CN115386295A - Super-wear-resistant high-hardness nano titanium-ceramic coating and preparation method thereof - Google Patents
Super-wear-resistant high-hardness nano titanium-ceramic coating and preparation method thereof Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- 238000005524 ceramic coating Methods 0.000 title claims abstract description 16
- 229920005989 resin Polymers 0.000 claims abstract description 63
- 239000011347 resin Substances 0.000 claims abstract description 63
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 55
- 239000002041 carbon nanotube Substances 0.000 claims abstract description 55
- 229910021393 carbon nanotube Inorganic materials 0.000 claims abstract description 55
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 40
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 40
- 239000010703 silicon Substances 0.000 claims abstract description 40
- 238000010438 heat treatment Methods 0.000 claims abstract description 34
- 238000000576 coating method Methods 0.000 claims abstract description 30
- 239000003822 epoxy resin Substances 0.000 claims abstract description 29
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 29
- 239000011248 coating agent Substances 0.000 claims abstract description 27
- 239000000945 filler Substances 0.000 claims abstract description 27
- 239000011159 matrix material Substances 0.000 claims abstract description 22
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000010936 titanium Substances 0.000 claims abstract description 20
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 20
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims abstract description 15
- -1 cerium ions Chemical class 0.000 claims abstract description 14
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910052573 porcelain Inorganic materials 0.000 claims abstract description 11
- RMQJECWPWQIIPW-OWOJBTEDSA-N 4-hydroxy-crotonic acid Chemical compound OC\C=C\C(O)=O RMQJECWPWQIIPW-OWOJBTEDSA-N 0.000 claims abstract description 10
- DLYUQMMRRRQYAE-UHFFFAOYSA-N tetraphosphorus decaoxide Chemical compound O1P(O2)(=O)OP3(=O)OP1(=O)OP2(=O)O3 DLYUQMMRRRQYAE-UHFFFAOYSA-N 0.000 claims abstract description 10
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 36
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 31
- 238000003756 stirring Methods 0.000 claims description 26
- 239000008367 deionised water Substances 0.000 claims description 24
- 229910021641 deionized water Inorganic materials 0.000 claims description 24
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 21
- 238000009210 therapy by ultrasound Methods 0.000 claims description 19
- 229910052757 nitrogen Inorganic materials 0.000 claims description 18
- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical compound C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 claims description 16
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 15
- 229910052739 hydrogen Inorganic materials 0.000 claims description 15
- 239000001257 hydrogen Substances 0.000 claims description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 14
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 14
- 239000002131 composite material Substances 0.000 claims description 14
- 238000001035 drying Methods 0.000 claims description 14
- 238000000967 suction filtration Methods 0.000 claims description 14
- 238000002156 mixing Methods 0.000 claims description 13
- 238000005406 washing Methods 0.000 claims description 12
- 238000001816 cooling Methods 0.000 claims description 10
- KSCAZPYHLGGNPZ-UHFFFAOYSA-N 3-chloropropyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)CCCCl KSCAZPYHLGGNPZ-UHFFFAOYSA-N 0.000 claims description 9
- QQZMWMKOWKGPQY-UHFFFAOYSA-N cerium(3+);trinitrate;hexahydrate Chemical compound O.O.O.O.O.O.[Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O QQZMWMKOWKGPQY-UHFFFAOYSA-N 0.000 claims description 9
- VILCJCGEZXAXTO-UHFFFAOYSA-N 2,2,2-tetramine Chemical compound NCCNCCNCCN VILCJCGEZXAXTO-UHFFFAOYSA-N 0.000 claims description 8
- AHDSRXYHVZECER-UHFFFAOYSA-N 2,4,6-tris[(dimethylamino)methyl]phenol Chemical compound CN(C)CC1=CC(CN(C)C)=C(O)C(CN(C)C)=C1 AHDSRXYHVZECER-UHFFFAOYSA-N 0.000 claims description 8
- XMSXQFUHVRWGNA-UHFFFAOYSA-N Decamethylcyclopentasiloxane Chemical compound C[Si]1(C)O[Si](C)(C)O[Si](C)(C)O[Si](C)(C)O[Si](C)(C)O1 XMSXQFUHVRWGNA-UHFFFAOYSA-N 0.000 claims description 8
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 8
- UFCXHBIETZKGHB-UHFFFAOYSA-N dichloro(diethoxy)silane Chemical compound CCO[Si](Cl)(Cl)OCC UFCXHBIETZKGHB-UHFFFAOYSA-N 0.000 claims description 8
- 239000003085 diluting agent Substances 0.000 claims description 8
- 235000010299 hexamethylene tetramine Nutrition 0.000 claims description 8
- 239000004312 hexamethylene tetramine Substances 0.000 claims description 8
- 239000003973 paint Substances 0.000 claims description 8
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 8
- 235000011152 sodium sulphate Nutrition 0.000 claims description 8
- 229960001124 trientine Drugs 0.000 claims description 8
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 7
- 239000000919 ceramic Substances 0.000 claims description 7
- 229910017604 nitric acid Inorganic materials 0.000 claims description 7
- 229910021536 Zeolite Inorganic materials 0.000 claims description 5
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims description 5
