CN106011971A - Method for preparing ceramic film/glaze film composite coating on titanium alloy surface - Google Patents
Method for preparing ceramic film/glaze film composite coating on titanium alloy surface Download PDFInfo
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- CN106011971A CN106011971A CN201610364730.9A CN201610364730A CN106011971A CN 106011971 A CN106011971 A CN 106011971A CN 201610364730 A CN201610364730 A CN 201610364730A CN 106011971 A CN106011971 A CN 106011971A
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- titanium alloy
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- arc oxidation
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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
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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
-
- 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
Abstract
The invention relates to a method for preparing a ceramic film/glaze film composite coating on a titanium alloy surface. First, a ceramic coating is prepared on the surface of a matrix by a micro-arc oxidation technology on a titanium alloy; and then, the ceramic surface is subjected to glazing and hole sealing, and is sintered to prepare the composite coating. The method combines the micro-arc oxidation (MAO) technology with the surface glazing technology to prepare the ceramic film/glaze film composite coating to improve the surface hardness, wear resistance and high-temperature heat stability of the matrix, and the coating has good film base binding force; and as the ceramic and the glaze layer are high in hardness and density, the wear resistance and the corrosion resistance of the titanium alloy are improved. The method is green and environment-friendly, low in equipment requirements, simple in operation and low in cost.
Description
(1) technical field
The present invention relates to a kind of method at preparing ceramic film on titanium alloy surface/glaze film composite coating.
(2) background technology
Titanium and alloy thereof have that relative density is little, specific strength is positioned at first of metal, elastic modelling quantity is about steel
The characteristic such as half.And titanium can the highest at 600 DEG C at a temperature of life-time service, simultaneously its
There is anti-resistance to low temperature, preferable ductility can be kept under the low temperature environment of subzero 196～253 DEG C
With toughness such that it is able to avoid the cold brittleness of metal.It addition, titanium also has without magnetic, nontoxic, to environment
The advantage such as pollution-free.Therefore, titanium and alloy thereof be widely used in Aero-Space, boats and ships, chemical industry,
The fields such as the medical device in terms of medical science and Implant, are described as " spatial metal ", " marine metal ".
Titanium alloy principle: as isomer, titanium structure can change at different temperatures, when
Titanium is in less than time under 882 DEG C of environment, and it is rendered as close-packed hexagonal lattice structure, the titanium of this structure
It is referred to as α-titanium；And when titanium is under 882 DEG C of environment above, it is rendered as body-centered cubic lattic knot
Structure, the titanium of this structure is referred to as β-titanium.Ti6Al4V due to its thermostability, intensity, plasticity,
Toughness, formability, solderability, corrosion resistance and biocompatibility are all preferable, become first practical
Trump alloy in titanium alloy, referred to as titanium alloy industry.This alloy usage amount has accounted for whole titanium alloy
75%～85%.Other many titanium alloys can be regarded as the remodeling of Ti6Al4V alloy.China opens
The large-scale production of beginning titanium and titanium alloy related industries has had more than 50 year, has the most ranked among the 5th
Big Ti industry manufacturing country.In view of the combination property that titanium alloy is excellent, it is likely to become after ferrum, aluminum
" the 3rd metal " emerged.
Titanium or titanium alloy has above-mentioned series of advantages, but it also also exists such as: case hardness is low, resistance to
The problems such as mill poor performance, are difficult to meet the requirement producing reality application under many circumstances.Therefore, exist
It is very urgent that titanium alloy surface preparation has research wear-resisting, decay resistance coating.The most main
Be application surface strengthening technology titanium or titanium alloy surface is optimized.At at present to metallic surface
In all kinds of methods of reason, the overwhelming majority has all had application to the surface of titanium alloy and has processed, including carburizing
(nitrogen, boron), metal plating, anodic oxidation, differential arc oxidation, ionic nitriding, vacuum electron beam table
Face process, Laser Surface Treatment plasma spraying etc..
While the process for treating surface of above-mentioned titanium or titanium alloy all contains respective advantage, also also exist bright
Aobvious defect.As: there is long processing period in the means such as carburizing tech, boronizing technology and nitridation technique
And the problem such as workpiece is yielding；Coating texture prepared by plasma spray technology is loose and coating with
The adhesion of matrix is more weak；The high energy surface treatment such as laser surface alloying have employed local heat treatment
Method, although the shortcoming overcoming the heating of thermo-chemical treatment entirety, but even in actual production is used
There is alloyed layer out-of-flatness and with matrix intersection, the defect such as crackle, cavity occur in you.The heaviest
, these methods above-mentioned are relatively costly, mostly rest on laboratory stage, are unfavorable for really anticipating
Mass market popularization and application in justice.Therefore, it is necessary to the method for research efficient and cost-effective is come titanium
And titanium alloy protects effectively, improve its wear-corrosion resistance so that it meets reality application
Requirement.
