CN115466482B - Light composite material with excellent mechanical property at high temperature and preparation method thereof - Google Patents
Light composite material with excellent mechanical property at high temperature and preparation method thereof Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 55
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
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- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 86
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- 238000002844 melting Methods 0.000 claims abstract description 18
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- 239000000835 fiber Substances 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 14
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- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 5
- 230000003647 oxidation Effects 0.000 claims abstract description 4
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 4
- 238000001746 injection moulding Methods 0.000 claims description 34
- 229920006260 polyaryletherketone Polymers 0.000 claims description 27
- 238000002156 mixing Methods 0.000 claims description 21
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Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/04—Reinforcing macromolecular compounds with loose or coherent fibrous material
- C08J5/06—Reinforcing macromolecular compounds with loose or coherent fibrous material using pretreated fibrous materials
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B9/00—Making granules
- B29B9/02—Making granules by dividing preformed material
- B29B9/06—Making granules by dividing preformed material in the form of filamentary material, e.g. combined with extrusion
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C45/00—Injection moulding, i.e. forcing the required volume of moulding material through a nozzle into a closed mould; Apparatus therefor
- B29C45/03—Injection moulding apparatus
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- 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
- C08J2361/16—Condensation polymers of aldehydes or ketones with phenols only of ketones with phenols
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2371/00—Characterised by the use of polyethers obtained by reactions forming an ether link in the main chain; Derivatives of such polymers
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
- C08K7/06—Elements
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/02—Ingredients treated with inorganic substances
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02T—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO TRANSPORTATION
- Y02T50/00—Aeronautics or air transport
- Y02T50/40—Weight reduction
Abstract
The invention belongs to the technical field of composite materials, and particularly relates to a light composite material with excellent mechanical properties at high temperature and a preparation method thereof. Forming acidic oxygen-containing functional groups on the surfaces of the carbonaceous particles by an oxidation treatment; carbon fiber is treated by ammonia gas, and forms strong chemical combination with a carbon modifier through electrostatic interaction, and nano carbon modifier is adhered on the surface of the carbon fiber; avoiding the serious problems of uneven structure, deterioration of mechanical property, reduction of temperature resistance and the like caused by the decomposition and melting of organic matters at high temperature; avoiding the problems that the agglomeration, adhesion and the like of the chopped carbon fibers in the modification process affect the dispersion of the later fibers in the resin matrix; the prepared composite material can be prepared into structural members and parts in various forms, particularly special-shaped members with complex structures, has simple processing and high precision, and is applied to the field requiring excellent mechanical properties under the condition of high temperature (the use temperature is more than or equal to 330 ℃).
Description
Technical Field
The invention belongs to the technical field of composite materials, and particularly relates to a light composite material with excellent mechanical properties at high temperature and a preparation method thereof.
Background
With the rapid development of aerospace and national defense industries, resin-based composite materials with the advantages of low density, high strength, good impact resistance, good creep resistance and the like are increasingly used for replacing metal materials, and become a core key technology for the development of related fields. Along with the increasing speed of aircrafts, advanced aerospace technology represented by hypersonic aircrafts brings higher requirements on the temperature resistance of resin matrix composite materials, and development of light composite materials with excellent mechanical properties at high temperature are increasingly emphasized.
Polyaryletherketones are a class of crystalline polymers formed from phenylene rings linked by an oxygen bridge (ether linkage) and a carbonyl group (ketone). Many different polymers can be formed according to the connection sequence and proportion of ether bond, ketone group and benzene ring in the molecular chain. Mainly comprises several varieties of polyether ketone, polyether-ether-ketone, polyether-ketone-ether-ketone, polyether-ether-ketone, polyether-ketone, etc. The polyaryletherketone molecular structure contains rigid benzene rings, so that the polyaryletherketone has the characteristics of excellent high-temperature performance, mechanical property, electrical insulation, radiation resistance, chemical resistance and the like, is suitable for being used as matrix resin and super engineering plastic of high-performance composite materials, and has been applied to industries such as automobiles, aerospace, medical treatment, electrical engineering and the like. However, the melt viscosity of the polyaryletherketone is high, so that the interfacial interaction between the polyaryletherketone and the carbon fiber reinforced phase is weak, the compatibility is poor, the mechanical properties of the composite material, especially the mechanical strength at high temperature, are far lower than the theoretical value, and the practical application of the composite material is limited.
