CN110219034A - Titanium alloy micro-arc oxidation electrolyte, method and products thereof - Google Patents
Titanium alloy micro-arc oxidation electrolyte, method and products thereof Download PDFInfo
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- CN110219034A CN110219034A CN201810173085.1A CN201810173085A CN110219034A CN 110219034 A CN110219034 A CN 110219034A CN 201810173085 A CN201810173085 A CN 201810173085A CN 110219034 A CN110219034 A CN 110219034A
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- titanium alloy
- arc oxidation
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- oxidation electrolyte
- electrolyte
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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
- C25D11/024—Anodisation under pulsed or modulated current or potential
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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
- 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
Abstract
The present invention relates to technical field of micro-arc oxidization, it is specifically related to a kind of titanium alloy micro-arc oxidation electrolyte, method and products thereof.Titanium alloy micro-arc oxidation electrolyte of the invention includes: sodium metasilicate 10-25g/L, and sodium phosphate 5-10g/L, alkaline conditioner 12-15g/L, coalescing agent 5-10g/L, ammonium vanadate 8-12g/L, organic ammonium salt 15-20g/L, solvent is deionized water.Titanium alloy differential arc oxidation method of the invention includes: that (1) prepares micro-arc oxidation electrolyte；(2) mao power source is set；(3) using titanium alloy sample as anode, differential arc oxidation is carried out by cathode of stainless steel plate；(4) it cleans the titanium alloy sample and dries.Compared to the prior art, titanium alloy micro-arc oxidation electrolyte of the invention does not need additionally to add alumina powder, needs not move through heating in vacuum yet, can be directly used as the micro-arc oxidation electrolyte of titanium alloy；One layer of fine and close black ceramic membrane is obtained, with hardness height, scratch resistance is good, highly resistance is salt fog, antioxidant is good, is suitable for mass operation.
Description
[technical field]
The present invention relates to technical field of micro-arc oxidization, be specifically related to a kind of titanium alloy micro-arc oxidation electrolyte, method and
Its product.
[background technique]
Titanium is a kind of important structural metal to grow up the 1950s, and titanium alloy intensity is high, corrosion resistance is good, resistance to
Hot height has more application in the fields such as aerospace industry, chemical industry, pharmaceutical engineering.Differential arc oxidation is micro- etc.
Gas ions surface ceramic deposition technology is referred on the basis of common anode oxidation, is enhanced using arc discharge and activated in anode
The reaction of upper generation, thus forming high-quality reinforcing ceramic membrane by the workpiece surface of material of aluminium, titanium, magnesium metal and its alloy
Method.Therefore, black ceramic membrane is prepared as a focus on research direction in titanium alloy surface by way of differential arc oxidation.
In the black ceramic membrane for preparing titanium alloy it is many in the prior art, 1 Chinese patent literature of documents
200710188529.0 disclose a kind of method for preparing titanium alloy black ceramic membrane: i.e. first by titanium alloy carry out anodic oxidation or
Then differential arc oxidation is placed in vacuum again after washing drying and is thermally formed black oxidation titanium film；It need to be in vacuum ring using the method
It is heated under border, process conditions are more demanding.2 Chinese patent literature 201310029887.2 of documents discloses a kind of titanium alloy
Surface black high temperature coatings preparation method: being added Al alloy powder in electrolyte and alumina powder carries out differential arc oxidation；
Preparation use need to just can be carried out with medicament and pure aluminium powder are modified using the method, technical process is relatively complicated.
In view of this, it is really necessary to develop a kind of more easy titanium alloy micro-arc oxidation electrolyte of process for preparation and the differential of the arc
Method for oxidation, to solve the above problems.
[summary of the invention]
Therefore, the purpose of the present invention is to provide a kind of titanium alloy micro-arc oxidation electrolytes, method and products thereof.
Titanium alloy micro-arc oxidation electrolyte of the invention includes:
Solvent is deionized water.
Preferably, the ratio of the sodium metasilicate and sodium phosphate is 0.8:1.
Preferably, the alkaline conditioner is sodium hydroxide, pH value is 12.0 or more.
Preferably, the coalescing agent is potassium fluoride.
Preferably, the organic ammonium salt is hexamethylenetetramine, the ratio of the ammonium vanadate and hexamethylenetetramine is 1:
2.5。
Titanium alloy differential arc oxidation method of the invention includes:
(1) micro-arc oxidation electrolyte is prepared；
(2) mao power source is set；
(3) using titanium alloy sample as anode, differential arc oxidation is carried out by cathode of stainless steel plate；
(4) it cleans the titanium alloy sample and dries.
