CN102899711A - Electrolytic polishing solution for titanium and titanium alloys and electrolytic polishing process - Google Patents
Electrolytic polishing solution for titanium and titanium alloys and electrolytic polishing process Download PDFInfo
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- CN102899711A CN102899711A CN2012104710903A CN201210471090A CN102899711A CN 102899711 A CN102899711 A CN 102899711A CN 2012104710903 A CN2012104710903 A CN 2012104710903A CN 201210471090 A CN201210471090 A CN 201210471090A CN 102899711 A CN102899711 A CN 102899711A
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Abstract
The invention discloses electrolytic polishing solution for titanium and titanium alloys and an electrolytic polishing process, wherein the polishing solution is prepared by perchloric acid with volume fraction of 8-15% and acetic acid with volume fraction of 85-92%. The polishing solution is convenient in material selection, easy in preparation and storage, simple in polishing process equipment, easy in operation, smooth in surface, free of obvious scratches and oxide films and high in EBSD (Electron Back-Scattered Diffraction) pattern recognition rate, and has the effects of greatly reducing the superficial stress of the samples and greatly improving the detection precision.
Description
Technical field
The present invention relates to field of metal surface treatment, specifically, relate to a kind of electrolytic polishing liquid and electrolytic polishing process for the preparation of titanium or titanium alloy Electron Back-Scattered Diffraction (election backscatter diffraction, EBSD) sample.
Technical background
Since the nineties in 20th century, be assemblied in electron backscattered style (the Electron Back-scattering Patterns on the SEM, being called for short EBSP) the crystal microcell is orientated and the analytical technology of crystalline structure has obtained larger development, and widespread use in microstructure and little texture sign.This technology is also referred to as Electron Back-Scattered Diffraction (Electron Backscattered Diffraction is called for short EBSD).The principal feature of EBSD is the diffraction (providing the data of crystallography) that carries out the spatial resolution submicron order in the conventional characteristics that keep scanning electronic microscope.At present, the EBSD technology can realize automatically gathering the microcell orientation information, sample preparation is simpler, acquisition speed fast (can reach approximately 360,000 points/hour in addition faster), resolving power high (spatial resolution and angular resolution can reach respectively 0.1 ° of m and 0.5m), for heterogeneous microstructure and the texture of rapidly and efficiently quantitative statistics research material are laid a good foundation, therefore become a kind of effective analysis means in the investigation of materials.
It is high that titanium or titanium alloy has specific tenacity, fine corrosion resistance, and therefore the advantage such as high-temperature behavior is good is widely used in fields such as the energy, chemical industry, metallurgy, automobile, space flight and aviation.Therefore, titanium or titanium alloy being carried out microstructure and crystallography analyzes significant.Now in the technology, use EBSD that titanium or titanium alloy is carried out in microstructure and the crystallography analytic process, in EBSD sample preparation process, the EBSD technology is strict to specimen surface, surface smoothing, can not there be stress, therefore be not easy preparation, need to carry out mechanical polishing or chemical rightenning processing to the EBSD sample.But mechanical polishing exists the cycle long, and there is unrelieved stress in the destructible specimen surface, reduces EBSD style recognition rate, and the defective such as the quartzy silicon latex of rumbling compound is expensive; And electropolishing needs special-purpose polishing fluid, and there is the problem of complicated component, difficult preparation and glossing less stable in domestic disclosed titanium or titanium alloy electrolytic polishing liquid at present.
Summary of the invention
For the prior art above shortcomings, the present invention solves the problem that there is complicated component in the titanium or titanium alloy electrolytic polishing liquid, is difficult for preparation and glossing less stable, and a kind of electrolytic polishing liquid for the preparation of titanium or titanium alloy EBSD sample is provided.
The present invention also provides a kind of easy handling, the high electrolytic polishing process that is used for titanium or titanium alloy EBSD sample of EBSD style recognition rate after the polishing.
Realize above-mentioned purpose, the present invention adopts following technical scheme: a kind of electrolytic polishing liquid for titanium or titanium alloy, it is characterized in that, and this polishing fluid is that 8-15% perchloric acid and 85-92% acetic acid are formulated by volume fraction.
