CN102312277A - Electrochemical polishing electrolyte adopted for titanium and titanium alloy, use method thereof - Google Patents
Electrochemical polishing electrolyte adopted for titanium and titanium alloy, use method thereof Download PDFInfo
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- CN102312277A CN102312277A CN201110327361A CN201110327361A CN102312277A CN 102312277 A CN102312277 A CN 102312277A CN 201110327361 A CN201110327361 A CN 201110327361A CN 201110327361 A CN201110327361 A CN 201110327361A CN 102312277 A CN102312277 A CN 102312277A
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Abstract
The invention discloses a electrochemical polishing electrolyte adopted for titanium and titanium alloy, and a use method thereof, and relates to a electrolyte. The electrolyte comprises 80-90% of formamide, 10-20% of ethylene glycol, sulfamic acid, sodium chloride and an additive. Each liter of the solution comprising the formamide and the ethylene glycol is added with 120-200 g of the sulfamic acid, 1-5 g of the sodium chloride and 0.1-0.5 g of the additive. The preparation method for the electrolyte comprises: dissolving the sulfamic acid in the formamide, adding the ethylene glycol, the sodium chloride and the additive to the resulting solution, and then carrying out mixing to obtain the electrolyte. The use method is that: during using the electrolyte, the temperature of the electrolyte is stabilized to 0-10 DEG C; the titanium requiring polishing or titanium alloy requiring polishing is adopted as the anode, the stainless steel plate or the titanium plate is adopted as the cathode; the cathode and the anode are immersed in the electrolyte, the power supply is switched on; the polished sample is removed, washed and dried by baking. The electrolyte provided by the present invention does not contain hydrofluoric acid, chromic acid, perchloric acid, methanol, ethers and other toxic and harmful substances to the human body and the environment, wherein the toxic and harmful substances are generally used in the traditional electrochemical polishing.
Description
Technical field
The present invention relates to a kind of electrolytic solution, especially relate to a kind of electrolytic solution and finishing method thereof of titanium or titanium alloy electrochemical etching.
Background technology
Titanium and alloy thereof obtain application more and more widely because of its good physics, chemistry and biological nature in fields such as medical device, chemical machinery, space flight and aviation or even daily living articles.Surface finish is significant to ornamental, solidity to corrosion, wear resistance and the biocompatibility etc. that improve titanium or titanium alloy.In numerous surface polishing techniques, electrochemical etching has high-level efficiency, high precision, speed is fast, labour intensity is little advantage because of it, and has series of advantages such as the no work hardening layer in surface, anti-corrosion, wear-resisting reflectivity height and be widely used.Yet, because the passivation and the self-passivation of titanium are very capable, therefore being difficult in the Traditional electrochemical polishing fluid, obtain gratifying polishing effect, the surface is prone to produce manufacturing deficiencies such as etch, spot corrosion and current mark.
In traditional titanium or titanium alloy electrochemical etching, normal, strong and stimulating volatile with hydrofluoric acid, perchloric acid, ethers, methyl alcohol, Aluminum chloride anhydrous and Zinc Chloride Anhydrous etc. and to human body and the poisonous and hazardous chemical of environment as basic electrolytic solution.This type electrolytic solution has not only increased the danger of operation, and human body and environment are all had serious toxic action.By contrast, methane amide-thionamic acid system obtains more concern because of characteristics such as the low evil of its low toxicity, environmental friendliness.Yet this system but exists fatal shortcomings such as the electrolytic solution easy ageing lost efficacy, is difficult to regenerate and cost an arm and a leg, and is difficult in industry, realize large-scale the application.Therefore, optimize methane amide-thionamic acid electrochemical etching system and have important industrial application meaning.
Chinese patent CN101798702A discloses a kind of electrolytic solution and surface polishing method thereof of titanium or titanium alloy electrochemical etching, and said electrolytic solution comprises hydrofluoric acid 1～3 quality %, deionized water 20～30 quality %, and surplus is a terepthaloyl moietie.Finishing method comprises the steps: (1) preparing electrolyte; (2) anodize; (3) the deoxidation layer is handled.Utilize this electrolytic solution to carry out polished finish and can obtain smooth titanium and titanium alloy surface.This electrolytic solution has the good security and the feature of environmental protection.
