CN108914187A - A kind of anti-oxidant complex gradient ceramic coating of titanium alloy surface high hardness wear-resisting and preparation method thereof - Google Patents
A kind of anti-oxidant complex gradient ceramic coating of titanium alloy surface high hardness wear-resisting and preparation method thereof Download PDFInfo
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- CN108914187A CN108914187A CN201810804475.4A CN201810804475A CN108914187A CN 108914187 A CN108914187 A CN 108914187A CN 201810804475 A CN201810804475 A CN 201810804475A CN 108914187 A CN108914187 A CN 108914187A
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/026—Anodisation with spark discharge
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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
- C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
- C23C28/04—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings of inorganic non-metallic material
- C23C28/042—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings of inorganic non-metallic material including a refractory ceramic layer, e.g. refractory metal oxides, ZrO2, rare earth oxides
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/26—Anodisation of refractory metals or alloys based thereon
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Abstract
The invention discloses anti-oxidant complex gradient ceramic coatings of a kind of titanium alloy surface high hardness wear-resisting and preparation method thereof.Wear-resisting anti-oxidant complex gradient ceramic coating is with the TC of high tenacity4Titanium alloy is as basis material, Al2O3Ceramic layer is as transition zone, SiO2As sealing of hole particle and top ceramic layer.This method includes：Pre-treatment, differential arc oxidation, sol-gal process.The present invention can prepare the wear-resistant coating of high rigidity by differential arc oxidation, then by sol-gal process sealing pores, prepared coating binding force is good, compact structure, multi-component ceramics, TiO2、Al2O3And SiO2, the limitation of one-component or bi-component is overcome, the wear-resistant and antioxygenic property of coating is improved.
Description
Technical field
The invention belongs to titanium alloy Microarc Oxidation Surface Treatment technical fields, are related to titanium alloy surface modification, specifically
It is related to a kind of anti-oxidant complex gradient ceramic coating of titanium alloy surface high hardness wear-resisting and preparation method thereof.
Background technique
Titanium alloy is since its density is small, and specific strength is high, good corrosion resistance, sends out at present in aerospace and automobile ship domain
Wave important function.However titanium alloy hardness is low, wears no resistance, oxidizable disadvantage, limits titanium alloy under high temperature environment
Extensive use.Titanium alloy surface coating processing is feasible solution.The method of traditional coating processing has plasma spraying, anodic oxygen
Change, chemical conversion and magnetron sputtering etc., these coating methods can improve to a certain extent the hardness of titanium alloy surface to improve
Wearability, but the hardness wearability that comprehensive can not have not only improved titanium alloy, but also improve its high temperature oxidation resistance.
Differential arc oxidization technique is widely used titanium alloy surface processing technique in recent years, easy to operate, high-efficient, coating
It is good with the set performance of matrix.By the micro-arc oxidation process of optimization, the resistance to of high rigidity can be prepared in titanium alloy surface
Ceramic coating is ground, but has its free defect in process aspect.Ceramic coating formed by micro-arc oxidation inevitably porous structure, electric discharge
Micro channel continues up to matrix surface from coating, this makes the high temperature resistant property of micro-arc oxidation films be difficult to meet complicated ring
Border.So it is quite important to be sealed processing to the gap of oxidation film.
Sol-gal process is exactly to make presoma with the compound containing high chemical active ingredient, under liquid phase that these raw materials are equal
Even mixing, and be hydrolyzed, be condensed chemical reaction, stable vitreosol system, the aged micelle of colloidal sol are formed in the solution
Between slowly polymerize, form the gel of three-dimensional net structure, be filled with the solvent to lose flowability between gel network, form gel.
Gel prepares the material of molecule or even nanometer substructure by dry, sintering curing.The process equipment is simple, low in cost,
Process is easy to control, can form nano particle in the gap of differential arc oxidation oxidation film, and then improve the defect of micro-arc oxidation films, answer
It is extensive with prospect.
