CN111117203A - Conductive, high-mechanical-property and low-warpage fiber-reinforced polyphenyl ether composite material and preparation method thereof - Google Patents
Conductive, high-mechanical-property and low-warpage fiber-reinforced polyphenyl ether composite material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a conductive, high-mechanical-property and low-warpage fiber reinforced polyphenyl ether composite material and a preparation method thereof; the polyphenyl ether composite material comprises the following components in parts by weight: 50-90% of polyphenyl ether resin, and polystyrene: 10-40% of flat carbon fiber, 10-40% of compatilizer and 0.1-1% of antioxidant. Compared with the common carbon fiber reinforced polyphenyl ether composite material with a circular cross section in the current market, the flat carbon fiber reinforced polyphenyl ether composite material has the excellent performances of stable size and low warpage while keeping higher mechanical property and electrical conductivity, improves the application additional value of the polyphenyl ether composite material, and can be used in the fields of IC trays and the like with higher requirements on flatness.
Description
Technical Field
The invention relates to the field of engineering plastics, in particular to a conductive, high-rigidity and low-warpage polyphenylene oxide composite material and a preparation method thereof.
Background
Polyphenyl ether is one of five engineering plastics, and has the advantages of good mechanical property, heat resistance, electrical property, dimensional stability and the like.
Materials used for semiconductor chip trays, integrated circuit trays and electronic tooling must have the characteristics of excellent mechanical properties, good static electricity dissipation capability, high heat resistance, dimensional stability, low warpage and the like. The polyphenyl ether material has the advantages of high heat resistance, dimensional stability and the like, is one of the materials selected for the semiconductor tray material, and in order to enable the polyphenyl ether material to have good static dissipation capability, the general method is to add conductive carbon black, carbon nano tubes, graphene and the like into the polyphenyl ether material. The polyphenyl ether material is filled with the carbon fibers, so that the problem of static dissipation is solved, the mechanical property of the polyphenyl ether composite material is improved, but the tray prepared from the conventional carbon fiber reinforced polyphenyl ether composite material is large in warping degree and meets the requirements of customers.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention provides a conductive, high-mechanical-property and low-warpage fiber reinforced polyphenyl ether composite material and a preparation method thereof.
The technical scheme adopted by the invention for solving the technical problems is as follows:
the conductive, high-mechanical-property and low-warpage fiber reinforced polyphenyl ether composite material is prepared from the following raw materials in percentage by weight:
polyphenylene ether: 50-90%;
polystyrene: 10-40%;
flat carbon fibers: 10-40%;
a compatilizer: 0 to 10 percent;
antioxidant: 0.1 to 1 percent.
The polyphenyl ether is linear high molecular weight polyphenyl thioether with molecular weight of 3-4.5 ten thousand and melt index of 10-40g/10min at 280 deg.c and 5 kg.
The polystyrene resin is one or a mixture of two of polystyrene and high impact polystyrene;
the surface of the flat carbon fiber is subjected to sizing and silanization treatment, the length of the flat carbon fiber is 6mm, and the bulk density is more than 300 g/L. The preparation method of the flat carbon fiber comprises the following steps: preparing polyacrylonitrile spinning solution, filtering and metering the demonomerized and defoamed polyacrylonitrile spinning solution, extruding the solution through a spinning nozzle to form a spinning trickle, wherein the spinning nozzle used in the production process is a rectangular nozzle combined spinning nozzle, the shape of the nozzle of a spinning nozzle cap is rectangular, the length-width ratio of the nozzle is 4:1, then the spinning dope enters a coagulating bath to be coagulated and formed, and is subjected to drafting, washing, drying and densification to obtain flat polyacrylonitrile precursor for high-performance carbon fibers, the flat polyacrylonitrile precursor is oxidized, carbonized at low temperature and carbonized at high temperature, then subjected to sizing and silanization treatment and then wound to obtain flat carbon fibers, and then the flat carbon fibers are cut into short flat carbon fibers with the thickness of 6mm, the stacking density of the short flat carbon fibers is greater than 300g/L, and the flat carbon fibers provided by a;
the compatilizer is one or more of SEBS-g-MAH, PPE-g-MAH and the like serving as the toughening agent.
