CN114316522B - High-performance liquid crystal polymer composite material and application thereof - Google Patents
High-performance liquid crystal polymer composite material and application thereof Download PDFInfo
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Abstract
The invention provides a high-performance liquid crystal polymer composite material and application thereof, and belongs to the technical field of high-polymer composite materials. The invention provides a high-performance liquid crystal polymer composite material, which comprises the following components in parts by weight: 60-90 parts of liquid crystal polymer, 10-40 parts of additive and 1-10 parts of compatilizer. The liquid crystal polymer composite material provided by the invention has the advantages of high temperature resistance, good electrical insulation performance, easiness in processing and the like. The high-performance liquid crystal polymer composite material provided by the invention is prepared into a composite film by a melt blow molding processing method, and the composite film has low anisotropy, good mechanical property and excellent high-frequency dielectric property, is suitable for high-speed circuits and high-frequency electronic devices, and is particularly suitable for circuit substrate materials required in the field of 5G high-frequency communication.
Description
Technical Field
The invention belongs to the technical field of high polymer composite materials, and particularly relates to a high-performance liquid crystal polymer composite material and application thereof.
Background
Liquid crystal polymer (Liquid CrystalPolymer, LCP) is a linear rigid aromatic polyester-based material. Compared with other high polymer materials, the LCP has a unique molecular structure, so that the LCP has excellent heat resistance, low hygroscopicity, low dielectric loss, high modulus strength, chemical corrosion resistance, flame retardance and the like, and has bright application prospect in the fields of electric/electronic, new energy automobiles, military industry, aerospace and the like.
However, since the LCP molecular chains are rigid rod-like, the molecular chain entanglement points are few and the entanglement force is weak in the molten state, the orientation in the flow direction is extremely easy to exhibit high anisotropy, resulting in problems of the difference in the properties of the molded article in the machine axis direction (MD) and the direction perpendicular to the machine axis (TD), and poor weld mark strength. Furthermore, since LCP materials are difficult to dissolve in conventional solvents, their main processing methods are extrusion casting and melt blowing. The LCP is limited to be easy to be anisotropic, low in melt tension and serious in sagging, and the LCP is processed and molded by the traditional extrusion casting method and blow molding method, so that the molded product often has the problems of high anisotropy, low tearing strength and the like, the rejection rate is high in practical application, the preparation cost is greatly increased, and the problems are difficult to solve by means of processing technology and equipment.
The electrical insulation performance of the LCP film can be improved by introducing different additives into the LCP resin raw material to prepare the composite material, but the problems of anisotropy, low tearing strength, high yield and the like of the LCP material molding can be solved on the basis of keeping the dielectric performance of the LCP film to meet the requirements, and the composite material has important significance for development and application of liquid crystal polymers.
Disclosure of Invention
In view of the above, the present invention is directed to providing a high performance liquid crystal polymer composite material and application thereof, in which the LCP composite material is prepared by introducing additives into the LCP resin material without changing the molecular structure and the processing and molding method of the LCP, and a film having low anisotropy, good mechanical properties and excellent high frequency dielectric properties is obtained by conventional melt blow molding processing, and the film is suitable for high-speed circuits and high frequency electronic devices, particularly suitable for circuit substrate materials required in the 5G high frequency communication field.
The invention provides a high-performance liquid crystal polymer composite material, which comprises the following components in parts by weight:
60-90 parts of liquid crystal polymer;
10-40 parts of additive;
1-10 parts of compatilizer;
the additive is selected from any one or more of polyether-ether-ketone, polyether-ketone, polyether-ether-ketone, PCT, PPS and PPO.
Preferably, the liquid crystal polymer is a thermotropic liquid crystal polymer.
Preferably, the compatilizer is polyimide substance.
The invention provides a preparation method of the high-performance liquid crystal polymer composite material, which comprises the following steps:
mixing a liquid crystal polymer, an additive and a compatilizer, and drying to obtain a dried product;
and mixing the dried product, and granulating to obtain the high-performance liquid crystal polymer composite material.
Preferably, the drying temperature is 100-160 ℃.
