CN114113176B - Preparation method of titanium alloy EBSD sample - Google Patents
Preparation method of titanium alloy EBSD sample Download PDFInfo
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- CN114113176B CN114113176B CN202111515947.2A CN202111515947A CN114113176B CN 114113176 B CN114113176 B CN 114113176B CN 202111515947 A CN202111515947 A CN 202111515947A CN 114113176 B CN114113176 B CN 114113176B
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Abstract
The invention relates to a novel preparation method of a titanium alloy EBSD sample, belongs to the field of titanium alloy tissue and texture detection, and solves the technical problems that the preparation of the titanium alloy EBSD sample is difficult and the efficiency is low in the prior art. The preparation method of the titanium alloy EBSD sample provided by the invention comprises the following steps: step 1, cutting a sample; performing linear cutting on the sample tissue; step 2, mechanically polishing; machine polishing the cut sample by using 400-mesh sand paper, and then directly manually polishing the sample by using 3000-mesh sand paper; step 3, electrolytic polishing; electrolytic polishing is carried out by using perchloric acid ethanol solution as electrolyte; step 4, cleaning and corroding; and after the sample is subjected to electrolytic polishing, cleaning by adopting a cleaning agent, after cleaning, carrying out corrosion treatment on the surface by using KROLL solution, and after corrosion, putting the sample into alcohol for cleaning and drying to obtain the titanium alloy EBSD sample. The invention realizes the efficient, rapid and high-quality preparation of the titanium alloy EBSD sample.
Description
Technical Field
The invention relates to the technical field of titanium alloy tissue and texture detection, in particular to a preparation method of a titanium alloy EBSD sample.
Background
With the continuous deep research of titanium alloy anisotropy phenomenon, the application of the back scattering diffraction technology (EBSD) in the titanium alloy texture characterization is continuously promoted. The titanium alloy material has high metal mobility, and the processes of polishing, polishing and the like often involve oxidation phenomena in the preparation process of an EBSD detection sample. In addition, the proton number of titanium is relatively small in the metal material, and in the process of detecting the structure and texture of the titanium by using an EBSD method, a back scattering electronic signal is relatively weak, and the texture information is relatively difficult to collect. For the titanium alloy EBSD detection sample, the detection surface quality of the sample is required to be high.
Therefore, a set of rapid, reliable, convenient and feasible preparation method for the titanium alloy texture detection sample is developed, and the method has great practical significance for improving the detection precision and efficiency of the titanium alloy texture and reducing the anisotropic characterization difficulty of the titanium alloy material.
Disclosure of Invention
In view of the above analysis, the invention aims to provide a novel preparation method of a titanium alloy EBSD sample, which is used for solving the problems of high sample preparation difficulty, low efficiency, poor surface quality of prepared samples and the like in the preparation process of the existing EBSD detection sample.
The aim of the invention is mainly realized by the following technical scheme:
the invention provides a preparation method of a titanium alloy EBSD sample, which comprises the following steps:
step 1, cutting a sample;
performing linear cutting on the sample tissue;
step 2, mechanically polishing;
machine polishing the cut sample by using 400-mesh sand paper, and then directly manually polishing the sample by using 3000-mesh sand paper;
step 3, electrolytic polishing;
electrolytic polishing is carried out by using perchloric acid ethanol solution as electrolyte;
step 4, cleaning and corroding;
and after the sample is subjected to electrolytic polishing, cleaning by adopting a cleaning agent, after cleaning, carrying out corrosion treatment on the surface by using KROLL solution, and after corrosion, putting the sample into alcohol for cleaning and drying to obtain the titanium alloy EBSD sample.
Further, in step 1, the titanium alloy EBSD sample detection surface size is controlled within the range of 10mm×10 mm.
Further, in the step 2, the cut sample is mechanically polished by a polishing machine, the rotating speed of the polishing machine is 400r/min-900r/min, and water is continuously introduced in the mechanical polishing process for cooling.
Further, in step 3, the volume fraction of the perchloric acid-ethanol solution is 2-10%.
Further, in the step 4, the cleaning agent is alcohol, after the sample is subjected to electrolytic polishing, the sample is immediately placed into the alcohol and then placed into ultrasonic cleaning equipment for cleaning for 10s-30s, and the ultrasonic cleaning frequency is 25-50kHz.
Further, in step 1, the cleaning frequency is 25-50kHz.
Further, in step 3, the electrolysis process is performed at room temperature, the electrolysis voltage is 25V-30V, and the electrolysis current is 350mA-800mA.
Further, in step 3, the sample immersion depth is controlled to be in the range of 2mm to 4mm, and the electrolysis time is 30s to 70s.
Further, in step 4, the mass ratio of the KROLL solution includes: 1-3% HF,2-6% HNO 3 The balance being water.
Further, the KROLL solution has an etching time of 4s to 10s.
Compared with the prior art, the invention has at least one of the following beneficial effects:
(1) The traditional mechanical polishing and sample preparation process needs 2 hours, the traditional mechanical polishing and electrolytic polishing combined one-time success rate is low, and the whole sample preparation process needs 30 minutes; the invention can prepare the high-quality EBSD detection surface in a short time, has higher one-time success rate, and shortens the whole sample preparation process to within 5 minutes. The preparation method of the titanium alloy EBSD detection sample provided by the invention obviously improves the preparation efficiency and success rate of the titanium alloy EBSD sample.
