CN111635615A - Preparation method of carbon fiber-titanium dioxide multistage reinforced resin matrix composite material - Google Patents
Preparation method of carbon fiber-titanium dioxide multistage reinforced resin matrix composite material Download PDFInfo
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 66
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 60
- 239000002131 composite material Substances 0.000 title claims abstract description 46
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 39
- 239000011347 resin Substances 0.000 title claims abstract description 34
- 229920005989 resin Polymers 0.000 title claims abstract description 34
- 239000011159 matrix material Substances 0.000 title claims abstract description 32
- 239000004408 titanium dioxide Substances 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 229920000049 Carbon (fiber) Polymers 0.000 claims abstract description 169
- 239000004917 carbon fiber Substances 0.000 claims abstract description 163
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical class C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 101
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims abstract description 25
- 238000000034 method Methods 0.000 claims abstract description 13
- 239000010409 thin film Substances 0.000 claims abstract description 10
- 239000010408 film Substances 0.000 claims abstract description 9
- 239000000243 solution Substances 0.000 claims description 68
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 60
- 238000002791 soaking Methods 0.000 claims description 44
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 40
- 238000001035 drying Methods 0.000 claims description 30
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 26
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 24
- 238000003756 stirring Methods 0.000 claims description 18
- 238000010438 heat treatment Methods 0.000 claims description 17
- 238000004513 sizing Methods 0.000 claims description 17
- 239000003795 chemical substances by application Substances 0.000 claims description 16
- 238000001816 cooling Methods 0.000 claims description 13
- 239000011259 mixed solution Substances 0.000 claims description 13
- 239000008367 deionised water Substances 0.000 claims description 12
- 229910021641 deionized water Inorganic materials 0.000 claims description 12
- 238000005406 washing Methods 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 239000007864 aqueous solution Substances 0.000 claims description 11
- 238000005520 cutting process Methods 0.000 claims description 11
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 claims description 10
- 238000004140 cleaning Methods 0.000 claims description 10
- 230000032683 aging Effects 0.000 claims description 9
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims description 8
- 239000005011 phenolic resin Substances 0.000 claims description 8
- 229920001568 phenolic resin Polymers 0.000 claims description 8
- 238000000465 moulding Methods 0.000 claims description 7
- 238000007731 hot pressing Methods 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 6
- 230000002787 reinforcement Effects 0.000 claims description 6
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 4
- 239000000805 composite resin Substances 0.000 claims description 3
- 230000003014 reinforcing effect Effects 0.000 claims description 2
- 239000002070 nanowire Substances 0.000 abstract description 11
- 239000011208 reinforced composite material Substances 0.000 abstract description 5
- 238000005452 bending Methods 0.000 abstract description 2
- 238000011065 in-situ storage Methods 0.000 abstract description 2
- 239000003623 enhancer Substances 0.000 abstract 1
- 238000003980 solgel method Methods 0.000 abstract 1
- 238000006243 chemical reaction Methods 0.000 description 21
- 239000004744 fabric Substances 0.000 description 14
- 238000007664 blowing Methods 0.000 description 9
- 238000003618 dip coating Methods 0.000 description 6
- 230000009286 beneficial effect Effects 0.000 description 4
- 239000002041 carbon nanotube Substances 0.000 description 4
- 229910021393 carbon nanotube Inorganic materials 0.000 description 4
- 239000000835 fiber Substances 0.000 description 4
- 238000002715 modification method Methods 0.000 description 3
- 239000002073 nanorod Substances 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 2
- VYFYYTLLBUKUHU-UHFFFAOYSA-N dopamine Chemical compound NCCC1=CC=C(O)C(O)=C1 VYFYYTLLBUKUHU-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000002783 friction material Substances 0.000 description 2
- 125000000524 functional group Chemical group 0.000 description 2
- 125000001967 indiganyl group Chemical group [H][In]([H])[*] 0.000 description 2
- 150000007965 phenolic acids Chemical class 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 238000005507 spraying Methods 0.000 description 2
- 230000003746 surface roughness Effects 0.000 description 2
- GFQYVLUOOAAOGM-UHFFFAOYSA-N zirconium(iv) silicate Chemical compound [Zr+4].[O-][Si]([O-])([O-])[O-] GFQYVLUOOAAOGM-UHFFFAOYSA-N 0.000 description 2
- CTENFNNZBMHDDG-UHFFFAOYSA-N Dopamine hydrochloride Chemical compound Cl.NCCC1=CC=C(O)C(O)=C1 CTENFNNZBMHDDG-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- MJOQJPYNENPSSS-XQHKEYJVSA-N [(3r,4s,5r,6s)-4,5,6-triacetyloxyoxan-3-yl] acetate Chemical compound CC(=O)O[C@@H]1CO[C@@H](OC(C)=O)[C@H](OC(C)=O)[C@H]1OC(C)=O MJOQJPYNENPSSS-XQHKEYJVSA-N 0.000 description 1
