A device for temperature-controlled preparation of a three-dimensional atom probe sample
By designing a temperature-controlled preparation device, uniform electrolysis of three-dimensional atomic probe samples was achieved, solving the problem of uneven corrosion on the sample surface and improving the amount of electrolyte and ease of operation.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- NANJING UNIV OF SCI & TECH
- Filing Date
- 2022-11-29
- Publication Date
- 2026-06-12
Smart Images
Figure CN115754356B_ABST
Abstract
Description
Technical Field
[0001] This invention belongs to the field of three-dimensional atomic probe technology, specifically a device for temperature-controlled preparation of three-dimensional atomic probe samples. Background Technology
[0002] Under the influence of a high electrostatic field, atoms at the tip of a three-dimensional atom probe will ionize and evaporate from the surface. After being evaporated by the field, the atoms on the sample surface leave the sample surface and fly along the DC electric field to the position-sensitive detector. By analyzing the type and position information of each ion, the three-dimensional distribution of ions in the material can be reconstructed. The three-dimensional atom probe is currently the most microscopic analytical instrument, capable of quantitative analysis of composition, and can play an important role in studying many problems of metallic materials.
[0003] The preparation of probes is crucial in three-dimensional atomic probes. Existing preparation methods mainly involve electrolytic polishing. The sample is cut into a long strip shape by wire cutting, immersed in an acidic solution, and connected to the positive terminal of a DC power supply. The negative electrode material is immersed in the acidic solution and connected to the negative terminal of a DC power supply. The sample undergoes electrolysis in the acidic solution, resulting in coarse electrolytic separation to form a needle-like sample. This is then further refined through micro-electrolytic separation to obtain the probe.
[0004] However, during the electrolytic separation of the probe, since the sample is in a static state in the acidic solution, the concentration of the acidic solution around the sample will change during electrolysis, resulting in uneven surface corrosion of the sample and increasing the difficulty of subsequent probe repair.
[0005] Therefore, the present invention provides an apparatus for temperature-controlled preparation of three-dimensional atomic probe samples. Summary of the Invention
[0006] In order to overcome the shortcomings of the prior art, at least one technical problem raised in the background art is solved.
[0007] The technical solution adopted by this invention to solve its technical problem is as follows: A device for temperature-controlled preparation of three-dimensional atomic probe samples, comprising a frame, a turntable, a ring gear, a motor, a spur gear, electric actuators, a fixed frame, and a negative electrode ring; a turntable is rotatably mounted in the center of the top seat of the frame; a ring gear is fixedly connected to the outer ring of the top surface of the turntable; a motor is fixedly connected to one side of the top surface of the frame; a spur gear is fixedly connected to the rotating shaft of the motor, and the spur gear meshes with the ring gear; three electric actuators are uniformly fixedly attached around the bottom surface of the turntable; a fixed frame is bolted to the bottom end of the piston rod of each electric actuator; multiple fixing slots are uniformly formed around the bottom of the fixed frame; multiple samples are uniformly installed inside the fixing slots; and the top surface of the base of the frame is uniformly... A coarse polishing tank, a fine polishing tank, and a cleaning tank are arranged around the perimeter. The coarse polishing tank is filled with coarse polishing electrolyte, the fine polishing tank is filled with fine polishing electrolyte, and the cleaning tank is filled with anhydrous alcohol. Negative electrode rings are arranged inside the coarse and fine polishing tanks, with the outer rings of multiple samples located within the inner rings of the negative electrode rings. The tops of the samples are connected to the positive terminal of a DC power supply, and the tops of the negative electrode rings are connected to the negative terminal of the DC power supply. An aluminum negative electrode ring is placed inside the coarse polishing tank and connected to the negative terminal of the DC power supply. A coarse polishing electrolyte prepared by mixing 30% perchloric acid and 70% glacial acetic acid is added to the coarse polishing tank. Multiple samples are installed into the fixing slots in the fixing frame above the coarse polishing tank, and the positive terminal of the DC power supply is connected... The sample is received; a platinum negative electrode ring is placed in the fine polishing tank and connected to the negative terminal of a DC power supply. A fine polishing electrolyte solution, prepared by mixing 5% perchloric acid and 95% ethylene glycol butyl ether, is added to the fine polishing tank. Anhydrous ethanol is added to the inside of the cleaning tank. An electric actuator pushes the fixing frame downwards, causing the sample to be inserted into the coarse polishing tank, immersing it in the coarse polishing electrolyte for the first stage of electrolysis. Simultaneously, the electric actuator reciprocates up and down, moving the sample in and out of the coarse polishing electrolyte, creating a pointed tip. This reciprocating motion also moves the surrounding coarse polishing electrolyte, reducing the probability of uneven concentration in the sample and improving the surface finish of the sample during the first stage of electrolysis. The smoothness and uniformity of the surface are improved. After the first stage of electrolysis is completed, the electric push rod drives the fixing frame to rise, which in turn lifts the sample after the first stage of electrolysis away from the coarse polishing barrel. At this time, the motor drives the spur gear to rotate, which in turn drives the ring gear meshing with it to rotate, which in turn drives the turntable to rotate. This causes the sample after the first stage of electrolysis to rotate to the top of the fine polishing barrel. The electric push rod pushes downward, which pushes the sample after the first stage of electrolysis into the fine polishing electrolyte inside the fine polishing barrel for the second stage of electrolysis. At the same time, the electric push rod drives the sample to move up and down, which in turn drives the fine polishing electrolyte around the sample to move. This reduces the probability of uneven concentration of the fine polishing electrolyte in the sample and improves the smoothness and uniformity of the sample surface during the second stage of electrolysis.After the second stage of electrolysis is completed, the electric actuator lifts the fixing frame, causing the sample to detach from the fine polishing tank. At this point, the motor drives the turntable to rotate, moving the sample above the cleaning tank. The electric actuator then pushes downwards, immersing the sample in anhydrous alcohol inside the cleaning tank for cleaning, reducing the probability of further corrosion. This completes the electrolytic preparation of the sample and improves the uniformity of electrolytic corrosion.
