CN106011971B - A kind of method in preparing ceramic film on titanium alloy surface/glaze film composite coating - Google Patents
A kind of method in preparing ceramic film on titanium alloy surface/glaze film composite coating Download PDFInfo
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- CN106011971B CN106011971B CN201610364730.9A CN201610364730A CN106011971B CN 106011971 B CN106011971 B CN 106011971B CN 201610364730 A CN201610364730 A CN 201610364730A CN 106011971 B CN106011971 B CN 106011971B
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- 229910001069 Ti alloy Inorganic materials 0.000 title claims abstract description 51
- 239000011248 coating agent Substances 0.000 title claims abstract description 32
- 238000000576 coating method Methods 0.000 title claims abstract description 32
- 238000000034 method Methods 0.000 title claims abstract description 26
- 239000000919 ceramic Substances 0.000 title claims abstract description 19
- 239000002131 composite material Substances 0.000 title claims abstract description 15
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 29
- 230000003647 oxidation Effects 0.000 claims abstract description 27
- 238000005524 ceramic coating Methods 0.000 claims abstract description 12
- 239000012528 membrane Substances 0.000 claims abstract description 6
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 19
- 239000000203 mixture Substances 0.000 claims description 14
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 238000005498 polishing Methods 0.000 claims description 10
- 229910045601 alloy Inorganic materials 0.000 claims description 9
- 239000000956 alloy Substances 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 7
- 229910052574 oxide ceramic Inorganic materials 0.000 claims description 7
- 239000011224 oxide ceramic Substances 0.000 claims description 7
- 238000012545 processing Methods 0.000 claims description 7
- 229910000883 Ti6Al4V Inorganic materials 0.000 claims description 6
- 239000003792 electrolyte Substances 0.000 claims description 6
- 238000009413 insulation Methods 0.000 claims description 6
- 244000137852 Petrea volubilis Species 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 239000004744 fabric Substances 0.000 claims description 5
- KKCBUQHMOMHUOY-UHFFFAOYSA-N Na2O Inorganic materials [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 claims description 4
- 229910052681 coesite Inorganic materials 0.000 claims description 4
- 229910052593 corundum Inorganic materials 0.000 claims description 4
- 229910052906 cristobalite Inorganic materials 0.000 claims description 4
- 239000000377 silicon dioxide Substances 0.000 claims description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 4
- 239000001509 sodium citrate Substances 0.000 claims description 4
- 235000011083 sodium citrates Nutrition 0.000 claims description 4
- 239000002904 solvent Substances 0.000 claims description 4
- 229910052682 stishovite Inorganic materials 0.000 claims description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 4
- 229910052905 tridymite Inorganic materials 0.000 claims description 4
- HRXKRNGNAMMEHJ-UHFFFAOYSA-K trisodium citrate Chemical class [Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O HRXKRNGNAMMEHJ-UHFFFAOYSA-K 0.000 claims description 4
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 claims description 4
- 229910000406 trisodium phosphate Inorganic materials 0.000 claims description 4
- 229910001845 yogo sapphire Inorganic materials 0.000 claims description 4
- 238000002203 pretreatment Methods 0.000 claims description 3
- 239000011734 sodium Substances 0.000 claims description 2
- 229910052911 sodium silicate Inorganic materials 0.000 claims description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims 1
- 238000002242 deionisation method Methods 0.000 claims 1
- 229910052760 oxygen Inorganic materials 0.000 claims 1
- 239000001301 oxygen Substances 0.000 claims 1
- 238000006213 oxygenation reaction Methods 0.000 claims 1
- 238000005516 engineering process Methods 0.000 abstract description 11
- 239000011159 matrix material Substances 0.000 abstract description 10
- 230000007797 corrosion Effects 0.000 abstract description 8
- 238000005260 corrosion Methods 0.000 abstract description 8
- 239000000758 substrate Substances 0.000 abstract description 5
- 230000001681 protective effect Effects 0.000 abstract description 3
- 238000007789 sealing Methods 0.000 abstract description 2
- 238000005245 sintering Methods 0.000 abstract 1
- 239000010936 titanium Substances 0.000 description 15
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 14
- 229910052719 titanium Inorganic materials 0.000 description 13
- 229910052751 metal Inorganic materials 0.000 description 6
- 239000002184 metal Substances 0.000 description 6
- 238000007745 plasma electrolytic oxidation reaction Methods 0.000 description 5
- 238000002360 preparation method Methods 0.000 description 5