Preferably, the granulation is extrusion granulation;
the extrusion temperature of the extrusion granulation is 260-400 ℃.
The invention provides a film which is prepared from the raw materials of the high-performance liquid crystal polymer composite material according to the technical scheme; or (b)
The high-performance liquid crystal polymer composite material is prepared from the raw materials of the high-performance liquid crystal polymer composite material prepared by the method.
The present invention provides a high-speed circuit, comprising: the film according to the technical scheme.
The present invention provides a high-frequency electronic device including: the film according to the technical scheme.
The present invention provides a circuit substrate, comprising: the film according to the technical scheme.
The additive in the high-performance liquid crystal polymer composite material provided by the invention has the advantages that the melt processing temperature is equivalent to that of an LCP material, and the prepared film has high tearing strength; after the additive is blended with the LCP material, on one hand, the single orientation of the molecular chain segments of the LCP can be broken in the melt processing process, and the anisotropism of the LCP film is reduced; on the other hand, the overall tearing strength of the LCP film can be improved, and the yield is improved. The tensile strength of the film prepared by the composite material in the mechanical axis direction is within the range of 198-210 MPa, and the tensile strength of the film in the direction orthogonal to the mechanical axis is within the range of 185-195 MPa, which is characterized by low anisotropy; the dielectric loss of the film provided by the invention is below 0.003 and the dielectric constant is below 3.3 under the high-frequency 25 GHz; meanwhile, the LCP composite material product is applied to circuit substrate materials required in the field of 5G high-frequency communication.
Detailed Description
The following description of the technical solutions in the embodiments of the present invention will be clear and complete, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The invention provides a high-performance liquid crystal polymer composite material, which comprises the following components in parts by weight:
60-90 parts of liquid crystal polymer;
10-40 parts of additive;
1-10 parts of compatilizer.
In the present invention, the weight part of the liquid crystal polymer is preferably 65 to 85 parts, more preferably 70 to 80 parts, and most preferably 75 parts.
In the present invention, the liquid crystal polymer is preferably a thermotropic liquid crystal polymer, which is preferably a rigid aromatic polyester-based material comprising repeating units of at least one of-HN-Ar-CO-, -HN-Ar-O-, -O-Ar-CO-and-O-Ar-O-, wherein Ar is selected from at least one of aromatic substituents of substituted and unsubstituted mono-phenylene, aromatic substituents of biphenylene, aromatic substituents of acene phenylene, the aromatic substituents being bonded with carbon or non-carbon element; such as Sumitomo chemical E600, E500, E400 series products, selanis A950, baoli GA series products, etc.
In the present invention, the weight part of the additive is preferably 15 to 35 parts, more preferably 20 to 30 parts, and most preferably 25 parts.
In the present invention, the additive is selected from any one or more of polyetheretherketone, polyetherketone, polyetherketoneketone, polyetheretherketone, PCT (triphenylmethane copolyester), PPS (polyphenylene sulfide), and PPO (polyphenylene oxide), more preferably selected from one or more of PPS, PCT, and polyetherketoneketone.
In the present invention, the compatibilizing agent is preferably a polyimide-based substance, more preferably an aromatic polyimide-based substance, and preferably has the following structure:
the invention provides a preparation method of the high-performance liquid crystal polymer composite material, which comprises the following steps:
mixing a liquid crystal polymer, an additive and a compatilizer, and drying to obtain a dried product;
and mixing the dried product, and granulating to obtain the high-performance liquid crystal polymer composite material.
In the present invention, the components and parts by weight of the liquid crystal polymer, the additive and the compatibilizer are consistent with the above technical solutions, and will not be described herein.
In the present invention, the mixing is preferably performed under stirring; the stirring speed is preferably 15-30 r/min, more preferably 20-25 r/min, and most preferably 22-23 r/min; the mixing time is preferably 20 to 40min, more preferably 25 to 35min, most preferably 30min.
In the present invention, the drying method is preferably vacuum drying; the drying temperature is preferably 100 to 160 ℃, more preferably 110 to 150 ℃, more preferably 120 to 140 ℃, and most preferably 130 ℃; the drying time is preferably 0.5 to 1.5 hours, more preferably 0.8 to 1.2 hours, and most preferably 1 hour.
