CN114182213A - Titanium alloy wear-resistant antioxidant composite coating and preparation method thereof - Google Patents
Titanium alloy wear-resistant antioxidant composite coating and preparation method thereof Download PDFInfo
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- 229910001069 Ti alloy Inorganic materials 0.000 title claims abstract description 105
- 238000000576 coating method Methods 0.000 title claims abstract description 71
- 239000011248 coating agent Substances 0.000 title claims abstract description 69
- 239000002131 composite material Substances 0.000 title claims abstract description 43
- 238000002360 preparation method Methods 0.000 title claims abstract description 31
- 239000003963 antioxidant agent Substances 0.000 title description 6
- 230000003078 antioxidant effect Effects 0.000 title description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 45
- 238000007733 ion plating Methods 0.000 claims abstract description 38
- 230000003647 oxidation Effects 0.000 claims abstract description 38
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 38
- 239000000758 substrate Substances 0.000 claims abstract description 34
- 239000011159 matrix material Substances 0.000 claims abstract description 33
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 32
- 239000007789 gas Substances 0.000 claims abstract description 23
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 23
- 229910052786 argon Inorganic materials 0.000 claims abstract description 16
- 230000007704 transition Effects 0.000 claims abstract description 14
- 238000005256 carbonitriding Methods 0.000 claims abstract description 12
- 238000004140 cleaning Methods 0.000 claims abstract description 12
- 238000007747 plating Methods 0.000 claims abstract description 7
- 239000010936 titanium Substances 0.000 claims description 23
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 20
- 238000000034 method Methods 0.000 claims description 20
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 16
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 13
- 238000010438 heat treatment Methods 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 239000003344 environmental pollutant Substances 0.000 claims description 6
- 231100000719 pollutant Toxicity 0.000 claims description 6
- 229910021529 ammonia Inorganic materials 0.000 claims description 5
- 238000005498 polishing Methods 0.000 claims description 3
- 238000005516 engineering process Methods 0.000 abstract description 7
- 238000004381 surface treatment Methods 0.000 abstract description 3
- 239000007769 metal material Substances 0.000 abstract description 2
- 230000002035 prolonged effect Effects 0.000 abstract 1
- 239000010410 layer Substances 0.000 description 39
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 15
- 230000008569 process Effects 0.000 description 12
- 238000005121 nitriding Methods 0.000 description 11
- 239000000463 material Substances 0.000 description 10
- 230000000694 effects Effects 0.000 description 8
- 229910052719 titanium Inorganic materials 0.000 description 8
- 239000000498 cooling water Substances 0.000 description 7
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 6
- 229910052799 carbon Inorganic materials 0.000 description 6
- 239000013078 crystal Substances 0.000 description 6
- 230000006872 improvement Effects 0.000 description 6
- 239000006104 solid solution Substances 0.000 description 6
- 238000002441 X-ray diffraction Methods 0.000 description 5
- 230000008595 infiltration Effects 0.000 description 5
- 238000001764 infiltration Methods 0.000 description 5
- 150000004767 nitrides Chemical class 0.000 description 5
- 230000001681 protective effect Effects 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 238000009529 body temperature measurement Methods 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 4
- 238000001816 cooling Methods 0.000 description 4
- 230000007797 corrosion Effects 0.000 description 4
- 238000005260 corrosion Methods 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- 238000011049 filling Methods 0.000 description 4
- 230000004048 modification Effects 0.000 description 4
- 238000012986 modification Methods 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 238000004321 preservation Methods 0.000 description 4
- 239000012495 reaction gas Substances 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 3
- 229910001873 dinitrogen Inorganic materials 0.000 description 3
- 238000010891 electric arc Methods 0.000 description 3
- 230000008093 supporting effect Effects 0.000 description 3
- NRTOMJZYCJJWKI-UHFFFAOYSA-N Titanium nitride Chemical compound [Ti]#N NRTOMJZYCJJWKI-UHFFFAOYSA-N 0.000 description 2
- 229910011208 Ti—N Inorganic materials 0.000 description 2
- 230000004075 alteration Effects 0.000 description 2
- 230000003064 anti-oxidating effect Effects 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 238000000407 epitaxy Methods 0.000 description 2
- 238000001755 magnetron sputter deposition Methods 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 230000006911 nucleation Effects 0.000 description 2
- 238000010899 nucleation Methods 0.000 description 2
- 230000000704 physical effect Effects 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000005728 strengthening Methods 0.000 description 2