- 238000005507 spraying Methods 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 230000007547 defect Effects 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- 239000005995 Aluminium silicate Substances 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 238000013019 agitation Methods 0.000 description 2
- 235000012211 aluminium silicate Nutrition 0.000 description 2
- 238000005255 carburizing Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 238000010422 painting Methods 0.000 description 2
- 238000010791 quenching Methods 0.000 description 2
- 230000000171 quenching effect Effects 0.000 description 2
- 238000004381 surface treatment Methods 0.000 description 2
- 238000012876 topography Methods 0.000 description 2
- 238000004506 ultrasonic cleaning Methods 0.000 description 2
- 229910001040 Beta-titanium Inorganic materials 0.000 description 1
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- ORILYTVJVMAKLC-UHFFFAOYSA-N adamantane Chemical compound C1C(C2)CC3CC1CC2C3 ORILYTVJVMAKLC-UHFFFAOYSA-N 0.000 description 1
- 229910001573 adamantine Inorganic materials 0.000 description 1
- 238000005275 alloying Methods 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 238000005271 boronizing Methods 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000000498 cooling water Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000010894 electron beam technology Methods 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000007943 implant Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 238000005121 nitriding Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 238000007750 plasma spraying Methods 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 238000007634 remodeling Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 230000003746 surface roughness Effects 0.000 description 1
Classifications
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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
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C8/00—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
- C03C8/02—Frit compositions, i.e. in a powdered or comminuted form
- C03C8/10—Frit compositions, i.e. in a powdered or comminuted form containing lead
- C03C8/12—Frit compositions, i.e. in a powdered or comminuted form containing lead containing titanium or zirconium
-
- 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
-
- 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
- C23D—ENAMELLING OF, OR APPLYING A VITREOUS LAYER TO, METALS
- C23D3/00—Chemical treatment of the metal surfaces prior to coating
-
- 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
- C23D—ENAMELLING OF, OR APPLYING A VITREOUS LAYER TO, METALS
- C23D5/00—Coating with enamels or vitreous layers
- C23D5/02—Coating with enamels or vitreous layers by wet methods
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Metallurgy (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Mechanical Engineering (AREA)
- General Chemical & Material Sciences (AREA)
- Ceramic Engineering (AREA)
- Inorganic Chemistry (AREA)
- Electrochemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Other Surface Treatments For Metallic Materials (AREA)
- Coating By Spraying Or Casting (AREA)
Abstract
The present invention relates to a kind of method in preparing ceramic film on titanium alloy surface/glaze film composite coating, ceramic coating is prepared in matrix surface using differential arc oxidization technique first on titanium alloy, then prepares composite coating then at ceramic surface glazing sealing of hole and sintering.The present invention wants to combine using differential arc oxidation (MAO) technology and surface glazing technology prepares ceramic membrane/glaze film composite coating to improve matrix surface hardness, wearability and the thermal stability of high temperature, and the film-substrate cohesion of coating is good；Since ceramics and glaze layer have high rigidity and high consistency, so as to improve the wearability and corrosion resistance of titanium alloy.This method is environmentally protective, and equipment requirement is low, easy to operate, and cost is low.
Description
(1) technical field
The present invention relates to a kind of method in preparing ceramic film on titanium alloy surface/glaze film composite coating.
(2) background technology
Titanium and its alloy have that relative density is small, specific strength is located at first of metal, elasticity modulus is about the spies such as the half of steel
Property.And titanium can the long-time service at a temperature of 600 DEG C of even more highs, while it is with anti-resistance to low temperature, subzero 196
Preferable ductility and toughness can be kept under~253 DEG C of low temperature environment so as to avoid the cold brittleness of metal.In addition, titanium is also
There is no magnetic, nontoxic, environmentally safe.Therefore, titanium and its alloy are widely used in aerospace, ship, change
The fields such as medical equipment and Implant in terms of work, medicine, are known as " spatial metal ", " marine metal ".
