CN111286155A - Heat-conducting, electromagnetic-shielding and high-strength PEEK composite material and preparation method thereof - Google Patents
Heat-conducting, electromagnetic-shielding and high-strength PEEK composite material and preparation method thereof Download PDFInfo
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- 239000004696 Poly ether ether ketone Substances 0.000 title claims abstract description 67
- 229920002530 polyetherether ketone Polymers 0.000 title claims abstract description 67
- 239000002131 composite material Substances 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- JUPQTSLXMOCDHR-UHFFFAOYSA-N benzene-1,4-diol;bis(4-fluorophenyl)methanone Chemical compound OC1=CC=C(O)C=C1.C1=CC(F)=CC=C1C(=O)C1=CC=C(F)C=C1 JUPQTSLXMOCDHR-UHFFFAOYSA-N 0.000 title claims abstract 15
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 37
- 229920000049 Carbon (fiber) Polymers 0.000 claims abstract description 36
- 239000004917 carbon fiber Substances 0.000 claims abstract description 36
- 239000011812 mixed powder Substances 0.000 claims abstract description 29
- 229910052790 beryllium Inorganic materials 0.000 claims abstract description 27
- ATBAMAFKBVZNFJ-UHFFFAOYSA-N beryllium atom Chemical compound [Be] ATBAMAFKBVZNFJ-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000011858 nanopowder Substances 0.000 claims abstract description 27
- 239000004065 semiconductor Substances 0.000 claims abstract description 27
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000000843 powder Substances 0.000 claims abstract description 19
- 229910000859 α-Fe Inorganic materials 0.000 claims abstract description 17
- 239000007822 coupling agent Substances 0.000 claims abstract description 16
- 238000002156 mixing Methods 0.000 claims abstract description 14
- 238000001125 extrusion Methods 0.000 claims abstract description 13
- 238000005469 granulation Methods 0.000 claims abstract description 11
- 230000003179 granulation Effects 0.000 claims abstract description 11
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 10
- 239000000853 adhesive Substances 0.000 claims description 7
- 230000001070 adhesive effect Effects 0.000 claims description 7
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 6
- 229910000906 Bronze Inorganic materials 0.000 claims description 5
- 239000010974 bronze Substances 0.000 claims description 5
- 229910017052 cobalt Inorganic materials 0.000 claims description 5
- 239000010941 cobalt Substances 0.000 claims description 5
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 5
- KUNSUQLRTQLHQQ-UHFFFAOYSA-N copper tin Chemical compound [Cu].[Sn] KUNSUQLRTQLHQQ-UHFFFAOYSA-N 0.000 claims description 5
- 229910052759 nickel Inorganic materials 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 5
- AMGQUBHHOARCQH-UHFFFAOYSA-N indium;oxotin Chemical compound [In].[Sn]=O AMGQUBHHOARCQH-UHFFFAOYSA-N 0.000 claims description 4
- 229920000604 Polyethylene Glycol 200 Polymers 0.000 claims description 3
- 229920002556 Polyethylene Glycol 300 Polymers 0.000 claims description 3
- 238000000034 method Methods 0.000 claims description 3
- 239000011787 zinc oxide Substances 0.000 claims description 3
- SKRWFPLZQAAQSU-UHFFFAOYSA-N stibanylidynetin;hydrate Chemical compound O.[Sn].[Sb] SKRWFPLZQAAQSU-UHFFFAOYSA-N 0.000 claims 1
- 239000004697 Polyetherimide Substances 0.000 description 26
- 229920001601 polyetherimide Polymers 0.000 description 26
- 239000000463 material Substances 0.000 description 9
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- 239000011347 resin Substances 0.000 description 4
- 229920001223 polyethylene glycol Polymers 0.000 description 3
- XXLJGBGJDROPKW-UHFFFAOYSA-N antimony;oxotin Chemical compound [Sb].[Sn]=O XXLJGBGJDROPKW-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- -1 polytetrafluoroethylene Polymers 0.000 description 2
- 238000005452 bending Methods 0.000 description 1
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- 238000010292 electrical insulation Methods 0.000 description 1
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- 239000000835 fiber Substances 0.000 description 1
- 239000003365 glass fiber Substances 0.000 description 1
- 230000009477 glass transition Effects 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 239000012761 high-performance material Substances 0.000 description 1
- 125000005462 imide group Chemical group 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 150000002484 inorganic compounds Chemical class 0.000 description 1
- 239000012784 inorganic fiber Substances 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000010954 inorganic particle Substances 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 229920006260 polyaryletherketone Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000010094 polymer processing Methods 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 229920005992 thermoplastic resin Polymers 0.000 description 1
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
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- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
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Abstract
The invention relates to a heat-conducting, electromagnetic-shielding and high-strength PEEK composite material which comprises the following components in parts by weight: 50-90 parts of PEEK, 0.5-10 parts of beryllium bronze powder, 2-10 parts of ferrite powder, 0.5-5 parts of semiconductor nano powder and 10-50 parts of PEI-based long carbon fiber; the preparation method comprises the following steps: (1) mixing beryllium bronze powder, ferrite powder and semiconductor nano powder in proportion to form mixed powder, adding a coupling agent into the mixed powder, and continuously and uniformly mixing to form modified mixed powder for later use; (2) and (2) adding PEEK into a main feeding port of a double-screw extruder, adding the modified mixed powder obtained in the step (1) into a side feeding port, adding PEI-based long carbon fiber into an exhaust port, and performing extrusion granulation to obtain the heat-conducting, electromagnetic shielding and high-strength PEEK composite material. The PEEK composite material has good heat conduction and electromagnetic shielding performance and high mechanical strength.