- 150000001721 carbon Chemical class 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000005234 chemical deposition Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 238000013016 damping Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 238000009990 desizing Methods 0.000 description 1
- 229960003638 dopamine Drugs 0.000 description 1
- 229960001149 dopamine hydrochloride Drugs 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 238000010335 hydrothermal treatment Methods 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000002135 nanosheet Substances 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- LLZRNZOLAXHGLL-UHFFFAOYSA-J titanic acid Chemical compound O[Ti](O)(O)O LLZRNZOLAXHGLL-UHFFFAOYSA-J 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/02—Ingredients treated with inorganic substances
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B15/00—Pretreatment of the material to be shaped, not covered by groups B29B7/00 - B29B13/00
- B29B15/08—Pretreatment of the material to be shaped, not covered by groups B29B7/00 - B29B13/00 of reinforcements or fillers
- B29B15/10—Coating or impregnating independently of the moulding or shaping step
- B29B15/12—Coating or impregnating independently of the moulding or shaping step of reinforcements of indefinite length
- B29B15/14—Coating or impregnating independently of the moulding or shaping step of reinforcements of indefinite length of filaments or wires
-
- 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
- B29C70/40—Shaping or impregnating by compression not applied
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
- C08K7/06—Elements
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- Mechanical Engineering (AREA)
- Composite Materials (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
- Reinforced Plastic Materials (AREA)
Abstract
The invention discloses a preparation method of a carbon fiber-titanium dioxide multistage reinforced resin matrix composite material, which comprises the steps of firstly preparing TiO with different thicknesses on the surface of activated carbon fiber by using a sol-gel method2A film prefabricated layer is formed, and then a mild hydrothermal in-situ growth method is adopted to construct the carbon fiber-TiO with stable structure2film-TiO2A nanowire multi-level enhancer. The carbon fiber-TiO prepared by the invention2Thin film layer-TiO2The bending strength of the nano-wire multistage reinforced resin matrix composite material is the maximum, about 104.5Mpa, which is 32.8 percent higher than 70.2Mpa of the original carbon fiber reinforced composite material, the mechanical property is obviously enhanced, and the wear rate is only 1.21 × 10‑5mm3The ratio of N to m is reduced by 39.8 percent compared with the original carbon fiber reinforced composite material, which shows that the carbon fiber-TiO prepared by the invention2Thin film layer-TiO2The nano-wire multistage reinforced resin matrix composite material has good mechanical property and tribological property.
Description
Technical Field
The invention belongs to a preparation method of a wet friction material, and particularly relates to a preparation method of a carbon fiber-titanium dioxide multistage reinforced resin matrix composite.
Background
Carbon fiber has become one of many materials with important technical significance designed by scholars at home and abroad at present, and not only has high temperature resistance, corrosion resistance, low thermal expansion coefficient and good chemical stability, but also has a series of excellent performances such as high specific gravity, specific modulus and the like. In the carbon fiber/resin composite material, resin is usually used as a matrix of the composite material and mainly plays a role in crosslinking fibers; the carbon fiber is used as a reinforcement body and is mainly used for bearing and transferring the friction external force. However, the carbon fiber has a disordered graphite structure on the surface, is smooth and inert, and cannot be well wetted and combined with the matrix, so that the carbon fiber is easily stripped and falls off from the matrix in the friction process, the friction coefficient is greatly fluctuated, and the friction stability is obviously reduced. Therefore, the surface treatment of carbon fibers to improve the specific surface area and the surface active functional groups thereof is a key to improve the interfacial bonding between the carbon fibers and the resin.
Chinese patent CN109181228A "preparation method of modified carbon fiber reinforced resin matrix structure-damping composite material with dopamine coated carbon nanotube" soaking carbon fiber with surface degumming in Fe (NO) dissolved in absolute ethyl alcohol3)3Is a nano-metalAnd (3) in a precursor solution of the catalyst, heating and depositing the carbon nanotubes in a tube furnace, and finally soaking the carbon fibers on which the carbon nanotubes are deposited in dopamine hydrochloride to finish the preparation of the composite material. The method adopts a chemical deposition method to prepare the carbon nano tube, the experimental conditions are harsh, the early treatment is complex, and further the carbon fiber is damaged, which is not beneficial to enhancing the mechanical property of the composite material.
