CN101798702A - Titanium and titanium alloy electrochemically polish electrolyte and surface polishing method thereof - Google Patents
Titanium and titanium alloy electrochemically polish electrolyte and surface polishing method thereof Download PDFInfo
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- CN101798702A CN101798702A CN201010101279A CN201010101279A CN101798702A CN 101798702 A CN101798702 A CN 101798702A CN 201010101279 A CN201010101279 A CN 201010101279A CN 201010101279 A CN201010101279 A CN 201010101279A CN 101798702 A CN101798702 A CN 101798702A
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- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims abstract description 44
- 239000010936 titanium Substances 0.000 title claims abstract description 44
- 238000000034 method Methods 0.000 title claims abstract description 39
- 229910001069 Ti alloy Inorganic materials 0.000 title claims abstract description 38
- 238000005498 polishing Methods 0.000 title claims abstract description 34
- 239000003792 electrolyte Substances 0.000 title claims abstract description 12
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 42
- 230000003647 oxidation Effects 0.000 claims abstract description 36
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 36
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 28
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 26
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000008367 deionised water Substances 0.000 claims abstract description 10
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 10
- 239000008151 electrolyte solution Substances 0.000 claims description 37
- 238000005530 etching Methods 0.000 claims description 13
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 6
- 230000001105 regulatory effect Effects 0.000 claims description 5
- 239000002904 solvent Substances 0.000 claims description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 4
- 238000011010 flushing procedure Methods 0.000 claims description 4
- 229910002804 graphite Inorganic materials 0.000 claims description 4
- 239000010439 graphite Substances 0.000 claims description 4
- 229910052697 platinum Inorganic materials 0.000 claims description 4
- 238000002360 preparation method Methods 0.000 claims description 4
- 238000002203 pretreatment Methods 0.000 claims description 4
- 239000004576 sand Substances 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- 238000005868 electrolysis reaction Methods 0.000 claims description 3
- 230000007613 environmental effect Effects 0.000 abstract description 4
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 abstract description 2
- 229910052751 metal Inorganic materials 0.000 description 8
- 239000002184 metal Substances 0.000 description 8
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 description 4
- AFVFQIVMOAPDHO-UHFFFAOYSA-N Methanesulfonic acid Chemical compound CS(O)(=O)=O AFVFQIVMOAPDHO-UHFFFAOYSA-N 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 210000004400 mucous membrane Anatomy 0.000 description 2
- 210000002345 respiratory system Anatomy 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 230000003746 surface roughness Effects 0.000 description 2
- 230000001988 toxicity Effects 0.000 description 2
- 231100000419 toxicity Toxicity 0.000 description 2
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- 208000027418 Wounds and injury Diseases 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 125000002091 cationic group Chemical group 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000006056 electrooxidation reaction Methods 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 208000014674 injury Diseases 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
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Abstract
The invention discloses a titanium and titanium alloy electrochemically polish electrolyte and a surface polishing method thereof. The electrolyte comprises the following components by mass percent: 1-3% of hydrofluoric acid, 20-30% of deionized water and balance of glycol. The polishing method comprises the following steps: (1) preparing the electrolyte; (2) carrying out anodic oxidation treatment; and (3) removing an oxide layer. Smooth titanium and titanium alloy surfaces can be obtained by utilizing the electrolyte for carrying out polishing treatment. The electrolyte has good safety and environmental protection.
Description
Technical field
The present invention relates to the metal surface polishing technical field, specifically, relate to a kind of titanium or titanium alloy electrochemical etching electrolytic solution and surface polishing method thereof.
Background technology
Advantages such as the titanium or titanium alloy material has that density is little, specific tenacity is high, excellent anti-corrosion performance, hot strength and excellent in low temperature toughness have been widely used in fields such as aerospace, nuclear industry, oil, chemical industry and daily living article.The production of titanium or titanium alloy goods for needs attractive in appearance or that assembling cooperates, often needs to carry out surface finish and handles.Surface finishing processing generally can be carried out by methods such as mechanical polishing, chemical rightenning, electrochemical etchings in the titanium or titanium alloy surface.Wherein, cost is low, efficient is high, polishing effect is good, polished surface is not limited to characteristics such as plane owing to having for electrochemical etching, has general application in industry.