The antioxidant is prepared by compounding an antioxidant 1010 and an antioxidant 168 according to the proportion of 1: 2.
The preparation method of the fiber reinforced polyphenyl ether composite material with low warpage, conductivity and high mechanical property comprises the following steps:
1) weighing the raw materials according to the weight ratio;
2) putting the raw materials except the flat carbon fibers into a high-speed mixer for dry mixing for 3-5 min;
3) feeding the substance obtained in the step 2) into a double-screw extruder through a main feeder, and adding carbon fibers into a side feeding port of the double-screw extruder;
4) extruding, cooling, granulating and drying the substance obtained in the step 3), wherein the rotating speed of a double-screw extruder is 300-400 r.p.m; the temperature of each section of the double-screw extruder is 220-310 ℃.
The invention has the advantages that:
according to the invention, the carbon fiber with a flat section is used for the modified polyphenyl ether composite material, and compared with the carbon fiber modified polyphenyl ether composite material with a round section, the product has the advantages of better dimensional stability, lower warping degree and more excellent flatness.
Detailed Description
The technical features of the present invention will be further described with reference to the following embodiments.
In the embodiment of the invention, polyphenylene oxide (PPO) is a PPO material of the Chinese Lanxinus group, and the brand number of the PPO material is LXR 040; the flat carbon fiber has a tensile strength of 4.0GPa and a tensile modulus of 230GPa in bulkThe bulk density was 350g/l, the tensile strength was 4.0GPa, the tensile modulus was 230GPa, and the density was 1.78g/cm3Supplied by the high performance laboratory of the university of east China; the chopped carbon fiber (short for circular carbon fiber) with the circular cross-sectional shape of the carbon fiber is a chopped round rod-shaped carbon fiber with the length of 6mm provided by Korean TYM company, and has the tensile strength of 4.0GPa, the tensile modulus of 230GPa and the density of 1.78g/cm3The bulk density is 350 g/L; the polystyrene is high impact resistant polystyrene. The compatilizer is PPE-g-MAH, and the grafting rate is more than 1.5 percent; the antioxidant is 1010 and the antioxidant 168 according to the weight ratio of 1:2, compounding in proportion.
Example 1:
(1) weighing 66.7% of polyphenyl ether, 20% of high impact polystyrene, 3% of compatilizer PPE-g-MAH and 0.3% of 1010 and 168 compound antioxidant according to the weight ratio;
(2) the raw materials are put into a high-speed mixer to be blended for 5 minutes and then are added from the main feeding port of a double-screw extruder.
(3) Adding 10% by weight of flat carbon fibers from a double-screw side feeding port.
(4) Extruding and granulating the materials by a double-screw extruder, wherein the temperature zone of the double-screw extruder is as follows: the temperature of the first zone is 190-250 ℃, the temperature of the second zone is 220-270 ℃, the temperature of the third zone is 270-300 ℃, the temperature of the fourth zone is 270-300 ℃, the temperature of the fifth zone is 270-300 ℃, the temperature of the sixth zone is 270-300 ℃, the temperature of the seventh zone is 270-300 ℃, the temperature of the eighth zone is 270-300 ℃, the temperature of the ninth zone is 270-300 ℃, the temperature of the machine head is 290-310 ℃, the rotating speed is 380r.p.m, and the mixture is subjected to composite treatment such as shearing, melting and the like in a double screw extruder.
(5) And (4) extruding, cooling, granulating and drying the substance obtained in the step (4).
Example 2:
(1) weighing 61.7 percent of polyphenyl ether, 20 percent of high impact polystyrene, 3 percent of compatilizer PPE-g-MAH and 0.3 percent of 1010 and 168 compound antioxidant according to the weight ratio;
(2) the raw materials are put into a high-speed mixer to be blended for 5 minutes and then are added from the main feeding port of a double-screw extruder.
(3) 15% by weight of flat carbon fibers were added from a feed inlet on the side of the twin screw.
