A device and method suitable for multi-type alloy ebsd electrolytic polishing

Abstract

The application discloses a device and method suitable for multi-type alloy EBSD electrolytic polishing, which comprises a magnetic stirrer, a cup-shaped container and a magnetic rotor, a spiral groove is fixedly arranged on the inner wall of the cup-shaped container, a sample placing plate is connected with the opening at the top of the cup-shaped container through buckling, a sample placing groove is formed in one side of the top surface of the sample placing plate, an electrolytic sample is placed on the top surface of the sample placing plate and located directly above the sample placing groove, the magnetic rotor drives the electrolyte to ascend along the spiral groove and enter the sample placing groove, a cathode plate is fixedly arranged on the other side of the top surface of the sample placing plate, and the surface of the electrolytic sample is connected with an anode plate; and a temperature adjusting device is arranged outside the cup-shaped container. The whole smooth surface does not need to be immersed in the electrolyte, the independent selection of the electrolysis area is realized, the electrolyte flow beam is continuously rotated to strip the sample surface, the electrolysis area is reduced, thereby the metal material and the chemical reagent are saved, and the success rate of the electrolytic polishing is improved.

Description

Technical Field

[0001] This invention relates to the field of electrochemical machining technology, and in particular to an apparatus and method suitable for EBSD electrochemical polishing of various types of alloys. Background Technology

[0002] Mechanical polishing is the most common method, with a wide range of applications and high polishing efficiency, but it easily causes stress and mechanical damage to the sample surface. Electrolytic polishing requires the selection of different polishing solutions depending on the material. Although commercially available electrolytic polishing solutions exist, they are relatively expensive. For some multiphase alloys, electrolytic polishing is more difficult due to the different electrolysis rates of different phases. As disclosed in Chinese invention patents CN114088497A, CN111551573A, and CN114113176A, the current electrolytic methods are similar, with the general steps as follows: 1. Electrolytic samples are obtained using wire cutting, but strict dimensional requirements apply. The thickness must be 0.5-1 mm, or the sample size must be strictly controlled within 10×10 mm, 7 mm×7 mm, or 10 mm×5 mm×3 mm, requiring high precision. 2. Perform mechanical grinding and polishing. The grinding process is complex and requires grinding with sandpaper of 400 grit, 600 grit, 800 grit, 1500 grit, and 2000 grit in sequence. The grit of the sandpaper and the grinding order must not be changed or reduced. 3. Immerse the obtained smooth surface entirely in the electrolyte, the immersion area is the electrolysis area, and then electrolyze it while using liquid nitrogen for cooling. 4. After electrolysis, remove the sample, ultrasonically clean the surface, dry it, and store it.

[0003] However, the above process has many shortcomings: 1. During EBSD electropolishing testing, the actual testing area is only required to be 0.2 × 0.2 mm (EBSD on-machine testing costs approximately 500 RMB / hour; testing a 0.1 × 0.1 mm sample takes about 1 hour, while testing a 0.2 × 0.2 mm sample takes 2-3 hours. The larger the testing area, the higher the cost, hence the need to control the area size). If the electrolytic area of ​​the electrolytic sample (such as a titanium alloy electrolytic sample) is too large, quality control becomes difficult; if the electrolytic area is too small, microstructure observation is hindered. Therefore, existing electrolytic methods all have varying degrees of size requirements. 2. The electrolytic surface needs to undergo a strict polishing process, requiring polishing with 400-mesh, 600-mesh, 800-mesh, 1500-mesh, and 2000-mesh sandpaper, which undoubtedly increases the time cost for researchers. 3. Existing electrolysis methods all involve immersing the entire smooth surface in the electrolyte, with the immersed area being the electrolysis area. This makes it impossible to select the electrolysis area according to testing requirements. Furthermore, large areas of electrolyte have poor quality and waste metal materials and chemical reagents, increasing electrolysis costs.

[0004] Therefore, in traditional electropolishing methods, the sample needs to be immersed in the electrolyte and an electrolysis method with face-to-face contact is used. That is, the surface of the sample should be parallel to the cathode and the distance between them should be kept constant. The sample size should not be too large, and localized spot polishing cannot be achieved in the electrolysis area. Traditional electropolishing methods are mostly carried out in non-constant temperature, static electrolyte environments, which are prone to pitting corrosion, surface blackening, uneven polishing and many other problems. Ion thinning is applicable to most materials. Although the polishing effect is better, the cost is high (up to 1500 yuan / sample) and the processing efficiency is also low. Summary of the Invention

[0005] The technical problem to be solved by this invention is: In view of the shortcomings of the existing technology, this invention proposes an apparatus and method for EBSD electropolishing of various types of alloys. Based on fully considering the existing electrolysis methods and the requirements of the detection area, it adopts a sample placement groove set on the sample plate. The electropolishing area is determined by the sample placement groove, thereby converting the requirement for sample size into the requirement for the sample placement groove. It is not necessary to immerse the entire smooth surface in the electrolyte. The electrolyte jet is formed by continuous rotating spiral ascent. After being energized, the electrolyte jet reacts immediately upon contact with the sample to etch the sample surface, which can automatically remove scratches and irregular and uneven areas on the surface.

[0006] To solve the above-mentioned technical problems, the present invention adopts the following technical solution: An apparatus suitable for EBSD electropolishing of various alloys includes a magnetic stirrer, a cup-shaped container placed on the top surface of the magnetic stirrer, and a magnetic rotor rotatably disposed at the bottom of the inner side of the cup-shaped container. The magnetic stirrer can drive the magnetic rotor to rotate unidirectionally to agitate the electrolyte in the cup-shaped container. A spiral groove is fixedly provided on the inner wall of the cup-shaped container. A sample plate made of insulating material is fastened to the top opening of the cup-shaped container. A sample groove communicating with the inside of the cup-shaped container is opened on one side of the top surface of the sample plate. An electrolytic sample is placed on the top surface of the sample plate, located directly above the sample groove. The rotating electrolyte can rise along the spiral groove and enter the sample groove, contacting the bottom surface of the electrolytic sample located in the electrolytic area within the sample groove. A cathode plate is fixedly installed on the other side of the top surface of the sample plate. The bottom end of the cathode plate is located in the electrolyte inside the cup-shaped container, and the top end is located above the top surface of the sample plate. An anode plate is connected to the surface of the electrolytic sample. The cup-shaped container is fitted with a temperature regulating device on its outer side.

[0007] Furthermore, the horizontal cross-sectional shape of the magnetic rotor is a pentagonal star, and a rotating shaft is rotatably connected to its central axis via a bearing. The bottom end of the rotating shaft is fixedly connected to the center of the inner bottom surface of the cup-shaped container.