Electrochemical etching provides electric current by means of power supply, and workpiece generally is connected to anode, at anode metal/electrolyte interface generation burning, oxide compound by electrolytic solution dissolved process.Dissolution process, metal breaks away from anode with cationic form and enters in the solution.The electrolytic solution of traditional titanium or titanium alloy electrochemical etching is generally and contains perchloric acid electrolytic solution (as CN101148774A) and hydrofluoric acid containing electrolytic solution (as CN1358240A).Perchloric acid has combustion-supporting property, and temperature is too high easily explosion caused, and has strong corrosion, and is dangerous high.The hydrofluoric acid volatility is stronger, and protection can not cause the grievous injury of human respiratory tract's mucous membrane, skeleton and tooth at that time, and HF content is higher in traditional hydrofluoric acid electrolytic solution, and volatilization seriously is unfavorable for the life-time service of workers ' health and equipment in the production process.Disclosed a United States Patent (USP) in 2008 and be applied to the surface of metal titanium polishing, it is essentially consist (US2008/0217186A1) with the methylsulfonic acid.Methylsulfonic acid has intense stimulus to mucous membrane, the upper respiratory tract, eye and skin, the human body of can burning, and easily cause water body and topsoil, so methylsulfonic acid electrolytic solution also has strong toxicity.
Therefore, the electrochemical electrolysis liquid of titanium or titanium alloy all has stronger toxicity and hazardness at present.So the electrochemical etching technology of research and development low toxicity, safety, environmental protection has obvious significance.
Summary of the invention
The objective of the invention is shortcoming, the electrolytic solution of the titanium or titanium alloy electrochemical etching of a kind of safety, environmental protection is provided at the prior art existence.
The electrolytic solution of titanium or titanium alloy electrochemical etching provided by the invention comprises hydrofluoric acid 1～3 quality %, deionized water 20～30 quality %, and surplus is an ethylene glycol.Electrolytic solution of the present invention as key component, is made solvent with ethylene glycol with hydrofluoric acid and deionized water.By improving deionized water content in the electrolytic solution, keep lower hydrofluoric acid concentration (being lower than 3.0 quality %), eliminate the electrolytic solution irritating smell thereby reach, reduce the purpose that electrolytic solution directly endangers human body.
Another object of the present invention provides the method for utilizing above-mentioned electrolytic solution that the titanium or titanium alloy surface is polished.
Titanium or titanium alloy surface polishing method of the present invention comprises the steps:
(1) preparation electrolytic solution: make solvent with ethylene glycol, the massfraction of hydrofluoric acid is 1～3 quality %, and deionized water quality mark is 20～30 quality %;
(2) anodic oxidation treatment: as anodic oxidation power supply, workpiece is connected on anode with D.C. regulated power supply, the negative electrode of power supply connects stereotype, graphite cake, titanium plate or platinized platinum; Anode and negative electrode be dipped in the anodic oxidation electrolyte handle; The core procedure of titanium or titanium alloy surface polishing method of the present invention is an anodic oxidation treatment.
(3) the deoxidation layer is handled: the gained workpiece is carried out drying, and then be dipped in Rinsing Area, and supersound process, zone of oxidation comes off, and takes out workpiece and dries.Workpiece surface after second step handled has the translucent zone of oxidation of one deck, and this step purpose is for removing this zone of oxidation.Workpiece after the anodic oxidation treatment is cleaned up in clear water.Dry.Zone of oxidation occurs slightly coming off owing to stress at this moment.This workpiece is dipped in the Rinsing Area supersound process once more greater than 5min.Zone of oxidation will all come off, and workpiece be taken out dry.
In above-mentioned titanium or titanium alloy surface polishing method, adopt D.C. regulated power supply as anodic oxidation power supply, the scope of voltage of supply is 10V～120V.
