CN111621841B - TiAl single crystal EBSD sample-based electrolytic polishing solution and electrolytic method thereof - Google Patents
TiAl single crystal EBSD sample-based electrolytic polishing solution and electrolytic method thereof Download PDFInfo
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Abstract
The invention discloses an electrolytic polishing solution based on a TiAl single crystal EBSD sample and an electrolytic method thereof, belonging to the technical field of TiAl alloy surface treatment. The electrolytic polishing solution comprises the following components in volume ratio: glycerol: absolute ethyl alcohol (12-15) = (8-11): 100-104), the electrolysis method is: and roughly polishing and finely polishing the polished EBSD sample, performing ultrasonic cleaning, and then performing electrolysis by taking the polished EBSD sample as an anode, a stainless steel sheet as a cathode and an electrolytic polishing solution as electrolyte. The electrolytic polishing method can effectively remove the stress layer and the oxide layer on the surface of the TiAl monocrystal, and the surface of the TiAl monocrystal after electrolytic polishing is flat, bright and clean and free of continuous corrosion pits.
Description
Technical Field
The invention relates to an electrolytic polishing solution based on a TiAl single crystal EBSD sample and an electrolytic method thereof, belonging to the field of surface treatment of TiAl alloy materials.
Background
The Electron backscattering Diffraction (EBSD) technique is a method for determining the crystal structure, orientation and related information based on the analysis of a Diffraction chrysanthemic zone formed by exciting an Electron beam on the surface of an inclined sample in a scanning Electron microscope. EBSD requires that the sample surface not have a residual mechanical polishing-induced processing strain layer, but also be smooth, free of an oxide film, and free of continuous etch pits, so that electropolishing is commonly used as the last processing step for preparing EBSD samples.
TiAl alloy is the only light heat-resistant structural material which can be used for a long time in an oxidation environment at the temperature of more than 600 ℃ at present, and the theoretical density is only 3.9 g/cm3And the Ni-based superalloy is about 8.5 g/cm3And the weight reduction benefit of replacing Ni-based high-temperature alloy with TiAl alloy is huge. The TiAl single crystal invented by Nanjing university of science and technology overcomes the two problems of large room temperature brittleness and low service temperature of TiAl alloy, realizes excellent combination of strength, plasticity and creep resistance and cross-over improvement of comprehensive performance, and has great application prospect (ZL 201410529844.5, ZL 201410528019.3). The TiAl single crystal removes crystal boundary, and the casting structure is a full lamellar structure, wherein alpha2-Ti3The Al phase is a hard phase, the gamma-TiAl phase is a soft phase, the corrosion resistance of the Al phase and the gamma-TiAl phase to the polishing solution is greatly different, and continuous corrosion pits can be generated on the surface by adopting the conventional electrolytic polishing solution, so that the calibration rate of a sample is low. In addition, the conventional electrolytic polishing solution adopts chemical solvents which are volatile, strong in irritation and toxic to human bodies, such as methanol, n-butanol, glacial acetic acid, hydrofluoric acid, ethers and the like as the polishing solution. Based on the reasons, the development of the electrolytic polishing solution and the electrolytic method thereof which have the advantages of low toxicity, no irritation, environmental protection, good stability of the polishing process and high calibration rate is urgently needed.
Disclosure of Invention
The invention aims to provide an electrolytic polishing solution for an EBSD sample based on TiAl single crystal and an electrolytic method thereof.
The technical solution for realizing the purpose of the invention is as follows: an electrolytic polishing solution based on a TiAl single crystal EBSD sample, which consists of the following components in volume ratio: glycerol (b): absolute ethyl alcohol (12-15) = (8-11): 100-104).