[0008] Furthermore, the bottom surface of the sample plate is integrally provided with a hydrophobic structure, which is composed of multiple coaxially arranged annular hydrophobic strips. The vertical cross-sectional shape of the annular hydrophobic strips is a triangle with the same direction and facing the axis of the sample groove.

[0009] Furthermore, a sealing gasket is fixedly provided on the top surface of the sample plate.

[0010] Furthermore, the top surface of the sample plate is provided with a sample clamping mechanism, which includes a hinge seat and a locking seat respectively fixed to the top surface of the sample plate. A clamping plate is hinged to the hinge seat, and the end of the clamping plate away from the hinge seat is detachably fastened to the top surface of the locking seat. Several set screws are threadedly connected to the top surface of the clamping plate, and the bottom end of the set screws presses against the top surface of the electrolytic sample.

[0011] Furthermore, the top surface of the hinge seat is provided with connecting grooves on both sides, and the bottom end of the pressure plate is integrally provided with sliding hinge shafts on both sides. The sliding hinge shafts are movably located in the connecting grooves and can slide along the connecting grooves. The end of the pressure plate away from the hinge seat is integrally provided with locking shafts on both sides. The top surface of the locking seat is provided with at least one L-shaped locking slot. When the pressure plate is in a horizontal state, the locking shaft is locked and connected in one of the locking slots.

[0012] Furthermore, the connecting groove is "┐" shaped, and when the sliding hinge shaft is located in the vertical section of the connecting groove, the clamping plate can be vertically inserted into the hinge seat.

[0013] Furthermore, the temperature control device includes a temperature controller, a refrigerant circulation supply device, an insulation layer sleeved on the outside of the cup-shaped container, an insulation cover snapped between the top of the cup-shaped container and the insulation layer, and at least one temperature sensor fixedly installed on the top of the inner wall of the cup-shaped container. The top surface of the insulation cover is integrally provided with an inlet and a outlet that communicate with the interior of the insulation layer on both sides. The feeding end of the refrigerant circulation supply device is connected to the inlet, and the return end is connected to the outlet. The temperature sensor is electrically connected to the temperature controller, and the temperature controller is electrically connected to the power drive mechanism of the refrigerant circulation supply device.

[0014] Furthermore, the top surface of the heat-insulating cover is integrally provided with an annular discharge cavity, and the bottom surface is integrally provided with an annular feed cavity; The discharge port is integrally disposed on the top surface of the annular discharge cavity, and at least one discharge collection port is integrally disposed on the bottom surface of the annular discharge cavity. The bottom end of the discharge collection port passes through the annular feed cavity and communicates with the interior of the insulation layer. The feed inlet is integrally and continuously disposed on the top surface of the annular feed cavity, and the top end of the feed inlet penetrates the annular discharge cavity and protrudes above the top surface of the annular discharge cavity. At least one feed pipe is integrally and continuously connected to the bottom surface of the annular feed cavity. The bottom end of the feed pipe is located at the inner bottom end of the insulation layer, and several material dispersing holes are opened on the side wall of the feed pipe.

[0015] Furthermore, the vertical cross-sectional shape of the outer surface of the sidewall of the cup-shaped container is wavy.

[0016] A method for EBSD electropolishing of multiple alloy types is also provided, applied to the aforementioned apparatus for EBSD electropolishing of multiple alloy types, comprising the following steps: S1. Prepare the appropriate electrolyte according to the specific metal material type of the electrolytic sample; S2. Pour the prepared electrolyte into a cup-shaped container placed on a magnetic stirrer. The volume of the electrolyte should be 85% to 95% of the volume of the cup-shaped container. S3. Fix the electrolytic sample on the sample plate and make the electrolytic area of ​​the electrolytic sample coincide with the position of the sample tank. Fix the cathode plate on the sample plate and the anode plate on the surface of the electrolytic sample. Then fix the sample plate on the top of the cup-shaped container. S4. Start the magnetic stirrer to drive the magnetic rotor to rotate until the magnetic rotor reaches the preset speed and stabilizes. The electrolyte rotates at a uniform speed to form a vortex and rises continuously along the spiral groove. S5. Start the temperature control device to keep the electrolyte temperature in the cup-shaped container at the preset electrolysis temperature; S6. Based on the type of metal material and the corresponding electrolyte of the electrolytic sample, set the corresponding stable output voltage through the voltage stabilizing output device and apply it to the anode plate and cathode plate respectively. S7. After being energized, the electrolyte circulates and rises and enters the sample tank, contacting the surface of the electrolysis area of ​​the electrolysis sample. The electrolyte flows and impacts the metal surface of the electrolysis area and electrolytically erodes it. After a preset time, the electrolytic polishing of the surface of the electrolysis sample is completed. S8. Turn off the voltage regulator, magnetic stirrer and temperature control device in sequence to stop the electrolytic polishing operation and remove the electrolytic sample.

