CN116288179A - TiSiBAgYN coating resistant to high-temperature lubrication - Google Patents
TiSiBAgYN coating resistant to high-temperature lubrication Download PDFInfo
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- CN116288179A CN116288179A CN202310523830.1A CN202310523830A CN116288179A CN 116288179 A CN116288179 A CN 116288179A CN 202310523830 A CN202310523830 A CN 202310523830A CN 116288179 A CN116288179 A CN 116288179A
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- coating
- tisibagyn
- resistant
- temperature lubrication
- lubrication
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- 238000000576 coating method Methods 0.000 title claims abstract description 140
- 239000011248 coating agent Substances 0.000 title claims abstract description 128
- 238000005461 lubrication Methods 0.000 title claims abstract description 72
- 239000000758 substrate Substances 0.000 claims abstract description 17
- 238000007733 ion plating Methods 0.000 claims abstract description 6
- 238000000034 method Methods 0.000 claims description 15
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- 150000004767 nitrides Chemical class 0.000 claims description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims description 7
- 238000005516 engineering process Methods 0.000 claims description 4
- 229910052751 metal Inorganic materials 0.000 claims description 4
- 239000002184 metal Substances 0.000 claims description 4
- 238000005240 physical vapour deposition Methods 0.000 claims description 4
- 238000000151 deposition Methods 0.000 claims description 3
- 230000008021 deposition Effects 0.000 claims description 3
- 239000000919 ceramic Substances 0.000 claims description 2
- 238000005520 cutting process Methods 0.000 claims 1
- 238000003754 machining Methods 0.000 claims 1
- 229940057995 liquid paraffin Drugs 0.000 abstract description 42
- 238000005498 polishing Methods 0.000 abstract description 23
- 239000000956 alloy Substances 0.000 abstract description 17
- 229910045601 alloy Inorganic materials 0.000 abstract description 17
- 239000002253 acid Substances 0.000 abstract description 15
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical class O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 36
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 27
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 24
- 239000008367 deionised water Substances 0.000 description 24
- 229910021641 deionized water Inorganic materials 0.000 description 24
- 238000012360 testing method Methods 0.000 description 23
- 238000002360 preparation method Methods 0.000 description 21
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 20
- 239000007822 coupling agent Substances 0.000 description 20
- 229910019142 PO4 Inorganic materials 0.000 description 19
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 19
- 239000010452 phosphate Substances 0.000 description 19
- 238000007789 sealing Methods 0.000 description 18
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 15
- YQOPHINZLPWDTA-UHFFFAOYSA-H [Al+3].[Cr+3].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O Chemical compound [Al+3].[Cr+3].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O YQOPHINZLPWDTA-UHFFFAOYSA-H 0.000 description 15
- 238000003756 stirring Methods 0.000 description 12
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 10
- 238000002156 mixing Methods 0.000 description 10
- 239000012188 paraffin wax Substances 0.000 description 10
- CYEJMVLDXAUOPN-UHFFFAOYSA-N 2-dodecylphenol Chemical compound CCCCCCCCCCCCC1=CC=CC=C1O CYEJMVLDXAUOPN-UHFFFAOYSA-N 0.000 description 8
- 239000011230 binding agent Substances 0.000 description 8
- 238000006243 chemical reaction Methods 0.000 description 8
- 239000000314 lubricant Substances 0.000 description 8
- 229940051841 polyoxyethylene ether Drugs 0.000 description 8
- 229920000056 polyoxyethylene ether Polymers 0.000 description 8
- 239000001278 2-(5-ethenyl-5-methyloxolan-2-yl)propan-2-ol Substances 0.000 description 7
- BRHDDEIRQPDPMG-UHFFFAOYSA-N Linalyl oxide Chemical compound CC(C)(O)C1CCC(C)(C=C)O1 BRHDDEIRQPDPMG-UHFFFAOYSA-N 0.000 description 7
- 239000002694 phosphate binding agent Substances 0.000 description 7
- 238000005507 spraying Methods 0.000 description 7
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 6
- 239000006185 dispersion Substances 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 6
- XTUSEBKMEQERQV-UHFFFAOYSA-N propan-2-ol;hydrate Chemical compound O.CC(C)O XTUSEBKMEQERQV-UHFFFAOYSA-N 0.000 description 6
- 229910052581 Si3N4 Inorganic materials 0.000 description 5
- 239000005350 fused silica glass Substances 0.000 description 5
- 239000000377 silicon dioxide Substances 0.000 description 5
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 5
- QQQSFSZALRVCSZ-UHFFFAOYSA-N triethoxysilane Chemical compound CCO[SiH](OCC)OCC QQQSFSZALRVCSZ-UHFFFAOYSA-N 0.000 description 5
- MUHFRORXWCGZGE-KTKRTIGZSA-N 2-hydroxyethyl (z)-octadec-9-enoate Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OCCO MUHFRORXWCGZGE-KTKRTIGZSA-N 0.000 description 4
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 4
- PVNIIMVLHYAWGP-UHFFFAOYSA-N Niacin Chemical compound OC(=O)C1=CC=CN=C1 PVNIIMVLHYAWGP-UHFFFAOYSA-N 0.000 description 4
- 229930040373 Paraformaldehyde Natural products 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 4
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 4
- 229940117975 chromium trioxide Drugs 0.000 description 4
