CN117698242A - Reinforced polyaryletherketone composite material with high interface adhesion and preparation method thereof - Google Patents
Reinforced polyaryletherketone composite material with high interface adhesion and preparation method thereof Download PDFInfo
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- CN117698242A CN117698242A CN202311743127.8A CN202311743127A CN117698242A CN 117698242 A CN117698242 A CN 117698242A CN 202311743127 A CN202311743127 A CN 202311743127A CN 117698242 A CN117698242 A CN 117698242A
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- 229920006260 polyaryletherketone Polymers 0.000 title claims abstract description 70
- 239000002131 composite material Substances 0.000 title claims abstract description 61
- 238000002360 preparation method Methods 0.000 title abstract description 24
- 229920000049 Carbon (fiber) Polymers 0.000 claims abstract description 55
- 239000004917 carbon fiber Substances 0.000 claims abstract description 55
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 54
- 238000000034 method Methods 0.000 claims abstract description 44
- 229910052731 fluorine Inorganic materials 0.000 claims abstract description 38
- 239000011737 fluorine Substances 0.000 claims abstract description 38
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims abstract description 37
- 239000000463 material Substances 0.000 claims abstract description 26
- 238000000748 compression moulding Methods 0.000 claims abstract description 17
- 239000004696 Poly ether ether ketone Substances 0.000 claims description 39
- 229920002530 polyetherether ketone Polymers 0.000 claims description 39
- 239000000843 powder Substances 0.000 claims description 17
- 239000002245 particle Substances 0.000 claims description 16
- 238000004513 sizing Methods 0.000 claims description 16
- 239000003795 chemical substances by application Substances 0.000 claims description 14
- 238000001125 extrusion Methods 0.000 claims description 14
- 238000000354 decomposition reaction Methods 0.000 claims description 12
- 238000012545 processing Methods 0.000 claims description 11
- 238000010030 laminating Methods 0.000 claims description 10
- 239000000126 substance Substances 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 9
- CJZGTCYPCWQAJB-UHFFFAOYSA-L calcium stearate Chemical compound [Ca+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O CJZGTCYPCWQAJB-UHFFFAOYSA-L 0.000 claims description 8
- 239000008116 calcium stearate Substances 0.000 claims description 8
- 235000013539 calcium stearate Nutrition 0.000 claims description 8
- 238000005266 casting Methods 0.000 claims description 7
- 238000005469 granulation Methods 0.000 claims description 7
- 230000003179 granulation Effects 0.000 claims description 7
- 239000000314 lubricant Substances 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 239000006185 dispersion Substances 0.000 claims description 5
- 229920001643 poly(ether ketone) Polymers 0.000 claims description 5
- HQKMJHAJHXVSDF-UHFFFAOYSA-L magnesium stearate Chemical compound [Mg+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O HQKMJHAJHXVSDF-UHFFFAOYSA-L 0.000 claims description 4
- 238000006116 polymerization reaction Methods 0.000 claims description 4
- 230000000630 rising effect Effects 0.000 claims description 4
- 239000004593 Epoxy Substances 0.000 claims description 2
- 235000021355 Stearic acid Nutrition 0.000 claims description 2
- 238000003475 lamination Methods 0.000 claims description 2
- 235000019359 magnesium stearate Nutrition 0.000 claims description 2
- 239000000155 melt Substances 0.000 claims description 2
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 2
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 2
- 229920001660 poly(etherketone-etherketoneketone) Polymers 0.000 claims description 2
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 2
- 239000008117 stearic acid Substances 0.000 claims description 2
- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 claims description 2
- 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 claims 1
- 229920001652 poly(etherketoneketone) Polymers 0.000 claims 1
- 239000011229 interlayer Substances 0.000 abstract description 6
- 125000001153 fluoro group Chemical group F* 0.000 abstract 1
- 239000004744 fabric Substances 0.000 description 21
- 229920000642 polymer Polymers 0.000 description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 13
- 238000010438 heat treatment Methods 0.000 description 12
- 230000000052 comparative effect Effects 0.000 description 11
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 9
- 238000001816 cooling Methods 0.000 description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 8
- 239000011259 mixed solution Substances 0.000 description 6
- 239000010410 layer Substances 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- -1 PEKK Polymers 0.000 description 4
- ZFVMWEVVKGLCIJ-UHFFFAOYSA-N bisphenol AF Chemical compound C1=CC(O)=CC=C1C(C(F)(F)F)(C(F)(F)F)C1=CC=C(O)C=C1 ZFVMWEVVKGLCIJ-UHFFFAOYSA-N 0.000 description 4
- 230000005855 radiation Effects 0.000 description 4
- 238000010992 reflux Methods 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 3
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 3
- 238000011084 recovery Methods 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 229920000106 Liquid crystal polymer Polymers 0.000 description 2
- 239000004977 Liquid-crystal polymers (LCPs) Substances 0.000 description 2
- 239000004642 Polyimide Substances 0.000 description 2
- 239000004734 Polyphenylene sulfide Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229920006351 engineering plastic Polymers 0.000 description 2
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 239000012467 final product Substances 0.000 description 2
- 238000007731 hot pressing Methods 0.000 description 2
- 230000007774 longterm Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 229920001721 polyimide Polymers 0.000 description 2
- 229920000069 polyphenylene sulfide Polymers 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 229920006395 saturated elastomer Polymers 0.000 description 2