Titanium alloy principle：As isomer, titanium structure can change at different temperatures, be less than when titanium is in
When under 882 DEG C of environment, it is rendered as close-packed hexagonal lattice structure, and the titanium of this structure is known as α-titanium；And when titanium is at 882 DEG C
When under environment above, it is rendered as body-centered cubic lattic structure, and the titanium of this structure is known as β-titanium.Ti6Al4V is resistance to due to its
Hot, intensity, plasticity, toughness, formability, solderability, corrosion resistance and biocompatibility are preferable, become first practical titanium
Alloy, the trump alloy being known as in titanium alloy industry.The alloy usage amount has accounted for the 75%~85% of whole titanium alloys.Other are permitted
More titanium alloys can be regarded as the remodeling of Ti6Al4V alloys.China starts the large-scale production of titanium and titanium alloy related industries
Have more than 50 years, ranked among the fifth-largest Ti industry producing country at present.In view of the comprehensive performance that titanium alloy is excellent, it may
As " the 3rd metal " to emerge after iron, aluminium.
Titanium or titanium alloy has an above-mentioned series of advantages, but its also there is such as：Case hardness is low, wear-resisting property is poor
The problems such as, it is difficult to the requirement for meeting produce reality application under many circumstances.Therefore, titanium alloy surface prepare have it is wear-resisting,
The research of corrosion resistance coating is very urgent.Wherein most importantly using surface strengthening technology to titanium or titanium alloy surface into
Row optimization.At present in all kinds of methods of metallic surface processing, the overwhelming majority has had application to the surface treatment of titanium alloy
On, including carburizing (nitrogen, boron), metal plating, anodic oxidation, differential arc oxidation, ionic nitriding, vacuum electron beam surface treatment, swash
Optical surface processing plasma spraying etc..
While the process for treating surface of above-mentioned titanium or titanium alloy contains respective advantage, also there is it is obvious the defects of.
Such as：The means such as carburizing tech, boronizing technology and nitridation technique there are long processing period and workpiece it is yielding the problems such as；Thermal jet
Coating texture prepared by painting technology is loose and the combination power of coating and matrix is weaker；The high energy beams such as laser surface alloying
The method for employing local heat treatment is heat-treated, although overcoming the shortcomings that thermo-chemical treatment is integrally heated, in actual life
Production use in occasionally there are alloyed layer out-of-flatness and with matrix intersection it is cracked, empty the defects of.It is most important
It is that these above-mentioned method costs are higher, rest on laboratory stage mostly, the mass market being unfavorable for truly is promoted
Using.Therefore, it is necessary to study the method for efficient and cost-effective effectively to be protected titanium or titanium alloy, it is wear-resisting resistance to improve its
Corrosive nature is so that it meets the requirement of practical application.
(3) content of the invention
It is an object of the invention to overcome existing titanium alloy surface coating technology defect, there is provided one kind improves titanium alloy table
The preparation method of the coating of finishing coat performance.The thermal stability of coating surface hardness height, wearability and high temperature is good, and coating
Film-substrate cohesion it is strong.This method is environmentally protective, and equipment requirement is low, easy to operate, and cost is low.
