CN113665188A - Titanium-carbon fiber-titanium sandwich composite material and preparation method thereof - Google Patents
Titanium-carbon fiber-titanium sandwich composite material and preparation method thereof Download PDFInfo
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- CN113665188A CN113665188A CN202110990356.4A CN202110990356A CN113665188A CN 113665188 A CN113665188 A CN 113665188A CN 202110990356 A CN202110990356 A CN 202110990356A CN 113665188 A CN113665188 A CN 113665188A
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- 239000010936 titanium Substances 0.000 title claims abstract description 66
- 229910052719 titanium Inorganic materials 0.000 title claims abstract description 64
- 239000002131 composite material Substances 0.000 title claims abstract description 55
- CYKMNKXPYXUVPR-UHFFFAOYSA-N [C].[Ti] Chemical compound [C].[Ti] CYKMNKXPYXUVPR-UHFFFAOYSA-N 0.000 title claims abstract description 50
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 229920000049 Carbon (fiber) Polymers 0.000 claims abstract description 99
- 239000004917 carbon fiber Substances 0.000 claims abstract description 99
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 88
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 61
- 239000010949 copper Substances 0.000 claims abstract description 61
- 229910052802 copper Inorganic materials 0.000 claims abstract description 61
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 32
- 239000000126 substance Substances 0.000 claims abstract description 32
- 238000007747 plating Methods 0.000 claims abstract description 31
- 238000010438 heat treatment Methods 0.000 claims abstract description 30
- 230000003647 oxidation Effects 0.000 claims abstract description 25
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 25
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 22
- -1 titanium hydride Chemical compound 0.000 claims abstract description 22
- 229910000048 titanium hydride Inorganic materials 0.000 claims abstract description 22
- 239000004744 fabric Substances 0.000 claims abstract description 18
- 239000000463 material Substances 0.000 claims abstract description 17
- 230000004913 activation Effects 0.000 claims abstract description 16
- 229910052786 argon Inorganic materials 0.000 claims abstract description 16
- 239000007789 gas Substances 0.000 claims abstract description 16
- 239000007791 liquid phase Substances 0.000 claims abstract description 16
- 238000001035 drying Methods 0.000 claims abstract description 15
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 14
- 206010070834 Sensitisation Diseases 0.000 claims abstract description 11
- 230000008313 sensitization Effects 0.000 claims abstract description 11
- 238000007731 hot pressing Methods 0.000 claims abstract description 10
- 238000006243 chemical reaction Methods 0.000 claims abstract description 9
- 239000011248 coating agent Substances 0.000 claims abstract description 9
- 238000000576 coating method Methods 0.000 claims abstract description 9
- 238000001816 cooling Methods 0.000 claims abstract description 8
- 238000001291 vacuum drying Methods 0.000 claims abstract description 8
- HEMHJVSKTPXQMS-UHFFFAOYSA-M sodium hydroxide Substances [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 23
- 238000000034 method Methods 0.000 claims description 14
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 14
- ROFVEXUMMXZLPA-UHFFFAOYSA-N Bipyridyl Chemical compound N1=CC=CC=C1C1=CC=CC=N1 ROFVEXUMMXZLPA-UHFFFAOYSA-N 0.000 claims description 7
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims description 7
- 229910021205 NaH2PO2 Inorganic materials 0.000 claims description 7
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 7
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 7
- 229910021626 Tin(II) chloride Inorganic materials 0.000 claims description 7
- 239000002253 acid Substances 0.000 claims description 7
- 239000003513 alkali Substances 0.000 claims description 7
- 239000012459 cleaning agent Substances 0.000 claims description 7
- 229910000365 copper sulfate Inorganic materials 0.000 claims description 7
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims description 7
- BEGBSFPALGFMJI-UHFFFAOYSA-N ethene;sodium Chemical group [Na].C=C BEGBSFPALGFMJI-UHFFFAOYSA-N 0.000 claims description 7
- 239000008098 formaldehyde solution Substances 0.000 claims description 7
- 229910017604 nitric acid Inorganic materials 0.000 claims description 7
- 230000001590 oxidative effect Effects 0.000 claims description 7
- 230000001235 sensitizing effect Effects 0.000 claims description 7
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 7
- AXZWODMDQAVCJE-UHFFFAOYSA-L tin(II) chloride (anhydrous) Chemical compound [Cl-].[Cl-].[Sn+2] AXZWODMDQAVCJE-UHFFFAOYSA-L 0.000 claims description 7
- 238000004321 preservation Methods 0.000 claims description 2
- 239000011734 sodium Substances 0.000 claims description 2
- 239000011159 matrix material Substances 0.000 abstract description 9
- 239000011156 metal matrix composite Substances 0.000 abstract description 8
- 239000003921 oil Substances 0.000 description 18
- 229910052751 metal Inorganic materials 0.000 description 9
- 239000002184 metal Substances 0.000 description 9
- 238000002441 X-ray diffraction Methods 0.000 description 6
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 5
- CDBYLPFSWZWCQE-UHFFFAOYSA-L sodium carbonate Substances [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 5
- 229910000029 sodium carbonate Inorganic materials 0.000 description 5
- 235000004237 Crocus Nutrition 0.000 description 4
- 241000596148 Crocus Species 0.000 description 4
- 238000001878 scanning electron micrograph Methods 0.000 description 4