The research and preparation of current titanium-alloy surface micro-arc oxidation film have the following problems：(1) titanium alloy surface coating is resistance to
It is poor to grind performance, wear rate is high.(2) oxidation resistance of coating is weak, it is difficult to meet the harsh use environment of high temperature.
Summary of the invention
The present invention is for hard low and high-temperature oxidation resistance difference the problem of titanium alloy surface, a kind of titanium alloy surface high rigidity
Wear-resisting anti-oxidant complex gradient ceramic coating and preparation method thereof.
Technical scheme is as follows：
A kind of anti-oxidant composite ceramic coat of titanium alloy surface high hardness wear-resisting and preparation method thereof,
Complex gradient ceramic coating includes TC4Titanium alloy is as basis material, Al2O3As ceramic interlayer, SiO2Make
For sealing of hole particle and outer layer.The preparation method includes pre-treatment, differential arc oxidation, sol-gal process.
Specific step is as follows：
Step 1, pre-treatment：Titanium alloy sheet material is polished, is cleaned by ultrasonic, it is dry；
Step 2, differential arc oxidation：In sodium aluminate-sodium phosphate electrolyte system, titanium alloy sheet material that step 1 is obtained into
Row micro-arc oxidation treatment, sodium aluminate mass concentration are 15g/L, and sodium phosphate mass concentration is 1.6g/L, and electrolyte PH is 12；
Step 3, SiO is configured2Colloidal sol, raw material use ethyl orthosilicate, hydrochloric acid, polyvinyl alcohol and dehydrated alcohol, configure SiO2
Colloidal sol；First ethyl orthosilicate is mixed in molar ratio with dehydrated alcohol, and is slowly added to appropriate amount of deionized water under stirring,
Then appropriate hydrochloric acid is added dropwise, continues stirring to solution viscosity and increases.
Step 4, the titanium alloy sheet material that step 2 obtains is put into the colloidal sol that step 3 obtains pulling film forming and quiet at room temperature
It sets for 24 hours, is then dried in vacuo at 60~80 DEG C.Coating needed for finally successively sintering is made at different temperatures.
Preferably, in step 2, micro-arc oxidation process parameter is 400~600V of voltage, duty ratio 40%, electrolyte temperature
Degree is 20 DEG C, handles 15~30min of time.
Preferably, in step 3, SiO is configured2In colloidal sol, the ratio of ethyl orthosilicate and dehydrated alcohol is 1:20~30, PH
Value is 2, and the molar ratio of ethyl orthosilicate and deionized water is 1:4.
Preferably, in step 4, the speed of pulling film forming is that 2~6cm/min can be repeated multiple times to meet different thickness
Lifting.Sintering temperature is followed successively by 100 DEG C, and 300 DEG C, 600 DEG C, sintering time is 1h.
Compared with prior art, the present invention has following remarkable advantage：
(1) sealing pores are carried out to differential arc oxidation layer by sol-gal process, the composite coating structure that can be is fine and close, antioxygen
Change ability is outstanding.
(2) multicomponent ceramics TiO2、Al2O3And SiO2It combines, overcomes the limitation of one-component, improve coating
Wear-resistant and antioxygenic property.
(3) present invention is low in cost, wear-resistant oxidation resistant coating can be prepared on complex component, not by Components Shape
Limitation.
Detailed description of the invention
Fig. 1 is present invention oxidation curve synoptic diagram.
Fig. 2 is the hardness of high hardness wear-resisting coating and the hardness schematic diagram of uncoated matrix.
Specific embodiment
Below with reference to embodiment and attached drawing, the invention will be further described.
Embodiment 1
(1) titanium alloy sheet material successively is polished to smooth, so using the sand paper of 120 mesh, 200 mesh, 400 mesh, 600 mesh, 800 mesh
It with alcohol wash clean and dries up afterwards；Then it is polished to specimen surface no marking.
