CN115418074A - Oriented multi-dimensional filler reinforced polyether ketone composite material and preparation method thereof - Google Patents
Oriented multi-dimensional filler reinforced polyether ketone composite material and preparation method thereof Download PDFInfo
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- 239000000945 filler Substances 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
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- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 claims description 4
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- 229910052863 mullite Inorganic materials 0.000 claims description 4
- -1 MXene Chemical compound 0.000 claims description 3
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- PQQKPALAQIIWST-UHFFFAOYSA-N oxomolybdenum Chemical compound [Mo]=O PQQKPALAQIIWST-UHFFFAOYSA-N 0.000 claims description 2
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- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/04—Reinforcing macromolecular compounds with loose or coherent fibrous material
- C08J5/0405—Reinforcing macromolecular compounds with loose or coherent fibrous material with inorganic fibres
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- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/005—Reinforced macromolecular compounds with nanosized materials, e.g. nanoparticles, nanofibres, nanotubes, nanowires, nanorods or nanolayered materials
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- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/04—Reinforcing macromolecular compounds with loose or coherent fibrous material
- C08J5/0405—Reinforcing macromolecular compounds with loose or coherent fibrous material with inorganic fibres
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- C08J2361/00—Characterised by the use of condensation polymers of aldehydes or ketones; Derivatives of such polymers
- C08J2361/04—Condensation polymers of aldehydes or ketones with phenols only
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Abstract
The invention belongs to the technical field of high-temperature-resistant composite materials, and particularly relates to an oriented multi-dimensional filler reinforced polyether ketone composite material and a preparation method thereof. Mixing, extruding and granulating and ultrasonic-assisted injection molding by using high-temperature-resistant polyether ketone as a matrix, micron-sized chopped fibers as a reinforcing phase and nano-sized fibers or nano sheets as an auxiliary reinforcing phase; the process of the ultrasonic-assisted injection molding is as follows: and under the assistance of ultrasonic waves, the material to be injected flows into a mold for molding. The composite material keeps the inherent excellent high temperature resistance of the polyether ketone, and the mechanical properties (strength and modulus) of the composite material are improved by anchoring under different scales through the synergistic effect of adding the multi-dimensional filler, so that the composite material is particularly applied to the field of requiring excellent mechanical properties under the high-temperature condition that the use temperature exceeds 330 ℃.
Description
Technical Field
The invention belongs to the technical field of high-temperature-resistant composite materials, and particularly relates to an oriented multi-dimensional filler reinforced polyether ketone composite material and a preparation method thereof.
Background
In recent years, the application of high temperature resistant polymer matrix composite materials in aerospace and military industries is receiving more and more extensive attention, and the high temperature resistant polymer matrix composite materials become important strategic materials of the country. The traditional polymer resin is usually decomposed, melted or softened below 300 ℃, so that the mechanical properties are deteriorated or even lost, and the polymer-based composite material is difficult to use in a high-temperature environment above 300 ℃. However, the design goals of new spacecraft, high power radars, and fifth generation military aircraft have pushed the operating temperature of the composite materials to 316-538 ℃ and even higher. The polyether ketone is a high-performance thermoplastic material with a highly stable chemical framework, has excellent performances such as high temperature resistance, high strength and high chemical resistance, can be used as an excellent metal substitute material in an extremely harsh environment, and can be used as a high-temperature resistant structural material to meet the requirements of high temperature environments of 300-400 ℃.
However, the mechanical property of the pure polyether ketone is insufficient, the pure polyether ketone is difficult to be directly applied, the mechanical property of the pure polyether ketone can be greatly improved by adding the filler as a reinforcing phase, the temperature resistance is improved, the use cost of the material can be reduced, and the popularization and the application are facilitated. Reinforcing phase fillers are largely classified into three types of fibers, flakes, and particles according to their morphology. The polyether ketone composite material is prepared by mutually matching the fillers with different dimensions, so that the advantages of the reinforced material and the matrix can be fully exerted, the mechanical property of the material is improved on the basis of high temperature resistance, and the substitution of a metal material is realized. How to effectively match fillers with different dimensions, and improving the mechanical properties as much as possible on the basis of meeting the processing performance still faces the technical bottleneck, for example, the heat-resistant temperature of some fillers or filler modifiers cannot reach 300 ℃ at the present stage, so that the use problem of the prepared compound is also limited. Besides, the fiber and flake fillers have anisotropic characteristics, and the orientation degree of the fillers in the matrix greatly influences the mechanical properties such as strength and modulus of the composite material. Therefore, designing the orientation of the filler to enhance the mechanical properties according to the application of the composite material is also an important research subject for the preparation of the composite material at present, and faces great difficulty.