Summary of the invention
The purpose of this invention is to provide a kind of hydrofluoric acid commonly used, chromic acid, perchloric acid, methyl alcohol, ethers etc. of not containing in traditional titanium electrochemical etching human body and environment hazardous and noxious substances be applicable to titanium and titanium alloy electrochemical polishing electrolytic solution and method of use thereof.
Said titanium or titanium alloy electrochemical etching electrolytic solution is made up of methane amide, terepthaloyl moietie, thionamic acid, sodium-chlor and additive; By volume; Said methane amide is 80%～90%; Terepthaloyl moietie is 10%～20%, in every liter of methane amide and ethylene glycol solution, adds thionamic acid 120～200g, sodium-chlor 1～5g and additive 0.1～0.5g.
Said additive can be selected a kind of in OP-10 emulsifying agent, sodium laurylsulfonate, X 2073, the cetyl trimethylammonium bromide etc. for use.
The preparation method of said titanium or titanium alloy electrochemical etching electrolytic solution is following:
Thionamic acid is dissolved in the methane amide, adds terepthaloyl moietie, sodium-chlor and additive more successively, promptly get titanium or titanium alloy electrochemical etching electrolytic solution after the mixing.
The method of use of said titanium or titanium alloy electrochemical etching electrolytic solution is:
1) utilize the cryogenic liquid recycle pump that electrolyte temperature is stabilized in 0～10 ℃;
2) select the power supply of D.C. regulated power supply as electrochemical etching for use, as anode, stainless steel plate or titanium plate are as negative electrode with polished titanium or titanium alloy; Negative electrode and anode are immersed in the titanium or titanium alloy electrochemical etching electrolytic solution, and energized is selected constant current mode for use;
3) sample after will polishing takes out, and after the cleaning, takes out oven dry.
In step 2) in, in the said constant current mode, current density is 0.8～2.0A/cm
2, the electrochemical etching time is 2～5min.
In step 3), said cleaning can be used flushing with clean water earlier, places the deionized water for ultrasonic ripple to clean again.
The surface effect of said titanium or titanium alloy behind the electrolytic solution electrochemical etching estimated with surfaceness and these two indexs of surface gloss, and detects comparative descriptions in addition through surface microscopic topographic, and concrete grammar is following:
1) surfaceness.Regulation according among the GB/T3505-2000 detects, and selects the evaluation index of evaluation profile arithmetic average error (Ra) as surfaceness for use.The Ra value is directly recorded by the TR200 hand-held roughmeter of Beijing Time Zhifeng Science Co., Ltd.
2) surface gloss.Come the surface gloss of reflection sample indirectly through surface reflectivity (R%).Surface albedo is recorded by the specular reflection pattern of Varian Cary 5000 ultraviolet-visibles-near infrared spectrometer.During mensuration, as benchmark, assert that promptly its surface albedo is 100%, investigate the surface albedo of titanium or titanium alloy then with this with the surface albedo of normalized optical minute surface.
3) microscopic appearance detects.The surface microscopic topographic of the titanium or titanium alloy before and after the polishing is detected by 1530 the high explanation of emission ESEMs of German LEO company.
With existing titanium or titanium alloy electrochemical etching compared with techniques, the present invention has following advantage:
1) titanium or titanium alloy electrochemical etching electrolytic solution provided by the invention; Do not contain in traditional titanium electrochemical etching that hydrofluoric acid, perchloric acid, ethers, methyl alcohol, Aluminum chloride anhydrous and Zinc Chloride Anhydrous etc. commonly used are volatile, strong and stimulating and to human body and the poisonous and hazardous chemical of environment, and do not produce poisonous and hazardous irritant gas in the electrochemical etching process.Electrolytic solution is little to environmental hazard, and security preferably and environment-friendly type are arranged.
2) than methane amide-thionamic acid electrolytic solution commonly used; In electrolytic solution according to the invention; The introducing of terepthaloyl moietie not only makes the work-ing life of said electrolytic solution and operational stability that tangible improvement has been arranged; And the cost of reduction electrolytic solution, this is because the terepthaloyl moietie price of equal volume is lower than methane amide.
