CN116836516B - Carbon fiber molded mobile phone middle frame and preparation method thereof - Google Patents
Carbon fiber molded mobile phone middle frame and preparation method thereof Download PDFInfo
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- CN116836516B CN116836516B CN202310717675.7A CN202310717675A CN116836516B CN 116836516 B CN116836516 B CN 116836516B CN 202310717675 A CN202310717675 A CN 202310717675A CN 116836516 B CN116836516 B CN 116836516B
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- 229920000049 Carbon (fiber) Polymers 0.000 title claims abstract description 121
- 239000004917 carbon fiber Substances 0.000 title claims abstract description 120
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 115
- 238000002360 preparation method Methods 0.000 title claims abstract description 29
- 238000007598 dipping method Methods 0.000 claims abstract description 47
- 239000004696 Poly ether ether ketone Substances 0.000 claims abstract description 46
- 229920002530 polyetherether ketone Polymers 0.000 claims abstract description 46
- 239000004642 Polyimide Substances 0.000 claims abstract description 43
- 229920001721 polyimide Polymers 0.000 claims abstract description 43
- 229910052746 lanthanum Inorganic materials 0.000 claims abstract description 38
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 claims abstract description 38
- 239000005416 organic matter Substances 0.000 claims abstract description 30
- 238000003825 pressing Methods 0.000 claims abstract description 19
- 239000007788 liquid Substances 0.000 claims abstract description 18
- CHTHALBTIRVDBM-UHFFFAOYSA-N furan-2,5-dicarboxylic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)O1 CHTHALBTIRVDBM-UHFFFAOYSA-N 0.000 claims abstract description 16
- 150000001412 amines Chemical class 0.000 claims abstract description 12
- IWBOPFCKHIJFMS-UHFFFAOYSA-N ethylene glycol bis(2-aminoethyl) ether Chemical compound NCCOCCOCCN IWBOPFCKHIJFMS-UHFFFAOYSA-N 0.000 claims abstract description 12
- KUCOHFSKRZZVRO-UHFFFAOYSA-N terephthalaldehyde Chemical compound O=CC1=CC=C(C=O)C=C1 KUCOHFSKRZZVRO-UHFFFAOYSA-N 0.000 claims abstract description 12
- YCGAZNXXGKTASZ-UHFFFAOYSA-N thiophene-2,5-dicarboxylic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)S1 YCGAZNXXGKTASZ-UHFFFAOYSA-N 0.000 claims abstract description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 66
- GLUUGHFHXGJENI-UHFFFAOYSA-N Piperazine Chemical compound C1CNCCN1 GLUUGHFHXGJENI-UHFFFAOYSA-N 0.000 claims description 44
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 33
- 239000000243 solution Substances 0.000 claims description 28
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 20
- 235000019441 ethanol Nutrition 0.000 claims description 20
- 238000010438 heat treatment Methods 0.000 claims description 20
- 239000004952 Polyamide Substances 0.000 claims description 19
- 229920002647 polyamide Polymers 0.000 claims description 19
- NAQMVNRVTILPCV-UHFFFAOYSA-N hexane-1,6-diamine Chemical compound NCCCCCCN NAQMVNRVTILPCV-UHFFFAOYSA-N 0.000 claims description 18
- 238000002156 mixing Methods 0.000 claims description 18
- 239000003822 epoxy resin Substances 0.000 claims description 14
- 239000004744 fabric Substances 0.000 claims description 14
- 229920000647 polyepoxide Polymers 0.000 claims description 14
- 239000002131 composite material Substances 0.000 claims description 13
- 229940101545 mi-acid Drugs 0.000 claims description 13
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 12
- 150000001721 carbon Chemical class 0.000 claims description 11
- 238000001035 drying Methods 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 10
- 229910052757 nitrogen Inorganic materials 0.000 claims description 10
- 238000005406 washing Methods 0.000 claims description 10
- ZWWQRMFIZFPUAA-UHFFFAOYSA-N dimethyl 2-methylidenebutanedioate Chemical compound COC(=O)CC(=C)C(=O)OC ZWWQRMFIZFPUAA-UHFFFAOYSA-N 0.000 claims description 9
- 238000006243 chemical reaction Methods 0.000 claims description 7
- GJKFIJKSBFYMQK-UHFFFAOYSA-N lanthanum(3+);trinitrate;hexahydrate Chemical compound O.O.O.O.O.O.[La+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O GJKFIJKSBFYMQK-UHFFFAOYSA-N 0.000 claims description 7
- 239000003208 petroleum Substances 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 5
- 238000005520 cutting process Methods 0.000 claims description 5
- 238000001704 evaporation Methods 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 5
- 239000011259 mixed solution Substances 0.000 claims description 5
- 238000002791 soaking Methods 0.000 claims description 5
- 239000002904 solvent Substances 0.000 claims description 5
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 238000004519 manufacturing process Methods 0.000 claims description 2
- -1 polytetrafluoroethylene Polymers 0.000 claims description 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 2
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 2
- 230000017525 heat dissipation Effects 0.000 abstract description 12
- 239000002994 raw material Substances 0.000 abstract description 8
- 239000002253 acid Substances 0.000 abstract description 5
- 229920006021 bio-based polyamide Polymers 0.000 abstract description 4
- 238000011065 in-situ storage Methods 0.000 abstract description 4
- 239000003446 ligand Substances 0.000 abstract description 4
- 230000002194 synthesizing effect Effects 0.000 abstract description 3
- 238000005215 recombination Methods 0.000 abstract 1
- 230000006798 recombination Effects 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 14
- 239000000203 mixture Substances 0.000 description 8
- 230000000694 effects Effects 0.000 description 6
- 238000007723 die pressing method Methods 0.000 description 5
- 239000013384 organic framework Substances 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- 230000002035 prolonged effect Effects 0.000 description 4
- 238000005452 bending Methods 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 238000007731 hot pressing Methods 0.000 description 3