Description
Technical Field
The invention relates to the technical field of polymer processing, in particular to a heat-conducting, electromagnetic-shielding and high-strength PEEK composite material and a preparation method thereof.
Background
Polyether ether ketone (PEEK) is the most representative one of polyarylether ketone polymers, and is thermoplastic resin with the best comprehensive performance. It has outstanding mechanical performance and very good performances in the aspects of high temperature resistance, corrosion resistance, flame retardance, irradiation resistance, electrical insulation and the like. Although the PEEK resin has excellent high temperature resistance, the glass transition temperature (143 ℃) of the PEEK resin is relatively low, the heat distortion temperature of pure resin is only 160 ℃, the wide application of the PEEK resin is limited, and the mechanical property of the PEEK material can be enhanced by utilizing glass fiber, carbon fiber, short carbon fiber, polytetrafluoroethylene, various whiskers or inorganic compounds, so that the properties of the PEEK material, such as the use temperature, the modulus, the strength, the dimensional stability and the like, can be improved. With the continuous development of science and technology and the continuous expansion of the demand of high-performance materials, the global yield of PEEK materials is rapidly expanded, and the PEEK materials are applied to the fields of automobiles, machining, aerospace, biomedical treatment and electronic and electrical appliances.
In order to improve the comprehensive performance of PEEK, in practical application, PEEK materials are mostly blended with other inorganic particles or fibers to prepare composite materials, and the preparation process of the common PEEK composite materials includes: melt blending, solution blending, in situ polymerization, and the like.
In the existing aviation field, the chassis equipment and the like need to have better heat dissipation and electromagnetic shielding performance, and the PEEK is used as a main material in the field, so that the defects of poor heat conductivity and poor electromagnetic shielding performance inevitably occur.
Disclosure of Invention
In order to solve the technical problems of poor heat conductivity and poor electromagnetic shielding property of the PEEK material, the PEEK composite material with heat conductivity, electromagnetic shielding property and high strength and the preparation method thereof are provided. The PEEK composite material prepared by the method has good heat conduction and electromagnetic shielding performance and high mechanical strength.
A heat-conducting, electromagnetic-shielding and high-strength PEEK composite material comprises the following components in parts by weight: 50-90 parts of PEEK, 0.5-10 parts of beryllium bronze powder, 2-10 parts of ferrite powder, 0.5-5 parts of semiconductor nano powder and 10-50 parts of PEI-based long carbon fiber.
Furthermore, the beryllium bronze powder contains 2 wt% of beryllium, 0.3 wt% of nickel, 0.3 wt% of cobalt and the balance of bronze.
Further, the average particle size of the semiconductor nano powder is 100nm to 500 nm.
Furthermore, the semiconductor nano powder is one or more of aluminum-doped zinc oxide, tin antimony oxide and indium tin oxide. The three semiconductor nano-powders have better electrical conductivity and thermal conductivity.