3) titanium or titanium alloy is after electrolytic solution polishing according to the invention, and surfacing is smooth, and has specular reflection effect preferably.
Description of drawings
Fig. 1 is that industrially pure titanium (TA2) is schemed through the SEM of surface topography after the polishing of 220 orders, 320 orders, 800 orders, 1000 orders, 1500 orders and 2000 order abrasive paper for metallograph successively.In Fig. 1, scale is 10 μ m.
Fig. 2 is the SEM figure of industrially pure titanium (TA2) through electrolytic solution according to the invention and electrochemical polishing method surface of polished pattern.In Fig. 2, scale is 10 μ m.
Fig. 3 is that titanium alloy (TC4) is schemed through the SEM of surface topography after the polishing of 220 orders, 320 orders, 800 orders, 1000 orders, 1500 orders and 2000 order abrasive paper for metallograph successively.In Fig. 3, scale is 20 μ m.
Fig. 4 is the SEM figure of titanium alloy (TC4) through electrolytic solution according to the invention and electrochemical polishing method surface of polished pattern.In Fig. 4, scale is 10 μ m.
Embodiment
Embodiment 1
(1) pre-treatment.With size is TA2 industrially pure titanium and warp 320 orders and the polishing of 800 purpose abrasive paper for metallograph successively of TC4 titanium alloy of 10mm * 10mm * 3mm, uses clear water and deionized water rinsing clean then successively, subsequent use after drying.
(2) configuration electrolytic solution.Electrolytic solution by following recipe configuration titanium electrochemical etching:
Used additive is selected cetyl trimethylammonium bromide for use.
In electrolytic solution when configuration, be dissolved in thionamic acid in the methane amide earlier, treats that thionamic acid all after the dissolving, adds terepthaloyl moietie, sodium-chlor and cetyl trimethylammonium bromide successively, promptly gets titanium or titanium alloy electrochemical etching electrolytic solution after mixing.Since the easy moisture absorption of methane amide, and this electropolishing system is not water-fast, is exposed to the moisture uptake that the airborne time reduces electrolytic solution thereby therefore in the preparation process, should reduce methane amide.
(3) electrochemical etching.Select the power supply of D.C. regulated power supply as electrochemical etching for use, as anode, stainless steel plate is as negative electrode with the polished titanium of clean dried or titanium alloy; Negative and positive the two poles of the earth are immersed in the electrolytic solution simultaneously.Carry out electrochemical etching by following operational condition:
Temperature: 0～5 ℃
Current density: 0.8A/cm
2
Two-plate spacing: 2cm
Stirring velocity: 600rpm
Time: 5min
(4) aftertreatment.Titanium or titanium alloy behind the electrochemical etching is used clear water and deionized water rinsing successively, then with ultrasonic cleaning 5min to remove the impurity on surface, at last sample is put into boiling water and seals 5min, take out and to get product after drying.
TA2 industrially pure titanium and TC4 titanium alloy have reduced surfaceness after electrolytic solution according to the invention and electrochemical polishing method processing, improved surface gloss, and mirror effect is obvious.Table 1 has provided without any processing, mechanical polishing (handling through the polishing of 220 orders, 320 orders, 800 orders, 1000 orders, 1500 orders and 2000 order abrasive paper for metallograph successively) with by the TA2 industrially pure titanium behind the electrolytic solution electrochemical etching according to the invention and the surfaceness and the reflectivity of TC4 titanium alloy.
Table 1 TA2 industrially pure titanium and forward and backward roughness and the reflectivity of TC4 titanium alloy electrochemical polishing
Can find out that from table 1 titanium or titanium alloy has reduced through its surfaceness after the mechanical polishing, and its surface albedo does not improve significantly.Different therewith is, titanium or titanium alloy is after electrolytic solution according to the invention and electrochemical polishing treatment, and not only surfaceness has reduced, and its surface albedo also improves significantly.
Embodiment 2
(1) pre-treatment.With size is the TA of 10mm * 10mm * 3mm
2Industrially pure titanium and TC
4Titanium alloy through 320 orders and the polishing of 800 purpose abrasive paper for metallograph, uses clear water and deionized water rinsing clean successively then successively, and is subsequent use after drying.