- 239000002344 surface layer Substances 0.000 description 2
- 238000005299 abrasion Methods 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 238000005255 carburizing Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- -1 nitride carbides Chemical class 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
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Classifications
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- 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
- C23C14/0021—Reactive sputtering or 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
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- 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
- C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C8/06—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases
- C23C8/28—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases more than one element being applied in one step
- C23C8/30—Carbo-nitriding
-
- 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
- C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C8/06—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases
- C23C8/36—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases using ionised gases, e.g. ionitriding
Abstract
The invention discloses a titanium alloy wear-resistant and oxidation-resistant composite coating and a preparation method thereof, and relates to the technical field of metal material surface treatment. The preparation method comprises the following steps: s1, placing the pretreated titanium alloy matrix in a vacuum furnace, and obtaining the titanium alloy matrix with the surface containing the carbonitriding layer under the vacuum condition; s2, after the obtained titanium alloy matrix containing the carbonitrided layer is subjected to ion cleaning, under the condition of mixed gas of argon and nitrogen, an arc ion plating Cr target is adopted, and a transition layer is firstly deposited on the surface of the titanium alloy matrix; and S3, plating a working layer on the surface of the obtained transition layer, namely obtaining the wear-resistant and oxidation-resistant composite coating on the surface of the titanium alloy substrate. The invention adopts the plasma carbonitriding/arc ion plating composite technology to prepare the impact-resistant and wear-resistant coating, so that the surface of the titanium alloy has good impact-resistant, wear-resistant and antifriction properties, and the service life of the titanium alloy on the armor is prolonged.
Description
Technical Field
The invention relates to the technical field of metal material processing, in particular to a titanium alloy wear-resistant and oxidation-resistant composite coating and a preparation method thereof.
Background
The titanium alloy has high specific rigidity and specific strength, good plasticity and toughness, and excellent heat resistance and corrosion resistance, and is an ideal armor material. However, titanium alloys have low hardness and poor wear resistance, are prone to adhesive wear, and greatly limit the service performance and service life of titanium alloy armors. Meanwhile, the titanium alloy armor is seriously oxidized at high temperature, the plasticity and toughness of the oxidized titanium alloy armor are obviously reduced, and the protective performance of the titanium alloy armor is directly influenced. Particularly, when the titanium alloy armor bears external impact rotating load, the friction characteristic formed by the rotating load can cause adhesion abrasion between an impact object and the titanium alloy armor, thereby scraping the titanium alloy armor. Meanwhile, oxidation caused by frictional heat causes the surface ductility and toughness of the titanium alloy armor to be obviously reduced, and the impact resistance of the titanium alloy armor is seriously reduced. Therefore, the improvement of the wear resistance and the oxidation resistance of the titanium alloy is of great importance for improving the service performance and the service life of the titanium alloy armor.
In order to improve the surface performance of the titanium alloy armor, the titanium alloy armor has higher hardness and good wear resistance, besides methods of improving alloy components, optimizing a preparation process and the like, a surface modification technology is also one of the most effective methods for improving the performance of the titanium alloy at present. However, the conventional surface treatment technology for titanium alloy only increases the surface hardness of titanium alloy to improve the wear resistance of the surface, thereby achieving the wear resistance effect, such as nitriding, carburizing, boriding and metal infiltration. However, these hardened layers are highly susceptible to failure at high temperatures and in the event of lubricant failure, and are susceptible to microcracking. Therefore, the improvement of the wear resistance of the titanium alloy by the single surface treatment technology is very limited.
Disclosure of Invention
The invention aims to solve the defects in the background technology, and provides a titanium alloy wear-resistant anti-oxidation composite coating and a preparation method thereof.