- 238000002791 soaking Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229920008285 Poly(ether ketone) PEK Polymers 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000007723 die pressing method Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000003733 fiber-reinforced composite Substances 0.000 description 1
- 229920006258 high performance thermoplastic Polymers 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000005470 impregnation Methods 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000005461 lubrication Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 229920000110 poly(aryl ether sulfone) Polymers 0.000 description 1
- 238000006068 polycondensation reaction Methods 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000006277 sulfonation reaction Methods 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 229920001169 thermoplastic Polymers 0.000 description 1
- 239000004416 thermosoftening plastic Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/28—Layered products comprising a layer of synthetic resin comprising synthetic resins not wholly covered by any one of the sub-groups B32B27/30 - B32B27/42
- B32B27/285—Layered products comprising a layer of synthetic resin comprising synthetic resins not wholly covered by any one of the sub-groups B32B27/30 - B32B27/42 comprising polyethers
-
- 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
- B29C70/00—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts
- B29C70/04—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts comprising reinforcements only, e.g. self-reinforcing plastics
- B29C70/28—Shaping operations therefor
- B29C70/30—Shaping by lay-up, i.e. applying fibres, tape or broadsheet on a mould, former or core; Shaping by spray-up, i.e. spraying of fibres on a mould, former or core
- B29C70/34—Shaping by lay-up, i.e. applying fibres, tape or broadsheet on a mould, former or core; Shaping by spray-up, i.e. spraying of fibres on a mould, former or core and shaping or impregnating by compression, i.e. combined with compressing after the lay-up operation
- B29C70/345—Shaping by lay-up, i.e. applying fibres, tape or broadsheet on a mould, former or core; Shaping by spray-up, i.e. spraying of fibres on a mould, former or core and shaping or impregnating by compression, i.e. combined with compressing after the lay-up operation using matched moulds
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29D—PRODUCING PARTICULAR ARTICLES FROM PLASTICS OR FROM SUBSTANCES IN A PLASTIC STATE
- B29D7/00—Producing flat articles, e.g. films or sheets
- B29D7/01—Films or sheets
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/06—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material
- B32B27/08—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/12—Layered products comprising a layer of synthetic resin next to a fibrous or filamentary layer
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B38/00—Ancillary operations in connection with laminating processes
- B32B38/0036—Heat treatment
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B7/00—Layered products characterised by the relation between layers; Layered products characterised by the relative orientation of features between layers, or by the relative values of a measurable parameter between layers, i.e. products comprising layers having different physical, chemical or physicochemical properties; Layered products characterised by the interconnection of layers
- B32B7/04—Interconnection of layers
- B32B7/10—Interconnection of layers at least one layer having inter-reactive properties
-
- 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
- C08J5/18—Manufacture of films or sheets
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2262/00—Composition or structural features of fibres which form a fibrous or filamentary layer or are present as additives
- B32B2262/10—Inorganic fibres
- B32B2262/106—Carbon fibres, e.g. graphite fibres
-
- 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
- C08J2371/08—Polyethers derived from hydroxy compounds or from their metallic derivatives
- C08J2371/10—Polyethers derived from hydroxy compounds or from their metallic derivatives from phenols
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Mechanical Engineering (AREA)
- Medicinal Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Composite Materials (AREA)
- Materials Engineering (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Laminated Bodies (AREA)
Abstract
The invention relates to a high-interface bonding reinforced polyaryletherketone composite material and a preparation method thereof, wherein the reinforced polyaryletherketone composite material comprises a plurality of unit structures which are laminated and pressed, and the layering of the unit structures is as follows from bottom to top in sequence: the first film, the second film, the carbon fiber and the second film; wherein the material of the first film is polyaryletherketone; the material of the second film is fluorine-containing polyaryletherketone, and the atomic percentage of fluorine contained in the fluorine-containing polyaryletherketone is more than 25%; the fluorine-containing polyaryletherketone film with high fluorine content is used as an intermediate bonding material of the carbon fiber and the polyaryletherketone film material, and the interface bonding performance between the carbon fiber and the polyaryletherketone can be enhanced to a great extent through high-temperature compression molding, so that the composite material has better interface bonding strength and is not easy to peel; the composite material obtained by the method has interlayer shear strength of more than 100 MPa; the method has the advantages of few steps, simplicity, practicability, good stability and convenience for realizing industrialization.
Description
Technical Field
The invention relates to the technical field of polymer material processing, in particular to a high-interface bonding reinforced polyaryletherketone composite material and a preparation method thereof.