An electrolysis method based on a TiAl single crystal EBSD sample comprises the following steps:
(1) firstly, roughly polishing an EBSD sample subjected to polishing treatment on flannelette, finely polishing the EBSD sample on synthetic fiber polishing cloth, and ultrasonically cleaning the EBSD sample for 10min by using absolute ethyl alcohol;
(2) electrolyzing by taking a stainless steel sheet as a cathode, the sample obtained in the step (1) as an anode and an electrolytic polishing solution as electrolyte, wherein during electrolysis, the polishing time is set to be 60-120s, the electrolytic voltage is 20-26V, the distance between the anode and the cathode is 80mm, and the polishing temperature is-30-15 DEG C0C。
Preferably, in the step (1), the polishing solution used for rough polishing and fine polishing is OP-S silicon oxide suspension with the grain size of 0.6 μm.
Preferably, the electrolysis process is stirred using an electromagnetic stirrer.
Compared with the prior art, the invention has the following beneficial effects:
(1) the invention relates to an electrolytic polishing method of TiAl single crystal materials for the first time.
(2) According to the method, the theoretical decomposition voltage of electrolytic polishing is obtained by obtaining the electrolytic characteristic curve, the electrolytic polishing efficiency is improved, the stability of the obtained electrolytic polishing process is good, the EBSD pattern calibration rate is high, and the detection precision is greatly improved.
(3) The electrolytic polishing solution has low cost, is easy to prepare and store and is harmless to human bodies.
(4) The polishing process has the advantages of simple equipment, easy operation, convenient material acquisition of cathode materials and simple manufacture.
Drawings
FIG. 1 is a graph showing the electropolishing characteristics in example 1 of the present invention.
FIG. 2 is a SEM scanning surface topography of a TiAl single crystal EBSD sample in example 1 of the invention.
FIG. 3 is a graph showing the electropolishing characteristics in example 2 of the present invention.
FIG. 4 is a SEM scanning surface topography of a TiAl single crystal EBSD sample in example 2 of the invention.
FIG. 5 is a relative contrast chart of EBSD analysis of TiAl single crystal in example 2 of the present invention.
FIG. 6 is a graph showing the electropolishing characteristics of example 3.
FIG. 7 is an SEM scanning surface topography of a TiAl single crystal EBSD sample in example 3 of the invention.
FIG. 8 is an SEM scanning surface topography of a TiAl single crystal EBSD sample in comparative example 1 of the invention.
FIG. 9 is a relative contrast chart of EBSD analysis of TiAl single crystal in comparative example 1 of the present invention.
Detailed Description
The invention is further elucidated with reference to the embodiments and the drawings. The scope of the invention is not limited to the disclosure.
In the method for electrolyzing the TiAl-single-crystal-based EBSD sample of the present invention described with reference to fig. 3, 5, and 8, the electrolytic voltage set at the time of electrolysis was 20 to 26V, which is a value obtained by recording a voltage-current change curve during electrolysis, and making a straight line intersecting the abscissa of the voltage-current change curve with the inflection point (points a1, C1, E1) of the critical potential, i.e., the current abrupt change point and the end point (points a2, C2, E2) of the curve, thereby obtaining an electropolishing characteristic curve, wherein the intersection point (I = 0) is the theoretical decomposition voltage of electropolishing (point B, D, F), i.e., the optimum electrolytic voltage.
Example 1
The present embodiment provides an electrolytic polishing solution based on a TiAl single crystal EBSD sample and an electrolytic method thereof, which specifically include the following steps:
(1) firstly, roughly polishing a sample subjected to polishing treatment on flannelette, finely polishing the sample on synthetic fiber polishing cloth, selecting OP-S silicon oxide suspension with the granularity of 0.6 mu m as polishing solution, then ultrasonically cleaning the suspension for 10min by using absolute ethyl alcohol, and finally observing the suspension by using an optical microscope;
(2) preparing an electrolytic polishing solution: preparing perchloric acid: glycerol: pouring the electrolytic polishing solution with the volume ratio of absolute ethyl alcohol =12:8:100 into an electrolytic cell;
(3) a stainless steel sheet is taken as a cathode, is connected with a negative electrode of a constant potential power supply and is immersed in the prepared electrolytic polishing solution;
(4) taking the sample obtained in the step (1) as an anode, connecting the anode with a constant potential power supply, and immersing the anode in the prepared electrolytic polishing solution at the polishing temperature of-30 DEG C0C；
(5) Recording a voltage and current change curve in the electrolytic process, drawing an electrolytic polishing characteristic curve by taking a straight line according to an inflection point A1 and an end point A2 of the critical potential, and obtaining the theoretical decomposition voltage of electrolytic polishing as 25V when the straight line segment of the curve at the inflection point reversely deduces that I is 0 (point B) as shown in figure 1;
(6) setting polishing time: 60s, electrolytic voltage setting: 25V, and the distance between the anode and the cathode is 80 mm;
(7) the surface morphology of the TiAl single crystal was analyzed by an electron scanning microscope, as shown in FIG. 2, and the orientation was analyzed by a Channel 5 electron backscatter spectrometer from the company OxFORD. The calibration rate of the TiAl single crystal EBSD pattern is 85 percent.