Chinese patent CN110938781A entitled "A modified carbon fiber reinforced phenolic resin-based composite material and its preparation" desizing carbon fibers at 800 deg.C in inert atmosphere, and oxidizing with nitric acid at 80 deg.C to obtain carbon fibers with-COOH functional groups. Spraying organic-inorganic hybrid zirconium silicate sol on the surface of the pretreated carbon fiber by using an air spraying mode, wherein the mass ratio of the organic-inorganic hybrid zirconium silicate sol to the pretreated carbon fiber is 7:3, and finally, impregnating according to the volume ratio of the carbon fiber to phenolic acid resin of 1:1 to finally obtain the modified carbon fiber reinforced phenolic acid resin matrix composite material. Although the modification method can improve the surface roughness and the surface activity of the carbon fiber, the experimental requirement is high, and the large-scale production and use are not facilitated.
Disclosure of Invention
The invention aims to provide carbon fiber-TiO2Thin film layer-TiO2The invention discloses a preparation method of a nano-wire multistage reinforced resin matrix composite material, which is used for overcoming the defects in the prior art2A thin film layer, and a mild hydrothermal in-situ growth method is adopted to construct the carbon fiber-TiO with stable structure2film-TiO2The nano-wire multi-stage reinforcement is used for preparing the resin-based friction material with excellent friction performance and low wear rate.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a carbon fiber-titanium dioxide multistage reinforced resin matrix composite material comprises the following steps:
step one, carbon fiber pretreatment: cutting carbon fiber, soaking in mixed solution of acetone and anhydrous alcohol to remove sizing agent on the surface of carbon fiber, and removing the sizing agentSoaking the treated carbon fiber in H2O2Soaking in the solution, taking out, washing with deionized water, and drying to obtain activated carbon fiber;
step two, prefabricating TiO on the surface of the carbon fiber2Film layer: preparing TiO2Sol, dissolving activated carbon fiber in TiO2Soaking in sol, taking out carbon fiber, heat treating, naturally cooling, and repeating soaking-heat treating-cooling process for several times to obtain TiO with different thicknesses2Film-carbon fiber;
step three, constructing TiO2Nanowire-thin film multilevel reinforcement: taking TiO with different thicknesses in the second step2Respectively immersing the film-carbon fiber in an aqueous solution of sodium hydroxide, then respectively carrying out homogeneous hydrothermal reaction, thoroughly immersing the obtained carbon fiber in an aqueous solution of hydrochloric acid, treating at 70 ℃ for 10h, then cleaning and drying the carbon fiber, and then carrying out heat treatment at 400 ℃ for 3h to finally obtain TiO with different thicknesses2nanowire-TiO2A thin film multi-stage reinforcing carbon fiber;
step four, preparing the carbon fiber/resin matrix composite material: taking the TiO with different thicknesses obtained in the step three2nanowire-TiO2The method comprises the following steps of respectively immersing the multistage reinforced carbon fibers of the film in a phenolic resin solution with the mass fraction of 20-30% to obtain a composite material prefabricated body, and then carrying out hot-press forming on the composite material prefabricated body to finally obtain the carbon fiber-titanium dioxide multistage carbon fiber reinforced resin matrix composite material.
Further, in the first step, the carbon fibers are cut into squares of 5cm multiplied by 9cm and are subjected to edge locking, then the squares are placed in a mixed solution of acetone and absolute ethyl alcohol according to the volume ratio of 1:1 to be soaked for 24-48 hours, and sizing agents on the surfaces of the carbon fibers are removed.
Further, in the step one, the carbon fiber with the sizing agent removed is soaked in H with the volume fraction of 30 percent2O2And soaking the solution for 24 hours, taking out the solution, washing the solution by using deionized water, and drying the solution at the temperature of 60 ℃ to obtain the activated carbon fiber.
Further, TiO in the second step2The sol preparation process is as follows: adding concentrated hydrochloric acid dropwise into anhydrous ethanol, stirring, and adding the above solutionAdding tetrabutyl titanate, continuously stirring for 30min, and aging for 12h to obtain TiO2And sol, wherein the volume ratio of the absolute ethyl alcohol to the concentrated hydrochloric acid to the tetrabutyl titanate is 100:1: 20.
Further, in the second step, the activated carbon fiber is arranged on a dip coater, and the carbon fiber is soaked in TiO2Dissolving in sol for 5min, taking out carbon fiber at speed of 10mm/min, heat treating at 60 deg.C for 15min, and naturally cooling.
Further, in the sodium hydroxide solution of the third step, every 500ml of H2To O was added 33.2g of NaOH.
Furthermore, in the third step, the temperature of the homogeneous hydrothermal reaction is 180 ℃ and the time is 8 hours.
Further, in the fourth step, the hot press molding temperature is 170 ℃, the pressure is 10MPa, and the time is 10 min.
Compared with the prior art, the invention has the following beneficial technical effects:
1) in the invention, the surface of the carbon fiber is coated by a layer of thick nano-wire, TiO2The nano sheets are uniformly distributed on the surface of the carbon fiber, and the nano wires are connected in a staggered manner, so that the infiltration among resin matrixes is facilitated. The treatment of growing the nano-wire on the surface of the carbon fiber has no obvious damage to the mechanical property of the fiber, which is beneficial to improving the mechanical property of the composite material.