Background
The high-temperature resistant (mainly refers to special engineering plastics with the long-term use temperature of more than 200 ℃) and mainly comprises Polyimide (PI), polyether ether ketone (PEEK), polyether ketone (PEKK), polyether ketone (PEK), polyphenylene sulfide (PPS), liquid Crystal Polymer (LCP) and the like, and the special engineering plastics have excellent physical properties and are widely applied to high-tech fields such as aerospace, military industry, electron and electricity, analytical instruments, semiconductors, petrochemical industry and the like.
Polyether ether ketone (PEEK) is taken as an example, has the characteristics of super corrosion resistance, wear resistance, excellent self-lubrication, hydrolysis resistance and the like when the long-term use temperature reaches more than 260 ℃, and is considered to be the thermoplastic high polymer with the most excellent comprehensive performance at present. The continuous carbon fiber reinforced polyaryletherketone composite material is used as an emerging high-performance thermoplastic composite material, has more excellent performance, can meet more severe application conditions, such as the thermal deformation temperature is more than 300 ℃, the tensile strength is more than 8 times that of a pure PEEK material, the specific strength is far higher than that of metal materials such as steel, aluminum alloy and the like, and can be used for replacing metals in high-end fields such as aerospace military industry and the like. However, the sizing agent on the surface of the conventional carbon fiber is generally decomposed at about 200 ℃, and the forming temperature of the polyaryletherketone resin is generally above 350 ℃, so that when the continuous fiber reinforced composite material is caused, the interface bonding is weak, and the performance of the composite material is affected.
The current common means is to introduce a novel high-temperature resistant sizing agent on the surface of carbon fiber, for example, the invention patent CN 111423694B discloses a CF/PEEK composite material with high interlayer shear strength and a preparation method thereof, wherein the preparation method comprises the following steps: (1) decomposing the original sizing agent on the surface of the CF at high temperature; (2) In a saturated steam environment, carrying out microwave radiation and ultraviolet radiation on CF simultaneously, and marking a product as ACF; (3) Immersing ACF into a polyether ketone oligomer/dichloromethane solution, taking out and drying to obtain sizing modified carbon fiber MCF; (4) hot pressing the MCF with the PEEK material stack; obtaining the CF/PEEK composite material with high interlayer shear strength; the interlayer shear strength is 80-90MPa; as another example, invention patent CN 111440342B discloses a CF/PEEK composite material with a strong interface of chemical bonds and a method for preparing the same, the method comprising the steps of: (1) decomposing the original sizing agent on the surface of the CF at high temperature; (2) In a saturated steam environment, carrying out microwave radiation and ultraviolet radiation on CF simultaneously, and marking a product as ACF; (3) Immersing ACF into an aminated PEEK/dimethylformamide/carbon nano tube suspension, heating to enable the aminated PEEK to react with the ACF, taking out and drying to obtain sizing modified carbon fiber MCF; (4) hot pressing the MCF with the PEEK material stack; obtaining the CF/PEEK composite material with a strong interface of chemical bonds; the final interface shear strength is 100-120MPa. The patent aims at improving the interfacial bonding strength of the CF and PEEK composite material, adopts the means of carrying out physical and chemical treatment on the surface of the carbon fiber, and connecting corresponding polyether ketone oligomer, aminated PEEK and the like, adopts the forming mode of CF and PEEK film die pressing, and also obtains better results, the interlayer shearing strength is improved to 80-90MPa and 100-120MPa, but the preparation method has more steps, focuses on microscopic modification, and is easy to have the problems of insufficient stability and difficult realization of large-scale production.
Disclosure of Invention
In order to solve the technical problem of weak interface combination of carbon fiber and polyaryletherketone, a reinforced polyaryletherketone composite material with high interface bonding and a preparation method thereof are provided. The composite material obtained by the method has higher interface bonding strength.
In order to achieve the above purpose, the invention is realized by the following technical scheme:
the reinforced polyaryletherketone composite material with high interface bonding comprises a plurality of unit structures which are laminated and pressed, wherein the layering of the unit structures is as follows from bottom to top: the first film, the second film, the carbon fiber and the second film;
wherein the material of the first film is polyaryletherketone; the second film is made of fluorine-containing polyaryletherketone, the atomic percentage of fluorine-containing elements is more than 25%, and the higher the fluorine content is, the obvious enhancement effect on the improvement of interface bonding strength is achieved.
Further, when the repetition amount of the unit structure is defined as N, the total number of carbon fiber layers in the laminated structure of the composite material is N sheets, the total number of first film layers is n+1 sheets, and the total number of second film layers is 2N sheets.
Further, the chemical structure of the fluorine-containing polyaryletherketone is as follows:
wherein N represents the degree of polymerization, the number average molecular weight M of the fluorine-containing polyaryletherketone N The molecular weight dispersion coefficient is 1.5-2.5, and the atomic percentage of fluorine element is 36.44%.