[0017] Compared with the prior art, the beneficial effects of the present invention are as follows: 1. This invention, based on a full consideration of existing electrolysis methods and testing area requirements, sets a sample plate on the top of a cup-shaped container and a sample groove on the sample plate. After the electrolysis sample is placed on the sample plate, the electrolysis polishing area is determined by the sample groove. The traditional requirement for sample size is transformed into a requirement for the sample groove. The sample groove of the corresponding size or shape is designed according to the testing requirements. Only the surface of the sample placed in the sample groove needs to be smoothed, and there is no need to strictly require the sample size. 2. This invention, by employing a sample placement plate, achieves separation of the electrolyte and the sample throughout the electrolysis process. This breaks away from the traditional method of immersing the entire smooth surface of the sample in the electrolyte. By autonomously selecting and determining the electrolysis area, an electrolysis tank of corresponding size and shape is designed. The area of ​​the sample to be electrolyzed is placed in the sample placement tank; the shape of the tank then determines the electrolysis shape. Non-electrolysis areas located elsewhere on the sample placement plate will not be electrolyzed. According to testing requirements, the fixed position of the electrolyzed sample can be adjusted, placing different electrolysis areas in the sample placement tank for separate electrolytic polishing. This achieves autonomous selection of the electrolysis area, reducing the electrolysis area, thus saving metal materials and chemical reagents, and improving the success rate of electrolysis. 3. This invention uses a magnetic rotor to agitate the electrolyte. Driven by a magnetic stirrer, the magnetic rotor rotates rapidly, causing the electrolyte to rise along the spiral grooves on the inner wall of the container until it reaches the sample placement tank. Since the electrolyte maintains a constant rotation speed, an electrolyte jet with a certain impact force can be formed at the top outlet of the spiral groove. The electrolyte jet rushes into the sample placement tank and contacts the surface of the electrolytic sample. Once the electrolyte is energized, an electrolytic reaction immediately occurs in the sample placement tank. The high-speed rotating electrolyte jet erodes the sample surface. Therefore, the surface treatment of the electrolytic sample does not require the traditional cumbersome mechanical polishing method. It only needs to be polished on 1200-mesh water-abrasive paper before electrolytic polishing. This can automatically remove scratches and irregular, uneven areas on the surface, with an erosion thickness of about 1µm. 4. This invention employs a cylindrical pentagonal magnetic rotor with a rotating shaft fixed within a cup-shaped container. This effectively prevents the magnetic rotor from deviating from its central position during the experiment, thus avoiding poor stirring performance. Compared to existing cylindrical magnetic rotors, the pentagonal magnetic rotor not only increases the rotation frequency but also improves rotational stability. This accelerates the electrolyte flow rate, allowing the electrolyte temperature and metal ions to mix rapidly and evenly within a short time. This prevents metal ion aggregation and localized temperature increases, thereby improving the electrolysis success rate. 5. In this invention, since the electrolyte in the container is not full and there is still a certain distance between it and the sample plate, by setting a spiral groove on the inner wall of the container, the electrolyte solution starts to rotate under the action of the magnetic rotor and can quickly rise along the spiral groove to the sample plate and contact the sample to form a complete passage, which can accelerate the rising speed of the electrolyte and shorten the electropolishing time. 6. In this invention, the electrolyte is not fully filled in the cup-shaped container, and the high-speed rotating electrolyte jet contacts the bottom surface of the sample plate with a small flow rate and a small area, which can minimize the corrosive effect of acidic electrolyte on the sample plate and sample tank. By setting an insulating hydrophobic structure on the bottom surface of the sample plate, the bottom surface of the sample plate has a biomimetic bird feather waterproof effect, which can minimize the contact time between the electrolyte and the bottom surface of the sample plate and the amount of electrolyte residue on the bottom surface of the sample plate, effectively preventing the electrolyte from sticking to the sample plate and providing a good protection for the sample plate. In addition, the outermost part of the hydrophobic structure is enlarged to fit tightly against the inner wall of the top of the cup-shaped container, which can prevent the electrolyte from flowing out and prevent the outer wall of the cup-shaped container from being corroded by acidic electrolyte. Attached Figure Description

[0018] Figure 1 This is a three-dimensional structural diagram of the electrolytic polishing apparatus of the present invention; Figure 2 This is a cross-sectional view of the electropolishing apparatus of the present invention in the state of removing the magnetic stirrer. Figure 3 This is a three-dimensional structural diagram of the cup-shaped container; Figure 4 This is a cross-sectional view of the cup-shaped container. Figure 5 This is a three-dimensional structural diagram showing the connection state between the magnetic rotor and the shaft; Figure 6 This is a cross-sectional structural diagram showing the connection between the magnetic rotor and the shaft; Figure 7 A three-dimensional structural diagram of the magnetic rotor in its assembled state inside a cup-shaped container; Figure 8 This is one of the three-dimensional structural schematic diagrams of the sample plate; Figure 9 This is the second three-dimensional structural schematic diagram of the sample plate. Figure 10 This is a cross-sectional view of the template. Figure 11 A schematic diagram of a sample placement groove with different cross-sectional shapes for the sample placement plate; Figure 12 This is a three-dimensional structural diagram of the cathode plate; Figure 13This is one of the three-dimensional structural schematic diagrams of the sample clamping mechanism; Figure 14 This is the second three-dimensional structural schematic diagram of the sample clamping mechanism; Figure 15 This is a three-dimensional structural diagram of the hinge seat and the locking seat; Figure 16 This is a three-dimensional structural diagram of the clamping plate; Figure 17 A three-dimensional structural diagram showing the clamping plate in a vertical position; Figure 18 This is one of the three-dimensional structural schematic diagrams of the heat-insulating cover and its components; Figure 19 This is the second three-dimensional structural schematic diagram of the heat-insulating cover and its components; Figure 20 This is a cross-sectional view of the heat insulation cover and its components; Figure 21 A photograph of a titanium alloy sample processed using the electropolishing method of the present invention. Figure 22 The results were obtained by observing the titanium alloy sample under a metallographic microscope. Figure 23 The results are the calibration of the titanium alloy sample under EBSD electron microscopy.

[0019] In the diagram: 1 Magnetic stirrer, 2 Cup-shaped container, 201 Spiral groove, 3 Magnetic rotor, 301 Rotating shaft, 302 Bearing end cover, 4 Sample plate, 401 Sample groove, 402 Hydrophobic structure, 5 Cathode plate, 6 Anode plate, 7 Temperature control device, 701 Insulation layer, 702 Insulation cover, 703 Feed inlet, 704 Discharge outlet, 705 Annular discharge chamber, 706 Annular feed chamber, 707 Discharge collection port, 708 Feed pipe, 709 Discharge hole, 710 Temperature sensor, 8 Sealing gasket, 9 Sample clamping mechanism, 901 Hinge seat, 9011 Connecting slide, 902 Locking seat, 9021 Locking slot, 903 Clamping plate, 9031 Sliding hinge shaft, 9032 Locking shaft, 904 Set screw. Detailed Implementation

[0020] The preferred embodiments of the present invention will now be described in detail with reference to the accompanying drawings, so that the advantages and features of the present invention can be more easily understood by those skilled in the art, thereby providing a clearer and more explicit definition of the scope of protection of the present invention.

[0021] Please see Figures 1 to 20An apparatus suitable for EBSD electropolishing of various alloy types includes a magnetic stirrer 1, a cup-shaped container 2 placed on the top surface of the magnetic stirrer 1, and a magnetic rotor 3 rotatably disposed inside the bottom of the cup-shaped container 2. The electrolyte is placed inside the cup-shaped container 2. When the magnetic stirrer 1 is energized, it generates a magnetic field, which drives the magnetic rotor 3 to rotate unidirectionally, thus agitating the electrolyte inside the cup-shaped container 2. This accelerates the free and uniform diffusion of various ions in the electrolyte, increasing the electrolyte content. To prevent the cup-shaped container 2 from reacting chemically with the electrolyte or participating in the electrolysis process, in this embodiment, the cup-shaped container 2 is a cylindrical glass cup. Figure 3 and Figure 4 As shown, the inner wall of the cup-shaped container 2. A spiral groove 201 is fixedly provided on the inner wall of the cup-shaped container 2, so that the rotating electrolyte can rise continuously along the spiral groove 201, thereby forming a small flow of electrolyte with a certain impact force.