- 230000001737 promoting effect Effects 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 125000003368 amide group Chemical group 0.000 description 2
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 2
- 238000000748 compression moulding Methods 0.000 description 2
- 238000004132 cross linking Methods 0.000 description 2
- 239000003431 cross linking reagent Substances 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 238000005530 etching Methods 0.000 description 2
- 239000003365 glass fiber Substances 0.000 description 2
- 239000003292 glue Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 238000005554 pickling Methods 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 229910052761 rare earth metal Inorganic materials 0.000 description 2
- 241001391944 Commicarpus scandens Species 0.000 description 1
- 239000004593 Epoxy Substances 0.000 description 1
- 244000137852 Petrea volubilis Species 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 230000008094 contradictory effect Effects 0.000 description 1
- 230000006837 decompression Effects 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000005470 impregnation Methods 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000013001 point bending Methods 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 239000004417 polycarbonate Substances 0.000 description 1
- 229920000515 polycarbonate Polymers 0.000 description 1
- 238000006068 polycondensation reaction Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000012745 toughening agent Substances 0.000 description 1
- 239000008832 zhongfu Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L63/00—Compositions of epoxy resins; Compositions of derivatives of epoxy resins
-
- 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
- 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
- B29C70/54—Component parts, details or accessories; Auxiliary operations, e.g. feeding or storage of prepregs or SMC after impregnation or during ageing
- B29C70/545—Perforating, cutting or machining during or after moulding
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29L—INDEXING SCHEME ASSOCIATED WITH SUBCLASS B29C, RELATING TO PARTICULAR ARTICLES
- B29L2031/00—Other particular articles
- B29L2031/34—Electrical apparatus, e.g. sparking plugs or parts thereof
- B29L2031/3431—Telephones, Earphones
- B29L2031/3437—Cellular phones
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Composite Materials (AREA)
- Mechanical Engineering (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Reinforced Plastic Materials (AREA)
Abstract
The invention relates to the field of mobile phones, in particular to a carbon fiber mould pressing mobile phone middle frame and a preparation method thereof, wherein carbon fibers are acidified by Mie acid, and then cross-linked branched bio-based polyamide is generated on the surface of carboxylated carbon fibers in situ; introducing low-modulus and high-toughness polyether-ether-ketone into the dipping liquid for toughening; synthesizing a double ligand by using 2, 5-furandicarboxylic acid, 2, 5-thiophenedicarboxylic acid and lanthanum to obtain a lanthanum-containing organic matter framework, and modifying polyether-ether-ketone by using the lanthanum-containing organic matter framework; the self-repairing polyimide with the soft chain segments is synthesized by taking terephthalaldehyde, bis- (3-dimethylpropanamino) amine and 1, 2-bis (2-aminoethoxy) ethane as raw materials, the synthesized self-repairing polyimide contains dynamic imine bonds, and the breaking and recombination of the imine bonds can be generated under the external stimulus of heat generated by the heat dissipation of a mobile phone and the like, so that the cohesive force between laminated plates in the middle frame of the mobile phone is improved, and the prepared middle frame of the mobile phone is guaranteed to have better impact resistance and deformation resistance.
Description
Technical Field
The invention relates to the field of mobile phones, in particular to a carbon fiber molded mobile phone middle frame and a preparation method thereof.
Background
Along with the high-speed development of communication technology, smart phones are necessities in life of people, requirements of people on appearance modeling of mobile phones are also increasingly improved, and the existing mobile phone middle frame is made of multipurpose metal, and has the advantages of low cost and high strength, but also has the problems of easy deformation, poor dyeing property, easy scratch generation and the like, and particularly electromagnetic shielding is serious, so that more researches are put on plastic mobile phone middle frames at present.
The plastic mobile phone middle frame popular in the existing market is made of materials such as polycarbonate, and the like, and has the advantages of high portability, no signal coverage and the like, but cannot have excellent heat dissipation, wear resistance and impact resistance.
Disclosure of Invention
The invention aims to provide a carbon fiber mould pressing mobile phone middle frame and a preparation method thereof, which are used for solving the problems in the prior art.
In order to solve the technical problems, the invention provides the following technical scheme:
a preparation method of a carbon fiber mould pressing mobile phone middle frame comprises the following steps:
s1: preparing a dipping solution by blending epoxy resin and lanthanum-containing organic matter framework modified polyether-ether-ketone and self-repairing polyimide;
s2: acidifying the carbon fiber cloth, and then treating the carbon fiber cloth with a polyamide prepolymer to obtain modified carbon fibers;
s3: dipping the modified carbon fibers in a dipping solution, stacking the dipped carbon fibers in a mold, and performing mold pressing and curing by adopting a flat vulcanizing machine to obtain a composite carbon fiber plate;
s4: cutting the composite carbon fiber plate into a carbon fiber frame or a carbon fiber middle plate with a riveting structure, and riveting the frame and the middle plate structure to obtain the carbon fiber mould pressing mobile phone middle frame.