- 238000000498 ball milling Methods 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 229910010271 silicon carbide Inorganic materials 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 238000005979 thermal decomposition reaction Methods 0.000 description 2
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 239000002313 adhesive film Substances 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005238 degreasing Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000007772 electroless plating Methods 0.000 description 1
- 239000002783 friction material Substances 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 229910021404 metallic carbon Inorganic materials 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000005011 phenolic resin Substances 0.000 description 1
- 229920001568 phenolic resin Polymers 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 239000002296 pyrolytic carbon Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
Images
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B5/00—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts
- B32B5/02—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by structural features of a fibrous or filamentary layer
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B15/00—Layered products comprising a layer of metal
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B15/00—Layered products comprising a layer of metal
- B32B15/14—Layered products comprising a layer of metal next to a fibrous or filamentary layer
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
- C23C18/08—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of metallic material
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/31—Coating with metals
- C23C18/38—Coating with copper
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2250/00—Layers arrangement
- B32B2250/40—Symmetrical or sandwich layers, e.g. ABA, ABCBA, ABCCBA
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2262/00—Composition or structural features of fibres which form a fibrous or filamentary layer or are present as additives
- B32B2262/10—Inorganic fibres
- B32B2262/106—Carbon fibres, e.g. graphite fibres
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- Chemical & Material Sciences (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Chemically Coating (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
Abstract
The invention relates to a titanium-carbon fiber-titanium sandwich-type composite material and a preparation method thereof, belonging to the technical field of metal matrix composite materials. The titanium-carbon fiber-titanium sandwich-type composite material has the structure that copper and titanium are sequentially arranged on two sides of carbon fibers from inside to outside. Carrying out hot air oxidation, liquid phase oxidation, ultrasonic alkaline oil removal, sensitization and activation treatment on the carbon fiber cloth; carrying out chemical copper plating on the carbon fiber cloth to obtain carbon fiber/copper; coating titanium hydride solution dissolved in absolute ethyl alcohol on two sides of the carbon fiber/copper, drying in a vacuum drying oven, and then heating in a high-temperature tube furnace with argon gas inlet flow of 80mL/min, wherein the argon gas is introduced from the beginning of heating to the end of reaction and is cooled to room temperature; and (3) placing the treated material into a mold for fixing, placing the mold into a vacuum hot-pressing furnace, and cooling the mold along with the furnace to obtain the titanium-carbon fiber-titanium sandwich-type composite material. The composite material prepared by the invention has stable combination of the matrix and excellent material performance.
Description
Technical Field
The invention relates to a titanium-carbon fiber-titanium sandwich-type composite material and a preparation method thereof, belonging to the technical field of metal matrix composite materials.
Background
Metal matrix composites having good electrical and thermal conductivity, excellent frictional wear and ductility have become increasingly popular in recent years. However, some metal matrixes have poor mechanical properties, and particularly, the properties such as strength and hardness of the metal matrixes are rapidly reduced in a high-temperature environment, so that the mechanical properties of the metal matrixes are generally improved by adopting fiber reinforcement. The carbon fiber has a series of advantages of high strength, high modulus, good lubricity, low thermal expansion coefficient, excellent electric conduction and heat conduction performance, no melting and softening at high temperature, no hardening at low temperature and the like. It is expected that the excellent mechanical properties of the carbon fiber can be obtained while maintaining the excellent properties of the metal matrix composite because of the excellent properties of the metal matrix composite and the carbon fiber.
The carbon fiber reinforced metal matrix composite material has the advantages of high electrical and thermal conductivity, good toughness and corrosion resistance of metal, high toughness and stable performance at high temperature of carbon fiber and the like, and is widely applied to the fields of heat conduction materials, conductive materials, friction materials and the like. The carbon fiber reinforced metal matrix composite has higher specific rigidity and specific strength, excellent corrosion resistance and high-temperature creep resistance, greatly improved tensile strength, hardness and Young modulus, and wide application prospect in the fields of aerospace, military industry, automobile industry, marine application, chemical energy, biomedical treatment and the like.