[0008] Preferably, the coarse polishing electrolyte is a mixture of 30% perchloric acid and 70% glacial acetic acid, and the fine polishing electrolyte is a mixture of 5% perchloric acid and 95% ethylene glycol butyl ether. The negative electrode ring inside the coarse polishing tank is an aluminum ring, and the negative electrode ring inside the fine polishing tank is a platinum ring. The DC power supply current of the coarse polishing tank does not exceed 0.05mA. If the current is too high, the sample corrosion rate will be too fast, causing damage to the sample and producing white smoke. The voltage is gradually adjusted from 5 to 8V to 21V. The voltage of the fine polishing tank is not lower than 16V, and the voltage is adjusted according to the corrosion rate of the sample.
[0009] Preferably, a liquid nitrogen thermostat is provided on one side of the frame, and a thermostat base is fixed to the top surface of the frame base. Multiple circular grooves are evenly distributed around the top surface of the thermostat base, corresponding to the coarse polishing tank, fine polishing tank, and cleaning tank, respectively. The thermostat base is filled with low-temperature heat-conducting oil. The medium inlet and outlet of the liquid nitrogen thermostat are both connected to the interior of the thermostat base. The liquid nitrogen thermostat uses liquid nitrogen as a cooling medium. Liquid nitrogen is filled in the liquid nitrogen chamber inside the thermostat. The heat leakage of the cold finger is kept stable at a certain value by adjusting the gap between the temperature control plug and the cold finger. The heating output power is adjusted by the temperature controller and its internal control system to rapidly change and stabilize the thermostat's temperature. At a certain set value, the sample undergoes rapid electrolytic corrosion at room temperature, making it difficult for operators to control the electrolysis. Controlling the electrolytic corrosion temperature between -10℃ and -20℃ reduces the corrosion rate and makes the corrosion more uniform, facilitating operator control. The low-temperature heat-conducting oil inside the thermostatic base enters the liquid nitrogen thermostat through the medium inlet and is controlled to a constant temperature of -10℃ to -20℃. It then exits through the medium outlet of the liquid nitrogen thermostat back into the thermostatic base, maintaining a constant temperature. This allows for precise control and adjustment of the sample electrolysis temperature, reducing the quality variations in sample preparation caused by temperature changes during electrolysis.
[0010] Preferably, multiple fixing clips are hinged to both sides of the fixing groove, and a torsion spring is sleeved on the outer ring of the rotating shaft of the fixing clip. A rubber pad is fixed to the side of the fixing clip near the sample, and the outer wall of the rubber pad is in pressure contact with the outer ring of the sample. During operation, when the operator installs the sample, the sample is inserted into the inside of the fixing groove from the bottom of the fixing frame, and the sample is clamped and fixed by the fixing clips on both sides. The elasticity of the rubber pad reduces damage to the sample surface.
[0011] Preferably, a blocking frame is fixed to the outer ring of the bottom surface of the fixing frame. The blocking frame is made of corrosion-resistant material, and the outer ring of the blocking frame is fitted around the inner ring of the negative electrode ring. When the electric push rod pushes the sample to move up and down reciprocatingly, the sample will vibrate. If the sample comes into contact with the negative electrode ring, it will cause a short circuit and damage the circuit. By setting the blocking frame, the sample is isolated from the negative electrode ring, reducing the probability of the sample coming into contact with the negative electrode ring, thereby improving the safety of the circuit.
[0012] Preferably, a stop bar is fixed to the top outer ring of the negative electrode ring. A groove is formed on the bottom surface of the stop bar. A screw is rotatably installed inside the groove. One end of the screw passes through the end of the stop bar away from the negative electrode ring. A slider is slidably installed inside the groove. The screw passes through the slider, and the screw and slider are threaded together. A rubber block is fixed to the bottom of the slider near the negative electrode ring. During operation, when the negative electrode ring is placed inside the coarse and fine polishing barrels, the stop bar rests on the top outer ring of the coarse and fine polishing barrels. Rotating the screw pushes the slider to slide along the groove, so that the bottom of the slider contacts and presses the top outer ring of the coarse and fine polishing barrels. At the same time, the sliding distance of each slider is controlled to adjust the position of the negative electrode ring so that the negative electrode ring is located in the middle of the coarse and fine polishing barrels. Meanwhile, the negative electrode ring is fixed and locked, thereby reducing the probability of the negative electrode ring shaking and contacting the sample.