(4) Extruding and granulating the materials by a double-screw extruder, wherein the temperature zone of the double-screw extruder is as follows: the temperature of the first zone is 190-250 ℃, the temperature of the second zone is 220-270 ℃, the temperature of the third zone is 270-300 ℃, the temperature of the fourth zone is 270-300 ℃, the temperature of the fifth zone is 270-300 ℃, the temperature of the sixth zone is 270-300 ℃, the temperature of the seventh zone is 270-300 ℃, the temperature of the eighth zone is 270-300 ℃, the temperature of the ninth zone is 270-300 ℃, the temperature of the machine head is 290-310 ℃, the rotating speed is 380r.p.m, and the mixture is subjected to composite treatment such as shearing, melting and the like in a double-screw extruder;
(5) and (4) extruding, cooling, granulating and drying the substance obtained in the step (4).
Example 3:
(1) weighing 56.7 percent of polyphenyl ether, 20 percent of high impact resistant polystyrene, 3 percent of compatilizer PPE-g-MAH and 0.3 percent of 1010 and 168 compound antioxidant according to the weight ratio;
(2) the raw materials are put into a high-speed mixer to be blended for 5 minutes and then are added from the main feeding port of a double-screw extruder.
(3) 20% by weight of flat carbon fibers were fed through a twin-screw side feed port.
(4) Extruding and granulating the materials by a double-screw extruder, wherein the temperature zone of the double-screw extruder is as follows: the temperature of the first zone is 190-250 ℃, the temperature of the second zone is 220-270 ℃, the temperature of the third zone is 270-300 ℃, the temperature of the fourth zone is 270-300 ℃, the temperature of the fifth zone is 270-300 ℃, the temperature of the sixth zone is 270-300 ℃, the temperature of the seventh zone is 270-300 ℃, the temperature of the eighth zone is 270-300 ℃, the temperature of the ninth zone is 270-300 ℃, the temperature of the machine head is 290-310 ℃, the rotating speed is 380r.p.m, and the mixture is subjected to composite treatment such as shearing, melting and the like in a double screw extruder.
(5) And (4) extruding, cooling, granulating and drying the substance obtained in the step (4).
Example 4:
(1) weighing 51.7% of polyphenyl ether, 20% of high impact polystyrene, 3% of compatilizer PPE-g-MAH and 0.3% of 1010 and 168 compound antioxidant according to the weight ratio;
(2) the raw materials are put into a high-speed mixer to be blended for 5 minutes and then are added from the main feeding port of a double-screw extruder.
(3) Adding 25% by weight of flat carbon fibers from a double-screw side feeding port.
(4) Extruding and granulating the materials by a double-screw extruder, wherein the temperature zone of the double-screw extruder is as follows: the temperature of the first zone is 190-250 ℃, the temperature of the second zone is 220-270 ℃, the temperature of the third zone is 270-300 ℃, the temperature of the fourth zone is 270-300 ℃, the temperature of the fifth zone is 270-300 ℃, the temperature of the sixth zone is 270-300 ℃, the temperature of the seventh zone is 270-300 ℃, the temperature of the eighth zone is 270-300 ℃, the temperature of the ninth zone is 270-300 ℃, the temperature of the machine head is 290-310 ℃, the rotating speed is 380r.p.m, and the mixture is subjected to composite treatment such as shearing, melting and the like in a double screw extruder.
(5) And (4) extruding, cooling, granulating and drying the substance obtained in the step (4).
Example 5:
(1) weighing 46.7 percent of polyphenyl ether, 20 percent of high impact polystyrene, 3 percent of compatilizer PPE-g-MAH and 0.3 percent of 1010 and 168 compound antioxidant according to the weight ratio;
(2) the raw materials are put into a high-speed mixer to be blended for 5 minutes and then are added from the main feeding port of a double-screw extruder.
(3) 30% by weight of flat carbon fibers were fed through a double-screw side feed port.