The method comprises the steps of carrying out pyrolytic carbon deposition-silicon carbide deposition treatment on carbon fibers, then coating the carbon fibers with phenolic resin, then carrying out ball milling on the carbon fibers and matrix metal to obtain uniformly mixed powder, and finally obtaining the SiC-coated carbon fiber reinforced metal matrix composite through a pressing-sintering process. However, in the preparation process of the composite material, carbon fibers, metal and the like are mixed by ball milling, so that the carbon fibers are seriously damaged, and meanwhile, the carbon fibers are unevenly distributed and the carbon fibers and the metal generate obvious interface incompatibility phenomenon by adopting a pressing and sintering mode to prepare the material, so that the material performance is further influenced.
The graphite-like structure of the carbon fiber causes the surface of the carbon fiber to have large inertia and lack of active functional groups, so the carbon fiber has poor adhesion with a metal matrix, has a series of interface problems and limits the application of the carbon fiber to a certain extent.
Disclosure of Invention
Aiming at the problems and the defects in the prior art, the invention provides a titanium-carbon fiber-titanium sandwich type composite material and a preparation method thereof. The composite material prepared by the invention has the advantages of stable combination of the matrix, excellent material performance, greatly improved mechanical property and conductivity, simple preparation process and low cost. The invention is realized by the following technical scheme.
A sandwich-type Ti-C-Ti composite material features that copper and Ti are sequentially arranged on both sides of carbon fibre from inside to outside.
A preparation method of a titanium-carbon fiber-titanium sandwich composite material comprises the following specific steps:
step 1, carrying out hot air oxidation, liquid phase oxidation, ultrasonic alkaline oil removal, sensitization and activation treatment on carbon fiber cloth;
step 2, placing the carbon fiber treated in the step 1 in a chemical plating tank at 60 ℃ and stirring for 1h for chemical copper plating, and then placing the sample in a drying oven at 80 ℃ for 15h to obtain carbon fiber/copper;
step 3, coating titanium hydride solution dissolved in absolute ethyl alcohol on two sides of the carbon fiber/copper obtained in the step 2, drying the carbon fiber/copper in a vacuum drying oven at the temperature of 80 ℃, and then heating the carbon fiber/copper in a high-temperature tube furnace with argon gas flow of 80mL/min, wherein the argon gas is introduced from the beginning of heating to the end of reaction and is cooled to room temperature;
and 4, putting the material processed in the step 3 into a mold for fixing, putting the mold into a vacuum hot pressing furnace, and cooling the mold along with the furnace to obtain the titanium-carbon fiber-titanium sandwich-type composite material.
And (3) oxidizing the carbon fiber cloth in the step (1) for 30min in hot air at the temperature of 300-450 ℃.
In the step 1, liquid-phase oxidation is carried out for 30-80 min at the temperature of 80 ℃ in a mixed acid solution of concentrated nitric acid (analytically pure) and concentrated sulfuric acid (analytically pure) in a volume ratio of 1: 1-5: 1.
The ultrasonic alkaline oil removal in the step 1 is carried out in the presence of 60-100 g/L, Na NaOH2CO310-30 g/L of alkali liquor and 1-5 g/L of cleaning agent for 20-50 min.
The sensitization in step 1 is to SnCl2·2H2O20~30g/L、NaH2PO2·H2Sensitizing for 30-60 min in sensitizing solution of O5-10 g/L, 36-38 wt% HCl 15-25 ml/L and tin block 10-20 g/L.
The activation treatment in the step 1 is to activate the silver nitrate solution in a concentration of 25-35 g/L at 30-45 ℃ for 40-80 min.
In the step 2, the chemical plating bath solution in the chemical plating bath is 10-20 g/L of anhydrous copper sulfate, 30-50 g/L of sodium ethylene diamine tetracetate, 20-30 ml/L of 37wt% formaldehyde solution, 0.04-0.06 g/L of 2, 2-bipyridine and 8-12 g/L of sodium hydroxide.
In the step 3, the mass ratio of titanium hydride to absolute ethyl alcohol in the titanium hydride solution dissolved in absolute ethyl alcohol is 1: 1-1: 4, the heating rate is 5-10 ℃/min, the temperature is 750-950 ℃, and the heating and heat preservation time is 20-60 min.
And in the step 4, the temperature of the vacuum hot-pressing furnace is 600-750 ℃, the pressure is increased to 2-4.5 MPa, and the pressure is maintained for 2-4 h.
The reagents mentioned above, which are not referred to in concentration, are all analytical reagents.
