CN106086981B - A kind of preparation method for the porous surface anodic oxide coating improving Ti-Al system alloy antioxygenic property - Google Patents
A kind of preparation method for the porous surface anodic oxide coating improving Ti-Al system alloy antioxygenic property Download PDFInfo
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- CN106086981B CN106086981B CN201610546032.0A CN201610546032A CN106086981B CN 106086981 B CN106086981 B CN 106086981B CN 201610546032 A CN201610546032 A CN 201610546032A CN 106086981 B CN106086981 B CN 106086981B
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- 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
- C25D11/04—Anodisation of aluminium or alloys based thereon
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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
A kind of preparation method for the porous surface anodic oxide coating improving Ti-Al system alloy antioxygenic property, the present invention relates to a kind of preparation methods of porous surface anodic oxide coating for improving Ti-Al system alloy antioxygenic property.The problem of it is insufficient that the present invention is to solve existing Ti-Al system alloy antioxygenic properties, and the germinating and extension that not can effectively prevent crackle cause oxide layer to fall off.Method: one, it pre-processes；Two, anodic oxidation；Three, subsequent processing.The present invention has, high temperature under element-free in diffusion phenomena high with substrate combinating strength by anodizing in the ordered porous anodic layer that Ti-Al system alloy surface generates.Anodizing has many advantages, such as simple process, easy to operate, low for equipment requirements simultaneously, low in cost, therefore suitable Practical Project application.
Description
Technical field
The present invention relates to a kind of preparation sides of porous surface anodic oxide coating for improving Ti-Al system alloy antioxygenic property
Method.
Background technique
Since Ti-Al system alloy has the characteristics that density is low, specific strength is high, in aerospace, ocean, automobile, stone
The fields such as oiling work have very wide application prospect, are the high temperature lightweight materials for the most application potential generally acknowledged 21st century
Material.But Ti-Al system alloy is when being exposed in high temperature air, the TiO that surface is formed2And Al2O3The oxide layer of two kinds of mixtures is simultaneously
It is not fine and close, it is unable to effective protection matrix and is not further oxided, therefore high-temperature oxidation resistance deficiency becomes restriction Ti-Al system alloy
Realize a big bottleneck of engineering application.
It improves there are mainly two types of the antioxidative methods of Ti-Al system alloy high-temp.One is alloyings, i.e., with two kinds of metals
Between compound be matrix, thereto be added can be improved its antioxidative alloying element, such as Zr, Nb, Mo, Mn.But it closes
When gold dollar cellulose content is excessive, the mechanical performance of meeting severe exacerbation matrix.Another be by process for treating surface between metal
Compound surface forms one layer of antioxidant coating, and the type of coating can be divided into depositing coating, diffusion according to preparation method difference
Coating and rich halogen coating.Coating can effectively improve the high-temperature oxidation resistance of matrix, but have strong in conjunction with matrix
Spend low, the disadvantages of opposite matrix mechanical performance is poor.
Since the 21th century, the mankind the fields such as aerospace, ocean, automobile, petrochemical industry achieve it is considerable into
Step and development.Especially in aerospace field, as speed of the various countries to aircraft proposes increasingly higher demands, to starting
The requirement of the military service performance of machine material is also higher and higher.As a kind of high temperature light material, Ti-Al system alloy is considered most suitable
Material of the conjunction for Ni based high-temperature alloy.But antioxygenic property deficiency is always to restrict Ti-Al system alloy engineering at high temperature
Change the principal element of application.Therefore, matrix antioxygenic property low-cost surface treatment work again can either be improved by seeking one kind
Skill is most important.
Summary of the invention
It is insufficient that the present invention is to solve existing Ti-Al system alloy antioxygenic properties, not can effectively prevent crackle germinating and
The problem of extension causes oxide layer to fall off, and a kind of porous surface anodic oxygen for improving Ti-Al system alloy antioxygenic property is provided
Change the preparation method of layer.