- 239000002808 molecular sieve Substances 0.000 claims description 5
- NWVVVBRKAWDGAB-UHFFFAOYSA-N p-methoxyphenol Chemical compound COC1=CC=C(O)C=C1 NWVVVBRKAWDGAB-UHFFFAOYSA-N 0.000 claims description 5
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims description 5
- 239000010457 zeolite Substances 0.000 claims description 5
- KTLXGYDOJZVEFA-UHFFFAOYSA-N dimethyl(triethylsilyloxy)silicon Chemical compound CC[Si](CC)(CC)O[Si](C)C KTLXGYDOJZVEFA-UHFFFAOYSA-N 0.000 claims description 4
- 238000000034 method Methods 0.000 claims description 4
- 239000003921 oil Substances 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims description 3
- 229920002050 silicone resin Polymers 0.000 claims description 2
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 2
- 238000010306 acid treatment Methods 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 4
- 239000011165 3D composite Substances 0.000 abstract description 3
- 229910052684 Cerium Inorganic materials 0.000 abstract description 3
- 150000002500 ions Chemical class 0.000 abstract description 3
- 238000005121 nitriding Methods 0.000 abstract description 3
- 230000001376 precipitating effect Effects 0.000 abstract description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 abstract 2
- 238000009830 intercalation Methods 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 22
- 229910052751 metal Inorganic materials 0.000 description 8
- 239000002184 metal Substances 0.000 description 8
- 239000000243 solution Substances 0.000 description 8
- 239000000463 material Substances 0.000 description 6
- 229910052761 rare earth metal Inorganic materials 0.000 description 6
- 239000000203 mixture Substances 0.000 description 4
- 239000000758 substrate Substances 0.000 description 4
- 235000019441 ethanol Nutrition 0.000 description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 238000005299 abrasion Methods 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 2
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical compound [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 230000001050 lubricating effect Effects 0.000 description 2
- 239000012299 nitrogen atmosphere Substances 0.000 description 2
- 238000010899 nucleation Methods 0.000 description 2
- 230000006911 nucleation Effects 0.000 description 2
- 125000002467 phosphate group Chemical group [H]OP(=O)(O[H])O[*] 0.000 description 2
- 229910000077 silane Inorganic materials 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 229910052581 Si3N4 Inorganic materials 0.000 description 1
- 238000007259 addition reaction Methods 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000007142 ring opening reaction Methods 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D183/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers
- C09D183/10—Block or graft copolymers containing polysiloxane sequences
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
- C09D7/62—Additives non-macromolecular inorganic modified by treatment with other compounds
-
- 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
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
Abstract
The invention discloses an ultra-wear-resistant high-hardness nano titanium-ceramic coating and a preparation method thereof, and relates to the technical field of coatings. According to the invention, 4-hydroxycrotonic acid and phosphorus pentoxide are firstly utilized to modify epoxy resin, and then the epoxy resin reacts with an organic silicon resin matrix, so that the stripping resistance of the coating is improved; then, the organic silicon resin matrix is further modified by using n-propanol, so that the stripping resistance of the coating is improved, and the coating has better compatibility with a self-made coating; and then, adsorbing cerium ions by using the acidified carbon nano tubes, precipitating to form layered hydroxide, then, intercalating butyl titanate in the layered hydroxide, heating twice to form titanium porcelain, thus obtaining the self-made filler which is in a three-dimensional composite structure and can be overlapped and arranged in a resin matrix, improving the wear resistance of the coating, and then, effectively improving the wear resistance of the coating through ion nitriding treatment. The coating prepared by the invention has the effects of wear resistance and stripping resistance.
Description
Technical Field
The invention relates to the technical field of coatings, in particular to an ultra-wear-resistant high-hardness nano titanium-ceramic coating and a preparation method thereof.
Background
The metal base material such as aluminum alloy has the characteristics of unique mechanical property, portability, attractive appearance and the like, and is widely applied to the fields of space equipment, airports, subways, architectural decoration and the like. Generally, in order to improve the properties of materials such as hardness and wear resistance, before a metal substrate is used, a coating protection treatment is required, resin, titanium porcelain and other fillers are mixed to improve the hardness of the coating, and a coating paint film is easy to wear and depaint due to long-term use, while the titanium porcelain and the other fillers are easy to stack due to uneven dispersion, so that the surface of the coating is uneven, the embedding degree with a resin matrix is not high, and the abrasion condition of the coating is aggravated.