(3) summary of the invention
It is an object of the invention to overcome existing titanium alloy surface coating technology defect, it is provided that Yi Zhongti
The preparation method of the coating of titanium master alloy face coat performance.Coating surface hardness height, wearability and height
The thermal stability of temperature is good, and the film-substrate cohesion of coating is strong.The method environmental protection, equipment is wanted
Ask low, simple to operate, low cost.
The technical solution used in the present invention is:
A kind of method at preparing ceramic film on titanium alloy surface/glaze film composite coating, described method includes:
(1) carry out differential arc oxidation at titanium alloy surface, prepare differential arc oxidation coating；The described differential of the arc
The electrolyte composition of oxidation is as follows: 8～10g/L Na2SiO3, 2～3g/L Na3PO4, 1～2
G/L NaOH, 3～4g/L sodium citrate, solvent is deionized water；Described differential arc oxidation
Parameter is as follows: voltage 350～380V, frequency 500Hz, processes the time 20～35min；
(2) by the glaze slip even application for preparing at the arc differential oxide ceramic coating surface of titanium alloy, treat
Spraying is stopped when arc differential oxide ceramic coating color is covered by glaze；Glaze used by preparation glaze slip
Material quality composition is as follows: SiO252～59%, PbO 16～19%, Al2O33～8%, B2O3
5～9%, Na2O 3～7%, TiO23～5%, ZnO 7～9%；Compound method is as follows: glaze
Expect 1380 DEG C of insulations melted, when mixture is completely melted and after good fluidity, pours into
Cold quenching (content of regulation water is 1:1 with glaze mass ratio) in ball grinder containing deionized water,
The Kaolin agitation grinding 100h together adding glaze quality 3wt% becomes glaze slip, will
Glaze slip is dissolved in water configuration solution by the mass ratio of 1:30, stirs stand-by；
(3) being placed in drying baker by the alloy workpiece having sprayed glaze slip, 50～60 DEG C are dried 20～30min
Until specimen surface solution moisture content testing volatilizees completely, glaze slip is deposited on ceramic surface and no longer flows
Dynamic, then take out；
(4) being placed on by workpiece in isobaric stove, be heated to 800～850 DEG C from room temperature, insulation 2～3 is little
Time come out of the stove, prepare ceramic membrane/glaze film composite coating.
The present invention utilizes differential arc oxidation (MAO) technology and surface glazing technology to want to combine preparation pottery
Film/glaze film composite coating is to improve matrix hardness, wearability and the thermal stability of high temperature, and is coated with
The film-substrate cohesion of layer is good.First utilize differential arc oxidization technique at matrix surface preparation pottery on titanium alloy
Porcelain coating, then prepares composite coating then at ceramic surface glazing sealing of hole sintering.At present, close at titanium
The relevant report of the composite coating that ceramic coating formed by micro-arc oxidation is combined is prepared with low temperature adamantine layer almost on gold
No.
Described titanium alloy is preferably Ti6Al4V.
Preferably, described titanium alloy first carries out differential arc oxidation, described pre-treatment side after pre-treatment again
Method is as follows: magnesium alloy is successively with 180#, 400#, 600#, 800#, 1200#, 1500#, 2000#
Sand papering, then combine the aluminium oxide antiscuffing paste of 1 μm by titanium alloy sample with buffing machine, polishing cloth
It is polished to Ra ≈ 0.3 μm.
Concrete, described method is as follows:
(1) Ti6Al4V titanium alloy 180#, 400#, 600#, 800#, 1200#, 1500#, 2000#
Sand papering, then combine the aluminium oxide antiscuffing paste of 1 μm by titanium conjunction with buffing machine, polishing cloth
Gold sample is polished to Ra ≈ 0.3 μm；
(2) carry out differential arc oxidation at titanium alloy surface, prepare differential arc oxidation coating；Described differential of the arc oxygen
The electrolyte composition changed is as follows: 8g/L Na2SiO3、2.5g/L Na3PO4、1.4g/L NaOH、
3g/L sodium citrate, solvent is deionized water；Described differential arc oxidation parameter is as follows: voltage
360V, frequency 500Hz, process time 25min；
(3) by the glaze slip even application for preparing at the arc differential oxide ceramic coating surface of titanium alloy；Preparation
Used by glaze slip, glaze quality composition is as follows: SiO255%, PbO 18%, Al2O35%, B2O3
6%, Na2O 4%, TiO24%, ZnO 8%；
(4) alloy workpiece having sprayed glaze slip is placed in drying baker, 50 DEG C of dry 20min, then takes
Go out；
(5) workpiece is placed in isobaric stove, is heated to 830 DEG C from room temperature, is incubated and comes out of the stove for 2 hours,
Obtain ceramic membrane/glaze film composite coating.