(2) in supersonic cleaning machine, 10min is cleaned by ultrasonic under alcoholic environment, the greasy dirt of surface remaining is removed, then does
It is dry stand-by.
(3) electrolyte, sodium aluminate content 15g/L are configured, phosphoric acid sodium content is 1.6g/L, and sodium hydroxide is added to electrolyte
PH is 12.Titanium alloy piece is in anode, and stainless steel sink is as cathode.The technological parameter of differential arc oxidation is voltage 400V, duty ratio
It is 40%, electrolyte temperature is 20 DEG C, and the processing time is 30min.
(4) raw material uses ethyl orthosilicate, hydrochloric acid, polyvinyl alcohol and dehydrated alcohol, configures SiO2Colloidal sol.First by positive silicic acid
Ethyl ester and dehydrated alcohol in molar ratio 1:20 mixing, and it is slowly added to appropriate amount of deionized water under stirring, wherein positive silicic acid
Ethyl ester and deionized water ratio are 1:4, it is 2 that appropriate hydrochloric acid, which is then added dropwise, to PH, continues stirring to solution viscosity and increases.
(5) the titanium alloy sheet material that step 2 obtains is put into pulling film forming in the colloidal sol that step 4 obtains, the speed of pulling film forming
It for 2cm/min, and stands for 24 hours, is then dried in vacuo at 60 DEG C at room temperature.Then under protection of argon gas, it is heat-treated.
100 DEG C first are warming up to by the speed of 10 DEG C/min, keeps the temperature 1h；300 DEG C are warming up to by the speed of 10 DEG C/min again, keeps the temperature 1h；Most
After be warming up to 600 DEG C, keep the temperature 1h.
Embodiment 2
(1) titanium alloy sheet material successively is polished to smooth, so using the sand paper of 120 mesh, 200 mesh, 400 mesh, 600 mesh, 800 mesh
It with alcohol wash clean and dries up afterwards；Then it is polished to specimen surface no marking.
(2) in supersonic cleaning machine, 10min is cleaned by ultrasonic under alcoholic environment, the greasy dirt of surface remaining is removed, then does
It is dry stand-by.
(3) electrolyte, sodium aluminate content 15g/L are configured, phosphoric acid sodium content is 1.6g/L, and sodium hydroxide is added to electrolyte
PH is 12.Titanium alloy piece is in anode, and stainless steel sink is as cathode.The technological parameter of differential arc oxidation is voltage 500V, duty ratio
It is 40%, electrolyte temperature is 20 DEG C, and the processing time is 20min.
(4) raw material uses ethyl orthosilicate, hydrochloric acid, polyvinyl alcohol and dehydrated alcohol, configures SiO2Colloidal sol.First by positive silicic acid
Ethyl ester and dehydrated alcohol in molar ratio 1:25 mixing, and it is slowly added to appropriate amount of deionized water under stirring, wherein positive silicic acid
Ethyl ester and deionized water ratio are 1:4, it is 2 that appropriate hydrochloric acid, which is then added dropwise, to PH, continues stirring to solution viscosity and increases.
(5) the titanium alloy sheet material that step 2 obtains is put into pulling film forming in the colloidal sol that step 4 obtains, the speed of pulling film forming
It for 4cm/min, and stands for 24 hours, is then dried in vacuo at 60 DEG C at room temperature.Then under protection of argon gas, it is heat-treated.
100 DEG C first are warming up to by the speed of 10 DEG C/min, keeps the temperature 1h；300 DEG C are warming up to by the speed of 10 DEG C/min again, keeps the temperature 1h；Most
After be warming up to 600 DEG C, keep the temperature 1h.
After embodiment 2,10h is heated at 700 DEG C, then cools down and weighs in air, is then reentered into 700 DEG C
It in heating furnace, so recycles, adds up heating 100h, measure oxidation curve shown in FIG. 1, from Fig. 1 this it appears that coating
Antioxygenic property has very big promotion.