(2) configuration electrolytic solution.Electrolytic solution by following recipe configuration titanium electrochemical etching:
Used additive is selected sodium laurylsulfonate for use.
In electrolytic solution when configuration, be dissolved in thionamic acid in the methane amide earlier, treats that thionamic acid all after the dissolving, adds terepthaloyl moietie, sodium-chlor and sodium laurylsulfonate successively, promptly gets titanium or titanium alloy electrochemical etching electrolytic solution after mixing.Since the easy moisture absorption of methane amide, and this electropolishing system is not water-fast, is exposed to the moisture uptake that the airborne time reduces electrolytic solution thereby therefore in the preparation process, should reduce methane amide.
(3) electrochemical etching.Select the power supply of D.C. regulated power supply as electrochemical etching for use, as anode, stainless steel plate is as negative electrode with the polished titanium of clean dried or titanium alloy; Negative and positive the two poles of the earth are immersed in the electrolytic solution simultaneously.Carry out electrochemical etching by following operational condition:
Temperature: 5～10 ℃
Current density: 1.4A/cm
2
Two-plate spacing: 3.5cm
Stirring velocity: 700rpm
Time: 4min
(4) aftertreatment.Titanium or titanium alloy behind the electrochemical etching is used clear water and deionized water rinsing successively, then with ultrasonic cleaning 5min to remove the impurity on surface, at last sample is put into boiling water and seals 5min, take out and to get product after drying.
TA2 industrially pure titanium and TC4 titanium alloy have reduced surfaceness after electrolytic solution according to the invention and electrochemical polishing method processing, improved surface gloss, and mirror effect is obvious.Table 2 has provided without any processing, mechanical polishing (handling through the polishing of 220 orders, 320 orders, 800 orders, 1000 orders, 1500 orders and 2000 order abrasive paper for metallograph successively) with by the TA2 industrially pure titanium behind the electrolytic solution electrochemical etching according to the invention and the surfaceness and the reflectivity of TC4 titanium alloy.
Table 2 TA2 industrially pure titanium and forward and backward roughness and the reflectivity of TC4 titanium alloy electrochemical polishing
Can find out that from table 2 titanium or titanium alloy has reduced through its surfaceness after the mechanical polishing, and its surface albedo does not improve significantly.Different therewith is, titanium or titanium alloy is after electrolytic solution according to the invention and electrochemical polishing treatment, and not only surfaceness has reduced, and its surface albedo also improves significantly.
Embodiment 3
(1) pre-treatment.With size is the TA of 10mm * 10mm * 3mm
2Industrially pure titanium and TC
4Titanium alloy through 320 orders and the polishing of 800 purpose abrasive paper for metallograph, uses clear water and deionized water rinsing clean successively then successively, and is subsequent use after drying.
(2) configuration electrolytic solution.Electrolytic solution by following recipe configuration titanium electrochemical etching:
Used additive is selected X 2073 for use
In electrolytic solution when configuration, be dissolved in thionamic acid in the methane amide earlier, treats that thionamic acid all after the dissolving, adds terepthaloyl moietie, sodium-chlor and X 2073 successively, promptly gets titanium or titanium alloy electrochemical etching electrolytic solution after mixing.Since the easy moisture absorption of methane amide, and this electropolishing system is not water-fast, is exposed to the moisture uptake that the airborne time reduces electrolytic solution thereby therefore in the preparation process, should reduce methane amide.
(3) electrochemical etching.Select the power supply of D.C. regulated power supply as electrochemical etching for use, as anode, stainless steel plate is as negative electrode with the polished titanium of clean dried or titanium alloy; Negative and positive the two poles of the earth are immersed in the electrolytic solution simultaneously.Carry out electrochemical etching by following operational condition:
Temperature: 0～5 ℃
Current density: 2.0A/cm
2
Between two-plate: 5cm
Stirring velocity: 800rpm
Time: 2min
(4) aftertreatment.Titanium or titanium alloy behind the electrochemical etching is used clear water and deionized water rinsing successively, then with ultrasonic cleaning 5min to remove the impurity on surface, at last sample is put into boiling water and seals 5min, take out and to get product after drying.
