CN111136278A - Titanium alloy self-lubricating coating and preparation method thereof - Google Patents
Titanium alloy self-lubricating coating and preparation method thereof Download PDFInfo
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- CN111136278A CN111136278A CN202010002206.3A CN202010002206A CN111136278A CN 111136278 A CN111136278 A CN 111136278A CN 202010002206 A CN202010002206 A CN 202010002206A CN 111136278 A CN111136278 A CN 111136278A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F7/00—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression
- B22F7/02—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite layers
- B22F7/04—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite layers with one or more layers not made from powder, e.g. made from solid metal
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K20/00—Non-electric welding by applying impact or other pressure, with or without the application of heat, e.g. cladding or plating
- B23K20/02—Non-electric welding by applying impact or other pressure, with or without the application of heat, e.g. cladding or plating by means of a press ; Diffusion bonding
- B23K20/023—Thermo-compression bonding
- B23K20/026—Thermo-compression bonding with diffusion of soldering material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K20/00—Non-electric welding by applying impact or other pressure, with or without the application of heat, e.g. cladding or plating
- B23K20/14—Preventing or minimising gas access, or using protective gases or vacuum during welding
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23P—METAL-WORKING NOT OTHERWISE PROVIDED FOR; COMBINED OPERATIONS; UNIVERSAL MACHINE TOOLS
- B23P15/00—Making specific metal objects by operations not covered by a single other subclass or a group in this subclass
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Abstract
The invention relates to a titanium alloy self-lubricating coating and a preparation method thereof, wherein the preparation method comprises the following steps: at least one pure transition metal foil layer and a porous bronze layer are sequentially formed on a titanium alloy substrate, solid lubricant is filled in pores of the porous bronze layer, and the transition metal is selected from one or more of VB and IB group elements. The invention improves the surface defects of titanium alloy surface such as wear resistance, difficult lubrication and the like. The material can greatly prolong the wear-resistant time of the material and reduce the surface friction coefficient of the material.
Description
Technical Field
The invention relates to the technical field of titanium alloy and lubrication, in particular to a titanium alloy self-lubricating coating and a preparation method thereof.
Background
Titanium alloy has the characteristics of low density, high specific strength, high temperature resistance, corrosion resistance and the like, but has the defects of poor frictional wear performance, difficulty in lubrication, low surface hardness and the like, so that the wide application of the titanium alloy is greatly limited. There are many methods for improving the surface performance of titanium alloy, including thermal spraying, nitriding, physical vapor deposition, ion implantation, etc., and the combination of these methods is that the bonding force of thermal spraying is low, nitriding can not improve the surface lubricity of titanium alloy well, the thickness of physical vapor deposition is thin, and the ion implantation lubricating effect is not obvious.
Disclosure of Invention
Aiming at the defects and shortcomings in the prior art, the surface defects of titanium alloy surface such as wear resistance, difficulty in lubrication and the like are improved. The invention provides a titanium alloy self-lubricating coating and a preparation method thereof.
One of the purposes of the invention is to provide a preparation method of a titanium alloy self-lubricating coating, which comprises the following steps: at least one pure transition metal foil layer and a porous bronze layer are sequentially formed on a titanium alloy substrate, solid lubricant is filled in pores of the porous bronze layer, and the transition metal is selected from one or more of VB and IB group elements. The invention improves the surface defects of titanium alloy surface such as wear resistance, difficult lubrication and the like. The material can greatly prolong the wear-resistant time of the material and reduce the surface friction coefficient of the material.
According to some preferred embodiments of the present invention, a titanium alloy substrate is scatter welded to at least one pure transition metal foil, and then a porous bronze layer is powder metallurgically sintered on the pure transition metal foil; preferably, the transition metal is selected from one or more of copper, niobium, vanadium, silver and gold; copper and niobium are preferred. The invention adopts the modes of diffusion welding and powder metallurgy to manufacture a soft metal solid self-lubricating layer on the surface of the titanium alloy. The transition metal and the titanium alloy are combined in the mode, so that the effect of self lubrication is achieved.