2) The modified carbon fiber-TiO of the invention2Prefabricated layer-TiO2The bending strength of the nano-wire multistage reinforced resin matrix composite material is the maximum, about 104.5Mpa, which is 32.8 percent higher than 70.2Mpa of the original carbon fiber reinforced composite material, the mechanical property is obviously enhanced, and the wear rate is only 1.21 × 10-5mm3the/N.m is reduced by 39.8 percent compared with the original carbon fiber reinforced composite material.
3) The invention has simple reaction process and short time consumption, and is beneficial to engineering application.
Drawings
FIG. 1 is a graph of surface topography analysis of carbon fibers treated by different modification methods of the present invention; wherein a and e are C0 obtained in modified example 1; b and f are C1 obtained in modified example 2; c and g are C3 obtained in modified example 3; d and h represent C5 obtained in modified example 4;
FIG. 2 is a graph showing the wear rate analysis of carbon fiber reinforced composite materials treated by different modification methods according to the present invention.
Detailed Description
The following examples are given to illustrate the present invention and should not be construed as limiting the scope of the present invention.
A preparation method of a carbon fiber-titanium dioxide multistage reinforced resin matrix composite material comprises the following steps:
firstly, pretreating carbon fibers, cutting the carbon fibers into squares of 5cm × 9cm, locking the squares, soaking the carbon fibers in a mixed solution of acetone and absolute ethyl alcohol in a volume ratio of 1:1 for 24-48H, removing a sizing agent on the surfaces of the carbon fibers, and then soaking the treated carbon fibers in H2O2And soaking the solution for 24-36 h, taking out the solution, washing the solution by using deionized water, and drying the solution in an electrothermal blowing drying oven at the temperature of 60 ℃ to obtain the activated carbon fiber.
Step two: prefabricated TiO on carbon fiber surface2A thin film layer. Preparing TiO2Sol: 300ml of absolute ethanol was taken in a beaker, and 3ml of concentrated hydrochloric acid was added dropwise with continuous stirring. Adding 60ml tetrabutyl titanate into the solution, continuously stirring for 30min, and aging for 12h to obtain TiO2And (3) sol. Installing the activated carbon fibers obtained in the step one on a lifting coating machine, and soaking the carbon fibers in the TiO2Taking out the carbon cloth at the speed of 10mm/min in the sol for 5min, placing the carbon cloth in a blast oven at the temperature of 60 ℃ for heat treatment for 15min, and then naturally cooling. The steps are respectively repeated for a plurality of times to obtain TiO with different thicknesses2Film-carbon fiber.
Step three: construction of TiO2Nanowire-thin film multilevel reinforcement. 33.2g of NaOH are weighed out and dissolved in 500ml of H2In O, taking the original carbon fiber in the first step and TiO with different thicknesses in the second step2The film-carbon fiber is respectively immersed in sodium hydroxide aqueous solution, put into a reaction kettle and transferred into a homogeneous phase hydrothermal instrument with the temperature of 180 ℃ for reaction for 8 hours. The obtained carbon fiber was thoroughly immersed in an aqueous hydrochloric acid solution and placed in a forced air oven at 70 deg.CAnd (5) 10 h. And then cleaning and drying the carbon fiber, and then placing the carbon fiber in a 400 ℃ muffle furnace for heat treatment for 3 h. Finally obtaining TiO with different thicknesses2nanowire-TiO2The film multi-stage reinforces the carbon fiber.
Step four: preparing the carbon fiber/resin matrix composite material. And (3) immersing the prepared carbon fiber in a phenolic resin solution with the mass fraction of about 20-30% to obtain a composite material prefabricated body. And then hot-pressing and molding the prefabricated body by adopting a flat vulcanizing machine, wherein the temperature is 170 ℃, the pressure is 10MPa, and the time is 10min, so that the carbon fiber reinforced resin matrix composite material is finally obtained.
Modified example 1
Cutting carbon fibers into squares of 5cm × 9cm, locking the edges, soaking the carbon fibers in a mixed solution of acetone and absolute ethyl alcohol at a ratio of 1:1 for 48 hours to remove a sizing agent on the surfaces of the carbon fibers, and then soaking the treated carbon fibers in H2O2And soaking the solution for 24 hours, taking out the solution, washing the solution by using deionized water, and placing the solution in an electrothermal blowing drying oven at 60 ℃ for drying to obtain activated carbon fibers C0.