- WGLPBDUCMAPZCE-UHFFFAOYSA-N chromium trioxide Inorganic materials O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 description 4
- GAMDZJFZMJECOS-UHFFFAOYSA-N chromium(6+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Cr+6] GAMDZJFZMJECOS-UHFFFAOYSA-N 0.000 description 4
- 229940095098 glycol oleate Drugs 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 239000011159 matrix material Substances 0.000 description 4
- 229920002866 paraformaldehyde Polymers 0.000 description 4
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 description 4
- 235000012239 silicon dioxide Nutrition 0.000 description 4
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- 108010009736 Protein Hydrolysates Proteins 0.000 description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 3
- 239000000413 hydrolysate Substances 0.000 description 3
- 238000002329 infrared spectrum Methods 0.000 description 3
- 230000001050 lubricating effect Effects 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- 238000004566 IR spectroscopy Methods 0.000 description 2
- 238000005299 abrasion Methods 0.000 description 2
- 238000010533 azeotropic distillation Methods 0.000 description 2
- 238000000498 ball milling Methods 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000006482 condensation reaction Methods 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000005755 formation reaction Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000003607 modifier Substances 0.000 description 2
- 229960003512 nicotinic acid Drugs 0.000 description 2
- 235000001968 nicotinic acid Nutrition 0.000 description 2
- 239000011664 nicotinic acid Substances 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 2
- 230000001376 precipitating effect Effects 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 230000002195 synergetic effect Effects 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910018540 Si C Inorganic materials 0.000 description 1
- 229910008482 TiSiN Inorganic materials 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 238000006459 hydrosilylation reaction Methods 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- QRXWMOHMRWLFEY-UHFFFAOYSA-N isoniazide Chemical compound NNC(=O)C1=CC=NC=C1 QRXWMOHMRWLFEY-UHFFFAOYSA-N 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 125000000325 methylidene group Chemical group [H]C([H])=* 0.000 description 1
- 239000007777 multifunctional material Substances 0.000 description 1
- 125000004433 nitrogen atom Chemical group N* 0.000 description 1
- 229940049964 oleate Drugs 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Images
Classifications
-
- 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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/24—Vacuum evaporation
- C23C14/32—Vacuum evaporation by explosion; by evaporation and subsequent ionisation of the vapours, e.g. ion-plating
- C23C14/325—Electric arc evaporation
-
- 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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/0641—Nitrides
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The invention discloses a TiSiBAgYN coating resistant to high-temperature lubrication, and relates to the technical field of surface coatings. The TiSiBAgYN coating adopts a TiSiBAgY alloy target to carry out arc ion plating on a substrate, and the prepared high-temperature lubrication resistant TiSiBAgYN coating has good wear resistance and lower residual stress, and has good bonding force with the substrate; the invention also adopts 2-allylmercaptonicotinic acid modified liquid paraffin, and then the modified liquid paraffin is used for polishing post-treatment of TiSiBAgYN coating; the TiSiBAgYN coating with high-temperature lubrication resistance has better wear resistance.
Description
Technical Field
The invention belongs to the technical field of surface coatings, and particularly relates to a TiSiBAgYN coating resistant to high-temperature lubrication.
Background
Along with the development of the modern cutter processing technology, the requirements of high-speed processing and dry processing on cutters and cutter coatings are higher and higher, and the requirements are mainly expressed by high processing temperature, especially the processing of hard processing, high-temperature alloy and other difficult-to-process materials, so that the processing temperature can reach about 1000 ℃, and the traditional AlTiN, alCrN and other coatings cannot be well qualified for the working condition. In recent years, si element is introduced into the coating to form Si 3 N 4 The amorphous structure wraps other coating grains, so that the grains are refined, and the residual stress of the coating is improved. Meanwhile, si element can form a compact oxide film at high temperature, so that the high-temperature oxidation resistance of the coating is greatly improved, but the friction coefficient of the coating containing Si is high and reaches about 0.7, and in the use process, the friction temperature is increased and the abrasion loss is increased due to the excessively high friction coefficient. How to effectively reduce the friction coefficient of the coating becomes an urgent problem to be solved.
Disclosure of Invention
The invention aims to provide a high-temperature-lubrication-resistant TiSiBAgYN coating, which has good wear resistance and lower residual stress, and has good binding force with a substrate.
