystal polymer film for 5G communication, which is different from the first embodiment in that:
in step 1, the liquid crystal polymer resin used is a wholly aromatic polyester liquid crystal polymer having a melting point of about 280 ℃, a glass transition temperature of about 200 ℃ and a heat distortion temperature of about 260 ℃. The liquid crystal polymer resin is dried for 4 hours at the temperature of 170 ℃. The width of the annular gap is 0.5mm, and the length of the annular gap is 15 times of the width, namely 7.5 mm. The processing temperature during extrusion was 330 ℃.
In step 2, the first draw ratio was 2.5.
In step 3, the pre-oriented tubular film is heated to 250 ℃, the second draw ratio is 3, and the blow-up ratio is 6.
EXAMPLE seven
The seventh embodiment of the present invention is a method for preparing a liquid crystal polymer film for 5G communication, which is different from the first embodiment in that:
in step 1, the liquid crystal polymer resin used is a wholly aromatic polyester liquid crystal polymer having a melting point of about 280 ℃, a glass transition temperature of about 200 ℃ and a heat distortion temperature of about 260 ℃. The liquid crystal polymer resin is dried for 4 hours at the temperature of 170 ℃. The width of the annular gap is 0.5mm, and the length of the annular gap is 15 times of the width, namely 7.5 mm. The processing temperature during extrusion was 290 ℃.
In step 2, the first draw ratio was 1.8.
In step 3, the pre-oriented tubular film is heated to 250 ℃, the second draw ratio is 4, and the blow-up ratio is 8.
Example eight
The eighth embodiment of the present invention is a method for preparing a liquid crystal polymer film for 5G communication, which is different from the first embodiment in that:
in step 1, the liquid crystal polymer resin used is a wholly aromatic polyester liquid crystal polymer having a melting point of about 280 ℃, a glass transition temperature of about 200 ℃ and a heat distortion temperature of about 260 ℃. The liquid crystal polymer resin is dried for 4 hours at the temperature of 170 ℃. The width of the annular gap is 0.5mm, and the length of the annular gap is 15 times of the width, namely 7.5 mm. The processing temperature during extrusion was 290 ℃.
In step 2, the first draw ratio was 1.5.
In step 3, the pre-oriented tubular film is heated to 250 ℃, the second draw ratio is 1, and the blow-up ratio is 3.
The liquid crystal polymer films prepared in examples two to eight were respectively tested for tensile strength, tensile modulus and linear expansion coefficient, and the test results are shown in table 1.
Performance testing
1. Tensile Properties
The samples were cut into dumbbell shapes with a cutter according to ISO-527-3 standard, and the tensile strength, and the tensile modulus were measured. As a test apparatus, a C45.102 electronic universal tester manufactured by New Satsu corporation was used. The tensile test was conducted at a speed of 10mm/min using a tensile tester to determine the strength at break and the tensile elongation at break of the specimen.
2. Coefficient of linear expansion
According to ISO-11359-2 standard, the sample is cut into a 15mm × 5mm strip shape by a cutter, and the linear expansion coefficient of the sample is measured by adopting a stretching mode. As test equipment, a thermomechanical analyzer of the type TMA4000 from the company PE (Perkin Elmer) was used. The load was 0.05N, and the temperature was raised at a rate of 10mm/min to determine the linear expansion coefficient of the sample in a temperature range of 50 to 100 ℃.
Table 1 results of performance testing
As can be seen from Table 1, the liquid crystal polymer films prepared by the method of the present invention have close mechanical properties in MD and TD directions and good dimensional stability. As can be seen from the comparison of the third and fourth examples, the liquid crystal polymer films prepared using different blow-up ratios have better mechanical properties and dimensional stability as the blow-up ratio increases.
In summary, the liquid crystal polymer film for 5G communication and the preparation method thereof provided by the invention can obtain the liquid crystal polymer film with good mechanical properties in TD and MD directions and excellent dimensional stability.
The above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and all equivalent modifications made by the present invention in the specification or directly or indirectly applied to the related technical field are included in the scope of the present invention.
Claims (8)
1. A preparation method of a liquid crystal polymer film for 5G communication is characterized in that a melt of liquid crystal polymer resin is extruded through a die head with an annular gap to obtain an extrudate; cooling the extrudate to below the glass transition temperature, and then winding at a first draw ratio to obtain a pre-oriented tubular film; heating the pre-oriented tubular film to a temperature between the glass transition temperature and the heat distortion temperature, then winding at a second drawing ratio, and expanding the pre-oriented tubular film at a preset blow-up ratio to obtain the liquid crystal polymer film.
2. The method of claim 1, wherein the annular gap has a rectangular shape, the length of the annular gap is 10 to 20 times the width of the annular gap, and the width of the annular gap is 0.5 to 5 mm.
3. The method for preparing a liquid crystal polymer film for 5G communication according to claim 1, wherein the first stretching ratio is 1 to 2.5.
4. The method for preparing a liquid crystal polymer film for 5G communication according to claim 1, wherein the second stretching ratio is 1 to 4.
5. The method of claim 4, wherein the preset inflation ratio is at least twice the second stretching ratio.
6. The method for preparing a liquid crystal polymer film for 5G communication according to claim 1, wherein the step of extruding the melt of the liquid crystal polymer resin through a die having an annular gap further comprises: drying the liquid crystal polymer resin at 150-170 ℃ for 4-6 h.
7. The method of producing a liquid crystal polymer film for 5G communication according to claim 1, wherein the temperature at the time of extrusion is from (Tm-10 ℃) to (Tm +50 ℃), Tm representing the melting point of the liquid crystal polymer.
8. A liquid crystal polymer film for 5G communication, characterized by being prepared by the method for preparing a liquid crystal polymer film for 5G communication according to any one of claims 1 to 7.
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| CN202010376604.1A CN111674007A (en) | 2020-05-07 | 2020-05-07 | Liquid crystal polymer film for 5G communication and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113352524A (en) * | 2021-06-21 | 2021-09-07 | 南京贝迪新材料科技股份有限公司 | Method for preparing LCP film from LCP particles by tape casting |
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