Further, the PEI-based long carbon fiber is a carbon fiber filament taking 0.3 wt% -1 wt% of PEI as an adhesive. The general carbon fiber is epoxy resin-based carbon fiber, namely the carbon fiber which is bonded by using epoxy resin as an adhesive, but the epoxy resin has poor high temperature resistance and is easy to decompose, and the compatibility of the epoxy resin and PEEK is poor, so that the epoxy resin-based carbon fiber inevitably used for reinforcing the PEEK has certain limitation, namely the reinforcing effect of the epoxy resin-based carbon fiber is limited; however, PEI (polyetherimide) is used as an adhesive, and PEEK (polyether ether ketone) is completely compatible with PEI, so that on one hand, carbon fiber filaments have a reinforcing effect, and on the other hand, the crystallinity of PEEK is improved due to the complete compatibility of PEI on the carbon fiber filaments and PEEK, and the PEI has a certain reinforcing effect on the tensile strength and the impact strength of PEEK. This makes PEEK fully compatible with PEI due to the dominant force of the imide group of PEI interacting with the phenyl group of PEEK.
The invention provides a preparation method of a heat-conducting, electromagnetic-shielding and high-strength PEEK composite material, which comprises the following steps:
(1) mixing beryllium bronze powder, ferrite powder and semiconductor nano powder in proportion to form mixed powder, adding a coupling agent into the mixed powder, and continuously and uniformly mixing to form modified mixed powder for later use;
(2) and (2) adding PEEK into a main feeding port of a double-screw extruder, adding the modified mixed powder obtained in the step (1) into a side feeding port, adding PEI-based long carbon fiber into an exhaust port, and performing extrusion granulation to obtain the heat-conducting, electromagnetic shielding and high-strength PEEK composite material.
Further, the dosage of the coupling agent in the step (1) is 0.5-1.2% of the weight of the mixed powder, and the coupling agent is one of PEG-200, PEG-300 and PEG-500. Due to the electrostatic adsorption effect of the PEG, the powder material in the step (1) can be uniformly dispersed in the PEEK matrix, and due to the small molecular weight of the PEG, the PEG can be decomposed during extrusion, so that the performance of the PEEK material is not affected basically.
Further, in the step (2), the feeding frequency of the main feeding port is 5Hz to 20Hz, the feeding frequency of the side feeding port is 1Hz to 5Hz, and the screw rotating speed of the double-screw extruder is 250rpm to 350 rpm.
Further, the temperature of the first zone, the temperature of the second zone to the tenth zone and the temperature of the die in the extrusion granulation in the step (2) are respectively 250 +/-10 ℃, 370 +/-20 ℃.
The beneficial technical effects are as follows:
the added beryllium bronze powder and ferrite powder have good thermal conductivity, are beneficial to heat transmission of motors and chassis equipment in the aviation field during working, and avoid the problems of high working temperature and the like; in addition, the beryllium bronze powder and the ferrite powder have good conductivity and are used together with the semiconductor nano powder and the long carbon fiber, so that the prepared PEEK composite material has good conductivity, and the long carbon fiber forms carbon fiber with a certain length-diameter ratio in the screw extrusion process, and can build a three-dimensional conductive network structure together with the granular beryllium bronze powder and the semiconductor nano powder, so that the high conductivity can be exerted to the maximum extent; the ferrite powder has better magnetic conductivity, so that the prepared PEEK composite material has better magnetic conductivity; the performance of the PEEK composite material in the aspect of electromagnetic shielding can be improved, and 'invisibility' on electromagnetic signals is realized; the added PEI-based long carbon fiber not only can improve the thermal conductivity of the composite material, but also has the effect of improving the mechanical property of the composite material, and compared with fiber powder, the effect of improving is remarkable.
Detailed Description
The invention is further described below with reference to specific examples, but without limiting the scope of the invention.
Example 1
A heat-conducting, electromagnetic-shielding and high-strength PEEK composite material comprises the following components in parts by weight: 75.5 parts of PEEK, 3 parts of beryllium bronze powder, 3 parts of ferrite powder, 3.5 parts of semiconductor nano powder and 15 parts of PEI-based long carbon fiber;
wherein, the beryllium bronze powder contains 2 wt% of beryllium, 0.3 wt% of nickel, 0.3 wt% of cobalt and the balance of bronze; the average particle size of the semiconductor nano powder is 200-300 nm, and the semiconductor nano powder is tin antimony oxide; the PEI-based long carbon fiber is a carbon fiber filament taking 1 wt% of PEI as an adhesive.