The carbon fiber is subjected to surface modification treatment, so that the interaction between the fiber and the matrix can be enhanced, the interfacial bonding strength is increased, and the mechanical property of the composite material is improved. Chinese patent CN109504030B discloses that the surface of carbon fiber is coated with water-soluble polyamide-imide and polyamide for improving the interfacial bonding strength between carbon fiber and polyetheretherketone, thereby improving the mechanical properties of fiber reinforced polyetheretherketone composite material. In certain high-temperature use occasions, such as high-temperature sealing rings, fireproof high-temperature sleeves, electronic smoke gun components and the like, higher requirements are set for the use temperature, and even the high-temperature sealing rings, fireproof high-temperature sleeves, electronic smoke gun components and the like can maintain a certain mechanical strength above 330 ℃ and can be stably used. The ultrahigh use temperature causes decomposition and performance degradation of most of organic matters (filler additives), so that the use requirement of the carbon fiber under the condition of high temperature is difficult to meet by adopting a mode of modifying the carbon fiber by the organic matters. In addition, for small products, especially profiled elements, it is often necessary to use chopped carbon fibers for reinforcement, and how to maintain high mechanical strength while avoiding fiber blocking when modifying chopped fibers is also a current technical bottleneck. Therefore, preparing a chopped fiber reinforced polyaryletherketone composite material and having excellent mechanical properties at high temperature is a problem to be solved in the field of the current composite materials.
Disclosure of Invention
The invention aims to provide a modified chopped carbon fiber reinforced polyaryletherketone composite material, which is subjected to oxidation treatment to form acidic oxygen-containing functional groups on the surfaces of carbonaceous particles; carbon fiber is treated by ammonia gas, and forms strong chemical combination with a carbon modifier through electrostatic interaction, and nano carbon modifier is adhered on the surface of the carbon fiber; avoiding the serious problems of uneven structure, deterioration of mechanical property, reduction of temperature resistance and the like caused by the decomposition and melting of organic matters at high temperature; avoiding the problems that the agglomeration, adhesion and the like of the chopped carbon fibers in the modification process affect the dispersion of the later fibers in the resin matrix; the prepared composite material can be prepared into structural members and parts in various forms, particularly special-shaped members with complex structures, has simple processing and high precision, and is applied to the field requiring excellent mechanical properties under the condition of high temperature (the use temperature is more than or equal to 330 ℃).
The second purpose of the invention is to provide a preparation method of the modified chopped carbon fiber reinforced polyaryletherketone composite material, wherein the modification method of the carbon fiber has simple process, no waste liquid and environmental protection, and can realize large-scale production; the chopped carbon fibers are uniformly dispersed in the polyaryletherketone matrix, and the interface combination between the chopped carbon fibers and the polyaryletherketone matrix is good, so that the mechanical property is excellent; the composite material is used for preparing products with high precision requirements and complex structures.
The technical scheme of the invention is as follows:
a preparation method of a light composite material with excellent mechanical properties at high temperature comprises the following steps:
(1) Ammoniation of carbon fiber: chopped carbon fiber, NH 3 High temperature treatment under atmosphere;
(2) Oxidizing a modifier: treating the nanoscale carbonaceous modifier at a high temperature in an oxygen-containing atmosphere;
(3) Modification of carbon fiber: fully mixing the ammoniated carbon fiber in the step (1) and the oxidized carbon modifier in the step (2) in an aqueous solution, and filtering and drying to obtain modified chopped carbon fiber;
(4) Mixing: uniformly mixing the modified chopped carbon fiber and high-temperature-resistant polyaryletherketone powder to obtain a mixture;
(5) And (3) extruding and granulating: adding the mixture into a screw extruder for melting, mixing, extruding and granulating to obtain composite material particles;
(6) Injection molding: the composite particles are added into an injection molding machine, heated to a molten state, and molded by a mold to produce composite products of various structures.
Preferably, the chopped carbon fibers are one or more of chopped polyacrylonitrile-based carbon fibers, chopped pitch-based carbon fibers and chopped viscose-based carbon fibers, and the fiber length is 300 mu m-3 cm; the NH is 3 The atmosphere treatment temperature is 600-1200 ℃ and the treatment time is 0.5-5 h.
Preferably, the nanoscale carbonaceous modifier is one or more of carbon nanotubes, graphene, carbon black and carbon nanofibers; the oxygen-containing atmosphere is one or more of oxygen, air, ozone or water vapor, the heating temperature is 500-1000 ℃, and the heating time is 0.5-5 h.