Example 2
The present embodiment provides an electrolytic polishing solution based on a TiAl single crystal EBSD sample and an electrolytic method thereof, which specifically include the following steps:
(1) firstly, roughly polishing a sample subjected to polishing treatment on flannelette, finely polishing the sample on synthetic fiber polishing cloth, selecting OP-S silicon oxide suspension with the granularity of 0.6 mu m as polishing solution, then ultrasonically cleaning the suspension for 10min by using absolute ethyl alcohol, and finally observing the suspension by using an optical microscope;
(2) preparing an electrolytic polishing solution: preparing perchloric acid: glycerol: pouring the electrolytic polishing solution with the volume ratio of absolute ethyl alcohol =13:9:102 into an electrolytic bath;
(3) a stainless steel sheet is taken as a cathode, is connected with a negative electrode of a constant potential power supply and is immersed in the prepared electrolytic polishing solution;
(4) taking the sample obtained in the step (1) as an anode and connecting a constant potential power supplyThe anode is connected and immersed into the prepared electrolytic polishing solution, and the polishing temperature is-10 DEG0C；
(5) Recording a voltage and current change curve in the electrolytic process, drawing an electrolytic polishing characteristic curve by taking a straight line according to an inflection point C1 and an end point C2 of the critical potential, and obtaining the theoretical decomposition voltage of electrolytic polishing as 20V when the straight line segment of the curve at the inflection point reversely deduces that I is 0 (point D) as shown in figure 3;
(6) setting polishing time: 90s, theoretical split voltage setting: 20V, and the distance between the anode and the cathode is 80 mm.
(7) The surface morphology of the TiAl single crystal was analyzed by an electron scanning microscope as shown in fig. 4 and the orientation was analyzed by a Channel 5 electron backscatter spectrometer from OXFORD as shown in fig. 5. The calibration rate of the TiAl single crystal EBSD pattern is 98 percent.
Example 3
The present embodiment provides an electrolytic polishing solution based on a TiAl single crystal EBSD sample and an electrolytic method thereof, which specifically include the following steps:
(1) firstly, roughly polishing a sample subjected to polishing treatment on flannelette, finely polishing the sample on synthetic fiber polishing cloth, selecting OP-S silicon oxide suspension with the granularity of 0.6 mu m as polishing solution, then ultrasonically cleaning the suspension for 10min by using absolute ethyl alcohol, and finally observing the suspension by using an optical microscope;
(2) preparing an electrolytic polishing solution: preparing perchloric acid: glycerol: pouring the electrolytic polishing solution with the volume ratio of absolute ethyl alcohol =15: 11:104 into an electrolytic cell;
(3) a stainless steel sheet is taken as a cathode, is connected with a negative electrode of a constant potential power supply and is immersed in the prepared electrolytic polishing solution;
(4) taking the sample obtained in the step (1) as an anode, connecting the anode with a constant potential power supply, and immersing the anode in the prepared electrolytic polishing solution, wherein the polishing temperature is 15 DEG0C；
(5) Recording a voltage and current change curve in the electrolytic process, drawing an electrolytic polishing characteristic curve by taking a straight line according to an inflection point E1 and an end point E2 of the critical potential, and obtaining the theoretical decomposition voltage of electrolytic polishing as 26V when the straight line segment of the curve at the inflection point reversely deduces that I is 0 (point F) as shown in FIG. 6;
(6) setting polishing time: 120s, polishing voltage: 26V, and the distance between the anode and the cathode is 80 mm.