(4) Extruding and granulating the materials by a double-screw extruder, wherein the temperature zone of the double-screw extruder is as follows: the temperature of the first zone is 190-250 ℃, the temperature of the second zone is 220-270 ℃, the temperature of the third zone is 270-300 ℃, the temperature of the fourth zone is 270-300 ℃, the temperature of the fifth zone is 270-300 ℃, the temperature of the sixth zone is 270-300 ℃, the temperature of the seventh zone is 270-300 ℃, the temperature of the eighth zone is 270-300 ℃, the temperature of the ninth zone is 270-300 ℃, the temperature of the machine head is 290-310 ℃, the rotating speed is 380r.p.m, and the mixture is subjected to composite treatment such as shearing, melting and the like in a double screw extruder.
(5) And (4) extruding, cooling, granulating and drying the substance obtained in the step (4).
Comparative example 1:
(1) weighing 66.7% of polyphenyl ether, 20% of high impact polystyrene, 3% of compatilizer PPE-g-MAH and 0.3% of 1010 and 168 compound antioxidant according to the weight ratio;
(2) the raw materials are put into a high-speed mixer to be blended for 5 minutes and then are added from the main feeding port of a double-screw extruder.
(3) Adding 10% of round carbon fiber by weight into the double-screw side feeding port.
(4) Extruding and granulating the materials by a double-screw extruder, wherein the temperature zone of the double-screw extruder is as follows: the temperature of the first zone is 190-250 ℃, the temperature of the second zone is 220-270 ℃, the temperature of the third zone is 270-300 ℃, the temperature of the fourth zone is 270-300 ℃, the temperature of the fifth zone is 270-300 ℃, the temperature of the sixth zone is 270-300 ℃, the temperature of the seventh zone is 270-300 ℃, the temperature of the eighth zone is 270-300 ℃, the temperature of the ninth zone is 270-300 ℃, the temperature of the machine head is 290-310 ℃, the rotating speed is 380r.p.m, and the mixture is subjected to composite treatment such as shearing, melting and the like in a double screw extruder.
(5) And (4) extruding, cooling, granulating and drying the substance obtained in the step (4).
Comparative example 2:
(1) weighing 61.7 percent of polyphenyl ether, 20 percent of high impact polystyrene, 3 percent of compatilizer PPE-g-MAH and 0.3 percent of 1010 and 168 compound antioxidant according to the weight ratio;
(2) the raw materials are put into a high-speed mixer to be blended for 5 minutes and then are added from the main feeding port of a double-screw extruder.
(3) Adding 15% by weight of round carbon fiber from a feeding port at the side of the double screw.
(4) Extruding and granulating the materials by a double-screw extruder, wherein the temperature zone of the double-screw extruder is as follows: the temperature of the first zone is 190-250 ℃, the temperature of the second zone is 220-270 ℃, the temperature of the third zone is 270-300 ℃, the temperature of the fourth zone is 270-300 ℃, the temperature of the fifth zone is 270-300 ℃, the temperature of the sixth zone is 270-300 ℃, the temperature of the seventh zone is 270-300 ℃, the temperature of the eighth zone is 270-300 ℃, the temperature of the ninth zone is 270-300 ℃, the temperature of the machine head is 290-310 ℃, the rotating speed is 380r.p.m, and the mixture is subjected to composite treatment such as shearing, melting and the like in a double-screw extruder;
(5) and (4) extruding, cooling, granulating and drying the substance obtained in the step (4).
Comparative example 3:
(1) weighing 56.7 percent of polyphenyl ether, 20 percent of high impact resistant polystyrene, 3 percent of compatilizer PPE-g-MAH and 0.3 percent of 1010 and 168 compound antioxidant according to the weight ratio;
(2) the raw materials are put into a high-speed mixer to be blended for 5 minutes and then are added from the main feeding port of a double-screw extruder.
(3) 20 percent of round carbon fiber by weight is added from a feeding port at the side of the double screw.
(4) Extruding and granulating the materials by a double-screw extruder, wherein the temperature zone of the double-screw extruder is as follows: the temperature of the first zone is 190-250 ℃, the temperature of the second zone is 220-270 ℃, the temperature of the third zone is 270-300 ℃, the temperature of the fourth zone is 270-300 ℃, the temperature of the fifth zone is 270-300 ℃, the temperature of the sixth zone is 270-300 ℃, the temperature of the seventh zone is 270-300 ℃, the temperature of the eighth zone is 270-300 ℃, the temperature of the ninth zone is 270-300 ℃, the temperature of the machine head is 290-310 ℃, the rotating speed is 380r.p.m, and the mixture is subjected to composite treatment such as shearing, melting and the like in a double screw extruder.