Further, the present invention also provides a kind of electrolytic polishing process of titanium or titanium alloy EBSD test, comprises the steps:
(1) at first, the titanium or titanium alloy sample is carried out the abrasive paper for metallograph polishing, the sand paper model is respectively 400 orders, 600 orders, 800 orders, 1500 orders and 2000 orders;
(2) preparation electrolytic polishing liquid: the dose volume mark is the perchloric acid acetic acid solution of 8-15% perchloric acid and 85-92% acetic acid, pours in the electrolyzer;
(3) take the titanium or titanium alloy sample as anode, link to each other with D.C. regulated power supply is anodal, immerse in the electrolytic polishing liquid of having prepared;
(4) take stainless steel substrates as negative electrode, link to each other with the D.C. regulated power supply negative pole, immerse in the polishing fluid of above-mentioned preparation and polish, polish temperature is
Subzero5-10 ℃.
Further, described polishing time is 15-60s, and polishing voltage is 50-80V, and the distance between anode and the negative electrode is 60-100mm; Polishing process uses agitator to stir.
Compared to existing technology, the present invention has following beneficial effect:
1, electrolytic polishing liquid of the present invention is drawn materials conveniently, and is with low cost, is easy to preparation and storage, harmless.
2, the EBSD analytical technology requires high to specimen surface, require specimen surface smooth smooth, fresh, unstressed, without obvious cut and oxide film etc., general commonly used polishing fluid and glossing can't meet the demands and the scope of application is little is difficult for preparation, adopts polishing fluid of the present invention and glossing can satisfy above-mentioned requirements, EBSD style recognition rate is high, increases substantially accuracy of detection.
3, adopt glossing of the present invention, equipment is simple, easily operation; Negative electrode is common stainless steel, draws materials conveniently, makes simple.
4, this glossing good stability, polishing velocity is fast, and polishing efficiency is high, can be used for the preparation of sample in enormous quantities.
?
Description of drawings
Fig. 1 is the Ti-3Al-4Cr-2Fe titanium alloy EBSD orientation mapping figure after embodiment 1 carries out electropolishing.
Fig. 2 is the TC4-1B titanium alloy EBSD orientation mapping figure after embodiment 2 carries out electropolishing.
Embodiment
Below in conjunction with the drawings and specific embodiments the present invention is described in further details.
One, being used for the electrolytic polishing liquid of titanium or titanium alloy EBSD sample preparation, take acetic acid as solvent, is that 8-15% perchloric acid and 85-92% acetic acid are formulated by volume fraction.
Wherein, perchloric acid and acetic acid all adopt chemical pure or analytically pure reagent.
Specific embodiment prescription (unit is volume fraction) as shown in the table:
| Raw material | Prescription 1 | Prescription 2 | Prescription 3 | Prescription 4 |
| Perchloric acid | 10 | 12 | 8 | 15 |
| Acetic acid | 90 | 88 | 92 | 85 |
| Add up to | 100 | 100 | 100 | 100 |
Two, be used for the electrolytic polishing process of titanium or titanium alloy EBSD sample, specific embodiment and step are as follows
Embodiment 1, and a kind of electrolytic polishing process for titanium or titanium alloy EBSD sample comprises the steps:
(1) sample polishing: with 400 orders, 600 orders, 800 orders, 1500 orders and 2000 purpose abrasive paper for metallograph the Ti-3Al-4Cr-2Fe titanium alloy is polished successively respectively, also dry on clean surface;
(2) preparation electrolytic polishing liquid: by upper table prescription 1 preparation;
(3) the Ti-3Al-4Cr-2Fe titanium alloy sample after the polishing is as anode, links to each other and immerses in the electrolyzer that fills the electrolytic polishing liquid that step (2) prepares with D.C. regulated power supply is anodal;
(4) take stainless steel substrates as negative electrode, link to each other with the D.C. regulated power supply negative pole and immerse in the electrolyzer that fills above-mentioned electrolytic polishing liquid;
(5) polish at above-mentioned electrolytic solution, polish temperature is
Subzero0 ~ 5 ℃, polishing time is 40s, and polishing voltage is 65V, and the distance between anode and the negative electrode is 70mm;
(6) will dry through the taking-up of the sample after the polishing, the surfacing light adopts the EBSD system of Nova 400 Nano-SEM field emission scanning electron microscopes that Ti-3Al-4Cr-2Fe titanium alloy sample is tested.