The invention aims to provide a preparation method of a titanium alloy wear-resistant and oxidation-resistant composite coating, which is characterized by comprising the following steps:
s1, placing the pretreated titanium alloy matrix in a vacuum furnace, heating to 900-950 ℃ under a vacuum condition, introducing a mixed gas of methane, ammonia and nitrogen, keeping the air pressure of a chamber at 80-120 Pa, and keeping the temperature for 8-12 h to obtain the titanium alloy matrix with the surface containing the carbonitrided layer;
s2, polishing the obtained titanium alloy matrix containing the carbonitriding layer, plating a transition layer on the polished surface of the titanium alloy matrix by adopting an arc ion plating Cr target under the mixed gas of argon and nitrogen;
and S3, plating a working layer on the surface of the obtained transition layer by adopting an arc ion plating Cr target, an Al target and a Ti target under the mixed gas of nitrogen and argon, namely obtaining the wear-resistant and oxidation-resistant composite coating on the surface of the titanium alloy substrate.
Preferably, in S2, when preparing the transition layer, the temperature of the titanium alloy matrix containing the carbonitriding layer is 200-500 ℃, the bias voltage of the arc ion plating matrix is-700-900V, the target power is 100-300W, the target base distance is 10-20cm, the Cr target current is 80A, the flow ratio of argon and nitrogen is 1: 1.6-3.5, and the plating time is 60 min.
Preferably, in S3, when the working layer is prepared, the temperature of the titanium alloy substrate containing the carbonitrided layer is 200-500 ℃, the bias voltage of the substrate is-100 to-400V, the current of the arc ion plating Cr target is 65A, the current of the Al target is 60A, and the current of the Ti target is 60A; the coating time is 60 min.
More preferably, in S3, the flow ratio of nitrogen to argon is 1:1, and the chamber pressure is 2.0 Pa.
Preferably, in S1, the titanium alloy substrate is pretreated by circularly cleaning the titanium alloy substrate with ethanol and acetone to ensure that the roughness of the titanium alloy substrate is Ra0.4-1.6.
Preferably, in S1, the ratio of methane to ammonia to nitrogen is 15-20: 5-10: 75.
Preferably, the surface of the titanium alloy matrix containing the carbonitrided layer is further subjected to glow treatment before the preparation of the transition layer, wherein the glow treatment condition is that the vacuum degree is 5 multiplied by 10-3Pa, bias voltage of-800V and Ar flow rate of 170sccm, and cleaning for 10-20 min to remove oxides and pollutants on the surface of the titanium alloy matrix containing the carbonitrided layer.
The second purpose of the invention is to provide a titanium alloy wear-resistant and oxidation-resistant composite coating.
Compared with the prior art, the invention has the beneficial effects that:
the titanium alloy wear-resistant anti-oxidation composite coating and the preparation method thereof provided by the invention have the advantages that after the surface of a titanium alloy substrate is subjected to plasma carbonitriding treatment, titanium and nitrogen react to form titanium nitride (Ti)2N, TiN) and Ti-N solid solutions. Carbon has a certain solid solubility in titanium, and the reaction of titanium and carbon can produce a hard phase containing TiC and a Ti-C solid solution. The TiN and the TiC are high-hardness phases, and the solid solution strengthening effect of the N, C element is added, so that the TiN and the TiC have better wear resistance, corrosion resistance and high-temperature oxidation resistance than the titanium alloy, the TiN and the TiC containing the high-hardness phases are formed on the surface of the titanium alloy, the advantages of high strength and high toughness of the titanium alloy are kept, the hardness of the surface layer is correspondingly improved, and the improvement of the hardness is very beneficial to the improvement of the wear resistance.
The CrTiAlN coating prepared by adopting the arc ion plating technology has good wear resistance and oxidation resistance. Because the physical property difference between the arc ion plating coating and the titanium alloy matrix is large, the hardness of the coating and the matrix is reduced sharply, the elastic modulus is different, stress concentration with different degrees exists at the interface of the coating and the matrix, and the interface is easy to crack and peel due to the existence of the stress at the interface, so that the coating fails. After the titanium alloy is subjected to ion nitrocarburizing treatment, the carburized layer has higher hardness (more than 1000HV) than a titanium alloy matrix, the hardness is gradually reduced from outside to inside, a better supporting effect can be achieved for an ion plating layer, and meanwhile, the fatigue resistance can also be improved. In addition, in the nitriding process, N element is combined with Ti, Al, V and other elements in the titanium alloy matrix to form nitride or nitrogen carbide with the same crystal structure and similar lattice constant as the coating phase. In the subsequent ion plating process, coating phase (AlN, CrN, TiN and Cp) is epitaxially grown on the nitride or the nitride carbide, so that the strain energy of a coating-substrate interface is reduced, and the bonding force between the coating and the substrate is improved; the compound layer has a higher hardness than the diffusion layer, so that the hardness is more than 2000HV, and a stronger supporting effect can be provided for the ion plating layer. In addition, the compound layer can be used as a phase epitaxy growth nucleation point of the ion plating coating, has high hardness, has a large amount of stacking faults and nanometer twin crystals, and can change the crack propagation direction and improve the toughness of the composite coating through the slip deformation of the stacking faults and the twin crystals.