(2) The invention has the important point that compared with the traditional sample preparation method, the preparation of the high-quality EBSD detection sample is completed quickly and efficiently, and the invention adopts a certain control for preventing the oxidation of the EBSD sample, for example, a surface is polished by mechanical water adding and a surface is removed by dry grinding with 3000-mesh sand paper to a certain degreeSurface oxidation, electrolytic polishing, soaking in alcohol solution to stabilize active metal, and etching with etchant (1-3% HF,2-6% HNO by mass ratio) 3 KROLL solution with the balance being water) to promote the homogenization of the surface oxidation of the sample. The titanium alloy EBSD sample prepared by the method has high surface quality, strong adaptability and high and low equipment configuration, can be detected, and the calibration rate of the detection result is up to 97%; the universality is high, and the method is suitable for various brands and technical titanium alloy samples; the stability is good, is applicable to sample batch detection.
(3) The invention improves the preparation efficiency and quality of the titanium alloy Electron Back Scattering Diffraction (EBSD) detection sample, simplifies the flow of the titanium alloy texture detection sample, forms a system scheme, effectively reduces the detection difficulty of the titanium alloy EBSD and promotes the application of the electron back scattering diffraction technology in the research of the titanium alloy anisotropy phenomenon.
In the invention, the technical schemes can be mutually combined to realize more preferable combination schemes. Additional features and advantages of the invention will be set forth in the description which follows, and in part will be obvious from the description, or may be learned by practice of the invention. The objectives and other advantages of the invention may be realized and attained by the embodiments of the invention particularly pointed out in the written description and drawings.
Drawings
The drawings are only for purposes of illustrating particular embodiments and are not to be construed as limiting the invention, like reference numerals being used to refer to like parts throughout the several views.
FIG. 1 is a schematic diagram of the structure of a titanium alloy EBSD sample preparation;
FIG. 2 is a detection surface of an EBSD detection sample;
FIG. 3 is a diagram showing the preparation of sample orientation imaging and polar image information by the EBSD method;
FIG. 4 test surface of EBSD sample prepared by conventional buffing and electropolishing methods.
Detailed Description
The following detailed description of preferred embodiments of the invention is made in connection with the accompanying drawings, which form a part hereof, and together with the description of the embodiments of the invention, are used to explain the principles of the invention and are not intended to limit the scope of the invention.
In one aspect, the invention also provides a preparation method of the titanium alloy EBSD sample, which comprises the following steps:
step 1, sample cutting
The linear cutting machining is adopted, the heat quantity in the machining process is small, the cooling condition is good, and the influence on the sample tissue is small.
In the above step 1, the sample detection surface size is controlled within the range of 10mm×10mm, and the preferred size is 7mm×7mm.
Step 2, mechanical polishing
The 400-mesh sand paper is fixed on a mechanical polishing machine and then mechanically polished to remove surface line cutting traces and rough layers, other-mesh sand paper is skipped, and then 3000-mesh sand paper is directly used for hand polishing to remove the surface oxide layer.
The step simplifies the polishing process, removes the rough layer on the surface of the titanium alloy sample, and obtains the polished surface of the titanium alloy sample with fine and uniform scratches.
Step 3, electrolytic polishing is carried out by taking perchloric acid ethanol solution as electrolyte;
specifically, 100-160 mL of perchloric acid ethanol solution with the volume fraction of 2% -10% is poured into a cup-shaped graphite tank as electrolyte, the electrolyte floods the 1/2 position of the volume of the cup-shaped graphite tank, a titanium alloy sample after mechanical polishing is placed into a cleaning tank of an ultrasonic cleaning unit, and after ultrasonic cleaning is performed for 10s-30s, the titanium alloy sample is fixed on an open-ended adjustable tweezer. Starting an adjustable-speed magnetic stirrer, controlling the rotating speed of a magnetic rotor to be 100-200 r/min, properly adjusting the central position of the magnetic rotor, switching on a direct-current power supply after electrolyte rotates stably along with the magnetic rotor, setting the voltage of the direct-current power supply to be 25-30V, setting the electrolysis current to be 350-800 mA, keeping the electrolytic surface immersed in the electrolyte for 2-4 mm in the electrolysis process, setting the electrolysis time to be 30-70 s, and putting the electrolyte into an ultrasonic cleaning unit for cleaning after the electrolysis is completed, thus obtaining a high-quality electrolytic polished titanium alloy sample;
step 4, cleaning and etching
And after the titanium alloy sample is subjected to electrolytic polishing, cleaning by adopting a cleaning agent, after cleaning, carrying out corrosion treatment on the surface by using KROLL solution, and after corrosion, putting the titanium alloy sample into alcohol for cleaning and drying to obtain the titanium alloy EBSD sample.
Step 5, preserving the titanium alloy sample
After the titanium alloy sample preparation is completed, the titanium alloy EBSD sample which cannot be subjected to texture detection immediately needs to be stored. The surface of the corroded titanium alloy EBSD sample is stable, and the sample can be stored by using a titanium alloy sample box and a self-sealing bag in short-term storage, so that the surface grinding is avoided. If long-term storage is needed, the anti-oxidation adhesive tape can be stuck on the detection surface of the titanium alloy sample, and a drying agent can be added into the titanium alloy sample box for long-term storage.
The existing polishing and electropolishing method is used for preparing a titanium alloy sample, the surface has concave-convex relief, the surface has a certain degree of dark oxidation trace, in the detection process of the EBSD method, the surface unevenness and slight relief have a certain influence on the accuracy of a detection result, and the surface oxidation of the titanium alloy sample used for detection can influence the calibration rate of the titanium alloy sample.