Still further, the method for obtaining the second film comprises the following steps: drying fluorine-containing polyaryletherketone powder, uniformly mixing the powder with a lubricant, and carrying out melt extrusion granulation to obtain fluorine-containing polyaryletherketone particles; preparing the fluorine-containing polyaryletherketone particles into a second film by an extrusion casting method;
the lubricant is one or more of stearic acid, zinc stearate, magnesium stearate, calcium stearate and PTFE, and the adding amount of the lubricant is 0.1-0.5% of the fluorine-containing polyaryletherketone powder;
wherein the processing temperature of the melt extrusion granulation is 360-420 ℃;
wherein the extrusion casting method has the following technological parameters of barrel temperature: first area 370-375 ℃, second area 370-375 ℃, third area 375-380 ℃, fourth area 375-380 ℃, fifth area 385-390 ℃, runner temperature setting 375-380 ℃, and mold temperature setting 360-365 ℃; setting roller temperature: front roller 175-180deg.C, middle roller 175-180deg.C, and rear roller 152-157 deg.C; the rotating speed of the host machine is 25-27r/min, and the current is 70-72A;
the thickness of the second film is 0.01-0.05mm, the width is 100-1500mm, and the length is continuously extruded.
Further, the polyaryletherketone is one or more of PEEK, PEK, PEKK, PEKEKK; the thickness of the first film is 0.1-0.8mm.
Further, the carbon fiber is continuous carbon fiber and the original sizing agent on the surface of the carbon fiber is removed;
the method for removing the original sizing agent on the surface of the carbon fiber is a high-temperature decomposition method, wherein the high-temperature decomposition method is to place the carbon fiber in an environment of 180-300 ℃ for at least 2 hours, and the original epoxy sizing agent on the surface of the carbon fiber can be thermally decomposed at high temperature.
The preparation method of the reinforced polyaryletherketone composite material with high interface adhesion comprises the following steps:
stacking a plurality of unit structures, wherein the layering of the unit structures is as follows from bottom to top: and laminating a layer of first film on the surface of the second film of the N unit after lamination, and performing compression molding to obtain the reinforced polyaryletherketone composite material with high interface adhesion.
Further, the temperature is raised to 370-400 ℃ at the temperature rising rate of 5-20 ℃/min during compression molding, the pressure is continuously increased to 0.5-3.5MPa during the temperature rising process, the processing time is 8-20h, and then the temperature is reduced to room temperature at the temperature reducing rate of 10-20 ℃/min.
The beneficial technical effects are as follows:
the fluorine-containing polyaryletherketone film with high fluorine content is used as an intermediate bonding material of the carbon fiber and the polyaryletherketone film material, and the fluorine-containing polyaryletherketone material with high fluorine content has high polarity, high impregnation force and high bonding force, so that the interfacial bonding performance between the carbon fiber and the polyaryletherketone can be enhanced to a great extent through high-temperature compression molding, and the composite material has high interfacial bonding strength and is not easy to peel; the composite material obtained by the method has interlayer shear strength of more than 100 MPa; the method has the advantages of few steps, simplicity, practicability, good stability and convenience for realizing industrialization.
Drawings
Fig. 1 is a composite lay-up structure.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and fully with reference to the accompanying drawings, in which it is evident that the embodiments described are only some, but not all embodiments of the invention. The following description of at least one exemplary embodiment is merely exemplary in nature and is in no way intended to limit the invention, its application, or uses. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The numerical values set forth in these examples do not limit the scope of the present invention unless specifically stated otherwise. Techniques, methods known to those of ordinary skill in the relevant art may not be discussed in detail, but should be considered part of the specification where appropriate. In all examples shown and discussed herein, any specific values should be construed as merely illustrative, and not a limitation. Thus, other examples of the exemplary embodiments may have different values.
In addition, the words "first", "second", etc. are used to define the film only for convenience of distinguishing the layers, and the words are not specifically defined unless otherwise stated, and therefore should not be construed as limiting the scope of the present invention.
The experimental methods in the following examples, for which specific conditions are not noted, are generally determined according to national standards; if the national standard is not corresponding, the method is carried out according to the general international standard or the standard requirements set by related enterprises.
The following process for preparing fluorine-containing polyaryletherketone (hereinafter abbreviated as F-PAEK) is described in China patent application No. 202311293270.1 of Shandong Jun-Hao high Performance Polymer Co., ltd, and the process for preparing the polymer, specifically, the polycondensation reaction product of 3,3 '-bis (3, 5-bis (trifluoromethyl) phenyl) -4,4' -difluorobenzophenone and hexafluorobisphenol A is described in detail in example 3.