[0022] like Figure 5 and Figure 6 As shown, in this embodiment, the horizontal cross-sectional shape of the magnetic rotor 3 is a pentagonal star. A rotating shaft 301 is rotatably connected to its central axis via a bearing. The bottom end of the rotating shaft 301 is fixedly connected (e.g., glued) to the center of the inner bottom surface of the cup-shaped container 2. Figure 7 As shown, bearing end caps located outside the bearings are fixedly inserted into the upper and lower end faces of the magnetic rotor 3 to achieve the installation and positioning of the bearings within the magnetic rotor 3. In this device, the rotation of the magnetic rotor 3 is required to create a vortex in the cup-shaped container 2, allowing the edge portion of the electrolyte to continuously rise along the spiral groove 201. Therefore, the pentagonal rotor structure, compared to a conventional cylindrical magnetic rotor, can improve the rotation frequency and stability of the magnetic rotor 3, resulting in better agitation and outward pushing of the electrolyte. Simultaneously, since the magnetic rotor 3 is positioned via the rotating shaft 301 and rotated through two bearings, positional shifts or axial tilts during rotation are effectively prevented, improving the smoothness of rotation and ensuring a uniform and stable stirring effect.

[0023] A sample placement plate 4, made of insulating material (such as rigid plastic), is fastened to the top opening of the cup-shaped container 2 for placing the electrolytic sample. Figures 8 to 10 As shown, the template 4 is a disc structure with the same outer diameter as the cup-shaped container 2. A boss is integrally formed on the bottom surface of the template 4, and the diameter of the boss matches the inner wall diameter of the cup-shaped container 2, allowing the boss to be tightly inserted into the top opening of the cup-shaped container 2, thus achieving a snap-fit ​​connection between the template 4 and the cup-shaped container 2. One side of the top surface of the template 4 (e.g., Figure 8 and Figure 9As shown on the left side, a sample placement groove 401 is provided, which penetrates the interior of the cup-shaped container 2. An electrolytic sample is placed on the top surface of the sample placement plate 4, directly above the sample placement groove 401. This allows for the separation of the electrolyte and the electrolytic sample throughout the electrolysis process, breaking away from the traditional electrolytic polishing process that requires immersing the entire electrolytic surface in the electrolyte. Only the area on the bottom surface of the electrolytic sample located within the sample placement groove 401 can contact the electrolyte in the cup-shaped container 2 for electrolytic polishing; the remaining areas will not undergo electrolytic polishing. Therefore, the areas of the sample requiring electrolysis can be placed within the sample placement groove 401, whose shape corresponds to the shape of the electrolytic area. Non-electrolytic areas of the sample located elsewhere on the sample placement plate 401 will not be electrolyzed. Furthermore, the sample can be moved and its position adjusted according to testing needs, allowing different deformed areas to be placed within the sample placement groove 401, thus enabling the autonomous selection of the electrolytic area. During electropolishing, the rotating electrolyte can rise along the spiral groove 201 and form a small flow of electrolyte with a certain impact force. The electrolyte flow enters the sample tank 401 and comes into contact with the electro-electrolysis area to complete the electrolysis process. The electrolyzed liquid and the ions etched from the surface of the electrolysis area fall back into the electrolyte in the cup-shaped container 2.

[0024] Preferably, since the requirements for EBSD detection depend on the pretreatment process, the sample placement slot 401 can be designed into polygons or circles of different shapes or sizes to meet the different needs in the actual experimental process, such as... Figure 11 As shown in the figure, the cross-sectional shape of the sample placement tank 401 of type (a) is circular. This shape of the electrolysis region can better reflect the size and phase distribution of the electrolytic sample grains at the center and edge. The cross-section of the sample placement tank 401 of type (b) is rectangular, with one side of the rectangle perpendicular to the direction of the line connecting the two electrolysis electrodes. The cross-section of the sample placement tank of type (c) is rhomboid, with one diagonal of the rhombus aligned with the direction of the line connecting the two electrolysis electrodes. The rectangular and rhomboid electrolysis regions can well reflect the variation trend of the electrolytic sample in the RD direction, that is, the entire variation from the core of the sample plate 4 to the edge. An excessively large electrolysis sample area makes it difficult to control the electrolyte amount, which not only wastes metal materials and chemical reagents but also increases the difficulty of electrolysis sample placement. However, by adopting the autonomous selection of the electrolysis region, the electrolysis area is reduced, metal materials and chemical reagents are saved, and the success rate of electrolysis is improved. Therefore, the shape and size of the sample tray 401 can be designed according to the detection requirements of various different detection objects, so as to solve some related problems with special requirements for the detection of the microstructure of metal materials.

[0025] like Figure 9 and Figure 10As shown, a hydrophobic structure 402 is integrally provided on the bottom surface of the sample plate 4. The hydrophobic structure 402 is composed of multiple layers of annular hydrophobic strips arranged coaxially. The vertical cross-sectional shape of the annular hydrophobic strips is a triangle with the same direction and facing the axis of the sample groove 401. Due to the inherent properties of the electrolytic sample material (such as titanium alloy), perchloric acid needs to be added to the electrolyte, making the entire electrolyte highly acidic. This would cause the sample plate 4 to adhere to the electrolyte for an extended period, significantly reducing its lifespan. Therefore, this device incorporates an insulating hydrophobic structure 402 (mimicking the waterproof effect of bird feathers) on the bottom surface of the sample plate 4 to minimize the contact time between the electrolyte and the bottom surface of the sample plate 4, and to reduce the amount of electrolyte residue on the bottom surface of the sample plate 4. This effectively prevents the electrolyte from adhering to the sample plate 4, providing excellent protection. Furthermore, the outermost layer of the sample plate 4 is enlarged to ensure a tight fit with the inner top wall of the cup-shaped container 2, preventing electrolyte outflow and avoiding corrosion of the outer wall of the cup-shaped container 2 by the acidic electrolyte. Furthermore, a sealing gasket 8 is fixedly provided on the top surface of the sample plate 4, which can effectively enhance the sealing effect on the outer side of the top edge of the sample groove 401, and prevent the electrolyte from overflowing from the top edge of the sample groove 401 and contacting the top surface of the sample plate 4 or the non-electrolytic area of ​​the electrolytic sample, so that the electrolytic area of ​​the electrolytic sample is reliably limited to the area covered by the sample groove 401.