The silicon-oxygen bond of the organic silicon resin contains higher bond energy, so the organic silicon resin has higher thermal oxidation stability and heat resistance, is superior to common organic resin, but has poorer adhesive force to a base material, and can generate larger paint film falling condition after being used for one year or even half a year, thereby limiting the application of the organic silicon resin to a certain extent.
Disclosure of Invention
The invention aims to provide an ultra-wear-resistant high-hardness nano titanium-ceramic coating and a preparation method thereof, and aims to solve the problems in the prior art.
In order to solve the technical problems, the invention provides the following technical scheme: the super wear-resistant high-hardness nano titanium ceramic coating is prepared by the following method of stirring and mixing self-made organic silicon resin and self-made filler, adding the diluent 660A, heating in a water bath to a preset temperature, introducing hydrogen and nitrogen, continuously heating, keeping the temperature for a period of time in vacuum, and then adding triethylene tetramine and DMP-30.
Further, the self-made organic silicon resin is prepared from modified epoxy resin, 3-chloropropyltriethoxysilane, diethoxydichlorosilane, decamethylcyclopentasiloxane, 2,4,6,8,10-cyclopentasiloxane, tetramethyldihydro disiloxane, 1,1,1-triethyl-3,3-dimethyldisiloxane and n-propyl alcohol.
Further, the modified epoxy resin is prepared from 4-hydroxycrotonic acid, epoxy resin E-51 and phosphorus pentoxide.
Further, the self-made filler is prepared by a method comprising the following steps of treating the carbon nano tube with nitric acid to obtain a pretreated carbon nano tube; placing the pretreated carbon nano tube in deionized water, performing ultrasonic dispersion, adding cerium nitrate hexahydrate, sodium sulfate and hexamethylenetetramine, heating to a preset temperature in an oil bath under the protection of nitrogen, stirring for reaction, and performing suction filtration, washing and drying to obtain a composite carbon nano tube; then placing in butyl titanate, after ultrasonic treatment, reacting for a period of time at high temperature, heating and raising temperature, preserving heat for a period of time, and then cooling and preserving heat.
Further, the preparation method of the super-wear-resistant high-hardness nano titanium-ceramic coating comprises the following preparation steps:
(1) Heating a resin matrix to 89-95 ℃, adding modified epoxy resin, KP220 and ethyl acetate according to the mass ratio of 1.0007 to 1;
(2) Mixing the self-made organic silicon resin and the self-made filler according to the mass ratio of 1.0-1.5, stirring at 200-300 rpm for 3-7 h, adding a diluent 660A with the mass of 0.006-0.01 time of that of the self-made organic silicon resin, heating in a water bath to 46-59 ℃, introducing hydrogen and nitrogen, heating to 220-242 ℃, keeping the temperature for 7-12 h under the vacuum degree of 30-70 Pa, adding triethylene tetramine with the mass of 0.01-0.03 time of that of the self-made organic silicon resin and DMP-30 with the mass of 0.002-0.005 time of that of the self-made organic silicon resin, and uniformly stirring to obtain the super-wear-resistant high-hardness nano titanium ceramic coating.
Further, the preparation method of the modified epoxy resin in the step (1) comprises the following steps: reacting epoxy resin E-51, 4-hydroxycrotonic acid, N-diethylbenzylamine, p-hydroxyanisole and absolute ethyl alcohol at the temperature of between 86 and 96 ℃ according to the mass ratio of 1.
Further, the preparation method of the resin matrix in the step (1) comprises the following steps: mixing 3-chloropropyltriethoxysilane, diethoxydichlorosilane, decamethylcyclopentasiloxane, 2,4,6,8,10-cyclopentasiloxane, toluene and a zeolite molecular sieve according to a mass ratio of 1.3.
Further, the preparation method of the self-made filler in the step (2) comprises the following steps:
A. placing the pretreated carbon nanotube in deionized water with the mass of 180-250 times of that of the pretreated carbon nanotube, carrying out ultrasonic treatment at 25-35 kHz for 10-26 min, adding cerium nitrate hexahydrate, sodium sulfate and hexamethylenetetramine according to the mass ratio of 1;
B. placing the composite carbon nano tube in butyl titanate with the mass 5-8 times of that of the composite carbon nano tube, carrying out ultrasonic treatment for 4-7 h at 25-35 kHz, reacting for 18-22 h at 200-220 ℃, heating to 600-630 ℃, keeping the temperature for 5-8 h, cooling to 322-367 ℃, keeping the temperature for 6-9 h, carrying out suction filtration, washing for 6-8 times by deionized water, and drying for 3-5 h at 60-70 ℃, thus obtaining the filler.