The detection surface of the EBSD sample is shown in figure 2, the detection surface of the EBSD sample prepared by the common polishing and electropolishing method is shown in figure 2, the orientation imaging diagram and the polar diagram information of the sample prepared by the novel EBSD method are shown in figure 3, and by comparison, the grain boundary of the size crystal grain of the titanium alloy EBSD sample prepared by the method provided by the invention is clear and definite, the grain orientation information is reliable and accurate, and the method has higher quality and can be used as an effective reference for statistics of the orientation information of the titanium alloy sample.
In the above step 1, the size of the detection surface of the titanium alloy sample structure should be controlled within the range of 10mm×10mm, and the preferred size is 7mm×7mm, with the purpose of: because the electrolytic quality is not easy to control due to the overlarge detection area of the titanium alloy sample structure, and the edge of the titanium alloy sample structure is easy to appear an arc surface due to the electrolytic action when the detection area of the titanium alloy sample structure is too small, thereby being unfavorable for structure observation.
In the step 2, compared with the traditional polishing method, the invention omits 600, 800, 1000, 1200 and 1500-mesh sand paper polishing processes, can greatly simplify the polishing process, reduces the sand paper use, greatly reduces the sample preparation time and sample preparation cost, and can achieve the same treatment effect. The polishing surface with fine scratches can be obtained under the action of 400-mesh sand paper due to the higher rotating speed (the rotating speed is 400-900 r/min) of the mechanical polishing machine in the mechanical polishing process, but the surface is oxidized after being polished due to continuous water cooling in the mechanical polishing process, so that the 3000-mesh sand paper is directly used for hand polishing after mechanical polishing to mainly remove the oxidized layer and further refine the scratches.
In order to further improve the sample preparation efficiency, in the step 2, a plurality of titanium alloy samples may be marked separately by using a mosaic method, and then mosaic may be performed intensively, followed by primary polishing.
It should be noted that, in the above step 3, the purpose of controlling the above electrolysis parameters within the respective ranges is to: the electrolytic process can be stable and uniform in the electrolytic polishing of the titanium alloy, and the surface of the titanium alloy sample can be well electrolyzed. Under the action of electrolyte and an externally applied electric field, the titanium alloy sample is used as an anode, electrons are lost to form metal ions, the titanium alloy sample is peeled off, and the titanium alloy sample exposes a smooth and unoxidized surface.
In the step 4, after the titanium alloy sample tissue is electropolished, the surface is bright and clean and has no oxidation, the activity of the titanium alloy material is higher, the titanium alloy material is unstable in contact with air, stabilization treatment is needed, alcohol is used as a cleaning agent, an ultrasonic cleaning machine is combined for vibration cleaning for 10s-30s, the cleaning frequency is 25-50kHz, and the oxidation process can be stabilized. After washing with alcohol, KROLL solution (1-3% HF,2-6% HNO by mass fraction) is used 3 Aqueous solution) to perform corrosion treatment on the surface, thereby realizing the stabilization of the electrolytic surface.
On the other hand, the invention also provides a titanium alloy EBSD sample preparation device, which has the design principle that:
in the electrolytic polishing process, microscopic fluctuation exists on the surface of the titanium alloy sample after polishing treatment, and under the action of an external electric field, the anode is oxidized to form metal ions, and after the metal ions are peeled off from the surface of the anode, the metal ions are gathered on the electrolytic surface in the traditional electrolytic polishing process, and the gathering at the concave part is more obvious. When the concentration reaches a certain level, a large amount of cations are accumulated or oxides are formed to adhere to the electrolytic surface, or the cations are unevenly distributed to prevent the electrolytic process from proceeding, so that the electrolytic surface is oxidized or rugged. According to the invention, by introducing the magnetic stirring device, a certain flow rate is applied to the electrolyte, under the action of external force, metal ions leave the surface of the anode and are rapidly diffused, so that the electrolytic polishing process is promoted to be carried out stably, and the polished part exposes a smooth and clean surface, thus a high-quality texture detection sample can be obtained.
Compared with the prior art, the novel titanium alloy EBSD sample preparation equipment is used for texture detection samples of the titanium alloy back scattering electron diffraction (EBSD) technology with higher surface quality requirements, fine tissues and higher analysis precision, and the electrolysis quality is improved by introducing a magnetic stirring device (an adjustable speed magnetic stirrer) in the sample electrolytic polishing process to forcedly diffuse ions.
According to the design principle, as shown in fig. 1, the preparation device of the titanium alloy EBSD sample comprises an operation table main body, wherein a direct current power supply unit, an ultrasonic cleaning unit and an electrolytic polishing unit are sequentially arranged on the operation table main body; the direct current power supply unit is used for providing stable electrolytic voltage; the ultrasonic cleaning unit is used for cleaning residual sand grains of the titanium alloy sample before electrolysis and residual electrolyte of the titanium alloy sample after electrolysis; the electrolytic polishing unit comprises an electrolytic tank, a speed-adjustable magnetic stirrer, a magnetic rotor, a cathode, an anode and electrolyte; the bottom of the electrolytic tank is arranged at the center above the speed-adjustable magnetic stirrer, the magnetic rotor and the electrolyte are arranged in the electrolytic tank, and the cathode and the anode are both arranged in the electrolytic tank; the speed-adjustable magnetic stirrer and the magnetic rotor are used for stirring the electrolyte to generate flow.