[0026] A cathode plate 5 is fixedly installed on the other side of the top surface of the sample plate 4. The bottom end of the cathode plate 5 is located in the electrolyte inside the cup-shaped container 2, and the top end is located above the top surface of the sample plate 4. Figure 12 As shown, in this invention, the cathode plate 5 includes a lower arc-shaped plate and a stud fixedly connected to the top of the arc-shaped plate. The arc-shaped plate is made of lead sheet material. Lead sheet material has strong corrosion resistance, is not easily reacted with the electrolyte, has good conductivity, and is soft and easy to process. In this device, during the electrolytic polishing process, the electrolyte in the cup-shaped container 2 is not fully filled, and when the electrolyte forms a vortex, a recessed hollow area is formed at the center of its top surface. Therefore, the bottom end of the arc-shaped plate is suspended above the top surface of the magnetic rotor 3, which will not cause motion interference to the rotation of the magnetic rotor 3, and can always keep a portion of it in the electrolyte. The bottom surface of the sample plate 4 is placed on one side (e.g., Figure 9 and Figure 10The right side (shown in the figure) has an arc-shaped groove that matches the arc-shaped cross-section of the arc plate. A cylindrical through-hole is connected to the top of the arc-shaped groove. The top of the arc plate is fitted into the arc-shaped groove, and its outer surface is in close contact with the inner wall of the arc-shaped groove to prevent electrolyte from overflowing from the arc-shaped groove onto the top surface of the sample plate 4. A smooth section is left at the bottom of the stud, and the outer diameter of the smooth section matches the diameter of the cylindrical through-hole, allowing the top of the stud to be inserted vertically upwards into the cylindrical through-hole from the bottom of the sample plate 4. A first nut is threaded onto the stud, and the bottom surface of the first connecting nut is in contact with the top surface of the sealing gasket 8, thereby fixing the cathode plate 5 onto the sample plate 4. A wiring hole is provided at the top of the stud for connecting the cathode output power line of the voltage stabilizing output device (not shown in the figure). Second nuts are provided above and below the wiring hole for clamping and fixing the power line connector.

[0027] An anode plate 6 is connected to the surface of the electrolytic sample. The anode plate 6 is used to connect the anode output power line of the voltage stabilizing output device (not shown in the figure). After the anode plate 6 comes into contact with the electrolytic sample, when the electrolyte flow connected to the cathode plate 5 impacts the surface of the electrolytic area of ​​the electrolytic sample, a connected circuit is formed between the anode plate 6 and the cathode plate 5, so that the electrolyte and the electrolytic sample undergo an electrolytic reaction, thereby eroding the surface material of the electrolytic area of ​​the electrolytic sample. It can automatically remove scratches and irregular and uneven areas on the sample surface, and the erosion thickness is about 1µm.

[0028] To facilitate the placement and positioning of the electrolytic sample on the top surface of the sample plate 4, and the connection between the anode plate 6 and the surface of the electrolytic sample 6, a sample clamping mechanism 9 is provided on the top surface of the sample plate 4. For example... Figure 13 and Figure 14 As shown, the sample clamping mechanism 9 includes a hinge seat 901 and a locking seat 902 respectively fixed to the top surface of the sample plate 4. A clamping plate 903 is hinged to the hinge seat 901. The end of the clamping plate 903 away from the hinge seat 901 is detachably fastened to the top surface of the locking seat 902. Several threads (such as...) are connected to the top surface of the clamping plate 903. Figure 13 The three set screws 904 shown have their bottom ends pressing against the top surface of the electrolytic sample. Specifically, as... Figure 15 and Figure 16 As shown, the top surface of the hinge seat 901 is provided with connecting grooves 9011 on both sides, and the bottom end of the pressure plate 903 is integrally provided with sliding hinge shafts 9031 on both sides. The sliding hinge shafts 9031 are movably located within the connecting grooves 9011 and can slide along the connecting grooves 9011. The end of the pressure plate 903 away from the hinge seat 901 is integrally provided with locking shafts 9032 on both sides. The top surface of the locking seat 902 has at least one (e.g., Figure 15 As shown in the diagram, when the pressing plate 903 is in a horizontal state, the locking shaft 9032 is locked and connected to one of the locking slots 9021.

[0029] When the electrolytic sample is placed on the top surface of the sample plate 4 and its position is adjusted so that the electrolytic area on its bottom surface coincides with the sample groove 401, the clamping plate 903 is pulled, causing the hinge shaft 9031 to slide horizontally within the connecting groove 9011. When the set screw 904 is in an appropriate clamping position on the top surface of the electrolytic sample, the locking shaft 9032 slides into the locking groove 9021 from the top opening. At this time, the clamping plate 903 is in a horizontal state. Then, the clamping plate 903 is slid horizontally towards the hinge seat 901, causing the locking shaft 9032 to slide into the horizontal section of the locking groove 9021, thus completing the vertical positioning of the clamping plate 903. Next, the set screws 904 are tightened one by one, so that the bottom end of the set screw 904 is pressed against different positions on the top surface of the electrolytic sample, thereby pressing and fixing the electrolytic sample on the sample plate 4. A relatively long screw is threaded onto the outer end of the clamping plate 903. The anode plate 6 is fixedly connected to the bottom end of the screw. By rotating the screw, the anode plate 6 can be brought into contact with or separated from the top surface of the electrolytic sample. When the anode plate 6 is in contact with the top surface of the electrolytic sample, the electrolytic sample can also be clamped. By adjusting the connection position of the set screw 904 on the clamping plate 903, the clamping and fixing of electrolytic samples of different heights or with non-planar top surfaces on the sample placement plate 4 can be achieved, and the position adjustment of the electrolytic sample is also convenient. Preferably, the connecting groove 9011 is "┐" shaped. When the sliding hinge shaft 9031 is located in the vertical section of the connecting groove 9011, the clamping plate 903 can be vertically inserted into the hinge seat 901, such as... Figure 17 As shown. In this way, after the electrolytic polishing of the electrolytic sample is completed, the clamping plate 903 and the anode plate 6 on it can be moved away from the locking position and remain in the same position, so as to complete the loading, unloading or position adjustment of the electrolytic sample.

