A polyphenylene ether composite material and preparation method thereof

Abstract

The invention discloses a kind of polyphenylene ether composite material and preparation method thereof, the polyphenylene ether composite material is prepared by weight by the following components:1000 parts of polyphenylene ether, 100 200 parts of high-impact polystyrene, 60 100 parts of polytetrafluoroethylene wax, 200 800 parts of soda lime borosilicate hollow glass microspheres, 2 10 parts of antioxidants.The present invention, by adding polytetrafluoroethylene wax in polyphenylene ether composite material, can not only enhance composition fluidity and plasticizing effect, improve its processing and mechanical property, the dielectric constant of composite material can also be further reduced.Compared with talcum powder, calcium carbonate, borosilicate hollow glass microspheres, soda lime borosilicate hollow glass microspheres are added in the present invention, the tensile strength, shock resistance of composite material can be further improved, the dielectric constant of composite material can also be significantly reduced.

Description

Technical Field

[0001] The present invention belongs to the technical field of polymer composite materials, and in particular relates to a polyphenylene ether composite material and a preparation method thereof. Background Art

[0002] Polyphenylene ether (PPO) is a high-strength engineering plastic developed in the 1960s. Its chemical name is poly-2,6-dimethyl-1,4-phenylene ether, abbreviated as PPO (Polyphenylene Oxide) or PPE (Polypheylene ether), also known as polyphenylene oxide or polyphenylene ether. PPO is non-toxic, transparent, and has a low relative density. It exhibits excellent mechanical strength, stress relaxation resistance, creep resistance, heat resistance, water resistance, water vapor resistance, and dimensional stability. It exhibits excellent electrical properties over a wide temperature and frequency range. However, its main drawback is its poor melt flowability, making it difficult to process and mold.

[0003] With the rapid development of electronic information technology, the integration density of ultra-large-scale integrated circuit (VLSI) devices is increasing, while their feature sizes are shrinking. This leads to increased resistance-capacitance (RC) delays, signal transmission delays, increased interference, and increased power loss. This limits the high-speed performance of these devices. One important way to alleviate this problem is to reduce the dielectric constant of the dielectric material—that is, to reduce the material's parasitic capacitance. As the thickness of silicon dioxide (SiO2), used as an insulating layer between conductors, increases its intrinsic capacitance, the thickness decreases. This charge accumulation interferes with signal transmission, reduces circuit reliability, and limits further increases in frequency. To address this issue, the microelectronics industry is adopting low-dielectric-constant materials to replace traditional silicon dioxide insulating materials. The application of polyphenylene ether (PPE) materials in the microelectronics industry to replace traditional silicon dioxide insulating materials requires not only improved processing properties but also further reductions in its dielectric properties. Summary of the Invention

[0004] In view of the problems existing in the prior art, the purpose of the present invention is to provide a polyphenylene ether composite material and a preparation method thereof, wherein the polyphenylene ether composite material has good processing performance and a low dielectric constant.

[0005] The object of the present invention is achieved through the following technical solutions:

[0006] A polyphenylene ether composite material is prepared from the following components in parts by weight:

[0007]

[0008]

[0009] As a preferred technical solution, the high-impact polystyrene has a melt index of 3-10 g / 10 min at 200° C. and 5 kg.

[0010] As a preferred technical solution, the soda lime borosilicate hollow glass microspheres are hollow, have a density of 0.1-0.3 g / cc, and a particle size of 20-30 μm.

[0011] As a preferred technical solution, the antioxidant is a mixture of antioxidant 1010 and antioxidant 168; further preferably, the mass ratio of antioxidant 1010 to antioxidant 168 in the mixture is 1:1.

[0012] The present invention also provides a method for preparing the above-mentioned polyphenylene ether composite material, comprising the following steps:

[0013] 1000 parts of polyphenylene ether, 100-200 parts of high-impact polystyrene, 200-800 parts of soda lime borosilicate hollow glass microspheres, 2-10 parts of an antioxidant, and 60-100 parts of polytetrafluoroethylene wax are uniformly mixed to obtain a mixture; the mixture is added to an extruder for melt extrusion to obtain a target product. Preferably, the temperature settings of the extruder zones are 200-210°C, 250-260°C, 260-270°C, 270-280°C, 280-290°C, and 290-300°C, respectively.

[0014] Compared with the prior art, the present invention has the following beneficial effects:

[0015] The present invention adds high-impact polystyrene to the polyphenylene ether composite material, the main purpose of which is to increase the flowability and plasticizing effect of the polyphenylene ether composition.

[0016] The present invention adds polytetrafluoroethylene wax to the polyphenylene ether composite material, which not only further enhances the fluidity and plasticizing effect of the composition, improves its processing and mechanical properties, but also further reduces the dielectric constant of the composite material.

[0017] Compared with talc, calcium carbonate and borosilicate hollow glass microspheres, the addition of soda lime borosilicate hollow glass microspheres in the present invention can further improve the tensile and impact resistance of the composite material and significantly reduce the dielectric constant of the composite material. DETAILED DESCRIPTION

[0018] The following examples are given to specifically describe the present invention. It is necessary to point out that the following examples are only used to further illustrate the present invention and are not to be construed as limiting the scope of protection of the present invention. Any non-essential improvements or adjustments made to the present invention by a person of ordinary skill in the art based on the examples still fall within the scope of protection of the present invention.