Preparation example 1
The chemical structure of the fluorine-containing polyaryletherketone is as follows:
the preparation method comprises the following steps: into a 100L reactor equipped with a mechanical stirrer, a nitrogen inlet and outlet, a water separator and reflux condensation, 2.714kg (4 mol) of 3,3 '-bis (3, 5-bis (trifluoromethyl) phenyl) -4,4' -difluorobenzophenone, 1.345kg (4 mol) of hexafluorobisphenol A,0.72kg (5.2 mol) of anhydrous K were added 2 CO 3 14LDMAc and 6L toluene; n (N) 2 Stirring, heating and refluxing at 140 ℃ for 3 hours under atmosphere, and then mixing the produced water with the firstBenzene azeotropes, and azeotropes are removed by a water separator; then, continuously stirring at 160 ℃ to perform polymerization reaction for 8.5 hours to obtain a viscous mixed solution; pouring the viscous mixed solution into 240L of mixed solution of ethanol and water (volume ratio is 1:1) to precipitate a polymer; soaking for 40min with hot ethanol water solution (volume ratio of ethanol to water is 1:2, and temperature is 80 ℃) for three times, filtering and drying to obtain fluorine-containing polyaryletherketone powder, wherein the number average molecular weight of the polymer is 8 ten thousand g/mol, and the molecular weight dispersion coefficient is 1.8 according to GPC test; the polymer was designated as F-PAEK-1 and contained 36.44 atomic percent of fluorine.
Preparation example 2
The chemical structure of the fluorine-containing polyaryletherketone is as follows:
the preparation method comprises the following steps: 2.714kg (4 mol) of 3,3 '-bis (3, 5-bis (trifluoromethyl) phenyl) -4,4' -difluorobenzophenone, 1.345kg (4 mol) of hexafluorobisphenol A,0.72kg (5.2 mol) of anhydrous K were charged into a 100L reactor equipped with a mechanical stirrer, a nitrogen inlet and outlet, a water separator and a reflux condenser 2 CO 3 14L of DMAc and 6L of toluene; n (N) 2 Stirring and heating at 140 ℃ for reflux reaction for 2.5 hours under atmosphere, and then azeotroping generated water and toluene, and removing azeotrope through a water separator; then, continuously stirring at 160 ℃ to perform polymerization reaction for 7.5 hours to obtain a viscous mixed solution; pouring the viscous mixed solution into 240L of mixed solution of ethanol and water (volume ratio is 1:1) to precipitate a polymer; soaking for 35min with hot ethanol water solution (volume ratio of ethanol to water is 1:2, and temperature is 80 ℃) for three times, filtering and drying to obtain fluorine-containing polyaryletherketone powder, wherein the number average molecular weight of the polymer is 6 ten thousand g/mol, and the molecular weight dispersion coefficient is 1.5 according to GPC test; the polymer was designated as F-PAEK-2 and contained 36.44 atomic percent of fluorine. The polymer of this example has a lower molecular weight than F-PAEK-1 and is therefore weaker than F-PAEK-1 in terms of interfacial adhesion and toughness.
Preparation example 3
The case is the preparation of hexafluorobisphenol A type polyaryletherketone, and the chemical structure is as follows:
synthetic method reference: jiang Zhenyu the synthesis and properties of polyaryletherketone and polyarylethersulfone containing hexafluoroisopropane structure [ J ]. University of Industry of China (Nature science edition), 2007, volume 33, 3 rd phase, P345-349, the polymer of this example is designated PAEK-AF, and the atomic percentage of fluorine contained is 22.18%.
Preparation example 4
The present case is sulfonated polyether ether ketone, denoted S-PEEK, with a degree of sulfonation of 36% and provided by Shandong Jun-Hao high performance Polymer Co., ltd.