[0013] Preferably, a pressure ring is bolted to the center of the top seat of the frame, the bottom surface of the pressure ring slides in contact with the outer ring of the turntable, and the outer ring of the turntable is provided with ball bearings; the pressure ring fixes the turntable, reducing the probability of the turntable shaking or detaching; the ball bearings improve the smoothness of the turntable rotation.
[0014] Preferably, a cleaning spray holder is fixed to the center of the bottom surface of the fixing frame. The bottom outer ring of the cleaning spray holder has multiple inclined nozzles. A water hole is opened in the center of the fixing frame. The bottom end of the water hole is connected to the interior of the cleaning spray holder, and the top end of the water hole is connected to an anhydrous alcohol storage tank. A water pump is installed on the anhydrous alcohol storage tank. The motor drives the turntable to rotate, and after the sample is rotated after the second stage of electrolysis, it is moved above the cleaning tank. The anhydrous alcohol in the anhydrous alcohol storage tank is pumped into the interior of the cleaning spray holder by the water pump. The anhydrous alcohol is sprayed out from the inclined nozzles and sprayed onto the surface of the sample to rinse the sample surface. This reduces the probability of the sample being corroded by the acidic solution on the surface and improves the quality of sample preparation.
[0015] Preferably, a ring seat is fixed to the outer ring of the middle part of the fixing frame, and multiple crossbars are fixed to the outer ring of the ring seat. The interior of the crossbars is connected to the interior of the ring seat. Multiple air holes are opened at the lower end of the crossbars. The crossbars correspond to the fixing grooves. The top of the ring seat is connected to an air pump through an air pipe. The air pump introduces high-pressure gas into the interior of the ring seat, and then into the interior of the crossbars, and sprays it downward from the air holes. After the sample is driven upward by the electric push rod, the downward sprayed gas blows away the acidic solution and anhydrous alcohol on the sample surface, thereby improving the cleanliness of the sample surface during sample preparation and reducing the probability of sample surface corrosion.
[0016] Preferably, a collection dish is slidably installed at the bottom of the coarse polishing tank, fine polishing tank, and washing tank, and multiple baffles are fixedly connected around the top surface of the inner ring of the collection dish. During operation, when the sample is corroded, the bottom of the sample will be corroded and broken, producing fine solid particles. Since these solid particles detach from the sample and are not electrolyzed, they cannot be dissolved and corroded in time. The solid particles settle into the interior of the collection dish and are separated by the baffles, reducing the movement of solid particles in the solution and their adhesion to the sample surface, thereby improving the cleanliness of the sample surface and improving the quality of the sample.
[0017] The beneficial effects of this invention are as follows:
[0018] 1. The device for temperature-controlled preparation of three-dimensional atomic probe samples according to the present invention comprises a frame, a turntable, a ring gear, a motor, a spur gear, an electric actuator, a fixed frame, and a negative electrode ring. The electric actuator reciprocates up and down, causing the sample to move in and out of the coarse polishing electrolyte, forming a pointed tip at the end of the sample. Simultaneously, the reciprocating motion of the sample moves the surrounding coarse polishing electrolyte, reducing the probability of uneven concentration of the electrolyte in the sample and improving the smoothness and uniformity of the sample surface during the first stage of electrolysis. After the first stage of electrolysis is completed, the electric actuator drives the fixed frame to rise, lifting the sample from the coarse polishing tank. At this time, the motor drives the turntable to rotate, rotating the sample above the fine polishing tank for the second stage of electrolysis. In the second-stage electrolysis, the electric actuator moves the sample up and down, causing the surrounding fine polishing electrolyte to move. This reduces the probability of uneven concentration of the fine polishing electrolyte on the sample and improves the smoothness and uniformity of the sample surface during the second-stage electrolysis. After the second-stage electrolysis is completed, the electric actuator drives the fixing frame to rise, lifting the sample from the fine polishing tank. At this time, the motor drives the turntable to rotate, moving the sample above the cleaning tank. The electric actuator then pushes downwards, immersing the sample in anhydrous alcohol inside the cleaning tank for cleaning, reducing the probability of further corrosion. This completes the electrolytic preparation of the sample and improves the uniformity of electrolytic corrosion.
[0019] 2. The device for temperature-controlled preparation of three-dimensional atomic probe samples according to the present invention comprises a liquid nitrogen thermostat and a thermostatic base. The low-temperature heat-conducting oil inside the thermostatic base enters the liquid nitrogen thermostat from the medium inlet and is controlled to a constant temperature of -10°C to -20°C. Then, it is discharged back into the thermostatic base from the medium outlet of the liquid nitrogen thermostat, so that the thermostatic base is kept at a constant temperature. This controls and adjusts the temperature of sample electrolysis, reducing the quality differences in sample preparation caused by temperature changes during sample electrolysis. Attached Figure Description
[0020] The invention will now be further described with reference to the accompanying drawings.
