CN111690326A - Preparation method of liquid crystal polymer film or liquid crystal polymer copper-clad plate - Google Patents
Preparation method of liquid crystal polymer film or liquid crystal polymer copper-clad plate Download PDFInfo
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- CN111690326A CN111690326A CN202010395415.9A CN202010395415A CN111690326A CN 111690326 A CN111690326 A CN 111690326A CN 202010395415 A CN202010395415 A CN 202010395415A CN 111690326 A CN111690326 A CN 111690326A
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- liquid crystal
- crystal polymer
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D201/00—Coating compositions based on unspecified macromolecular compounds
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
- B05D3/02—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by baking
- B05D3/0254—After-treatment
- B05D3/0263—After-treatment with IR heaters
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
- B05D7/14—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials to metal, e.g. car bodies
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
- B05D7/24—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials for applying particular liquids or other fluent materials
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D2202/00—Metallic substrate
- B05D2202/40—Metallic substrate based on other transition elements
- B05D2202/45—Metallic substrate based on other transition elements based on Cu
Abstract
The invention discloses a preparation method of a liquid crystal polymer film or a liquid crystal polymer copper-clad plate, which comprises the steps of carrying out melting treatment on a liquid crystal polymer, coating the liquid crystal polymer after the melting treatment onto a carrier through a high-temperature coating port die, and carrying out baking and cooling treatment on the carrier coated with the liquid crystal polymer to obtain the liquid crystal polymer film or the liquid crystal polymer copper-clad plate. The preparation process is simple and has high efficiency; the prepared liquid crystal polymer film or liquid crystal polymer copper-clad plate has good uniformity in MD direction and TD direction.
Description
Technical Field
The invention relates to the technical field of high molecular materials, in particular to a preparation method of a liquid crystal polymer film or a liquid crystal polymer copper-clad plate.
Background
Liquid Crystal Polymer (LCP) is an excellent electrical property and excellent physical and mechanical properties, and is often used as an insulating substrate in flexible circuit boards, for example: smart phones, tablet computers, automotive electronics, and other application scenarios.
The liquid crystal polymer film is processed from liquid crystal polymer resins, which are classified into lyotropic liquid crystal polymer resins and thermotropic liquid crystal polymer resins. The lyotropic liquid crystalline polymer resin can be dissolved in a suitable solvent, coated or coated on a suitable substrate by solution coating, and then the solvent is dried at a high temperature, which makes it easier to prepare a liquid crystalline polymer film. Thermotropic liquid crystal polymer films are often prepared by hot melt processing, and the current main methods are as follows: the melt extrusion double-pulling method is characterized in that a polymer is melted by heat inside an extruder and extruded and double-pulled in a neck mold of the extruder, and the MD and TD directions are subjected to orientation effect together, so that the problem of large orientation difference in different directions is solved; in the melt blow molding method, a polymer is heated and melted in a blow molding machine, extruded from a blow film opening, and blown into a film. However, the liquid crystal polymer film prepared by the method often depends on equipment and a process to a large extent, the process difficulty is large, the prepared liquid crystal polymer film still has strong orientation in a certain direction, the product yield is low, the cleaning difficulty of the equipment of a shutdown machine is large, the difficulty is increased for the forming of the LCP film, and the capacity is limited.
After the liquid crystal polymer film is formed, if a copper-clad process is needed to prepare the LCP copper-clad plate, the LCP film and the copper foil are needed to be selected for high-temperature lamination, so that the problem of two procedures is involved.
In the literature or patent reports at home and abroad, the thermotropic liquid crystal polymer is generally improved or upgraded by aiming at the two schemes, such as improving the blowing-up mode of a melt blown out from a blowing die, changing a die head into a blowing mode of a rotary die head to control orientation, but the orientation problem is still difficult to solve essentially, the process difficulty is high, and the yield is not high.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: the preparation method of the liquid crystal polymer film or the liquid crystal polymer copper-clad plate is high in production efficiency, and the liquid crystal polymer copper-clad plate does not need secondary processing.