Modified example 2
Cutting carbon fibers into squares of 5cm × 9cm, locking the edges, soaking the carbon fibers in a mixed solution of acetone and absolute ethyl alcohol at a ratio of 1:1 for 24 hours, removing a sizing agent on the surfaces of the carbon fibers, and then soaking the treated carbon fibers in H2O2And soaking the solution for 24 hours, taking out the solution, washing the solution by using deionized water, and placing the solution in an electrothermal blowing drying oven at 60 ℃ for drying to obtain the activated carbon fiber.
Step two: preparing TiO2Sol: 300ml of absolute ethanol was taken in a beaker, and 3ml of concentrated hydrochloric acid was added dropwise with continuous stirring. Adding 60ml tetrabutyl titanate into the solution, continuously stirring for 30min, and aging for 12h to obtain TiO2And (3) sol. Installing the activated carbon fibers in the step (1) on a dip coating machine, and soaking the carbon fibers in the TiO2Taking out the carbon cloth at the speed of 10mm/min in the sol for 5min, placing the carbon cloth in a blast oven at the temperature of 60 ℃ for heat treatment for 15min, and then naturally cooling.
Step three: 33.2g of NaOH are weighed out and dissolved in 500ml of H2In OAnd immersing the carbon fibers in a sodium hydroxide aqueous solution, putting the carbon fibers into a reaction kettle, and transferring the reaction kettle to a homogeneous phase hydrothermal instrument with the temperature of 180 ℃ for reaction for 8 hours. The resulting carbon fibers were thoroughly immersed in a 0.2M aqueous hydrochloric acid solution and placed in a 70 ℃ forced air oven for 10 h. And then, cleaning and drying the carbon fiber, and then, placing the carbon fiber in a 400 ℃ muffle furnace for heat treatment for 3h to obtain C1.
Modified example 3
Cutting carbon fibers into squares of 5cm × 9cm, locking the edges, soaking the carbon fibers in a mixed solution of acetone and absolute ethyl alcohol at a ratio of 1:1 for 36 hours to remove a sizing agent on the surfaces of the carbon fibers, and then soaking the treated carbon fibers in H2O2And soaking the solution for 24 hours, taking out the solution, washing the solution by using deionized water, and placing the solution in an electrothermal blowing drying oven at 60 ℃ for drying to obtain the activated carbon fiber.
Step two: preparing TiO2Sol: 300ml of absolute ethanol was taken in a beaker, and 3ml of concentrated hydrochloric acid was added dropwise with continuous stirring. Adding 60ml tetrabutyl titanate into the solution, continuously stirring for 30min, and aging for 12h to obtain TiO2And (3) sol. Installing the activated carbon fibers in the step (1) on a dip coating machine, and soaking the carbon fibers in the TiO2Taking out the carbon cloth at the speed of 10mm/min in the sol for 5min, placing the carbon cloth in a blast oven at the temperature of 60 ℃ for heat treatment for 15min, and then naturally cooling. This operation was repeated 3 times.
Step three: 33.2g of NaOH are weighed out and dissolved in 500ml of H2And O, immersing the carbon fibers in a sodium hydroxide aqueous solution, putting the carbon fibers into a reaction kettle, and transferring the reaction kettle to a 180 ℃ homogeneous phase hydrothermal instrument for reaction for 8 hours. The resulting carbon fibers were thoroughly immersed in a 0.2M aqueous hydrochloric acid solution and placed in a 70 ℃ forced air oven for 10 h. And then, cleaning and drying the carbon fiber, and then, placing the carbon fiber in a 400 ℃ muffle furnace for heat treatment for 3h to obtain C3.
Modified example 4
Cutting carbon fibers into squares of 5cm × 9cm, locking the edges, soaking the carbon fibers in a mixed solution of acetone and absolute ethyl alcohol at a ratio of 1:1 for 36 hours to remove a sizing agent on the surfaces of the carbon fibers, and then soaking the treated carbon fibers in H2O2Soaking the solution for 24h, taking out the soaked solution, and adding deionized waterAnd cleaning, and drying in an electrothermal blowing dry box at 60 ℃ to obtain the activated carbon fiber.
Step two: preparing TiO2Sol: 300ml of absolute ethanol was taken in a beaker, and 3ml of concentrated hydrochloric acid was added dropwise with continuous stirring. Adding 60ml tetrabutyl titanate into the solution, continuously stirring for 30min, and aging for 12h to obtain TiO2And (3) sol. Installing the activated carbon fibers in the step (1) on a dip coating machine, and soaking the carbon fibers in the TiO2Taking out the carbon cloth at the speed of 10mm/min in the sol for 5min, placing the carbon cloth in a blast oven at the temperature of 60 ℃ for heat treatment for 15min, and then naturally cooling. This operation was repeated 5 times.