Further, the carbon fiber after the impregnation treatment comprises the following components in parts by weight: 60-80 parts of modified carbon fiber and 20-40 parts of dipping solution.
Further, when the composite carbon fiber plate is cut into a carbon fiber middle plate with a riveting structure, the frame is one of a carbon fiber frame, a metal frame and a glass fiber frame, and the frame and the carbon fiber middle plate are riveted to obtain the carbon fiber die-pressed mobile phone middle frame.
Further, when the composite carbon fiber plate is cut into the carbon fiber frame with the riveting structure, the middle plate is one of the carbon fiber middle plate and the glass fiber middle plate, and the carbon fiber frame and the middle plate structure are riveted to obtain the carbon fiber die pressing mobile phone middle frame.
Further, the thickness of the frame is 5-7mm, and the thickness of the middle plate is 0.25-0.41mm.
The carbon fiber molded mobile phone middle frame is prepared by adopting a compression molding process, has the advantages of low raw material loss, high production efficiency, low product shrinkage, low internal stress, high repeatability, low buckling deformation degree and the like, and has stable mechanical properties; firstly, sequentially acidifying the carbon fibers, and then, treating the carbon fibers by using a polyamide prepolymer to improve the conditions that the carbon fibers are easy to break and have strong inertia and easy demarcation when the carbon fibers act with other substances; and then, the mechanical property of the modified carbon fiber is further improved by using the dipping solution, and the modified carbon fiber has better self-repairing property while endowing the surface of the modified carbon fiber with better wear resistance, heat dissipation and impact resistance, so that the service life of the middle frame of the carbon fiber die-pressing mobile phone is prolonged.
Further, the preparation of the modified carbon fiber comprises the following steps:
1) Soaking carbon fiber cloth in ethanol solution of Mi's acid at 25-30deg.C for 2-3 hr, washing with water for 3-5 times, and drying to obtain acid-washed carbon fiber;
2) Under the protection of nitrogen, mixing and stirring anhydrous piperazine and dimethyl itaconate, and then using the following components in mass ratio of 1: recrystallizing the ethanol and petroleum ether for 3-5 times to obtain piperazine tetraester;
3) Mixing piperazine tetraester and 1, 6-hexamethylenediamine under the protection of nitrogen, preserving heat at 155-160 ℃ for 40-50min to obtain a polyamide prepolymer, immersing the pickled carbon fiber, decompressing for 10-20min at 155-160 ℃, and preserving heat for 12-14h to obtain the modified carbon fiber.
Further, the molar ratio of the anhydrous piperazine to the dimethyl itaconate is 1:2; the molar ratio of the piperazine tetraester to the 1, 6-hexamethylenediamine is 1:2.
according to the invention, the carbon fiber is acidified by the Mi's acid, and the Mi's acid is weak acid with smaller corrosiveness, so that the etching effect on the surface of the carbon fiber is smaller, the surface of the carbon fiber is carboxylated while the performance of the carbon fiber is not damaged, then the bio-based dimethyl itaconate and anhydrous piperazine are used for synthesizing the cross-linking agent bio-based piperazine tetraester, when the amide group is formed by replacing carboxylic acid, the reaction temperature is greatly reduced, and then the reaction product is polycondensed with 1, 6-hexamethylenediamine, so that cross-linked branched polyamide is generated on the surface of the carboxylated carbon fiber in situ, and the effect of promoting interface adhesion is realized; in addition, the raw material of the cross-linked branched polyamide is from bio-based renewable, and accords with the sustainable development concept.
Further, the working conditions of the compression molding and curing are as follows: the pressure is 2-6MPa, the temperature is raised to 110 ℃ at the speed of 3-6 ℃/min, the temperature is kept for 30-60min, and then the temperature is raised to 130 ℃ and the temperature is kept for 10-30min.
Further, the composition of the dipping solution is as follows in parts by weight: 25-35 parts of epoxy resin, 5-10 parts of self-repairing polyimide and 1-3 parts of lanthanum-containing organic matter framework modified polyether-ether-ketone.
According to the invention, the impregnated carbon fibers are laminated and then put into a mould for mould pressing, and the laminated plate has larger brittleness and is easy to crack under the action of stronger external force, and the situation of composite plate layering can occur, so that the low-modulus and high-toughness polyether-ether-ketone toughening is introduced into the impregnating solution, the stress concentration situation is effectively relieved, and the fracture toughness of the middle frame of the mobile phone is improved; however, the polyether-ether-ketone and the epoxy resin are independently added to have the problem of compatibility, so the invention uses the lanthanum-containing organic matter frame to carry out modification treatment on the polyether-ether-ketone, and uses 2, 5-furandicarboxylic acid, 2, 5-thiophene dicarboxylic acid and lanthanum to synthesize double ligands according to the unique chemical activity of rare earth elements to obtain the lanthanum-containing organic matter frame, thereby solving the problem of dispersibility of the polyether-ether-ketone in the epoxy resin and enhancing the friction resistance and the heat dissipation of the dipping liquid.
Further, the preparation of the lanthanum containing organic framework comprises the following steps: lanthanum nitrate hexahydrate, 2, 5-furandicarboxylic acid, 2, 5-thiophenedicarboxylic acid and dimethylformamide are mixed, ultrasonic stirring is carried out for 10-20min, polyether-ether-ketone is added into a reaction kettle with a lining of polytetrafluoroethylene, the temperature is kept for 20-22h at 115-120 ℃, cooling and filtering are carried out, dimethylformamide and absolute ethyl alcohol are sequentially used for washing for 3-5 times, and drying is carried out, thus obtaining the organic framework containing rare earth elements.