The technical scheme adopted by the invention for achieving the purpose is as follows:
a TiSiBAgYN coating resistant to high temperature lubrication, said TiSiBAgYN coating comprising a nitride layer; the nitride layer comprises Ti, si, B, ag, Y and the TiSiBAgYN coating is deposited on the substrate; the substrate comprises one of metal, cemented carbide or ceramic; the friction coefficient of the TiSiBAgYN coating is less than 0.3.
According to the embodiment of the invention, the residual stress of the high-temperature-resistant lubricating TiSiBAgYN coating is 300-360MPa.
According to the embodiment of the invention, the thickness of the TiSiBAgYN coating resistant to high temperature lubrication is 2-6 mu m.
According to an embodiment of the present invention, the nitrogen content in the above nitride layer is 45 to 55at.%.
The invention also discloses a preparation method of the TiSiBAgYN coating resistant to high-temperature lubrication, which comprises the following steps: nitrogen is introduced, and a nitride coating is deposited on the substrate by utilizing a physical vapor deposition technology, so that the TiSiBAgYN coating resistant to high-temperature lubrication is prepared.
According to an embodiment of the present invention, the physical vapor deposition technique includes arc ion plating.
The invention introduces Si element into TiN coating, probably due to the formation of Si 3 N 4 The amorphous structure wraps other coating grains, so that the grains are refined, and the residual stress of the coating is improved. Meanwhile, si element can form a compact oxide film at high temperature, so that the high-temperature oxidation resistance of the coating is greatly improved. The high temperature resistance of the coating can be further improved by introducing a high temperature resistant element Y into the TiSiN coating and the synergistic effect of Si and Y. In addition, by adding B element, tiB of lubricating phase can be formed in the coating process 2 And BN. By adding Ag element, ag is a soft phase and is easy to move under the action of external force, so that the friction coefficient of the coating is reduced. Through the synergistic effect of the Si, Y, B, ag four elements, the TiSiBAgYN coating resistant to high-temperature lubrication can be formed.
Specifically, the preparation method of the high-temperature lubrication resistant TiSiBAgYN coating comprises the following steps:
introducing nitrogen, controlling the air pressure at 5-7Pa, starting an arc target power supply of the TiSiBAgY alloy target to perform arc ion coating, wherein the target current is 100-200A, the substrate bias voltage is-80V to 100V, and the deposition time is 1.5-5.5h, so that the TiSiBAgYN coating resistant to high temperature lubrication is prepared.
According to the embodiment of the invention, in the TiSiBAgY alloy target, the content of Si is 10-20wt%, the content of B is 5-15wt%, the content of Ag is 2-5wt%, the content of Y is 2-5wt%, and the balance is Ti.
The invention also discloses application of the high-temperature-lubrication-resistant TiSiBAgYN coating in cutter processing.
In order to further improve the performance of the TiSiBAgYN coating resistant to high-temperature lubrication, the invention also carries out post-treatment on the coating.
According to an embodiment of the present invention, the above post-treatment method includes a polishing treatment.
According to an embodiment of the present invention, the above polishing treatment conditions include: polishing with lubricant with polishing load of 40-170g/cm 2 The polishing rotation speed is 40-160rpm/min, and the polishing time is 80-170min.
According to an embodiment of the present invention, the lubricant is formed by mixing ethylene glycol oleate and modified liquid paraffin.
According to an embodiment of the invention, the mass ratio of the modified liquid paraffin to the glycol oleate is as follows: 1:0.02-0.04.
According to an embodiment of the present invention, the lubricant is used in an amount of 0.03 to 0.08g/cm 2 。
The invention also discloses application of the lubricant in preparing a TiSiBAgYN coating resistant to high-temperature lubrication.
The invention also discloses a preparation method of the modified liquid paraffin, which comprises the following steps: the modified liquid paraffin is prepared by grafting reaction of 2-allylmercaptonicotinic acid and liquid paraffin.
The invention provides a preparation method of modified liquid paraffin, which adopts 2-allylmercapto nicotinic acid as a modifier, grafts the modified liquid paraffin, and the prepared modified liquid paraffin is used for preparing a lubricant and then is used for polishing a TiSiBAgYN coating with high-temperature lubrication resistance, so that the TiSiBAgYN coating has good wear resistance and lower residual stress; the reason is probably because the nitrogen atom in the 2-allylmercapto nicotinic acid can be combined with the positive charge position on the metal surface in the friction process, and can also be complexed with the empty d orbit of the metal atom, so that the formed lubricating film can effectively separate the friction pair surface, and the functions of wear resistance and friction reduction are achieved.
Specifically, the preparation method of the modified liquid paraffin comprises the following steps:
1) Adding liquid paraffin into deionized water (the deionized water accounts for 25-35wt% of the total amount of the deionized water in the emulsified paraffin), stirring at 80-90 ℃ for 15-20min at 900-1100r/min, adding dodecylphenol polyoxyethylene ether and deionized water (the deionized water accounts for 25-35wt% of the total amount of the deionized water in the emulsified paraffin), stirring and mixing at constant temperature for 15-20min, adding the rest deionized water, and stirring and mixing at constant temperature for 15-20min to obtain the emulsified paraffin;
2) Adding dodecylphenol polyoxyethylene ether and 2-allylmercaptonicotinic acid into deionized water, stirring for 15-25min at 900-1100r/min, adding into the emulsified paraffin, heating to 65-80 ℃, adding potassium persulfate, stirring for reacting for 2.5-4h at 900-1100r/min, precipitating with acetone, washing, and drying to obtain the modified liquid paraffin.