Preferably, the mass ratio of the ammoniated carbon fibers to the oxidized carbon modifier is 1:0.02-0.2.
Preferably, the high temperature resistant polyaryletherketone is one or more of polyetherketone, polyetheretherketone ketone, polyetheretherketone ketone and polyetherketone ketone; the melting temperature of the high-temperature-resistant polyaryletherketone is above 330 ℃, and the particle size of the high-temperature-resistant polyaryletherketone is below 300 mu m; the mass ratio of the modified chopped carbon fiber to the polyaryletherketone is 1:1-9.
Preferably, the melting, mixing, extruding and granulating are carried out, the heating temperature of each section from a feed inlet to a die is 250-330 ℃, 300-380 ℃, 330-400 ℃, 350-420 ℃, 350-450 ℃ and 340-400 ℃ in sequence, the rotating speed of a screw is 50-200 r/min, and the temperature of a cooling water tank is set to 40-70 ℃.
According to the preparation method of the light composite material with excellent mechanical properties at high temperature, the injection molding temperature of injection molding is 160-250 ℃, the injection molding pressure is 50-180 MPa, and the injection molding period is 20-50 s.
Forming acidic oxygen-containing functional groups on the surfaces of the carbonaceous particles by an oxidation treatment; the carbon fiber and the carbon modifier form strong chemical combination through electrostatic interaction, and the nano carbon modifier is adhered on the surface of the carbon fiber; particularly strong, the carbon fiber is modified by using the nano carbonaceous modifier, and organic matters are not used for modification, so that serious problems of uneven structure, deterioration of mechanical properties, reduction of temperature resistance and the like caused by decomposition and melting of the organic matters at high temperature are avoided. The modification method aims at the chopped carbon fibers, and avoids the problem that the dispersion of the later fibers in the resin matrix is affected due to the aggregation, adhesion and other phenomena of the chopped carbon fibers in the modification process.
The composite material can be prepared into structural members and parts in various forms, particularly special-shaped members with complex structures, has simple processing and high precision, and is applied to the field requiring excellent mechanical properties under the condition of high temperature (the use temperature is more than or equal to 330 ℃).
Compared with the prior art, the invention has the advantages that:
(1) The composite material keeps inherent excellent high temperature resistance of the polyaryletherketone, and the chopped carbon fiber is added to endow the polyaryletherketone with good mechanical properties (strength and modulus), and the advantages of the polyaryletherketone and the chopped carbon fiber are complementary, so that the requirement on the mechanical strength under the condition that the using temperature exceeds 330 ℃ is especially met.
(2) The carbon fiber surface modification technology is used for grafting the nano carbon modified material on the surface of the carbon fiber, the carbon fiber surface modification technology and the nano carbon modified material are firmly combined through chemistry, the roughness of the carbon fiber surface is enhanced on the premise that the carbon fiber structure is not damaged by the nano carbon material, the effective anchor points of the fiber and the polyaryletherketone are increased, the interface bonding strength of the fiber and a matrix is improved, and the tensile strength/modulus, the bending strength/modulus and the interlaminar shear strength of the composite material are further improved. Especially, at high temperature, the polyaryletherketone matrix is changed from solid to melt, and the uneven surface of the modified carbon fiber enhances the shearing force of the melt flow of the polyaryletherketone, and improves the melting temperature and high-temperature mechanical properties of the composite material.
(3) The modification method is suitable for chopped carbon fibers, avoids the influence of aggregation, adhesion and the like of the fibers on the dispersion performance of the fibers in a resin matrix, and is different from reinforcing bodies such as carbon fiber filaments or carbon fiber fabrics. Meanwhile, the invention does not use an organic matter modifier used in the conventional modification method, so that the problem of degradation of the composite material performance caused by decomposition and melting of organic matters in the high-temperature processing and use environment process is avoided.
(4) The carbon fiber surface modification process has no waste liquid, is economical and environment-friendly, has simple process and obvious effect, can realize large-scale production, and has industrial technical conditions;
(5) The invention adopts the injection molding process, can meet the preparation requirements of structural members and parts in various forms, in particular to special-shaped members, has simple processing and high precision, and has unique advantages for small-sized precise construction.