According to some preferred embodiments of the present invention, a titanium alloy substrate is welded to a pure niobium foil and a pure copper foil in this order; preferably, the titanium alloy substrate is 1-100 mm, the pure niobium foil is 0.05-0.1 mm, and the pure copper foil is 0.05-0.1 mm; and/or the titanium alloy is TC4 titanium alloy.
According to some preferred embodiments of the present invention, the porous bronze layer is sintered from CuSn8Zn3 powder or CuSn10 powder, and the porosity of the porous bronze layer is 85% to 90%.
According to some preferred embodiments of the invention, the solid lubricant is selected from one or more of PTFE/MoS2, PTFE/BN and PTFE/CaF, preferably a PTFE/MoS2 mixture.
According to some preferred embodiments of the present invention, the method comprises the steps of:
step 2), spot welding and fixing the to-be-connected piece according to the sequence of the pure copper foil, the pure niobium foil and the TC4 titanium alloy;
step 3), welding the to-be-connected piece in the step 2) in a diffusion welding mode;
step 4), sintering a porous bronze layer on the pure copper foil in a powder sintering mode;
and 5) curing and doping PTFE/MoS2 in the porous bronze layer.
According to some preferred embodiments of the present invention, further comprising step 1) material pre-treatment; and/or, step 6) coating homogenization treatment; and/or, step 7) plasticizing and sintering; and/or, step 8) shaping the workpiece; and/or, step 9) finishing.
According to some preferred embodiments of the invention, step 1) material pre-treatment: immersing the titanium alloy substrate into an acetone solution for water bath heat preservation, then carrying out acid cleaning, ultrasonic cleaning and air drying for standby application, wherein the acid cleaning preferably adopts 5% HF + 35% HNO3Acid washing solution; and/or immersing the pure copper foil into an acetone solution, preserving heat in a water bath, then ultrasonically cleaning, and airing for later use; and/or immersing the pure niobium foil into an acetone solution, preserving heat in a water bath, pickling, ultrasonically cleaning, and airing for later use, wherein the pickling is preferably performed by adopting 65% of nitric acid, 95% of sulfuric acid and not less than 40% of hydrofluoric acid in a volume ratio of 5: 5: 2, pickling solution; preferably, the water bath heat preservation conditions are as follows: and (3) preserving the heat in a water bath at 30-50 ℃, preferably 50 ℃, for 10-40 min, preferably 30 min. In the invention, the diffusion welding has high requirements on the surface of the metal to be welded, oxides, organic matters and any other pollutants must be removed, and the surface to be welded must be flat and smooth so as to ensure that the connecting surface is easy to obtain close and uniform contact.
According to some preferred embodiments of the present invention, in step 3), the conditions of the diffusion welding are: and (3) selecting a vacuum diffusion welding furnace, heating to 920-980 ℃ at a speed of 10-30 ℃/min, preferably 20 ℃/min, preferably 950 ℃, preserving heat for 20-60 min for 30min, and preferably 2MPa at a welding pressure of 0.5-5 MPa.
According to some preferred embodiments of the invention, in step 4), the sintering conditions are: sintering in a vacuum sintering furnace at 800-850 ℃, preferably 830 ℃; and/or in the step 5), pouring 20-30 kg of PTFE emulsion preferably with the weight of 25kg and 300-500 g of MoS2 emulsion preferably with the purity of 99.9% into the porous bronze layer, and curing at the temperature of 450-500 ℃ preferably 480 ℃.
The invention also provides a titanium alloy self-lubricating coating prepared by the method.
The invention has the beneficial effects that: the self-lubricating material not only overcomes the characteristic of poor wear resistance of the titanium alloy material, but also can fully utilize the characteristics of light weight, strong corrosion resistance and the like of the titanium alloy, and can be widely used by departments such as civil engineering machinery, aviation rocket technology and the like.