The beneficial effects are mainly as follows: the present invention utilizes differential arc oxidation (MAO) technology
With surface glazing technology think combination prepare ceramic membrane/glaze film composite coating with improve matrix surface hardness,
Wearability and the thermal stability of high temperature, and the film-substrate cohesion of coating is good；Due to pottery and glaze layer
There is high rigidity and high consistency, thus improve wearability and the decay resistance of titanium alloy.Should
Method environmental protection, equipment requirements is low, simple to operate, low cost.
(4) accompanying drawing explanation
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 sources；3 control
Device；4 cooling water；5 electrolyte；6 samples；7 cooling towers；8 agitators；
Fig. 3 is glaze spraying device schematic diagram；1. sample；2. storage glaze bottle；3. air pump；4. support；5. glaze pipe is led；
6. airway.
(5) detailed description of the invention
Below in conjunction with specific embodiment, the present invention is described further, but protection scope of the present invention
It is not limited to that:
Embodiment 1:
1, titanium alloy sample experiment pre-treatment
Titanium alloy TC 4 sample is processed into as it is shown in figure 1, thick is 20mm.By machine
Sample uses 180#, 400#, 600#, 800#, 1200#, 1500#, 2000# sand papering respectively
To surfacing.Titanium alloy is tried by the aluminium oxide antiscuffing paste combining 1 μm again with buffing machine, polishing cloth
Sample is polished to the minute surface pattern of Ra ≈ 0.3 μm.
2, the preparation of differential arc oxidation coating
Polished titanium alloy sample is rinsed with clear water respectively, then sample is placed in acetone soln super
Sound wave cleans 10min oil removing, and cleaning frequency is 100,000HZ.Make after ultrasonic waves for cleaning to spend from
Sub-water rinses, and taking-up dries up.Then sample is arranged 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
3, the preparation of composite coating
Preparing low-temperature glaze, its chemical composition is as shown in table 2.Glaze is melted 1380 DEG C of insulations,
When mixture is completely melted and after good fluidity, pours cold quenching in the ball grinder containing deionized water into and (adjusts
The content of water saving and glaze mass ratio are 1:1), add the Kaolin agitation grinding together of 3wt%
100h becomes glaze slip, by the mass ratio of 1:30, glaze slip is dissolved in water configuration solution, is sufficiently stirred for
The most stand-by.
Table 2: the chemical composition of low-temperature glaze
The differential arc oxidation sample upper step prepared lies on the glass plate of cleaning, uses homemade spray
Glaze device (as shown in Figure 3), inserts in glaze solution, opens air pump, produces air-flow at pressure difference
Effect under by glaze solution equably spray covering at arc differential oxide ceramic coating upper surface, treat glaze
Spraying is stopped when being covered by arc differential oxide ceramic coating color.Sample is placed in dry together with glass plate
In dry case, opening drying baker, temperature is set as 50 DEG C, takes out after being dried 20min；Then, will
Above-mentioned glaze sinters in 830 DEG C of isobaric stoves, about time 2 h, finally obtains qualified products,
Checking and accepting through use company, surface property meets requirement.
Utilize scanning electron microscope and laser confocal microscope, UMT-3 type fretting wear examination
The equipment such as machine, Ivium electrochemical workstation, micro Vickers of testing are to above-mentioned prepared being combined
Coating morphology fineness, roughness, hardness, wearability and corrosion resistance are tested: result
As follows:
More than case hardness HV710；Surface roughness 0.15-0.19um；
Sample Tafel polarization curve test in 3.5wt.%NaCl solution shows: the corruption of ceramic coating
Erosion current potential is :-0.3V (matrix is-0.6V), ceramic coating corrosion electric current density/Acm be: 2.0*10-10
Matrix is 1.58*10-7；After corroding three hours under room temperature, the etching extent of ceramic layer is only matrix
1/3.Scratch test shows: the film-substrate cohesion of coating is more than 60N.
The present invention is not limited to above-described embodiment, and differential arc oxidation parameter wherein used can do suitably tune
Whole, electrolyte prescription and glaze formula can also make suitably change, last roasting according to performance requirement
Temperature can change accordingly according to the formula of glaze.
Claims (4)
1., in a method for preparing ceramic film on titanium alloy surface/glaze film composite coating, described method includes:
(1) carry out differential arc oxidation at titanium alloy surface, prepare differential arc oxidation coating；The described differential of the arc
The electrolyte composition of oxidation is as follows: 8～10g/L Na2SiO3, 2～3g/L Na3PO4, 1～2g/L
NaOH, 3～4g/L sodium citrate, solvent is deionized water；Described differential arc oxidation parameter
As follows: voltage 350～380V, frequency 500Hz, process the time 20～35min；
(2) by the glaze slip even application for preparing at the arc differential oxide ceramic coating surface of titanium alloy；Join
Enamel frit makeing slurry glaze quality used composition is as follows: SiO252～59%, PbO 16～19%, Al2O3
3～8%, B2O35～9%, Na2O 3～7%, TiO23～5%, ZnO 7～9%；
(3) alloy workpiece having sprayed glaze slip is placed in drying baker, at 50～60 DEG C, is dried 20～30
Min, then takes out；
(4) workpiece is placed in isobaric stove, is heated to 800～850 DEG C from room temperature, is incubated 2～3 hours
Come out of the stove, obtain ceramic membrane/glaze film composite coating.