[0021] Figure 1 This is a perspective view of Embodiment 1 of the present invention;
[0022] Figure 2 This is a cross-sectional view of Embodiment 1 of the present invention;
[0023] Figure 3 This is a perspective view of the fixing frame and negative electrode ring in Embodiment 1 of the present invention;
[0024] Figure 4 This is an exploded view of the fixing frame and negative electrode ring in Embodiment 1 of the present invention;
[0025] Figure 5 This is a cross-sectional view of the fine throwing barrel in Embodiment 1 of the present invention;
[0026] Figure 6 yes Figure 5 Enlarged view of a portion of point A in the middle;
[0027] Figure 7 yes Figure 5 Enlarged view of a section at point B in the middle;
[0028] Figure 8 This is an internal structural diagram of the coarse blasting barrel in Embodiment 2 of the present invention;
[0029] In the diagram: 1. Frame; 2. Turntable; 3. Ring gear; 4. Motor; 5. Spur gear; 6. Electric actuator; 7. Fixing frame; 8. Negative electrode ring; 9. Fixing groove; 10. Sample; 11. Coarse polishing barrel; 12. Fine polishing barrel; 13. Cleaning barrel; 14. Liquid nitrogen thermostat; 15. Thermostatic base; 16. Circular groove; 17. Fixing clamp; 18. Rubber pad; 19. Blocking frame; 20. Stop bar; 21. Slide groove; 22. Screw; 23. Sliding block; 24. Pressure ring; 25. Cleaning spray holder; 26. Inclined nozzle; 27. Water hole; 28. Ring seat; 29. Crossbar; 30. Air hole; 31. Collection dish; 32. Partition. Detailed Implementation
[0030] To make the technical means, creative features, objectives and effects of this invention easier to understand, the invention will be further described below in conjunction with specific embodiments.
[0031] Example 1
[0032] like Figures 1 to 5As shown in the embodiment of the present invention, a device for temperature-controlled preparation of three-dimensional atomic probe samples includes a frame 1, a turntable 2, a ring gear 3, a motor 4, a spur gear 5, electric actuators 6, a fixing frame 7, and a negative electrode ring 8. The turntable 2 is rotatably mounted on the center of the top seat of the frame 1. The ring gear 3 is fixedly connected to the outer ring of the top surface of the turntable 2. The motor 4 is fixedly connected to one side of the top surface of the frame 1. The spur gear 5 is fixedly connected to the rotating shaft of the motor 4, and the spur gear 5 meshes with the ring gear 3. Three electric actuators 6 are evenly and fixedly connected around the bottom surface of the turntable 2. The bottom end of the piston rod of each electric actuator 6 is bolted to the fixing frame 7. The bottom of the frame 7 is evenly surrounded by multiple fixing grooves 9, and multiple samples 10 are evenly installed inside the fixing grooves 9. The top surface of the base of the frame 1 is evenly surrounded by a coarse polishing barrel 11, a fine polishing barrel 12, and a cleaning barrel 13. The coarse polishing barrel 11 is filled with coarse polishing electrolyte, the fine polishing barrel 12 is filled with fine polishing electrolyte, and the cleaning barrel 13 is filled with anhydrous alcohol. Negative electrode rings 8 are arranged inside the coarse polishing barrel 11 and the fine polishing barrel 12. The outer rings of the multiple samples 10 are located within the inner rings of the negative electrode rings 8. The top of each sample 10 is connected to the positive terminal of a DC power supply. The top is connected to the negative terminal of a DC power supply; an aluminum negative electrode ring 8 is placed inside the coarse polishing barrel 11 and connected to the negative terminal of the DC power supply; a coarse polishing electrolyte prepared by mixing 30% perchloric acid and 70% glacial acetic acid is added to the coarse polishing barrel 11; multiple samples 10 are installed inside the fixing slot 9 in the fixing frame 7 above the coarse polishing barrel 11, and the positive terminal of the DC power supply is connected to the sample 10; a platinum negative electrode ring 8 is placed inside the fine polishing barrel 12 and connected to the negative terminal of the DC power supply; a fine polishing electrolyte prepared by mixing 5% perchloric acid and 95% ethylene glycol butyl ether is added to the fine polishing barrel 12. Anhydrous alcohol is added to the inside of the cleaning tank 13; the electric push rod 6 pushes the fixing frame 7 down, causing the sample 10 to be inserted into the inside of the coarse polishing tank 11, so that the sample 10 is immersed in the coarse polishing electrolyte for the first stage of electrolysis. At the same time, the electric push rod 6 moves up and down, causing the sample 10 to move in and out of the coarse polishing electrolyte, so that the end of the sample 10 forms a sharp point. At the same time, the up and down reciprocating motion of the sample 10 causes the coarse polishing electrolyte around the sample 10 to move, reducing the probability of uneven concentration of the coarse polishing electrolyte in the sample 10, and improving the smoothness and uniformity of the surface of the sample 10 during the first stage of electrolysis.After the first stage of electrolysis is completed, the electric push rod 6 drives the fixing frame 7 to rise, lifting the sample 10, which has completed the first stage of electrolysis, away from the coarse polishing tank 11. At this time, the motor 4 drives the spur gear 5 to rotate, which in turn drives the meshing ring gear 3 to rotate, causing the turntable 2 to rotate. This rotates the sample 10, which has completed the first stage of electrolysis, to the top of the fine polishing tank 12. The electric push rod 6 then pushes downward, immersing the sample 10, which has completed the first stage of electrolysis, into the fine polishing electrolyte inside the fine polishing tank 12 for the second stage of electrolysis. Simultaneously, the electric push rod 6 drives the sample 10 to move up and down, causing the fine polishing electrolyte around the sample 10 to move, reducing the uneven concentration of the fine polishing electrolyte in the sample 10. This increases the probability of further corrosion and improves the smoothness and uniformity of the sample 10 surface during the second stage of electrolysis. After the second stage of electrolysis is completed, the electric push rod 6 drives the fixing frame 7 to rise, lifting the sample 10 from the fine polishing tank 12. At this time, the motor 4 drives the turntable 2 to rotate, rotating the sample 10 above the cleaning tank 13. The electric push rod 6 pushes downward, immersing the sample 10 in the anhydrous alcohol inside the cleaning tank 13 for cleaning, reducing the probability of further corrosion. This completes the electrolytic preparation of the sample 10 and improves the uniformity of electrolytic corrosion.