In the present invention, the kneading is preferably melt-kneading; the mixing is preferably carried out in a twin-screw extruder.
In the present invention, the granulation is preferably extrusion granulation; the extrusion temperature of the extrusion granulation is preferably 260-400 ℃, more preferably 280-400 ℃, more preferably 300-400 ℃ and most preferably 350 ℃; the extrusion speed of the extrusion granulation is preferably 40-110 r/min, more preferably 50-105 r/min, more preferably 60-90 r/min, and most preferably 70-80 r/min; the feeding speed in the extrusion granulation process is preferably 3-10 r/min, more preferably 4-9 r/min, more preferably 5-8 r/min, and most preferably 6-7 r/min.
The invention provides a film which is prepared from the raw materials of the high-performance liquid crystal polymer composite material according to the technical scheme; or (b)
The high-performance liquid crystal polymer composite material is prepared from the raw materials of the high-performance liquid crystal polymer composite material prepared by the method.
In the present invention, the thickness of the film is preferably 80 to 120 micrometers, more preferably 90 to 110 micrometers, and most preferably 100 micrometers.
In the present invention, the method for producing a film preferably comprises:
and carrying out melt blow molding on the high-performance liquid crystal polymer to obtain a film.
In the present invention, the melt blowing is preferably performed in an extruder; the extrusion temperature of the melt blowing is preferably 280-320 ℃, more preferably 290-310 ℃, and most preferably 300 ℃; the extrusion pressure is preferably 0.8 to 2.8MPa, more preferably 1 to 1.5MPa, most preferably 1.2 to 1.3MPs; in the process of melting and blowing, a forming and cooling system air ring is preferably regulated, the air outlet temperature of the first air ring is preferably 220-260 ℃, more preferably 230-250 ℃ and most preferably 240 ℃; the outlet air temperature of the second air ring is preferably 40-60 ℃, more preferably 45-55 ℃ and most preferably 50 ℃; the film bubble inflation ratio in the fusion blowing process is stable when 5, the film with the thickness of 100 micrometers is obtained, and the film is led out to form a roll along the traction direction.
The present invention provides a high-speed circuit, comprising: the film according to the technical scheme.
The present invention provides a high-frequency electronic device including: the film according to the technical scheme.
The present invention provides a circuit substrate, comprising: the film according to the technical scheme.
The additive in the high-performance liquid crystal polymer composite material provided by the invention has the advantages that the melt processing temperature is equivalent to that of an LCP material, and the prepared film has high tearing strength; after the additive is blended with the LCP material, on one hand, the single orientation of the molecular chain segments of the LCP can be broken in the melt processing process, and the anisotropism of the LCP film is reduced; on the other hand, the overall tearing strength of the LCP film can be improved, and the yield is improved. The tensile strength of the film prepared by the composite material in the mechanical axis direction is within the range of 198-210 MPa, and the tensile strength of the film in the direction orthogonal to the mechanical axis is within the range of 185-195 MPa, which is characterized by low anisotropy; the dielectric loss of the film provided by the invention is below 0.003 and the dielectric constant is below 3.3 under the high-frequency 25 GHz; meanwhile, the LCP composite material product is applied to circuit substrate materials required in the field of 5G high-frequency communication.
In the embodiment of the invention, the LCP body material is Seranis A950 (component A for short), the polyether ketone material is polyether ketone (component K for short), the compatilizer is aromatic linear polyimide, and the product is Kapton (component C for short) provided by DuPont company.
Example 1
The preparation raw materials of the liquid crystal polymer composite material comprise the following raw materials in parts by weight: a is 60 parts, K is 40 parts, and C is 5 parts.
The preparation method of the liquid crystal polymer composite material comprises the following steps:
uniformly blending the weighed A, K and C raw materials in a mixer, wherein the mixing speed is 20r/min, and the mixing time is 30min; after being uniformly mixed, the mixture is put into a vacuum dryer for drying treatment, the drying treatment temperature is 120 ℃, and the drying time is 1 hour;
adding the dried blending material into a double-screw extruder for melt mixing, and extruding and granulating to obtain a liquid crystal polymer composite material; wherein the extrusion temperature is 320 ℃, the extrusion speed is 90r/min, and the feeding speed is 5r/min.