[0030] Because the electrolyte contains perchloric acid, it generates heat during the etching process on the metal surface. If the electrolyte temperature becomes too high, the sample surface will blacken and pit, leading to electropolishing failure. Therefore, a temperature control device 7 is installed on the outside of the cup-shaped container 2 to maintain the electrolyte temperature at 0°C. The temperature control device 7 includes a temperature controller, a cold medium circulation supply device, an insulation layer 701 fitted on the outside of the cup-shaped container 2, an insulation cover 702 snapped between the top of the cup-shaped container 2 and the insulation layer 701, and at least one temperature sensor 710 fixedly installed on the top of the inner wall of the cup-shaped container 2. The insulation layer 701 is a cylindrical cup-shaped structure coaxially arranged on the outside of the cup-shaped container 2, and the insulation cover 702 is an annular cover structure. Both the insulation layer 701 and the insulation cover 702 are made of hydrogel material. A general-purpose temperature control system controller can be used for the temperature controller, and a commonly used liquid nitrogen cooling device is used for the cold medium circulation supply device. The liquid nitrogen cooling device continuously injects cryogenic liquid nitrogen into the cavity between the insulation layer 701 and the cup-shaped container 2 to absorb the heat generated by the electrolysis reaction and maintain the electrolyte temperature at 0°C. The temperature sensor 710 is electrically connected to the temperature controller, and the temperature controller is electrically connected to the power drive mechanism of the cold medium circulation supply device. The temperature sensor 710 monitors the electrolyte temperature in real time and feeds the detection result back to the temperature controller in real time. The temperature controller adjusts the liquid nitrogen supply flow rate of the liquid nitrogen cooling device according to the difference between the detected temperature and the preset working temperature, thereby realizing closed-loop feedback dynamic temperature regulation. A closed space is formed between the insulation layer 701 and the insulation cover 702 to prevent the liquid nitrogen from being disturbed by the external environment. This not only improves the utilization rate of liquid nitrogen but also prevents safety issues such as operator contact with liquid nitrogen during electrolysis.

[0031] like Figures 18 to 20As shown, the top surface of the insulation cover 702 is integrally provided with an inlet 703 and a outlet 704 that communicate with the interior of the insulation layer 701 on both sides. The feeding end of the cold medium circulation supply device is connected to the inlet 703, and the return end is connected to the outlet 704. The cold medium circulation supply device (i.e., the liquid nitrogen cooling device in this embodiment) continuously fills the sealed cooling chamber between the insulation layer 701 and the cup-shaped container 2 with low-temperature cold medium (liquid nitrogen) from the inlet 703. After absorbing the heat generated by the electrolysis reaction, it is then returned to the cold medium circulation supply device through the outlet 704 for forced cooling. The working principle of the cold medium circulation supply device is prior art and will not be described in detail here. Preferably, the vertical cross-sectional shape of the outer surface of the side wall of the cup-shaped container 2 is wavy, which is beneficial to increasing the contact area between the side wall of the cup-shaped container 2 and the liquid nitrogen, thereby accelerating the cooling rate of the solution during electrolysis. It can effectively reduce the temperature of the electrolyte in a short time and maintain the electrolyte at a low temperature. As the high-speed flowing electrolyte beam impacts the electrolysis area of ​​the electrolysis sample, the heat generated by the reaction can be carried into the electrolyte in the cup-shaped container 2 along with the electrolyte beam, and the heat of the electrolyte can be quickly exchanged. The heat of the electrolyte is further exchanged with the liquid nitrogen through the side wall of the cup-shaped container 2, so that the temperature of the electrolyte is kept in dynamic equilibrium.

[0032] Furthermore, in order to make the flow distribution of liquid nitrogen in the sealed cooling chamber more uniform, the top surface of the heat insulation cover 702 is integrally provided with an annular discharge cavity 705 and the bottom surface is integrally provided with an annular feed cavity 706. A discharge port 704 is integrally disposed on the top surface of the annular discharge cavity 705. At least one discharge collection port 707 is integrally disposed on the bottom surface of the annular discharge cavity 705. The bottom end of the discharge collection port 707 penetrates the annular feed cavity 706 and communicates with the interior of the insulation layer 701. A feed port 703 is integrally disposed on the top surface of the annular feed cavity 706, and the top end of the feed port 703 penetrates the annular discharge cavity 705 and protrudes above the top surface of the annular discharge cavity 705. At least one feed pipe 708 is integrally connected to the bottom surface of the annular feed cavity 706. The bottom end of the feed pipe 708 is located at the inner bottom end of the insulation layer 701, and several material dispersing holes 709 are opened on the side wall of the feed pipe 708. Figure 18 and Figure 19As shown, in this embodiment, there are three discharge collection ports 707, evenly distributed around the axis of the annular discharge cavity 705. There are also three feed pipes 708, evenly distributed around the axis of the annular feed cavity 706, and they are alternately arranged at equal intervals with the three discharge collection ports 707 and the three feed pipes 708. Thus, liquid nitrogen, having absorbed the heat generated by the electrolysis reaction, can simultaneously converge from the three discharge collection ports 707 at the top of the sealed cooling chamber into the annular discharge cavity 705 and be discharged from the discharge port 704. Meanwhile, cryogenic liquid nitrogen enters the annular feed cavity 706 through the feed port 703, and then evenly passes through the three feed pipes 708 and the evenly distributed dispersing holes 709 at the bottom into the bottom of the sealed cooling chamber, where it exchanges heat with the electrolyte.

[0033] A method for EBSD electropolishing of various alloys is provided, which is applied to the aforementioned device for EBSD electropolishing of various alloys. This method can be applied to EBSD electropolishing of various alloys, such as titanium alloys, aluminum alloys, and stainless steel. The calibration success rate can reach over 90%. Generally, a calibration success rate of over 70% is considered qualified, 80% is considered good, and over 90% is considered excellent.

[0034] Traditional metal sample electrolysis involves immersing the sample in an electrolyte solution, employing a face-to-face electrolysis method. This device separates the sample from the electrolyte, eliminating the need for electrolysis of the entire immersed surface, which is particularly beneficial for samples with inhomogeneous structures. The electrolysis area can be selected based on specific needs, such as the sample center, a quarter-radius circle, or the edges; alternatively, a radial path can be chosen to characterize the variation in sample size from the core to the edge. In practice, the area used for electrolysis characterization is only 0.2 × 0.2 mm. Large-area electrolysis not only wastes metal materials and chemical reagents but also increases the difficulty of sample placement and makes electrolyte concentration difficult to control. Conversely, an excessively small electrolysis area is detrimental to microstructure characterization. The ability to autonomously select the electrolysis area reduces the electrolysis area, saves metal materials and chemical reagents, and improves the success rate of electrolysis. Based on full consideration of existing electrolysis methods and testing area requirements, this device transforms the traditional requirement for sample size into a requirement for sample placement tank. The sample placement tank of appropriate size and shape is designed according to the testing requirements. Only the surface of the sample placed in the sample placement tank needs to be smoothed, and there is no need to strictly require the sample size.

[0035] Traditional titanium alloy electrolysis methods involve immersing the sample in an electrolyte solution. Existing methods require sample thicknesses of 0.5-1 mm, or strict size control at 10×10 mm, 7 mm×7 mm, or 10 mm×5 mm×3 mm, demanding high precision and stringent surface finish requirements. Especially for hard alloys like titanium, mechanically grinding large surfaces to meet dimensional requirements is time-consuming and labor-intensive, necessitating a strict grinding sequence: 400 grit, 600 grit, 800 grit, 1500 grit, and 2000 grit. Furthermore, experiments such as nitriding and laser cladding require specific surface depths. This device overcomes these limitations by creating linear, arc-shaped, or zigzag-shaped strips on the sample plate 4, allowing for flexible selection of the sample's thickness direction for strip-shaped electrolysis. This device separates the sample from the electrolyte, thus eliminating the need to adhere to traditional sample preparation size and thickness requirements. The mechanical polishing process only requires 1200-mesh wet-polished paper. Therefore, this device effectively solves both of the aforementioned problems. There are no specific dimensional requirements for length and width; the only requirement for the electrolytic surface is appropriate surface smoothing.