Drawings
Fig. 1 is a scanning electron microscope image of the wear-resistant and oxidation-resistant composite coating of the titanium alloy provided in example 1.
FIG. 2 is an XRD (X-ray diffraction) pattern of the wear-resistant and oxidation-resistant composite coating of the titanium alloy provided in examples 1 to 4.
FIG. 3 is a graph of the friction coefficient of the titanium alloy wear-resistant and oxidation-resistant composite coating and the titanium alloy substrate provided in example 1.
Detailed Description
In order to make the technical solutions of the present invention better understood and implemented by those skilled in the art, the present invention is further described below with reference to the following specific embodiments and the accompanying drawings, but the embodiments are not meant to limit the present invention.
It should be noted that the experimental methods described in the following examples are all conventional methods unless otherwise specified; the reagents and materials used are commercially available, unless otherwise specified.
In each of the following examples, one arc ion plating Cr target (purity 99.99%), two Al targets (purity 99.99%) and one Ti target (purity 99.99%) were used.
Example 1
A preparation method of a titanium alloy wear-resistant antioxidant composite coating comprises the following steps:
1. gas phase plasma carbonitriding process:
1) the sample to be treated washed with alcohol and acetone (roughness requirement: Ra0.4-Ra1.6) is placed in an auxiliary heating device on a cathode of a nitriding furnace, and a sample is placed to ensure that one surface of the sample is right opposite to an observation hole, so that the temperature measurement is convenient. And opening a mechanical pump, vacuumizing to the limit vacuum, filling argon for about five minutes, closing the gas (preventing oxygen in the furnace from reacting with the surface of the sample to generate oxide skin when the temperature is raised and influencing the infiltration effect), and vacuumizing to the limit vacuum.
2) Opening a nitriding furnace control power supply, slowly increasing current and voltage, heating a sample to 900 ℃, and introducing methane, ammonia and nitrogen according to the proportion: 15:10:75, the air pressure is 100Pa, and the heat preservation time is 10 h.
3) And (5) closing the furnace. And reducing and finally turning off the power supply voltage, cooling the sample to room temperature in the furnace, stopping gas supply, finally turning off the cooling water, and turning off the mechanical pump. Finally, the sample is taken out after the sample is cooled to room temperature.
4) A carbonitrided layer containing TiN and TiC with a thickness of 1mm is formed on the surface of the titanium alloy substrate, the hardness reaches more than 1000HV, and the impact toughness can be improved to 60J/cm2The above.
2. Arc ion plating CrTiAlN wear-resistant oxidation-resistant composite coating
The preparation method is characterized in that nitrogen (reaction gas) and argon (protective gas) are introduced into an arc ion plating Cr target (the purity is 99.99%), two Al targets (the purity is 99.99%) and a Ti target (the purity is 99.99%) for preparation.
1) Placing the sample in an ultrasonic container, cleaning the sample for 10 minutes by using an acetone solution, dehydrating and drying the sample, and then placing the sample into a vacuum chamber;
2) glow treatment: background vacuum degree of 5X 10-3Cleaning at Pa, bias voltage of-800V and Ar flow rate of 170sccm (standard condition milliliter per minute) for 15min to remove surface oxides and pollutants;
3) transition layer process: base material temperature: 300 ℃, the electric arc ion plating matrix bias voltage is-800V, the target power is 200W, the target base distance is 15cm, the Cr target current is 80A, the Ar flow is 30sccm, and N2The flow rate is 50 sccm;
4) the preparation process of the working layer comprises the following steps: base material temperature: the matrix bias voltage is-200V at 300 ℃, the current of the arc ion plating Cr target is 65A, the current of the Al target is 60A, and the current of the Ti target is 60A; n is a radical of2The flow rate is 22sccm, the Ar flow rate is 22sccm, the air pressure of the chamber is kept at 2.0Pa, and the coating time is 60 min;
namely, the CrTiAlN wear-resistant and oxidation-resistant composite coating is prepared on the surface of the titanium alloy substrate.