According to an embodiment of the present invention, the volume ratio of the liquid paraffin to the total deionized water in the emulsified paraffin in the step 1) is: 1:5-7.5; the dosage of the dodecylphenol polyoxyethylene ether is 7-10wt% of the liquid paraffin.
According to an embodiment of the present invention, the mass volume ratio of the 2-allylmercaptonicotinic acid to deionized water in the step 2) is: 1g:1-2.5mL; the dosage of the dodecylphenol polyoxyethylene ether is 1.5-3wt% of the liquid paraffin; the mass ratio of the 2-allylmercaptonicotinic acid to the liquid paraffin is as follows: 1:6-8; the mass ratio of the liquid paraffin to the potassium persulfate is as follows: 1:0.015-0.023.
The invention also discloses application of the modified liquid paraffin in preparing a TiSiBAgYN coating resistant to high-temperature lubrication.
The beneficial effects of the invention include:
the invention obtains the high-temperature lubrication-resistant TiSiBAgYN coating, adopts the TiSiBAgY alloy target to carry out arc ion plating on the substrate, and the prepared high-temperature lubrication-resistant TiSiBAgYN coating has good wear resistance and lower residual stress, and has good bonding force with the substrate; the invention also adopts liquid paraffin modified by 2-allylmercaptonicotinic acid to carry out polishing post-treatment on the prepared TiSiBAgYN coating; the TiSiBAgYN coating with high-temperature lubrication resistance has better wear resistance.
Therefore, the invention provides the high-temperature lubrication-resistant TiSiBAgYN coating, which has good wear resistance and lower residual stress, and has good binding force with a substrate.
Drawings
FIG. 1 is an infrared spectrum of modified liquid paraffin and liquid paraffin prepared in example 5;
FIG. 2 is an infrared spectrum of the modified silica sol prepared in example 7;
FIG. 3 is the residual stress test results of the high temperature lubrication resistant TiSiBAgYN coatings prepared in examples 1-8;
FIG. 4 is the results of the abrasion resistance test of the high temperature lubrication resistant TiSiBAgYN coatings prepared in examples 1-8;
fig. 5 shows the results of the test of the bonding force between the high temperature lubrication resistant TiSiBAgYN coating prepared in examples 1 to 8 and the substrate.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more clear and clear, the technical solutions of the present invention are described in further detail below with reference to the specific embodiments:
the glycol oleate used in the examples of the present invention was purchased from Hebei Tuo Lubricant sales Co., ltd;
the TiSiBAgY alloy targets used in the examples of the present invention were purchased from New Material technology Co., ltd.
Example 1:
a preparation method of a high-temperature lubrication resistant TiSiBAgYN coating comprises the following steps:
introducing nitrogen, controlling the air pressure at 5Pa, starting an arc target power supply of the TiSiBAgY alloy target to perform arc ion coating, wherein the target current is 100A, the bias voltage of a matrix is 50V, and the deposition time is 1.5h, so that the TiSiBAgYN coating resistant to high temperature lubrication is prepared; wherein the thickness of the TiSiBAgYN coating resistant to high-temperature lubrication is 3.2 mu m; in the TiSiBAgY alloy target, the content of Si is 10wt%, the content of B is 10wt%, the content of Ag is 3wt%, the content of Y is 3wt%, and the content of Ti is 74wt%.
Example 2:
the preparation method of the TiSiBAgYN coating resistant to high-temperature lubrication is different from that of example 1: the TiSiBAg alloy target is adopted to replace the TiSiBAgY alloy target.
Example 3:
the preparation method of the TiSiBAgYN coating resistant to high-temperature lubrication is different from that of example 1: the TiSiBY alloy target is adopted to replace the TiSiBAgY alloy target.
Example 4:
the preparation method of the TiSiBAgYN coating resistant to high-temperature lubrication is different from that of example 1: the TiSiAgY alloy target is adopted to replace the TiSiBAgY alloy target.
Example 5:
the preparation method of the TiSiBAgYN coating resistant to high-temperature lubrication is different from that of example 1: and polishing the TiSiBAgYN coating with high-temperature lubrication resistance.