Example 1
The reinforced polyaryletherketone composite material with high interface adhesion in the present case comprises a stack of N unit structures 10, wherein the stacks of the unit structures are sequentially from bottom to top: the method comprises the steps of laminating a first film 1 on the surface of a second film 2 with an N-th unit structure after laminating a first film 1, a second film 2, carbon fibers 3 and a second film 2, and performing compression molding to obtain a reinforced polyaryletherketone composite material with high interface adhesion, wherein the schematic cross-sectional structure of the composite material is shown in figure 1;
the material of the first film 1 is polyether-ether-ketone, the thickness of the PEEK film is 0.4mm, and the PEEK film is provided by Jiangsu junhua special high polymer material Co., ltd;
wherein the material of the second film 2 is F-PAEK-1 of preparation example 1, the thickness of the F-PAEK-1 film is 0.02mm, the width is 1000mm, and the length is continuously extruded; the obtaining method comprises the following steps: (1) F-PAEK-1 powder is dried for 5 hours at the temperature of 180 ℃ to remove water; mixing F-PAEK-1 powder with calcium stearate (calcium stearate accounts for 0.2% of the weight of the F-PAEK powder), adding into a feed port, performing melt extrusion granulation, setting the processing temperature to be 380 ℃, and setting the conveyor belt speed to be 12Hz to obtain F-PAEK-1 particles with the diameter of 2mm and the length of 3mm; (2) Drying F-PAEK-1 particles in an oven to remove moisture in the particles, wherein the treatment temperature is 180 ℃ and the treatment time is 6 hours; adding the dried particles into a feed hopper, and adjusting an extrusion casting process to obtain the F-PAEK-1 film, wherein the process is as follows: barrel temperature of first zone 370-375 ℃, second zone 370-375 ℃, third zone 375-380 ℃, fourth zone 375-380 ℃, fifth zone 385-390 ℃, runner temperature setting 375-380 ℃, mold temperature setting 360-365 ℃, roller temperature setting: front roller 175-180 deg.c, middle roller 175-180 deg.c, back roller 152-157 deg.c, main machine rotation speed 25-27r/min and current 70-72A;
wherein the carbon fiber 3 is carbon fiber cloth (12K, 230 g/cm) 2 ) The carbon fiber cloth is provided by a middle recovery eagle; removing the original sizing agent from the carbon fiber cloth by adopting a high-temperature decomposition method, wherein the high-temperature decomposition method is to place the carbon fiber cloth in an environment of 220 ℃ for 5 hours;
the preparation method of the composite material comprises the following steps: layering according to the structure shown in the above figure 1, setting n=12, namely, 12 carbon fiber cloth, 13 PEEK films and 24F-PAEK-1 films are needed, performing compression molding, heating to 385 ℃ at the heating rate of 10 ℃/min during compression molding, continuously pressurizing to 1.2MPa in the heating process, keeping the total processing time for 15h, then cooling to room temperature at the cooling rate of 15 ℃/min, keeping the highest temperature for 40min, and cooling to room temperature to obtain the reinforced polyaryletherketone composite material with high interface adhesion.
Example 2
The reinforced polyaryletherketone composite material with high interface adhesion in the present case comprises a stack of N unit structures 10, wherein the stacks of the unit structures are sequentially from bottom to top: the method comprises the steps of laminating a first film 1 on the surface of a second film 2 with an N-th unit structure after laminating a first film 1, a second film 2, carbon fibers 3 and a second film 2, and performing compression molding to obtain a reinforced polyaryletherketone composite material with high interface adhesion, wherein the schematic cross-sectional structure of the composite material is shown in figure 1;
the material of the first film 1 is polyether-ether-ketone, the thickness of the PEEK film is 0.4mm, and the PEEK film is provided by Jiangsu junhua special high polymer material Co., ltd;
wherein the material of the second film 2 is F-PAEK-2,F-PAEK-2 film of preparation example 2, the thickness is 0.03mm, the width is 1000mm, and the length is continuously extruded; the obtaining method comprises the following steps: (1) F-PAEK-2 powder is dried for 5 hours at the temperature of 180 ℃ to remove water; mixing F-PAEK-2 powder with calcium stearate (calcium stearate accounts for 0.2% of the weight of the F-PAEK powder), adding into a feed port, performing melt extrusion granulation, wherein the processing temperature is 390 ℃, and the speed of a conveyor belt is 12Hz to obtain F-PAEK-2 particles with the diameter of 2mm and the length of 3mm; (2) Drying F-PAEK-2 particles in an oven to remove moisture in the particles, wherein the treatment temperature is 180 ℃ and the treatment time is 6 hours; adding the dried particles into a feed hopper, and adjusting an extrusion casting process to obtain the F-PAEK-2 film, wherein the process is as follows: barrel temperature of first zone 370-375 ℃, second zone 370-375 ℃, third zone 375-380 ℃, fourth zone 375-380 ℃, fifth zone 385-390 ℃, runner temperature setting 375-380 ℃, mold temperature setting 360-365 ℃, roller temperature setting: front roller 175-180 deg.c, middle roller 175-180 deg.c, back roller 152-157 deg.c, main machine rotation speed 25-27r/min and current 70-72A;
wherein the carbon fiber 3 is carbon fiber cloth (12K, 230 g/cm) 2 ) The carbon fiber cloth is provided by a middle recovery eagle; removing the original sizing agent from the carbon fiber cloth by adopting a high-temperature decomposition method, wherein the high-temperature decomposition method is to place the carbon fiber cloth in an environment of 250 ℃ for 10 hours;
the preparation method of the composite material comprises the following steps: layering according to the structure shown in the above figure 1, setting n=12, namely, 12 carbon fiber cloth, 13 PEEK films and 24F-PAEK-2 films are required, performing compression molding, heating to 395 ℃ at a heating rate of 15 ℃/min during compression molding, continuously pressurizing to 2MPa in the heating process, keeping the total processing time for 12 hours, then cooling to room temperature at a cooling rate of 20 ℃/min, keeping the highest temperature for 60min, and cooling to room temperature to obtain the reinforced polyaryletherketone composite material with high interface adhesion.