Example 2
A preparation method of a titanium alloy wear-resistant antioxidant composite coating comprises the following steps:
1. gas phase plasma carbonitriding process:
1) the sample to be treated washed with alcohol and acetone (roughness requirement: Ra0.4-Ra1.6) is placed in an auxiliary heating device on a cathode of a nitriding furnace, and a sample is placed to ensure that one surface of the sample is right opposite to an observation hole, so that the temperature measurement is convenient. And opening a mechanical pump, vacuumizing to the limit vacuum, filling argon for about five minutes, closing the gas (preventing oxygen in the furnace from reacting with the surface of the sample to generate oxide skin when the temperature is raised and influencing the infiltration effect), and vacuumizing to the limit vacuum.
2) And (3) turning on a nitriding furnace control power supply, slowly increasing the current and the voltage, heating the sample to 900 ℃, and turning on cooling water. Introducing methane, ammonia gas and nitrogen gas in the following proportion: 20:5:75, the air pressure is 120Pa, and the heat preservation time is 12 h.
3) And (5) closing the furnace. And reducing and finally turning off the power supply voltage, cooling the sample to room temperature in the furnace, stopping gas supply, finally turning off the cooling water, and turning off the mechanical pump. Finally, the sample is taken out after the sample is cooled to room temperature.
4) A carbonitrided layer containing TiN and TiC with a thickness of 2mm is formed on the surface of the titanium alloy substrate, the hardness reaches over 1000HV, and the impact toughness can be improved to 60J/cm2The above.
2 electric arc ion plating CrTiAlN wear-resistant oxidation-resistant composite coating
The preparation method is characterized in that nitrogen (reaction gas) and argon (protective gas) are introduced into an arc ion plating Cr target (the purity is 99.99%), two Al targets (the purity is 99.99%) and a Ti target (the purity is 99.99%) for preparation.
1) The method comprises the steps of pretreating a sample subjected to gas-phase plasma carbonitriding before coating, sequentially grinding the sample by using 800# -2000# abrasive paper, and then polishing the sample to a mirror surface.
2) Placing the sample in an ultrasonic container, cleaning the sample for 10 minutes by using an acetone solution, dehydrating and drying the sample, and then placing the sample into a vacuum chamber;
3) glow treatment: background vacuum degree of 5X 10-3Cleaning at Pa, bias voltage of-800V and Ar flow rate of 170sccm (standard condition milliliter per minute) for 15min to remove surface oxides and pollutants;
4) transition layer process: base material temperature: 500 ℃, arc ion plating matrix bias voltage of-900V, target power of 300W, target base distance of 20cm, Cr target current of 80A, Ar flow of 30sccm, N2The flow rate is 50 sccm;
5) the preparation process of the working layer comprises the following steps: base material temperature: the substrate bias voltage is-400V at 500 ℃, the current of the arc ion plating Cr target is 65A, the current of the Al target is 60A, and the current of the Ti target is 60A; n is a radical of2The flow rate is 22sccm, the Ar flow rate is 22sccm, the air pressure of the chamber is kept at 2.0Pa, and the coating time is 60 min;
namely, the CrTiAlN wear-resistant and oxidation-resistant composite coating is prepared on the surface of the titanium alloy substrate.
Example 3
A preparation method of a titanium alloy wear-resistant antioxidant composite coating comprises the following steps:
1. gas phase plasma carbonitriding process:
1) the sample to be treated washed with alcohol and acetone (roughness requirement: Ra0.4-Ra1.6) is placed in an auxiliary heating device on a cathode of a nitriding furnace, and a sample is placed to ensure that one surface of the sample is right opposite to an observation hole, so that the temperature measurement is convenient. And opening a mechanical pump, vacuumizing to the limit vacuum, filling argon for about five minutes, closing the gas (preventing oxygen in the furnace from reacting with the surface of the sample to generate oxide skin when the temperature is raised and influencing the infiltration effect), and vacuumizing to the limit vacuum.