Further, the preparation method of the pretreated carbon nanotube in the step A comprises the following steps: putting the carbon nano tube into nitric acid with mass fraction of 68 percent and mass time of 25-36 times of the mass of the carbon nano tube, carrying out ultrasonic treatment at 25-35 kHz for 24-36 min, stirring at 60-80 rpm for 3-7 h, adding deionized water until the pH value of the solution is 6-7, carrying out suction filtration, and drying at 68-80 ℃ for 6-11 h.
Further, the flow ratio of the hydrogen to the nitrogen in the step (2) is 3:1, and the total flow of the hydrogen and the nitrogen is 150mm 3 /s。
Compared with the prior art, the invention has the following beneficial effects:
the coating is obtained by utilizing the self-made organic silicon resin and the self-made filler, and can be used on the surface of a metal base material to realize the effects of stripping resistance and super wear resistance.
Firstly, 4-hydroxycrotonic acid is utilized to carry out ring-opening reaction on epoxy resin, and hydroxyl of the epoxy resin reacts with phosphorus pentoxide to form phosphate ester group, so as to obtain modified epoxy resin; then 3-chloropropyltriethoxysilane and diethoxydichlorosilane are used as reaction monomers together with decamethylcyclopentasiloxane and 2,4,6,8,10-cyclopentasiloxane, and then tetramethyldihydro-disiloxane and 1,1,1-triethyl-3,3-dimethyldisiloxane are used as end-capping to obtain a resin matrix; then, the silicon-hydrogen bond of the resin matrix reacts with the double bond of the modified epoxy resin to perform addition reaction, the high viscosity of the epoxy resin can improve the stripping resistance of the coating, and the phosphorus hydroxyl of the phosphate group can form stronger chelating action with the surface of the metal substrate and is connected in a covalent bond mode, so that the stripping resistance of the coating is improved; then the hydroxyl of the n-propanol reacts with chloride ions, and the obtained product is grafted in a molecular chain of the self-made organic silicon resin, and can be bridged with the surface of a metal base material by virtue of a silane bond, so that the stripping resistance of the coating is improved.
Secondly, firstly acidifying the carbon nano tube to enable the surface to have carboxyl, opening the end cap, then adsorbing cerium ions by the carboxyl, precipitating as nucleation points, continuously growing to form layered rare earth hydroxide, then inserting butyl titanate into the layered rare earth hydroxide, carrying out first heating, carrying out crystallization molding to form titanium dioxide, then carrying out second heating to form titanium porcelain, wherein the carbon nano tube, the layered rare earth hydroxide and the titanium porcelain are mutually embedded to form a three-dimensional composite structure, are tightly stacked and can be overlapped and arranged in a resin matrix, so that micro bubbles, cracks and molecular cavities in the resin are mutually divided, a compact coating structure is formed, the carbon nano tube, the layered rare earth hydroxide and the titanium porcelain play a role of a wear-resistant framework, the wear resistance of the coating is improved, and the self-made organic silicon resin and the self-made filler are connected by silicon-oxygen bonds, so that the degree of compactness is improved, and the wear resistance of the coating is improved; and then the self-made organic silicon resin and the self-made filler are mixed, and then the ion nitriding treatment is carried out, so that a lubricating layer is formed on the surface of the self-made filler while grains are refined, and the wear resistance of the coating is effectively improved.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, belong to the protection scope of the present invention.
In order to more clearly illustrate the method provided by the invention, the following examples are used for detailed description, and the index test method of the super wear-resistant high-hardness nano titanium ceramic coating prepared in the following examples is as follows:
coating the surface of the metal substrate to the same thickness in the embodiment and the comparative example, and carrying out super wear resistance and anti-stripping effect tests;
super wear resistance: using an HT-1000 type friction wear testing machine, wherein the normal load is 20N, the friction time is 120min, the rotating speed is 400r/min, the friction radius is 4mm, a silicon nitride ceramic ball with the diameter of 5mm is used as a grinding ball, samples before and after abrasion are cleaned by ultrasonic alcohol, dried and weighed for 3 times, and the average value is taken to calculate the wear loss;
peel resistance: the adhesion rating was tested with reference to GB/T13448.