The invention has the beneficial effects that:
the method comprises the steps of carrying out hot air oxidation, liquid phase oxidation, alkaline degreasing, sensitization and activation on carbon fibers so as to remove various adhesive films and oil stains on the surfaces of the carbon fibers; the chemical activity of the surface of the carbon fiber is improved; the surface of the carbon fiber cloth is adsorbed with a large amount of particles or granules which are easy to oxidize, so that the surface of the carbon fiber cloth is easier to nucleate, the induction period is shortened, and a catalytic active layer is easier to form. The chemical plating method ensures that the copper plating layer is uniformly, finely and completely distributed on the surface of the carbon fiber, enhances the bonding strength between the non-metallic carbon and the metallic copper, and improves the interface adhesive force. The thermal decomposition method is simple and convenient to operate, easy to meet conditions, easy to control reaction, rich in raw material reserves and convenient for large-scale production and use. Compared with a titanium-based matrix material, the prepared titanium-carbon fiber-titanium sandwich composite material has greatly improved bending strength, elastic modulus and Brinell hardness, and can provide ideas and methods for preparing other reinforced metal-based composite materials.
Drawings
FIG. 1 is a schematic structural view of a titanium-carbon fiber-titanium "sandwich" type composite material of the present invention;
FIG. 2 is an XRD pattern of a carbon fiber obtained in example 1 of the present invention;
FIG. 3 is an XRD pattern of carbon fiber/copper obtained in example 1 of the present invention;
FIG. 4 is an XRD pattern of a titanium-carbon fiber-titanium "sandwich" type composite material obtained in example 1 of the present invention;
FIG. 5 is an SEM image of carbon fiber/copper obtained in example 1 of the present invention;
FIG. 6 is an SEM image of a titanium-carbon fiber-titanium "sandwich" type composite material obtained in example 1 of the present invention.
Detailed Description
The invention is further described with reference to the following drawings and detailed description.
Example 1
As shown in fig. 1, the titanium-carbon fiber-titanium sandwich composite material has a structure that copper and titanium are sequentially arranged on two sides of a carbon fiber from inside to outside. .
The preparation method of the titanium-carbon fiber-titanium sandwich composite material comprises the following specific steps:
step 1, carrying out hot air oxidation, liquid phase oxidation, ultrasonic alkaline oil removal, sensitization and activation treatment on carbon fiber cloth;
oxidizing the carbon fiber cloth in hot air at 450 ℃ for 30 min;
performing liquid-phase oxidation treatment for 30min at 80 ℃ in a mixed acid solution of concentrated nitric acid (analytically pure, 65-68 wt%) and concentrated sulfuric acid (analytically pure, 95-98 wt%) in a volume ratio of 2: 1;
the ultrasonic alkaline oil removal is carried out in the presence of NaOH60g/L, Na2CO330g/L of cleaning agent (blue moon oil stain crocus) 2g/L of alkali liquor, and ultrasonic vibration (ultrasonic frequency is 20 KHz) for 50 min;
sensitised to presence of SnCl2·2H2O30g/L、NaH2PO2·H2Sensitizing for 60min in sensitizing solution of O10g/L, 36-38 wt% HCl25ml/L and tin block 20 g/L;
the activation treatment is carried out in 35g/L silver nitrate solution at 45 deg.C for 70 min.
Step 2, placing the carbon fiber treated in the step 1 in a chemical plating tank at 60 ℃ and stirring for 1h for chemical copper plating, and then placing the sample in a drying oven at 80 ℃ for 15h to obtain carbon fiber/copper; wherein the chemical plating bath solution in the chemical plating bath is 18g/L of anhydrous copper sulfate, 45g/L of sodium ethylene diamine tetracetate, 25ml/L of 37wt% formaldehyde solution, 0.06g/L of 2, 2-bipyridine and 11g/L of sodium hydroxide;
step 3, coating titanium hydride solution dissolved in absolute ethyl alcohol on two sides of the carbon fiber/copper obtained in the step 2 (the mass ratio of titanium hydride to absolute ethyl alcohol in the titanium hydride solution of absolute ethyl alcohol is 1: 3), putting the carbon fiber/copper into a vacuum drying oven at 80 ℃, drying the carbon fiber/copper, putting the carbon fiber/copper into a high-temperature tube furnace with argon gas inlet flow of 80mL/min, heating the carbon fiber/copper to 800 ℃ at the heating rate of 6 ℃/min, and keeping the temperature for 40min, wherein the argon gas is introduced from the beginning of heating to the end of reaction and is cooled to room temperature;
and 4, putting the material processed in the step 3 into a mold for fixing, putting the mold into a vacuum hot pressing furnace, heating to 700 ℃, pressurizing to 4MPa, keeping the pressure for 2 hours, and cooling along with the furnace to obtain the titanium-carbon fiber-titanium sandwich-type composite material.