In above-mentioned titanium or titanium alloy surface polishing method, the thermostat temperature of described electrolytic solution is 10～40 ℃.
In above-mentioned titanium or titanium alloy surface polishing method, workpiece is connected on anode, the negative electrode of power supply connects stereotype, graphite cake, titanium plate or platinized platinum; Anode workpiece and cathode-workpiece spacing are 5～30mm.
In above-mentioned titanium or titanium alloy surface polishing method, anode and negative electrode are dipped in when carrying out electrolysis in the electrolytic solution, electrolytic solution is stirred, its stirring velocity is 0～600rpm.
In above-mentioned titanium or titanium alloy surface polishing method, the anodic oxidation polishing time is 1～10h.
In above-mentioned titanium or titanium alloy surface polishing method, the time of described supersound process is greater than 5min.
In above-mentioned titanium or titanium alloy surface polishing method, before anodic oxidation treatment, workpiece is carried out pre-treatment, described pre-treatment is: use 400 orders, 600 orders, 800 orders, 1000 orders and 1200 order sand papering workpiece respectively, and clean with flushing with clean water.
Compared with prior art, the present invention has following useful result:
1, the electrolytic solution of titanium or titanium alloy electrochemical etching provided by the invention in glycol system, increases the dissolving that water-content can aggravate oxide compound, and the order of disruptive oxidation film also reduces its thickness.In the fluorine-containing ethylene glycol solution of high water content, carry out anodic oxidation,, generate loose porous oxide film on the titanium or titanium alloy surface, and make the metal base leveling by electrochemical oxidation and solvency action.Remove oxide film, can obtain smooth titanium and titanium alloy surface.Owing to improve deionized water content in the electrolytic solution, keep lower hydrofluoric acid concentration (being lower than 3.0 quality %) in addition, eliminate the electrolytic solution irritating smell, reduce the purpose that electrolytic solution directly endangers human body thereby reach.This electrolytic solution has the good security and the feature of environmental protection.
2, utilize electrolytic solution of the present invention and finishing method to handle after, gained workpiece surface mirror-smooth presents certain glossiness.Surface roughness parameter is: profile arithmetic average error is about 34nm, and 10 of nao-and micro reliefs highly are about 118nm, and maximum height of the profile is about 184nm.
Description of drawings
Fig. 1 is the scanning electron microscope picture under the titanium metal workpiece high power before glossing is handled.
Fig. 2 is the scanning electron microscope picture under the titanium metal workpiece high power after the glossing processing.
Fig. 3 is atomic force microscope picture and the profile analysis result of titanium metal workpiece 30 * 30 μ m after glossing is handled.
Fig. 4 is the current density-time curve in the anodic oxidation treatment process.
Embodiment
Embodiment 1
The polishing of the first step workpiece:
Use 400 orders, 600 orders, 800 orders, 1000 orders and 1200 order SiC sand papering workpiece respectively, and clean with flushing with clean water.Dry stand-by.
Second step preparation anodic oxidation electrolyte: electrolytic solution is made solvent with ethylene glycol, and the massfraction of hydrofluoric acid is 1% in the electrolytic solution, and deionized water quality mark is 20%.
The 3rd step anodic oxidation treatment: as anodic oxidation power supply, workpiece is connected on anode with D.C. regulated power supply, the negative electrode of power supply connects stereotype.Anode workpiece and negative electrode stereotype be dipped in the anodic oxidation electrolyte handle.
Condition is:
Voltage of supply: 60V
Electrolytic solution thermostat temperature: 25 ℃
Anode workpiece and cathode-workpiece spacing: 10mm
Stirring velocity: do not have and stir
Anodic oxidation polishing time: 3h
The 4th step deoxidation layer is handled:
The 3rd step gained workpiece is carried out drying.After drying finishes, this workpiece is dipped in Rinsing Area once more, and supersound process 10min, zone of oxidation will all come off.The workpiece taking-up is dried.