Further, the molar ratio of lanthanum nitrate hexahydrate, 2, 5-furandicarboxylic acid, 2, 5-thiophenedicarboxylic acid is 1:1:1.
according to the invention, terephthalaldehyde, bis- (3-dimethylpropanamino) amine and 1, 2-bis (2-aminoethoxy) ethane are used as raw materials to synthesize self-repairing polyimide with a flexible chain segment, the self-repairing polyimide is introduced into a dipping liquid, and when heated, the self-repairing polyimide plays a role of softening between layers, so that the bonding strength between layers is enhanced, and the mechanical property of a middle frame of a mobile phone is improved; the synthesized self-repairing polyimide contains dynamic imine bonds, so that the imine bonds are broken and recombined under the external stimulus such as heat generated by heat dissipation of a mobile phone, and a network structure is rearranged, so that the bonding force between the laminated plates in the middle frame of the mobile phone has self-repairing property, the service life of the middle frame of the mobile phone is greatly prolonged, and the prepared middle frame of the mobile phone is guaranteed to have good impact resistance and deformation resistance.
Further, the preparation of the self-repairing polyimine comprises the following steps: mixing terephthalaldehyde and ethanol, heating to 70-75 ℃, stirring at 400rpm for 15-20min, adding a mixed solution of 1, 2-bis (2-aminoethoxy) ethane, bis- (3-dimethylpropanamino) amine and ethanol, performing ultrasonic dispersion for 5-10min, evaporating the solvent, heating to 80 ℃, preserving heat for 3h, heating to 95 ℃, preserving heat for 1h, and heating to 105 ℃ for 1h to obtain self-repairing polyimide.
Further, the mass ratio of terephthalaldehyde, 1, 2-bis (2-aminoethoxy) ethane and bis- (3-dimethylpropanamino) amine is 1:0.39:0.4.
further, the mass ratio of the lanthanum-containing organic matter framework modified polyether-ether-ketone to the self-repairing polyimide is 0.2-0.3; the mass ratio of the lanthanum-containing organic matter framework modified polyether-ether-ketone to the self-repairing polyimide is controlled, so that the soft and hard use of the dipping glue layer formed by the dipping glue solution is realized, and the comprehensive mechanical property of the mobile phone middle frame is improved.
The invention has the beneficial effects that:
the invention provides a carbon fiber die-pressed mobile phone middle frame and a preparation method thereof, and the prepared mobile phone middle frame has better wear resistance, heat dissipation and impact resistance and better self-repairing property.
According to the invention, the carbon fiber is acidified by the Mi's acid, and then the crosslinked branched bio-based polyamide is generated on the surface of the carboxylated carbon fiber in situ, so that the effect of promoting interface adhesion is achieved, and the self-repairing polyimide in the bio-based polyamide and the dipping liquid are subjected to dynamic covalent crosslinking, so that the bonding strength of the dipping liquid to the carbon fiber is greatly improved.
The polyether-ether-ketone toughening agent is introduced into the dipping liquid to toughen the polyether-ether-ketone with low modulus and high toughness, so that the stress concentration condition is effectively relieved, and the fracture toughness of the middle frame of the mobile phone is improved; the polyether-ether-ketone is modified by a lanthanum-containing organic matter frame, and double ligands are synthesized by using 2, 5-furandicarboxylic acid, 2, 5-thiophene dicarboxylic acid and lanthanum to obtain the lanthanum-containing organic matter frame, so that the friction resistance and heat dissipation of the dipping liquid are enhanced while the problem of the dispersion uniformity of the polyether-ether-ketone in epoxy resin is solved.
According to the invention, terephthalaldehyde, bis- (3-dimethylpropanamino) amine and 1, 2-bis (2-aminoethoxy) ethane are used as raw materials to synthesize self-repairing polyimide with a flexible chain segment, the self-repairing polyimide is introduced into a dipping liquid, and when heated, the self-repairing polyimide plays a role of softening between layers, so that the bonding strength between layers is enhanced, and the mechanical property of a middle frame of a mobile phone is improved; the synthesized self-repairing polyimide contains dynamic imine bonds, so that the imine bonds are broken and recombined under the external stimulus such as heat generated by heat dissipation of a mobile phone, and a network structure is rearranged, so that the bonding force between the laminated plates in the middle frame of the mobile phone has self-repairing property, the service life of the middle frame of the mobile phone is greatly prolonged, and the impact resistance and deformation resistance of the prepared middle frame of the mobile phone are ensured.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely in connection with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, but not all embodiments. 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.
It should be noted that, if directional indications such as up, down, left, right, front, and rear … … are involved in the embodiment of the present invention, the directional indications are merely used to explain a relative positional relationship, a movement condition, and the like between a certain posture such as the respective components, and if the certain posture is changed, the directional indications are changed accordingly. In addition, the technical solutions of the embodiments may be combined with each other, but it is necessary to base that the technical solutions can be realized by those skilled in the art, and when the technical solutions are contradictory or cannot be realized, the combination of the technical solutions should be considered to be absent and not within the scope of protection claimed in the present invention.
The following description of the embodiments of the present invention will be presented in further detail with reference to the examples, which should be understood as being merely illustrative of the present invention and not limiting.