The XRD pattern of the carbon fibers in this example is shown in FIG. 2; the XRD pattern of carbon fiber/copper is shown in fig. 3; the XRD pattern of the titanium-carbon fiber-titanium "sandwich" type composite material is shown in figure 4; the SEM image of the resulting carbon fiber/copper is shown in fig. 5; the SEM image of the resulting titanium-carbon fiber-titanium "sandwich" type composite material is shown in fig. 6; it can be seen from fig. 2 to 6 that the metallic copper and titanium can be uniformly and densely coated on the entire carbon fiber in sequence by the electroless plating and the thermal decomposition.
The thickness of the titanium-carbon fiber-titanium sandwich composite material prepared by the embodiment is 0.59mm, compared with the titanium-based matrix material with the same volume, the weight is reduced by 22%, the tensile strength is improved by 18.7%, and the resistivity is reduced by 5.85%.
Example 2
As shown in fig. 1, the titanium-carbon fiber-titanium sandwich composite material has a structure that copper and titanium are sequentially arranged on two sides of a carbon fiber from inside to outside.
The preparation method of the titanium-carbon fiber-titanium sandwich composite material comprises the following specific steps:
step 1, carrying out hot air oxidation, liquid phase oxidation, ultrasonic alkaline oil removal, sensitization and activation treatment on carbon fiber cloth;
oxidizing the carbon fiber cloth in hot air at 450 ℃ for 30 min;
performing liquid-phase oxidation treatment for 30min at 80 ℃ in a mixed acid solution of concentrated nitric acid (analytically pure, 65-68 wt%) and concentrated sulfuric acid (analytically pure, 95-98 wt%) in a volume ratio of 2: 1;
the ultrasonic alkaline oil removal is carried out in the presence of NaOH60g/L, Na2CO330g/L of cleaning agent (blue moon oil stain crocus) 2g/L of alkali liquor, and ultrasonic vibration (ultrasonic frequency is 20 KHz) for 50 min;
sensitised to presence of SnCl2·2H2O30g/L、NaH2PO2·H2Sensitizing for 60min in sensitizing solution of O10g/L, 36-38 wt% HCl25ml/L and tin block 20 g/L;
the activation treatment is carried out in 35g/L silver nitrate solution at 45 deg.C for 70 min.
Step 2, placing the carbon fiber treated in the step 1 in a chemical plating tank at 60 ℃ and stirring for 1h for chemical copper plating, and then placing the sample in a drying oven at 80 ℃ for 15h to obtain carbon fiber/copper; wherein the chemical plating bath solution in the chemical plating bath is 18g/L of anhydrous copper sulfate, 45g/L of sodium ethylene diamine tetracetate, 25ml/L of 37wt% formaldehyde solution, 0.06g/L of 2, 2-bipyridine and 11g/L of sodium hydroxide;
step 3, coating titanium hydride solution dissolved in absolute ethyl alcohol on two sides of the carbon fiber/copper obtained in the step 2 (the mass ratio of titanium hydride to absolute ethyl alcohol in the titanium hydride solution of absolute ethyl alcohol is 1: 3), putting the carbon fiber/copper into a vacuum drying oven at 80 ℃, drying the carbon fiber/copper, putting the carbon fiber/copper into a high-temperature tube furnace with argon gas inlet flow of 80mL/min, heating the carbon fiber/copper to 800 ℃ at the heating rate of 6 ℃/min, and keeping the temperature for 40min, wherein the argon gas is introduced from the beginning of heating to the end of reaction and is cooled to room temperature;
and 4, putting the material processed in the step 3 into a mold for fixing, putting the mold into a vacuum hot pressing furnace, heating to 700 ℃, pressurizing to 4MPa, keeping the pressure for 3 hours, and cooling along with the furnace to obtain the titanium-carbon fiber-titanium sandwich-type composite material.
The thickness of the titanium-carbon fiber-titanium sandwich-type composite material prepared by the embodiment is 0.61mm, and compared with a titanium-based matrix material with the same volume, the titanium-carbon fiber-titanium sandwich-type composite material has the advantages that the mass is reduced by 22.7%, the tensile strength is improved by 19.2%, and the resistivity is reduced by 6.14%.
Example 3
As shown in fig. 1, the titanium-carbon fiber-titanium sandwich composite material has a structure that copper and titanium are sequentially arranged on two sides of a carbon fiber from inside to outside.