The technical solution adopted by the present invention is：
A kind of method in preparing ceramic film on titanium alloy surface/glaze film composite coating, the described method includes：
(1) differential arc oxidation is carried out in titanium alloy surface, differential arc oxidation coating is prepared；The electrolyte of the differential arc oxidation
Composition is as follows：8~10g/L Na2SiO3, 2~3g/L Na3PO4, 1~2g/L NaOH, 3~4g/L sodium citrates, solvent is goes
Ionized water；The differential arc oxidation parameter is as follows：350~380V of voltage, frequency 500Hz, 20~35min of processing time；
(2) treat glaze by the differential of the arc in the arc differential oxide ceramic coating surface of titanium alloy prepared glaze slip even application
Stop spraying when oxide ceramic coating color covers；It is as follows to prepare glaze quality composition used in glaze slip：SiO252~59%, PbO
16~19%, Al2O33~8%, B2O35~9%, Na2O 3~7%, TiO23~5%, ZnO 7~9%；Preparation method is such as
Under：Glaze is in 1380 DEG C of insulation meltings, when mixture melts and after good fluidity completely, pours into the ball grinder containing deionized water
(it is 1 to adjust the content of water and glaze mass ratio to middle cold quenching:1) kaolin of glaze quality 3wt% agitation grinding together, is added
Glaze slip is pressed 1 by 100h into glaze slip:30 mass ratio, which is dissolved into water, configures solution, stirs stand-by；
(3) alloy workpiece for having sprayed glaze slip is placed in drying box, 50~60 DEG C of dry 20~30min are until sample table
Face solution moisture content testing volatilizees completely, and glaze slip is deposited on ceramic surface and no longer flows, and then takes out；
(4) workpiece is placed in isobaric stove, is heated to 800~850 DEG C from room temperature, insulation 2~3 is come out of the stove when small, is prepared
Obtain ceramic membrane/glaze film composite coating.
The present invention wants to combine using differential arc oxidation (MAO) technology and surface glazing technology prepares ceramic membrane/compound painting of glaze film
Layer is to improve matrix hardness, wearability and the thermal stability of high temperature, and the film-substrate cohesion of coating is good.First in titanium alloy
It is upper to prepare ceramic coating in matrix surface using differential arc oxidization technique, then then at ceramic surface glazing sealing of hole and to sinter preparation multiple
Close coating.At present, the relevant report for the composite coating that ceramic coating formed by micro-arc oxidation is combined with low temperature adamantine layer is prepared on titanium alloy
Almost without.
The titanium alloy is preferably Ti6Al4V.
Preferably, for the titanium alloy first through carrying out differential arc oxidation again after pre-treatment, the pre-treating method is as follows：Magnesium closes
Gold is polished with 180#, 400#, 600#, 800#, 1200#, 1500#, 2000# sand paper successively, then combines 1 μ with polishing machine, polishing cloth
Titanium alloy sample is polished to Ra=0.3 μm by the aluminium oxide antiscuffing paste of m.
Specifically, the method is as follows：
(1) Ti6Al4V titanium alloys 180#, 400#, 600#, 800#, 1200#, 1500#, 2000# sand paper polish, then with throwing
Titanium alloy sample is polished to Ra=0.3 μm by ray machine, polishing cloth with reference to 1 μm of aluminium oxide antiscuffing paste；
(2) differential arc oxidation is carried out in titanium alloy surface, differential arc oxidation coating is prepared；The electrolyte of the differential arc oxidation
Composition is as follows：8g/L Na2SiO3、2.5g/L Na3PO4, 1.4g/L NaOH, 3g/L sodium citrates, solvent is deionized water；Institute
It is as follows to state differential arc oxidation parameter：Voltage 360V, frequency 500Hz, processing time 25min；
(3) by prepared glaze slip even application titanium alloy arc differential oxide ceramic coating surface；Prepare used in glaze slip
Glaze quality composition is as follows：SiO255%, PbO 18%, Al2O35%, B2O36%, Na2O 4%, TiO24%, ZnO
8%；
(4) alloy workpiece for having sprayed glaze slip is placed in drying box, 50 DEG C of dry 20min, then take out；
(5) workpiece is placed in isobaric stove, is heated to 830 DEG C from room temperature, insulation 2 is come out of the stove when small, obtains ceramic membrane/glaze
Film composite coating.
The beneficial effects are mainly as follows：The present invention utilizes differential arc oxidation (MAO) technology and surface glazing technology
Want to combine and prepare ceramic membrane/glaze film composite coating to improve matrix surface hardness, wearability and the thermal stability of high temperature, and
The film-substrate cohesion of coating is good；Since ceramics and glaze layer have high rigidity and high consistency, so as to improve the resistance to of titanium alloy
Mill property and corrosion resistance.This method is environmentally protective, and equipment requirement is low, easy to operate, and cost is low.