Example 1: a preparation method of a carbon fiber mould pressing mobile phone middle frame comprises the following steps:
s1: preparing a dipping solution by blending epoxy resin and lanthanum-containing organic matter framework modified polyether-ether-ketone and self-repairing polyimide;
the dipping liquid comprises the following components in parts by weight: 25 parts of epoxy resin, 5 parts of self-repairing polyimide and 1 part of lanthanum-containing organic matter framework modified polyether-ether-ketone;
the preparation method of the lanthanum-containing organic matter framework modified polyether-ether-ketone comprises the following steps:
mixing 324.9mg lanthanum nitrate hexahydrate, 156.2mg2, 5-furandicarboxylic acid, 172.2mg2, 5-thiophenedicarboxylic acid and 20mL dimethylformamide, ultrasonically stirring for 10min, transferring into a polytetrafluoroethylene-lined reaction kettle, adding 2g polyether-ether-ketone, preserving heat at 115 ℃ for 22h, cooling, filtering, washing with dimethylformamide and absolute ethyl alcohol for 3 times in sequence, and drying to obtain lanthanum-containing organic matter framework modified polyether-ether-ketone;
the preparation of the self-repairing polyimide comprises the following steps:
mixing 1g of terephthalaldehyde and 3mL of ethanol, heating to 70 ℃, stirring at 400rpm for 20min, adding a mixed solution of 0.39g of 1, 2-bis (2-aminoethoxy) ethane, 0.4g of bis- (3-dimethylpropanamino) amine and 1mL of ethanol, performing ultrasonic dispersion for 5min, evaporating the solvent, heating to 80 ℃, preserving heat for 3h, heating to 95 ℃ for 1h, and heating to 105 ℃ for 1h to obtain self-repairing polyimide;
s2: acidifying the carbon fiber cloth with Mi's acid, and then treating with a polyamide prepolymer to obtain modified carbon fibers;
the preparation of the modified carbon fiber comprises the following steps:
1) Soaking carbon fiber cloth in ethanol solution of 2wt% Mi's acid at 25 deg.c for 3 hr, washing with water for 3 times, and drying to obtain pickled carbon fiber;
2) 3.44g of anhydrous piperazine and 12.66g of dimethyl itaconate are mixed and stirred under the protection of nitrogen, and then the mixture is prepared by the following steps of: recrystallizing the ethanol and petroleum ether for 3 times to obtain piperazine tetraester;
3) Under the protection of nitrogen, 8.04g of piperazine tetraester and 4.7g of 1, 6-hexamethylenediamine are mixed, the mixture is kept at 155 ℃ for 50min to obtain a polyamide prepolymer, then 0.4g of carbon fiber after pickling is immersed in the polyamide prepolymer, the pressure is reduced for 10min at 155 ℃, and then the mixture is kept at the temperature for 12h to obtain modified carbon fiber;
s3: dipping the modified carbon fibers in a dipping solution, stacking the dipped carbon fibers in a mold, and performing mold pressing and curing by adopting a flat vulcanizing machine to obtain a composite carbon fiber plate;
the carbon fiber after the dipping treatment comprises the following components in parts by weight: 60 parts of modified carbon fiber and 20 parts of gum dipping liquid;
the working conditions of the die pressing and curing are as follows: the pressure is 2MPa, the temperature is raised to 110 ℃ at a speed of 3 ℃/min, the temperature is kept for 30min, and then the temperature is raised to 130 ℃ and the temperature is kept for 10min;
s4: cutting the composite carbon fiber plate into a carbon fiber frame and a carbon fiber middle plate with riveting structures, and riveting the frame and the middle plate structure to obtain the carbon fiber mould pressing mobile phone middle frame.
Example 2: a preparation method of a carbon fiber mould pressing mobile phone middle frame comprises the following steps:
s1: preparing a dipping solution by blending epoxy resin and lanthanum-containing organic matter framework modified polyether-ether-ketone and self-repairing polyimide;
the dipping liquid comprises the following components in parts by weight: 30 parts of epoxy resin, 8 parts of self-repairing polyimide and 2 parts of lanthanum-containing organic matter framework modified polyether-ether-ketone;
the preparation method of the lanthanum-containing organic matter framework modified polyether-ether-ketone comprises the following steps:
mixing 324.9mg lanthanum nitrate hexahydrate, 156.2mg2, 5-furandicarboxylic acid, 172.2mg2, 5-thiophenedicarboxylic acid and 20mL dimethylformamide, ultrasonically stirring for 15min, transferring into a polytetrafluoroethylene-lined reaction kettle, adding 2g polyether-ether-ketone, preserving heat at 1118 ℃ for 21h, cooling, filtering, washing with dimethylformamide and absolute ethyl alcohol for 4 times in sequence, and drying to obtain lanthanum-containing organic matter framework modified polyether-ether-ketone;
the preparation of the self-repairing polyimide comprises the following steps:
mixing 1g of terephthalaldehyde and 3mL of ethanol, heating to 73 ℃, stirring at 400rpm for 18min, adding a mixed solution of 0.39g of 1, 2-bis (2-aminoethoxy) ethane, 0.4g of bis- (3-dimethylpropanamino) amine and 1mL of ethanol, performing ultrasonic dispersion for 5-10min, evaporating the solvent, heating to 80 ℃, preserving heat for 3h, heating to 95 ℃, preserving heat for 1h, and heating to 105 ℃ for 1h to obtain self-repairing polyimide;
s2: acidifying the carbon fiber cloth with Mi's acid, and then treating with a polyamide prepolymer to obtain modified carbon fibers;