2) And (3) turning on a nitriding furnace control power supply, slowly increasing the current and the voltage, heating the sample to 900 ℃, and turning on cooling water. Introducing methane, ammonia gas and nitrogen gas in the following proportion: 15:10:75, the air pressure is 80Pa, and the heat preservation time is 8 h.
3) And (5) closing the furnace. And reducing and finally turning off the power supply voltage, cooling the sample to room temperature in the furnace, stopping gas supply, finally turning off the cooling water, and turning off the mechanical pump. Finally, the sample is taken out after the sample is cooled to room temperature.
4) A carbonitrided layer containing TiN and TiC with a thickness of 0.5mm is formed on the surface of the titanium alloy substrate, the hardness reaches more than 1000HV, and the impact toughness can be improved to 60J/cm2The above.
2. Arc ion plating CrTiAlN wear-resistant oxidation-resistant composite coating
The preparation method is characterized in that nitrogen (reaction gas) and argon (protective gas) are introduced into an arc ion plating Cr target (the purity is 99.99%), two Al targets (the purity is 99.99%) and a Ti target (the purity is 99.99%) for preparation.
1) Placing the sample in an ultrasonic container, cleaning the sample for 10 minutes by using an acetone solution, dehydrating and drying the sample, and then placing the sample into a vacuum chamber;
2) glow treatment: background vacuum degree of 5X 10-3Pa, magnetron sputtering power 400W, bias voltage 800V, Ar flow rate 170sccm (standard condition milliliter per minute) for 15min to remove surface oxides and pollutants;
3) transition layer process: base material temperature: 200 ℃, the bias voltage of an arc ion plating substrate is-700V, the target power is 100W, the target base distance is 10cm, the Cr target current is 80A, the Ar flow is 30sccm, and N is2The flow rate is 50 sccm;
4) the preparation process of the working layer comprises the following steps: base material temperature: the substrate bias voltage is-100V at 200 ℃, the current of the arc ion plating Cr target is 65A, the current of the Al target is 60A, and the current of the Ti target is 60A; magnetron sputtering with C target current of 1A, N2The flow rate is 22sccm, the Ar flow rate is 22sccm, the air pressure of the chamber is kept at 2.0Pa, and the coating time is 60 min;
namely, the CrTiAlN wear-resistant and oxidation-resistant composite coating is prepared on the surface of the titanium alloy substrate.
Example 4
A preparation method of a titanium alloy wear-resistant antioxidant composite coating comprises the following steps:
1. gas phase plasma carbonitriding process:
1) the sample to be treated washed with alcohol and acetone (roughness requirement: Ra0.4-Ra1.6) is placed in an auxiliary heating device on a cathode of a nitriding furnace, and a sample is placed to ensure that one surface of the sample is right opposite to an observation hole, so that the temperature measurement is convenient. And opening a mechanical pump, vacuumizing to the limit vacuum, filling argon for about five minutes, closing the gas (preventing oxygen in the furnace from reacting with the surface of the sample to generate oxide skin when the temperature is raised and influencing the infiltration effect), and vacuumizing to the limit vacuum.
2) And (3) turning on a nitriding furnace control power supply, slowly increasing the current and the voltage, heating the sample to 900 ℃, and turning on cooling water. Introducing methane, ammonia gas and nitrogen gas in the following proportion: 15:10:75, the air pressure is 100Pa, and the heat preservation time is 10 h.
3) And (5) closing the furnace. And reducing and finally turning off the power supply voltage, cooling the sample to room temperature in the furnace, stopping gas supply, finally turning off the cooling water, and turning off the mechanical pump. Finally, the sample is taken out after the sample is cooled to room temperature.
4) A carbonitrided layer containing TiN and TiC with a thickness of 1mm is formed on the surface of the titanium alloy substrate, the hardness reaches more than 1000HV, and the impact toughness can be improved to 60J/cm2The above.