In order to solve the technical problems, the invention adopts the technical scheme that:
a preparation method of a liquid crystal polymer film or a liquid crystal polymer copper-clad plate comprises the steps of carrying out melting treatment on a liquid crystal polymer, coating the liquid crystal polymer after the melting treatment onto a carrier through a high-temperature coating neck mold, and carrying out baking and cooling treatment on the carrier coated with the liquid crystal polymer to obtain the liquid crystal polymer film or the liquid crystal polymer copper-clad plate.
The invention has the beneficial effects that: the film or the copper-clad plate is processed from the resin raw material at one time in a high-temperature coating mode, so that the original structure of the polymer is not damaged, and the performance of a processed product is not influenced; organic solvents are avoided in the processing process, so that the processing method is more environment-friendly; the thickness range of the coating film is large, and the coating film can be adjusted according to requirements; when the carrier adopts the copper foil, the liquid crystal polymer copper clad laminate can be obtained at one time, the second pressing procedure is reduced, the time and the process cost are reduced, the continuous production can be realized, and the efficiency is high; the liquid crystal polymer film or the liquid crystal polymer copper clad laminate can be prepared into the liquid crystal polymer film or the liquid crystal polymer copper clad laminate with small orientation difference in different directions, the polymer crystallization degree is uniform, and the film has good uniformity in different directions; the high-temperature coating mode brings a new idea for the hot-melt type liquid crystal polymer which is difficult to form.
Drawings
Fig. 1 is a schematic diagram of the cooling rate of the baking cooling process according to the second embodiment of the present invention.
Detailed Description
In order to explain technical contents, achieved objects, and effects of the present invention in detail, the following description is made with reference to the accompanying drawings in combination with the embodiments.
The most key concept of the invention is as follows: the film or the copper-clad plate is obtained by processing the resin raw material at one time in a high-temperature coating mode, the original structure of the polymer is not damaged, and the performance of a processed product is not influenced.
A preparation method of a liquid crystal polymer film or a liquid crystal polymer copper-clad plate comprises the steps of carrying out melting treatment on a liquid crystal polymer, coating the liquid crystal polymer after the melting treatment onto a carrier through a high-temperature coating neck mold, and carrying out baking and cooling treatment on the carrier coated with the liquid crystal polymer to obtain the liquid crystal polymer film or the liquid crystal polymer copper-clad plate.
From the above description, the beneficial effects of the present invention are: the film or the copper-clad plate is processed from the resin raw material at one time in a high-temperature coating mode, so that the original structure of the polymer is not damaged, and the performance of a processed product is not influenced; organic solvents are avoided in the processing process, so that the processing method is more environment-friendly; the thickness range of the coating film is large, and the coating film can be adjusted according to requirements; when the carrier adopts the copper foil, the liquid crystal polymer copper clad laminate can be obtained at one time, the second pressing procedure is reduced, the time and the process cost are reduced, the continuous production can be realized, and the efficiency is high; the liquid crystal polymer film or the liquid crystal polymer copper clad laminate can be prepared into the liquid crystal polymer film or the liquid crystal polymer copper clad laminate with small orientation difference in different directions, the polymer crystallization degree is uniform, and the film has good uniformity in different directions; the high-temperature coating mode brings a new idea for the hot-melt type liquid crystal polymer which is difficult to form.
Further, the carrier is a steel belt, an aluminum foil or a copper foil.
As can be seen from the above description, when the support is a steel belt or an aluminum foil, a liquid crystal polymer film is obtained; when the carrier is copper foil, the obtained liquid crystal polymer copper-clad plate is.
