CN108103552A - For the technique of TA2 titanium alloy material thick film anodes - Google Patents
For the technique of TA2 titanium alloy material thick film anodes Download PDFInfo
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- CN108103552A CN108103552A CN201711211671.2A CN201711211671A CN108103552A CN 108103552 A CN108103552 A CN 108103552A CN 201711211671 A CN201711211671 A CN 201711211671A CN 108103552 A CN108103552 A CN 108103552A
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- anodic 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
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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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Abstract
The invention belongs to field of material surface treatment, are related to a kind of technique mainly for TA2 titanium alloy material thick film anodes, the step of including anodic oxidation, carry out anodic oxidation using superimposed pulses mode during anodic oxidation, the basic voltage of superimposed pulses is 80V；The pulse voltage of anodic oxidation is 180V 220V；The duty cycle of anodic oxidation is 1/2；Tank liquor temperature during anodic oxidation is 6 ± 2 DEG C；The reaction time of anodic oxidation includes slow opening 1 minute time, anodising time 50 70 minutes and ramp down time would 1 minute；It is slow that open the time be the time risen to from no-voltage used in basic voltage；Ramp down time would is the time being down to from basic voltage used in no-voltage.A kind of technique for TA2 titanium alloy material thick film anodes for the pollution that can reach 8 10 microns the present invention provides thicknesses of layers, corrosion resistance can be significantly improved and prevent other metal impurities such as iron.
Description
Technical field
The invention belongs to field of material surface treatment, are related to a kind of material anodic process more particularly to a kind of main pin
To the technique of TA2 titanium alloy material thick film anodes.
Background technology
TA2 titanium alloys are industrially pure titaniums, be mainly used as the operating temperatures such as chemical industry, shipbuilding and medical treatment below 350 DEG C by
The little anti-corrosion part of power.With high specific strength, light-weight, heat resistance is strong and many advantages such as corrosion-resistant.In titanium alloy
Part is in preparation process if surface is by iron contamination, in the dielectric, titanium and iron formation micro cell, in electrochemical action
Under, hydrogen is made to penetrate into titanium, causes the hydrogenation of titanium and becomes fragile, the service life and safety of critical titanium alloy component.To titanium alloy into
Row anodization enhances its corrosion resistance and prevents iron contamination.In HB/Z 347-2002《Titanium and its alloy anode oxidation work
Skill and quality inspection》In provide the technological parameter of the 8-10 such as TC4, TC6 microns of thick film anode, do not provide TA2 thick films 8-10
The anode oxidation process parameter of micron.Meanwhile periodicals and magazines both domestic and external, there are no carry out 8-10 specifically for TA2 titanium alloys
The data of micron Thick film anodizing.
Ti-alloy anode thicknesses of layers is according to material trademark and treatment process difference.TA2 material chemical composition contents
It is shown in Table 1.
The chemical analysis content of 1 TA2 of table
| Fe | C | N | H | O |
| ≤ 0.3% | ≤ 0.1% | ≤ 0.05% | ≤ 0.015% | ≤0.25 |
The content of the invention
In order to solve above-mentioned technical problem present in background technology, the present invention provides a kind of thicknesses of layers can reach 8-
10 microns, the pollution that corrosion resistance can be significantly improved and prevent other metal impurities such as iron be used for TA2 titanium alloy material thick films
The technique of anodization.
To achieve these goals, the present invention adopts the following technical scheme that：
A kind of technique for TA2 titanium alloy material thick film anodes, the step of including anodic oxidation, it is characterised in that：
Anodic oxidation is carried out using superimposed pulses mode during the anodic oxidation, the basic voltage of the superimposed pulses is 80V；The sun
The pulse voltage of pole oxidation is 180V-220V；The duty cycle of the anodic oxidation is 1/2；Tank liquor temperature during the anodic oxidation
Degree is 6 ± 2 DEG C；The reaction time of the anodic oxidation includes slow opening 1 minute time, anodising time 50-70 minute and delaying
1 minute time dropped；It is described that slow to open the time be the time risen to from no-voltage used in basic voltage；The ramp down time would is from basis
Voltage is down to the time used in no-voltage.
The burst length of above-mentioned anodic oxidation is 0.5S.
The final concentration of component and component is respectively in tank liquor during above-mentioned anodic oxidation：Sulfuric acid 200-220mL/L, phosphoric acid
15-25mL/L、Ti 4+5 g/l of ＜ and surplus are distilled water or deionized water；The density of the sulfuric acid is 1.84g/mL；Institute
The density for stating phosphoric acid is 1.7g/mL.
The step of being stirred with clean compressed air is further included while above-mentioned anodic oxidation.