2. Arc ion plating CrTiAlN wear-resistant oxidation-resistant composite coating
The preparation method is characterized in that nitrogen (reaction gas) and argon (protective gas) are introduced into an arc ion plating Cr target (the purity is 99.99%), two Al targets (the purity is 99.99%) and a Ti target (the purity is 99.99%) for preparation.
1) Placing the sample in an ultrasonic container, cleaning the sample for 10 minutes by using an acetone solution, dehydrating and drying the sample, and then placing the sample into a vacuum chamber;
2) glow treatment: background vacuum degree of 5X 10-3Cleaning at Pa, bias voltage of-800V and Ar flow rate of 170sccm (standard condition milliliter per minute) for 15min to remove surface oxides and pollutants;
3) transition layer process: base material temperature: 300 ℃, the electric arc ion plating matrix bias voltage is-800V, the target power is 200W, the target base distance is 15cm, the Cr target current is 80A, the Ar flow is 30sccm, and N2The flow rate is 50 sccm;
4) the preparation process of the working layer comprises the following steps: base material temperature: at 300 ℃ and a substrate bias of100V, arc ion plating Cr target current is 65A, Al target current is 60A respectively, and Ti target current is 60A respectively; n is a radical of2The flow rate is 22sccm, the Ar flow rate is 22sccm, the air pressure of the chamber is kept at 2.0Pa, and the coating time is 60 min;
namely, the CrTiAlN wear-resistant and oxidation-resistant composite coating is prepared on the surface of the titanium alloy substrate.
In order to illustrate the relevant performance of the titanium alloy wear-resistant and oxidation-resistant composite coating prepared by the preparation method provided by the invention, only examples 1 to 3 are tested, and the test is shown in the figures 1 to 3.
FIG. 1 is a scanning electron microscope image of the wear-resistant and oxidation-resistant composite coating of titanium alloy provided in example 1; as can be seen from FIG. 1, the density of the plating layer is high, and no agglomeration phenomenon is seen.
FIG. 2 is an XRD (X-ray diffraction) pattern of the wear-resistant and oxidation-resistant composite coating of the titanium alloy provided in examples 1 to 4. As can be seen from FIG. 2, when the XRD phases of the coatings at different voltages are used for preparing the working layers, the obtained coatings form wear-resistant phases such as AlN, CrN, TiN and the like.
FIG. 3 is a graph of the friction coefficient of the titanium alloy wear-resistant and oxidation-resistant composite coating and the titanium alloy substrate provided in example 1; as can be seen from fig. 3, the friction coefficient of the titanium alloy wear-resistant and oxidation-resistant composite coating provided in example 1 is reduced by more than 60% compared with that of the matrix, which indicates that the wear resistance of the coating is significantly improved.
In summary, the preparation method of the titanium alloy wear-resistant oxidation-resistant composite coating provided by the invention comprises the steps of firstly carrying out plasma carbonitriding treatment on the surface of a titanium alloy substrate, and then reacting titanium and nitrogen to form titanium nitride (Ti)2N, TiN) and Ti-N solid solutions. Carbon has a certain solid solubility in titanium, and the reaction of titanium and carbon can produce a hard phase containing TiC and a Ti-C solid solution. The TiN and the TiC are high-hardness phases, and the solid solution strengthening effect of the N, C element is added, so that the TiN and the TiC have better wear resistance, corrosion resistance and high-temperature oxidation resistance than the titanium alloy, the TiN and the TiC containing the high-hardness phases are formed on the surface of the titanium alloy, the advantages of high strength and high toughness of the titanium alloy are kept, the hardness of the surface layer is correspondingly improved, and the improvement of the hardness is very beneficial to the improvement of the wear resistance.