Test result as shown in Figure 1, EBSD style recognition rate is high, average confidence index (Average Confidence Index) can reach 0.75.
Embodiment 2: a kind of electrolytic polishing process for titanium or titanium alloy EBSD sample comprises the steps:
(1) sample polishing: with embodiment 1;
(2) preparation electrolytic polishing liquid: by upper table prescription 2 preparations;
(3) the TC4 titanium alloy sample after the polishing is as anode, links to each other and immerses in the electrolyzer that fills electrolytic polishing liquid with D.C. regulated power supply is anodal;
(4) take stainless steel substrates as negative electrode, link to each other with the D.C. regulated power supply negative pole and immerse in the electrolyzer that fills electrolytic polishing liquid;
(5) polish in above-mentioned electrolytic solution, polish temperature is
Subzero5-10 ℃, polishing time is 35s, and polishing voltage is 60V, and the distance between anode and the negative electrode is 60mm.
(6) will dry through the taking-up of the sample after the polishing, the surfacing light adopts the EBSD system of Nova 400 Nano-SEM field emission scanning electron microscopes that TC4 titanium alloy sample is tested test result as shown in Figure 2.
Test result as shown in Figure 2, EBSD style recognition rate is that EBSD style recognition rate is high, average confidence index is 0.81.
Explanation is at last, above embodiment is only unrestricted in order to technical scheme of the present invention to be described, although by invention has been described with reference to the preferred embodiments of the present invention, but those of ordinary skill in the art is to be understood that, can make various changes to it in the form and details, and not depart from the spirit and scope of the present invention that appended claims limits.
Claims (3)
1. an electrolytic polishing liquid that is used for titanium or titanium alloy is characterized in that, this polishing fluid is that 8-15% perchloric acid and 85-92% acetic acid are formulated by volume fraction.
2. the electrolytic polishing process of a titanium or titanium alloy EBSD test is characterized in that, comprises the steps:
(1) at first, the titanium or titanium alloy sample is carried out the abrasive paper for metallograph polishing, the sand paper model is respectively 400 orders, 600 orders, 800 orders, 1500 orders and 2000 orders;
(2) preparation electrolytic polishing liquid: the dose volume mark is the perchloric acid acetic acid solution of 8-15% perchloric acid and 85-92% acetic acid, pours in the electrolyzer;
(3) take the titanium or titanium alloy sample as anode, link to each other with D.C. regulated power supply is anodal, immerse in the electrolytic polishing liquid of having prepared;
(4) take stainless steel substrates as negative electrode, link to each other with the D.C. regulated power supply negative pole, immerse in the polishing fluid of above-mentioned preparation and polish, polish temperature is subzero 5-10 ℃.
3. the electrolytic polishing process of described titanium or titanium alloy EBSD test according to claim 2 is characterized in that, polishing time is 15-60s, and polishing voltage is 50-80V, and the distance between anode and the negative electrode is 60-100mm;
Polishing process uses agitator to stir.