Step three: 33.2g of NaOH are weighed out and dissolved in 500ml of H2And O, immersing the carbon fibers in a sodium hydroxide aqueous solution, putting the carbon fibers into a reaction kettle, and transferring the reaction kettle to a 180 ℃ homogeneous phase hydrothermal instrument for reaction for 8 hours. The resulting carbon fibers were thoroughly immersed in a 0.2M aqueous hydrochloric acid solution and placed in a 70 ℃ forced air oven for 10 h. And then, cleaning and drying the carbon fiber, and then, placing the carbon fiber in a 400 ℃ muffle furnace for heat treatment for 3h to obtain C4.
Comparative example
Cutting carbon fibers into squares of 5cm × 9cm, locking the edges, soaking the carbon fibers in a mixed solution of acetone and absolute ethyl alcohol at a ratio of 1:1 for 36 hours to remove a sizing agent on the surfaces of the carbon fibers, and then soaking the treated carbon fibers in H2O2And soaking the solution for 24 hours, taking out the solution, washing the solution by using deionized water, and placing the solution in an electrothermal blowing drying oven at 60 ℃ for drying to obtain the activated carbon fiber.
Step two: and (3) taking the prepared carbon fiber, and immersing the carbon fiber in a phenolic resin solution with the mass fraction of about 30% to obtain a composite material prefabricated body. And then hot-pressing and molding the prefabricated body by adopting a flat vulcanizing machine, wherein the temperature is 170 ℃, the pressure is 10MPa, and the time is 10min, so that the carbon fiber reinforced resin matrix composite material CFRP0 is finally obtained.
Example 1
Cutting carbon fibers into squares of 5cm × 9cm, locking the edges, soaking the carbon fibers in a mixed solution of acetone and absolute ethyl alcohol at a ratio of 1:1 for 48 hours to remove a sizing agent on the surfaces of the carbon fibers, and then removing the sizing agent on the surfaces of the carbon fibersSoaking the treated carbon fiber in H2O2And soaking the solution for 24 hours, taking out the solution, washing the solution by using deionized water, and placing the solution in an electrothermal blowing drying oven at 60 ℃ for drying to obtain the activated carbon fiber.
Step two: preparing TiO2Sol: 300ml of absolute ethanol was taken in a beaker, and 3ml of concentrated hydrochloric acid was added dropwise with continuous stirring. Adding 60ml tetrabutyl titanate into the solution, continuously stirring for 30min, and aging for 12h to obtain TiO2And (3) sol. Installing the activated carbon fibers in the step (1) on a dip coating machine, and soaking the carbon fibers in the TiO2Taking out the carbon cloth at the speed of 10mm/min in the sol for 5min, placing the carbon cloth in a blast oven at the temperature of 60 ℃ for heat treatment for 15min, and then naturally cooling.
Step three: 33.2g of NaOH are weighed out and dissolved in 500ml of H2And O, immersing the carbon fibers in a sodium hydroxide aqueous solution, putting the carbon fibers into a reaction kettle, and transferring the reaction kettle to a 180 ℃ homogeneous phase hydrothermal instrument for reaction for 8 hours. The resulting carbon fibers were thoroughly immersed in a 0.2M aqueous hydrochloric acid solution and placed in a 70 ℃ forced air oven for 10 h. And then cleaning and drying the carbon fiber, and then placing the carbon fiber in a 400 ℃ muffle furnace for heat treatment for 3 h.
Step four: and (3) taking the prepared carbon fiber, and immersing the carbon fiber in a phenolic resin solution with the mass fraction of about 30% to obtain a composite material prefabricated body. And then hot-pressing and molding the prefabricated body by adopting a flat vulcanizing machine, wherein the temperature is 170 ℃, the pressure is 10MPa, and the time is 10min, so that the carbon fiber-titanium dioxide multistage reinforced resin matrix composite material CFRP1 is finally obtained.
Example 2
Cutting carbon fibers into squares of 5cm × 9cm, locking the edges, soaking the carbon fibers in a mixed solution of acetone and absolute ethyl alcohol at a ratio of 1:1 for 24 hours, removing a sizing agent on the surfaces of the carbon fibers, and then soaking the treated carbon fibers in H2O2And soaking the solution for 24 hours, taking out the solution, washing the solution by using deionized water, and placing the solution in an electrothermal blowing drying oven at 60 ℃ for drying to obtain the activated carbon fiber.
Step two: preparing TiO2Sol: 300ml of absolute ethanol was taken in a beaker, and 3ml of concentrated hydrochloric acid was added dropwise with continuous stirring. 60ml of titanic acid tetra-acetate was added to the above solutionButyl ester, continuously stirring for 30min, aging for 12h to obtain TiO2And (3) sol. Installing the activated carbon fibers in the step (1) on a dip coating machine, and soaking the carbon fibers in the TiO2Taking out the carbon cloth at the speed of 10mm/min in the sol for 5min, placing the carbon cloth in a blast oven at the temperature of 60 ℃ for heat treatment for 15min, and then naturally cooling. This operation was repeated 3 times.