A kind of preparation method for the porous surface anodic oxide coating for improving Ti-Al system alloy antioxygenic property of the present invention is specific
It is to sequentially include the following steps:
One, it pre-processes: successively being polished using 400# sand paper, 800# sand paper and 2000# sand paper titanium aluminium sample, then
The surface of the titanium aluminium sample after polishing is thrown to mirror surface using mechanical polishing, first uses deionized water cleaning 3~5 times, every time
3min~5min, then be placed in ultrasonic oscillation in acetone and clean 5min, finally ultrasonic oscillation cleans 5min in dehydrated alcohol
Afterwards, cold wind drying is taken out, titanium aluminium sample to be processed is obtained；
Two, anodic oxidation: using titanium aluminium sample to be processed as working electrode, platinum electrode or graphite electrode as auxiliary electrode,
Working electrode and auxiliary electrode are totally submerged in the electrolytic solution, carry out anodic oxidation, institute under conditions of voltage is 1V~60V
The time for stating anodic oxidation is 0.1h~20h, and it is 0 DEG C~85 DEG C that electrolyte temperature is controlled during anodic oxidation, reaction
Terminate, the sample after obtaining anodic oxidation；The electrolyte is the H that concentration is 0.1mol/L~10mol/L2SO4Aqueous solution and institute
State the H that concentration is 0.1mol/L~10mol/L2SO4Added with the fluoride for accounting for gross mass 0.1%~5% in aqueous solution；
Three, subsequent processing: using deionized water by sample wash 3~5 times after anodic oxidation, 3~5min every time, then
In dehydrated alcohol after ultrasonic oscillation cleaning 5min, cold wind drying is taken out, that is, completes to improve Ti-Al system alloy antioxygenic property
Porous surface anodic oxide coating preparation.
Beneficial effects of the present invention: the present invention, which prepares one layer in Ti-Al system alloy surface using the method for anodic oxidation, to be had
The oxide layer of sequence porous structure, effective solution Ti-Al system alloy antioxygenic property insufficient technical bottleneck.Moreover, passing through
The antioxygenic property that anodizing improves matrix have it is low for equipment requirements, it is easy to operate, it is low in cost the advantages that, meet real
The requirement of border engineering application.
Detailed description of the invention
Fig. 1 is the surface topography map of treated the TiAl intermetallic compound of embodiment one；
Fig. 2 is the surface topography map of treated the TiAl intermetallic compound of embodiment two；
Fig. 3 is TiAl intermetallic compound not processed by the invention, treated the TiAl intermetallic of embodiment one
The oxidizing dynamics curve of object and embodiment two treated TiAl intermetallic compound；Wherein 1 is not processed by the invention
TiAl intermetallic compound, 2 be treated the TiAl intermetallic compound of embodiment one, and 3 be treated the TiAl of embodiment two
Intermetallic compound.
Specific embodiment
Specific embodiment 1: a kind of porous surface anode for improving Ti-Al system alloy antioxygenic property of present embodiment
The preparation method of oxide layer is specifically to sequentially include the following steps:
One, it pre-processes: successively being polished using 400# sand paper, 800# sand paper and 2000# sand paper titanium aluminium sample, then
The surface of the titanium aluminium sample after polishing is thrown to mirror surface using mechanical polishing, first uses deionized water cleaning 3~5 times, every time
3min~5min, then be placed in ultrasonic oscillation in acetone and clean 5min, finally ultrasonic oscillation cleans 5min in dehydrated alcohol
Afterwards, cold wind drying is taken out, titanium aluminium sample to be processed is obtained；
Two, anodic oxidation: using titanium aluminium sample to be processed as working electrode, platinum electrode or graphite electrode as auxiliary electrode,
Working electrode and auxiliary electrode are totally submerged in the electrolytic solution, carry out anodic oxidation, institute under conditions of voltage is 1V~60V
The time for stating anodic oxidation is 0.1h~20h, and it is 0 DEG C~85 DEG C that electrolyte temperature is controlled during anodic oxidation, reaction
Terminate, the sample after obtaining anodic oxidation；The electrolyte is the H that concentration is 0.1mol/L~10mol/L2SO4Aqueous solution and institute
State the H that concentration is 0.1mol/L~10mol/L2SO4Added with the fluoride for accounting for gross mass 0.1%~5% in aqueous solution；
Three, subsequent processing: using deionized water by sample wash 3~5 times after anodic oxidation, 3~5min every time, then
In dehydrated alcohol after ultrasonic oscillation cleaning 5min, cold wind drying is taken out, that is, completes to improve Ti-Al system alloy antioxygenic property
Porous surface anodic oxide coating preparation.