the preparation of the modified carbon fiber comprises the following steps:
1) Soaking carbon fiber cloth in ethanol solution of 2wt% Mi's acid at 28 deg.c for 2.5 hr, washing with water for 4 times, and drying to obtain pickled carbon fiber;
2) 3.44g of anhydrous piperazine and 12.66g of dimethyl itaconate are mixed and stirred under the protection of nitrogen, and then the mixture is prepared by the following steps of: recrystallizing the ethanol and petroleum ether for 4 times to obtain piperazine tetraester;
3) Under the protection of nitrogen, 8.04g of piperazine tetraester and 4.7g of 1, 6-hexamethylenediamine are mixed, heat preservation is carried out for 45min at 158 ℃ to obtain a polyamide prepolymer, then 0.4g of carbon fiber after pickling is immersed in the polyamide prepolymer, decompression is carried out for 15min at 158 ℃, and heat preservation is carried out for 13h to obtain modified carbon fiber;
s3: dipping the modified carbon fibers in a dipping solution, stacking the dipped carbon fibers in a mold, and performing mold pressing and curing by adopting a flat vulcanizing machine to obtain a composite carbon fiber plate;
the carbon fiber after the dipping treatment comprises the following components in parts by weight: 70 parts of modified carbon fiber and 35 parts of gum dipping liquid;
the working conditions of the die pressing and curing are as follows: the pressure is 4MPa, the temperature is raised to 110 ℃ at a speed of 5 ℃/min, the temperature is kept for 40min, and then the temperature is raised to 130 ℃ and the temperature is kept for 20min;
s4: cutting the composite carbon fiber plate into a carbon fiber frame and a carbon fiber middle plate with riveting structures, and riveting the frame and the middle plate structure to obtain the carbon fiber mould pressing mobile phone middle frame.
Example 3: a preparation method of a carbon fiber mould pressing mobile phone middle frame comprises the following steps:
s1: preparing a dipping solution by blending epoxy resin and lanthanum-containing organic matter framework modified polyether-ether-ketone and self-repairing polyimide;
the dipping liquid comprises the following components in parts by weight: 35 parts of epoxy resin, 10 parts of self-repairing polyimide and 3 parts of lanthanum-containing organic matter framework modified polyether-ether-ketone;
the preparation method of the lanthanum-containing organic matter framework modified polyether-ether-ketone comprises the following steps:
mixing 324.9mg lanthanum nitrate hexahydrate, 156.2mg2, 5-furandicarboxylic acid, 172.2mg2, 5-thiophenedicarboxylic acid and 20mL dimethylformamide, ultrasonically stirring for 20min, transferring into a polytetrafluoroethylene-lined reaction kettle, adding 2g polyether-ether-ketone, preserving heat at 120 ℃ for 20h, cooling, filtering, washing with dimethylformamide and absolute ethyl alcohol for 5 times in sequence, and drying to obtain lanthanum-containing organic matter framework modified polyether-ether-ketone;
the preparation of the self-repairing polyimide comprises the following steps:
mixing 1g of terephthalaldehyde and 3mL of ethanol, heating to 75 ℃, stirring at 400rpm for 20min, adding a mixed solution of 0.39g of 1, 2-bis (2-aminoethoxy) ethane, 0.4g of bis- (3-dimethylpropanamino) amine and 1mL of ethanol, performing ultrasonic dispersion for 10min, evaporating the solvent, heating to 80 ℃, preserving heat for 3h, heating to 95 ℃ for 1h, and heating to 105 ℃ for 1h to obtain self-repairing polyimide;
s2: acidifying the carbon fiber cloth with Mi's acid, and then treating with a polyamide prepolymer to obtain modified carbon fibers;
the preparation of the modified carbon fiber comprises the following steps:
1) Soaking carbon fiber cloth in ethanol solution of 2wt% Mi's acid at 30 deg.c for 2 hr, washing with water for 5 times, and drying to obtain pickled carbon fiber;
2) 3.44g of anhydrous piperazine and 12.66g of dimethyl itaconate are mixed and stirred under the protection of nitrogen, and then the mixture is prepared by the following steps of: recrystallizing the ethanol and petroleum ether for 5 times to obtain piperazine tetraester;
3) Under the protection of nitrogen, 8.04g of piperazine tetraester and 4.7g of 1, 6-hexamethylenediamine are mixed, the mixture is kept at 160 ℃ for 40min to obtain a polyamide prepolymer, then 0.4g of acid-washed carbon fiber is immersed in the polyamide prepolymer, the pressure is reduced for 10min at 160 ℃, and then the mixture is kept at the temperature for 14h to obtain modified carbon fiber;
s3: dipping the modified carbon fibers in a dipping solution, stacking the dipped carbon fibers in a mold, and performing mold pressing and curing by adopting a flat vulcanizing machine to obtain a composite carbon fiber plate;
the carbon fiber after the dipping treatment comprises the following components in parts by weight: 80 parts of modified carbon fiber and 40 parts of gum dipping liquid;
the working conditions of the die pressing and curing are as follows: the pressure is 6MPa, the temperature is raised to 110 ℃ at the speed of 6 ℃/min, the temperature is kept for 60min, and then the temperature is raised to 130 ℃ and the temperature is kept for 30min;
s4: cutting the composite carbon fiber plate into a carbon fiber frame and a carbon fiber middle plate with riveting structures, and riveting the frame and the middle plate structure to obtain the carbon fiber mould pressing mobile phone middle frame.