Step three: 33.2g of NaOH are weighed out and dissolved in 500ml of H2And O, immersing the carbon fibers in a sodium hydroxide aqueous solution, putting the carbon fibers into a reaction kettle, and transferring the reaction kettle to a 180 ℃ homogeneous phase hydrothermal instrument for reaction for 8 hours. The resulting carbon fibers were thoroughly immersed in a 0.2M aqueous hydrochloric acid solution and placed in a 70 ℃ forced air oven for 10 h. And then cleaning and drying the carbon fiber, and then placing the carbon fiber in a 400 ℃ muffle furnace for heat treatment for 3 h.
Step four: and (3) taking the prepared carbon fiber, and immersing the carbon fiber in a phenolic resin solution with the mass fraction of about 30% to obtain a composite material prefabricated body. And then hot-pressing and molding the prefabricated body by adopting a flat vulcanizing machine, wherein the temperature is 170 ℃, the pressure is 10MPa, and the time is 10min, so that the carbon fiber-titanium dioxide multistage reinforced resin matrix composite material CFRP3 is finally obtained.
Example 3
Cutting carbon fibers into squares of 5cm × 9cm, locking the edges, soaking the carbon fibers in a mixed solution of acetone and absolute ethyl alcohol at a ratio of 1:1 for 36 hours to remove a sizing agent on the surfaces of the carbon fibers, and then soaking the treated carbon fibers in H2O2And soaking the solution for 24 hours, taking out the solution, washing the solution by using deionized water, and placing the solution in an electrothermal blowing drying oven at 60 ℃ for drying to obtain the activated carbon fiber.
Step two: preparing TiO2Sol: 300ml of absolute ethanol was taken in a beaker, and 3ml of concentrated hydrochloric acid was added dropwise with continuous stirring. Adding 60ml tetrabutyl titanate into the solution, continuously stirring for 30min, and aging for 12h to obtain TiO2And (3) sol. Installing the activated carbon fibers in the step (1) on a dip coating machine, and soaking the carbon fibers in the TiO2Taking out the carbon cloth at the speed of 10mm/min in the sol for 5min, placing the carbon cloth in a blast oven at the temperature of 60 ℃ for heat treatment for 15min, and then naturally cooling. This operation was repeated 5 times.
Step three: balance33.2g of NaOH are dissolved in 500ml of H2And O, immersing the carbon fibers in a sodium hydroxide aqueous solution, putting the carbon fibers into a reaction kettle, and transferring the reaction kettle to a 180 ℃ homogeneous phase hydrothermal instrument for reaction for 8 hours. The resulting carbon fibers were thoroughly immersed in a 0.2M aqueous hydrochloric acid solution and placed in a 70 ℃ forced air oven for 10 h. And then cleaning and drying the carbon fiber, and then placing the carbon fiber in a 400 ℃ muffle furnace for heat treatment for 3 h.
Step four: and (3) taking the prepared carbon fiber, and immersing the carbon fiber in a phenolic resin solution with the mass fraction of about 30% to obtain a composite material prefabricated body. And then hot-pressing and molding the prefabricated body by adopting a flat vulcanizing machine, wherein the temperature is 170 ℃, the pressure is 10MPa, and the time is 10min, so that the carbon fiber-titanium dioxide multistage reinforced resin matrix composite material CFRP5 is finally obtained.
FIG. 1 shows: the surface of the original carbon fibers (a, e in fig. 1) is relatively smooth and regular, and during the production process of the fibers, narrow parallel grooves are generated along the longitudinal direction of the fibers. As can be seen from b and f in FIG. 1, the surface of the carbon fiber coated with 1 layer of film is largely coated with TiO2And (4) covering the nanorods. The high magnification SEM image (f in fig. 1) shows that the nanorods are cubic in shape and radially distributed along the cross section of the carbon fiber, growing disorderly. The low magnification and partial magnification SEM images of the 3-layer film coated carbon fiber after hydrothermal treatment are shown in fig. 1 c, g. As shown in fig. 1 c, the carbon fiber surface is covered with TiO in a dense and linear form2Nanorods, and the wires are approximately uniform in size. The TiO is clearly observable after high magnification (g in FIG. 1)2The nano wires grow vertically and are closely arranged and are connected with each other in a staggered manner, so that the surface roughness of the carbon fiber is obviously improved, the contact area is greatly increased, and the bonding strength of the composite material is favorably improved. The scanned graph of sample C5 is shown in fig. 1 d, h, and the carbon fiber surface has many small spheres with different sizes randomly stacked on top of the nanowire and disordered.