Present embodiment directly utilizes the method for electrochemistry to form one layer of anodic oxide coating in Ti-Al system alloy surface, from
And improve the antioxygenic property of matrix.Compared with alloyage process and traditional coat preparing technology, anodic oxidation does not introduce it
Its alloying element, therefore diffusion phenomena in element-free.Meanwhile in anode oxidation process, anodic oxide coating is by life in situ
What long mode was formed, thus it is higher with the bond strength of matrix.In addition, anodic oxidation is low for equipment requirements, simple process, at
This is cheap, meets the needs of practical engineering application.Present embodiment is by special anode oxidation process, in Ti-Al system alloy
Surface forms orderly porous anode layer, can effectively improve the antioxygenic property of Ti-Al system alloy, and orderly is porous
Structure not only can be with, so that oxide layer be made to be not easy to peel off, matrix can persistently be effectively protected, meanwhile, porous structure is in high temperature
Densification can also occur when heating, further improve the antioxygenic property of Ti-Al system alloy.
Specific embodiment 2: the present embodiment is different from the first embodiment in that: titanium aluminium sample described in step 1
For Ti-Al system alloy.It is other same as the specific embodiment one.
Specific embodiment 3: the present embodiment is different from the first and the second embodiment in that: titanium aluminium described in step 1
Sample is Ti3Al, TiAl or TiAl3.It is other the same as one or two specific embodiments.
Specific embodiment 4: unlike one of present embodiment and specific embodiment one to three: in step 2
Voltage carries out anodic oxidation under conditions of being 30V~50V.It is other identical as one of specific embodiment one to three.
Specific embodiment 5: unlike one of present embodiment and specific embodiment one to four: institute in step 2
The time for stating anodic oxidation is 6h.It is other identical as one of specific embodiment one to four.
Specific embodiment 6: unlike one of present embodiment and specific embodiment one to five: in step 2
Electrolyte temperature is controlled during anodic oxidation to be 25 DEG C and keep constant temperature constant.It is other with specific embodiment one to five it
One is identical.
Specific embodiment 7: unlike one of present embodiment and specific embodiment one to six: institute in step 2
Stating electrolyte is the H that concentration is 0.1mol/L~5mol/L2SO4Aqueous solution and the concentration are 0.1mol/L~5mol/L's
H2SO4Added with the fluoride for accounting for gross mass 0.1%~5% in aqueous solution.Other phases one of with specific embodiment one to six
Together.
Specific embodiment 8: unlike one of present embodiment and specific embodiment one to seven: institute in step 2
Stating electrolyte is the H that concentration is 1mol/L2SO4The H that aqueous solution and the concentration are 1mol/L2SO4It is total added with Zhan in aqueous solution
The fluoride of quality 0.1%~5%.It is other identical as one of specific embodiment one to seven.
Specific embodiment 9: unlike one of present embodiment and specific embodiment one to eight: institute in step 2
Stating electrolyte is the H that concentration is 1mol/L2SO4The H that aqueous solution and the concentration are 1mol/L2SO4It is total added with Zhan in aqueous solution
The fluoride of quality 0.1%~1%.It is other identical as one of specific embodiment one to eight.
Specific embodiment 10: unlike one of present embodiment and specific embodiment one to nine: institute in step 2
Stating fluoride is hydrofluoric acid, ammonium fluoride, sodium fluoride, potassium fluoride, calcirm-fluoride or potassium hydrogen fluoride.It is other with specific embodiment one to
One of nine is identical.
Beneficial effects of the present invention are verified by following embodiment:
A kind of embodiment one: preparation method for the porous surface anodic oxide coating improving Ti-Al system alloy antioxygenic property
Specifically sequentially include the following steps:
One, it pre-processes: successively TiAl intermetallic compound being carried out using 400# sand paper, 800# sand paper and 2000# sand paper
Then the surface of TiAl intermetallic compound after polishing is thrown to mirror surface using mechanical polishing, first uses deionized water by polishing
Cleaning 3~5 times, each 3min~5min, then be placed in ultrasonic oscillation in acetone and clean 5min, it is finally ultrasonic in dehydrated alcohol
After wave concussion cleaning 5min, cold wind drying is taken out, TiAl intermetallic compound to be processed is obtained；
Two, anodic oxidation: using TiAl intermetallic compound to be processed as working electrode, platinum electrode, will as auxiliary electrode
Working electrode and auxiliary electrode are totally submerged in the electrolytic solution, and the working electrode and auxiliary electrode are in voltage at a distance of 2.5cm
Anodic oxidation is carried out under conditions of 30V, the time of the anodic oxidation is 2h, and electrolyte temperature is controlled during anodic oxidation
Degree is 25 DEG C, and reaction terminates, the sample after obtaining anodic oxidation；The electrolyte is the H that concentration is 1mol/L2SO4Aqueous solution and
The concentration is the H of 1mol/L2SO4Added with the hydrogen fluoride for accounting for gross mass 0.25% in aqueous solution；
Three, subsequent processing: using deionized water by sample wash 3~5 times after anodic oxidation, 3~5min every time, then
In dehydrated alcohol after ultrasonic oscillation cleaning 5min, cold wind drying is taken out, that is, completes to improve Ti-Al system alloy antioxygenic property
Porous surface anodic oxide coating preparation.