Drawings
Fig. 1 is a gold phase diagram of an optical microscope of a wear-resistant coating provided in example 1 of the present invention (wherein 1-3 correspond to 50 x, 100 x, and 200 x, respectively).
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention are clearly and completely described below, and it is obvious that the described embodiments are a part of the embodiments of the present invention, but not all of the embodiments. The technical solution of the present invention is not limited to the following specific embodiments, and includes any combination of the specific embodiments, and all other embodiments obtained by a person of ordinary skill in the art without creative efforts based on the embodiments of the present invention belong to the protection scope of the present invention.
In the present invention, the specific techniques or conditions not specified in the examples are performed according to the techniques or conditions described in the literature in the art or according to the product specification. The instruments and the like are conventional products which are purchased by normal distributors and are not indicated by manufacturers. The chemical raw materials used in the invention can be conveniently bought in domestic chemical product markets.
Example 1
The embodiment provides a titanium alloy self-lubricating coating, which specifically comprises the following steps:
first, pretreatment of Ti/Cu/Nb material
Immersing TC4 titanium alloy in acetone solution, holding in 50 deg.C water bath for 30min to remove oil, adding 5% HF + 35% HNO3Removing the surface oxide film by using the pickling solution, then putting the pickling solution into deionized water for ultrasonic cleaning, and airing the pickling solution for later use after the ultrasonic cleaning is finished.
Immersing pure copper foil into acetone solution, keeping the temperature in water bath at 50 ℃ for 30min, removing grease, then putting into deionized water for ultrasonic cleaning, and airing for later use after the ultrasonic cleaning is finished.
Immersing the pure niobium foil into an acetone solution, preserving the temperature in a water bath at 50 ℃ for 30min, removing grease, and carrying out treatment on the pure niobium foil with 65% of nitric acid, 95% of sulfuric acid and hydrofluoric acid with the weight ratio of 5: 5: 2, removing the surface oxide film by acid washing, then putting into deionized water for ultrasonic cleaning, and airing for later use after the ultrasonic cleaning is finished.
Second step, fixing of the parts to be connected
Spot welding and fixing the to-be-connected piece according to the following sequence:
0.05mm pure copper foil → 0.05mm pure niobium foil → 10mm TC4 board.
Third, diffusion welding
And (3) selecting a vacuum diffusion welding furnace, heating to 950 ℃ at the speed of 20 ℃/min, preserving the heat for 60min, and welding the pressure to 5 MPa.
Fourth, powder sintering of porous copper
A powder of CuSn10 was selected and the porous bronze layer was sintered in a vacuum sintering furnace at a temperature of 830 c.
Fifthly, solidifying the polytetrafluoroethylene doped with MoS2
25kg of PTFE emulsion was poured into the porous bronze layer, mixed with 300g of MoS2 emulsion of 99.9% purity and cured at 480 ℃. Fig. 1 shows the titanium alloy self-lubricating coating prepared in this example.
Example 2
The embodiment provides a titanium alloy self-lubricating coating, which specifically comprises the following steps:
first, pretreatment of Ti/Cu/Nb material
Immersing TC4 titanium alloy in acetone solution, holding in 50 deg.C water bath for 30min to remove oil, adding 5% HF + 35% HNO3Removing the surface oxide film by using the pickling solution, then putting the pickling solution into deionized water for ultrasonic cleaning, and airing the pickling solution for later use after the ultrasonic cleaning is finished.
Immersing pure copper foil into acetone solution, keeping the temperature in water bath at 50 ℃ for 30min, removing grease, then putting into deionized water for ultrasonic cleaning, and airing for later use after the ultrasonic cleaning is finished.