Specifically, the above polishing treatment conditions include: the lubricant prepared by mixing glycol oleate and modified liquid paraffin is adopted for polishing treatment, and the polishing load is 100g/cm 2 The polishing rotation speed is 100rpm/min, and the polishing time is 120min; wherein, the mass ratio of the modified liquid paraffin to the glycol oleate is as follows: 1:0.02; the lubricant dosage is 0.05g/cm 2 。
The preparation method of the modified liquid paraffin comprises the following steps:
1) Adding liquid paraffin into deionized water (the deionized water amount is 25wt% of the total amount of the deionized water in the emulsified paraffin), stirring at 80 ℃ for 20min at 900r/min, adding dodecylphenol polyoxyethylene ether and deionized water (the deionized water amount is 35wt% of the total amount of the deionized water in the emulsified paraffin), stirring and mixing at constant temperature for 15min, adding the rest deionized water, stirring and mixing at constant temperature for 20min, and obtaining the emulsified paraffin;
2) Adding dodecyl phenol polyoxyethylene ether and 2-allylmercaptonicotinic acid into deionized water, stirring for 25min at 900r/min, adding into the emulsified paraffin, heating to 65 ℃, adding potassium persulfate, stirring for 4h at 900r/min, precipitating with acetone, washing, and drying to obtain the modified liquid paraffin. Wherein, the volume ratio of the liquid paraffin to the total deionized water in the emulsified paraffin in the step 1) is as follows: 1:5; the dosage of the dodecylphenol polyoxyethylene ether is 7wt% of the liquid paraffin; the mass volume ratio of the 2-allylmercaptonicotinic acid to the deionized water in the step 2) is as follows: 1g 1mL; the dosage of the dodecylphenol polyoxyethylene ether is 1.5wt% of the liquid paraffin; the mass ratio of the 2-allylmercaptonicotinic acid to the liquid paraffin is as follows: 1:6; the mass ratio of the liquid paraffin to the potassium persulfate is as follows: 1:0.015.
Example 6:
the preparation method of the TiSiBAgYN coating resistant to high-temperature lubrication is different from that of example 5: the polishing treatment conditions are different.
Polishing treatment conditions were different from those of example 5: liquid paraffin is adopted to replace modified liquid paraffin.
Example 7:
the preparation method of the TiSiBAgYN coating resistant to high-temperature lubrication is different from that of example 1: and (3) carrying out hole sealing treatment on the TiSiBAgYN coating with high-temperature lubrication resistance.
The invention also discloses a hole sealing treatment method, which comprises the following steps: and (3) spraying a phosphate coating on the surface of the high-temperature lubrication resistant TiSiBAgYN coating, and curing to obtain the hole sealing layer.
Specifically, the hole sealing treatment method comprises the following steps: spraying phosphate paint on the surface of the high-temperature lubrication resistant TiSiBAgYN coating, wherein the spraying air pressure is 0.5-0.6MPa, the spraying distance is 25-30cm, and then curing for 1.5-3h at 300-320 ℃ to obtain a hole sealing layer, and the thickness of the hole sealing layer is 0.5-0.8 mu m.
For the purposes of the present invention, the phosphate coating described above comprises: aluminum chromium phosphate binder, fused silica, alumina, silicon nitride, ultrafine silica, and modified silica sol.
The invention also discloses a preparation method of the phosphate coating, which comprises the following steps:
adding deionized water and chromium trioxide into phosphoric acid, stirring and mixing for 15-30min at 75-85 ℃, then adding aluminum hydroxide, heating to 95-98 ℃ for reaction for 1-1.5h, then cooling to 80-88 ℃, adding paraformaldehyde for reaction for 5-8min, and then heating to 100-105 ℃ for reaction for 15-20min to prepare an aluminum-chromium phosphate binder; and then mixing the aluminum chromium phosphate binder with fused quartz, alumina, silicon nitride, superfine silicon dioxide and modified silica sol, and performing ball milling and dispersion to obtain the phosphate coating.
Wherein the mass volume ratio of phosphoric acid to deionized water is as follows: 1g, 0.5-0.8mL; the mass ratio of phosphoric acid to chromium trioxide is as follows: 1:0.065-0.08; the molar mass ratio of phosphoric acid to aluminum hydroxide is as follows: 1:0.3-0.4; the mass ratio of phosphoric acid to paraformaldehyde is as follows: 1:0.03-0.05; the mass ratio of the aluminum chromium phosphate binder to the fused quartz is as follows: 1:0.2-0.25; the mass ratio of the aluminum phosphate chromium binder to the aluminum oxide is as follows: 1:0.2-0.25; the mass ratio of the aluminum phosphate chromium binder to the silicon nitride is as follows: 1:0.2-0.25; the mass ratio of the aluminum phosphate chromium binder to the superfine silicon dioxide is as follows: 1:0.1-0.15; the mass ratio of the aluminum phosphate chromium binder to the modified silica sol is as follows: 1:0.2-0.3.
The invention also discloses a preparation method of the modified silica sol, which comprises the following steps: the coupling agent is prepared by hydrosilylation reaction of linalool oxide and triethoxysilane, and the coupling agent is hydrolyzed and then subjected to dehydration condensation reaction with silica sol to prepare the modified silica sol.