TA2 industrially pure titanium and TC4 titanium alloy have reduced surfaceness after electrolytic solution according to the invention and electrochemical polishing method processing, improved surface gloss, and mirror effect is obvious.Table 3 has provided without any processing, mechanical polishing (handling through the polishing of 220 orders, 320 orders, 800 orders, 1000 orders, 1500 orders and 2000 order abrasive paper for metallograph successively) with by the TA2 industrially pure titanium behind the electrolytic solution electrochemical etching according to the invention and the surfaceness and the reflectivity of TC4 titanium alloy.
Table 3 TA2 industrially pure titanium and forward and backward roughness and the reflectivity of TC4 titanium alloy electrochemical polishing
Can find out that from table 3 titanium or titanium alloy has reduced through its surfaceness after the mechanical polishing, and its surface albedo does not improve significantly.Different therewith is, titanium or titanium alloy is after electrolytic solution according to the invention and electrochemical polishing treatment, and not only surfaceness has reduced, and its surface albedo has also taken place to improve significantly.
Embodiment 4
(1) pre-treatment.With size is TA2 industrially pure titanium and warp 320 orders and the polishing of 800 purpose abrasive paper for metallograph successively of TC4 titanium alloy of 10mm * 10mm * 3mm, uses clear water and deionized water rinsing clean then successively, subsequent use after drying.
(2) configuration electrolytic solution.Electrolytic solution by following recipe configuration titanium electrochemical etching:
Used additive is selected the OP-10 emulsifying agent for use.
In electrolytic solution when configuration, be dissolved in thionamic acid in the methane amide earlier, treats that thionamic acid all after the dissolving, adds terepthaloyl moietie, sodium-chlor and OP-10 emulsifying agent successively, promptly gets titanium or titanium alloy electrochemical etching electrolytic solution after mixing.Since the easy moisture absorption of methane amide, and this electropolishing system is not water-fast, is exposed to the moisture uptake that the airborne time reduces electrolytic solution thereby therefore in the preparation process, should reduce methane amide.
(3) electrochemical etching.Select the power supply of D.C. regulated power supply as electrochemical etching for use, as anode, stainless steel plate is as negative electrode with the polished titanium of clean dried or titanium alloy; Negative and positive the two poles of the earth are immersed in the electrolytic solution simultaneously.Carry out electrochemical etching by following operational condition:
Temperature: 0～10 ℃
Current density: 1.5A/cm
2
Two-plate spacing: 4cm
Stirring velocity: 700rpm
Time: 3min
(4) aftertreatment.Titanium or titanium alloy behind the electrochemical etching is used clear water and deionized water rinsing successively, then with ultrasonic cleaning 5min to remove the impurity on surface, at last sample is put into boiling water and seals 5min, take out and to get product after drying.
TA2 industrially pure titanium and TC4 titanium alloy are after electrolytic solution according to the invention and electrochemical polishing method are handled, and not only surfaceness has reduced, and surface gloss improves widely, and mirror effect clearly.Table 4 has provided without any processing, mechanical polishing (handling through the polishing of 220 orders, 320 orders, 800 orders, 1000 orders, 1500 orders and 2000 order abrasive paper for metallograph successively) with by the TA2 industrially pure titanium behind the electrolytic solution electrochemical etching according to the invention and the surfaceness and the reflectivity of TC4 titanium alloy.
Table 4 TA2 industrially pure titanium and forward and backward roughness and the reflectivity of TC4 titanium alloy electrochemical polishing
Can find out that from table 4 titanium or titanium alloy has reduced through its surfaceness after the mechanical polishing, and its surface albedo does not improve significantly.Different therewith is, titanium or titanium alloy is after electrolytic solution according to the invention and electrochemical polishing treatment, and not only surfaceness has reduced, and its surface albedo has also taken place to improve significantly.
From Fig. 1 and 3, can obviously see the cut that mechanical polishing is left, particularly pure titanium, its surface exists more darker depression.
Can see that from Fig. 2 and 4 titanium or titanium alloy is through behind the electrochemical etching, not only its surface mach vestige has originally disappeared, and does not have tangible depression or projection, surfacing.