Immersing the pure niobium foil into an acetone solution, preserving the temperature in a water bath at 50 ℃ for 30min, removing grease, and carrying out treatment on the pure niobium foil with 65% of nitric acid, 95% of sulfuric acid and hydrofluoric acid with the weight ratio of 5: 5: 2, removing the surface oxide film by acid washing, then putting into deionized water for ultrasonic cleaning, and airing for later use after the ultrasonic cleaning is finished.
Second step, fixing of the parts to be connected
Spot welding and fixing the to-be-connected piece according to the following sequence:
0.05mm pure copper foil → 0.05mm pure niobium foil → 4.8mm TC4 board.
Third, diffusion welding
And (3) selecting a vacuum diffusion welding furnace, heating to 1050 ℃ at the speed of 20 ℃/min, preserving the temperature for 30min, and welding the pressure to 5 MPa.
Fourth, powder sintering of porous copper
A powder of CuSn10 was selected and the porous bronze layer was sintered in a vacuum sintering furnace at a temperature of 850 ℃.
Fifthly, solidifying and doping MoS2Of polytetrafluoroethylene (D)
Pouring 25kg of PTFE emulsion into the porous bronze layer to blend 500g of MoS with the purity of 99.9 percent2Emulsion and curing at a temperature of 450 ℃.
Example 3
The embodiment provides a titanium alloy self-lubricating coating, which specifically comprises the following steps:
first, pretreatment of Ti/Cu/Nb material
Immersing TC4 titanium alloy in acetone solution, holding in 50 deg.C water bath for 30min to remove oil, adding 5% HF + 35% HNO3Removing the surface oxide film by using the pickling solution, then putting the pickling solution into deionized water for ultrasonic cleaning, and airing the pickling solution for later use after the ultrasonic cleaning is finished.
Immersing pure copper foil into acetone solution, keeping the temperature in water bath at 50 ℃ for 30min, removing grease, then putting into deionized water for ultrasonic cleaning, and airing for later use after the ultrasonic cleaning is finished.
Immersing the pure niobium foil into an acetone solution, preserving the temperature in a water bath at 50 ℃ for 30min, removing grease, and carrying out treatment on the pure niobium foil with 65% of nitric acid, 95% of sulfuric acid and hydrofluoric acid with the weight ratio of 5: 5: 2, removing the surface oxide film by acid washing, then putting into deionized water for ultrasonic cleaning, and airing for later use after the ultrasonic cleaning is finished.
Second step, fixing of the parts to be connected
Spot welding and fixing the to-be-connected piece according to the following sequence:
0.05mm pure copper foil → 0.05mm pure niobium foil → 20mm TC4 board.
Third, diffusion welding
And (3) selecting a vacuum diffusion welding furnace, heating to 950 ℃ at the speed of 20 ℃/min, preserving the temperature for 30min, and welding the pressure to 10 MPa.
Fourth, powder sintering of porous copper
A powder of CuSn10 was selected and the porous bronze layer was sintered in a vacuum sintering furnace at a temperature of 830 c.
Fifthly, solidifying the polytetrafluoroethylene doped with MoS2
Pouring 25kg of PTFE emulsion into the porous bronze layer to blend 300g of MoS with the purity of 99.9 percent2Emulsion and curing at 480 ℃.
Although the invention has been described in detail hereinabove with respect to a general description and specific embodiments thereof, it will be apparent to those skilled in the art that modifications or improvements may be made thereto based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.
Claims (10)
1. The preparation method of the titanium alloy self-lubricating coating is characterized by comprising the following steps of: at least one pure transition metal foil layer and a porous bronze layer are sequentially formed on a titanium alloy substrate, solid lubricant is filled in pores of the porous bronze layer, and the transition metal is selected from one or more of VB and IB group elements.
2. The method of claim 1, wherein a titanium alloy substrate is scatter welded to at least one pure transition metal foil, and then a porous bronze layer is powder metallurgically sintered on the pure transition metal foil; preferably, the transition metal is selected from one or more of copper, niobium, vanadium, silver and gold; copper and niobium are preferred.