[0033] The coarse polishing electrolyte is a mixture of 30% perchloric acid and 70% glacial acetic acid, and the fine polishing electrolyte is a mixture of 5% perchloric acid and 95% ethylene glycol butyl ether. The negative electrode ring 8 inside the coarse polishing tank 11 is an aluminum ring, and the negative electrode ring 8 inside the fine polishing tank 12 is a platinum ring. The DC power supply current of the coarse polishing tank 11 does not exceed 0.05mA. If the current is too high, the corrosion rate of sample 10 will be too fast, causing damage to sample 10 and producing white smoke. The voltage is gradually adjusted from 5 to 8V to 21V. The voltage of the fine polishing tank 12 is not lower than 16V, and the voltage is adjusted according to the corrosion rate of sample 10.
[0034] like Figures 1 to 2As shown, a liquid nitrogen thermostat 14 is installed on one side of the frame 1. A thermostat base 15 is fixed to the top surface of the base of the frame 1. Multiple circular grooves 16 are evenly distributed around the top surface of the thermostat base 15, corresponding to the coarse polishing tank 11, fine polishing tank 12, and cleaning tank 13, respectively. The thermostat base 15 is filled with low-temperature heat-conducting oil. The medium inlet and outlet of the liquid nitrogen thermostat 14 are both connected to the interior of the thermostat base 15. The liquid nitrogen thermostat 14 uses liquid nitrogen as a cooling medium. Liquid nitrogen is filled into the liquid nitrogen chamber inside the thermostat 14. The heat leakage of the cold finger is kept stable at a certain value by adjusting the gap between the temperature control plug and the cold finger. The heating output power is adjusted through the internal control system of the temperature controller, allowing the thermostat to rapidly change temperature and stabilize quickly. At a certain set value; when sample 10 is at room temperature, the electrolytic corrosion rate of sample 10 is relatively fast, which is not convenient for operators to control the electrolysis. When the temperature during electrolytic corrosion is controlled at -10℃ to -20℃, the electrolytic corrosion rate of sample 10 will decrease, and the electrolytic corrosion of sample 10 will be more uniform, making it easier for operators to operate and control; the low-temperature heat transfer oil inside the constant temperature base 15 enters the liquid nitrogen constant temperature 14 from the medium inlet of the liquid nitrogen constant temperature 14 and is controlled to a constant temperature of -10℃ to -20℃, and then is discharged back into the constant temperature base 15 from the medium outlet of the liquid nitrogen constant temperature 14, so that the constant temperature base 15 is kept at a constant temperature, thereby controlling and adjusting the electrolysis temperature of sample 10, reducing the quality difference of sample 10 preparation caused by temperature changes during electrolysis.
[0035] like Figure 3 , Figure 4 and Figure 6 As shown, multiple fixing clips 17 are hinged to both sides of the fixing groove 9. A torsion spring is sleeved on the outer ring of the rotating shaft of the fixing clip 17. A rubber pad 18 is fixed to the side of the fixing clip 17 near the sample 10. The outer wall of the rubber pad 18 is in contact with the outer ring of the sample 10. During operation, when the operator installs the sample 10, the sample 10 is inserted into the fixing groove 9 from the bottom of the fixing frame 7, and the sample 10 is clamped and fixed by the fixing clips 17 on both sides. The elasticity of the rubber pad 18 reduces damage to the surface of the sample 10.
[0036] like Figures 2 to 5 As shown, a blocking frame 19 is fixed to the outer ring of the bottom surface of the fixing frame 7. The blocking frame 19 is made of corrosion-resistant material, and the outer ring of the blocking frame 19 is fitted around the inner ring of the negative electrode ring 8. When the electric push rod 6 pushes the sample 10 to move up and down reciprocally, the sample 10 will vibrate. If the sample 10 comes into contact with the negative electrode ring 8, it will cause a short circuit and damage the circuit. By setting the blocking frame 19, the sample 10 is isolated from the negative electrode ring 8, reducing the probability of the sample 10 coming into contact with the negative electrode ring 8, thereby improving the safety of the circuit.