(5) And (4) extruding, cooling, granulating and drying the substance obtained in the step (4).
Comparative example 4:
(1) weighing 51.7% of polyphenyl ether, 20% of high impact polystyrene, 3% of compatilizer PPE-g-MAH and 0.3% of 1010 and 168 compound antioxidant according to the weight ratio;
(2) the raw materials are put into a high-speed mixer to be blended for 5 minutes and then are added from the main feeding port of a double-screw extruder.
(3) Adding 25% round carbon fiber by weight into the double-screw side feeding port.
(4) Extruding and granulating the materials by a double-screw extruder, wherein the temperature zone of the double-screw extruder is as follows: the temperature of the first zone is 190-250 ℃, the temperature of the second zone is 220-270 ℃, the temperature of the third zone is 270-300 ℃, the temperature of the fourth zone is 270-300 ℃, the temperature of the fifth zone is 270-300 ℃, the temperature of the sixth zone is 270-300 ℃, the temperature of the seventh zone is 270-300 ℃, the temperature of the eighth zone is 270-300 ℃, the temperature of the ninth zone is 270-300 ℃, the temperature of the machine head is 290-310 ℃, the rotating speed is 380r.p.m, and the mixture is subjected to composite treatment such as shearing, melting and the like in a double screw extruder.
(5) And (4) extruding, cooling, granulating and drying the substance obtained in the step (4).
Comparative example 5:
(1) weighing 46.7 percent of polyphenyl ether, 20 percent of high impact polystyrene, 3 percent of compatilizer PPE-g-MAH and 0.3 percent of 1010 and 168 compound antioxidant according to the weight ratio;
(2) the raw materials are put into a high-speed mixer to be blended for 5 minutes and then are added from the main feeding port of a double-screw extruder.
(3) 30 percent of circular carbon fiber by weight is added from a feeding port at the side of the double screw.
(4) Extruding and granulating the materials by a double-screw extruder, wherein the temperature zone of the double-screw extruder is as follows: the temperature of the first zone is 190-250 ℃, the temperature of the second zone is 220-270 ℃, the temperature of the third zone is 270-300 ℃, the temperature of the fourth zone is 270-300 ℃, the temperature of the fifth zone is 270-300 ℃, the temperature of the sixth zone is 270-300 ℃, the temperature of the seventh zone is 270-300 ℃, the temperature of the eighth zone is 270-300 ℃, the temperature of the ninth zone is 270-300 ℃, the temperature of the machine head is 290-310 ℃, the rotating speed is 380r.p.m, and the mixture is subjected to composite treatment such as shearing, melting and the like in a double screw extruder.
(5) And (4) extruding, cooling, granulating and drying the substance obtained in the step (4).
Comparison of the performance tests was carried out on the samples prepared according to the examples and comparative examples, the tensile performance test being carried out according to ISO527-2, the test specimen size being 150 x 10 x 4mm, the tensile speed being 50 mm/min; bending performance testing was performed according to ISO 178, with a sample size of 80 x 10 x 4mm and a bending speed of 2 mm/min; impact strength of the simply supported beam was according to ISO 179, sample size 55 × 6 × 4; the melt flow index is tested according to ISO 1183 by adopting an ISO test standard, the surface resistance is tested by a quick 4990 surface resistance meter, the warpage is evaluated by a feeler gauge test, the test method comprises the steps of firstly beating a plate by a mould, wherein the size of the mould is 150mm x 100mm x 2mm, and the warpage is compared by a test plate at the same position. The test properties are shown in tables 1 and 2 below.