Further, the baking and cooling treatment specifically comprises: initially, carrying out infrared baking and cooling at the speed of 0.8-1.2 ℃/min; then carrying out infrared baking and cooling at the speed of 1.8-3.2 ℃/min; and when the temperature is lower than the glass transition temperature, carrying out infrared baking and cooling at the speed of 4.8-5.2 ℃/min.
As can be seen from the above description, the cooling rate is relatively slow at the beginning, and the cooling rate can be increased appropriately at the later stage.
Further, the baking and cooling treatment is carried out under the protection of inert gas.
Further, stretching the liquid crystal polymer in the baking and cooling treatment process, wherein the stretching treatment comprises longitudinal stretching and transverse stretching in sequence.
Further, the stretching ratio of the stretching treatment is 1.1-1.3.
As can be seen from the above description, the film or copper-clad plate prepared by adopting the double-stretching mode has high strength and modulus and good mechanical properties.
Example one
The first embodiment of the invention is as follows: a preparation method of a liquid crystal polymer film or a liquid crystal polymer copper-clad plate comprises the following steps:
1. the liquid crystalline polymer is subjected to a melt processing.
In the present embodiment, the liquid crystal polymer used may be an aromatic liquid crystal polymer, for example, a meltable liquid crystal polymer synthesized by copolymerizing polycyclic rigid molecules, introducing naphthalene rings into the molecular structure, using aliphatic segments in the molecular chain, or other meltable polymers, for example, polyvinylidene fluoride, engineering plastics (polyethylene terephthalate, polyaryletherketone, and the like). The liquid crystal polymer resin can be baked at 120 ℃ for 6h before use.
2. And coating the liquid crystal polymer after the melting treatment onto a carrier through a high-temperature coating die.
In this embodiment, the liquid crystal polymer is melted in the high-temperature extruder, the high-temperature coating die is assembled on the high-temperature extruder, and the high-temperature extruder needs to meet the requirement that the internal extrusion temperature is higher than the melting point of the liquid crystal polymer, so as to ensure that the liquid crystal polymer is uniformly plasticized in the high-temperature extruder. The high-temperature coating neck ring mold is made of high-temperature resistant materials, and the height of the gap of the neck ring mold can be adjusted according to requirements. The carrier is a steel belt, an aluminum foil or a copper foil, when the carrier is the steel belt and the aluminum foil, the liquid crystal polymer film is obtained subsequently, and when the carrier is the copper foil, the liquid crystal polymer copper-clad plate is obtained subsequently.
3. And baking and cooling the carrier coated with the liquid crystal polymer to obtain the liquid crystal polymer film or the liquid crystal polymer copper-clad plate.
The baking and cooling treatment specifically comprises the following steps: initially, carrying out infrared baking and cooling at the speed of 0.8-1.2 ℃/min; then carrying out infrared baking and cooling at the speed of 1.8-3.2 ℃/min; and when the temperature is lower than the glass transition temperature, carrying out infrared baking and cooling at the speed of 4.8-5.2 ℃/min. Preferably, the infrared baking cooling is carried out at the speed of 1 ℃/min at the beginning; after the temperature is reduced to 280 ℃, carrying out infrared baking and cooling at the speed of 2 ℃/min; after the temperature is reduced to 180 ℃, carrying out infrared baking and cooling at the speed of 3 ℃/min; and when the temperature is lower than the glass transition temperature, carrying out infrared baking and cooling at the speed of 5 ℃/min. The baking and cooling treatment is carried out under the protection of inert gas, and the inert gas can be nitrogen, argon and the like. In the embodiment, the carrier coated with the liquid crystal polymer melt is gradually cooled in a high-temperature oven, the oven is heated by infrared, a blast drying oven is not used, and the melt is prevented from being interfered by air flow to influence the flatness of the melt.
In this embodiment, the liquid crystal polymer may be further stretched in the baking and cooling process, and the stretching process includes sequentially performing longitudinal stretching and transverse stretching. The stretching ratio of the stretching treatment is 1.1-1.3, and the temperature of the stretching treatment is 10-20 ℃ lower than the melting point of the liquid crystal polymer.