Drawings
FIG. 1 is an SEM image of a sample prepared in example 1 according to the invention;
FIG. 2 is an SEM image of a sample prepared according to example 5 of the present invention.
Detailed Description
The present invention is described in further detail below with reference to specific examples, but embodiments of the present invention are not limited thereto.
A first part: carbon fiber modification
Example 1 graphene-modified carbon fiber
(1) Ammoniation of carbon fiber: placing chopped polyacrylonitrile-based carbon fiber with the length of 300 mu m-3 mm into a rotary furnace, and introducing NH at 800 DEG C 3 Treating for 2 hours at high temperature in atmosphere to obtain amino-functionalized carbon fibers;
(2) Oxidizing a modifier: placing graphene powder into a rotary furnace, and heating to 600 ℃ under the steam atmosphere for high-temperature treatment for 1h to obtain graphene oxide;
(3) Modification of carbon fiber: ultrasonically dispersing the ammoniated carbon fiber and the carbon oxide nano tube in an aqueous solution according to the mass ratio of 1:0.02, fully stirring and uniformly mixing, and performing suction filtration and drying to obtain graphene modified chopped carbon fiber;
as shown in figure 1, the surface of the carbon fiber is adhered with the flaky graphene, the flaky graphene and the flaky graphene are tightly combined, the surface roughness of the carbon fiber is greatly enhanced, and a large number of effective anchor points are provided for the later-stage compounding with the polyaryletherketone body.
EXAMPLE 2 carbon nanotube-modified carbon fiber
(1) Ammoniation of carbon fiber: placing chopped asphalt-based carbon fibers with the length of 3 mm-3 cm into a rotary furnace, and introducing NH at 600 DEG C 3 Performing high-temperature treatment for 5 hours in the atmosphere to obtain amino-functionalized carbon fibers;
(2) Oxidizing a modifier: placing the carbon nano tube powder into a rotary furnace, and heating to 500 ℃ under the air atmosphere for high-temperature treatment for 5 hours to obtain oxidized carbon nano tubes;
(3) Modification of carbon fiber: ultrasonically dispersing the ammoniated carbon fiber and the carbon oxide nano tube in an aqueous solution according to the mass ratio of 1:0.2, fully stirring and uniformly mixing, and performing suction filtration and drying to obtain carbon nano tube modified chopped carbon fiber;
EXAMPLE 3 carbon Black modified carbon fiber
(1) Ammoniation of carbon fiber: placing chopped viscose-based carbon fiber with the length of 1 mm-1 cm into a rotary furnace, and introducing NH at 1200 DEG C 3 Treating for 0.5h at high temperature in the atmosphere to obtain amino-functionalized carbon fibers;
(2) Oxidizing a modifier: placing carbon black powder into a rotary furnace, and heating to 800 ℃ under an oxygen atmosphere for high-temperature treatment for 1h to obtain oxidized carbon black;
(3) Modification of carbon fiber: ultrasonically dispersing the ammoniated carbon fiber and the oxidized carbon black in an aqueous solution according to the mass ratio of 1:0.05, fully stirring and uniformly mixing, and performing suction filtration and drying to obtain carbon black modified chopped carbon fiber;
EXAMPLE 4 carbon nanofiber modified carbon fiber
(1) Ammoniation of carbon fiber: placing chopped polyacrylonitrile-based carbon fiber with the length of 500 mu m-2 mm into a rotary furnace, and introducing NH at 1000 DEG C 3 Treating for 1h at high temperature in atmosphere to obtain amino-functionalized carbon fibers;
(2) Oxidizing a modifier: placing carbon nanofiber powder into a rotary furnace, and heating to 1000 ℃ under ozone atmosphere for high-temperature treatment for 0.5h to obtain carbon oxide nanofiber;
(3) Modification of carbon fiber: ultrasonically dispersing the ammoniated carbon fiber and the carbon oxide nanofiber in an aqueous solution according to the mass ratio of 1:0.1, fully stirring and uniformly mixing, and performing suction filtration and drying to obtain carbon nanofiber modified chopped carbon fibers;
a second part: preparation of composite materials
Example 5 carbon fiber reinforced polyetheretherketone-1
(1) Mixing: taking polyether-ether-ketone powder with the melting point of 340 ℃ and the particle size of 300 mu m as a matrix, taking graphene modified carbon fiber as a reinforcing phase, and adding the carbon fiber and the polyether-ether-ketone into a high-speed mixer according to the mass ratio of 1:2 to uniformly mix to obtain a mixture;
(2) And (3) extruding and granulating: adding the mixture into a screw extruder for melting, mixing, extruding and granulating, wherein the heating temperature of each section from a feed inlet to a die is 280 ℃, 320 ℃, 340 ℃, 370 ℃, 380 ℃ and 360 ℃ in sequence, the rotating speed of the screw is 80r/min, and the temperature of a cooling water tank is set to be 50 ℃ to obtain composite material particles;
(3) Injection molding: and adding the composite material particles into an injection molding machine, heating to a molten state, and molding by a mold, wherein the injection molding temperature is 200 ℃, the injection molding pressure is 150MPa, and the injection molding period is 30s, so as to obtain the carbon fiber reinforced polyether-ether-ketone composite material product with the designed structure.