The invention discloses a preparation method of modified silica sol, which comprises the steps of hydrolyzing a coupling agent prepared by taking linalool oxide as a modifier, performing condensation reaction with the silica sol, preparing the prepared modified silica sol into phosphate coating, and then using the phosphate coating for hole sealing treatment of TiSiBAgYN coating, so that the TiSiBAgYN coating with high-temperature lubrication resistance has better wear resistance and lower residual stress, and has good bonding force with a substrate; the reason is probably because phosphate can go deep into the coating as hole sealing agent, and the branched chain and the ring structure in the linalool oxide can increase the crosslinking performance of the hole sealing agent, thereby further enhancing the wear resistance of TiSiBAgYN coating and the binding force between the coating and the matrix, and being beneficial to eliminating residual stress.
Specifically, the preparation method of the modified silica sol comprises the following steps:
adding triethoxysilane into linalool oxide, adding 8-12ppm chloroplatinic acid at 65-75 ℃, reacting for 1-1.5h, and distilling under reduced pressure to obtain a coupling agent; adjusting the pH of an isopropanol water solution to 3-4 by adopting acetic acid, then slowly adding the isopropanol water solution into the coupling agent, reacting for 2.5-4 hours at 65-80 ℃ to prepare a coupling agent hydrolysate, adjusting the pH of silica sol to 2-2.5, adding isopropanol (the mass ratio of the silica sol to the isopropanol is 1:5-8), performing azeotropic distillation for 30-60 minutes to prepare an isopropanol dispersion liquid of the silica sol, then slowly adding the coupling agent hydrolysate, and reacting for 2.5-4 hours at 65-75 ℃ to prepare the modified silica sol.
Wherein, the mole ratio of linalool oxide to triethoxysilane is: 1:0.8-1.2; the volume ratio of isopropanol to water in the aqueous isopropanol solution is as follows: 1:0.05-0.08; the mass ratio of the coupling agent to the isopropanol water solution is as follows: 1:3.5-5; the mass ratio of the isopropanol dispersion liquid of the silica sol to the coupling agent hydrolysate is as follows: 1:0.3-0.5.
Further, the method comprises the steps of,
a method of pore sealing treatment comprising: and (3) spraying a phosphate coating on the surface of the high-temperature lubrication resistant TiSiBAgYN coating, wherein the spraying air pressure is 0.5MPa, the spraying distance is 25cm, and then curing for 3 hours at 300 ℃ to prepare a hole sealing layer, and the thickness of the hole sealing layer is 0.6 mu m.
A method of preparing a phosphate coating comprising:
adding deionized water and chromium trioxide into phosphoric acid, stirring and mixing for 30min at 75 ℃, then adding aluminum hydroxide, heating to 98 ℃ for reaction for 1h, then cooling to 80 ℃, adding paraformaldehyde for reaction for 8min, and then heating to 105 ℃ for reaction for 15min to obtain an aluminum-chromium phosphate binder; and then mixing the aluminum chromium phosphate binder with fused quartz, alumina, silicon nitride, superfine silicon dioxide and modified silica sol, and performing ball milling and dispersion to obtain the phosphate coating. Wherein the mass volume ratio of phosphoric acid to deionized water is as follows: 1g:0.5ml; the mass ratio of phosphoric acid to chromium trioxide is as follows: 1:0.065; the molar mass ratio of phosphoric acid to aluminum hydroxide is as follows: 1:0.3; the mass ratio of phosphoric acid to paraformaldehyde is as follows: 1:0.03; the mass ratio of the aluminum chromium phosphate binder to the fused quartz is as follows: 1:0.2; the mass ratio of the aluminum phosphate chromium binder to the aluminum oxide is as follows: 1:0.2; the mass ratio of the aluminum phosphate chromium binder to the silicon nitride is as follows: 1:0.2; the mass ratio of the aluminum phosphate chromium binder to the superfine silicon dioxide is as follows: 1:0.1; the mass ratio of the aluminum phosphate chromium binder to the modified silica sol is as follows: 1:0.2.
The preparation method of the modified silica sol comprises the following steps:
adding triethoxysilane into linalool oxide, adding 8ppm chloroplatinic acid at 65 ℃, reacting for 1.5h, and distilling under reduced pressure to obtain a coupling agent; acetic acid is adopted to adjust the pH value of the isopropanol water solution to 3, then the isopropanol water solution is slowly added into the coupling agent to react for 4 hours at 65 ℃ to prepare coupling agent hydrolysate, the pH value of the silica sol is adjusted to 2, isopropanol (the mass ratio of the silica sol to the isopropanol is 1:5) is added, azeotropic distillation is carried out for 60 minutes to prepare isopropanol dispersion liquid of the silica sol, then the coupling agent hydrolysate is slowly added to react for 4 hours at 65 ℃ to prepare the modified silica sol. Wherein, the mole ratio of linalool oxide to triethoxysilane is: 1:0.8; the volume ratio of isopropanol to water in the aqueous isopropanol solution is as follows: 1:0.05; the mass ratio of the coupling agent to the isopropanol water solution is as follows: 1:3.5; the mass ratio of the isopropanol dispersion liquid of the silica sol to the coupling agent hydrolysate is as follows: 1:0.3.
