Low dielectric LCP composite material and preparation method and application thereof
By adding components such as fluorinated porous silica to LCP, a low-dielectric LCP composite material was prepared, which solved the problem of high dielectric constant of LCP and achieved low dielectric loss and improved mechanical properties, making it suitable for 5G communication components.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- DONGGUAN ZHONGDING PLASTIC PRODUCTION CO LTD
- Filing Date
- 2026-02-11
- Publication Date
- 2026-06-02
AI Technical Summary
The dielectric constant of LCPs on the market is between 3.5 and 4.5, which cannot meet the requirements of 5G communication components and affects the propagation rate of electrical signals.
Low-dielectric LCP composites were prepared by adding low-dielectric filler fluorinated porous silica, surface modifiers, antioxidants, and lubricants to LCP. The pores of fluorinated porous silica and surface modifiers reduced the dielectric constant, antioxidants prevented material degradation, and lubricants improved processing fluidity.
The prepared low-dielectric LCP composite material has excellent low dielectric constant, low dielectric loss, mechanical properties and thermal stability, which meet the requirements of 5G communication components.
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Abstract
Description
Technical Field
[0001] This invention relates to the field of polymer materials technology, specifically to a low dielectric LCP composite material, its preparation method, and its application. Background Technology
[0002] Millimeter-wave communication technology, as one of the core technologies of 5G, has been widely used in various fields such as communications. It not only solves the problems of spectrum congestion and scarcity of spectrum resources in the low-frequency band (below 6GHz), but also meets the needs of 5G for high-capacity and high-speed communication. With the continuous development of millimeter-wave integrated circuits and radio frequency communication systems, future mobile communications will inevitably be based on millimeter-wave communication technology.
[0003] Low-dielectric liquid crystal polyarylate (LCP) is an advanced polymer material that exhibits liquid crystal properties in the molten state. With its excellent high strength, high rigidity, high temperature resistance, electrical insulation, and processability, it is used in electronics, electrical engineering, optical fibers, automotive manufacturing, and even aerospace. When LCP is applied to 5G communication, its dielectric constant becomes a key factor affecting the propagation speed of electrical signals; the lower the dielectric constant of the LCP, the faster the electrical signal propagates.
[0004] Although LCPs have many advantages and are suitable for frequencies below 110Hz, the dielectric constant of commercially available LCPs is between 3.5 and 4.5, which cannot meet the requirements of 5G communication components. Therefore, this invention aims to provide a low-dielectric LCP composite material, its preparation method, and its applications. Summary of the Invention
[0005] In order to overcome the shortcomings and deficiencies of the existing technology, one of the objectives of this invention is to provide a low dielectric LCP composite material, which has excellent low dielectric constant, low dielectric loss, mechanical properties and thermal stability.
[0006] To achieve the above-mentioned technical objectives and effects, the present invention is implemented through the following technical solution: A low-dielectric LCP composite material comprises the following raw materials in the following mass fractions: 70-95% LCP, 5-30% low-dielectric filler, 1-5% surface modifier, 0.1-1% antioxidant, and 0.1-1% lubricant.
[0007] Preferably, the melt index (MI) of the LCP is 10-100 g / 10 min (300℃ / 2.16 kg).
[0008] Preferably, the low-dielectric filler is fluorinated porous silica. On one hand, the pores of porous silica (air phase ε≈1.0) effectively reduce the dielectric constant. On the other hand, fluorine grafting reduces the surface polarity of porous silica, preventing agglomeration and improving its compatibility with LCP materials. Furthermore, porous silica possesses excellent mechanical properties and thermal stability. The addition of fluorinated silica results in LCP composite materials exhibiting excellent low dielectric constant, low dielectric loss, mechanical properties, and thermal stability.
[0009] Preferably, the surface modifier is selected from one or more of vinyltrimethoxysilane, methacryloxytrimethoxysilane, and phenyltrimethylsilane. Non-amino surface modifiers have lower dielectric constants, and adding a small amount of surface modifier can improve the interfacial compatibility between the low-dielectric filler and the LCP material, and prevent the low-dielectric filler from agglomerating.
[0010] Preferably, the antioxidant is selected from one or more of antioxidant 1010, antioxidant 168, and antioxidant 1098. LCP material is a semi-crystalline polymer with low hygroscopicity. By adding antioxidants, the degradation of the melt caused by the appearance of trace amounts of moisture under high temperature conditions can be prevented.
[0011] Preferably, the lubricant is selected from one or more of erucamide, polytetrafluoroethylene, and paraffin wax. Adding lubricant mainly improves processing fluidity and prevents low-dielectric filler from sticking to the screw.