[0019] The material models and manufacturers of the comparative examples of the present invention are as follows:

[0020] Polyphenylene ether is Asahi Kasei 340Z from Japan;

[0021] The high-impact polystyrene was BASF-Yangtze 2710, and the melt index was 5 g / 10 min (200° C., 5 kg).

[0022] Soda lime borosilicate hollow glass microspheres, brand K20, particle size 25 μm, density 0.2 g / cc, from 3M Company, USA.

[0023] Borosilicate hollow glass microspheres, particle size 25 μm, density 0.2 g / cc, Hebei Jiegui Mineral Products Co., Ltd.

[0024] The particle size of talcum powder and calcium carbonate is 2000 mesh, Changxing Huayang Plastic Material Co., Ltd.

[0025] The antioxidant is a mixture of antioxidant 1010 and antioxidant 168 in a mass ratio of 1:1, a product of BASF, Germany;

[0026] The polytetrafluoroethylene wax was Clariant 9322F.

[0027] The present invention will be further described below with reference to the examples.

[0028] Example 1

[0029] A preparation method of a polyphenylene ether composite material comprises the following steps: adding 1000 parts of polyphenylene ether, 200 parts of high-impact polystyrene, 800 parts of soda lime borosilicate hollow glass microspheres, 10 parts of an antioxidant and 100 parts of polytetrafluoroethylene wax into a high-speed mixer, mixing them evenly and then adding them into an extruder, and melt-extruding them through the extruder to obtain a product; the temperature of each zone of the extruder is 210° C., 260° C., 270° C., 280° C., 290° C. and 300° C.

[0030] Example 2

[0031] A preparation method of a polyphenylene ether composite material comprises the following steps: adding 1000 parts of polyphenylene ether, 180 parts of high-impact polystyrene, 600 parts of soda lime borosilicate hollow glass microspheres, 8 parts of an antioxidant and 80 parts of polytetrafluoroethylene wax into a high-speed mixer, mixing them evenly and then adding them into an extruder, and melt-extruding them through the extruder to obtain a product; the temperature of each zone of the extruder is 210° C., 250° C., 260° C., 270° C., 280° C. and 290° C.

[0032] Example 3

[0033] A preparation method of a polyphenylene ether composite material comprises the following steps: adding 1000 parts of polyphenylene ether, 150 parts of high-impact polystyrene, 400 parts of soda lime borosilicate hollow glass microspheres, 4 parts of an antioxidant and 60 parts of polytetrafluoroethylene wax into a high-speed mixer, mixing them evenly, adding them into an extruder, and melt-extruding them through the extruder to obtain a product; the temperatures of the various zones of the extruder are 200° C., 260° C., 270° C., 280° C., 290° C. and 300° C.

[0034] Example 4

[0035] A preparation method of a polyphenylene ether composite material comprises the following steps: adding 1000 parts of polyphenylene ether, 100 parts of high-impact polystyrene, 200 parts of soda lime borosilicate hollow glass microspheres, 2 parts of an antioxidant and 60 parts of polytetrafluoroethylene wax into a high-speed mixer, mixing them evenly and then adding them into an extruder, and melt-extruding them through the extruder to obtain a product; the temperature of each zone of the extruder is 200° C., 250° C., 260° C., 270° C., 280° C. and 290° C.

[0036] Example 5

[0037] A preparation method of a polyphenylene ether composite material comprises the following steps: adding 1000 parts of polyphenylene ether, 120 parts of high-impact polystyrene, 500 parts of soda lime borosilicate hollow glass microspheres, 5 parts of an antioxidant and 70 parts of polytetrafluoroethylene wax into a high-speed mixer, mixing them evenly and then adding them into an extruder, and melt-extruding them through the extruder to obtain a product; the temperature of each zone of the extruder is 200°C, 250°C, 260°C, 270°C, 280°C and 290°C.

[0038] Comparative Example 1

[0039] A preparation method of a polyphenylene ether composite material comprises the following steps: adding 1000 parts of polyphenylene ether, 190 parts of high-impact polystyrene, 500 parts of soda lime borosilicate hollow glass microspheres and 5 parts of an antioxidant into a high-speed mixer, mixing them evenly and then adding them into an extruder, and melt-extruding them through the extruder to obtain a product; the temperature of each zone of the extruder is 200°C, 250°C, 260°C, 270°C, 280°C and 290°C.

[0040] Comparative Example 2

[0041] A preparation method of a polyphenylene ether composite material comprises the following steps: adding 1000 parts of polyphenylene ether, 120 parts of high-impact polystyrene, 500 parts of borosilicate hollow glass microspheres, 5 parts of antioxidant and 70 parts of polytetrafluoroethylene wax into a high-speed mixer, mixing them evenly and then adding them into an extruder, and melt-extruding them through the extruder to obtain a product; the temperature of each zone of the extruder is 200°C, 250°C, 260°C, 270°C, 280°C and 290°C.