[0037] like Figure 3 , Figure 4 , Figure 5 and Figure 7 As shown, a stop bar 20 is fixedly connected to the top outer ring of the negative electrode ring 8. A groove 21 is formed on the bottom surface of the stop bar 20. A screw 22 is rotatably installed inside the groove 21. One end of the screw 22 passes through the end of the stop bar 20 away from the negative electrode ring 8. A slider 23 is slidably installed inside the groove 21. The screw 22 passes through the slider 23, and the screw 22 and the slider 23 are threaded together. A rubber block is fixedly connected to the bottom of the slider 23 near the negative electrode ring 8. During operation, the negative electrode ring 8 is placed in the coarse polishing barrel 11 and the fine polishing barrel 12. When the sample is inside the coarse and fine throwing barrels 12, the stop bar 20 rests on the top outer ring of the coarse and fine throwing barrels 11. The screw 22 is rotated to push the slider 23 to slide along the groove 21, so that the bottom of the slider 23 contacts and presses the top outer ring of the coarse and fine throwing barrels 11 and 12. At the same time, the sliding distance of each slider 23 is controlled to adjust the position of the negative electrode ring 8 so that the negative electrode ring 8 is located in the middle of the coarse and fine throwing barrels 11 and 12. Meanwhile, the negative electrode ring 8 is fixed and locked, thereby reducing the probability of the negative electrode ring 8 shaking and contacting the sample 10.
[0038] like Figures 1 to 2 As shown, a pressure ring 24 is bolted to the middle of the top seat of the frame 1. The bottom surface of the pressure ring 24 slides with the outer ring of the turntable 2, and the outer ring of the turntable 2 is provided with balls. The pressure ring 24 fixes the turntable 2, reducing the probability of the turntable 2 shaking or falling off. The balls improve the smoothness of the turntable 2 when rotating.
[0039] like Figure 4 and Figure 6 As shown, a cleaning spray base 25 is fixedly connected to the center of the bottom surface of the fixing frame 7. The bottom outer ring of the cleaning spray base 25 has multiple inclined nozzles 26. A water hole 27 is opened in the center of the fixing frame 7. The lower end of the water hole 27 is connected to the interior of the cleaning spray base 25, and the top pipe of the water hole 27 is connected to the anhydrous alcohol storage tank. A water pump is installed on the anhydrous alcohol storage tank. The motor 4 drives the turntable 2 to rotate, which drives the sample 10 after the second stage of electrolysis to rotate above the cleaning tank 13. The anhydrous alcohol in the anhydrous alcohol storage tank is pumped into the interior of the cleaning spray base 25 by the water pump. The anhydrous alcohol is sprayed out from the inclined nozzles 26 and sprayed onto the surface of the sample 10 to rinse the surface of the sample 10, reducing the probability of the sample 10 being corroded by the acidic solution on the surface and improving the quality of the sample 10 preparation.
[0040] like Figure 4 and Figure 6As shown, a ring seat 28 is fixed to the outer ring of the middle part of the fixing frame 7. Multiple crossbars 29 are fixed to the outer ring of the ring seat 28. The interior of the crossbars 29 is connected to the interior of the ring seat 28. Multiple air holes 30 are opened at the lower end of the crossbars 29. The crossbars 29 correspond to the fixing groove 9. The top of the ring seat 28 is connected to the air pump through the air pipe. The air pump introduces high-pressure gas into the interior of the ring seat 28 and then into the interior of the crossbars 29, and sprays it downward from the air holes 30. After the sample 10 is driven to rise by the electric push rod 6, the downward sprayed gas blows away the acidic solution and anhydrous alcohol on the surface of the sample 10, thereby improving the cleanliness of the sample 10 surface during preparation and reducing the probability of corrosion of the sample 10 surface.
[0041] Example 2
[0042] like Figure 8 As shown in the comparative embodiment one, another embodiment of the present invention is as follows: a collection dish 31 is slidably installed at the bottom of the coarse polishing tank 11, the fine polishing tank 12 and the washing tank 13. A plurality of partitions 32 are fixedly connected around the top surface of the inner ring of the collection dish 31. During operation, when the sample 10 is corroded, the bottom of the sample 10 will be corroded and broken, producing fine solid particles. Since the solid particles are separated from the sample 10 and are not electrolyzed, the solid particles cannot be dissolved and corroded in time. The solid particles settle into the interior of the collection dish 31 and are separated by the partitions 32, which reduces the movement of solid particles in the solution and their adhesion to the surface of the sample 10, thereby improving the cleanliness of the sample 10 surface and improving the quality of the sample 10.