The CrTiAlN coating prepared by adopting the arc ion plating technology has good wear resistance, corrosion resistance and oxidation resistance. Because the physical property difference between the arc ion plating coating and the titanium alloy matrix is large, the hardness of the coating and the matrix is reduced sharply, the elastic modulus is different, stress concentration with different degrees exists at the interface of the coating and the matrix, and the interface is easy to crack and peel due to the existence of the stress at the interface, so that the coating fails. After the titanium alloy is subjected to ion nitrocarburizing treatment, the carburized layer has higher hardness (more than 1000HV) than a titanium alloy matrix, the hardness is gradually reduced from outside to inside, a better supporting effect can be achieved for an ion plating layer, and meanwhile, the fatigue resistance can also be improved. In addition, in the nitriding process, N element is combined with Ti, Al, V and other elements in the titanium alloy matrix to form nitride or nitrogen carbide with the same crystal structure and similar lattice constant as the coating phase. In the subsequent ion plating process, coating phases (AlN, CrN and TiN) are epitaxially grown on the nitrides or the nitride carbides, so that the strain energy of a coating-substrate interface is reduced, and the bonding force between the coating and the substrate is improved; the compound layer has a higher hardness than the diffusion layer, such that the hardness is greater than 2000HV, and provides a stronger support for the ion plating layer. In addition, the compound layer can be used as a phase epitaxy growth nucleation point of the ion plating coating, has high hardness, has a large amount of stacking faults and nanometer twin crystals, and can change the crack propagation direction and improve the toughness of the composite coating through the slip deformation of the stacking faults and the twin crystals.
The present invention describes preferred embodiments and effects thereof. Additional variations and modifications in those embodiments may occur to those skilled in the art once they learn of the basic inventive concepts. Therefore, it is intended that the appended claims be interpreted as including preferred embodiments and all such alterations and modifications as fall within the scope of the invention.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (8)
1. The preparation method of the wear-resistant and oxidation-resistant titanium alloy composite coating is characterized by comprising the following steps of:
s1, placing the pretreated titanium alloy matrix in a vacuum furnace, heating to 900-950 ℃ under a vacuum condition, introducing a mixed gas of methane, ammonia and nitrogen, keeping the air pressure of a chamber at 80-120 Pa, and keeping the temperature for 8-12 h to obtain the titanium alloy matrix with the surface containing the carbonitrided layer;
s2, polishing the obtained titanium alloy matrix containing the carbonitriding layer, plating a transition layer on the polished surface of the titanium alloy matrix by adopting an arc ion plating Cr target under the mixed gas of argon and nitrogen;
and S3, plating a working layer on the surface of the obtained transition layer by adopting an arc ion plating Cr target, an Al target and a Ti target under the mixed gas of nitrogen and argon, namely obtaining the wear-resistant and oxidation-resistant composite coating on the surface of the titanium alloy substrate.
2. The method for preparing the titanium alloy wear-resistant and oxidation-resistant composite coating according to claim 1, wherein in S2, when preparing the transition layer, the temperature of the titanium alloy matrix containing the carbonitrided layer is 200-.
3. The method for preparing the titanium alloy wear-resistant and oxidation-resistant composite coating according to claim 1, wherein in S3, when the working layer is prepared, the temperature of the titanium alloy substrate containing the carbonitrided layer is 200-500 ℃, the bias voltage of the substrate is-100 to-400V, the target current of arc ion plating Cr is 65A, the target current of Al is 60A, and the target current of Ti is 60A; the coating time is 60 min.
4. The method for preparing the titanium alloy wear-resistant and oxidation-resistant composite coating according to claim 3, wherein in S3, the flow ratio of nitrogen to argon is 1:1, and the chamber pressure is 2.0 Pa.
5. The method for preparing the titanium alloy wear-resistant and oxidation-resistant composite coating according to claim 1, wherein in S1, the titanium alloy substrate is pretreated by circularly cleaning the titanium alloy substrate with ethanol and acetone, so that the roughness of the titanium alloy substrate is Ra0.4-1.6.
6. The preparation method of the titanium alloy wear-resistant and oxidation-resistant composite coating according to claim 1, wherein in S1, the ratio of methane to ammonia to nitrogen is 15-20: 5-10: 75.
7. The method for preparing the titanium alloy wear-resistant and oxidation-resistant composite coating according to claim 1, wherein the titanium alloy substrate surface containing the carbonitrided layer is further subjected to glow treatment before a transition layer is prepared, wherein the glow treatment condition is that the vacuum degree is 5 x 10-3Pa, bias voltage of-800V and Ar flow rate of 170sccm, and cleaning for 10-20 min to remove oxides and pollutants on the surface of the titanium alloy matrix containing the carbonitrided layer.
8. The titanium alloy wear-resistant and oxidation-resistant composite coating prepared by the preparation method of any one of claims 1 to 7.
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