Fig. 1 is the surface topography map of treated the TiAl intermetallic compound of embodiment one；It can be seen from the figure that passing through
After anodized, the anodic oxide coating that TiAl intermetallic compound surface is formed not is fine and close, but is advised by shape
Whole, aperture is uniform, the ordered nano hole structure composition of proper alignment.
Embodiment two: the present embodiment and embodiment the difference is that: in step 2 voltage be 50V under conditions of into
Row anodic oxidation.Others are the same as example 1.
Fig. 2 is the surface topography map of treated the TiAl intermetallic compound of embodiment two；As can be seen from the figure work as sun
When pole oxidation voltage increases, the diameter of nano-pore is consequently increased, and there is also many diameter dimensions inside every nano-pore
Smaller nano-pore.
Fig. 3 is TiAl intermetallic compound not processed by the invention, treated the TiAl intermetallic of embodiment one
The oxidizing dynamics curve of object and embodiment two treated TiAl intermetallic compound, wherein 1 is not processed by the invention
TiAl intermetallic compound, 2 be treated the TiAl intermetallic compound of embodiment one, and 3 be treated the TiAl of embodiment two
Intermetallic compound；As can be seen from the figure after anodized, the antioxygenic property of TiAl intermetallic compound is obtained
Apparent improvement is arrived.Untreated sample oxidation weight gain is obvious, is approximately that straight line increases after 20h, single after cyclic oxidation 50h
Plane product weight gain is 20.775mg/cm2.And 50V voltage anodic oxygenization treated sample oxidation weight gain rate very little, circulation
Unit area weight gain is only 0.598mg/cm after aoxidizing 50h2。
Implementation is assessed using the unit area gain in weight after the cyclic high-temperature oxidation 50h in 800 DEG C of still airs respectively
The antioxygenic property of treated the TiAl intermetallic compound of example one and embodiment two treated TiAl intermetallic compound, knot
Fruit is shown in Table one.
One different voltages anodic oxygen sample cyclic high-temperature of table aoxidizes the unit area gain in weight after 50h
Embodiment three: the present embodiment and embodiment one the difference is that: the time of anodic oxidation described in step 2
For 1h.Others are the same as example 1.
Embodiment three is assessed using the unit area gain in weight after the cyclic high-temperature oxidation 50h in 800 DEG C of still airs
The antioxygenic property for TiAl intermetallic compound that treated, the results are shown in Table two.
Unit area gain in weight under the different anodizing times of table two after sample cyclic high-temperature oxidation 50h
Example IV: the present embodiment and embodiment one the difference is that: electrolyte described in step 2 is that concentration is
The H of 1mol/L2SO4The H that aqueous solution and the concentration are 1mol/L2SO4Added with the fluorination for accounting for gross mass 0.35% in aqueous solution
Hydrogen.Others are the same as example 1.
Example IV is assessed using the unit area gain in weight after the cyclic high-temperature oxidation 50h in 800 DEG C of still airs
The antioxygenic property for TiAl intermetallic compound that treated, the results are shown in Table three.