Example 1
(1) Reacting epoxy resin E-51, 4-hydroxycrotonic acid, N-diethylbenzylamine, p-hydroxyanisole and absolute ethyl alcohol at 86 ℃ for 40min according to a mass ratio of 1;
(2) Mixing 3-chloropropyltriethoxysilane, diethoxydichlorosilane, decamethylcyclopentasiloxane, 2,4,6,8,10-cyclopentasiloxane, toluene and a zeolite molecular sieve according to a mass ratio of 1:0.3:0.4:0.5:13, stirring uniformly, placing in a 67 ℃ oil bath pan, adding an ethanol aqueous solution 4 times the mass of 3-chloropropyltriethoxysilane, wherein the mass ratio of anhydrous ethanol to deionized water in the ethanol aqueous solution is 1:1, reacting for 2h, adding tetramethyldihydrogen disiloxane, 1,1,1-triethyl-3,3-dimethyldisiloxane according to a mass ratio of 1:0.6, reacting for 1.5h, filtering, layering, distilling for 4h at 143 ℃, 400mmHg, and baking for 20min at 190 ℃ to obtain a resin matrix;
(3) Heating a resin matrix to 89 ℃, adding modified epoxy resin, KP220 and ethyl acetate according to a mass ratio of 1.0007 to 1, stirring at 150rpm for 1h, reacting for 9h under a nitrogen atmosphere, cooling to 20 ℃, adding n-propanol which is 0.9 times of the mass of the resin matrix, reacting for 5h, washing with deionized water until the pH of the solution is 6, and distilling at 300rpm and 77 ℃ for 3h to obtain the self-made organic silicon resin;
(4) Putting the carbon nano tube into nitric acid with mass fraction of 68% and mass which is 25 times of the mass of the carbon nano tube, carrying out ultrasonic treatment at 25kHz for 24min, stirring at 60rpm for 3h, adding deionized water until the pH of the solution is 6, carrying out suction filtration, and drying at 68 ℃ for 6h to obtain a pretreated carbon nano tube;
(5) Placing the pretreated carbon nanotube in deionized water 180 times of the mass of the pretreated carbon nanotube, performing ultrasonic treatment at 25kHz for 10min, adding cerium nitrate hexahydrate, sodium sulfate and hexamethylenetetramine according to the mass ratio of 1 to 0.08;
(6) Placing the composite carbon nanotube in butyl titanate with the mass 5 times of that of the composite carbon nanotube, carrying out ultrasonic treatment for 4 hours at 25kHz, reacting for 18 hours at 200 ℃, heating to 600 ℃, keeping the temperature for 5 hours, cooling to 322 ℃, keeping the temperature for 6 hours, carrying out suction filtration, washing for 6 times by using deionized water, and drying for 3 hours at 60 ℃, thus obtaining the filler;
(7) Mixing the self-made organic silicon resin and the self-made filler according to the mass ratio of l:1, stirring at 200rpm for 3h, adding a diluent 660A with the mass being 0.006 time of that of the self-made organic silicon resin, heating in a water bath to 46 ℃, introducing hydrogen and nitrogen according to the flow ratio of 3:1, wherein the total flow of the hydrogen and the nitrogen is 150mm 3 And/s, heating to 220 ℃, keeping the temperature for 7h under the vacuum degree of 300Pa, adding triethylene tetramine with the mass of 0.01 time of that of the self-made organic silicon resin and DMP-30 with the mass of 0.002 time of that of the self-made organic silicon resin, and uniformly stirring to obtain the super-wear-resistant high-hardness nano titanium ceramic coating.
Example 2
(1) Reacting epoxy resin E-51, 4-hydroxycrotonic acid, N-diethylbenzylamine, p-hydroxyanisole and absolute ethyl alcohol at the mass ratio of 1.1;
(2) Mixing 3-chloropropyltriethoxysilane, diethoxydichlorosilane, decamethylcyclopentasiloxane, 2,4,6,8,10-cyclopentasiloxane, toluene and a zeolite molecular sieve according to a mass ratio of 1.55;
(3) Heating a resin matrix to 92 ℃, adding modified epoxy resin, KP220 and ethyl acetate according to a mass ratio of 1.0009 to 11.5, stirring at 175rpm for 2h, reacting for 13.5h under a nitrogen atmosphere, cooling to 25 ℃, adding n-propanol which is 1.4 times of the mass of the resin matrix, reacting for 7.5h, washing with deionized water until the pH of the solution is 6.5, and distilling at 350rpm and 81 ℃ for 4.5h to obtain the self-made organic silicon resin;
(4) Putting the carbon nano tube into nitric acid with mass fraction of 68% and mass of 30.5 times of the mass of the carbon nano tube, performing ultrasonic treatment at 30kHz for 30min, stirring at 70rpm for 5h, adding deionized water until the pH of the solution is 6.5, performing suction filtration, and drying at 74 ℃ for 8.5h to obtain a pretreated carbon nano tube;
(5) Placing the pretreated carbon nanotube in deionized water 215 times the mass of the pretreated carbon nanotube, performing ultrasonic treatment at 30kHz for 18min, adding cerium nitrate hexahydrate, sodium sulfate and hexamethylenetetramine according to the mass ratio of 1 to 0.15, heating the mixture to 101 ℃ in an oil bath under the protection of nitrogen, stirring the mixture at 115rpm for 19h, performing suction filtration, washing the mixture with deionized water and absolute ethyl alcohol in sequence for 5min, and drying the mixture at 65 ℃ for 10h to obtain the composite carbon nanotube, wherein the mass ratio of the cerium nitrate hexahydrate to the pretreated carbon nanotube is 0.8;
(6) Placing the composite carbon nanotube in butyl titanate with the mass 6.5 times of that of the composite carbon nanotube, carrying out ultrasonic treatment at 30kHz for 5.5h, reacting at 210 ℃ for 20h, heating to 615 ℃, keeping the temperature for 6.5h, cooling to 344 ℃, keeping the temperature for 7.5h, carrying out suction filtration, washing with deionized water for 7 times, drying at 65 ℃ for 4h, and obtaining a filler;
(7) Mixing the self-made organic silicon resin and the self-made filler according to the mass ratio of l:1.2, stirring at 250rpm for 5 hours, adding a diluent 660A with the mass 0.008 time of that of the self-made organic silicon resin, heating in a water bath to 52 ℃, introducing hydrogen and nitrogen according to the flow ratio of 3:1, wherein the total flow of the hydrogen and the nitrogen is 150mm 3 And/s, heating to 231 ℃, keeping the temperature for 9.5 hours under the vacuum degree of 50Pa, adding triethylene tetramine accounting for 0.02 time of the mass of the self-made organic silicon resin and DMP-30 accounting for 0.0035 time of the mass of the self-made organic silicon resin, and uniformly stirring to obtain the super-wear-resistant high-hardness nano titanium ceramic coating.