The preparation method of the heat-conducting, electromagnetic-shielding and high-strength PEEK composite material comprises the following steps:
(1) mixing beryllium bronze powder, ferrite powder and semiconductor nano powder according to the proportion to form mixed powder, adding a coupling agent into the mixed powder, and continuously and uniformly mixing to form modified mixed powder for later use;
(2) and (2) adding PEEK into a main feeding port of a double-screw extruder, adding the modified mixed powder obtained in the step (1) into a side feeding port, adding PEI-based long carbon fiber into an exhaust port, and performing extrusion granulation to obtain the heat-conducting, electromagnetic shielding and high-strength PEEK composite material.
Wherein the dosage of the coupling agent in the step (1) is 1% of the weight of the mixed powder, and the coupling agent is PEG-300; in the step (2), the feeding frequency of the main feeding port is 15Hz, the feeding frequency of the side feeding port is 2Hz, and the rotating speed of a screw of the double-screw extruder is 320 rpm; temperature of each zone of extrusion granulation: the temperature of the first zone is 250 ℃, the temperature of the second zone to the tenth zone of the machine barrel is 360 ℃, and the temperature of the neck mold is 340 ℃.
Example 2
This example is prepared identically to example 1, except that: the composite material comprises, by weight, PEEK72 parts, beryllium bronze powder 4 parts, ferrite powder 4 parts, semiconductor nano powder 4 parts and PEI-based long carbon fiber 16 parts.
Example 3
This example is prepared identically to example 1, except that: the composite material comprises, by weight, PEEK75 parts, beryllium bronze powder 4 parts, ferrite powder 4 parts, semiconductor nano powder 2 parts and PEI-based long carbon fiber 14 parts.
Example 4
A heat-conducting, electromagnetic-shielding and high-strength PEEK composite material comprises the following components in parts by weight: 68 parts of PEEK, 1 part of beryllium bronze powder, 2 parts of ferrite powder, 2 parts of semiconductor nano powder and 27 parts of PEI-based long carbon fiber;
wherein, the beryllium bronze powder contains 2 wt% of beryllium, 0.3 wt% of nickel, 0.3 wt% of cobalt and the balance of bronze; the average particle size of the semiconductor nano powder is 100-300 nm, and the semiconductor nano powder is prepared from aluminum-doped zinc oxide and indium tin oxide according to the mass ratio of 2: 1; the PEI-based long carbon fiber is a carbon fiber filament taking 1 wt% of PEI as an adhesive.
The preparation method of the heat-conducting, electromagnetic-shielding and high-strength PEEK composite material comprises the following steps:
(1) mixing beryllium bronze powder, ferrite powder and semiconductor nano powder according to the proportion to form mixed powder, adding a coupling agent into the mixed powder, and continuously and uniformly mixing to form modified mixed powder for later use;
(2) and (2) adding PEEK into a main feeding port of a double-screw extruder, adding the modified mixed powder obtained in the step (1) into a side feeding port, adding PEI-based long carbon fiber into an exhaust port, and performing extrusion granulation to obtain the heat-conducting, electromagnetic shielding and high-strength PEEK composite material.
Wherein the dosage of the coupling agent in the step (1) is 0.8 percent of the weight of the mixed powder, and the coupling agent is PEG-500; in the step (2), the feeding frequency of the main feeding port is 20Hz, the feeding frequency of the side feeding port is 5Hz, and the rotating speed of a screw of the double-screw extruder is 350 rpm; the temperature of the first zone of the temperature of each zone for extrusion granulation is 260 ℃, the temperature of the second zone to the tenth zone of the cylinder temperature is 350 ℃, and the temperature of the neck mold is 350 ℃.
Example 5
A heat-conducting, electromagnetic-shielding and high-strength PEEK composite material comprises the following components in parts by weight: 65 parts of PEEK, 1 part of beryllium bronze powder, 3 parts of ferrite powder, 1 part of semiconductor nano powder and 30 parts of PEI-based long carbon fiber;
wherein, the beryllium bronze powder contains 2 wt% of beryllium, 0.3 wt% of nickel, 0.3 wt% of cobalt and the balance of bronze; the average particle size of the semiconductor nano powder is 200-500 nm, and the semiconductor nano powder is indium tin oxide; the PEI-based long carbon fiber is a carbon fiber filament taking 1 wt% of PEI as an adhesive.