Comparative example 1: using example 3 as a control, no self-healing polyimide was prepared, and the other procedures were normal.
Comparative example 2: with example 3 as a control group, polyether-ether-ketone is used for replacing lanthanum-containing organic matter framework modified polyether-ether-ketone, and other procedures are normal.
Comparative example 3: taking example 3 as a control group, the mass ratio of the lanthanum-containing organic framework modified polyether-ether-ketone to the self-repairing polyimide is 0.32, namely 10 parts of the self-repairing polyimide and 3.2 parts of the lanthanum-containing organic framework modified polyether-ether-ketone, and other working procedures are normal.
Comparative example 4: using example 3 as a control, no Michaelis acid was added and the other procedures were normal.
Comparative example 5: using example 3 as a control, no polyamide prepolymer was prepared and the other procedures were normal.
Comparative example 6: with example 3 as a control group, the modified carbon fibers were replaced with carbon fiber cloth, and the other procedures were normal.
The carbon fiber frame used in the examples and comparative examples was 6mm and the carbon fiber middle plate was 0.35mm.
The raw material sources are as follows:
epoxy E871957, lanthanum nitrate hexahydrate L812372: shanghai Miclin Biochemical technologies Co., ltd; 2, 5-furandicarboxylic acid 722081, 2, 5-thiophenedicarboxylic acid 405191, dimethylformamide D301788, polyetheretherketone P462877, terephthalaldehyde P105980, 1, 2-bis (2-aminoethoxy) ethane B152231, mitsui acid M110151, anhydrous piperazine P105274, dimethyl itaconate D154394, 1, 6-hexamethylenediamine H103909: ala Ding Shiji; bis- (3-dimethylpropanamino) amine 6711-48-4: hubei zhen Bo chemical industry Co., ltd; absolute ethanol, petroleum ether, analytically pure: a national drug group reagent; the carbon fiber cloth is woven by SYT55S-12K of Zhongfu eagle carbon fiber Co., ltd, and has a thickness of 50 μm.
Performance test: performance tests were performed on the mobile phone center frames prepared in examples 1 to 3 and comparative examples 1 to 6:
bending strength test: referring to an ASTMD7264 test, a three-point bending method is adopted, a bending loading head with the diameter of 6mm is used, a sample is cut into a thickness of 0.35mm and a width of 13mm, a test span is 32 times of the thickness, and the bending speed is 1mm/min; the average value of the groups is taken from the parallel test 5;
heat dissipation property: detecting the heat conductivity coefficient by adopting a heat conductivity coefficient tester according to ASTMD5470, wherein the sample size is 40mm multiplied by 10mm multiplied by 0.35mm;
impact strength: with reference to GB/T1843-2008 test, the impact energy is 5.5J, the sample size is 80mm×10mm×0.35mm;
self-repairability: polishing the surface of the frame and the middle plate for 10 times by using 80-mesh sand paper, wherein the maximum scratch width is 2.5 mu m, placing the polished sample between two steel plates, performing hot pressing at 105 ℃, the hot pressing pressure is 2MPa, the hot pressing time is 1h, and observing surface scratches; the results are shown in Table 1;
TABLE 1
The invention provides a carbon fiber die-pressed mobile phone middle frame and a preparation method thereof, and the prepared mobile phone middle frame has better wear resistance, heat dissipation and impact resistance and better self-repairing property.
Comparing example 3 with comparative example 1, it is known that the invention synthesizes self-repairing polyimide with flexible chain segments by using terephthalaldehyde, bis- (3-dimethylpropanamino) amine and 1, 2-bis (2-aminoethoxy) ethane as raw materials, and introduces self-repairing polyimide into the dipping solution, and the self-repairing polyimide can play a role of softening between layers when heated, so as to enhance the bonding strength between each layer and improve the mechanical property of the middle frame of the mobile phone; the synthesized self-repairing polyimide contains dynamic imine bonds, so that the imine bonds are broken and recombined under the external stimulus such as heat generated by heat dissipation of a mobile phone, and a network structure is rearranged, so that the bonding force between the laminated plates in the middle frame of the mobile phone has self-repairing property, the service life of the middle frame of the mobile phone is greatly prolonged, and the impact resistance and deformation resistance of the prepared middle frame of the mobile phone are ensured.
Comparing example 3 with comparative example 2, the invention introduces low-modulus and high-toughness polyether-ether-ketone toughening into the dipping liquid, effectively relieves stress concentration and improves fracture toughness of the mobile phone middle frame; the polyether-ether-ketone is modified by using the lanthanum-containing organic matter framework modified polyether-ether-ketone, and double ligands are synthesized by using 2, 5-furandicarboxylic acid, 2, 5-thiophene dicarboxylic acid and lanthanum to obtain the lanthanum-containing organic matter framework, so that the friction resistance and heat dissipation of the dipping solution are enhanced while the problem of the dispersion uniformity of the polyether-ether-ketone in epoxy resin is solved.
Comparing example 3 with comparative example 3, it can be seen that the mass ratio of lanthanum-containing organic framework modified polyether-ether-ketone to self-repairing polyimide is controlled to make the gum dipping layer formed by the gum dipping solution soft and hard, thereby improving the comprehensive mechanical properties of the mobile phone middle frame.