Specifically, the preparation device comprises an operation table main body, wherein a direct-current power supply unit, an ultrasonic cleaning unit and an electrolytic polishing unit are sequentially arranged on the operation table main body; the direct current power supply unit is used for providing stable electrolytic voltage, can provide an adjustable voltage range of 0-45V, and is used for ensuring that the electrolytic polishing process can be stably and uniformly carried out, thereby ensuring that a good electrolytic effect can be generated. The ultrasonic cleaning unit is used for cleaning residual sand grains of the titanium alloy sample before electrolysis and residual electrolyte of the titanium alloy sample after electrolysis.
The electrolytic polishing unit comprises an electrolytic tank, a speed-adjustable magnetic stirrer, a magnetic rotor, a cathode, an anode and electrolyte; wherein, the electrolysis trough locates the center department above the adjustable speed magnetic stirrer, or put in the center department of adjustable speed magnetic stirrer top surface in the electrolysis trough, and magnetic rotor and electrolyte are arranged in the electrolysis trough, and the cathode is located in the electrolysis trough, and the negative pole is connected with the power negative pole, and the positive pole submerges in the electrolyte to be connected with power positive pole. The speed-adjustable magnetic stirrer and the magnetic rotor are used for stirring the electrolyte to generate flow; when the power is on, an electric field can be formed in the electrolyte, under the action of the electric field, electrons of the anode material lose to form metal ions and are separated from the surface, and meanwhile, the speed-adjustable magnetic stirrer stirs the electrolyte to flow so as to force the metal ions to diffuse, thereby reducing the ion concentration on the surface of the electrolytic titanium alloy sample and finally promoting the uniform progress of the electrolytic process.
Compared with the prior art, the invention integrates the direct-current power supply unit, the ultrasonic cleaning unit and the electrolytic polishing unit on the operating table main body, thereby not only shortening the operation flow, but also having simple preparation process and being capable of obviously improving the preparation efficiency of the titanium alloy EBSD sample; in addition, the invention can finish the electrolytic polishing process of the titanium alloy sample within 1min by arranging the speed-adjustable magnetic stirrer and the magnetic rotor, the prepared titanium alloy EBSD sample has high success rate and good surface quality, and the high-quality calibration can be realized in a tungsten filament scanning electron microscope with lower energy and poorer configuration and an EBSD device matched with the tungsten filament scanning electron microscope; it is also emphasized that the preparation device of the invention is operated under room temperature submission without liquid nitrogen cooling low temperature conditions, so the preparation process of the titanium alloy EBSD sample is greatly simplified.
In order to avoid the reaction of cathode materials and electrolyte, the electrolytic tank is a cup-shaped glass tank, cup-shaped graphite is arranged on the inner wall of the cup-shaped glass tank, and the outer wall of the cup-shaped graphite is attached to the inner wall of the electrolytic tank to form a cup-shaped graphite tank; taking cup-shaped graphite as a cathode; the anode was a titanium alloy sample.
Specifically, the adjustable speed magnetic stirrer is embedded in the operation panel main body, a cup-shaped glass groove is arranged in the center of the upper part of the adjustable speed magnetic stirrer, cup-shaped graphite is arranged in the cup-shaped glass groove, the outer wall of the cup-shaped graphite is attached to the inner wall of the cup-shaped glass groove, electrolyte is contained in the cup-shaped graphite, and a magnetic rotor is arranged at the bottom of the cup-shaped graphite. It should be noted that the cup-shaped graphite of the present invention has the following specifications(diameter x height), graphite thickness 2mm; the specification of the magnetic rotor is phi 6mm multiplied by 20mm. The electrolyte adopts perchloric acid ethanol solution with the volume fraction of 2-10 percent.
The cathode materials adopted in the prior art are generally metal materials, and the metal materials are adopted as the cathode to easily react with electrolyte; compared with the prior art, the invention adopts cup-shaped graphite as the cathode material, because the graphite material has stable property, is not easy to react with electrolyte, has good conductivity, is soft and is easy to process and form.
The ultrasonic cleaning unit comprises an ultrasonic cleaning machine, wherein the ultrasonic cleaning frequency is 25-50kHz, and the vibration cleaning time of the ultrasonic cleaning machine is 10-30 s.
The preparation device of the invention also comprises a mechanical polishing unit, wherein the mechanical polishing unit comprises a mechanical polishing machine (for example, a stepless speed change metallographic specimen mechanical polishing machine), 400-mesh sand paper and 3000-mesh sand paper; the mechanical polishing process includes: 400 mesh sandpaper was fixed on a mechanical polisher for mechanical polishing, and then hand-polished directly with 3000 mesh sandpaper.
Compared with the prior art, the invention uses a mechanical polishing machine to carry out 400-mesh sand paper machine polishing to remove surface line cutting traces and rough layers, skips other mesh sand paper, and then directly uses 3000-mesh sand paper to remove surface oxide layers by hand polishing. The invention can remove the rough layer on the surface of the titanium alloy sample by arranging the mechanical polishing unit, thereby obtaining the polished surface with fine and uniform scratches.