And after the liquid crystal polymer film or the liquid crystal polymer copper-clad plate is shaped, sequentially carrying out edge cutting and rolling.
Example two
The second embodiment of the invention is a preparation method of a liquid crystal polymer film or a liquid crystal polymer copper-clad plate, which is different from the first embodiment in that:
the liquid crystalline polymer used in step 1 was a VECTRA C950 having a melting point of 320 ℃ and available on the acriba platform, and the temperature of the extruder was set in stages up to 325 ℃.
In the step 2, the carrier is aluminum foil, and the initial temperature of the aluminum foil is 320-325 ℃.
In step 3, the baking and cooling treatment specifically comprises: initially, carrying out infrared baking and cooling at the speed of 1 ℃/min; when the temperature is reduced to 280 ℃, the temperature is reduced at the speed of 2 ℃/min; after the temperature is reduced to 180 ℃, carrying out infrared baking and cooling at the speed of 3 ℃/min; when the temperature is lower than 90 ℃, the temperature is reduced to the room temperature at the speed of 5 ℃/min, and the schematic diagram of the temperature reduction speed is shown in figure 1.
In this embodiment, the stretching process is not performed in the baking and cooling process.
EXAMPLE III
The third embodiment of the invention is a preparation method of a liquid crystal polymer film or a liquid crystal polymer copper-clad plate, and is different from the second embodiment in that:
in step 2, the carrier is a steel belt.
In step 3, the infrared baking is firstly carried out at the speed of 1 ℃/min for cooling, after the temperature is reduced to 305 ℃, the material is longitudinally stretched to 1.3 times, then transversely stretched to 1.2 times, under the condition of maintaining the stretching tension, the temperature is reduced to 180 ℃ at the cooling speed of 2 ℃/min, then the temperature is reduced to 90 ℃ at the cooling speed of 3 ℃/min, and then the temperature is reduced to the room temperature at the cooling speed of 5 ℃/min.
Example four
The fourth embodiment of the invention is a preparation method of a liquid crystal polymer film or a liquid crystal polymer copper-clad plate, and is different from the second embodiment in that:
in step 2, the carrier is a copper foil.
EXAMPLE five
The fifth embodiment of the invention is a preparation method of a liquid crystal polymer film or a liquid crystal polymer copper-clad plate, and is different from the third embodiment in that:
in the step 3, the infrared baking is firstly carried out at the speed of 0.8 ℃/min for cooling, after the temperature is reduced to 305 ℃, the material is longitudinally stretched to 1.2 times, then transversely stretched to 1.1 times, under the condition of maintaining the stretching tension, the temperature is reduced to 180 ℃ at the cooling rate of 2 ℃/min, then the temperature is reduced to 90 ℃ at the cooling rate of 3 ℃/min, and then the material is reduced to the room temperature at the cooling rate of 5.2 ℃/min.
EXAMPLE six
The sixth embodiment of the invention is a preparation method of a liquid crystal polymer film or a liquid crystal polymer copper-clad plate, and is different from the third embodiment in that:
in the step 3, the infrared baking is firstly carried out at the speed of 1.2 ℃/min for cooling, after the temperature is reduced to 305 ℃, the material is longitudinally stretched to 1.3 times, then transversely stretched to 1.2 times, under the condition of keeping the stretching tension, the temperature is reduced to 180 ℃ at the cooling speed of 1.8 ℃/min, then the temperature is reduced to 90 ℃ at the cooling speed of 3.2 ℃/min, and then the material is reduced to the room temperature at the cooling speed of 4.8 ℃/min.