Disclosure of Invention
The invention aims to provide an oriented multi-dimensional filler reinforced polyether ketone composite material, which takes high-temperature resistant polyether ketone as a matrix, takes multi-dimensional filler as a reinforcing phase, takes micron-sized fibers as a main reinforcing body and takes nano-sized fibers or nano-sheets as auxiliary reinforcing bodies, wherein the nano-sized fibers or nano-sheets are distributed in gaps among the micron-sized fibers, and the supplement and the improvement of strength/modulus are realized.
The invention also aims to provide a preparation method of the oriented multi-dimensional filler reinforced polyether ketone composite material, which is characterized in that chopped fibers, nano-scale fibers or nano-sheets and polyether ketone are mixed and then are subjected to extrusion granulation and ultrasonic-assisted injection molding to prepare the composite material with fibers or thin sheets highly oriented along the melt flow direction, and the mechanical property of the composite material is greatly improved by means of the high orientation of anisotropic fillers.
The technical scheme of the invention is as follows:
an oriented multi-dimensional filler reinforced polyether ketone composite material is prepared by taking high-temperature resistant polyether ketone as a matrix, taking micron-sized chopped fibers as a reinforcing phase and taking nano-sized fibers or nano-sheets as an auxiliary reinforcing phase, and adopting mixing, extrusion granulation and ultrasonic-assisted injection molding; the process of the ultrasonic-assisted injection molding is as follows: and under the assistance of ultrasonic waves, the material to be injected flows into a mold for molding.
Preferably, the micron-sized chopped fibers are one or more of carbon fibers, glass fibers, mullite fibers, alumina fibers and basalt fibers, and the length of the fibers is 300-3 cm.
Preferably, the nano-scale fiber is carbon nano-tube, carbon nano-fiber, siC whisker, si 3 N 4 One or more of whiskers; the nano sheet is one or more of graphene, boron nitride, MXene, molybdenum sulfide, tungsten sulfide, manganese oxide, titanium oxide and molybdenum oxide.
Preferably, the mass ratio of the micron-sized chopped fibers to the nano-sized fibers or nano-sheets is 1.
Preferably, the high-temperature resistant polyether ketone is polyether ketone with a melting temperature of more than 330 ℃ and particle size of less than 300 μm; the mass ratio of the addition amount of the reinforcing phase and the auxiliary reinforcing phase to the polyaryletherketone is 1 to 9.
The preparation method of the oriented multi-dimensional filler reinforced polyether ketone composite material comprises the following steps:
(1) Mixing: adding the micron-sized chopped fibers, the nano-sized fibers or the nano-sheets and the high-temperature resistant polyether ketone powder into a high-speed mixer according to a certain proportion, and uniformly mixing to obtain a mixture;
(2) And (3) extruding and granulating: adding the mixture into a screw extruder for melting, mixing, extruding and granulating to obtain composite material particles;
(3) Injection molding: adding the composite material particles into an injection molding machine, heating to a molten state, and making the material to be injected flow into a mold to be molded under the assistance of ultrasonic waves, thereby obtaining a composite material product.
Preferably, the conditions for melt-kneading, extrusion and granulation in the step (2) are as follows: heating temperatures of all sections from a charging opening to a die are sequentially 280-330 ℃, 320-380 ℃, 350-400 ℃, 370-420 ℃, 390-450 ℃ and 360-400 ℃, the rotation speed of a screw is 50-150r/min, and the temperature of a cooling water tank is set to be 40-70 ℃.
Preferably, the injection molding conditions of the step (3) are as follows: the injection molding temperature is 160-250 ℃, the injection molding pressure is 50-180MPa, and the injection molding cycle is 20-50s.
Preferably, the ultrasonic wave of step (3) has the following conditions: the ultrasonic frequency is 1 kHz to 50kHz, and the ultrasonic time is 5 to 50s.
Further, the tensile strength at 330 ℃ is more than 140 MPa.
Compared with the prior art, the invention has the advantages that:
(1) The composite material keeps the inherent excellent high temperature resistance of the polyether ketone, and the mechanical properties (strength and modulus) of the composite material are improved by anchoring under different scales through the synergistic effect of adding the multi-dimensional filler, so that the composite material is particularly applied to the field of requiring excellent mechanical properties under the high-temperature condition that the use temperature exceeds 330 ℃.