In order to adjust the position of the titanium alloy sample immersed in the electrolyte, the electrolytic polishing unit further comprises a first conductive connecting part, a second conductive connecting part and a third conductive connecting part; the first conductive connecting part is 7-shaped, the vertical part of the first conductive connecting part is fixed on the operating platform main body and is connected with the positive electrode of the power supply, and the transverse part of the first conductive connecting part is provided with a first screw hole; the second conductive connecting part comprises a first hollow screw rod, the external thread of the first hollow screw rod is matched with the internal thread of the first screw hole, and the first hollow screw rod penetrates through the first screw hole; the bottom end of the first hollow screw is provided with a first clamping part, and the first clamping part is used for clamping and fixing the titanium alloy sample, so that the titanium alloy sample is immersed in the electrolyte; the third conductive connecting part is used for connecting the cup-shaped graphite and the power supply negative electrode.
Specifically, when the immersion position of the titanium alloy sample needs to be adjusted, the adjustment of the relative position between the first hollow screw and the first screw hole can be realized, for example, the immersion depth of the titanium alloy sample is large, so that the distance between the titanium alloy sample and the bottom surface of the cup-shaped graphite is too small, at the moment, the first hollow screw is screwed, and the first hollow screw is enabled to move upwards relative to the first screw hole, so that the distance between the titanium alloy sample and the bottom surface of the cup-shaped graphite is increased.
Compared with the prior art, the method can realize the adjustment of the position of the titanium alloy sample in the electrolyte by adjusting the relative positions of the first hollow screw and the first screw hole, thereby avoiding the excessively fast or slow electrolysis rate caused by the excessively close or excessively far distance between the titanium alloy sample and the bottom surface of the cup-shaped graphite, and being unfavorable for the formation of high-quality surfaces; in addition, the titanium alloy sample is firmly clamped by the clamping part arranged at the bottom end of the first hollow screw rod, so that the titanium alloy sample is stably immersed in the electrolyte.
It should be noted that the clamping part of the invention is an opening-adjustable tweezer, and the titanium alloy sample is clamped by the opening-adjustable tweezer, so that the electrolytic polishing surface of the titanium alloy sample is parallel to the liquid surface of the electrolyte.
In order to conveniently adjust the position of the titanium alloy sample immersed in the electrolyte, the top of the first hollow screw rod is provided with the first rotary handle, and the immersed position of the titanium alloy sample at the bottom of the first hollow screw rod can be adjusted through the first rotary handle.
It should be noted that, in the electrolytic polishing process, the magnetic rotor can exert stirring effect and does not interfere with the electrolytic polishing process; in addition, the distance between the electrolytic surface of the titanium alloy sample and the bottom surface of the cup-shaped graphite is controlled within the range of 20-40mm in the electrolytic polishing process, and if the distance between the electrolytic surface and the bottom surface of the cup-shaped graphite is smaller than 20mm or larger than 40mm, the electrolytic rate is too fast or too slow, which is not beneficial to the formation of the high-quality surface of the titanium alloy sample.
In order to prepare a plurality of titanium alloy EBSD samples at the same time, the preparation efficiency of the samples is further improved, and a second screw hole and a third screw hole are further formed in the transverse part of the first conductive connecting part; the second connecting conductive part further comprises a second hollow screw rod and a third hollow screw rod, and the second hollow screw rod penetrates through the second screw hole and is matched with the second screw hole in screw threads; the third hollow screw rod penetrates through the third screw hole, and the threads of the third hollow screw rod and the third screw hole are matched; the bottom end of the second hollow screw is provided with a second clamping part, and the bottom end of the third hollow screw is provided with a third clamping part; the second clamping part and the third clamping part are used for clamping and fixing the titanium alloy sample.
Compared with the prior art, the invention can realize the simultaneous preparation of a plurality of titanium alloy samples by arranging the plurality of hollow screws and arranging the clamping parts at the bottoms of the hollow screws correspondingly, and can further improve the preparation efficiency of the titanium alloy EBSD samples.
It should be noted that the first screw hole, the second screw hole and the third screw hole have the same specification; the first hollow screw, the second hollow screw and the third hollow screw are identical in structure and size; the first clamping part, the second clamping part and the third clamping part are identical in structure and size.
It is emphasized that the number of the electrolytic polishing units is 2-3, and the preparation efficiency of the titanium alloy EBSD samples is further improved by arranging 2-3 electrolytic polishing units to realize batch preparation of the titanium alloy EBSD samples.
Example 1
The embodiment provides a novel preparation method of a titanium alloy EBSD sample, which comprises the steps of cutting, mechanically polishing, electropolishing, cleaning and corroding the titanium alloy sample and preserving the titanium alloy sample.
a. Titanium alloy sample cutting
In this example, a TA2 brand titanium alloy hot rolled plate is taken as an example, after the warp cutting, the size of a titanium alloy sample is 7mm multiplied by 6mm multiplied by 5mm (rolling direction multiplied by transverse multiplied by normal direction), and the detection surface is a rolling surface. After removing the stains on the surface of the titanium alloy sample, a polishing process can be performed.
b. Mechanical polishing
The polishing process uses a mechanical polishing machine for a continuously variable metallographic specimen fixed with 400-mesh sand paper to coarsely grind the rolled surface of the titanium alloy sample, the rotating speed can be controlled within the range of 400-900 r/min, water is introduced in the whole process of polishing, water is cooled in the whole process of polishing, and after coarsely grinding, 3000-mesh sand paper is used for manually grinding the surface of the titanium alloy sample to remove a surface oxide layer. In addition, in order to further improve the sample preparation efficiency, a mosaic method can be used, a plurality of titanium alloy samples are subjected to distinguishing and marking, are centrally mosaic and are polished once through a mechanical polishing machine.