Preparation of the film:
preparing a film from the prepared liquid crystal polymer composite material by a melt blow molding processing method (the extrusion temperature is 300 ℃, the extrusion pressure is 2MPa, the air outlet temperature of a first air ring is 240 ℃, the air outlet temperature of a second air ring is 50 ℃, and the film bubble inflation ratio is 5; the film thickness was 100 microns with a tolerance of 10%.
Example 2
The preparation raw materials of the liquid crystal polymer composite material comprise the following raw materials in parts by weight: a is 70 parts, K is 30 parts, and C is 5 parts.
The preparation method of the liquid crystal polymer composite material comprises the following steps:
uniformly blending the weighed A, K and C raw materials in a mixer, wherein the mixing speed is 20r/min, and the mixing time is 30min; after being uniformly mixed, the mixture is put into a vacuum dryer for drying treatment, the drying treatment temperature is 120 ℃, and the drying time is 1 hour;
adding the dried blending material into a double-screw extruder for melt mixing, and extruding and granulating to obtain a liquid crystal polymer composite material; wherein the extrusion temperature is 320 ℃, the extrusion speed is 90r/min, and the feeding speed is 5r/min.
Preparation of the film:
preparing a film from the prepared liquid crystal polymer composite material by a melt blow molding processing method (the extrusion temperature is 300 ℃, the extrusion pressure is 2MPa, the air outlet temperature of a first air ring is 240 ℃, the air outlet temperature of a second air ring is 50 ℃, and the film bubble inflation ratio is 5; the film thickness was 100 microns with a tolerance of 10%.
Example 3
The preparation raw materials of the liquid crystal polymer composite material comprise the following raw materials in parts by weight: a is 80 parts, K is 20 parts, and C is 5 parts.
A method of preparing a liquid crystal polymer composite comprising:
uniformly blending the weighed A, K and C raw materials in a mixer, wherein the mixing speed is 20r/min, and the mixing time is 30min; after being uniformly mixed, the mixture is put into a vacuum dryer for drying treatment, the drying treatment temperature is 120 ℃, and the drying time is 1 hour;
adding the dried blending material into a double-screw extruder for melt mixing, and extruding and granulating to obtain a liquid crystal polymer composite material; wherein the extrusion temperature is 320 ℃, the extrusion speed is 90r/min, and the feeding speed is 5r/min.
Preparation of the film:
the liquid crystal polymer composite material prepared by the method is prepared into a film by a melt blow molding processing method (the extrusion temperature is 300 ℃, the extrusion pressure is 2MPa, the air outlet temperature of a first air ring is 240 ℃, the air outlet temperature of a second air ring is 50 ℃, and the film bubble inflation ratio is 5; the film thickness was 100 microns with a tolerance of 10%.
Example 4
The preparation raw materials of the liquid crystal polymer composite material comprise the following raw materials in parts by weight: a is 90 parts, K is 10 parts, and C is 5 parts.
Uniformly blending the weighed A, K and C raw materials in a mixer, wherein the mixing speed is 20r/min, the mixing time is 30min; after being uniformly mixed, the mixture is put into a vacuum dryer for drying treatment, the drying treatment temperature is 120 ℃, and the drying time is 1 hour;
adding the dried blending material into a double-screw extruder for melt mixing, and extruding and granulating to obtain a liquid crystal polymer composite material; wherein the extrusion temperature is 320 ℃, the extrusion speed is 90r/min, and the feeding speed is 5r/min.
Preparation of the film:
the liquid crystal polymer composite material prepared by the method is prepared into a film by a melt blow molding processing method (the extrusion temperature is 300 ℃, the extrusion pressure is 2MPa, the air outlet temperature of a first air ring is 240 ℃, the air outlet temperature of a second air ring is 50 ℃, and the film bubble inflation ratio is 5, so that the film is stable); the film thickness was 100 microns with a tolerance of 10%.