The preparation method of the titanium-carbon fiber-titanium sandwich composite material comprises the following specific steps:
step 1, carrying out hot air oxidation, liquid phase oxidation, ultrasonic alkaline oil removal, sensitization and activation treatment on carbon fiber cloth;
oxidizing the carbon fiber cloth in hot air at 450 ℃ for 30 min;
performing liquid-phase oxidation treatment for 30min at 80 ℃ in a mixed acid solution of concentrated nitric acid (analytically pure, 65-68 wt%) and concentrated sulfuric acid (analytically pure, 95-98 wt%) in a volume ratio of 2: 1;
the ultrasonic alkaline oil removal is carried out in the presence of NaOH80g/L, Na2CO3Ultrasonic vibration (ultrasonic frequency is 20 KHz) for 30min in 20g/L alkali liquor and 3g/L cleaning agent (blue moon oil stain Kexing);
sensitised to presence of SnCl2·2H2O25g/L、NaH2PO2·H2Sensitizing for 40min in sensitizing solution of O8g/L, 36-38 wt% of HCl20ml/L and 15g/L of tin blocks;
the activation treatment is carried out in 30g/L silver nitrate solution at 40 deg.C for 60 min.
Step 2, placing the carbon fiber treated in the step 1 in a chemical plating tank at 60 ℃ and stirring for 1h for chemical copper plating, and then placing the sample in a drying oven at 80 ℃ for 15h to obtain carbon fiber/copper; wherein the chemical plating bath solution in the chemical plating bath is 15g/L of anhydrous copper sulfate, 40g/L of sodium ethylene diamine tetracetate, 25ml/L of 37wt% formaldehyde solution, 0.05g/L of 2, 2-bipyridine and 10g/L of sodium hydroxide;
step 3, coating titanium hydride solution dissolved in absolute ethyl alcohol on two sides of the carbon fiber/copper obtained in the step 2 (the mass ratio of titanium hydride to absolute ethyl alcohol in the titanium hydride solution of absolute ethyl alcohol is 1: 2), putting the carbon fiber/copper into a vacuum drying oven at 80 ℃, drying the carbon fiber/copper, putting the carbon fiber/copper into a high-temperature tube furnace with argon gas inlet flow of 80mL/min, heating the carbon fiber/copper to 900 ℃ at the heating rate of 10 ℃/min, and keeping the temperature for 30min, wherein the argon gas is introduced from the beginning of heating to the end of reaction and is cooled to room temperature;
and 4, putting the material processed in the step 3 into a mold for fixing, putting the mold into a vacuum hot pressing furnace, heating to 700 ℃, pressurizing to 4MPa, keeping the pressure for 3 hours, and cooling along with the furnace to obtain the titanium-carbon fiber-titanium sandwich-type composite material.
The thickness of the titanium-carbon fiber-titanium sandwich-type composite material prepared by the embodiment is 0.63mm, and compared with a titanium-based base material with the same volume, the titanium-carbon fiber-titanium sandwich-type composite material has the advantages that the mass is reduced by 23.3%, the tensile strength is improved by 19.8%, and the resistivity is reduced by 6.73%.
Example 4
As shown in fig. 1, the titanium-carbon fiber-titanium sandwich composite material has a structure that copper and titanium are sequentially arranged on two sides of a carbon fiber from inside to outside.
The preparation method of the titanium-carbon fiber-titanium sandwich composite material comprises the following specific steps:
step 1, carrying out hot air oxidation, liquid phase oxidation, ultrasonic alkaline oil removal, sensitization and activation treatment on carbon fiber cloth;
oxidizing the carbon fiber cloth in hot air at the temperature of 300 ℃ for 30 min;
liquid-phase oxidation is carried out for 40min at the temperature of 80 ℃ in a mixed acid solution of concentrated nitric acid (analytically pure, 65-68 wt%) and concentrated sulfuric acid (analytically pure, 95-98 wt%) in a volume ratio of 1: 1;
the ultrasonic alkaline oil removal is carried out in the presence of NaOH80g/L, Na2CO3Ultrasonic vibration (ultrasonic frequency is 20 KHz) for 30min in 20g/L alkali liquor and 5g/L cleaning agent (blue moon oil stain crocus);
sensitised to presence of SnCl2·2H2O25g/L、NaH2PO2·H2Sensitizing for 40min in sensitizing solution of O8g/L, 36-38 wt% of HCl20ml/L and 15g/L of tin blocks;
the activation treatment is carried out in 30g/L silver nitrate solution at 40 deg.C for 40 min.
