CN102899711B - A kind of electrolytic polishing liquid for titanium or titanium alloy and electrolytic polishing process - Google Patents
A kind of electrolytic polishing liquid for titanium or titanium alloy and electrolytic polishing process Download PDFInfo
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- CN102899711B CN102899711B CN201210471090.3A CN201210471090A CN102899711B CN 102899711 B CN102899711 B CN 102899711B CN 201210471090 A CN201210471090 A CN 201210471090A CN 102899711 B CN102899711 B CN 102899711B
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Abstract
The invention discloses a kind of electrolytic polishing liquid for titanium or titanium alloy and electrolytic polishing process, the peracetic acid formulation that described polishing fluid is 8-15% perchloric acid and 85-92% by volume fraction forms.This polishing fluid is drawn materials conveniently, and be easy to preparation and store, glossing equipment is simple, easy handling, significantly can reduce the stress on sample top layer, and smooth surface is smooth simultaneously, without obvious cut and oxide film, EBSD style recognition rate is high, increases substantially accuracy of detection.
Description
Technical field
The present invention relates to field of metal surface treatment, specifically, relate to a kind of electrolytic polishing liquid of preparing for titanium or titanium alloy Electron Back-Scattered Diffraction (electionbackscatterdiffraction, EBSD) sample and electrolytic polishing process.
Technical background
Since the nineties in 20th century, be assemblied in the electron backscattered style (ElectronBack-scatteringPatterns on SEM, being called for short EBSP) analytical technology of crystal microcell orientation and crystalline structure achieves larger development, and widespread use in microstructure and micro-texture characterize.This technology is also referred to as Electron Back-Scattered Diffraction (ElectronBackscatteredDiffraction is called for short EBSD).The principal feature of EBSD is the diffraction (providing the data of crystallography) carrying out spatial resolution submicron order while the conventional feature retaining scanning electronic microscope.At present, EBSD technology can realize automatically gathering microcell orientation information, sample preparation is simpler, acquisition speed fast (can reach about 360,000 points/hour even faster), resolving power high (spatial resolution and angular resolution can reach 0.1 ° of m and 0.5m respectively), for the heterogeneous microstructure of quantitative statistics research material rapidly and efficiently and texture are laid a good foundation, therefore become a kind of effective analysis means in investigation of materials.
The advantages such as it is high that titanium or titanium alloy has specific tenacity, fine corrosion resistance, and high-temperature behavior is good, are therefore widely used in fields such as the energy, chemical industry, metallurgy, automobile, space flight and aviation.Therefore, microstructure is carried out to titanium or titanium alloy and crystallography analysis significant.Now in the art, EBSD is used to carry out in microstructure and crystallography analysis process to titanium or titanium alloy, in EBSD sample preparation, EBSD technology requires strict to specimen surface, surface smoothing, can not stress be there is, therefore be not easy preparation, need to carry out mechanical polishing or chemical rightenning process to EBSD sample.But it is long that mechanical polishing exists the cycle, there is unrelieved stress in destructible specimen surface, reduces EBSD style recognition rate, and the defect such as rumbling compound quartz silicon latex is expensive; And electropolishing, needing special polishing fluid, there is the problem of complicated component, not easily preparation and glossing less stable in current domestic disclosed titanium or titanium alloy electrolytic polishing liquid.
Summary of the invention
For prior art above shortcomings, the present invention solves the problem that titanium or titanium alloy electrolytic polishing liquid exists complicated component, not easily preparation and glossing less stable, provides a kind of electrolytic polishing liquid prepared for titanium or titanium alloy EBSD sample.
The present invention also provides a kind of easy handling, the electrolytic polishing process for titanium or titanium alloy EBSD sample that after polishing, EBSD style recognition rate is high.
Realize above-mentioned purpose, the present invention adopts following technical scheme: a kind of electrolytic polishing liquid for titanium or titanium alloy, is characterized in that, this polishing fluid is that 8-15% perchloric acid and 85-92% peracetic acid formulation form by volume fraction.
Further, the present invention also provides a kind of titanium or titanium alloy EBSD electrolytic polishing process tested, and comprises the steps:
(1) first, titanium or titanium alloy sample is carried out abrasive paper for metallograph polishing, sand paper model is respectively 400 orders, 600 orders, 800 orders, 1500 orders and 2000 orders;
(2) electrolytic polishing liquid is prepared: dose volume mark is the perchloric acid acetic acid solution of 8-15% perchloric acid and 85-92% acetic acid, pours in electrolyzer;
(3) with titanium or titanium alloy sample for anode, be connected with D.C. regulated power supply positive pole, immerse in the electrolytic polishing liquid prepared;
(4) take stainless steel substrates as negative electrode, be connected with D.C. regulated power supply negative pole, immerse in the polishing fluid of above-mentioned preparation and carry out polishing, polish temperature is
subzero5-10 DEG C.
Further, described polishing time is 15-60s, and polishing voltage is 50-80V, and the distance between anode and 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, with low cost, is easy to preparation and stores, harmless.
2, EBSD analytical technology requires high to specimen surface, require that specimen surface is smooth, fresh, unstressed, without obvious cut and oxide film etc., general conventional polishing fluid and glossing cannot meet the demands and the scope of application is little, not easily prepares, adopts polishing fluid of the present invention and glossing to meet 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 operates; 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.