(2) The reinforcing phase filler realizes high orientation along the flow direction of the melt, and greatly improves the mechanical properties of the composite material product such as tensile strength, bending strength and the like along the fiber orientation direction.
(3) The invention adopts an injection molding process, can meet the preparation requirements of structural parts and parts in various forms, particularly special-shaped components, has simple product processing and high precision, and particularly has unique advantages for small-sized precise construction.
Drawings
FIG. 1 is a schematic structural view of a sample prepared in the present invention;
FIG. 2 is an SEM photograph of a cross-section of a sample prepared in example 1 of the present invention.
Detailed Description
The present invention will be described in further detail with reference to specific examples, but the embodiments of the present invention are not limited thereto.
Example 1 carbon fiber and graphene reinforced polyetheretherketone
(1) Mixing: mixing chopped carbon fibers with the lengths of 1mm to 3mm with graphene powder according to the mass ratio of 1.1 to obtain a reinforcing material, taking polyether ketone powder with the melting point of 370 ℃ and the particle size of 300 mu m as a matrix, adding the reinforcing material and the polyether ketone into a high-speed mixer according to the mass ratio of 1:2, and uniformly mixing to obtain a mixture;
(2) And (3) extruding and granulating: adding the mixture into a screw extruder to carry out melting, mixing, extruding and granulating, wherein the heating temperature of each section from a feed inlet to a die is 280 ℃, 320 ℃, 350 ℃, 370 ℃, 390 ℃ and 360 ℃, the rotation speed of a screw is 80r/min, and the temperature of a cooling water tank is set to be 50 ℃ to obtain composite particles;
(3) Injection molding: adding the composite material particles into an injection molding machine, heating to a molten state, molding through a mold with an ultrasonic vibration system, wherein an ultrasonic amplitude transformer is connected with a mold core, transmitting ultrasonic energy to a polymer melt in the mold cavity by means of the mold core when a plastic part is molded, the injection molding temperature is 200 ℃, the injection molding pressure is 150MPa, the injection molding cycle is 30s, the ultrasonic frequency is 40kHz, and the ultrasonic time is 30s, and finally obtaining a composite material product with highly oriented filler.
As shown in the attached figure 1, the carbon fibers and the graphene have good compatibility with a resin matrix, no obvious crack is formed at an interface, and the carbon fibers are highly oriented and arranged in the resin, so that excellent mechanical properties are provided.
Example 2 mullite fiber and carbon nanotube reinforced polyetheretherketone
(1) Mixing: mixing chopped mullite fibers with the length of 1cm to 3cm and carbon nanotube powder according to the mass ratio of 1 to 0.5 to obtain a reinforcing material, taking polyether ketone powder with the melting point of 350 ℃ and the particle size of 100 mu m as a matrix, and adding the reinforcing material and the polyether ketone into a high-speed mixer according to the mass ratio of 1:1 to mix uniformly to obtain a mixture;
(2) And (3) extruding and granulating: adding the mixture into a screw extruder to carry out melting, mixing, extruding and granulating, wherein the heating temperature of each section from a feed inlet to a die is 300 ℃, 340 ℃, 370 ℃, 390 ℃, 420 ℃ and 380 ℃ in sequence, the rotation speed of the screw is 50r/min, and the temperature of a cooling water tank is set to be 70 ℃, so that composite particles are obtained;
(3) Injection molding: adding composite material particles into an injection molding machine, heating to a molten state, and molding through a mold with an ultrasonic vibration system, wherein an ultrasonic amplitude transformer is connected with a mold core of the mold, ultrasonic energy can be transferred to a polymer melt in the mold cavity by means of the mold core when a plastic part is molded, the injection molding temperature is 220 ℃, the injection molding pressure is 50MPa, the injection molding period is 50s, the ultrasonic frequency is 10kHz, and the ultrasonic time is 50s, so that a composite material product with highly oriented filler is finally obtained.