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103603027A (en) * | 2013-11-07 | 2014-02-26 | 昆明理工大学 | Electrochemical polishing method of palladium and alloy thereof |
| CN104846426A (en) * | 2015-04-29 | 2015-08-19 | 中国航空工业集团公司北京航空材料研究院 | Corrosive agent for Nb - Si material microstructure specimens and an electrolyte corrosion technique |
| CN105369340A (en) * | 2015-11-11 | 2016-03-02 | 无锡清杨机械制造有限公司 | Titanium alloy polishing method |
| CN107402150A (en) * | 2017-07-24 | 2017-11-28 | 东北大学 | A kind of electrobrightening preparation method of titanium aluminium base alloy EBSD sample for analysis |
| CN108118388A (en) * | 2017-11-08 | 2018-06-05 | 山东理工大学 | A kind of Ni-Ti alloys electrochemical polish liquid and polishing method |
| CN108760784A (en) * | 2018-04-03 | 2018-11-06 | 安徽大学 | Quantitative analysis method for metallographic volume fraction gradient distribution of surface layer of cutting processing of dual-phase titanium alloy |
| CN108802076A (en) * | 2018-06-12 | 2018-11-13 | 黄淮学院 | A kind of electrolytic polishing method preparing pure titanium or titanium alloy EBSD samples |
| CN109900727A (en) * | 2019-03-18 | 2019-06-18 | 中国科学院金属研究所 | A kind of ultralow temperature light current flow control metal material EBSD sample preparation methods |
| CN109991254A (en) * | 2019-04-29 | 2019-07-09 | 福建工程学院 | A kind of preparation method of pure iron EBSD sample |
| CN110044939A (en) * | 2019-04-22 | 2019-07-23 | 广东省材料与加工研究所 | A kind of steel/iron double metal composite sample preparation method for EBSD test |
| CN110565159A (en) * | 2019-09-19 | 2019-12-13 | 西安理工大学 | Method for preparing titanium and titanium alloy EBSD sample |
| CN110618153A (en) * | 2019-09-04 | 2019-12-27 | 西安理工大学 | Preparation method of electropolished titanium alloy large-size rod-shaped or plate-shaped sample |
| CN110726743A (en) * | 2019-11-13 | 2020-01-24 | 河北科技大学 | Method for preparing pure titanium EBSD sample at room temperature |
| CN111621841A (en) * | 2020-05-21 | 2020-09-04 | 南京理工大学 | TiAl single crystal EBSD sample-based electrolytic polishing solution and electrolytic method thereof |
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| TWI602956B (en) * | 2016-10-04 | 2017-10-21 | 中國鋼鐵股份有限公司 | Method of analyzing steel microstructures with improved phase identification capability |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH03120400A (en) * | 1989-09-29 | 1991-05-22 | Showa Electric Wire & Cable Co Ltd | Matting treatment of titanium alloy |
| US5911867A (en) * | 1996-07-19 | 1999-06-15 | Sandvik Ab | Method for obtaining a high surface finish on titanium-based coatings by electropolishing |
| CN1358240A (en) * | 1999-06-25 | 2002-07-10 | 欧洲核研究组织 | Bath composition for electropolishing of titanium and method for using same |
| CN102634840A (en) * | 2012-05-02 | 2012-08-15 | 浙江大学 | Electrochemical polishing electrolytic solution of zirconium alloy and electrochemical polishing method of electrochemical polishing electrolytic solution |
-
2012
- 2012-11-20 CN CN201210471090.3A patent/CN102899711B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH03120400A (en) * | 1989-09-29 | 1991-05-22 | Showa Electric Wire & Cable Co Ltd | Matting treatment of titanium alloy |
| US5911867A (en) * | 1996-07-19 | 1999-06-15 | Sandvik Ab | Method for obtaining a high surface finish on titanium-based coatings by electropolishing |
| CN1358240A (en) * | 1999-06-25 | 2002-07-10 | 欧洲核研究组织 | Bath composition for electropolishing of titanium and method for using same |
| CN102634840A (en) * | 2012-05-02 | 2012-08-15 | 浙江大学 | Electrochemical polishing electrolytic solution of zirconium alloy and electrochemical polishing method of electrochemical polishing electrolytic solution |