(4) illustrate
Fig. 1 is titanium alloy component scale topography；
Fig. 2 is micro-arc oxidation device schematic diagram；1 three phase mains；2 differential arc oxidation DC power supplies；3 controllers；4 cooling waters；5
Electrolyte；6 samples；7 cooling towers；8 blenders；
Fig. 3 is glaze spraying device schematic diagram；1. sample；2. store up glaze bottle；3. air pump；4. stent；5. lead glaze pipe；6. gas-guide tube.
(5) embodiment
With reference to specific embodiment, the present invention is described further, but protection scope of the present invention is not limited in
This：
Embodiment 1：
1st, titanium alloy sample experiment pre-treatment
Titanium alloy TC 4 sample is processed into as shown in Figure 1, thickness is 20mm.By the sample machined respectively using 180#,
400#, 600#, 800#, 1200#, 1500#, 2000# sand paper are polishing to surfacing.Again with polishing machine, polishing cloth with reference to 1 μm
Titanium alloy sample is polished to the minute surface pattern of 0.3 μm of Ra ≈ by aluminium oxide antiscuffing paste.
2nd, the preparation of differential arc oxidation coating
Polished titanium alloy sample is rinsed with clear water respectively, then sample is placed in ultrasonic cleaning in acetone soln
10min oil removings, cleaning frequency 100,000HZ.Rinsed after ultrasonic cleaning using deionized water, take out drying.Then will examination
Sample is installed on microarc oxidation equipment provided (as shown in Figure 2), its bath composition and differential arc oxidation parameter are as shown in table 1.
Table 1：Bath composition and differential arc oxidation parameter
3rd, the preparation of composite coating
Low-temperature glaze is prepared, its chemical composition is as shown in table 2.Glaze is melted in 1380 DEG C of insulations, when mixture is complete
After melting and good fluidity, pouring into cold quenching in the ball grinder containing deionized water, (it is 1 to adjust the content of water and glaze mass ratio:
1), adding the kaolin of 3wt%, glaze slip into glaze slip, is pressed 1 by agitation grinding 100h together:30 mass ratio, which is dissolved into water, matches somebody with somebody
Solution is put, is stirred stand-by.
Table 2：The chemical composition of low-temperature glaze
The differential arc oxidation sample that upper step prepares is lain on clean glass plate, using homemade glaze spraying device (such as
Shown in Fig. 3), it is inserted into glaze solution, opens air pump, produces air-flow and equably spray glaze solution under the action of pressure difference
Arc differential oxide ceramic coating upper surface is covered in, stops spraying when glaze covers arc differential oxide ceramic coating color.Will examination
Sample is placed in drying box together with glass plate, opens drying box, and temperature is set as 50 DEG C, is taken out after dry 20min；Then,
Above-mentioned glaze is sintered in 830 DEG C of isobaric stoves, time 2 h or so, finally obtains qualified products, by being tested using company
Receive, surface property is met the requirements.
Utilize scanning electron microscope and laser confocal microscope, UMT-3 types friction wear testing machine, Ivium electricity
The equipment such as chem workstation, micro Vickers are to above-mentioned prepared composite coating surface topography finish, roughness, hard
Degree, wearability and corrosion resistance are tested：As a result it is as follows：
More than case hardness HV710；Surface roughness 0.15-0.19um；
Sample Tafel polarization curves test in 3.5wt.%NaCl solution shows：The corrosion potential of ceramic coating is：-
0.3V (matrix is -0.6V), ceramic coating corrosion electric current density is：2.0*10-10A/cm2, matrix corrosion current density is
1.58*10-7A/cm2；After corroding three hours under room temperature, the etching extent of ceramic layer is only the 1/3 of matrix.Scratch test shows：Apply
The film-substrate cohesion of layer is more than 60N.
The present invention is not limited to above-described embodiment, wherein differential arc oxidation parameter used can make the appropriate adjustments, electrolyte
Formula and glaze formula can also make appropriate change according to performance requirement, last calcination temperature can according to the formula of glaze into
Row is corresponding to be changed.