Example 3 basalt fiber and boron nitride sheet reinforced polyetheretherketone
(1) Mixing: mixing chopped basalt fibers with the length of 300-1 mm and two-dimensional boron nitride sheet powder according to the mass ratio of 1.2 to obtain a reinforcing material, taking polyether ketone powder with the melting point of 380 ℃ and the particle size of 200 mu m as a matrix, adding the reinforcing material and the polyether ketone into a high-speed mixer according to the mass ratio of 1:5, and uniformly mixing to obtain a mixture;
(2) And (3) extruding and granulating: adding the mixture into a screw extruder to carry out melting, mixing, extruding and granulating, wherein the heating temperature of each section from a feed inlet to a die is 310 ℃, 350 ℃, 380 ℃, 400 ℃, 430 ℃ and 390 ℃, the rotation speed of the screw is 100r/min, and the temperature of a cooling water tank is 40 ℃ to obtain composite particles;
(3) Injection molding: adding the composite material particles into an injection molding machine, heating to a molten state, and molding through a mold with an ultrasonic vibration system, wherein an ultrasonic amplitude transformer is connected with a mold core of the mold, ultrasonic energy can be transferred to a polymer melt in the mold cavity by means of the mold core when a plastic part is molded, the injection molding temperature is 230 ℃, the injection molding pressure is 150MPa, the injection molding period is 20s, the ultrasonic frequency is 50kHz, and the ultrasonic time is 5s, so that a composite material product with highly oriented filler is finally obtained.
Example 4 glass fiber and carbon nanofiber reinforced polyetheretherketone
(1) Mixing: mixing chopped glass fibers with the lengths of 1mm-3mm with carbon nanofiber powder according to the mass ratio of 1:1 to obtain a reinforcing material, taking polyether ketone powder with the melting point of 390 ℃ and the particle size of 100 mu m as a matrix, adding the reinforcing material and the polyether ketone into a high-speed mixer according to the mass ratio of 1:9, and uniformly mixing to obtain a mixture;
(2) And (3) extruding and granulating: adding the mixture into a screw extruder to carry out melting, mixing, extruding and granulating, wherein the heating temperature of each section from a feed inlet to a die is 330 ℃, 380 ℃, 400 ℃, 420 ℃, 450 ℃ and 400 ℃, the rotation speed of the screw is 150r/min, and the temperature of a cooling water tank is set to be 40 ℃ to obtain composite particles;
(3) Injection molding: adding the composite material particles into an injection molding machine, heating to a molten state, and molding through a mold with an ultrasonic vibration system, wherein an ultrasonic amplitude transformer is connected with a mold core of the mold, ultrasonic energy can be transferred to a polymer melt in the mold cavity by means of the mold core when a plastic part is molded, the injection molding temperature is 250 ℃, the injection molding pressure is 180MPa, the injection molding period is 50s, the ultrasonic frequency is 50kHz, and the ultrasonic time is 50s, so that a composite material product with highly oriented filler is finally obtained.
Comparative example 1 pure carbon fiber reinforced polyetheretherketone
The same procedures as in example 1 were carried out except that the reinforcing phase was composed of only micron-sized carbon fibers, and the production and evaluation of the product were carried out, the results of which are shown in Table 1. The heat distortion temperature of the sample is basically unchanged, and the mechanical property is slightly poor.
Comparative example 2 pure carbon nanotube reinforced polyetheretherketone
The production and evaluation of the product were carried out in the same manner as in example 1 except that the reinforcing phase was composed of only the nano-sized carbon nanotube powder, and the results are shown in Table 1. The thermal deformation temperature of the sample is basically unchanged, and the mechanical property is deteriorated.
Comparative example 3 carbon fiber and graphene reinforced polyetheretherketone without ultrasonic treatment
The production and evaluation of the product were carried out in the same manner as in example 1 except that the ultrasonic-assisted mold was not used in the injection molding step, and the results are shown in table 1. The thermal deformation temperature of the sample is basically unchanged, and the mechanical property is deteriorated.
Comparative example 4 carbon fiber and graphene reinforced polyetherimide
(1) Mixing: mixing chopped carbon fibers with the lengths of 1mm to 3mm with graphene powder according to the mass ratio of 1.1 to obtain a reinforcing material, taking thermoplastic resin polyetherimide powder with the melting point of 200 ℃ and the particle size of 300 mu m as a matrix, and adding the reinforcing material and the polyetherimide into a high-speed mixer according to the mass ratio of 1:2 to mix uniformly to obtain a mixture;
(2) Extruding and granulating: adding the mixture into a screw extruder to carry out melting, mixing, extruding and granulating, wherein the heating temperature of each section from a feed inlet to a die is 160 ℃, 190 ℃, 220 ℃, 250 ℃, 230 ℃ and 220 ℃, the rotation speed of the screw is 50r/min, and the temperature of a cooling water tank is set to be 50 ℃, so that composite particles are obtained;
(3) Injection molding: adding the composite material particles into an injection molding machine, heating to a molten state, and molding through a mold with an ultrasonic vibration system, wherein an ultrasonic amplitude transformer is connected with a mold core of the mold, ultrasonic energy can be transferred to a polymer melt in the mold cavity by means of the mold core when a plastic part is molded, the injection molding temperature is 120 ℃, the injection molding pressure is 100MPa, the injection molding period is 30s, the ultrasonic frequency is 40kHz, and the ultrasonic time is 30s, so that a composite material product with highly oriented filler is finally obtained.