Example 3
(1) Reacting epoxy resin E-51, 4-hydroxycrotonic acid, N-diethylbenzylamine, p-hydroxyanisole and absolute ethyl alcohol at the mass ratio of 1.4;
(2) Mixing 3-chloropropyltriethoxysilane, diethoxydichlorosilane, decamethylcyclopentasiloxane, 2,4,6,8,10-cyclopentasiloxane, toluene and a zeolite molecular sieve according to a mass ratio of 1.8;
(3) Heating a resin matrix to 95 ℃, adding modified epoxy resin, KP220 and ethyl acetate according to a mass ratio of 1.001;
(4) Putting the carbon nano tube in nitric acid with the mass fraction of 68% and the mass of 36 times of that of the carbon nano tube, carrying out 35kHz ultrasonic treatment for 36min, then stirring at 80rpm for 7h, then adding deionized water until the pH of the solution is 7, carrying out suction filtration, and drying at 80 ℃ for 11h to obtain a pretreated carbon nano tube;
(5) Placing the pretreated carbon nanotube in deionized water with the mass 250 times that of the pretreated carbon nanotube, carrying out ultrasonic treatment at 35kHz for 26min, adding cerium nitrate hexahydrate, sodium sulfate and hexamethylenetetramine according to the mass ratio of 1 to 0.2;
(6) Placing the composite carbon nanotube in butyl titanate with the mass 8 times of that of the composite carbon nanotube, carrying out ultrasonic treatment for 7 hours at 35kHz, reacting for 22 hours at 220 ℃, heating to 630 ℃, keeping the temperature for 8 hours, cooling to 367 ℃, carrying out suction filtration after keeping the temperature for 9 hours, washing for 8 times by using deionized water, and drying for 5 hours at 70 ℃ to obtain a filler;
(7) Mixing the self-made organic silicon resin and the self-made filler according to the mass ratio of 1.5, stirring at 300rpm for 7 hours, adding a diluent 660A with the mass 0.01 time that of the self-made organic silicon resin, heating in a water bath to 59 ℃, introducing hydrogen and nitrogen according to the flow ratio of 3:1, wherein the total flow of the hydrogen and the nitrogen is 150mm 3 And/s, heating to 242 ℃, keeping the temperature for 12h under the vacuum degree of 70Pa, adding triethylene tetramine with the mass of 0.03 time of that of the self-made organic silicon resin and DMP-30 with the mass of 0.005 time of that of the self-made organic silicon resin, and uniformly stirring to obtain the super-wear-resistant high-hardness nano titanium ceramic coating.
Comparative example 1
Comparative example 1 differs from example 2 in that there is no step (1) and step (3) is changed to: and (2) placing the resin matrix in a container at 25 ℃, adding n-propanol of which the mass is 1.4 times that of the resin matrix, reacting for 7.5h, washing with deionized water until the pH of the solution is 6.5, and distilling at 350rpm and 81 ℃ for 4.5h to obtain the self-made organic silicon resin. The rest of the preparation steps are the same as example 2.
Comparative example 2
Comparative example 2 differs from example 2 in that step (2) is not present and step (3) is changed to: heating polymethyl silicone resin to 92 ℃, adding modified epoxy resin, KP220 and ethyl acetate according to a mass ratio of 1.0009. The rest of the preparation steps are the same as example 2.