3. The method according to claim 1 or 2, wherein a titanium alloy substrate is welded with a pure niobium foil and a pure copper foil in this order; preferably, the titanium alloy substrate is 1-100 mm, the pure niobium foil is 0.05-0.1 mm, and the pure copper foil is 0.05-0.1 mm; and/or the titanium alloy is TC4 titanium alloy.
4. The method according to any one of claims 1 to 3, wherein the porous bronze layer is sintered from CuSn8Zn3 powder or CuSn10 powder, and has a porosity of 85% to 90%.
5. Method according to any of claims 1-4, wherein the solid lubricant is selected from one or more of PTFE/MoS2, PTFE/BN and PTFE/CaF, preferably a PTFE/MoS2 mixture.
6. Method according to any of claims 1-5, characterized in that it comprises the steps of:
step 2), spot welding and fixing the to-be-connected piece according to the sequence of the pure copper foil, the pure niobium foil and the TC4 titanium alloy;
step 3), welding the to-be-connected piece in the step 2) in a diffusion welding mode;
step 4), sintering a porous bronze layer on the pure copper foil in a powder sintering mode;
and 5) curing and doping PTFE/MoS2 in the porous bronze layer.
7. The method of claim 6, further comprising the steps of 1) pre-treating the material; and/or, step 6) coating homogenization treatment; and/or, step 7) plasticizing and sintering; and/or, step 8) shaping the workpiece; and/or, step 9) finishing;
preferably, the material pretreatment in the step 1): immersing the titanium alloy substrate into an acetone solution for water bath heat preservation, then carrying out acid washing, ultrasonic cleaning and air drying for later use, wherein the acid washing preferably adopts 5% HF + 35% HNO3 acid washing liquid; and/or immersing the pure copper foil into an acetone solution, preserving heat in a water bath, then ultrasonically cleaning, and airing for later use; and/or immersing the pure niobium foil into an acetone solution, preserving heat in a water bath, pickling, ultrasonically cleaning, and airing for later use, wherein the pickling is preferably performed by adopting 65% of nitric acid, 95% of sulfuric acid and not less than 40% of hydrofluoric acid in a volume ratio of 5: 5: 2, pickling solution; preferably, the water bath heat preservation conditions are as follows: and (3) preserving the heat in a water bath at 30-50 ℃, preferably 50 ℃, for 10-40 min, preferably 30 min.
8. The method according to claim 4, wherein in step 3), the conditions of the diffusion welding are as follows: and (3) selecting a vacuum diffusion welding furnace, heating to 920-980 ℃ at a speed of 10-30 ℃/min, preferably 20 ℃/min, preferably 950 ℃, preserving heat for 20-60 min for 30min, and preferably 2MPa at a welding pressure of 0.5-5 MPa.
9. The method according to claim 4, wherein in step 4), the sintering conditions are as follows: sintering in a vacuum sintering furnace at 800-850 ℃, preferably 830 ℃; and/or in the step 5), pouring 20-30 kg of PTFE emulsion preferably with the weight of 25kg and 300-500 g of MoS2 emulsion preferably with the purity of 99.9% into the porous bronze layer, and curing at the temperature of 450-500 ℃ preferably 480 ℃.
10. A titanium alloy self-lubricating coating prepared according to the method of any one of claims 1 to 9.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113787311A (en) * | 2021-09-14 | 2021-12-14 | 南通市荣泰电化学设备制造有限公司 | Preparation process of titanium polar plate with firmly-adhered coating |
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| CN113787311A (en) * | 2021-09-14 | 2021-12-14 | 南通市荣泰电化学设备制造有限公司 | Preparation process of titanium polar plate with firmly-adhered coating |
| CN113787311B (en) * | 2021-09-14 | 2022-03-18 | 南通市荣泰电化学设备制造有限公司 | Preparation process of titanium polar plate with firmly-adhered coating |
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