Sample Performance testing
Taking the composite materials prepared in each example and comparative example as examples, standard sample strips are prepared by the same process method, and the samples are subjected to thermal property and mechanical property tests, and the results are shown in table 1.
Table 1: results of sample Performance test
Claims (10)
1. An oriented multi-dimensional filler reinforced polyether ketone composite material is characterized in that high-temperature resistant polyether ketone is used as a matrix, micron-sized chopped fibers are used as a reinforcing phase, nano-sized fibers or nano-sheets are used as an auxiliary reinforcing phase, and mixing, extrusion granulation and ultrasonic-assisted injection molding are adopted; the process of the ultrasonic-assisted injection molding is as follows: and under the assistance of ultrasonic waves, the material to be injected flows into a mold for molding.
2. The oriented multi-dimensional filler reinforced polyether ketone composite material as claimed in claim 1, wherein the micron-sized chopped fibers are one or more of carbon fibers, glass fibers, mullite fibers, alumina fibers and basalt fibers, and the fiber length is 300 μm-3 cm.
3. The oriented multi-dimensional filler reinforced polyetherketoneketone composite material according to claim 1, wherein the nano-scale fibers are carbon nanotubes, carbon nanofibers, siC whiskers, si 3 N 4 One or more of whiskers; the nano sheet is one or more of graphene, boron nitride, MXene, molybdenum sulfide, tungsten sulfide, manganese oxide, titanium oxide and molybdenum oxide.
4. The oriented multi-dimensional filler reinforced polyether ketone composite material as claimed in claim 1, wherein the mass ratio of the micron-sized chopped fibers to the nano-sized fibers or nano-sheets is 1.
5. The oriented multi-dimensional filler reinforced polyether ketone composite material as claimed in claim 1, wherein the high temperature resistant polyether ketone is polyether ketone having a melting temperature of above 330 ℃ and a particle size of below 300 μm; the mass ratio of the addition amount of the reinforcing phase and the auxiliary reinforcing phase to the polyaryletherketone is 1 to 9.
6. A process for the preparation of an oriented multi-dimensional filler reinforced polyetherketoneketone composite as claimed in any one of claims 1 to 5, characterized in that it comprises the following steps:
(1) Mixing: adding the micron-sized chopped fibers, the nano-sized fibers or the nano-sheets and the high-temperature resistant polyether ketone powder into a high-speed mixer according to a certain proportion, and uniformly mixing to obtain a mixture;
(2) And (3) extruding and granulating: adding the mixture into a screw extruder for melting, mixing, extruding and granulating to obtain composite material particles;
(3) Injection molding: adding the composite material particles into an injection molding machine, heating to a molten state, and flowing the material to be injection molded into a mold to be molded under the assistance of ultrasonic waves, so as to obtain the composite material product.
7. The method according to claim 6, wherein the melt-kneading extrusion granulation conditions in the step (2) are as follows: heating temperatures of all sections from a charging opening to a die are sequentially 280-330 ℃, 320-380 ℃, 350-400 ℃, 370-420 ℃, 390-450 ℃ and 360-400 ℃, the rotation speed of a screw is 50-150r/min, and the temperature of a cooling water tank is set to be 40-70 ℃.
8. The production method according to claim 6, wherein the injection molding conditions of the step (3) are: the injection molding temperature is 160-250 ℃, the injection molding pressure is 50-180MPa, and the injection molding cycle is 20-50s.
9. The production method according to claim 6, wherein the conditions of the ultrasonic wave of the step (3) are: the ultrasonic frequency is 1 kHz to 50kHz, and the ultrasonic time is 5 to 50s.
10. The oriented multi-dimensional filler reinforced polyether ketone composite material as claimed in claim 1, wherein the tensile strength at 330 ℃ is greater than 140 MPa.
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