Non-Patent Citations (7)
| Title |
|---|
| L.L. MEISNER, ET AL.: "Surface Modification of TiNi Alloy by Electron Beam Influence", 《2008-9-21-26 15TH INTERNATIONAL SYMPOSIUM ON HIGH-CURRENT ELECTRONICS》 * |
| MATHIEU, J.B., ET AL.: "Electropolishing of titanium in perchloric acid-acetic acid solution. II. Polarization behavior and stoichiometry", 《J. ELECTROCHEM. SOC.》 * |
| 余存烨: "钛及钛合金的金相制样实用技术与经验", 《理化检验.物理分册》 * |
| 宋志华等: "Ti3Al激光焊接接头EBSD试样的制备", 《焊接学报》 * |
| 张素银等: "钛膜的电解抛光技术研究", 《强激光与粒子束》 * |
| 王耿洁等: "热轧TA1钛的电子背散射衍射分析", 《材料导报B：研究篇》 * |
| 雷娜等: "工业纯钛电子背散射衍射试样的制备", 《材料导报》 * |
Cited By (20)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103603027B (en) * | 2013-11-07 | 2017-01-04 | 昆明理工大学 | A kind of palladium and the electrochemical polishing method of alloy thereof |
| CN103603027A (en) * | 2013-11-07 | 2014-02-26 | 昆明理工大学 | Electrochemical polishing method of palladium and alloy thereof |
| CN104846426A (en) * | 2015-04-29 | 2015-08-19 | 中国航空工业集团公司北京航空材料研究院 | Corrosive agent for Nb - Si material microstructure specimens and an electrolyte corrosion technique |
| CN105369340A (en) * | 2015-11-11 | 2016-03-02 | 无锡清杨机械制造有限公司 | Titanium alloy polishing method |
| CN107402150A (en) * | 2017-07-24 | 2017-11-28 | 东北大学 | A kind of electrobrightening preparation method of titanium aluminium base alloy EBSD sample for analysis |
| CN108118388B (en) * | 2017-11-08 | 2020-01-14 | 山东理工大学 | Ni-Ti alloy electrochemical polishing solution and polishing method |
| CN108118388A (en) * | 2017-11-08 | 2018-06-05 | 山东理工大学 | A kind of Ni-Ti alloys electrochemical polish liquid and polishing method |
| CN108760784A (en) * | 2018-04-03 | 2018-11-06 | 安徽大学 | Quantitative analysis method for metallographic volume fraction gradient distribution of surface layer of cutting processing of dual-phase titanium alloy |
| CN108760784B (en) * | 2018-04-03 | 2021-04-09 | 安徽大学 | Quantitative analysis method for metallographic volume fraction gradient distribution of surface layer of cutting processing of dual-phase titanium alloy |
| CN108802076A (en) * | 2018-06-12 | 2018-11-13 | 黄淮学院 | A kind of electrolytic polishing method preparing pure titanium or titanium alloy EBSD samples |
| CN109900727A (en) * | 2019-03-18 | 2019-06-18 | 中国科学院金属研究所 | A kind of ultralow temperature light current flow control metal material EBSD sample preparation methods |
| CN110044939A (en) * | 2019-04-22 | 2019-07-23 | 广东省材料与加工研究所 | A kind of steel/iron double metal composite sample preparation method for EBSD test |
| CN110044939B (en) * | 2019-04-22 | 2021-11-23 | 广东省材料与加工研究所 | Preparation method of steel/iron bimetal composite material sample for EBSD test |
| CN109991254A (en) * | 2019-04-29 | 2019-07-09 | 福建工程学院 | A kind of preparation method of pure iron EBSD sample |
| CN110618153A (en) * | 2019-09-04 | 2019-12-27 | 西安理工大学 | Preparation method of electropolished titanium alloy large-size rod-shaped or plate-shaped sample |
| CN110565159A (en) * | 2019-09-19 | 2019-12-13 | 西安理工大学 | Method for preparing titanium and titanium alloy EBSD sample |
| CN110565159B (en) * | 2019-09-19 | 2022-02-22 | 西安理工大学 | Method for preparing titanium and titanium alloy EBSD sample |
| CN110726743A (en) * | 2019-11-13 | 2020-01-24 | 河北科技大学 | Method for preparing pure titanium EBSD sample at room temperature |
| CN111621841A (en) * | 2020-05-21 | 2020-09-04 | 南京理工大学 | TiAl single crystal EBSD sample-based electrolytic polishing solution and electrolytic method thereof |
| CN111621841B (en) * | 2020-05-21 | 2022-05-10 | 南京理工大学 | TiAl single crystal EBSD sample-based electrolytic polishing solution and electrolytic method thereof |
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