And (3) carrying out performance tests on the liquid crystal polymer film or the liquid crystal polymer copper-clad plate prepared in the second to sixth embodiments, wherein the performance tests comprise tensile strength, bending performance and stripping force. The tensile strength test is carried out by adopting the ASTM D882 standard, and before the tensile strength test of the fourth embodiment (the liquid crystal polymer copper clad laminate), the copper foil is etched to obtain the liquid crystal polymer film. In addition, the fourth embodiment (liquid crystal polymer copper clad laminate) also represents the bending performance and the peeling force index, and the specific requirements of the bending performance test are as follows: the bending radius R is 0.38mm, the frequency is 175R/min, the load is 500gf, the bending angle is +/-135 degrees, and the fracture failure is judged by the open circuit of the copper foil or the mechanical fracture of the sample; the peel force test adopts 90-degree peeling, and before the test, the copper foil on the tested surface of the sample is etched into 3.2mm of equidistant copper stripes.
The test results are shown in table 1.
TABLE 1 Performance test results of liquid crystal polymer films or liquid crystal polymer copper clad laminates
As can be seen from the above table, the prepared liquid crystal polymer film or liquid crystal polymer copper clad laminate has good uniformity in MD direction and TD direction; if the stretching treatment is carried out in the baking and cooling process, the mechanical strength of the material can be improved; the prepared liquid crystal polymer copper-clad plate has good bending resistance and high peel strength.
In conclusion, the preparation method of the liquid crystal polymer film or the liquid crystal polymer copper-clad plate provided by the invention has the advantages of simple preparation process and high efficiency; the prepared liquid crystal polymer film or liquid crystal polymer copper-clad plate has good uniformity in MD direction and TD direction.
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 changes made by using the contents of the present specification and the drawings, or applied directly or indirectly to the related technical fields, are included in the scope of the present invention.
Claims (6)
1. The preparation method of the liquid crystal polymer film or the liquid crystal polymer copper-clad plate is characterized by comprising the steps of carrying out melting treatment on a liquid crystal polymer, coating the liquid crystal polymer subjected to melting treatment onto a carrier through a high-temperature coating port die, and carrying out baking and cooling treatment on the carrier coated with the liquid crystal polymer to obtain the liquid crystal polymer film or the liquid crystal polymer copper-clad plate.
2. The method for preparing the liquid crystal polymer film or the liquid crystal polymer copper clad laminate according to claim 1, wherein the carrier is a steel belt, an aluminum foil or a copper foil.
3. The method for preparing the liquid crystal polymer film or the liquid crystal polymer copper-clad plate according to claim 1, wherein the baking and cooling treatment specifically comprises: initially, carrying out infrared baking and cooling at the speed of 0.8-1.2 ℃/min; then carrying out infrared baking and cooling at the speed of 1.8-3.2 ℃/min; and when the temperature is lower than the glass transition temperature, carrying out infrared baking and cooling at the speed of 4.8-5.2 ℃/min.
4. The method for preparing the liquid crystal polymer film or the liquid crystal polymer copper clad laminate according to claim 3, wherein the baking and cooling treatment is performed under the protection of inert gas.
5. The method for preparing the liquid crystal polymer film or the liquid crystal polymer copper-clad plate according to claim 1, wherein the liquid crystal polymer is stretched in the baking and cooling process, and the stretching process comprises longitudinal stretching and transverse stretching in sequence.
6. The method for preparing the liquid crystal polymer film or the liquid crystal polymer copper clad laminate according to claim 5, wherein the stretching ratio of the stretching treatment is 1.1-1.3.
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CN109867982A (en) * | 2019-01-07 | 2019-06-11 | 江阴骏驰复合材料有限公司 | Liquid crystal polymer composite and the application of a kind of low thermal coefficient of expansion and the low loss factor |
CN110256850A (en) * | 2019-07-08 | 2019-09-20 | 苏州固泰新材股份有限公司 | Modified liquid crystal polymer film and its preparation method and application |
CN110760310A (en) * | 2019-09-27 | 2020-02-07 | 深圳市信维通信股份有限公司 | Method for improving mechanical property of liquid crystal polymer product |
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2020
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