[0012] Preferably, the preparation process of the low dielectric filler is as follows: (1) Porous silica is added to an ethanol-ammonia aqueous solution and ultrasonically dispersed to obtain a dispersion; (2) Perfluorooctyltriethoxysilane is added to a cyclohexane solvent and stirred to obtain a perfluorooctyltriethoxysilane-cyclohexane mixture; (3) The dispersion and the perfluorooctyltriethoxysilane-cyclohexane mixture are added together to a reaction vessel and stirred at room temperature for 24 hours. After the reaction, the mixture is filtered, washed, and dried to obtain fluorinated porous silica. By modifying porous silica with perfluorooctyltriethoxysilane, the silanol groups generated by the hydrolysis of perfluorooctyltriethoxysilane undergo a dehydration condensation reaction with the -OH group of porous silica to form a covalent bond, thereby grafting fluorocarbon long chains onto the porous silica and effectively improving the dispersibility of the fluorinated porous silica.
[0013] Preferably, the volume ratio of ethanol solution to ammonia in the ethanol-ammonia aqueous solution is (20-30):1, the volume fraction of ethanol in the ethanol solution is 90%, the mass fraction of NH3·H2O in the ammonia solution is 25-28%, and the concentration of perfluorooctyltriethoxysilane in the perfluorooctyltriethoxysilane-cyclohexane mixture is 0.1-0.5 g / mL.
[0014] Another object of the present invention is to provide a method for preparing the above-mentioned low-dielectric LCP composite material, comprising the following steps: S1. Weigh each raw material according to its mass fraction and dry it for later use; S2. Add each raw material to a twin-screw extruder for extrusion granulation to obtain a low-dielectric LCP composite material.
[0015] Preferably, the temperature of the feeding section of the twin-screw extruder is 250-270℃, the temperature of the compression section is 270-300℃, the temperature of the melting section is 290-310℃, and the temperature of the die head section is 280-300℃.
[0016] One object of the present invention is to provide the above-mentioned low dielectric LCP composite material for use in high frequency electronic components.
[0017] Compared with the prior art, the beneficial effects of the present invention are as follows: 1. The low-dielectric LCP composite material provided by the present invention effectively reduces the dielectric constant and dielectric loss of LCP material by adding fluorinated porous silica. The resulting low-dielectric LCP composite material has excellent low dielectric constant, low dielectric loss, mechanical properties and thermal stability.
[0018] 2. The preparation method of the low dielectric LCP composite material provided by the present invention is simple and easy to operate, and the obtained low dielectric LCP composite material has stable dielectric properties, thermal stability and mechanical properties. Detailed Implementation
[0019] The present invention will now be described in detail with reference to specific embodiments. It should also be noted that, to make the embodiments more comprehensive, the following embodiments are the best and preferred embodiments; those skilled in the art can also use other alternative methods to implement the invention for some well-known technologies.
[0020] It should be noted that the use of terms such as "an embodiment," "an embodiment," "an exemplary embodiment," and "some embodiments" in the specification indicates that the described embodiment may include a specific feature, structure, or characteristic, but not every embodiment necessarily includes that specific feature, structure, or characteristic. Furthermore, when a specific feature, structure, or characteristic is described in connection with an embodiment, implementing such a feature, structure, or characteristic in conjunction with other embodiments (whether explicitly described or not) should be within the knowledge of those skilled in the art.
[0021] Generally, terms can be understood at least partly from their use in context. For example, depending at least partly on the context, the term "one or more" as used herein can be used to describe any feature, structure, or characteristic in a singular sense, or a combination of features, structures, or characteristics in a plural sense. Additionally, the term "based on" can be understood not necessarily to convey an exclusive set of factors, but rather, alternatively, depending at least partly on the context, to allow for the presence of other factors that are not necessarily explicitly described.
[0022] Example 1 A low-dielectric LCP composite material comprises the following raw materials in the indicated mass fractions: 70% LCP, 5% low-dielectric filler, 1% surface modifier, 0.1% antioxidant, and 0.1% lubricant.
[0023] Preferably, the melt index (MI) of the LCP is 10 g / 10 min (300 °C / 2.16 kg).
[0024] Preferably, the low dielectric filler is fluorinated porous silica.
[0025] Preferably, the surface modifier is vinyltrimethoxysilane.
[0026] Preferably, the antioxidant is antioxidant 1010.
[0027] Preferably, the lubricant is erucamide.
[0028] Preferably, the preparation process of the low dielectric filler is as follows: (1) Porous silica is added to an ethanol-ammonia aqueous solution and ultrasonically dispersed to obtain a dispersion; (2) Perfluorooctyltriethoxysilane is added to a cyclohexane solvent and stirred to obtain a perfluorooctyltriethoxysilane-cyclohexane mixture; (3) The dispersion and the perfluorooctyltriethoxysilane-cyclohexane mixture are added together to a reaction vessel and stirred at room temperature for 24 hours. After the reaction, the mixture is filtered, washed and dried to obtain fluorinated porous silica.