After embodiment 2, microhardness testers measure the hardness of coating and matrix, as shown in Figure 2.
Embodiment 3
(1) titanium alloy sheet material successively is polished to smooth, so using the sand paper of 120 mesh, 200 mesh, 400 mesh, 600 mesh, 800 mesh
It with alcohol wash clean and dries up afterwards；Then it is polished to specimen surface no marking.
(2) in supersonic cleaning machine, 10min is cleaned by ultrasonic under alcoholic environment, the greasy dirt of surface remaining is removed, then does
It is dry stand-by.
(3) electrolyte, sodium aluminate content 15g/L are configured, phosphoric acid sodium content is 1.6g/L, and sodium hydroxide is added to electrolyte
PH is 12.Titanium alloy piece is in anode, and stainless steel sink is as cathode.The technological parameter of differential arc oxidation is voltage 600V, duty ratio
It is 40%, electrolyte temperature is 20 DEG C, and the processing time is 15min.
(4) raw material uses ethyl orthosilicate, hydrochloric acid, polyvinyl alcohol and dehydrated alcohol, configures SiO2Colloidal sol.First by positive silicic acid
Ethyl ester and dehydrated alcohol in molar ratio 1:30 mixing, and it is slowly added to appropriate amount of deionized water under stirring, wherein positive silicic acid
Ethyl ester and deionized water ratio are 1:4, it is 2 that appropriate hydrochloric acid, which is then added dropwise, to PH, continues stirring to solution viscosity and increases.
(5) the titanium alloy sheet material that step 2 obtains is put into pulling film forming in the colloidal sol that step 4 obtains, the speed of pulling film forming
It for 6cm/min, and stands for 24 hours, is then dried in vacuo at 60 DEG C at room temperature.Then under protection of argon gas, it is heat-treated.
100 DEG C first are warming up to by the speed of 10 DEG C/min, keeps the temperature 1h；300 DEG C are warming up to by the speed of 10 DEG C/min again, keeps the temperature 1h；Most
600 DEG C are warming up to by the speed of 10 DEG C/min afterwards, keeps the temperature 1h.
Claims (6)
1. a kind of anti-oxidant complex gradient ceramic coating of titanium alloy surface high hardness wear-resisting, which is characterized in that the coating is
It is made up of：The micro-arc oxidation films of wear-resisting supporting role and the nano ceramics for playing sealing of hole for filling micro-arc oxidation films hole
Particle.
2. the anti-oxidant complex gradient ceramic coating of titanium alloy surface high hardness wear-resisting as described in claim 1, which is characterized in that multiple
It closes in gradient ceramic coating, the main component of micro-arc oxidation films is Al2O3, submember is TiO2And Al2TiO5, fill hole
Nano-ceramic particle is SiO2。
3. a kind of preparation method of the anti-oxidant complex gradient ceramic coating of titanium alloy surface high hardness wear-resisting, which is characterized in that should
Method the specific steps are：
Step 1, pre-treatment：Titanium alloy sheet material is polished, is cleaned by ultrasonic, it is dry；
Step 2, differential arc oxidation：In sodium aluminate-sodium phosphate electrolyte system, the titanium alloy sheet material that step 1 obtains is carried out micro-
Arc oxidation processes, sodium aluminate mass concentration are 15g/L, and sodium phosphate mass concentration is 1.6g/L, and electrolyte PH is 12；
Step 3, SiO is configured2Colloidal sol is mixed using raw material ethyl orthosilicate, hydrochloric acid, polyvinyl alcohol and dehydrated alcohol, is configured to
SiO2Colloidal sol；Ethyl orthosilicate is mixed with dehydrated alcohol again, and is slowly added to deionized water under stirring, is then added dropwise
Hydrochloric acid continues stirring to solution viscosity and increases；
Step 4, the titanium alloy sheet material that step 2 obtains is put into pulling film forming in the colloidal sol that step 3 obtains and stood at room temperature
For 24 hours, it is then dried in vacuo at 60~80 DEG C；Coating needed for finally successively sintering is made at different temperatures.