It is an advantage of the invention that：
The present invention provides a kind of technique for TA2 titanium alloy material thick film anodes, mainly from change process
It tested, groped and is improved, including tank liquor formula, pulse voltage, tank liquor temperature, duty cycle and oxidization time etc.,
By tank liquor formula, pulse voltage, tank liquor temperature, the mutual synergistic effect of duty cycle and oxidization time in terms of these, sun
Polarization thicknesses of layers reaches 8-10 microns, can significantly improve its corrosion resistance and prevent the pollution of other metal impurities such as iron, fill out
Mend blank of the material in anodic oxidation thick-film technique.
Description of the drawings
Fig. 1 is oxidization time of the present invention and pulse voltage curved line relation schematic diagram；
Fig. 2 is the flow diagram of the technique provided by the present invention for TA2 titanium alloy material thick film anodes.
Specific embodiment
The present invention provides a kind of technique for TA2 titanium alloy material thick film anodes, with existing technique in principle
On be all identical, referring to Fig. 2, all including anodic oxidation the step of, unlike, the present invention is adopted in anode oxidation process
Technological parameter is entirely different, and technological parameter of the present invention can not be groped simultaneously by the experiment of limited number of time
It obtains, specifically, the technique provided by the present invention for TA2 titanium alloy material thick film anodes, especially anodic oxidation
When technique it is as follows：Anodic oxidation (referring to Fig. 1), the basis electricity of superimposed pulses are carried out using superimposed pulses mode during anodic oxidation
Pressure is 80V；The pulse voltage of anodic oxidation is 180V-220V；The duty cycle of anodic oxidation is 1/2；Tank liquor during anodic oxidation
Temperature is 6 ± 2 DEG C；The reaction time of anodic oxidation includes slow opening 1 minute time, anodising time 50-70 minute and slow dropping
1 minute time；It is slow that open the time be the time risen to from no-voltage used in basic voltage；Ramp down time would is to be down to zero from basic voltage
Time used in voltage.
The burst length of anodic oxidation is 0.5S；Further include what is be stirred with clean compressed air while anodic oxidation
Step.
At the same time, the tank liquor when present invention is also to anodic oxidation redesigns, the tool of the tank liquor of the anodic oxidation
Body formula is：Sulfuric acid 200-220mL/L (final concentration), phosphatase 11 5-25mL/L (final concentration), Ti4+5 g/l of ＜ (final concentration) with
And surplus is distilled water or deionized water；Wherein, sulfuric acid is the concentrated sulfuric acid, and the density of sulfuric acid is 1.84g/mL；The density of phosphoric acid is
1.7g/mL。
Present invention is generally directed to material for spaceport pump part TA2 titanium alloy materials in sulfuric-phosphoric solution into sun
Pole aoxidizes, and the anodic film layer thickness of such material is reached 8-10 microns, improves its corrosion resistance and prevents other gold such as iron
Belong to the pollution of impurity, fill up blank of the material in anodic oxidation thick-film technique.
Continuous adjustment tank formula of liquid and technological parameter divide three phases (parameter stage of fumbling, examination in sulfuric-phosphoric solution
Verification, the processing of formal part) it is tested, draw the superimposed pulses pattern using 200A/300V Anodizing power supplies.
The present invention is mainly tested from change process, including tank liquor formula, pulse voltage, tank liquor temperature, duty
Than oxidization time etc..The following table 2 counts for the situation of main experiment several times.
2 TA2 exemplar anodization test situation of table is detailed
| Sequence number | Part situation | Pulse voltage (V) | Tank liquor temperature | Duty cycle | Oxidization time | Thicknesses of layers (μm) | Remarks |
| 1 | TA2 exemplars | 180 | 6 | 1/2 | 60 | 9 | It meets the requirements |
| 2 | TA2 exemplars | 190 | 8 | 1/2 | 70 | 10 | It meets the requirements |
| 3 | TA2 exemplars | 200 | 4 | 1/2 | 50 | 8 | It meets the requirements |
| 4 | TA2 exemplars | 210 | 6 | 1/2 | 60 | 10 | It meets the requirements |
| 5 | TA2 exemplars | 200 | 8 | 1/2 | 60 | 10 | It meets the requirements |
| 6 | TA2 exemplars | 190 | 6 | 1/2 | 70 | 9 | It meets the requirements |
It is tested by multiple authentication, thicknesses of layers reaches 8-10 microns.
Binding tests situation should be noted：
Note：
A, operating personnel must tape insulation gloves, wear insulated shoes, operating personnel do not allow catalytic oxidation slot during energization, in order to avoid
Electric injury.
B, must every two axis to tank liquor carry out once analyze (whether elder generation's visual inspection electrolytic cell leaks during analytical sampling), analysis item
Mesh includes the content of sulfuric acid, phosphoric acid and titanium ion, carries out analysis and adjustment record, and properly preserves.
If Ti content, more than 5 g/l, whole slot tank liquor is scrapped, and reconfigures tank liquor.It reconfigures tank liquor method and sees guidance
Book-groove liquid is analyzed and collocation method.
C, to equipment and power-source maintenance is controlled once daily.
D, anodizing time can be adjusted according to part thicknesses of layers, can generally be floated downwards 10 minutes, upwards
10 minutes.