Example 3
The reinforced polyaryletherketone composite material with high interface adhesion in the present case comprises a stack of N unit structures 10, wherein the stacks of the unit structures are sequentially from bottom to top: the method comprises the steps of laminating a first film 1 on the surface of a second film 2 with an N-th unit structure after laminating a first film 1, a second film 2, carbon fibers 3 and a second film 2, and performing compression molding to obtain a reinforced polyaryletherketone composite material with high interface adhesion, wherein the schematic cross-sectional structure of the composite material is shown in figure 1;
the material of the first film 1 is polyether-ether-ketone, the thickness of the PEEK film is 0.5mm, and the PEEK film is provided by Jiangsu junhua special high polymer material Co., ltd;
wherein the material of the second film 2 is F-PAEK-2,F-PAEK-2 film of preparation example 2, the thickness is 0.03mm, the width is 1000mm, and the length is continuously extruded; the obtaining method comprises the following steps: (1) F-PAEK-2 powder is dried for 5 hours at the temperature of 180 ℃ to remove water; mixing F-PAEK-2 powder with calcium stearate (calcium stearate accounts for 0.2% of the weight of the F-PAEK powder), adding into a feed port, performing melt extrusion granulation, setting the processing temperature to 385 ℃, and setting the conveyor belt speed to 12Hz to obtain F-PAEK-2 particles with the diameter of 2mm and the length of 3mm; (2) Drying F-PAEK-2 particles in an oven to remove moisture in the particles, wherein the treatment temperature is 180 ℃ and the treatment time is 6 hours; adding the dried particles into a feed hopper, and adjusting an extrusion casting process to obtain the F-PAEK-2 film, wherein the process is as follows: barrel temperature of first zone 370-375 ℃, second zone 370-375 ℃, third zone 375-380 ℃, fourth zone 375-380 ℃, fifth zone 385-390 ℃, runner temperature setting 375-380 ℃, mold temperature setting 360-365 ℃, roller temperature setting: front roller 175-180 deg.c, middle roller 175-180 deg.c, back roller 152-157 deg.c, main machine rotation speed 25-27r/min and current 70-72A;
wherein the carbon fiber 3 is carbon fiber cloth (12K, 230 g/cm) 2 ) The carbon fiber cloth is provided by a middle recovery eagle; removing the original sizing agent from the carbon fiber cloth by adopting a high-temperature decomposition method, wherein the high-temperature decomposition method is to place the carbon fiber cloth in an environment of 280 ℃ for 4 hours;
the preparation method of the composite material comprises the following steps: layering according to the structure shown in fig. 1, setting n=10, namely 10 carbon fiber cloths, 11 PEEK films and 20F-PAEK-2 films, performing compression molding, heating to 375 ℃ at a heating rate of 5 ℃/min during compression molding, continuously pressurizing to 3MPa in the heating process, keeping the total processing time at 18h, then cooling to room temperature at a cooling rate of 10 ℃/min, keeping the highest temperature for 50min, and cooling to room temperature to obtain the reinforced polyaryletherketone composite material with high interface adhesion.
Comparative example 1
The carbon fiber cloth is manufactured by alternately laminating and compression molding carbon fiber cloth and PEEK films which are not treated by a high-temperature decomposition method, wherein 12 carbon fiber cloth blocks and 13 PEEK films are used; the materials used and the process parameters were identical to those of example 1.
Comparative example 2
The carbon fiber cloth is prepared by alternately laminating and compression molding carbon fiber cloth and PEEK films treated by a high-temperature decomposition method, wherein the total number of the carbon fiber cloth is 12, and the total number of the PEEK films is 13; the materials used and the process parameters were identical to those of example 1.
Comparative example 3
The composite material of this comparative example was prepared in the same manner as in example 1, except that the material of the second film was PAEK-AF, and the film was prepared in the same manner as in example 1.
Comparative example 4
The composite material of this comparative example was prepared in the same manner as in example 1, except that the material of the second film was S-PEEK of preparation example 3, and the preparation process of the film was the same as in example 1.
Comparative example 5
The composite of this comparative example was prepared in the same manner as in example 1, except that the material of the second film had the following chemical structure:
the polymer was obtained with reference to the final product of example 1 in chinese patent application No. 202311293270.1, of the company Shandong jun high performance polymer limited; the film was prepared in the same manner as in example 1.
Comparative example 6
The composite of this comparative example was prepared in the same manner as in example 1, except that the material of the second film had the following chemical structure:
the polymer was obtained with reference to the final product of example 2 in chinese patent application No. 202311293270.1, of the company Shandong jun high performance polymer limited; the film was prepared in the same manner as in example 1.
The composite materials obtained above were subjected to performance tests, and specific results are shown in table 1 below.