c. Electrolytic polishing
100mL of electrolyte (3% perchloric acid ethanol solution by volume) is poured into the cup-shaped glass tank, the electrolyte submerges the 1/2 part of the volume of the cup-shaped graphite tank, the polished sample is placed into a cleaning tank of an ultrasonic cleaning unit, after ultrasonic cleaning is performed for 30 seconds, the first hollow screw is fixed in the first screw hole, then a titanium alloy sample is clamped by tweezers at the bottom end of the first hollow screw, and the titanium alloy sample is immersed into the electrode liquid. Starting the speed-adjustable magnetic stirring unit, controlling the rotating speed of the magnetic rotor to be 110r/min, properly adjusting the central position of the magnetic rotor, switching on a direct current power supply after the electrolyte rotates stably along with the magnetic rotor, setting the voltage of the direct current power supply to be 26V, setting the electrolytic current to be 360mA, keeping the electrolytic surface immersed in the electrolyte for 2mm in the electrolytic process, and setting the current of the direct current power supply to have certain change along with the surface size and the immersion depth of a sample without influencing the electrolytic effect, wherein the electrolytic duration is 30s, and placing the sample into an ultrasonic cleaning unit for cleaning after the electrolytic process is completed, so that the electrolytic process can be completed, and the high-quality detection titanium alloy sample is obtained.
d. Cleaning and etching
Immediately placing the titanium alloy sample into alcohol after the electrolytic polishing is finished, then placing the titanium alloy sample into ultrasonic cleaning equipment to clean for 12s, minimizing contact with air, and immersing the polished surface of the titanium alloy sample into HF (high frequency) and HNO (high frequency) with the ratio of 1% and HNO (high frequency) of 2% after the surface is stable 3 And (3) corroding the KROLL solution with the balance of water for 4s, and then placing the solution into alcohol for cleaning and drying to finish the cleaning and corrosion processes of the titanium alloy sample. The titanium alloy sample is subjected to structure and texture detection, as shown in fig. 3, the structure of the titanium alloy sample under the light mirror is clear, the EBSD detection grain boundary is clear, and the calibration is good.
e. Titanium alloy sample preservation
After the preparation of the titanium alloy sample is completed, the titanium alloy sample which cannot be immediately subjected to texture detection needs to be stored. The corroded titanium alloy sample has a stable surface, and can be stored by using a titanium alloy sample box and a self-sealing bag in short-term storage, so that surface grinding is avoided. If long-term storage is needed, the anti-oxidation adhesive tape can be stuck on the detection surface of the titanium alloy sample, and a drying agent can be added into the titanium alloy sample box for long-term storage.
Example 2
The embodiment provides a novel preparation method of a titanium alloy EBSD sample, which comprises the steps of cutting, mechanically polishing, electropolishing, cleaning and corroding the titanium alloy sample and preserving the titanium alloy sample.
a. Titanium alloy sample cutting
The invention is generally used for various brands of titanium alloy samples, in the embodiment, a TA2 brand titanium alloy hot rolled plate is taken as an example, after the titanium alloy samples are cut by a warp, the size of the titanium alloy samples is 7mm multiplied by 6mm multiplied by 5mm (rolling direction multiplied by transverse multiplied by normal direction), and the detection surface is a rolled surface. After removing the stains on the surface of the titanium alloy sample, a polishing process can be performed.
b. Mechanical polishing
The whole process is simplified in the polishing process, a mechanical polishing machine for a continuously variable metallographic specimen with 400-mesh sand paper fixed is used for carrying out rough polishing on the rolled surface of a titanium alloy sample, the rotating speed can be controlled at 750r/min, water is introduced in the whole polishing process, after the rough polishing, 3000-mesh sand paper is used for hand polishing the surface of the titanium alloy sample, the surface oxide layer is removed, and in order to further improve the sample preparation efficiency, a mosaic method can be used for carrying out distinguishing marking on a plurality of titanium alloy samples, and then the titanium alloy samples are centrally mosaic and polished once.
c. Electrolytic polishing
120mL of electrolyte (7.5% perchloric acid ethanol solution by volume) is poured into the cup-shaped glass tank, the electrolyte submerges the 1/2 part of the volume of the cup-shaped graphite tank, the polished sample is put into a cleaning tank of an ultrasonic cleaning unit, after the sample is cleaned by ultrasonic for 22 seconds, the first hollow screw rod is fixed in the first screw hole, then a titanium alloy sample is clamped by tweezers at the bottom end of the first hollow screw rod, and the titanium alloy sample is immersed in the electrode liquid. Starting the speed-adjustable magnetic stirring unit, controlling the rotating speed of the magnetic rotor to be 130r/min, properly adjusting the central position of the magnetic rotor, switching on a direct current power supply after the electrolyte rotates stably along with the magnetic rotor, setting the voltage of the direct current power supply to be 27V, setting the electrolytic current to be 650mA, keeping the electrolytic surface immersed in the electrolyte for 3mm in the electrolytic process, ensuring that the electrolytic effect is not affected, setting the electrolytic duration to be 55s, and placing the electrolyte into an ultrasonic cleaning unit for cleaning after the electrolytic process is completed, thereby obtaining a high-quality detection titanium alloy sample.