Hydrogen spectrum of coupling agent: 1 H NMR（400MHz，CDCl 3 ）：1.23（t，9H，O-CH 2 -CH 3 ），3.81（m，6H，O-CH 2 ），0.61（t，2H，Si-CH 2 ），1.28（m，2H，Si-CH 2 -CH 2 ），1.23（s，3H，O-C-CH 3 ），3.51（m，1H，O-CH），1.65（m，2H，O-CH-CH 2 ），1.73（m，2H，O-CH-CH 2 -CH 2 ），1.16（s，6H，OH-C-CH 3 ）。HRMS(ESI)：C 16 H 34 O 5 Si，m/z [M+H] + ，334.53。
example 8:
the preparation method of the TiSiBAgYN coating resistant to high-temperature lubrication is different from that of example 7: the preparation methods of phosphate coatings are different.
The preparation method of the phosphate coating is different from that of example 7: adopts silica sol to replace modified silica sol.
Test example:
1. infrared spectroscopy testing
The samples were subjected to infrared spectroscopy using an FTIR-8400S Fourier infrared spectrometer.
The modified liquid paraffin and liquid paraffin prepared in example 5 were subjected to the above-described test, and the results are shown in fig. 1. As can be seen from FIG. 1, andcompared with the infrared spectrogram of the liquid paraffin, the infrared spectrogram of the modified liquid paraffin is 1245cm -1 An infrared characteristic absorption peak of the C-S bond exists at the position; at 1694cm -1 An infrared characteristic absorption peak with c=o bond; indicating that the 2-allylmercaptonicotinic acid participates in the formation reaction of the modified liquid paraffin.
The modified silica sol and silica sol prepared in example 7 were subjected to the above test, and the results are shown in fig. 2. As can be seen from FIG. 2, the infrared spectrum of the modified silica sol was 2976cm -1 、2907cm -1 There is an infrared characteristic absorption peak of methyl and methylene, and 3446cm -1 Absorption peak of hydroxyl group at 1627cm -1 The peak of the adsorbed water layer is obviously weakened, which indicates that the coupling agent participates in the generation reaction of the modified silica sol.
2. Elemental composition testing of coatings
The elemental distribution in the coating samples was analyzed using an energy spectrum analyzer.
TABLE 1 results of elemental content test
| Element(s) | Content (at.) |
| Ti | 34.6 |
| Si | 4.6 |
| B | 4.7 |
| Ag | 1.4 |
| Y | 1.5 |
| N | 53.2 |
The above test was performed on the high temperature lubrication resistant TiSiBAgYN coating prepared in example 1, and the element content test results of the TiSiBAgYN coating are shown in Table 1.
3. Residual stress test
Carrying out residual stress analysis on the sample by using an X-350A type X-ray stress meter; the experimental grouping included: example 1 is designated N1; example 2 is designated N2; example 3 is designated N3; example 4 is designated N4; example 5 is designated N5; example 6 is designated N6; example 7 is designated N7; example 8 is designated N8.
The above tests were performed on the high temperature lubrication resistant TiSiBAgYN coatings prepared in examples 1-8, and the results are shown in FIG. 3. As can be seen from fig. 3, the residual stress in example 6 was reduced compared with example 1, indicating that the polishing treatment can reduce the residual stress in the coating; example 5 shows that the residual stress has little change compared with example 6, and the 2-allylmercaptonicotinic acid modified liquid paraffin is used for polishing treatment of the high-temperature-resistant lubrication TiSiBAgYN coating, and has little influence on the residual stress of the high-temperature-resistant lubrication TiSiBAgYN coating; compared with example 8, the residual stress of example 7 is reduced, which shows that after the coupling agent is used for modifying the silica sol, the modified silica sol is used for preparing the phosphate coating, and then the phosphate coating is used for carrying out hole sealing treatment on the TiSiBAgYN coating, so that the TiSiBAgYN coating resistant to high-temperature lubrication has lower residual stress; example 8 also showed a reduction in residual stress compared to example 1, demonstrating that sealing the TiSiBAgYN coating is beneficial to the elimination of residual stress; example 1 has reduced residual stress compared to examples 2-4, indicating that the mixed use of TiSiBAgY alloys has a reduced effect on residual stress within the coating.
4. Wear resistance test
Testing the friction coefficient of the sample by adopting a CETR UMT-2 high-temperature friction and wear testing machine; the experimental group was the same as that of test example 3.