2. the method for claim 1, it is characterised in that described titanium alloy is Ti6Al4V.
3. method as claimed in claim 1 or 2, it is characterised in that described titanium alloy is first after pre-treatment
Carrying out differential arc oxidation again, described pre-treating method is as follows: magnesium alloy successively with 180#, 400#, 600#,
800#, 1200#, 1500#, 2000# sand papering, then combine 1 μm with buffing machine, polishing cloth
Titanium alloy sample is polished to Ra ≈ 0.3 μm by aluminium oxide antiscuffing paste.
4. the method for claim 1, it is characterised in that described method is as follows:
(1) Ti6Al4V titanium alloy 180#, 400#, 600#, 800#, 1200#, 1500#, 2000#
Sand papering, then combine the aluminium oxide antiscuffing paste of 1 μm by titanium conjunction with buffing machine, polishing cloth
Gold sample is polished to Ra ≈ 0.3 μm；
(2) carry out differential arc oxidation at titanium alloy surface, prepare differential arc oxidation coating；The described differential of the arc
The electrolyte composition of oxidation is as follows: 8g/L Na2SiO3、2.5g/L Na3PO4、1.4g/L
NaOH, 3g/L sodium citrate, solvent is deionized water；Described differential arc oxidation parameter is such as
Under: voltage 360V, frequency 500Hz, process time 25min；
(3) by the glaze slip even application for preparing at the arc differential oxide ceramic coating surface of titanium alloy；Join
Enamel frit makeing slurry glaze quality used composition is as follows: SiO255%, PbO 18%, Al2O35%,
B2O36%, Na2O 4%, TiO24%, ZnO 8%；
(4) alloy sample having sprayed glaze slip is placed in drying baker, is dried 20min at 50 DEG C, so
Rear taking-up；
(5) workpiece is placed in isobaric stove, is heated to 830 DEG C from room temperature, is incubated and comes out of the stove for 2 hours,
Obtain ceramic membrane/glaze film composite coating.
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Cited By (7)
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| CN108385156A (en) * | 2018-05-31 | 2018-08-10 | 东北大学 | The flexibly coating or passivation layer preparation facilities and application method of control environmental parameter |
| CN108624851A (en) * | 2018-04-25 | 2018-10-09 | 中国振华集团云科电子有限公司 | A kind of special ceramics surface metal-layer exterior appearance changes method and new ceramics substrate |
| 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 |
| CN109652838A (en) * | 2018-12-27 | 2019-04-19 | 浙江工业大学 | A kind of method of titanium-niobium alloy surface anodization coloring |
| CN109868386A (en) * | 2019-03-08 | 2019-06-11 | 安徽信息工程学院 | A kind of wear-resistant material and preparation method thereof |
| CN110983408A (en) * | 2019-11-25 | 2020-04-10 | 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 |
| CN112779583A (en) * | 2020-12-26 | 2021-05-11 | 常州市钛宇新材料科技有限公司 | Color and thick film combined titanium alloy surface treatment method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108624851A (en) * | 2018-04-25 | 2018-10-09 | 中国振华集团云科电子有限公司 | A kind of special ceramics surface metal-layer exterior appearance changes method and new ceramics substrate |
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| CN109652838A (en) * | 2018-12-27 | 2019-04-19 | 浙江工业大学 | A kind of method of titanium-niobium alloy surface anodization coloring |
| CN109868386A (en) * | 2019-03-08 | 2019-06-11 | 安徽信息工程学院 | A kind of wear-resistant material and preparation method thereof |
| CN109868386B (en) * | 2019-03-08 | 2020-09-01 | 安徽信息工程学院 | Wear-resistant material and preparation method thereof |
| CN112251651A (en) * | 2019-03-08 | 2021-01-22 | 安徽信息工程学院 | Preparation method of wear-resistant material |
| CN112251651B (en) * | 2019-03-08 | 2021-08-10 | 安徽信息工程学院 | Preparation method of wear-resistant material |
| CN110983408A (en) * | 2019-11-25 | 2020-04-10 | 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 |
| 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 |
| CN112779583A (en) * | 2020-12-26 | 2021-05-11 | 常州市钛宇新材料科技有限公司 | Color and thick film combined titanium alloy surface treatment method |
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