[0029] Preferably, the volume ratio of ethanol solution to ammonia in the ethanol-ammonia solution is 20:1, the volume fraction of ethanol in the ethanol solution is 90%, the mass fraction of NH3·H2O in the ammonia solution is 25%, and the concentration of perfluorooctyltriethoxysilane in the perfluorooctyltriethoxysilane-cyclohexane mixture is 0.1 g / mL.
[0030] The preparation method of the above-mentioned low-dielectric LCP composite material includes the following steps: S1. Weigh each raw material according to its mass fraction and dry it for later use; S2. Add each raw material to a twin-screw extruder for extrusion granulation to obtain a low-dielectric LCP composite material.
[0031] Preferably, the temperature of the feeding section of the twin-screw extruder is 250°C, the temperature of the compression section is 270°C, the temperature of the melting section is 290°C, and the temperature of the die head section is 280°C.
[0032] Example 2 A low-dielectric LCP composite material comprises the following raw materials by mass fraction: 95% LCP, 25% low-dielectric filler, 5% surface modifier, 1% antioxidant, and 1% lubricant.
[0033] Preferably, the melt index (MI) of the LCP is 85 g / 10 min (300 °C / 2.16 kg).
[0034] Preferably, the low dielectric filler is fluorinated porous silica.
[0035] Preferably, the surface modifier is methacryloyloxytrimethoxysilane.
[0036] Preferably, the antioxidant is antioxidant 168.
[0037] Preferably, the lubricant is polytetrafluoroethylene.
[0038] Preferably, the preparation process of the low dielectric filler is as follows: (1) Porous silica is added to an ethanol-ammonia aqueous solution and ultrasonically dispersed to obtain a dispersion; (2) Perfluorooctyltriethoxysilane is added to a cyclohexane solvent and stirred to obtain a perfluorooctyltriethoxysilane-cyclohexane mixture; (3) The dispersion and the perfluorooctyltriethoxysilane-cyclohexane mixture are added together to a reaction vessel and stirred at room temperature for 24 hours. After the reaction, the mixture is filtered, washed and dried to obtain fluorinated porous silica.
[0039] Preferably, the volume ratio of ethanol solution to ammonia in the ethanol-ammonia solution is 30:1, the volume fraction of ethanol in the ethanol solution is 90%, the mass fraction of NH3·H2O in the ammonia solution is 28%, and the concentration of perfluorooctyltriethoxysilane in the perfluorooctyltriethoxysilane-cyclohexane mixture is 0.5 g / mL.
[0040] The preparation method of the above-mentioned low-dielectric LCP composite material includes the following steps: S1. Weigh each raw material according to its mass fraction and dry it for later use; S2. Add each raw material to a twin-screw extruder for extrusion granulation to obtain a low-dielectric LCP composite material.
[0041] Preferably, the temperature of the feeding section of the twin-screw extruder is 270°C, the temperature of the compression section is 300°C, the temperature of the melting section is 310°C, and the temperature of the die head section is 300°C.
[0042] Example 3 A low-dielectric LCP composite material comprises the following raw materials in the indicated mass fractions: 85% LCP, 15% low-dielectric filler, 3% surface modifier, 0.5% antioxidant, and 0.3% lubricant.
[0043] Preferably, the melt index (MI) of the LCP is 50 g / 10 min (300 °C / 2.16 kg).
[0044] Preferably, the low dielectric filler is fluorinated porous silica.
[0045] Preferably, the surface modifier is phenyltrimethylsilane.
[0046] Preferably, the antioxidant is antioxidant 1098.
[0047] Preferably, the lubricant is paraffin wax.
[0048] Preferably, the preparation process of the low dielectric filler is as follows: (1) Porous silica is added to an ethanol-ammonia aqueous solution and ultrasonically dispersed to obtain a dispersion; (2) Perfluorooctyltriethoxysilane is added to a cyclohexane solvent and stirred to obtain a perfluorooctyltriethoxysilane-cyclohexane mixture; (3) The dispersion and the perfluorooctyltriethoxysilane-cyclohexane mixture are added together to a reaction vessel and stirred at room temperature for 24 hours. After the reaction, the mixture is filtered, washed and dried to obtain fluorinated porous silica.