The above tests were performed on the high temperature lubrication resistant TiSiBAgYN coatings prepared in examples 1-8, and the results are shown in FIG. 4. As can be seen from fig. 4, the friction coefficient of example 6 is reduced compared with that of example 1, which demonstrates that the polishing treatment provides the TiSiBAgYN coating with good wear resistance to high temperature lubrication; example 5 has a reduced coefficient of friction compared with example 6, demonstrating that 2-allylmercaptonicotinic acid modified liquid paraffin is used for polishing treatment of high temperature lubrication resistant TiSiBAgYN coating, so that the high temperature lubrication resistant TiSiBAgYN coating has good wear resistance; compared with example 8, the friction coefficient of example 7 is also reduced, which shows that after the coupling agent is used for modifying the silica sol, the modified silica sol is used for preparing the phosphate coating, and then the phosphate coating is used for carrying out hole sealing treatment on the TiSiBAgYN coating, so that the TiSiBAgYN coating with high-temperature lubrication resistance has good wear resistance; compared with the example 1, the friction coefficient of the TiSiBAgYN coating is also reduced, which shows that the TiSiBAgYN coating resistant to high-temperature lubrication has good wear resistance after hole sealing treatment; the reduction in coefficient of friction of example 1 compared to examples 2-4 demonstrates that the use of a mixture of TiSiBAgY alloys results in a TiSiBAgY coating with good wear resistance that is resistant to high temperature lubrication.
5. Binding force test
Adopting a MFY-400 multifunctional material surface performance testing machine to test the binding force between the sample coating and the matrix; the experimental group was the same as that of test example 3.
The above tests were performed on the high temperature lubrication resistant TiSiBAgYN coatings prepared in examples 1-8, and the results are shown in FIG. 5. As can be seen from fig. 5, the binding force of example 6 is not much different from that of example 1, which shows that the polishing treatment has little influence on the binding force of the high-temperature lubrication resistant TiSiBAgYN coating and the substrate; example 5 and example 6 have little difference in binding force, which indicates that the 2-allylmercaptonicotinic acid modified liquid paraffin is used for polishing treatment of the high-temperature-resistant lubrication TiSiBAgYN coating and has little influence on the binding force of the high-temperature-resistant lubrication TiSiBAgYN coating and a matrix; compared with the embodiment 8, the embodiment 7 has an increased binding force, which shows that after the coupling agent modifies the silica sol, the modified silica sol is used for the phosphate coating, and then the phosphate coating is used for sealing the TiSiBAgYN coating, so that the TiSiBAgYN coating with high-temperature lubrication resistance has good binding force; compared with the embodiment 1, the embodiment 8 has higher binding force, which shows that the TiSiBAgYN coating has good binding force after the TiSiBAgYN coating is subjected to hole sealing treatment; compared with the embodiment 2-embodiment 4, the embodiment 1 has increased binding force, which shows that the TiSiBAgY alloy is mixed for use, so that the TiSiBAgYN coating with high temperature lubrication resistance has good binding force with the substrate.
The conventional technology in the above embodiments is known to those skilled in the art, and thus is not described in detail herein.
The foregoing is merely illustrative of the present invention, and the present invention is not limited thereto, and any person skilled in the art will readily recognize that variations or substitutions are within the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (9)
1. A TiSiBAgYN coating resistant to high-temperature lubrication is characterized in that: the TiSiBAgYN coating comprises a nitride layer; the nitride layer contains Ti, si, B, ag, Y and the TiSiBAgYN coating is deposited over the substrate; the substrate comprises one of metal, cemented carbide or ceramic; the friction coefficient of the TiSiBAgYN coating is less than 0.3.
2. The high temperature lubrication resistant TiSiBAgYN coating of claim 1, wherein: the residual stress of the high-temperature lubrication resistant TiSiBAgYN coating is 300-360MPa.
3. The high temperature lubrication resistant TiSiBAgYN coating of claim 1, wherein: the thickness of the TiSiBAgYN coating resistant to high-temperature lubrication is 2-6 mu m.
4. The high temperature lubrication resistant TiSiBAgYN coating of claim 1, wherein: the nitrogen content in the nitride layer is 45-55at.%.
5. The method for preparing the high-temperature lubrication-resistant TiSiBAgYN coating, which comprises the following steps: nitrogen is introduced, and a nitride coating is deposited on the substrate by utilizing a physical vapor deposition technology, so that the TiSiBAgYN coating resistant to high-temperature lubrication is prepared.
6. The method for preparing the high-temperature lubrication-resistant TiSiBAgYN coating, which is characterized by comprising the following steps of: the physical vapor deposition technique includes arc ion plating.
7. The method for preparing the high-temperature lubrication-resistant TiSiBAgYN coating, which is characterized in that: the target current during the arc ion plating is 100-200A.
8. The method for preparing the high-temperature lubrication-resistant TiSiBAgYN coating, which is characterized in that: the deposition time of the arc ion plating film is 1.5-5.5h.
9. Use of a TiSiBAgYN coating resistant to high temperature lubrication according to any of claims 1 to 4 in cutting tool machining.
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