Step 2, placing the carbon fiber treated in the step 1 in a chemical plating tank at 60 ℃ and stirring for 1h for chemical copper plating, and then placing the sample in a drying oven at 80 ℃ for 15h to obtain carbon fiber/copper; wherein the chemical plating bath solution in the chemical plating bath is 10g/L of anhydrous copper sulfate, 30g/L of sodium ethylene diamine tetracetate, 20ml/L of 37wt% formaldehyde solution, 0.05g/L of 2, 2-bipyridine and 12g/L of sodium hydroxide;
step 3, coating titanium hydride solution dissolved in absolute ethyl alcohol on two sides of the carbon fiber/copper obtained in the step 2 (the mass ratio of titanium hydride to absolute ethyl alcohol in the titanium hydride solution of absolute ethyl alcohol is 1: 1), putting the carbon fiber/copper into a vacuum drying oven at 80 ℃, drying the carbon fiber/copper, putting the carbon fiber/copper into a high-temperature tube furnace with argon gas inlet flow of 80mL/min, heating the carbon fiber/copper to 950 ℃ at the heating rate of 10 ℃/min, and keeping the temperature for 20min, wherein the argon gas is introduced from the beginning of heating to the end of reaction and is cooled to room temperature;
and 4, putting the material processed in the step 3 into a mold for fixing, putting the mold into a vacuum hot pressing furnace, heating to 750 ℃, pressurizing to 4.5MPa, maintaining the pressure for 3 hours, and cooling along with the furnace to obtain the titanium-carbon fiber-titanium sandwich-type composite material.
The thickness of the titanium-carbon fiber-titanium sandwich composite material prepared by the embodiment is 0.65mm, and compared with a titanium-based matrix material with the same volume, the titanium-carbon fiber-titanium sandwich composite material has the advantages that the mass is reduced by 22.4%, the tensile strength is improved by 18.8%, and the resistivity is reduced by 5.94%.
Example 5
As shown in fig. 1, the titanium-carbon fiber-titanium sandwich composite material has a structure that copper and titanium are sequentially arranged on two sides of a carbon fiber from inside to outside.
The preparation method of the titanium-carbon fiber-titanium sandwich composite material comprises the following specific steps:
step 1, carrying out hot air oxidation, liquid phase oxidation, ultrasonic alkaline oil removal, sensitization and activation treatment on carbon fiber cloth;
oxidizing the carbon fiber cloth in hot air at the temperature of 400 ℃ for 30 min;
performing liquid-phase oxidation treatment for 80min at the temperature of 80 ℃ in a mixed acid solution of concentrated nitric acid (analytically pure, 65-68 wt%) and concentrated sulfuric acid (analytically pure, 95-98 wt%) in a volume ratio of 5: 1;
the ultrasonic alkaline oil removal is carried out in the presence of NaOH100g/L, Na2CO3Ultrasonic vibration (ultrasonic frequency is 20 KHz) is carried out for 20min in 10g/L of alkali liquor with 1g/L of cleaning agent (blue moon oil stain crocus);
sensitised to presence of SnCl2·2H2O20g/L、NaH2PO2·H2Sensitizing for 30min in sensitizing solution of O5g/L, 36-38 wt% of HCl15ml/L and 10g/L of tin block;
the activation treatment is carried out for 80min in 25g/L silver nitrate solution at 30 deg.C.
Step 2, placing the carbon fiber treated in the step 1 in a chemical plating tank at 60 ℃ and stirring for 1h for chemical copper plating, and then placing the sample in a drying oven at 80 ℃ for 15h to obtain carbon fiber/copper; wherein the chemical plating bath solution in the chemical plating bath is 20g/L of anhydrous copper sulfate, 50g/L of sodium ethylene diamine tetracetate, 30ml/L of 37wt% formaldehyde solution, 0.04g/L of 2, 2-bipyridine and 8g/L of sodium hydroxide;
step 3, coating titanium hydride solution dissolved in absolute ethyl alcohol on two sides of the carbon fiber/copper obtained in the step 2 (the mass ratio of titanium hydride to absolute ethyl alcohol in the titanium hydride solution of absolute ethyl alcohol is 1: 4), putting the carbon fiber/copper into a vacuum drying oven at 80 ℃, drying the carbon fiber/copper, putting the carbon fiber/copper into a high-temperature tube furnace with argon gas inlet flow of 80mL/min, heating the carbon fiber/copper to 750 ℃ at the heating rate of 5 ℃/min, and keeping the temperature for 60min, wherein the argon gas is introduced from the beginning of heating to the end of reaction and is cooled to room temperature;
and 4, putting the material processed in the step 3 into a mold for fixing, putting the mold into a vacuum hot-pressing furnace, heating to 600 ℃, pressurizing to 2MPa, keeping the pressure for 4 hours, and cooling along with the furnace to obtain the titanium-carbon fiber-titanium sandwich-type composite material.