(7) The surface morphology of the TiAl single crystal was analyzed by an electron scanning microscope, as shown in fig. 7, and the orientation was analyzed by a tunnel 5 electron backscatter meter from OXFORD. The calibration rate of the TiAl single crystal EBSD pattern is 90 percent.
To illustrate the beneficial effects of the present invention, a series of comparative experiments were performed, wherein the electrolytic polishing solution in comparative example 1 is currently most commonly used in TiAl polycrystalline alloys, and in the electrolytic polishing solution, the volume ratio of methanol: n-butanol: perchloric acid = (12-13): (6-7): (1-2). Meanwhile, in order to further explain that the electrolyte of the invention has the optimal component proportion, in comparative example 4, in the electrolytic polishing solution, by volume ratio, perchlorate: glycerol: absolute ethanol =11:12: 100.
Comparative example 1
The preparation method and the process steps are as follows:
(1) firstly, roughly polishing a sample subjected to polishing treatment on flannelette, finely polishing the sample on synthetic fiber polishing cloth, selecting OP-S silicon oxide suspension with the granularity of 0.6 mu m as polishing solution, then ultrasonically cleaning the suspension for 10min by using absolute ethyl alcohol, and finally observing the suspension by using an optical microscope;
(2) preparing an electrolytic polishing solution: preparing methanol: n-butanol: perchloric acid =12: 7: 1, pouring the electrolytic polishing solution into an electrolytic bath;
(3) a stainless steel sheet is taken as a cathode, is connected with a negative electrode of a constant potential power supply and is immersed in the prepared electrolytic polishing solution;
(4) taking the sample obtained in the step (1) as an anode, connecting the anode with a constant potential power supply, and immersing the anode in the prepared electrolytic polishing solution at the polishing temperature of-30 DEG C0C；
(5) Setting polishing time: 60s, electrolytic voltage setting: 25V, and the distance between the anode and the cathode is 80 mm;
(6) the surface morphology of the TiAl single crystal was analyzed by an electron scanning microscope as shown in fig. 8, and the orientation was analyzed by a Channel 5 electron backscatter spectrometer from OXFORD as shown in fig. 9. The calibration rate of the TiAl single crystal EBSD pattern is 50 percent.
Comparative example 2
The preparation method and the process steps are as follows:
(1) firstly, roughly polishing a sample subjected to polishing treatment on flannelette, finely polishing the sample on synthetic fiber polishing cloth, selecting OP-S silicon oxide suspension with the granularity of 0.6 mu m as polishing solution, then ultrasonically cleaning the suspension for 10min by using absolute ethyl alcohol, and finally observing the suspension by using an optical microscope;
(2) preparing an electrolytic polishing solution: preparing methanol: n-butanol: perchloric acid =13: 6: 2, pouring the electrolytic polishing solution into an electrolytic bath;
(3) a stainless steel sheet is taken as a cathode, is connected with a negative electrode of a constant potential power supply and is immersed in the prepared electrolytic polishing solution;
(4) taking the sample obtained in the step (1) as an anode, connecting the anode with a constant potential power supply, and immersing the anode in the prepared electrolytic polishing solution at the polishing temperature of-25 DEG C0C；
(5) Setting polishing time: 60s, electrolytic voltage setting: 25V, and the distance between the anode and the cathode is 80 mm;
(6) TiAl single crystal surface morphology analysis is carried out by an electron scanning microscope, and orientation analysis is carried out by a Channel 5 electron backscattering instrument of the company OxFORD. The calibration rate of the TiAl single crystal EBSD pattern is 40 percent.