FIG. 2 shows the wear rates of the four samples through the above-mentioned continuous friction test, and it can be seen from the graph that the wear rates of the samples CFRP0, CFRP1, CFRP3 and CFRP5 are 2.01 × 10 respectively-5mm3/N·m、1.75×10-5mm3/N·m、1.21×10- 5mm3N.m and 1.58 × 10-5mm3M, where the wear rate of CFRP3 was the lowest, which was 39.8% lower than the wear rate of the original CFRP0 composite. It has further been demonstrated that CFRP3 composites have optimal wear resistance. Thus, TiO was constructed2nanowire-TiO2The film as the reinforcement of the resin-based composite material can improve the wear resistance of the material and prolong the service life of the material.
Claims (8)
1. A preparation method of a carbon fiber-titanium dioxide multistage reinforced resin matrix composite is characterized by comprising the following steps:
step one, carbon fiber pretreatment: cutting carbon fiber, soaking in mixed solution of acetone and anhydrous alcohol to eliminate the surface sizing agent, and soaking the carbon fiber in H2O2Soaking in the solution, taking out, washing with deionized water, and drying to obtain activated carbon fiber;
step two, prefabricating TiO on the surface of the carbon fiber2Film layer: preparing TiO2Sol, dissolving activated carbon fiber in TiO2Soaking in sol, taking out carbon fiber, heat treating, naturally cooling, and repeating soaking-heat treating-cooling process for several times to obtain TiO with different thicknesses2Film-carbon fiber;
step three, constructing TiO2Nanowire-thin film multilevel reinforcement: taking TiO with different thicknesses in the second step2Respectively immersing the film-carbon fiber in an aqueous solution of sodium hydroxide, then respectively carrying out homogeneous hydrothermal reaction, thoroughly immersing the obtained carbon fiber in an aqueous solution of hydrochloric acid, treating at 70 ℃ for 10h, then cleaning and drying the carbon fiber, and then carrying out heat treatment at 400 ℃ for 3h to finally obtain TiO with different thicknesses2nanowire-TiO2A thin film multi-stage reinforcing carbon fiber;
step four, preparing the carbon fiber/resin matrix composite material: taking the TiO with different thicknesses obtained in the step three2nanowire-TiO2Respectively immersing the film multilevel reinforced carbon fibers in phenolic resin solution with the mass fraction of 20-30% to obtain a composite material prefabricated body, and then prefabricating the composite materialAnd (3) hot-pressing and forming to finally obtain the carbon fiber-titanium dioxide multistage carbon fiber reinforced resin matrix composite.
2. The preparation method of the carbon fiber-titanium dioxide multistage reinforced resin matrix composite material according to claim 1, characterized in that in the step one, the carbon fibers are cut into a square of 5cm x 9cm and are locked, and then the square is soaked in a mixed solution of acetone and absolute ethyl alcohol in a volume ratio of 1:1 for 24-48 hours, and a sizing agent on the surfaces of the carbon fibers is removed.
3. The method for preparing the carbon fiber-titanium dioxide multistage reinforced resin matrix composite material as claimed in claim 1, wherein in the first step, the carbon fiber without sizing agent is soaked in H with a volume fraction of 30%2O2And soaking the solution for 24 hours, taking out the solution, washing the solution by using deionized water, and drying the solution at the temperature of 60 ℃ to obtain the activated carbon fiber.
4. The method for preparing the carbon fiber-titanium dioxide multistage reinforced resin matrix composite material according to claim 1, wherein TiO in the second step2The sol preparation process is as follows: dropwise adding concentrated hydrochloric acid into absolute ethyl alcohol, continuously stirring, adding tetrabutyl titanate into the solution, continuously stirring for 30min, and aging for 12h to obtain TiO2And sol, wherein the volume ratio of the absolute ethyl alcohol to the concentrated hydrochloric acid to the tetrabutyl titanate is 100:1: 20.
5. The method for preparing the carbon fiber-titanium dioxide multistage reinforced resin-based composite material as claimed in claim 1, wherein in the second step, the activated carbon fiber is installed on a dip coater, and the carbon fiber is soaked in TiO2Dissolving in sol for 5min, taking out carbon fiber at speed of 10mm/min, heat treating at 60 deg.C for 15min, and naturally cooling.
6. The method for preparing the carbon fiber-titanium dioxide multistage reinforced resin matrix composite material according to claim 1,in the sodium hydroxide solution of the third step, every 500ml of H2To O was added 33.2g of NaOH.
7. The method for preparing the carbon fiber-titanium dioxide multistage reinforced resin matrix composite material according to claim 1, wherein the temperature of the homogeneous hydrothermal reaction in the third step is 180 ℃ and the time is 8 hours.
8. The method for preparing the carbon fiber-titanium dioxide multistage reinforced resin matrix composite material according to claim 1, wherein the hot press molding temperature in the fourth step is 170 ℃, the pressure is 10MPa, and the time is 10 min.
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