E, whole operation process must have two operating personnel and more than at the scene be responsible for monitoring.
F, in the case where stopping the supple of gas or steam (compressed air), having a power failure, by operator immediately within three minutes by part from anode
Change and taken out in slot, carry out static cleaning, flowing cleaning process immediately after.
G, according to titanium alloy pulse Anodizing power supply specification, power supply control accuracy：± 5%, allow due to power-supply device
Current error ± 10A caused by itself.
H, part is not processed anodization slot and should be capped, and prevents tank liquor cross contamination.
Embodiment
1) present invention is a kind of tank liquor formula and anodization process for TA2 titanium alloy thick film anodes.It is right
XX03020-20-01 parts carry out anodic oxidation.
2) tank liquor formula is：
Sulfuric acid (H2SO4, ρ=1.84g/mL) and it is prepared by 200mL/L；
Phosphoric acid (H3PO4, ρ=1.7g/mL) and it is prepared by 20mL/L；
Ti4+5 g/l of ＜；
Remaining is distilled water or deionized water.
Anodic oxidation is carried out using superimposed pulses mode：Pulse voltage 200V, duty cycle 1/2；
Anodization temperature：6℃；
Compressed air stirs；
Anodising time (does not include delaying opening time and ramp down time would)：50min；
It is slow to open the time：1min；
Ramp down time would：1min；
To voltage should rise to 80V in 1 minute after electricity, anodic oxidation, burst length are carried out using superimposed pulses mode
0.5 second, anodic oxidation is carried out using superimposed pulses mode, after anodic oxidation in 1 minute by voltage will be 0.
3) result of the test：Film layer appearance is the grey of uniformly continuous, and thickness is 8 microns.
Claims (4)
1. a kind of technique for TA2 titanium alloy material thick film anodes, the step of including anodic oxidation, it is characterised in that：Institute
Anodic oxidation is carried out using superimposed pulses mode when stating anodic oxidation, the basic voltage of the superimposed pulses is 80V；The anode
The pulse voltage of oxidation is 180V-220V；The duty cycle of the anodic oxidation is 1/2；The tank liquor temperature during anodic oxidation
It is 6 ± 2 DEG C；The reaction time of the anodic oxidation includes slow opening 1 minute time, anodising time 50-70 minute and slow dropping
1 minute time；It is described that slow to open the time be the time risen to from no-voltage used in basic voltage；The ramp down time would is from basic electricity
Time used in pressure drop to no-voltage.
2. the technique according to claim 1 for TA2 titanium alloy material thick film anodes, it is characterised in that：The sun
The burst length of pole oxidation is 0.5S.
3. the technique according to claim 1 or 2 for TA2 titanium alloy material thick film anodes, it is characterised in that：It is described
The final concentration of component and component is respectively in tank liquor during anodic oxidation：Sulfuric acid 200-220mL/L, phosphatase 11 5-25mL/L, Ti4+
5 g/l of ＜ and surplus are distilled water or deionized water；The density of the sulfuric acid is 1.84g/mL；The density of the phosphoric acid is
1.7g/mL。
4. the technique according to claim 3 for TA2 titanium alloy material thick film anodes, it is characterised in that：The sun
Pole further includes the step of being stirred with clean compressed air while oxidation.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201711211671.2A CN108103552A (en) | 2017-11-28 | 2017-11-28 | For the technique of TA2 titanium alloy material thick film anodes |
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| CN201711211671.2A CN108103552A (en) | 2017-11-28 | 2017-11-28 | For the technique of TA2 titanium alloy material thick film anodes |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110863227A (en) * | 2019-11-07 | 2020-03-06 | 西安工业大学 | Titanium alloy pulse-direct current anodic oxidation surface treatment method |
| CN111826700A (en) * | 2020-07-27 | 2020-10-27 | 上海市特种设备监督检验技术研究院 | Pickling and passivating combined liquid for anodizing titanium material and pickling and passivating method |
| CN115961323A (en) * | 2022-12-05 | 2023-04-14 | 中国航发长春控制科技有限公司 | Device and process for strengthening surface of TC6 titanium alloy inner cavity with double-cylinder structure |
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| CN1403632A (en) * | 2002-10-10 | 2003-03-19 | 上海交通大学 | Macroporous thick-film process for anode oxidization of phosphoric acid |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110863227A (en) * | 2019-11-07 | 2020-03-06 | 西安工业大学 | Titanium alloy pulse-direct current anodic oxidation surface treatment method |
| CN111826700A (en) * | 2020-07-27 | 2020-10-27 | 上海市特种设备监督检验技术研究院 | Pickling and passivating combined liquid for anodizing titanium material and pickling and passivating method |
| CN115961323A (en) * | 2022-12-05 | 2023-04-14 | 中国航发长春控制科技有限公司 | Device and process for strengthening surface of TC6 titanium alloy inner cavity with double-cylinder structure |
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