Table 1 composite properties for each case
From the results, when only carbon fiber cloth and PEEK film are adopted for compounding, the interlaminar shear strength (ILSS) of the composite material is only 53MPa, which also shows that the interface bonding performance of PEEK and carbon fiber is poor, thereby affecting the overall service performance and service life of the material; after the original sizing agent on the surface of the carbon fiber is removed at high temperature, the ILSS of the composite material is improved to 72MPa. After the F-PAEK-1 film is used, the ILSS of the composite material is raised to 112MPa, and in comparative examples 3, 4, 5 and 6, the ILSS value of the composite material added with different second films is improved, but the improvement value of the embodiment 1 is the largest, and the interface bonding force is stronger because the second film F-PAEK-1 contains higher proportion of fluorine content; in examples 2-3, F-PAEK-2 was used which had the same fluorine content, but a small molecular weight (6 ten thousand g/mol), and the interfacial adhesion and toughness were reduced, which also reduced the composite properties as compared to example 1. In example 3, the F-PAEK-2 film used was thicker than that of example 2, the adhesion was enhanced, and the properties of the composite were also improved.
The foregoing is only a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art, who is within the scope of the present invention, should make equivalent substitutions or modifications according to the technical scheme of the present invention and the inventive concept thereof, and should be covered by the scope of the present invention.
Claims (8)
1. The reinforced polyaryletherketone composite material with high interface adhesion is characterized by comprising a plurality of unit structures which are laminated and pressed, wherein the layering of the unit structures is formed by sequentially: the first film, the second film, the carbon fiber and the second film;
wherein the material of the first film is polyaryletherketone; the second film is made of fluorine-containing polyaryletherketone, and the atomic percentage of fluorine contained in the fluorine-containing polyaryletherketone is more than 25%.
2. The reinforced polyaryletherketone composite material of claim 1, wherein the total number of carbon fiber layers in the laminated structure of the composite material is N, the total number of first film layers is n+1, and the total number of second film layers is 2N, when the repetition amount of the unit structure is defined as N.
3. The high interface adhesion reinforced polyaryletherketone composite of claim 1, wherein the fluorine-containing polyaryletherketone has the chemical structure:
wherein N represents the degree of polymerization, the number average molecular weight M of the fluorine-containing polyaryletherketone N The molecular weight dispersion coefficient is 1.5-2.5, and the molecular weight dispersion coefficient is 1 ten thousand-10 ten thousand g/mol.
4. A reinforced polyaryletherketone composite having high interfacial adhesion as claimed in claim 3, wherein said second film is obtained by: drying fluorine-containing polyaryletherketone powder, uniformly mixing the powder with a lubricant, and carrying out melt extrusion granulation to obtain fluorine-containing polyaryletherketone particles; preparing the fluorine-containing polyaryletherketone particles into a second film by an extrusion casting method;
the lubricant is one or more of stearic acid, zinc stearate, magnesium stearate, calcium stearate and PTFE, and the adding amount of the lubricant is 0.1-0.5% of the fluorine-containing polyaryletherketone powder;
wherein the processing temperature of the melt extrusion granulation is 360-420 ℃;
wherein the extrusion casting method has the following technological parameters of barrel temperature: first area 370-375 ℃, second area 370-375 ℃, third area 375-380 ℃, fourth area 375-380 ℃, fifth area 385-390 ℃, runner temperature setting 375-380 ℃, and mold temperature setting 360-365 ℃; setting roller temperature: front roller 175-180deg.C, middle roller 175-180deg.C, and rear roller 152-157 deg.C; the rotating speed of the host machine is 25-27r/min, and the current is 70-72A;
the thickness of the second film is 0.01-0.05mm, the width is 100-1500mm, and the length is continuously extruded.
5. The high interfacial adhesion reinforced polyaryletherketone composite of claim 1, wherein the polyaryletherketone is one or more of PEEK, PEK, PEKK, PEKEKK; the thickness of the first film is 0.1-0.8mm.
6. The high interfacial adhesion reinforced polyaryletherketone composite material of claim 1, wherein the carbon fiber is a continuous carbon fiber and the original sizing agent on the surface thereof is removed;
the method for removing the original sizing agent on the surface of the carbon fiber is a high-temperature decomposition method, wherein the high-temperature decomposition method is to place the carbon fiber in an environment of 180-300 ℃ for at least 2 hours, and the original epoxy sizing agent on the surface of the carbon fiber can be thermally decomposed at high temperature.
7. The method for preparing the reinforced polyaryletherketone composite material with high interfacial adhesion according to any one of claims 1 to 6, comprising the steps of:
stacking a plurality of unit structures, wherein the layering of the unit structures is as follows from bottom to top: and laminating a layer of first film on the surface of the second film of the N unit after lamination, and performing compression molding to obtain the reinforced polyaryletherketone composite material with high interface adhesion.
8. The method for preparing the reinforced polyaryletherketone composite material with high interface adhesion according to claim 7, wherein the temperature is raised to 370-400 ℃ at a temperature rising rate of 5-20 ℃/min during compression molding, the pressure is continuously increased to 0.5-3.5MPa during the temperature rising process, the processing time is 8-20h, and then the temperature is reduced to room temperature at a temperature reducing rate of 10-20 ℃/min.
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