Comparative example 3
The preparation method and the process steps are as follows:
(1) firstly, roughly polishing a sample subjected to polishing treatment on flannelette, finely polishing the sample on synthetic fiber polishing cloth, selecting OP-S silicon oxide suspension with the granularity of 0.6 mu m as polishing solution, then ultrasonically cleaning the suspension for 10min by using absolute ethyl alcohol, and finally observing the suspension by using an optical microscope;
(2) preparing an electrolytic polishing solution: preparing methanol: n-butanol: perchloric acid =12: 7: 1, pouring the electrolytic polishing solution into an electrolytic bath;
(3) a stainless steel sheet is taken as a cathode, is connected with a negative electrode of a constant potential power supply and is immersed in the prepared electrolytic polishing solution;
(4) taking the sample obtained in the step (1) as an anode, connecting the anode with a constant potential power supply, and immersing the anode in the prepared electrolytic polishing solution at the polishing temperature of-10 DEG C0C；
(5) Setting polishing time: 90s, electrolytic voltage setting: 20V, and the distance between the anode and the cathode is 80 mm;
(6) TiAl single crystal surface morphology analysis was performed by an electron scanning microscope and orientation analysis was performed by a Channel 5 electron backscatter spectrometer from OXFORD. The calibration rate of the TiAl single crystal EBSD pattern is 45 percent.
Comparative example 4
The preparation method and the process steps are as follows:
(1) firstly, roughly polishing a sample subjected to polishing treatment on flannelette, finely polishing the sample on synthetic fiber polishing cloth, selecting OP-S silicon oxide suspension with the granularity of 0.6 mu m as polishing solution, then ultrasonically cleaning the suspension for 10min by using absolute ethyl alcohol, and finally observing the suspension by using an optical microscope;
(2) preparing an electrolytic polishing solution: preparing perchloric acid: glycerol: pouring the electrolytic polishing solution with the volume ratio of absolute ethyl alcohol =11:12:100 into an electrolytic cell;
(3) a stainless steel sheet is taken as a cathode, is connected with a negative electrode of a constant potential power supply and is immersed in the prepared electrolytic polishing solution;
(4) taking the sample obtained in the step (1) as an anode, connecting the anode with a constant potential power supply, and immersing the anode in the prepared electrolytic polishing solution at the polishing temperature of-10 DEG C0C；
(5) Setting polishing time: 90s, electrolytic voltage setting: 20V, and the distance between the anode and the cathode is 80 mm;
(6) TiAl single crystal surface morphology analysis is carried out by an electron scanning microscope, and orientation analysis is carried out by a Channel 5 electron backscattering instrument of the company OxFORD. The calibration rate of the TiAl single crystal EBSD pattern is 75 percent.
Claims (5)
1. An electrolytic polishing solution based on a TiAl single crystal EBSD sample is characterized by comprising the following components in volume ratio: glycerol (b): absolute ethyl alcohol (12-15) = (8-11): 100-104).
2. An electrolysis method based on a TiAl single crystal EBSD sample is characterized by comprising the following steps:
(1) firstly, roughly polishing an EBSD sample subjected to polishing treatment on flannelette, finely polishing the EBSD sample on synthetic fiber polishing cloth, and ultrasonically cleaning the EBSD sample for 10min by using absolute ethyl alcohol;
(2) electrolyzing by using a stainless steel sheet as a cathode, the sample obtained in the step (1) as an anode and the electrolytic polishing solution as the electrolyte according to claim 1, wherein the polishing time is set to be 60-120s, the electrolytic voltage is 20-26V, the distance between the anode and the cathode is 80mm, and the polishing temperature is-30-15 DEG C0C。
3. The method according to claim 2, wherein in the step (1), the polishing liquid used for the rough polishing and the fine polishing is OP-S silica suspension with a particle size of 0.6 μm.
4. The method of claim 2, wherein the electrolysis process is stirred using an electromagnetic stirrer.
5. The method of claim 2, wherein the voltage-current curve is recorded during the electrolysis, and the inflection point of the curve at the critical potential and the end point of the potential are taken as straight lines, which intersect with the abscissa of the voltage-current curve, and the resulting intersection point is the theoretical decomposition voltage, i.e., the electrolysis voltage.
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