Preferably, the mao power source is 250A750V type unidirectional pulse power supply.
Preferably, the titanium alloy sample is TC4 titanium alloy.
Preferably, the titanium alloy differential arc oxidation method further includes step (5), i.e., salt fog is carried out to the titanium alloy sample
Test, scratch resistance performance test, hydrolysis test.
The invention also includes a kind of titanium alloy products handled using the titanium alloy micro-arc oxidation electrolyte.
Compared to the prior art, titanium alloy micro-arc oxidation electrolyte of the invention does not need additionally to add alumina powder,
Heating in vacuum is needed not move through, the differential arc oxidation of titanium alloy can be directly used as.It can be obtained after differential arc oxidation in titanium alloy surface
The black ceramic membrane fine and close to one layer has the advantages that hardness is high, scratch resistance is good, highly resistance is salt fog, antioxidant is good；The present invention
Titanium alloy micro-arc oxidation electrolyte process for preparation it is simple, be suitable for titanium alloy high-volume differential arc oxidation operation.
[specific embodiment]
Preferred embodiments below is provided with regard to the present invention.
Selecting TC4 titanium alloy is sample made of material.Then abundant degreasing degreasing processing is carried out to the sample, by sample
It is put into ultrasonic cleaning 5-10 minutes in the mixing cleaning agent of acetone and dehydrated alcohol.It is then placed in oven, in 150 DEG C of temperature
It is under degree, sample drying is spare.
Micro-arc oxidation electrolyte is configured, the present embodiment selects 20g/L sodium metasilicate and 8g/L sodium phosphate, the usage ratio of the two
For 0.8:1, the coalescing agent potassium fluoride of 10g/L is added after mixing, and adds the sodium hydroxide of 15g/L, adjust electrolyte PH to
12 or more.It is eventually adding color additive i.e. 10g/L ammonium vanadate and 20g/L hexamethylenetetramine, usage ratio 1:2.5.It is mixed
Conjunction, which stirs evenly, is made micro-arc oxidation electrolyte.
Mao power source is set, and it is the unidirectional pulse power supply that 250A voltage is 750V that the present embodiment was selected, which is electric current,.
Using TC4 titanium alloy sample as anode, stainless steel plate powers on as cathode to carry out differential arc oxidation operation.The present embodiment
Current density be set as 8A/dm2, voltage is set as 410V, frequency 600Hz, duty ratio 20%, and the differential arc oxidation time is
10min。
After the completion of differential arc oxidation, the fine and close black that a layer thickness is 7um and uniform color is generated in titanium alloy specimen surface
Oxidation film.With pure water washed samples micro-arc oxidation electrolyte remained on surface, then sample is dried 60 minutes at 150 DEG C.
A series of performance tests finally are carried out to the titanium alloy sample that differential arc oxidation is completed.
As seen from the above table, the salt spray test of titanium alloy sample, scratch resistance performance test, hydrolysis test are all satisfied after differential arc oxidation
Associated test standards.
Wherein, the usage ratio Different Effects film forming speed of electrolyte host agent sodium metasilicate and sodium phosphate, specifically, working as phosphorus
When sour na concn is higher, the film forming speed of micro-arc oxidation films is more faster；And sodium silicate silicate is then related to arcing voltage.
Wherein, the usage ratio of color additive ammonium vanadate and hexamethylenetetramine is different, then titanium alloy specimen surface
Ceramic membrane color has difference.Concrete reason is that different face can be presented in different valence states for the vanadium radical ion in ammonium vanadate
Color, when+trivalent are navy blue when being black ,+4 valence, and to allow vanadium ion in different valence state, key is the hydrogen ion in solution
Concentration, therefore a large amount of hydrionic hexamethylenetetramines can be precipitated in addition, be in vanadium ion between+3 and+4 valence states, to make
Titanium surface deposits the micro-arc oxidation films of one layer of black.
Wherein, in above-described embodiment clean titanium alloy sample when, can be used acetone and dehydrated alcohol mixture and
It uses individually.Washes of absolute alcohol is mostly used in laboratory, and multi-purpose aqueous acetone solution is clear when batch processing on production line
It washes.
Wherein, TC4 titanium alloy refers to that the group of TC4 material becomes the titanium alloy of Ti-6Al-4V, belongs to (alpha+beta) Type Titanium Alloy,
With good comprehensive mechanics mechanical performance, specific strength is big.
Microarc oxidation electrolyte formula of the invention is in being capable of forming micro-arc oxidation films, this implementation within the scope of respective concentration
Example is only chosen wherein one group of concentration and is illustrated.