[0043] Working principle: When the negative electrode ring 8 is placed inside the coarse polishing tank 11 and the fine polishing tank 12, the stop rod 20 rests on the top outer ring of the coarse polishing tank 11 and the fine polishing tank 12. Rotating the screw 22 pushes the slider 23 to slide along the groove 21, causing the bottom of the slider 23 to contact and press against the top outer ring of the coarse polishing tank 11 and the fine polishing tank 12. Simultaneously, the sliding distance of each slider 23 is controlled to adjust the position of the negative electrode ring 8, ensuring it is located in the middle of the coarse polishing tank 11 and the fine polishing tank 12. A coarse polishing electrolyte prepared by mixing 30% perchloric acid and 70% glacial acetic acid is added to the coarse polishing tank 11. A mixture of 5% perchloric acid and 95% ethylene glycol butyl ether is also added. The fine polishing electrolyte is prepared and added to the fine polishing tank 12. Anhydrous alcohol is added to the cleaning tank 13. The low-temperature heat transfer oil inside the constant temperature base 15 enters the liquid nitrogen thermostat 14 through the medium inlet and is controlled to a constant temperature of -10°C to -20°C. Then it is discharged back into the constant temperature base 15 from the medium outlet of the liquid nitrogen thermostat 14, so that the constant temperature base 15 is kept at a constant temperature, and the coarse polishing tank 11, fine polishing tank 12 and cleaning tank 13 are kept at a constant temperature. The sample 10 is inserted into the fixing groove 9 from the bottom of the fixing frame 7 and clamped and fixed by the fixing clips 17 on both sides.
[0044] The electric push rod 6 pushes the fixing frame 7 down, causing the sample 10 to be inserted into the coarse polishing barrel 11, so that the sample 10 is immersed in the coarse polishing electrolyte for the first stage of electrolysis. At the same time, the electric push rod 6 moves up and down, causing the sample 10 to move in and out of the coarse polishing electrolyte, so that the end of the sample 10 forms a sharp point. At the same time, the up and down reciprocating motion of the sample 10 causes the coarse polishing electrolyte around the sample 10 to move, reducing the probability of uneven concentration of the coarse polishing electrolyte on the sample 10 and improving the smoothness and uniformity of the surface of the sample 10 during the first stage of electrolysis. After the first stage of electrolysis is completed, the electric push rod 6 drives the fixing frame 7 up, causing the sample 10 to rise and detach from the coarse polishing barrel 11. At the same time, the air pump introduces high-pressure gas into the ring seat 28 and then into the crossbar 29, and sprays it downward from the air hole 30, blowing the coarse polishing electrolyte on the surface of the sample 10 back into the coarse polishing barrel 11.
[0045] At this time, the motor 4 drives the spur gear 5 to rotate, which in turn drives the ring gear 3 to rotate, causing the turntable 2 to rotate. This rotates the sample 10, which has completed the first stage of electrolysis, to the top of the fine polishing tank 12. The electric push rod 6 pushes downward, immersing the sample 10, which has completed the first stage of electrolysis, into the fine polishing electrolyte inside the fine polishing tank 12 for the second stage of electrolysis. At the same time, the electric push rod 6 drives the sample 10 to move up and down, causing the fine polishing electrolyte around the sample 10 to move, reducing the probability of uneven concentration of the fine polishing electrolyte on the sample 10, and improving the smoothness and uniformity of the sample 10 surface during the second stage of electrolysis. After the second stage of electrolysis is completed, the electric push rod 6 drives the fixing frame 7 to rise, causing the sample 10, which has completed the second stage of electrolysis, to rise and detach from the fine polishing tank 12. At the same time, the downward-spraying airflow blows the fine polishing electrolyte on the surface of the sample 10 back into the fine polishing tank 12.
[0046] Motor 4 drives turntable 2 to rotate, causing sample 10, after the second stage of electrolysis, to rotate above cleaning tank 13. Electric push rod 6 pushes downward, immersing sample 10, after the second stage of electrolysis, into anhydrous alcohol inside cleaning tank 13 for cleaning. Simultaneously, anhydrous alcohol in the anhydrous alcohol storage tank is pumped into cleaning spray nozzle 25 by water pump. Anhydrous alcohol is sprayed out from inclined nozzle 26, spraying anhydrous alcohol onto the surface of sample 10 to rinse the surface of sample 10, reducing the probability of sample 10 being corroded by acidic solution on the surface and improving the quality of sample 10 preparation; thus completing the electrolytic preparation of sample 10 and improving the uniformity of electrolytic corrosion of sample 10.
[0047] The foregoing has shown and described the basic principles, main features, and advantages of the present invention. Those skilled in the art should understand that the present invention is not limited to the above embodiments. The embodiments and descriptions in the specification are merely illustrative of the principles of the invention. Various changes and modifications can be made to the invention without departing from its spirit and scope, and all such changes and modifications fall within the scope of the present invention as claimed. The scope of protection of the present invention is defined by the appended claims and their equivalents.