Table 1 shows the test data of examples 1 to 3 and comparative examples 1 to 3
As can be seen from the table, the mechanical property and the electrical conductivity of the polyphenylene ether reinforced by the flat carbon fibers are basically consistent with those of the polyphenylene ether reinforced by the round carbon fibers, but the warpage of the flat carbon fibers is obviously lower than that of the polyphenylene ether composite material prepared by the round carbon fibers, namely the flatness of the polyphenylene ether composite material plate reinforced by the flat carbon fibers is obviously better than that of the round carbon fibers.
The foregoing is a more detailed description of the invention in connection with specific preferred embodiments and is not intended to limit the invention. Several equivalent variations, which can be made by a person skilled in the art without departing from the inventive concept, are to be considered within the scope of the invention.
Claims (8)
1. A conductive, high-mechanical-property and low-warpage fiber reinforced polyphenyl ether composite material is characterized in that: the composite material consists of the following raw materials in percentage by weight:
polyphenylene ether: 50-90%;
polystyrene: 10-40%;
flat carbon fibers: 10-40%;
a compatilizer: 0 to 10 percent;
antioxidant: 0.1 to 1 percent.
2. The conductive, high mechanical property and low warpage fiber reinforced polyphenylene ether composite material according to claim 1, wherein: the polyphenyl ether is linear high molecular weight polyphenyl thioether with molecular weight of 3-4.5 ten thousand and melt index of 10-40g/10min at 280 deg.c and 5 kg.
3. The conductive, high mechanical property and low warpage fiber reinforced polyphenylene ether composite material according to claim 1, wherein: the polystyrene resin is one or a mixture of two of polystyrene and high impact polystyrene;
4. the conductive, high mechanical property and low warpage fiber reinforced polyphenylene ether composite material according to claim 1, wherein: the surface of the flat carbon fiber is subjected to sizing and silanization treatment, the length of the flat carbon fiber is 6mm, and the bulk density is more than 300 g/L.
5. The conductive, high mechanical property and low warpage fiber reinforced polyphenylene ether composite material according to claim 4, wherein: the preparation method of the flat carbon fiber comprises the following steps: preparing polyacrylonitrile spinning solution, filtering and metering the demonomerized and defoamed polyacrylonitrile spinning solution, extruding the solution through a spinning nozzle to form a spinning trickle, wherein the spinning nozzle used in the production process is a rectangular nozzle combined spinning nozzle, the shape of the nozzle of a spinning nozzle cap is rectangular, the length-width ratio of the nozzle is 4:1, then the spinning dope enters a coagulating bath to be coagulated and formed, and is subjected to drafting, washing, drying and densification to obtain flat polyacrylonitrile precursor for high-performance carbon fibers, the flat polyacrylonitrile precursor is oxidized, carbonized at low temperature and carbonized at high temperature, then subjected to sizing and silanization treatment and then wound to obtain flat carbon fibers, and then the flat carbon fibers are cut into short flat carbon fibers with the thickness of 6mm, the stacking density of the short flat carbon fibers is greater than 300g/L, and the flat carbon fibers provided by a;
6. the conductive, high mechanical property and low warpage fiber reinforced polyphenylene ether composite material according to claim 1, wherein: the compatilizer is one or more of SEBS-g-MAH, PPE-g-MAH and the like serving as the toughening agent.
7. The conductive, high mechanical property and low warpage fiber reinforced polyphenylene ether composite material according to claim 1, wherein: the antioxidant is prepared by compounding an antioxidant 1010 and an antioxidant 168 according to the proportion of 1: 2.
8. The method for preparing the conductive, high mechanical property and low warpage fiber reinforced polyphenylene ether composite material according to any one of claims 1 to 7, wherein: the method is characterized in that:
1) weighing the raw materials according to the weight ratio;
2) putting the raw materials except the flat carbon fibers into a high-speed mixer for dry mixing for 3-5 min;
3) feeding the substance obtained in the step 2) into a double-screw extruder through a main feeder, and adding carbon fibers into a side feeding port of the double-screw extruder;
4) extruding, cooling, granulating and drying the substance obtained in the step 3), wherein the rotating speed of a double-screw extruder is 300-400 r.p.m; the temperature of each section of the double-screw extruder is 220-310 ℃.
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