Unit area weight gain when the addition of the different amounts of hydrogen fluoride of table three after anodic oxidation sample cyclic high-temperature oxidation 50h
Amount
Claims (2)
1. improving the preparation method of the porous surface anodic oxide coating of Ti-Al system alloy antioxygenic property, it is characterised in that improve
The preparation method of the porous surface anodic oxide coating of Ti-Al system alloy antioxygenic property is specifically to sequentially include the following steps:
One, it pre-processes: successively being polished using 400# sand paper, 800# sand paper and 2000# sand paper TiAl intermetallic compound,
Then the surface of the TiAl intermetallic compound after polishing is thrown to mirror surface, first using deionized water cleaning 3 using mechanical polishing
~5 times, each 3min~5min, then be placed in ultrasonic oscillation in acetone and clean 5min, finally ultrasonic wave shakes in dehydrated alcohol
After swinging cleaning 5min, cold wind drying is taken out, TiAl intermetallic compound to be processed is obtained；
Two, anodic oxidation: using TiAl intermetallic compound to be processed as working electrode, platinum electrode is as auxiliary electrode, by work
Electrode and auxiliary electrode are totally submerged in the electrolytic solution, and the working electrode and auxiliary electrode are 30V in voltage at a distance of 2.5cm
Under conditions of carry out anodic oxidation, the time of the anodic oxidation is 2h, controls electrolyte temperature during anodic oxidation
It is 25 DEG C, reaction terminates, the sample after obtaining anodic oxidation；The electrolyte is the H that concentration is 1mol/L2SO4Aqueous solution and institute
State the H that concentration is 1mol/L2SO4Added with the hydrogen fluoride for accounting for gross mass 0.25% in aqueous solution；
Three, subsequent processing: using deionized water by sample wash 3~5 times after anodic oxidation, 3~5min every time, then in nothing
In water-ethanol after ultrasonic oscillation cleaning 5min, cold wind drying is taken out, that is, completes the table for improving Ti-Al system alloy antioxygenic property
The preparation of face porous anode layer, the TiAl intermetallic compound that obtains that treated；It will treated TiAl intermetallic
Unit area weight gain is 3.33mg/cm to object after cyclic high-temperature oxidation 50h in 800 DEG C of still airs2。
2. improving the preparation method of the porous surface anodic oxide coating of Ti-Al system alloy antioxygenic property, it is characterised in that improve
The preparation method of the porous surface anodic oxide coating of Ti-Al system alloy antioxygenic property is specifically to sequentially include the following steps:
One, it pre-processes: successively being polished using 400# sand paper, 800# sand paper and 2000# sand paper TiAl intermetallic compound,
Then the surface of the TiAl intermetallic compound after polishing is thrown to mirror surface, first using deionized water cleaning 3 using mechanical polishing
~5 times, each 3min~5min, then be placed in ultrasonic oscillation in acetone and clean 5min, finally ultrasonic wave shakes in dehydrated alcohol
After swinging cleaning 5min, cold wind drying is taken out, TiAl intermetallic compound to be processed is obtained；
Two, anodic oxidation: using TiAl intermetallic compound to be processed as working electrode, platinum electrode is as auxiliary electrode, by work
Electrode and auxiliary electrode are totally submerged in the electrolytic solution, and the working electrode and auxiliary electrode are 50V in voltage at a distance of 2.5cm
Under conditions of carry out anodic oxidation, the time of the anodic oxidation is 2h, controls electrolyte temperature during anodic oxidation
It is 25 DEG C, reaction terminates, the sample after obtaining anodic oxidation；The electrolyte is the H that concentration is 1mol/L2SO4Aqueous solution and institute
State the H that concentration is 1mol/L2SO4Added with the hydrogen fluoride for accounting for gross mass 0.25% in aqueous solution；
Three, subsequent processing: using deionized water by sample wash 3~5 times after anodic oxidation, 3~5min every time, then in nothing
In water-ethanol after ultrasonic oscillation cleaning 5min, cold wind drying is taken out, that is, completes the table for improving Ti-Al system alloy antioxygenic property
The preparation of face porous anode layer, the TiAl intermetallic compound that obtains that treated；It will treated TiAl intermetallic
Unit area weight gain is 0.598mg/cm to object after cyclic high-temperature oxidation 50h in 800 DEG C of still airs2。
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| CN106835227B (en) * | 2016-12-05 | 2018-11-13 | 浙江工业大学 | A method of titanium-base alloy high temperature oxidation resistance is improved based on halide effect and ceramic coating |
| CN107541764B (en) * | 2017-09-07 | 2019-05-31 | 上海脉诺金属表面处理技术有限公司 | A kind of High-silicon and high-copper die casting aluminium anode oxidation process and High-silicon and high-copper pack alloy |
| CN109594113B (en) * | 2017-09-30 | 2021-02-09 | 北京小米移动软件有限公司 | Equipment shell, machining method thereof and electronic equipment |
| CN108486631A (en) * | 2018-03-13 | 2018-09-04 | 浙江工业大学 | A method of improving titanium-base alloy resistance to high temperature oxidation |
| CN114182318B (en) * | 2021-12-31 | 2023-02-28 | 北京科技大学 | TiAl porous alloy with oxide film and preparation method and application thereof |
| CN114657501B (en) * | 2022-02-28 | 2023-10-27 | 太原理工大学 | Method for improving high-temperature oxidation resistance of high-Nb-TiAl alloy |
| CN114808073A (en) * | 2022-05-10 | 2022-07-29 | 上海交通大学 | Method for improving anti-stripping performance of high-temperature alloy oxide film |
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