d. Cleaning and etching
Immediately placing the titanium alloy sample into alcohol after the electrolytic polishing is finished, then placing the titanium alloy sample into ultrasonic cleaning equipment to clean for 21s, minimizing contact with air, and immersing the polished surface of the titanium alloy sample into HF (hydrogen fluoride) with the proportion of 2% and HNO (hydrogen fluoride) with the proportion of 4% after the surface is stable 3 And (3) corroding the KROLL solution with the balance of water for 7s, and then placing the solution into alcohol for cleaning and drying to finish the cleaning and corrosion processes of the titanium alloy sample. And the structure and texture of the titanium alloy sample are detected, the structure of the titanium alloy sample under the optical lens is clear, the EBSD detection grain boundary is clear, and the calibration is good.
e. Titanium alloy sample preservation
After the preparation of the titanium alloy sample is completed, the titanium alloy sample which cannot be immediately subjected to texture detection needs to be stored. The corroded titanium alloy sample has a stable surface, and can be stored by using a titanium alloy sample box and a self-sealing bag in short-term storage, so that surface grinding is avoided. If long-term storage is needed, the anti-oxidation adhesive tape can be stuck on the detection surface of the titanium alloy sample, and a drying agent can be added into the titanium alloy sample box for long-term storage.
Example 3
The embodiment provides a novel preparation method of a titanium alloy EBSD sample, which adopts the preparation device, and the preparation process comprises the steps of cutting the titanium alloy sample, mechanically polishing, electropolishing, cleaning and corroding, and preserving the titanium alloy sample.
a. Titanium alloy sample cutting
In this example, the TA2 brand titanium alloy hot rolled sheet is taken as an example, the size of a titanium alloy sample after being cut by a warp is 7mm multiplied by 6mm multiplied by 5mm (rolling direction multiplied by transverse multiplied by normal direction), and the detection surface is a rolling surface. After removing the stains on the surface of the titanium alloy sample, a polishing process can be performed.
b. Mechanical polishing
The whole process is simplified in the polishing process, a mechanical polishing machine for a continuously variable metallographic specimen with 400-mesh sand paper fixed is used for carrying out rough polishing on the rolled surface of a titanium alloy sample, the rotating speed can be controlled to 900r/min, water is introduced in the whole polishing process, after the rough polishing, 3000-mesh sand paper is used for hand polishing the surface of the titanium alloy sample, the surface oxide layer is removed, and in order to further improve the sample preparation efficiency, a mosaic method can be used for carrying out distinguishing marking on a plurality of titanium alloy samples, and then the titanium alloy samples are centrally mosaic and polished once.
c. Electrolytic polishing
And (3) carrying out electrolytic polishing treatment on the polished surface, wherein the electrolyte is a perchloric acid ethanol solution with the volume fraction of 9.7%, the first hollow screw is fixed in the first screw hole, then a titanium alloy sample is clamped by tweezers at the bottom end of the first hollow screw and immersed in the electrolyte, the electrolytic process is carried out at room temperature, the electrolytic voltage is 25-30V, the electrolytic current is 790mA, the immersion depth of the titanium alloy sample is controlled to be 4mm, and the high-quality detection titanium alloy sample can be obtained after 69s of electrolysis.
155mL of electrolyte (9.5% perchloric acid ethanol solution by volume) is poured into the cup-shaped glass tank, the electrolyte submerges the 1/2 part of the volume of the cup-shaped graphite tank, the polished sample is put into a cleaning tank of an ultrasonic cleaning unit, after the sample is cleaned by ultrasonic for 29 seconds, the first hollow screw is fixed in the first screw hole, then a titanium alloy sample is clamped by tweezers at the bottom end of the first hollow screw, and the titanium alloy sample is immersed into the electrode liquid. Starting the speed-adjustable magnetic stirring unit, controlling the rotating speed of the magnetic rotor to be 190r/min, properly adjusting the central position of the magnetic rotor, switching on a direct current power supply after the electrolyte rotates stably along with the magnetic rotor, setting the voltage of the direct current power supply to be 30V, setting the electrolytic current to 790mA, keeping the electrolytic surface immersed in the electrolyte for 4mm in the electrolytic process, and setting the current of the direct current power supply to have certain change along with the surface size and the immersion depth of a sample, so that the electrolytic effect is not affected, setting the electrolytic duration to be 69s, and placing the sample into an ultrasonic cleaning unit for cleaning after the electrolytic process is completed, thereby completing the electrolytic process and obtaining the high-quality detection titanium alloy sample.
d. Cleaning and etching
Immediately placing the titanium alloy sample into alcohol after the electrolytic polishing is finished, then placing the titanium alloy sample into ultrasonic cleaning equipment to clean for 10s-30s, minimizing contact with air, and immersing the polished surface of the titanium alloy sample into HF (hydrogen fluoride) with the proportion of 3% and HNO (hydrogen fluoride) of 6% after the surface is stable 3 And (3) corroding the KROLL solution with the balance of water for 9s, and then placing the solution into alcohol for cleaning and drying to finish the cleaning and corrosion processes of the titanium alloy sample. And the structure and texture of the titanium alloy sample are detected, the structure of the titanium alloy sample under the optical lens is clear, the EBSD detection grain boundary is clear, and the calibration is good.
e. Titanium alloy sample preservation
After the preparation of the titanium alloy sample is completed, the titanium alloy sample which cannot be immediately subjected to texture detection needs to be stored. The corroded titanium alloy sample has a stable surface, and can be stored by using a titanium alloy sample box and a self-sealing bag in short-term storage, so that surface grinding is avoided. If long-term storage is needed, the anti-oxidation adhesive tape can be stuck on the detection surface of the titanium alloy sample, and a drying agent can be added into the titanium alloy sample box for long-term storage.