As shown in figure 2, the carbon fiber has good compatibility with the resin matrix, no obvious cracks are formed at the interface, and the interface is tightly combined, so that the excellent mechanical property is provided.
Example 6 carbon fiber reinforced polyetherketone
(1) Mixing: taking polyether ketone powder with the melting point of 330 ℃ and the particle size of 100 mu m as a matrix, taking carbon nanotube modified carbon fiber as a reinforcing phase, and adding the carbon fiber and the polyether ketone into a high-speed mixer according to the mass ratio of 1:1 to uniformly mix to obtain a mixture;
(2) And (3) extruding and granulating: adding the mixture into a screw extruder for melting, mixing, extruding and granulating, wherein the heating temperature of each section from a feed inlet to a die is 250 ℃, 300 ℃, 330 ℃, 350 ℃, 360 ℃ and 340 ℃ in sequence, the rotating speed of the screw is 200r/min, and the temperature of a cooling water tank is set to 40 ℃ to obtain composite material particles;
(3) Injection molding: and adding the composite material particles into an injection molding machine, heating to a molten state, and molding by a mold, wherein the injection molding temperature is 160 ℃, the injection molding pressure is 100MPa, and the injection molding period is 20s, so as to obtain the carbon fiber reinforced polyether-ether-ketone composite material product with the designed structure.
Example 7 carbon fiber reinforced polyetherketoneketone
(1) Mixing: taking polyether ketone powder with a melting point of 360 ℃ and a particle size of 50 mu m as a matrix, taking carbon black modified carbon fiber as a reinforcing phase, and adding the carbon fiber and the polyether ketone into a high-speed mixer according to a mass ratio of 1:4 to uniformly mix to obtain a mixture;
(2) And (3) extruding and granulating: adding the mixture into a screw extruder for 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 ℃ in sequence, the rotating speed of the screw is 50r/min, and the temperature of a cooling water tank is set to 70 ℃ to obtain composite material particles;
(3) Injection molding: and adding the composite material particles into an injection molding machine, heating to a molten state, and molding by a mold, wherein the injection molding temperature is 250 ℃, the injection molding pressure is 180MPa, and the injection molding period is 50s, so as to obtain the carbon fiber reinforced polyether ketone composite material product with the designed structure.
Example 8 carbon fiber reinforced polyetheretherketone ketone
(1) Mixing: taking polyether-ether-ketone powder with a melting point of 370 ℃ and a particle size of 50 mu m as a matrix, taking carbon nanotube modified carbon fibers as a reinforcing phase, and adding the carbon fibers and the polyether-ether-ketone into a high-speed mixer according to a mass ratio of 1:9 to uniformly mix to obtain a mixture;
(2) And (3) extruding and granulating: adding the mixture into a screw extruder for 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 ℃ in sequence, the rotating speed of the screw is 80r/min, and the temperature of a cooling water tank is set to 70 ℃ to obtain composite material particles;
(3) Injection molding: and adding the composite material particles into an injection molding machine, heating to a molten state, and molding by a mold, wherein the injection molding temperature is 220 ℃, the injection molding pressure is 150MPa, and the injection molding period is 30s, so as to obtain the carbon fiber reinforced polyether ketone composite material product with the designed structure.
Comparative example 1 unmodified carbon fiber reinforced polyetheretherketone
The production and evaluation of the product were carried out in the same manner as in example 5, except that the carbon fiber was not modified, and the results are shown in Table 1. The thermal deformation temperature of the sample is slightly lower, and the mechanical property is poor.