Accompanying drawing explanation
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, for electrolytic polishing liquid prepared by titanium or titanium alloy EBSD sample, taking acetic acid as solvent, is that 8-15% perchloric acid and 85-92% peracetic acid formulation form by volume fraction.
Wherein, perchloric acid and acetic acid all adopt chemical pure or analytically pure reagent.
Specific embodiment formula (unit is volume fraction) as shown in the table:
| Raw material | Formula 1 | Formula 2 | Formula 3 | Formula 4 |
| Perchloric acid | 10 | 12 | 8 | 15 |
| Acetic acid | 90 | 88 | 92 | 85 |
| Add up to | 100 | 100 | 100 | 100 |
Two, for the electrolytic polishing process of titanium or titanium alloy EBSD sample, specific embodiment and step as follows
Embodiment 1, a kind of electrolytic polishing process for titanium or titanium alloy EBSD sample, comprises the steps:
(1) sample polishing: polish successively to Ti-3Al-4Cr-2Fe titanium alloy with 400 orders, 600 orders, 800 orders, 1500 orders and 2000 object abrasive paper for metallograph respectively, cleans surface and dries;
(2) electrolytic polishing liquid is prepared: prepare by upper table formula 1;
(3) with the Ti-3Al-4Cr-2Fe titanium alloy sample after polishing for anode, be connected with D.C. regulated power supply positive pole and immerse in the electrolyzer filling the electrolytic polishing liquid that step (2) is prepared;
(4) take stainless steel substrates as negative electrode, be connected with D.C. regulated power supply negative pole and immerse in the electrolyzer filling above-mentioned electrolytic polishing liquid;
(5) carry out polishing at above-mentioned electrolytic solution, polish temperature is
subzero0 ~ 5 DEG C, polishing time is 40s, and polishing voltage is 65V, and the distance between anode and negative electrode is 70mm;
(6) the sample taking-up after polishing is dried, surfacing light, adopt the EBSD system of Nova400Nano-SEM field emission scanning electron microscope to test Ti-3Al-4Cr-2Fe titanium alloy sample.
As shown in Figure 1, EBSD style recognition rate is high for test result, and average confidence index (AverageConfidenceIndex) 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) electrolytic polishing liquid is prepared: prepare by upper table formula 2;
(3) with the TC4 titanium alloy sample after polishing for anode, being connected with D.C. regulated power supply positive pole and immersing fills in the electrolyzer of electrolytic polishing liquid;
(4) take stainless steel substrates as negative electrode, being connected with D.C. regulated power supply negative pole and immersing fills in the electrolyzer of electrolytic polishing liquid;
(5) in above-mentioned electrolytic solution, carry out polishing, polish temperature is
subzero5-10 DEG C, polishing time is 35s, and polishing voltage is 60V, and the distance between anode and negative electrode is 60mm.
(6) the sample taking-up after polishing is dried, surfacing light, adopt the EBSD system of Nova400Nano-SEM field emission scanning electron microscope to carry out test test result as shown in Figure 2 to TC4 titanium alloy sample.
As shown in Figure 2, EBSD style recognition rate is that EBSD style recognition rate is high to test result, and average confidence index is 0.81.
What finally illustrate is, above embodiment is only in order to illustrate technical scheme of the present invention and unrestricted, although by referring to the preferred embodiments of the present invention, invention has been described, but those of ordinary skill in the art is to be understood that, various change can be made to it in the form and details, and not depart from the spirit and scope of the present invention that appended claims limits.
Claims (1)
1. an electrolytic polishing process for titanium or titanium alloy EBSD sample, is characterized in that, step is as follows:
(1) sample polishing: polish successively to Ti-3Al-4Cr-2Fe titanium alloy with 400 orders, 600 orders, 800 orders, 1500 orders and 2000 object abrasive paper for metallograph respectively, cleans surface and dries;
(2) electrolytic polishing liquid is prepared: volume fraction is the perchloric acid acetic acid solution of 8-15% perchloric acid and 85 ~ 92% acetic acid;
(3) with the Ti-3Al-4Cr-2Fe titanium alloy sample after polishing for anode, be connected with D.C. regulated power supply positive pole and immerse in the electrolyzer filling the electrolytic polishing liquid that step (2) is prepared;
(4) take stainless steel substrates as negative electrode, be connected with D.C. regulated power supply negative pole and immerse in the electrolyzer filling above-mentioned electrolytic polishing liquid;
(5) carry out polishing at above-mentioned electrolytic solution, polish temperature is
subzero0 ~ 5 DEG C, polishing time is 40s, and polishing voltage is 65V, and the distance between anode and negative electrode is 70mm;
(6) the sample taking-up after polishing is dried, surfacing light, adopt the EBSD system of Nova400Nano-SEM field emission scanning electron microscope to test Ti-3Al-4Cr-2Fe titanium alloy sample.
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Cited By (1)
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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 |
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| CN105369340A (en) * | 2015-11-11 | 2016-03-02 | 无锡清杨机械制造有限公司 | Titanium alloy polishing method |
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| 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 |
| CN110565159B (en) * | 2019-09-19 | 2022-02-22 | 西安理工大学 | Method for preparing titanium and titanium alloy EBSD sample |
| CN110726743B (en) * | 2019-11-13 | 2022-06-14 | 河北科技大学 | Method for preparing pure titanium EBSD sample at room temperature |
| 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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