4. preparation method as claimed in claim 3, which is characterized in that in step 2, micro-arc oxidation process parameter is voltage 400
~600V, duty ratio 40%, electrolyte temperature are 20 DEG C, handle 15~30min of time.
5. preparation method as claimed in claim 3, which is characterized in that in step 3, configure SiO2In colloidal sol, ethyl orthosilicate and
The molar ratio of dehydrated alcohol is 1:20~30, pH value 2, the molar ratio of ethyl orthosilicate and deionized water is 1:4.
6. preparation method as claimed in claim 3, which is characterized in that in step 4, the speed of pulling film forming is 2~6cm/
Min repeated multiple times can lift to meet different thickness；Sintering temperature is followed successively by 100 DEG C, and 300 DEG C, 600 DEG C, sintering time
It is 1h.
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Cited By (7)
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| CN109137036A (en) * | 2018-11-26 | 2019-01-04 | 南京理工大学 | A kind of composite coating and preparation method thereof of titanium alloy surface ceramic layer grafting hydrogel |
| CN111041538A (en) * | 2019-12-25 | 2020-04-21 | 八龙应用材料科技(海南)有限公司 | Preparation method of non-ferrous alloy anticorrosive coating |
| WO2020190251A1 (en) * | 2019-03-20 | 2020-09-24 | Олександр Анатолийовыч САМОЙЛЕНКО | Antibacterial ceramic coating and method for coating titanium alloy implants |
| CN112481675A (en) * | 2020-11-27 | 2021-03-12 | 佳木斯大学 | Preparation method of pure titanium surface double-layer protective film layer |
| CN113089047A (en) * | 2021-04-12 | 2021-07-09 | 四川九洲电器集团有限责任公司 | Aluminum alloy component and preparation method and application thereof |
| CN115106532A (en) * | 2022-07-04 | 2022-09-27 | 浙江兰欣复合材料科技有限公司 | Metal base material containing wear-resistant coating and preparation method thereof |
| CN115521707A (en) * | 2022-09-21 | 2022-12-27 | 宁波虔宁特种合金有限公司 | Copper roller coating of strip casting furnace and preparation method thereof |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109137036A (en) * | 2018-11-26 | 2019-01-04 | 南京理工大学 | A kind of composite coating and preparation method thereof of titanium alloy surface ceramic layer grafting hydrogel |
| WO2020190251A1 (en) * | 2019-03-20 | 2020-09-24 | Олександр Анатолийовыч САМОЙЛЕНКО | Antibacterial ceramic coating and method for coating titanium alloy implants |
| CN111041538A (en) * | 2019-12-25 | 2020-04-21 | 八龙应用材料科技(海南)有限公司 | Preparation method of non-ferrous alloy anticorrosive coating |
| CN112481675A (en) * | 2020-11-27 | 2021-03-12 | 佳木斯大学 | Preparation method of pure titanium surface double-layer protective film layer |
| CN112481675B (en) * | 2020-11-27 | 2022-03-11 | 佳木斯大学 | Preparation method of pure titanium surface double-layer protective film layer |
| CN113089047A (en) * | 2021-04-12 | 2021-07-09 | 四川九洲电器集团有限责任公司 | Aluminum alloy component and preparation method and application thereof |
| CN115106532A (en) * | 2022-07-04 | 2022-09-27 | 浙江兰欣复合材料科技有限公司 | Metal base material containing wear-resistant coating and preparation method thereof |
| CN115521707A (en) * | 2022-09-21 | 2022-12-27 | 宁波虔宁特种合金有限公司 | Copper roller coating of strip casting furnace and preparation method thereof |
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