The thickness of the titanium-carbon fiber-titanium sandwich composite material prepared by the embodiment is 0.60mm, and compared with a titanium-based matrix material with the same volume, the titanium-carbon fiber-titanium sandwich composite material has the advantages that the mass is reduced by 21.8%, the tensile strength is improved by 18.9%, and the resistivity is reduced by 6.07%.
While the present invention has been described in detail with reference to the embodiments shown in the drawings, the present invention is not limited to the embodiments, and various changes can be made without departing from the spirit and scope of the present invention.
Claims (10)
1. A titanium-carbon fiber-titanium sandwich composite material is characterized in that: the structure is that copper and titanium are arranged on two sides of the carbon fiber from inside to outside in sequence.
2. The preparation method of the titanium-carbon fiber-titanium sandwich composite material according to claim 1, which is characterized by comprising the following steps:
step 1, carrying out hot air oxidation, liquid phase oxidation, ultrasonic alkaline oil removal, sensitization and activation treatment on carbon fiber cloth;
step 2, placing the carbon fiber treated in the step 1 in a chemical plating tank at 60 ℃ and stirring for 1h for chemical copper plating, and then placing a sample in a drying oven at 80 ℃ for 15h to obtain carbon fiber/copper;
step 3, coating titanium hydride solution dissolved in absolute ethyl alcohol on two sides of the carbon fiber/copper obtained in the step 2, drying in a vacuum drying oven, and then heating in a high-temperature tube furnace with argon gas inlet flow of 80mL/min, wherein the argon gas is introduced from the beginning of heating to the end of reaction and is cooled to room temperature;
and 4, putting the material processed in the step 3 into a mold for fixing, putting the mold into a vacuum hot pressing furnace, and cooling the mold along with the furnace to obtain the titanium-carbon fiber-titanium sandwich-type composite material.
3. The method for preparing a titanium-carbon fiber-titanium "sandwich" type composite material according to claim 2, characterized in that: and (3) oxidizing the carbon fiber cloth in the step (1) for 30min in hot air at the temperature of 300-450 ℃.
4. The method for preparing a titanium-carbon fiber-titanium "sandwich" type composite material according to claim 2, characterized in that: in the step 1, liquid-phase oxidation is carried out for 30-80 min at the temperature of 80 ℃ in a mixed acid solution of concentrated nitric acid (analytically pure) and concentrated sulfuric acid (analytically pure) in a volume ratio of 1: 1-5: 1.
5. The method for preparing a titanium-carbon fiber-titanium "sandwich" type composite material according to claim 2, characterized in that: the ultrasonic alkaline oil removal in the step 1 is carried out in the presence of 60-100 g/L, Na NaOH2CO310-30 g/L of alkali liquor and 1-5 g/L of cleaning agent for 20-50 min.
6. The method for preparing a titanium-carbon fiber-titanium "sandwich" type composite material according to claim 2, characterized in that: the sensitization in step 1 is to SnCl2·2H2O20~30g/L、NaH2PO2·H2Sensitizing for 30-60 min in sensitizing solution of O5-10 g/L, 36-38 wt% HCl 15-25 ml/L and tin block 10-20 g/L.
7. The method for preparing a titanium-carbon fiber-titanium "sandwich" type composite material according to claim 2, characterized in that: the activation treatment in the step 1 is to activate the silver nitrate solution in a concentration of 25-35 g/L at 30-45 ℃ for 40-80 min.
8. The method for preparing a titanium-carbon fiber-titanium "sandwich" type composite material according to claim 2, characterized in that: in the step 2, the chemical plating bath solution in the chemical plating bath is 10-20 g/L of anhydrous copper sulfate, 30-50 g/L of sodium ethylene diamine tetracetate, 20-30 ml/L of 37wt% formaldehyde solution, 0.04-0.06 g/L of 2, 2-bipyridine and 8-12 g/L of sodium hydroxide.
9. The method for preparing a titanium-carbon fiber-titanium "sandwich" type composite material according to claim 2, characterized in that: in the step 3, the mass ratio of titanium hydride to absolute ethyl alcohol in the titanium hydride solution dissolved in absolute ethyl alcohol is 1: 1-1: 4, the heating rate is 5-10 ℃/min, the temperature is 750-950 ℃, and the heating and heat preservation time is 20-60 min.
10. The method for preparing a titanium-carbon fiber-titanium "sandwich" type composite material according to claim 2, characterized in that: and in the step 4, the temperature of the vacuum hot-pressing furnace is 600-750 ℃, the pressure is increased to 2-4.5 MPa, and the pressure is maintained for 2-4 h.
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