[0042] Comparative Example 3

[0043] A preparation method of a polyphenylene ether composite material comprises the following steps: adding 1000 parts of polyphenylene ether, 120 parts of high-impact polystyrene, 500 parts of talc, 5 parts of antioxidant and 70 parts of polytetrafluoroethylene wax into a high-speed mixer, mixing them evenly and then adding them into an extruder, and melt-extruding them through the extruder to obtain a product; the temperature of each zone of the extruder is 200°C, 250°C, 260°C, 270°C, 280°C and 290°C.

[0044] Comparative Example 4

[0045] A preparation method of a polyphenylene ether composite material comprises the following steps: adding 1000 parts of polyphenylene ether, 120 parts of high-impact polystyrene, 500 parts of calcium carbonate, 5 parts of an antioxidant and 70 parts of polytetrafluoroethylene wax into a high-speed mixer, mixing them evenly and then adding them into an extruder, and melt-extruding them through the extruder to obtain a product; the temperature of each zone of the extruder is 200°C, 250°C, 260°C, 270°C, 280°C and 290°C.

[0046] Performance testing method:

[0047] The performance of the composite material prepared by the present invention was tested, and the relevant test conditions were as follows:

[0048] The tensile strength was tested according to ASTM D638. The test specimen was dumbbell-shaped with dimensions (length × width × thickness) of 170 mm × 13 mm × 3.2 mm. The tensile speed was 5 mm / min.

[0049] The simply supported beam notched impact strength is tested according to the standard ASTM D6110-2018. The test specimen size (length × width × thickness) is 127mm × 13mm × 3.2mm, with a V-notch and a notch depth of 1 / 5.

[0050] The dielectric constant test specimen has a size of 8 mm × 3.2 mm × 1.6 mm. Silver electrodes are evenly coated on the surface of the test specimen before the dielectric constant test is performed. The test is carried out in accordance with GB / T 1409-2006 at a test frequency of 1 MHz.

[0051] The performance test results of the products obtained in each embodiment and comparative example are shown in Table 1

[0052] Table 1 Performance test results of the products obtained in various embodiments and comparative examples

[0053] Test items Tensile strength (MPa) <![CDATA[Notched Izod impact strength of simply supported beam (kJ / m 2 )]]> Dielectric constant Example 1 71.9 19.8 1.9 Example 2 71.3 21.3 1.9 Example 3 69.4 18.9 2.0 Example 4 65.6 17.5 2.3 Example 5 71.2 22.1 1.9 Comparative Example 1 63.5 21.1 2.7 Comparative Example 2 64.7 16.8 3.8 Comparative Example 3 62.3 12.2 5.9 Comparative Example 4 63.8 13.9 4.5

[0054] It can be seen from the above data that the addition of polytetrafluoroethylene wax to the composite material of the present invention can not only enhance the fluidity and plasticizing effect of the composition, improve its processing and mechanical properties, but also further reduce the dielectric constant of the composite material.

[0055] Compared with talc, calcium carbonate and borosilicate hollow glass microspheres, the addition of soda lime borosilicate hollow glass microspheres in the present invention can further improve the tensile and impact resistance of the composite material and significantly reduce the dielectric constant of the composite material.

[0056] It should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention, rather than to limit it. Although the present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that they can still modify the technical solutions described in the aforementioned embodiments, or make equivalent replacements for some of the technical features therein. However, these modifications or replacements do not deviate the essence of the corresponding technical solutions from the spirit and scope of the technical solutions of the various embodiments of the present invention.

Claims

1. A polyphenylene ether composite material, characterized in that: It is prepared from the following components in parts by weight: 1000 parts of polyphenylene ether, High impact polystyrene 120-200 parts, 70-100 parts of polytetrafluoroethylene wax, 500-800 parts of soda lime borosilicate hollow glass microspheres, 5-10 parts of antioxidant; The antioxidant is a mixture of antioxidant 1010 and antioxidant 168.

2. The polyphenylene ether composite material according to claim 1, characterized in that: The high-impact polystyrene has a melt index of 3-10 g / 10 min at 200° C. and 5 kg.

3. The polyphenylene ether composite material according to claim 1, characterized in that: The soda lime borosilicate hollow glass microspheres are in a hollow state, have a density of 0.1-0.3 g / cc, and a particle size of 20-30 μm.

4. The polyphenylene ether composite material according to claim 1, characterized in that: The mass ratio of the antioxidant 1010 to the antioxidant 168 in the mixture is 1:

1.

5. The method for preparing the polyphenylene ether composite material according to any one of claims 1 to 4, wherein: The following steps are involved: Polyphenylene ether, high-impact polystyrene, soda lime borosilicate hollow glass microspheres, antioxidant and polytetrafluoroethylene wax are uniformly mixed to obtain a mixture; the mixture is added into an extruder for melt extrusion to obtain a target product.

6. The method for preparing the polyphenylene ether composite material according to claim 5, wherein: The temperature settings of each zone of the extruder are 200-210°C, 250-260°C, 260-270°C, 270-280°C, 280-290°C, and 290-300°C, respectively.

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