Comparative example 3
The difference between the comparative example 3 and the example 2 is that the step (3) is different, and the step (3) is changed into: heating the resin matrix to 92 ℃, adding the modified epoxy resin, KP220 and ethyl acetate according to the mass ratio of 1.0009 to 11.5, stirring at 175rpm for 2h under the atmosphere of nitrogen, reacting for 13.5h, and distilling at 350rpm and 81 ℃ for 4.5h to obtain the self-made organic silicon resin. The rest of the preparation steps are the same as example 2.
Comparative example 4
Comparative example 4 differs from example 2 in that step (5) is not present, and step (6) is changed to: placing the pretreated carbon nano tube in butyl titanate with the mass 6.5 times of that of the composite carbon nano tube, carrying out ultrasonic treatment at 30kHz for 5.5h, reacting at 210 ℃ for 20h, heating to 615 ℃, keeping the temperature for 6.5h, cooling to 344 ℃, keeping the temperature for 7.5h, carrying out suction filtration, washing with deionized water for 7 times, and drying at 65 ℃ for 4h to obtain the filler. The rest of the preparation steps are the same as example 2.
Comparative example 5
Comparative example 5 differs from example 2 in that step (6) is not present and step (5) is changed to: placing the pretreated carbon nanotube in deionized water 215 times the mass of the pretreated carbon nanotube, carrying out ultrasonic treatment at 30kHz for 18min, adding cerium nitrate hexahydrate, sodium sulfate and hexamethylenetetramine according to the mass ratio of 1: 0.14. The rest of the preparation steps are the same as example 2.
Comparative example 6
Comparative example 6 differs from example 2 in that step (7) is different, step (7) being changed to: mixing the self-made organic silicon resin and the self-made filler according to the mass ratio l:1.2, stirring at 250rpm for 5 hours, adding a diluent 660A with the mass being 0.008 time of that of the self-made organic silicon resin, triethylene tetramine with the mass being 0.02 time of that of the self-made organic silicon resin and DMP-30 with the mass being 0.0035 time of that of the self-made organic silicon resin, and stirring uniformly to obtain the super-wear-resistant high-hardness nano titanium ceramic coating. The rest of the preparation steps are the same as example 2.
Effects of the invention
The following table 1 shows the results of performance analysis of the ultra-wear-resistant high-hardness nano titanium porcelain coatings using examples 1 to 3 of the present invention and comparative examples 1 to 6.
TABLE 1
| Amount of wear (g) | Grade of adhesion | |
| Example 1 | 0.011 | Level 1 |
| Example 2 | 0.010 | Level 1 |
| Example 3 | 0.012 | Level 1 |
| Comparative example 1 | 0.015 | 4 stage |
| Comparative example 2 | 0.012 | Grade 3 |
| Comparative example 3 | 0.11 | Grade 3 |
| Comparative example 4 | 1.15 | Level 1 |
| Comparative example 5 | 0.99 | Level 1 |
| Comparative example 6 | 0.25 | Level 1 |
The comparison of the wear loss experimental data of the embodiment and the comparative example shows that the acidified carbon nano tube can adsorb cerium ions, precipitate as nucleation points, grow to form layered rare earth hydroxide, then intercalate butyl titanate, heat twice to form titanium porcelain, the carbon nano tube, the layered rare earth hydroxide and the titanium porcelain are mutually embedded to form a three-dimensional composite structure, are tightly stacked to play a role of a wear-resistant framework, are connected with self-made filler through silicon-oxygen bonds to improve the compactness, and form a lubricating layer on the surface of the self-made filler while refining grains through ion nitriding treatment, so that the wear resistance of the coating is effectively improved; compared with the adhesion force grade experimental data of the comparative example, the invention discovers that the epoxy resin is modified by utilizing 4-hydroxycrotonic acid and phosphorus pentoxide and then reacts with the resin matrix, the high viscosity of the epoxy resin can improve the stripping resistance of the coating, and the phosphate group can form stronger chelating action with the surface of the metal base material, thereby improving the stripping resistance of the coating; then the resin matrix is further modified by normal propyl alcohol, and can be bridged with the surface of a metal substrate by virtue of a silane bond, so that the stripping resistance of the coating is improved.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Claims (10)
1. The super-wear-resistant high-hardness nano titanium ceramic coating is characterized by being prepared by the following method, stirring and mixing the self-made organic silicon resin and the self-made filler, adding the diluent 660A, heating in a water bath to a preset temperature, introducing hydrogen and nitrogen, continuing to heat, keeping the temperature for a period of time in vacuum, and adding the triethylene tetramine and the DMP-30.
2. The super-wear-resistant high-hardness nano titanium porcelain coating as claimed in claim 1, wherein the self-made silicone resin is prepared from modified epoxy resin, 3-chloropropyltriethoxysilane, diethoxydichlorosilane, decamethylcyclopentasiloxane, 2,4,6,8,10-cyclopentasiloxane, tetramethyldihydro-disiloxane, 1,1,1-triethyl-3,3-dimethyldisiloxane and n-propanol.