[0049] Preferably, the volume ratio of ethanol solution to ammonia in the ethanol-ammonia solution is 25:1, the volume fraction of ethanol in the ethanol solution is 90%, the mass fraction of NH3·H2O in the ammonia solution is 26%, and the concentration of perfluorooctyltriethoxysilane in the perfluorooctyltriethoxysilane-cyclohexane mixture is 0.3 g / mL.
[0050] The preparation method of the above-mentioned low-dielectric LCP composite material includes the following steps: S1. Weigh each raw material according to its mass fraction and dry it for later use; S2. Add each raw material to a twin-screw extruder for extrusion granulation to obtain a low-dielectric LCP composite material.
[0051] Preferably, the temperature of the feeding section of the twin-screw extruder is 260°C, the temperature of the compression section is 290°C, the temperature of the melting section is 300°C, and the temperature of the die head section is 290°C.
[0052] Comparative Example 1 The difference between this comparative example and Example 3 is that an equal amount of porous silica is used to replace fluorinated porous silica.
[0053] Comparative Example 2 The difference between this comparative example and Example 3 is that an equal amount of fluorinated silicon dioxide is used to replace fluorinated porous silicon dioxide.
[0054] Dielectric property testing: The LCP composite materials prepared in Examples 1-3 and Comparative Examples 1-2 were cut into planar samples with a thickness of 0.1 mm. Conductive electrodes were attached to both sides of each sample and the samples were placed in a dielectric spectrometer for testing. The test results are shown in the table below.
[0055] Tensile strength test: The test shall be conducted in accordance with GB / T 1040.2-2022 standard.
[0056]
[0057] As can be seen from the table above, by adding fluorinated porous silica to LCP materials, LCP composite materials exhibit excellent low dielectric constant, low dielectric loss, and mechanical properties.
[0058] This invention encompasses any substitutions, modifications, equivalent methods, and solutions made within the spirit and scope of this invention. To provide the public with a thorough understanding of this invention, specific details are described in detail in the following preferred embodiments; however, those skilled in the art will fully understand the invention even without these details. Furthermore, to avoid unnecessary misunderstanding of the essence of this invention, well-known methods, processes, procedures, components, and circuits are not described in detail.
[0059] The above description is only a preferred embodiment of the present invention. It should be noted that for those skilled in the art, several improvements and modifications can be made without departing from the principle of the present invention, and these improvements and modifications should also be considered within the scope of protection of the present invention.
Claims
1. A low-dielectric LCP composite material, characterized in that: The raw materials include the following mass fractions: LCP 70-95%, low dielectric filler 5-30%, surface modifier 1-5%, antioxidant 0.1-1%, and lubricant 0.1-1%.
2. The low-dielectric LCP composite material according to claim 1, characterized in that: The melt index (MI) of the LCP is 10-100 g / 10 min (300℃ / 2.16 kg).
3. The low-dielectric LCP composite material according to claim 1, characterized in that: The low dielectric filler is selected from fluorinated porous silica.
4. The low-dielectric LCP composite material according to claim 1, characterized in that: The surface modifier is selected from one or more of vinyltrimethoxysilane, methacryloxytrimethoxysilane, and phenyltrimethylsilane.
5. The low-dielectric LCP composite material according to claim 1, characterized in that: The antioxidant is selected from one or more of antioxidant 1010, antioxidant 168 and antioxidant 1098.
6. The low-dielectric LCP composite material according to claim 1, characterized in that: The lubricant is selected from one or more of erucamide, polytetrafluoroethylene and paraffin.
7. The low-dielectric LCP composite material according to claim 1, characterized in that: The preparation process of the low dielectric filler is as follows: (1) Porous silica is added to an ethanol-ammonia aqueous solution and ultrasonically dispersed to obtain a dispersion; (2) Perfluorooctyltriethoxysilane is added to a cyclohexane solvent and stirred to obtain a perfluorooctyltriethoxysilane-cyclohexane mixture; (3) The dispersion and the perfluorooctyltriethoxysilane-cyclohexane mixture are added together to a reaction vessel and stirred at room temperature for 24 hours. After the reaction, the mixture is filtered, washed and dried to obtain fluorinated porous silica.
8. A method for preparing a low-dielectric LCP composite material as described in claims 1-7, characterized in that: Includes the following steps: S1. Weigh each raw material according to its mass fraction and dry it for later use; S2. Add each raw material to a twin-screw extruder for extrusion granulation to obtain a low-dielectric LCP composite material.
9. The method for preparing a low-dielectric LCP composite material according to claim 8, characterized in that: The temperature of the feeding section of the twin-screw extruder is 250-270℃, the temperature of the compression section is 270-300℃, the temperature of the melting section is 290-310℃, and the temperature of the die head section is 280-300℃.
10. A low-dielectric LCP composite material as described in any one of claims 1-7, applied to high-frequency electronic components.