[0036] The success of electropolishing depends on the reasonable selection and setting of polishing parameters (such as stirring speed, output voltage, electrolyte ratio, polishing time, electrolyte temperature, etc.). These parameters can only be obtained through a lot of experimental exploration. The research team of this invention has now successfully mastered the electropolishing related parameters of 15 different materials and different processes through experiments, as shown in Table 1.

[0037] Table 1. Electropolishing parameters of metallic materials with different materials and processes in 15.

[0038] The method for EBSD electropolishing of various alloy types includes the following steps: S1. Prepare the appropriate electrolyte according to the specific metal material type of the electrolytic sample; The types and amounts of metallic elements contained in each metal material vary, resulting in significant differences in the electrolyte ratio for different types of metal materials. Even with the same metal material, despite different initial processing methods, the same electrolyte ratio can be used, but there will be significant differences in the time required. Currently, the electrolyte ratios for 15 different materials and processes have been successfully mastered, as shown in Table 1.

[0039] S2. Pour the prepared electrolyte into a cup-shaped container placed on a magnetic stirrer. The volume of the electrolyte should be 85% to 95% of the volume of the cup-shaped container. Because the electrolyte contains expensive perchloric acid (market price is about 1890 / bottle, and it is a controlled drug that can only be purchased by reservation six months in advance), the cup-shaped container 2 is designed as a straight cylindrical container with a diameter of 50×70mm, pre-filled with 90% electrolyte, which is 123ml, while the perchloric acid content in the corresponding volume of electrolyte is only a few milliliters.

[0040] S3. Fix the electrolytic sample on the sample placement plate, and make the electrolytic area of ​​the electrolytic sample coincide with the position of the sample placement tank. Fix the cathode plate on the sample placement plate, fix the anode plate on the surface of the electrolytic sample, and then fix the sample placement plate to the top of the cup-shaped container.

[0041] S4. Start the magnetic stirrer to drive the magnetic rotor to rotate until the magnetic rotor reaches the preset speed and stabilizes. The electrolyte rotates at a uniform speed to form a vortex and rises continuously along the spiral groove. Through sufficient comparative experiments, it has been verified that the optimal magnetic rotor speed in this device is 800 r / min. Low stirring speeds prevent the electrolyte from forming an upward vortex, while high speeds result in excessive force on the magnetic rotor, causing it to deviate from the center. Furthermore, excessively fast electrolyte rotation speeds mean that ions in the electrolyte beam do not have enough time to remain on the surface of the electrolytic sample for sufficient reaction, leading to insufficient surface erosion in the electrolytic region and ultimately experimental failure. Moreover, excessively high impact velocities of the electrolyte beam exert significant impact on the bottom surface of the sample plate, accelerating the wear and tear on the sample plate and sealing gasket.

[0042] S5. Start the temperature control device to keep the electrolyte temperature in the cup-shaped container at the preset electrolysis temperature; Because many electrolytes contain perchloric acid, they generate rapid heat during the etching process of metal surfaces. If the electrolyte temperature becomes too high, the sample surface will exhibit blackening and pitting, leading to electropolishing failure. Therefore, liquid nitrogen cooling devices are generally used to control the electrolyte temperature to remain stable at 0°C. Simultaneously, the high-speed flowing electrolyte beam impacts the electrolysis area of ​​the sample, carrying the heat generated by the reaction into the electrolyte within the cup-shaped container 2 for rapid heat exchange. The heat from the electrolyte is further exchanged rapidly with the liquid nitrogen through the sidewall of the cup-shaped container 2, thus maintaining a dynamic temperature equilibrium for the electrolyte.

[0043] S6. Based on the type of metal material and the corresponding electrolyte of the electrolytic sample, set the corresponding stable output voltage through the voltage stabilizing output device and apply it to the anode plate and cathode plate respectively. Since each metal material contains different elements, its voltage parameters will also be different. At present, the electrolytic polishing voltage parameters of 15 different materials and processes have been successfully mastered, as shown in Table 1.

[0044] S7. After being energized, the electrolyte circulates and rises and enters the sample tank, contacting the surface of the electrolysis area of ​​the electrolysis sample. The electrolyte flows and impacts the metal surface of the electrolysis area and electrolytically erodes it. After a preset time, the electrolytic polishing of the surface of the electrolysis sample is completed. Polishing time is also a crucial factor. If the time is too short, the surface layer won't be completely etched away, resulting in a low calibration success rate. If the time is too long, the etched layer deepens over time, causing the surface area to decrease with increasing etch depth, forming a near-conical pitted etched structure. This creates vacuum cavitation near the deepest inner layer of the etched structure, preventing further contact between the electrolyte and the sample surface, leading to increasingly poor sample cleanliness. Currently, the optimal polishing times for 15 different materials and processes have been successfully determined, as listed in Table 1.

[0045] S8. Turn off the voltage regulator, magnetic stirrer and temperature control device in sequence to stop the electrolytic polishing operation and remove the electrolytic sample.

[0046] The titanium alloy EBSD sample prepared using the method provided in this invention has the following appearance: Figure 21 As shown, the sample surface is bright, white, and flawless, as can be observed visually. Grain observation under a metallographic microscope yields the following results: Figure 22 As shown. The sample was calibrated under an EBSD electron microscope, and the calibration results are as follows. Figure 23 As shown, the surface of the alloy after electrolytic polishing has clear and distinct grain size and grain boundaries, and the grain orientation information is reliable and accurate, indicating high quality. The calibration success rate is 98%, which can serve as an effective reference for the statistical analysis of orientation information of titanium alloy samples.

[0047] The above description is merely an embodiment of the present invention and does not limit the patent scope of the present invention. Any equivalent structural or procedural transformations made based on the content of the present invention's specification and drawings, or direct or indirect applications in other related technical fields, are similarly included within the patent protection scope of the present invention.