3. The nano titanium porcelain coating with ultra wear resistance and high hardness as claimed in claim 2, wherein the modified epoxy resin is prepared from 4-hydroxycrotonic acid, epoxy resin E-51 and phosphorus pentoxide.
4. The super wear-resistant high-hardness nano titanium-ceramic paint as claimed in claim 1, wherein the self-made filler is prepared by subjecting carbon nanotubes to nitric acid treatment to obtain pretreated carbon nanotubes; placing the pretreated carbon nano tube in deionized water, carrying out ultrasonic dispersion, adding cerium nitrate hexahydrate, sodium sulfate and hexamethylenetetramine, heating to a preset temperature in an oil bath under the protection of nitrogen, stirring for reaction, and then carrying out suction filtration, washing and drying to obtain a composite carbon nano tube; then placing in butyl titanate, after ultrasonic treatment, reacting for a period of time at high temperature, heating and raising temperature, preserving heat for a period of time, and then cooling and preserving heat.
5. The preparation method of the super-wear-resistant high-hardness nano titanium-ceramic coating is characterized by comprising the following preparation steps of:
(1) Heating a resin matrix to 89-95 ℃, adding modified epoxy resin, KP220 and ethyl acetate according to the mass ratio of 1.0007 to 1;
(2) Mixing the self-made organic silicon resin and the self-made filler according to a mass ratio of l: 1.0-1.5, stirring for 3-7 h at 200-300 rpm, adding a diluent 660A with the mass of 0.006-0.01 times of that of the self-made organic silicon resin, heating in a water bath to 46-59 ℃, introducing hydrogen and nitrogen, heating to 220-242 ℃, keeping the temperature for 7-12 h at the vacuum degree of 30-70 Pa, adding triethylene tetramine with the mass of 0.01-0.03 times of that of the self-made organic silicon resin and DMP-30 with the mass of 0.002-0.005 times of that of the self-made organic silicon resin, and uniformly stirring to obtain the super-wear-resistant high-hardness nano titanium ceramic coating.
6. The preparation method of the super wear-resistant high-hardness nano titanium-ceramic paint according to claim 5, wherein the preparation method of the modified epoxy resin in the step (1) is as follows: reacting epoxy resin E-51, 4-hydroxycrotonic acid, N-diethylbenzylamine, p-hydroxyanisole and absolute ethyl alcohol at the temperature of between 86 and 96 ℃ according to the mass ratio of 1.
7. The preparation method of the ultra-wear-resistant high-hardness nano titanium-ceramic paint as claimed in claim 5, wherein the preparation method of the resin matrix in the step (1) is as follows: mixing 3-chloropropyltriethoxysilane, diethoxydichlorosilane, decamethylcyclopentasiloxane, 2,4,6,8,10-cyclopentasiloxane, toluene and a zeolite molecular sieve according to a mass ratio of 1.3.
8. The preparation method of the super wear-resistant high-hardness nano titanium-ceramic paint according to claim 5, wherein the preparation method of the self-made filler in the step (2) is as follows:
A. placing the pretreated carbon nanotube in deionized water with the mass of 180-250 times of that of the pretreated carbon nanotube, carrying out ultrasonic treatment at 25-35 kHz for 10-26 min, adding cerium nitrate hexahydrate, sodium sulfate and hexamethylenetetramine according to the mass ratio of 1;
B. placing the composite carbon nano tube in butyl titanate with the mass 5-8 times of that of the composite carbon nano tube, carrying out ultrasonic treatment at 25-35 kHz for 4-7 h, reacting at 200-220 ℃ for 18-22 h, heating to 600-630 ℃, keeping the temperature for 5-8 h, cooling to 322-367 ℃, keeping the temperature for 6-9 h, carrying out suction filtration, washing with deionized water for 6-8 times, and drying at 60-70 ℃ for 3-5 h to obtain the filler.
9. The preparation method of the ultra-wear-resistant high-hardness nano titanium-ceramic paint as claimed in claim 8, wherein the preparation method of the pretreated carbon nanotubes in the step A is as follows: putting the carbon nano tube into nitric acid with mass fraction of 68% and mass of 25-36 times of the mass of the carbon nano tube, carrying out ultrasonic treatment at 25-35 kHz for 24-36 min, then stirring at 60-80 rpm for 3-7 h, adding deionized water until the pH of the solution is 6-7, carrying out suction filtration, and drying at 68-80 ℃ for 6-11 h.
10. The preparation method of the ultra-wear-resistant high-hardness nano titanium-ceramic paint as claimed in claim 5, wherein the flow ratio of the hydrogen to the nitrogen in the step (2) is 3:1, and the total flow of the hydrogen and the nitrogen is 150mm 3 /s。
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