The gained workpiece, surperficial mirror-smooth presents certain glossiness.Can judge that by scanning electron microscopic observation (Fig. 1) and atomic force microscope profile analysis (Fig. 2) the described glossing of this patent can obtain titanium or the titanium alloy product that workpiece surface is smooth, have certain glossiness.Surface roughness parameter is: profile arithmetic average error is about 34nm, and 10 of nao-and micro reliefs highly are about 118nm, and maximum height of the profile is about 184nm.Fig. 4 is current density-time curve in the anodic oxidation treatment process, and through behind the 1h, current curve tends towards stability, show anodic oxidation treatment 1h after, can reach the purpose of step 3, further anodic oxidation can increase the polishing degree of depth of workpiece surface.
The polishing of the first step workpiece:
Use 400 orders, 600 orders, 800 orders, 1000 orders and 1200 order SiC sand papering workpiece respectively, and clean with flushing with clean water.Dry stand-by.
Second step preparation anodic oxidation electrolyte: electrolytic solution is made solvent with ethylene glycol, and the massfraction of hydrofluoric acid is 3% in the electrolytic solution, and deionized water quality mark is 30%.
The 3rd step anodic oxidation treatment: identical with embodiment 1.
The 4th step deoxidation layer is handled:
The 3rd step gained workpiece is carried out drying.After drying finishes, this workpiece is dipped in Rinsing Area once more, and supersound process 10min, zone of oxidation will all come off.The workpiece taking-up is dried.
The gained workpiece, surperficial mirror-smooth presents certain glossiness.
Claims (10)
1. the electrolytic solution of a titanium or titanium alloy electrochemical etching is characterized in that comprising hydrofluoric acid 1～3 quality %, deionized water 20～30 quality %, and surplus is an ethylene glycol.
2. a titanium or titanium alloy surface polishing method comprises the method that adopts electrochemical etching, it is characterized in that the electrolytic solution that adopts in the described electrochemical etching is the described electrolytic solution of claim 1.
3. titanium or titanium alloy surface polishing method according to claim 2 is characterized in that comprising the steps:
(1) preparation electrolytic solution: make solvent with ethylene glycol, the massfraction of hydrofluoric acid is 1～3 quality %, and deionized water quality mark is 20～30 quality %;
(2) anodic oxidation treatment: as anodic oxidation power supply, workpiece is connected on anode with D.C. regulated power supply, the negative electrode of power supply connects stereotype, graphite cake, titanium plate or platinized platinum; Anode and negative electrode be dipped in the anodic oxidation electrolyte handle;
(3) the deoxidation layer is handled: the gained workpiece is carried out drying, and then be dipped in Rinsing Area, and supersound process, zone of oxidation comes off, and takes out workpiece and dries.
4. titanium or titanium alloy surface polishing method according to claim 3 is characterized in that adopting D.C. regulated power supply as anodic oxidation power supply, and the scope of voltage of supply is 10V～120V.
5. titanium or titanium alloy surface polishing method according to claim 3, the thermostat temperature that it is characterized in that described electrolytic solution is 10～40 ℃.
6. titanium or titanium alloy surface polishing method according to claim 3 is characterized in that workpiece is connected on anode, and the negative electrode of power supply connects stereotype, graphite cake, titanium plate or platinized platinum; Anode workpiece and cathode-workpiece spacing are 5～30mm.
7. titanium or titanium alloy surface polishing method according to claim 6 is characterized in that anode and negative electrode are dipped in when carrying out electrolysis in the electrolytic solution, and electrolytic solution is stirred, and its stirring velocity is 0～600rpm.
8. titanium or titanium alloy surface polishing method according to claim 3 is characterized in that the anodic oxidation polishing time is 1～10h.
9. titanium or titanium alloy surface polishing method according to claim 3, the time that it is characterized in that described supersound process is greater than 5min.
10. titanium or titanium alloy surface polishing method according to claim 3, it is characterized in that before anodic oxidation treatment, workpiece being carried out pre-treatment, described pre-treatment is: use 400 orders, 600 orders, 800 orders, 1000 orders and 1200 order sand papering workpiece respectively, and clean with flushing with clean water.