Claims (6)
1. one kind is applicable to titanium and titanium alloy electrochemical polishing electrolytic solution; It is characterized in that forming by methane amide, terepthaloyl moietie, thionamic acid, sodium-chlor and additive; By volume; Said methane amide is 80%～90%, and terepthaloyl moietie is 10%～20%, in every liter of methane amide and ethylene glycol solution, adds thionamic acid 120～200g, sodium-chlor 1～5g and additive 0.1～0.5g.
2. a kind of titanium and titanium alloy electrochemical polishing electrolytic solution that is applicable to as claimed in claim 1 is characterized in that said additive selects a kind of in OP-10 emulsifying agent, sodium laurylsulfonate, X 2073, the cetyl trimethylammonium bromide for use.
3. a kind of preparation method who is applicable to titanium and titanium alloy electrochemical polishing electrolytic solution as claimed in claim 1 is characterized in that its concrete steps are following:
Thionamic acid is dissolved in the methane amide, adds terepthaloyl moietie, sodium-chlor and additive more successively, promptly get titanium or titanium alloy electrochemical etching electrolytic solution after the mixing.
4. a kind of method of use that is applicable to titanium and titanium alloy electrochemical polishing electrolytic solution as claimed in claim 1 is characterized in that the steps include:
1) utilize the cryogenic liquid recycle pump that electrolyte temperature is stabilized in 0～10 ℃;
2) select the power supply of D.C. regulated power supply as electrochemical etching for use, as anode, stainless steel plate or titanium plate are as negative electrode with polished titanium or titanium alloy; Negative electrode and anode are immersed in the titanium or titanium alloy electrochemical etching electrolytic solution, and energized is selected constant current mode for use;
3) sample after will polishing takes out, and after the cleaning, takes out oven dry.
5. a kind of method of use that is applicable to titanium and titanium alloy electrochemical polishing electrolytic solution as claimed in claim 4 is characterized in that in step 2) in, in the said constant current mode, current density is 0.8～2.0A/cm
2, the electrochemical etching time is 2～5min.
6. a kind of method of use that is applicable to titanium and titanium alloy electrochemical polishing electrolytic solution as claimed in claim 4 is characterized in that in step 3) said cleaning is to use flushing with clean water earlier, places the deionized water for ultrasonic ripple to clean again.
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| CN102534744A (en) * | 2012-03-14 | 2012-07-04 | 淮阴工学院 | Polishing solution and polishing method for medical titanium alloy |
| CN104532338A (en) * | 2014-12-11 | 2015-04-22 | 沈阳富创精密设备有限公司 | Hastelloy electrolytic polishing process |
| CN104668677A (en) * | 2013-12-02 | 2015-06-03 | 天津大学 | Non-water-based electrolyte used for titanium alloy electrolytic machining and preparation method of non-water-based electrolyte |
| CN106048708A (en) * | 2016-07-22 | 2016-10-26 | 昆明理工大学 | Electrolytic polishing method for titanium alloy |
| 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 |
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| CN106048708B (en) * | 2016-07-22 | 2017-12-01 | 昆明理工大学 | A kind of method of titanium alloy electrobrightening |
| 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 |
| CN107460534A (en) * | 2017-09-05 | 2017-12-12 | 宝鸡市同业精密科技有限责任公司 | The electrochemical polish liquid and polishing method of a kind of titanium or titanium alloy |
| CN108360059A (en) * | 2018-04-24 | 2018-08-03 | 东北大学 | A kind of electrochemical polish liquid and polishing method of the special-shaped titanium alloy of laser gain material manufacture |
| CN110578165A (en) * | 2019-11-01 | 2019-12-17 | 灵宝华鑫铜箔有限责任公司 | Electrochemical polishing solution for titanium cathode roller and method for polishing cathode roller by using same |
| CN110726743A (en) * | 2019-11-13 | 2020-01-24 | 河北科技大学 | Method for preparing pure titanium EBSD sample at room temperature |
| CN110726743B (en) * | 2019-11-13 | 2022-06-14 | 河北科技大学 | Method for preparing pure titanium EBSD sample at room temperature |
| CN112522774A (en) * | 2020-10-27 | 2021-03-19 | 沈阳富创精密设备股份有限公司 | Titanium tube flowing type electrolytic polishing special method |
| CN114108065A (en) * | 2021-12-30 | 2022-03-01 | 左毛毛 | Aluminum alloy processing technology |
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