Example 4
The difference between the preparation device of the titanium alloy EBSD sample adopted in the embodiment and the titanium alloy sample and the preparation condition of the titanium alloy sample in the embodiment is that the preparation device of the titanium alloy EBSD sample adopted in the embodiment comprises a first hollow screw, a second hollow screw and a third hollow screw, wherein the three hollow screws are arranged in corresponding screw holes, the bottoms of the first hollow screw and the third hollow screw are correspondingly provided with a first clamping part and a third clamping part, the first clamping part and the third clamping part are used for clamping the titanium alloy sample, namely the embodiment simultaneously carries out electrolytic polishing treatment on the 3 titanium alloy samples, and the 3 titanium alloy EBSD samples with clear tissues are finally obtained after the electrolytic polishing treatment and cleaning and corrosion.
It is emphasized that the traditional mechanical polishing and sample preparation of a single titanium alloy sample needs 2 hours, the traditional mechanical polishing and electrolytic polishing combined one-time success rate is low, and the whole process of sample preparation of a single titanium alloy sample needs 30 minutes; compared with the prior art, the method can prepare the high-quality EBSD detection surface in a short time, has higher one-time success rate, and shortens the whole preparation flow of the titanium alloy sample to be within 5 minutes, wherein the electrolytic polishing process is completed within 1 minute; the invention obviously improves the preparation efficiency and success rate of the titanium alloy EBSD sample.
The titanium alloy sample is prepared by using a common polishing and electropolishing method, the surface has concave-convex relief, the surface has a certain degree of dark oxidation trace, in the detection process of the EBSD method, the surface unevenness and slight relief have a certain influence on the accuracy of a detection result, and the surface oxidation of the detected titanium alloy sample can influence the calibration rate of the titanium alloy sample. Compared with the prior art, the EBSD titanium alloy sample prepared by the method has high surface quality, strong adaptability, detectable equipment configured with high and low levels and high calibration rate of detection results; the universality is high, and the method is suitable for various brands and technical titanium alloy samples; the stability is good, and the method is suitable for batch detection of titanium alloy samples.
In conclusion, the preparation efficiency and quality of the titanium alloy Electron Back Scattering Diffraction (EBSD) detection titanium alloy sample are improved, the preparation flow of the titanium alloy EBSD sample is simplified, the detection difficulty of the titanium alloy EBSD sample is effectively reduced, and the application of the electron back scattering diffraction technology in the titanium alloy anisotropic phenomenon research is finally promoted.
The present invention is not limited to the above-mentioned embodiments, and any changes or substitutions that can be easily understood by those skilled in the art within the technical scope of the present invention are intended to be included in the scope of the present invention.
Claims (9)
1. The preparation method of the titanium alloy EBSD sample is characterized by comprising the following steps of:
step 1, cutting a sample;
performing linear cutting on the sample tissue;
step 2, mechanically polishing;
performing machine polishing on the cut sample by using 400-mesh sand paper, skipping other-mesh sand paper, and directly performing hand polishing on the sample by using 3000-mesh sand paper to remove a surface oxide layer so as to obtain a sample polished surface with fine and uniform scratches;
the mechanical polishing comprises the steps of mechanically polishing a cut sample by adopting a polishing machine, wherein the rotating speed of the polishing machine is 400-900 r/min, and water is continuously introduced in the mechanical polishing process;
step 3, electrolytic polishing;
electrolytic polishing is carried out by using perchloric acid ethanol solution as electrolyte;
step 4, cleaning and corroding;
and after the sample is subjected to electrolytic polishing, cleaning by adopting a cleaning agent, after cleaning, carrying out corrosion treatment on the surface by using KROLL solution, and after corrosion, putting the sample into alcohol for cleaning and drying to obtain the titanium alloy EBSD sample.
2. The method for preparing a titanium alloy EBSD sample according to claim 1, wherein in said step 1, the size of the detection surface of the titanium alloy EBSD sample is controlled within the range of 10mm x 10 mm.
3. The method for preparing a titanium alloy EBSD sample according to claim 1, wherein in said step 3, the volume fraction of the perchloric acid ethanol solution is 2-10%.
4. The method for preparing a titanium alloy EBSD sample according to claim 1, wherein in the step 4, the cleaning agent is alcohol, and the sample is immediately put into alcohol after the electrolytic polishing, and then is put into an ultrasonic cleaning device for cleaning for 10s-30s.
5. The method for preparing a titanium alloy EBSD sample according to claim 4, wherein in said step 4, the cleaning frequency is 25-50kHz.
6. The method for preparing a titanium alloy EBSD sample according to claim 1, wherein in said step 3, the electrolysis process is performed at room temperature, the electrolysis voltage is 25V-30V, and the electrolysis current is 350mA-800mA.
7. The method for preparing a titanium alloy EBSD sample according to claim 4, wherein in said step 3, the immersion depth of the sample is controlled within the range of 2mm-4mm, and the electrolysis time is 30s-70s.
8. The method for preparing a titanium alloy EBSD sample according to claim 4, wherein in said step 4, the mass ratio of said KROLL solution comprises: 1-3% HF,2-6% HNO 3 The balance being water.
9. The method for producing a titanium alloy EBSD sample according to any one of claims 1 to 8, characterized in that in said step 4, the etching time of said KROLL solution is 4s-10s.
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