The preparation method of the heat-conducting, electromagnetic-shielding and high-strength PEEK composite material comprises the following steps:
(1) mixing beryllium bronze powder, ferrite powder and semiconductor nano powder according to the proportion to form mixed powder, adding a coupling agent into the mixed powder, and continuously and uniformly mixing to form modified mixed powder for later use;
(2) and (2) adding PEEK into a main feeding port of a double-screw extruder, adding the modified mixed powder obtained in the step (1) into a side feeding port, adding PEI-based long carbon fiber into an exhaust port, and performing extrusion granulation to obtain the heat-conducting, electromagnetic shielding and high-strength PEEK composite material.
Wherein the dosage of the coupling agent in the step (1) is 1.2 percent of the weight of the mixed powder, and the coupling agent is PEG-200; in the step (2), the feeding frequency of the main feeding port is 10Hz, the feeding frequency of the side feeding port is 1Hz, and the rotating speed of a screw of the double-screw extruder is 280 rpm; the temperature of the first zone of the temperature of each zone for extrusion granulation is 250 ℃, the temperature of the second zone to the tenth zone of the cylinder temperature is 360 ℃, and the temperature of the neck mold is 340 ℃.
The proportions of the components in the composite material of the above examples are shown in Table 1.
TABLE 1 proportions of the components of the composites of examples 1-5
The composite material prepared by the above embodiment is subjected to performance tests, and the performance tests comprise thermal conductivity, electromagnetic shielding (50-1500MHz), tensile strength, bending strength, impact strength and compression strength. The performance data are shown in Table 2.
TABLE 2 Performance data for composites of examples 1-5
Claims (9)
1. A heat-conducting, electromagnetic-shielding and high-strength PEEK composite material is characterized by comprising the following components in parts by weight: 50-90 parts of PEEK, 0.5-10 parts of beryllium bronze powder, 2-10 parts of ferrite powder, 0.5-5 parts of semiconductor nano powder and 10-50 parts of PEI-based long carbon fiber.
2. The heat conductive, electromagnetic shielding, high strength PEEK composite of claim 1, wherein the beryllium bronze powder contains 2 wt% beryllium, 0.3 wt% nickel, 0.3 wt% cobalt, and the balance bronze.
3. The heat-conducting, electromagnetic-shielding and high-strength PEEK composite material of claim 1, wherein the semiconductor nanopowder has an average particle size of 100-500 nm.
4. The PEEK composite material of claim 3, wherein the semiconductor nano powder is one or more of aluminum-doped zinc oxide, antimony tin oxide and indium tin oxide.
5. The heat-conducting, electromagnetic-shielding and high-strength PEEK composite material of claim 1, wherein the PEI-based long carbon fiber is a carbon fiber filament with 0.3-1 wt% of PEI as an adhesive.
6. The preparation method of the heat-conducting, electromagnetic-shielding and high-strength PEEK composite material according to any one of claims 1-5, comprising the following steps:
(1) mixing beryllium bronze powder, ferrite powder and semiconductor nano powder in proportion to form mixed powder, adding a coupling agent into the mixed powder, and continuously and uniformly mixing to form modified mixed powder for later use;
(2) and (2) adding PEEK into a main feeding port of a double-screw extruder, adding the modified mixed powder obtained in the step (1) into a side feeding port, adding PEI-based long carbon fiber into an exhaust port, and performing extrusion granulation to obtain the heat-conducting, electromagnetic shielding and high-strength PEEK composite material.
7. The preparation method according to claim 6, wherein the amount of the coupling agent used in the step (1) is 0.5-1.2% of the weight of the mixed powder; the coupling agent is one of PEG-200, PEG-300 and PEG-500.
8. The preparation method of claim 6, wherein the feeding frequency of the main feeding port in the step (2) is 5Hz to 20Hz, the feeding frequency of the side feeding port is 1Hz to 5Hz, and the screw rotating speed of the twin-screw extruder is 250rpm to 350 rpm.
9. The method according to claim 6, wherein the extrusion granulation in the step (2) has a zone temperature of 250. + -. 10 ℃, a zone temperature of two to ten and a die temperature of 370. + -. 20 ℃.
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| CN108192277A (en) * | 2017-12-23 | 2018-06-22 | 湛江正信科技服务有限公司 | A kind of high temperature resistant polyether-ether-ketone composite material and preparation method thereof |
| CN108929487A (en) * | 2018-07-17 | 2018-12-04 | 杭州高兴工程塑料有限公司 | A kind of thermally conductive electromagnetic shielding polypropylene composite material and preparation method |
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