The above differential arc oxidation electrical parameter may be arranged as current density 5-10A/dm2, voltage 370-450V, frequency
600Hz, duty ratio 20%, differential arc oxidation time are 8-15min, can finally obtain the fine and close black oxide film of 5-25um.Electricity
Parameter and oxidization time are different, and having on film forming thickness influences.The present embodiment only has chosen the preferable one group of electrical parameter of effect.
Micro-arc oxidation electrolyte configuration process of the invention is simple, the high-volume differential of the arc oxygen suitable for titanium alloy on production line
It is turned into industry.
It should be pointed out that the present invention is not limited to the above embodiments, any person skilled in the art is based on this
Inventive technique scheme both falls within protection of the invention to any simple modification, equivalent change and modification made by above-described embodiment
In range.
Claims (10)
1. a kind of titanium alloy micro-arc oxidation electrolyte, characterized in that it comprises:
2. titanium alloy micro-arc oxidation electrolyte according to claim 1, which is characterized in that the sodium metasilicate and sodium phosphate
Ratio is 0.8:1.
3. titanium alloy micro-arc oxidation electrolyte according to claim 1, which is characterized in that the alkaline conditioner is hydrogen-oxygen
Change sodium, pH value is 12.0 or more.
4. titanium alloy micro-arc oxidation electrolyte according to claim 1, which is characterized in that the coalescing agent is fluorination
Potassium.
5. titanium alloy micro-arc oxidation electrolyte according to claim 1, which is characterized in that the organic ammonium salt is six first
The ratio of urotropine, the ammonium vanadate and hexamethylenetetramine is 1:2.5.
6. a kind of titanium alloy differential arc oxidation method, to use the titanium alloy differential of the arc oxygen as described in any one of claim 1 to 5
Change the method for electrolyte processing, which comprises the steps of:
(1) micro-arc oxidation electrolyte is prepared；
(2) mao power source is set；
(3) using titanium alloy sample as anode, differential arc oxidation is carried out by cathode of stainless steel plate；
(4) it cleans the titanium alloy sample and dries.
7. titanium alloy differential arc oxidation method according to claim 6, which is characterized in that the mao power source is
250A750V type unidirectional pulse power supply.
8. titanium alloy differential arc oxidation method according to claim 6, which is characterized in that the titanium alloy sample is TC4 titanium
Alloy.
9. titanium alloy differential arc oxidation method according to claim 6, which is characterized in that the titanium alloy differential arc oxidation method
Further include step (5), i.e., salt spray test, scratch resistance performance test, hydrolysis test is carried out to the titanium alloy sample.
10. a kind of titanium alloy product, which is characterized in that it is micro- using the titanium alloy as described in any one of claim 1 to 5
The titanium alloy product that arc oxidation electrolyte is handled.
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| CN201810173085.1A CN110219034A (en) | 2018-03-02 | 2018-03-02 | Titanium alloy micro-arc oxidation electrolyte, method and products thereof |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101660190A (en) * | 2009-09-18 | 2010-03-03 | 西北有色金属研究院 | Preparation method of titanium and titanium alloy surface black protective film for surgical implantation |
| CN102230205A (en) * | 2011-06-20 | 2011-11-02 | 华南理工大学 | Aluminum alloy micro-arc oxidation black ceramic membrane and preparation method thereof |
| CN103173836A (en) * | 2012-11-22 | 2013-06-26 | 华南理工大学 | Magnesium alloy microarc oxidation low energy consumption black ceramic coating and preparation method thereof |
| CN104651908A (en) * | 2013-11-25 | 2015-05-27 | 中国兵器科学研究院宁波分院 | Preparation method and hole sealing method of magnesium alloy surface ceramic coating |
-
2018
- 2018-03-02 CN CN201810173085.1A patent/CN110219034A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101660190A (en) * | 2009-09-18 | 2010-03-03 | 西北有色金属研究院 | Preparation method of titanium and titanium alloy surface black protective film for surgical implantation |
| CN102230205A (en) * | 2011-06-20 | 2011-11-02 | 华南理工大学 | Aluminum alloy micro-arc oxidation black ceramic membrane and preparation method thereof |
| CN103173836A (en) * | 2012-11-22 | 2013-06-26 | 华南理工大学 | Magnesium alloy microarc oxidation low energy consumption black ceramic coating and preparation method thereof |
| CN104651908A (en) * | 2013-11-25 | 2015-05-27 | 中国兵器科学研究院宁波分院 | Preparation method and hole sealing method of magnesium alloy surface ceramic coating |
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