Comparative example 1
The component A (LCP body material) is prepared into a film by a melt blow molding processing method (extrusion temperature is 300 ℃, extrusion pressure is 2MPa, the air outlet temperature of a first air ring is 240 ℃, the air outlet temperature of a second air ring is 50 ℃, and the film bubble inflation ratio is 5; the film thickness was 100 microns with a tolerance of 10%.
Comparative example 2
Preparing component K (polyether ketone body material) into a film through a hot press forming machine, placing component K in a mould, then clamping between an upper electric heating plate and a lower electric heating plate, applying pressure to the electric heating plate at 320 ℃ for 10min, and cooling to obtain a film product; the film thickness was 100 microns with a tolerance of 10%.
Comparative example 3
The preparation raw materials of the liquid crystal polymer composite material comprise the following raw materials in parts by weight: a is 70 parts, K is 30 parts, and C is 0 part.
A method of preparing a liquid crystal polymer composite comprising:
uniformly blending the weighed raw materials A and K in a mixer, wherein the mixing speed is 20r/min, and the mixing time is 30min; after being uniformly mixed, the mixture is put into a vacuum dryer for drying treatment, the drying treatment temperature is 120 ℃, and the drying time is 1 hour;
adding the dried blending material into a double-screw extruder for melt mixing, and extruding and granulating to obtain a liquid crystal polymer composite material; wherein the extrusion temperature is 320 ℃, the extrusion speed is 90r/min, and the feeding speed is 5r/min.
Preparation of the film:
the liquid crystal polymer composite material prepared by the method is prepared into a film by a melt blow molding processing method (the extrusion temperature is 300 ℃, the extrusion pressure is 2MPa, the air outlet temperature of a first air ring is 240 ℃, the air outlet temperature of a second air ring is 50 ℃, and the film bubble inflation ratio is 5, so that the film is stable); the film thickness was 100 microns with a tolerance of 10%.
Comparative example 4
The preparation raw materials of the liquid crystal polymer composite material comprise the following raw materials in parts by weight: a is 80 parts, K is 20 parts, and C is 0 part.
The preparation method of the liquid crystal polymer composite material comprises the following steps:
uniformly blending the weighed raw materials A and K in a mixer, wherein the mixing speed is 20r/min, and the mixing time is 30min; after being uniformly mixed, the mixture is put into a vacuum dryer for drying treatment, the drying treatment temperature is 120 ℃, and the drying time is 1 hour;
adding the dried blending material into a double-screw extruder for melt mixing, and extruding and granulating to obtain a liquid crystal polymer composite material; wherein the extrusion temperature is 320 ℃, the extrusion speed is 90r/min, and the feeding speed is 5r/min.
Preparation of the film:
the liquid crystal polymer composite material prepared by the method is prepared into a film by a melt blow molding processing method (the extrusion temperature is 300 ℃, the extrusion pressure is 2MPa, the air outlet temperature of a first air ring is 240 ℃, the air outlet temperature of a second air ring is 50 ℃, and the film bubble inflation ratio is 5; the film thickness was 100 microns with a tolerance of 10%.
Performance detection
The liquid crystal polymer composite films prepared in examples and comparative examples were subjected to dielectric and mechanical property tests:
testing the dielectric constant (Dk) and dielectric loss (Df) of the polymer composite film at 25GHz frequency by an Agilent 85071E type instrument by adopting a resonant cavity method; simultaneously, according to ISO 527-3 and ISO6383-1 standards, the film sample is subjected to tensile strength test and tearing strength test by a universal testing machine; the test results are shown in Table 1.
TABLE 1 dielectric and mechanical Properties of films prepared in examples and comparative examples of the present invention
Note that: in table 1, Δ refers to the difference between the average tensile strengths in the MD and TD directions.