Claims (4)
1. a kind of method in preparing ceramic film on titanium alloy surface/glaze film composite coating, the described method includes：
(1) differential arc oxidation is carried out in titanium alloy surface, differential arc oxidation coating is prepared；The electrolyte composition of the differential arc oxidation
It is as follows：8~10g/L Na2SiO3, 2~3g/L Na3PO4, 1~2g/L NaOH, 3~4g/L sodium citrates, solvent is deionization
Water；The differential arc oxidation parameter is as follows：350~380V of voltage, frequency 500Hz, 20~35min of processing time；
(2) by prepared glaze slip even application titanium alloy arc differential oxide ceramic coating surface；Prepare glaze used in glaze slip
Quality composition is as follows：SiO252~59%, PbO 16~19%, Al2O33~8%, B2O35~9%, Na2O 3~7%,
TiO23~5%, ZnO 7~9%；
(3) alloy workpiece for having sprayed glaze slip is placed in drying box, dry 20~30min, then takes out at 50~60 DEG C；
(4) workpiece is placed in isobaric stove, is heated to 800~850 DEG C from room temperature, insulation 2~3 is come out of the stove when small, obtains ceramics
Film/glaze film composite coating.
2. the method as described in claim 1, it is characterised in that the titanium alloy is Ti6Al4V.
3. method as claimed in claim 1 or 2, it is characterised in that the titanium alloy first through carrying out differential of the arc oxygen again after pre-treatment
Change, the pre-treating method is as follows：Titanium alloy is beaten with 180#, 400#, 600#, 800#, 1200#, 1500#, 2000# sand paper successively
Mill, then titanium alloy sample is polished to Ra=0.3 μm with reference to 1 μm of aluminium oxide antiscuffing paste with polishing machine, polishing cloth.
4. the method as described in claim 1, it is characterised in that the method is as follows：
(1) Ti6Al4V titanium alloys 180#, 400#, 600#, 800#, 1200#, 1500#, 2000# sand paper polish, then with polishing machine,
Titanium alloy sample is polished to Ra=0.3 μm by polishing cloth with reference to 1 μm of aluminium oxide antiscuffing paste；
(2) differential arc oxidation is carried out in titanium alloy surface, differential arc oxidation coating is prepared；The electrolyte composition of the differential arc oxidation
It is as follows：8g/L Na2SiO3、2.5g/L Na3PO4, 1.4g/L NaOH, 3g/L sodium citrates, solvent is deionized water；It is described micro-
Arc oxygenation parameters are as follows：Voltage 360V, frequency 500Hz, processing time 25min；
(3) by prepared glaze slip even application titanium alloy arc differential oxide ceramic coating surface；Prepare glaze used in glaze slip
Quality composition is as follows：SiO255%, PbO 18%, Al2O35%, B2O36%, Na2O 4%, TiO24%, ZnO 8%；
(4) alloy sample for having sprayed glaze slip is placed in drying box, dry 20min, then takes out at 50 DEG C；
(5) workpiece is placed in isobaric stove, is heated to 830 DEG C from room temperature, insulation 2 is come out of the stove when small, is obtained ceramic membrane/glaze film and is answered
Close coating.
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| CN109023479A (en) * | 2018-08-31 | 2018-12-18 | 四川工程职业技术学院 | Resistance to high temperature oxidation and the titanium alloy composite material of hot salt corrosion and preparation method thereof |
| CN109652838B (en) * | 2018-12-27 | 2021-05-18 | 浙江工业大学 | Titanium-niobium alloy surface anodic oxidation coloring method |
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| CN110983408B (en) * | 2019-11-25 | 2021-11-30 | 中国科学院金属研究所 | Method for preparing nano ceramic coating by utilizing ceramic particle chemical self-sintering micro-arc oxidation technology |
| CN112779583B (en) * | 2020-12-26 | 2023-07-07 | 常州市钛宇新材料科技有限公司 | Titanium alloy surface treatment method combining color and thick film |
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