Claims

1. An apparatus suitable for EBSD electropolishing of various alloys, comprising a magnetic stirrer (1), a cup-shaped container (2) placed on the top surface of the magnetic stirrer (1), and a magnetic rotor (3) rotatably disposed on the bottom inner side of the cup-shaped container (2), wherein the magnetic stirrer (1) can drive the magnetic rotor (3) to rotate unidirectionally to stir the electrolyte in the cup-shaped container (2), characterized in that: A spiral groove (201) is fixedly provided on the inner wall of the cup-shaped container (2). A sample plate (4) made of insulating material is fastened to the top opening of the cup-shaped container (2). A sample groove (401) that communicates with the inside of the cup-shaped container (2) is opened on one side of the top surface of the sample plate (4). An electrolytic sample is placed on the top surface of the sample plate (4) directly above the sample groove (401). The rotating electrolyte can rise along the spiral groove (201) to form a small flow of electrolyte with a certain impact force that is continuously rotating and spiraling upward. The electrolyte flow rushes into the sample groove (401) and contacts the bottom surface of the electrolytic sample in the electrolytic area located in the sample groove (401), thereby eroding only the local surface of the electrolytic area. A cathode plate (5) is fixedly installed on the other side of the top surface of the sample plate (4). The bottom end of the cathode plate (5) is located in the electrolyte in the cup-shaped container (2), and the top end is located above the top surface of the sample plate (4). An anode plate (6) is connected to the surface of the electrolytic sample. A temperature regulating device (7) is fitted on the outside of the cup-shaped container (2).

2. The apparatus for EBSD electropolishing of various alloy types according to claim 1, characterized in that: The horizontal cross-section of the magnetic rotor (3) is pentagonal, and a rotating shaft (301) is rotatably connected to its central axis via a bearing. The bottom end of the rotating shaft (301) is fixedly connected to the center of the inner bottom surface of the cup-shaped container (2).

3. The apparatus for EBSD electropolishing of various alloy types according to claim 1, characterized in that: The bottom surface of the sample plate (4) is integrally provided with a hydrophobic structure (402). The hydrophobic structure (402) is composed of multiple layers of annular hydrophobic strips arranged coaxially. The vertical cross-sectional shape of the annular hydrophobic strips is a triangle with the same direction and facing the axis of the sample groove (401).

4. The apparatus for EBSD electropolishing of various alloy types according to claim 1, characterized in that: A sealing gasket (8) is fixedly installed on the top surface of the sample plate (4).

5. The apparatus for EBSD electropolishing of various alloy types according to claim 1, characterized in that: The top surface of the sample plate (4) is provided with a sample clamping mechanism (9). The sample clamping mechanism (9) includes a hinge seat (901) and a locking seat (902) respectively fixed on the top surface of the sample plate (4). A clamping plate (903) is hinged on the hinge seat (901). The end of the clamping plate (903) away from the hinge seat (901) is detachably fastened to the top surface of the locking seat (902). A number of set screws (904) are threaded on the top surface of the clamping plate (903). The bottom end of the set screws (904) presses against the top surface of the electrolytic sample.

6. An apparatus for EBSD electropolishing of multiple types of alloys according to any one of claims 1 to 5, characterized in that: The temperature control device (7) includes a temperature controller, a cold medium circulation supply device, a heat insulation layer (701) sleeved on the outside of the cup-shaped container (2), a heat insulation cover (702) snapped between the top of the cup-shaped container (2) and the heat insulation layer (701), and at least one temperature sensor (710) fixedly installed on the top of the inner wall of the cup-shaped container (2). The top surface of the heat insulation cover (702) is integrally provided with an inlet (703) and a discharge port (704) that communicate with the interior of the heat insulation layer (701). The feeding end of the cold medium circulation supply device is connected to the inlet (703), and the return end is connected to the discharge port (704). The temperature sensor (710) is electrically connected to the temperature controller, and the temperature controller is electrically connected to the power drive mechanism of the cold medium circulation supply device.

7. The apparatus for EBSD electropolishing of various alloy types according to claim 6, characterized in that: The top surface of the heat insulation cover (702) is integrally provided with an annular discharge cavity (705), and the bottom surface is integrally provided with an annular feed cavity (706). The discharge port (704) is integrally disposed on the top surface of the annular discharge cavity (705), and at least one discharge collection port (707) is integrally disposed on the bottom surface of the annular discharge cavity (705). The bottom end of the discharge collection port (707) passes through the annular feed cavity (706) and communicates with the interior of the insulation layer (701). The feed inlet (703) is integrally disposed on the top surface of the annular feed cavity (706), and the top end of the feed inlet (703) passes through the annular discharge cavity (705) and protrudes above the top surface of the annular discharge cavity (705). At least one feed pipe (708) is integrally connected to the bottom surface of the annular feed cavity (706). The bottom end of the feed pipe (708) is located at the bottom inside the insulation layer (701), and several material dispersing holes (709) are opened on the side wall of the feed pipe (708).

8. The apparatus for EBSD electropolishing of multiple types of alloys according to claim 6, characterized in that: The cooling medium circulation supply device is a liquid nitrogen cooling device.

9. An apparatus for EBSD electropolishing of multiple types of alloys according to claim 7 or 8, characterized in that: The vertical cross-sectional shape of the outer side wall of the cup-shaped container (2) is wavy.

10. A method for EBSD electropolishing of multiple types of alloys, applied to the apparatus for EBSD electropolishing of multiple types of alloys as described in any one of claims 1 to 9, characterized in that, Includes the following steps: S1. Prepare the appropriate electrolyte according to the specific metal material type of the electrolytic sample; S2. Pour the prepared electrolyte into a cup-shaped container placed on a magnetic stirrer. The volume of the electrolyte should be 85% to 95% of the volume of the cup-shaped container. S3. Fix the electrolytic sample on the sample plate and make the electrolytic area of ​​the electrolytic sample coincide with the position of the sample tank. Fix the cathode plate on the sample plate and the anode plate on the surface of the electrolytic sample. Then fix the sample plate on the top of the cup-shaped container. S4. Start the magnetic stirrer to drive the magnetic rotor to rotate until the magnetic rotor reaches the preset speed and stabilizes. The electrolyte rotates at a uniform speed to form a vortex and rises continuously along the spiral groove. S5. Start the temperature control device to keep the electrolyte temperature in the cup-shaped container at the preset electrolysis temperature; S6. Based on the type of metal material and the corresponding electrolyte of the electrolytic sample, set the corresponding stable output voltage through the voltage stabilizing output device and apply it to the anode plate and cathode plate respectively. S7. After being energized, the electrolyte circulates and rises and enters the sample tank, contacting the surface of the electrolysis area of ​​the electrolysis sample. The electrolyte flows and impacts the metal surface of the electrolysis area and electrolytically erodes it. After a preset time, the electrolytic polishing of the surface of the electrolysis sample is completed. S8. Turn off the voltage regulator, magnetic stirrer and temperature control device in sequence to stop the electrolytic polishing operation and remove the electrolytic sample.

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