Comparative example 2 pure polyetheretherketone
The production and evaluation of the product were carried out in the same manner as in example 5, except that no carbon fiber was added as the reinforcing phase, and the results are shown in Table 1. The thermal deformation temperature of the sample is slightly poor, and the mechanical property is very poor.
Comparative example 3 preparation of composite Material by Hot pressing Process
The composite material product is prepared without adopting extrusion granulation and injection molding processes, carbon fiber and polyether-ether-ketone are mixed, hot-press molding is directly carried out to prepare a plate, and sample performance evaluation is carried out according to the standard, and the results are shown in table 1. The thermal deformation temperature of the sample is basically unchanged, and the mechanical property is deteriorated.
Sample Performance test
Using the composite materials prepared in each example and comparative example as an example, standard sample bars were prepared by the same process, and thermal and mechanical properties of these samples were tested, and the results are shown in Table 1.
Table 1: sample Performance test results
。
Claims (7)
1. The preparation method of the light composite material with excellent mechanical properties at high temperature is characterized by comprising the following steps:
(1) Chopped carbon fiber ammoniation: treating the chopped carbon fiber at high temperature in an ammonia atmosphere to obtain an ammoniated chopped carbon fiber;
(2) Oxidation of nanoscale carbonaceous modifier: treating the nanoscale carbonaceous modifier at a high temperature in an oxygen-containing atmosphere to obtain an oxidized nanoscale carbonaceous modifier;
(3) Modifying ammoniated chopped carbon fibers: fully mixing the ammoniated chopped carbon fiber in the step (1) and the oxidized nano-scale carbonaceous modifier in the step (2) in an aqueous solution, and filtering and drying to obtain modified chopped carbon fiber;
(4) Mixing: uniformly mixing the modified chopped carbon fiber and high-temperature-resistant polyaryletherketone powder to obtain a mixture;
(5) And (3) extruding and granulating: adding the mixture into a screw extruder for melting, mixing, extruding and granulating to obtain composite material particles;
(6) Injection molding: adding the composite material particles into an injection molding machine, heating to a molten state, and molding by a mold to produce composite material products with various structures;
the nanoscale carbonaceous modifier is one or more of carbon nanotubes, graphene, carbon black and carbon nanofibers.
2. The method for preparing the light composite material with excellent mechanical properties at high temperature according to claim 1, wherein the chopped carbon fibers are one or more of chopped polyacrylonitrile-based carbon fibers, chopped pitch-based carbon fibers and chopped viscose-based carbon fibers, and the fiber length is 300 μm-3 cm; the treatment temperature of the ammonia gas atmosphere is 600-1200 ℃, and the treatment time is 0.5-5 h.
3. The method for preparing the light composite material with excellent mechanical properties at high temperature according to claim 1, wherein the oxygen-containing atmosphere is one or more of oxygen, air, ozone or water vapor, the heating temperature is 500-1000 ℃, and the heating time is 0.5-5 h.
4. The method for preparing the light composite material with excellent mechanical properties at high temperature according to claim 1, wherein the mass ratio of the ammoniated chopped carbon fiber to the oxidized nanoscale carbonaceous modifier is 1:0.02-0.2.
5. The method for preparing the light composite material with excellent mechanical properties at high temperature according to claim 1, wherein the high-temperature-resistant polyaryletherketone is one or more of polyetherketone, polyetheretherketone ketone, polyetheretherketone and polyetherketone ketone; the melting temperature of the high-temperature-resistant polyaryletherketone is above 330 ℃, and the particle size of the high-temperature-resistant polyaryletherketone is below 300 mu m; the mass ratio of the modified chopped carbon fiber to the high-temperature-resistant polyaryletherketone is 1:1-9.
6. The method for producing a lightweight composite material excellent in mechanical properties at high temperatures according to claim 1, characterized in that the heating temperature of each stage from a feed port to a die is 250 to 330 ℃, 300 to 380 ℃, 330 to 400 ℃, 350 to 420 ℃, 350 to 450 ℃, 340 to 400 ℃, the screw rotation speed is 50 to 200r/min, and the cooling water tank temperature is set to 40 to 70 ℃.
7. The method for preparing the light composite material with excellent mechanical properties at high temperature according to any one of claims 1 to 6, wherein the injection molding temperature of injection molding is 160-250 ℃, the injection molding pressure is 50-180 MPa, and the injection molding period is 20-50 s.
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