Claims
1. An apparatus for temperature-controlled preparation of three-dimensional atomic probe samples, characterized in that: The system includes a frame (1), a turntable (2), a ring gear (3), a motor (4), a spur gear (5), electric actuators (6), a fixed frame (7), and a negative electrode ring (8). The turntable (2) is rotatably mounted on the top seat of the frame (1). The ring gear (3) is fixedly connected to the outer ring of the top surface of the turntable (2). The motor (4) is fixedly connected to one side of the top surface of the frame (1). The spur gear (5) is fixedly connected to the shaft of the motor (4). The spur gear (5) meshes with the ring gear (3). Three electric actuators (6) are evenly fixed around the bottom surface of the turntable (2). The piston rod of the electric actuator (6) is bolted to the lower end of the piston rod of the electric actuator (6). The bottom of the fixed frame (7) is evenly surrounded by multiple fixed electrodes. The fixed tank (9) is uniformly equipped with multiple samples (10). The base of the frame (1) is uniformly surrounded by a coarse polishing tank (11), a fine polishing tank (12) and a cleaning tank (13). The coarse polishing tank (11) is filled with coarse polishing electrolyte, the fine polishing tank (12) is filled with fine polishing electrolyte, and the cleaning tank (13) is filled with anhydrous alcohol. The coarse polishing tank (11) and the fine polishing tank (12) are equipped with negative electrode rings (8). The outer ring of the multiple samples (10) is located in the inner ring of the negative electrode ring (8). The top of the sample (10) is connected to the positive terminal of the DC power supply, and the top of the negative electrode ring (8) is connected to the negative terminal of the DC power supply. A liquid nitrogen thermostat (14) is provided on one side of the frame (1). A thermostat base (15) is fixed to the top surface of the base of the frame (1). A plurality of circular grooves (16) are evenly distributed around the top surface of the thermostat base (15). The plurality of circular grooves (16) correspond to the coarse blasting barrel (11), the fine blasting barrel (12) and the cleaning barrel (13) respectively. The thermostat base (15) is filled with low temperature heat transfer oil. The medium inlet and medium outlet of the liquid nitrogen thermostat (14) are both connected to the interior of the thermostat base (15).
2. The apparatus for temperature-controlled preparation of three-dimensional atomic probe samples according to claim 1, characterized in that: The coarse polishing electrolyte is a mixture of 30% perchloric acid and 70% glacial acetic acid, and the fine polishing electrolyte is a mixture of 5% perchloric acid and 95% ethylene glycol butyl ether. The negative electrode ring (8) inside the coarse polishing barrel (11) is an aluminum ring, and the negative electrode ring (8) inside the fine polishing barrel (12) is a platinum ring. The DC power supply current of the coarse polishing barrel (11) does not exceed 0.05mA, and the voltage is gradually adjusted from 5 to 8V to 21V. The voltage of the fine polishing barrel (12) is not lower than 16V.
3. The apparatus for temperature-controlled preparation of three-dimensional atomic probe samples according to claim 1, characterized in that: Multiple fixing clips (17) are hinged to both sides of the fixing groove (9). A torsion spring is sleeved on the outer ring of the rotating shaft of the fixing clip (17). A rubber pad (18) is fixed to the side of the fixing clip (17) near the sample (10). The outer wall of the rubber pad (18) is pressed against the outer ring of the sample (10).
4. The apparatus for temperature-controlled preparation of three-dimensional atomic probe samples according to claim 1, characterized in that: The bottom outer ring of the fixed frame (7) is fixedly connected to a blocking frame (19), which is made of corrosion-resistant material, and the outer ring of the blocking frame (19) is fitted around the inner ring of the negative electrode ring (8).
5. The apparatus for temperature-controlled preparation of three-dimensional atomic probe samples according to claim 1, characterized in that: A stop bar (20) is fixedly connected to the top outer ring of the negative electrode ring (8). A groove (21) is provided on the bottom surface of the stop bar (20). A screw (22) is rotatably installed inside the groove (21). One end of the screw (22) passes through the end of the stop bar (20) away from the negative electrode ring (8). A slider (23) is slidably installed inside the groove (21). The screw (22) passes through the slider (23), and the screw (22) and the slider (23) are threaded together. A rubber block is fixedly connected to the bottom of the slider (23) on the side close to the negative electrode ring (8).
6. The apparatus for temperature-controlled preparation of three-dimensional atomic probe samples according to claim 1, characterized in that: A pressure ring (24) is bolted to the middle of the top seat of the frame (1). The bottom surface of the pressure ring (24) slides with the outer ring of the turntable (2), and the outer ring of the turntable (2) is provided with balls.
7. The apparatus for temperature-controlled preparation of three-dimensional atomic probe samples according to claim 1, characterized in that: A cleaning spray base (25) is fixedly connected to the middle of the bottom surface of the fixed frame (7). Multiple inclined nozzles (26) are opened on the outer ring of the bottom of the cleaning spray base (25). A water hole (27) is opened in the middle of the fixed frame (7). The lower end of the water hole (27) is connected to the interior of the cleaning spray base (25). The top pipe of the water hole (27) is connected to the anhydrous alcohol storage tank, and a water pump is installed on the anhydrous alcohol storage tank.
8. The apparatus for temperature-controlled preparation of three-dimensional atomic probe samples according to claim 7, characterized in that: The middle outer ring of the fixed frame (7) is fixedly connected to a ring seat (28), and the outer ring of the ring seat (28) is fixedly connected to a plurality of crossbars (29). The interior of the crossbars (29) is connected to the interior of the ring seat (28). The lower end of the crossbars (29) is provided with a plurality of air holes (30). The crossbars (29) correspond to the fixed groove (9). The top end of the ring seat (28) is connected to an air pump through an air pipe.
9. The apparatus for temperature-controlled preparation of three-dimensional atomic probe samples according to claim 1, characterized in that: The bottom of the coarse throwing barrel (11), fine throwing barrel (12) and washing barrel (13) are all slidably installed with a collection dish (31), and the inner top surface of the collection dish (31) is surrounded and fixed with multiple partitions (32).