Comparing example 3 with comparative example 4, comparative example 5 and comparative example 6, it is known that in the invention, the carbon fiber is acidified by Mi's acid firstly, because Mi's acid is weak acid with low corrosiveness, etching effect on the surface of the carbon fiber is low, the surface of the carbon fiber is carboxylated while the performance of the carbon fiber is not damaged, and then bio-based dimethyl itaconate and anhydrous piperazine are used for synthesizing cross-linking agent bio-based piperazine tetraester, when the carboxylic acid is replaced to form an amide group, the reaction temperature is greatly reduced, and then polycondensation is carried out with 1, 6-hexamethylenediamine, so that cross-linked branched polyamide is generated on the surface of the carboxylated carbon fiber in situ, and the effect of promoting interface adhesion is achieved; in addition, the raw material of the cross-linked branched polyamide is from bio-based renewable, and accords with the sustainable development concept. And the self-repairing polyimide in the bio-based polyamide and the dipping liquid has dynamic covalent crosslinking, so that the bonding strength of the dipping liquid to the carbon fiber is greatly improved.
The foregoing description is only exemplary embodiments of the present invention and is not intended to limit the scope of the invention, and all equivalent structural changes made by the present invention or direct/indirect application in other related technical fields are included in the scope of the present invention.
Claims (4)
1. The preparation method of the carbon fiber mould pressing mobile phone middle frame is characterized by comprising the following steps of:
s1: preparing a dipping solution by blending epoxy resin and lanthanum-containing organic matter framework modified polyether-ether-ketone and self-repairing polyimide;
s2: sequentially acidizing the carbon fiber cloth, and then treating the carbon fiber cloth with polyamide prepolymer to obtain modified carbon fibers;
s3: dipping the modified carbon fibers in a dipping solution, stacking the dipped carbon fibers in a mold, and performing mold pressing and curing by adopting a flat vulcanizing machine to obtain a composite carbon fiber plate;
s4: cutting the composite carbon fiber plate into a carbon fiber frame or a carbon fiber middle plate with a riveting structure, and riveting the frame and the middle plate structure to obtain a carbon fiber mould pressing mobile phone middle frame;
the carbon fiber after the dipping treatment comprises the following components in parts by weight: 60-80 parts of modified carbon fiber and 20-40 parts of dipping solution;
the dipping liquid comprises the following components in parts by weight: 25-35 parts of epoxy resin, 5-10 parts of self-repairing polyimide and 1-3 parts of lanthanum-containing organic matter framework modified polyether-ether-ketone;
the mass ratio of the lanthanum-containing organic matter framework modified polyether-ether-ketone to the self-repairing polyimide is 0.2-0.3;
the preparation of the self-repairing polyimide comprises the following steps: mixing terephthalaldehyde and ethanol, heating to 70-75 ℃, stirring at 400rpm for 15-20min, adding a mixed solution of 1, 2-bis (2-aminoethoxy) ethane, bis- (3-dimethylpropanamino) amine and ethanol, performing ultrasonic dispersion for 5-10min, evaporating a solvent, heating to 80 ℃, preserving heat for 3h, heating to 95 ℃ for 1h, and heating to 105 ℃ for 1h to obtain self-repairing polyimide;
the preparation method of the lanthanum-containing organic matter framework modified polyether-ether-ketone comprises the following steps: mixing lanthanum nitrate hexahydrate, 2, 5-furandicarboxylic acid, 2, 5-thiophenedicarboxylic acid and dimethylformamide, ultrasonically stirring for 10-20min, transferring polytetrafluoroethylene lining, adding polyether-ether-ketone into a reaction kettle, preserving heat for 20-22h at 115-120 ℃, cooling, filtering, washing with dimethylformamide and absolute ethyl alcohol for 3-5 times in sequence, and drying to obtain lanthanum-containing organic matter framework modified polyether-ether-ketone;
the preparation of the modified carbon fiber comprises the following steps:
1) Soaking carbon fiber cloth in ethanol solution of Mi's acid at 25-30deg.C for 2-3 hr, washing with water for 3-5 times, and drying to obtain acid-washed carbon fiber;
2) Under the protection of nitrogen, mixing and stirring anhydrous piperazine and dimethyl itaconate, and then using the following components in mass ratio of 1:1, recrystallizing the ethanol and petroleum ether for 3-5 times to obtain piperazine tetraester;
3) Mixing piperazine tetraester and 1, 6-hexamethylenediamine under the protection of nitrogen, preserving heat at 155-160 ℃ for 40-50min to obtain a polyamide prepolymer, immersing the pickled carbon fiber, decompressing for 10-20min at 155-160 ℃, and preserving heat for 12-14h to obtain the modified carbon fiber.
2. The method for manufacturing the carbon fiber molded mobile phone middle frame according to claim 1, wherein the working conditions of mold pressing and curing are as follows: the pressure is 2-6MPa, the temperature is raised to 110 ℃ at the speed of 3-6 ℃/min, the temperature is kept for 30-60min, and then the temperature is raised to 130 ℃ and the temperature is kept for 10-30min.
3. The method for preparing the carbon fiber molded mobile phone middle frame according to claim 1, wherein in the preparation of the self-repairing polyimide, the mass ratio of terephthalaldehyde, 1, 2-bis (2-aminoethoxy) ethane and bis- (3-dimethylpropanamine) amine is 1:0.39:0.4.
4. a carbon fiber molded mobile phone center, characterized in that it is prepared by the preparation method according to any one of claims 1 to 3.
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