As can be seen from the test results in Table 1, the composite film prepared in the embodiment of the invention has dielectric loss below 0.003 and dielectric constant below 3.3 at high frequency of 25GHz, which shows that the composite film has excellent dielectric property at high frequency; secondly, as the content of the polyetherketoneketone component is reduced, the difference between the tensile strength of the liquid crystal polymer composite material film prepared in the embodiments 1-4 in the MD and TD directions is obviously increased, which indicates that the composite film is changed from anisotropy to isotropy, but compared with the comparative example 1, the difference between the MD and TD directions is smaller, which indicates that the introduction of the polyetherketoneketone component can effectively improve the anisotropy problem of the LCP bulk material film; meanwhile, compared with comparative examples 1 and 2, the tearing strength of the liquid crystal polymer composite material film prepared in examples 1-4 is gradually reduced along with the reduction of the content of the polyether ketone component, which indicates that the introduction of the polyether ketone component can effectively improve the overall tearing strength of the LCP bulk material film and improve the yield; in addition, comparative examples 3 and 4, in which no compatibilizing agent was added, exhibited lower tear strengths than examples 2 and 3, indicating that the inclusion of the compatibilizing agent could improve the tear strength of the LCP composite film, but the tensile strength was less affected by the compatibilizing agent.
The composite film prepared by the liquid crystal polymer composite material provided by the invention through a melt blow molding processing method has the characteristics of low anisotropy, good mechanical property, excellent high-frequency dielectric property and the like, and the excellent property of the composite film enables the composite film to be suitable for high-speed circuits and high-frequency electronic devices, and particularly to be used for circuit substrate materials required in the field of 5G high-frequency communication.
The additive in the high-performance liquid crystal polymer composite material provided by the invention has the advantages that the melt processing temperature is equivalent to that of an LCP material, and the prepared film has high tearing strength; after the additive is blended with the LCP material, on one hand, the single orientation of the molecular chain segments of the LCP can be broken in the melt processing process, and the anisotropism of the LCP film is reduced; on the other hand, the overall tearing strength of the LCP film can be improved, and the yield is improved. The tensile strength of the film prepared by the composite material in the mechanical axis direction is within the range of 198-210 MPa, and the tensile strength of the film in the direction orthogonal to the mechanical axis is within the range of 185-195 MPa, which is characterized by low anisotropy; the dielectric loss of the film provided by the invention is below 0.003 and the dielectric constant is below 3.3 under the high-frequency 25 GHz; meanwhile, the LCP composite material product is applied to circuit substrate materials required in the field of 5G high-frequency communication.
While the invention has been described and illustrated with reference to specific embodiments thereof, the description and illustration is not intended to limit the invention. It will be apparent to those skilled in the art that various changes may be made in this particular situation, material, composition of matter, substance, method or process without departing from the true spirit and scope of the invention as defined by the following claims, so as to adapt the objective, spirit and scope of the present application. All such modifications are intended to be within the scope of this appended claims. Although the methods disclosed herein have been described with reference to particular operations being performed in a particular order, it should be understood that these operations may be combined, sub-divided, or reordered to form an equivalent method without departing from the teachings of the present disclosure. Thus, unless specifically indicated herein, the order and grouping of operations is not a limitation of the present application.
Claims (8)
1. The high-performance liquid crystal polymer composite material comprises the following concrete components in parts by weight:
60 parts of liquid crystal polymer;
40 parts of additive;
5 parts of a compatilizer;
the liquid crystal polymer is Seranias A950, the additive is polyether ketone, and the compatilizer is Kapton product provided by DuPont company.
2. A method of preparing the high performance liquid crystal polymer composite of claim 1, comprising:
mixing a liquid crystal polymer, an additive and a compatilizer, and drying to obtain a dried product;
and mixing the dried product, and granulating to obtain the high-performance liquid crystal polymer composite material.
3. The method according to claim 2, wherein the drying temperature is 100-160 ℃.
4. The method of claim 2, wherein the granulating is extrusion granulating;
the extrusion temperature of the extrusion granulation is 260-400 ℃.
5. A film prepared from a raw material comprising the high performance liquid crystalline polymer composite material of claim 1; or (b)
Is prepared from the raw materials comprising the high-performance liquid crystal polymer composite material prepared by the method of claim 2.
6. A high speed circuit comprising: the film of claim 5.
7. A high frequency electronic device comprising: the film of claim 5.
8. A circuit substrate, comprising: the film of claim 5.
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