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| CN201010101279A CN101798702A (en) | 2010-01-22 | 2010-01-22 | Titanium and titanium alloy electrochemically polish electrolyte and surface polishing method thereof |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102198610A (en) * | 2011-04-18 | 2011-09-28 | 武汉飞米思科技有限公司 | Mirror polishing method for complex ceramic surface |
| CN102312277A (en) * | 2011-10-25 | 2012-01-11 | 厦门大学 | Electrochemical polishing electrolyte adopted for titanium and titanium alloy, use method thereof |
| CN102534744A (en) * | 2012-03-14 | 2012-07-04 | 淮阴工学院 | Polishing solution and polishing method for medical titanium alloy |
| CN102660765A (en) * | 2012-04-01 | 2012-09-12 | 南京工业大学 | Chemical preparation method of novel porous titanium |
| CN103014577A (en) * | 2013-01-05 | 2013-04-03 | 江苏大学 | Tissue superfining and electrochemical polishing based method for improving biomedical performance of titanium product |
| CN106567122A (en) * | 2017-02-17 | 2017-04-19 | 大博医疗科技股份有限公司 | Electrochemical polishing electrolyte and polishing method for titanium and titanium alloy |
| CN108221041A (en) * | 2016-12-21 | 2018-06-29 | 空中客车防务和空间有限责任公司 | For the method for the electrobrightening of metal base |
| CN114192802A (en) * | 2021-10-27 | 2022-03-18 | 北京星航机电装备有限公司 | Surface polishing method and device for additive manufacturing titanium alloy structure |
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2010
- 2010-01-22 CN CN201010101279A patent/CN101798702A/en active Pending
Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102198610A (en) * | 2011-04-18 | 2011-09-28 | 武汉飞米思科技有限公司 | Mirror polishing method for complex ceramic surface |
| CN102198610B (en) * | 2011-04-18 | 2014-08-20 | 武汉飞米思科技有限公司 | Mirror polishing method for complex ceramic surface |
| CN102312277B (en) * | 2011-10-25 | 2014-04-30 | 厦门大学 | Electrochemical polishing electrolyte adopted for titanium and titanium alloy, use method thereof |
| CN102312277A (en) * | 2011-10-25 | 2012-01-11 | 厦门大学 | Electrochemical polishing electrolyte adopted for titanium and titanium alloy, use method thereof |
| CN102534744A (en) * | 2012-03-14 | 2012-07-04 | 淮阴工学院 | Polishing solution and polishing method for medical titanium alloy |
| CN102660765A (en) * | 2012-04-01 | 2012-09-12 | 南京工业大学 | Chemical preparation method of novel porous titanium |
| CN102660765B (en) * | 2012-04-01 | 2016-03-30 | 南京工业大学 | A kind of preparation method of POROUS TITANIUM |
| CN103014577A (en) * | 2013-01-05 | 2013-04-03 | 江苏大学 | Tissue superfining and electrochemical polishing based method for improving biomedical performance of titanium product |
| CN103014577B (en) * | 2013-01-05 | 2015-05-27 | 江苏大学 | Tissue superfining and electrochemical polishing based method for improving biomedical performance of titanium product |
| CN108221041A (en) * | 2016-12-21 | 2018-06-29 | 空中客车防务和空间有限责任公司 | For the method for the electrobrightening of metal base |
| CN108221041B (en) * | 2016-12-21 | 2021-06-04 | 空中客车防务和空间有限责任公司 | Method for electropolishing metal substrates |
| US11162185B2 (en) | 2016-12-21 | 2021-11-02 | Airbus Defence and Space GmbH | Process for the electrolytic polishing of a metallic substrate |
| CN106567122A (en) * | 2017-02-17 | 2017-04-19 | 大博医疗科技股份有限公司 | Electrochemical polishing electrolyte and polishing method for titanium and titanium alloy |
| CN114192802A (en) * | 2021-10-27 | 2022-03-18 | 北京星航机电装备有限公司 | Surface polishing method and device for additive manufacturing titanium alloy structure |
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Application publication date: 20100811 |