A method and apparatus for cleaning a crucible

Abstract

The application discloses a kind of crucible cleaning method and equipment, it is related to the field of semiconductor manufacturing technology, wherein the method comprises: the material frame of loading indium phosphide crucible is sent into the front section processing area, and is sequentially carried out pickling and rapid flushing;After completing rapid flushing, the partition between the front section processing area and the rear section rinsing area is opened, and the material frame is sent into the rear section rinsing area to carry out ultrasonic rinsing;The water resistivity of rinsing liquid is detected, when not reaching preset threshold, the material frame is returned to pickling procedure and is cleaned again, when reaching preset threshold, slow pull drying and discharging are carried out.The application is automatically connected through pickling, rapid flushing, ultrasonic rinsing and slow pull drying, reduces manual operation;Through the control mode of being flushed first and then transferred into the rear section rinsing area, residual acid liquid is reduced to the carrying of rear section station;Through water resistivity detection and rewashing control combination, the controllability and batch consistency of cleaning process are improved.

Description

Technical Field

[0001] This application relates to the field of regulatory technology, and in particular to a crucible cleaning method and equipment. Background Technology

[0002] Indium phosphide (IP) is a semiconductor material used in the fabrication of high-frequency chips, optical communication devices, and infrared detectors. In the preparation of IPT single crystals, crystal growth processes such as the high-temperature Czochralski method and the Bridgman process can be employed, utilizing containers such as quartz crucibles or silicon carbide crucibles to hold the growth material. As the process container in contact with the growth material, the cleanliness of the crucible's inner surface significantly impacts the subsequent crystal growth process.

[0003] After the crystal growth process, the inner wall of the crucible may be adhered to by indium phosphide microcrystals, indium oxide impurities, elemental phosphorus residues, and dense deposits formed by high temperatures. With repeated use, some of these deposits may form a strong bond with the inner wall of the crucible. If these residues are not thoroughly removed, impurities may be introduced during subsequent use, increasing the risk of defects such as dislocations, inclusions, polycrystalline structures, and surface black spots in the single crystal, thus affecting the quality and production yield of the single crystal product.

[0004] Existing methods for cleaning indium phosphide crucibles mainly include manual knocking to remove slag, manual acid and alkali soaking, manual rinsing with pure water, and natural air drying. These cleaning methods are highly dependent on personnel experience and operating habits, and it is difficult to maintain consistent mechanical action, contact time with the chemical solution, and degree of rinsing during the cleaning process.

[0005] When manually removing slag by tapping, the force is easily concentrated in certain areas, and the tapping force is difficult to control accurately, which may cause scratches or micro-cracks on the inner wall of the crucible. When the crucible is reused under subsequent high-temperature conditions, the above-mentioned damage may further affect its service life.

[0006] During manual soaking and rinsing, the cleaning time, solution concentration, solution temperature, and number of rinses lack uniform control, which can easily lead to differences between different personnel and different batches. For dense deposits on the inner wall of the crucible and locally retained solution, relying solely on soaking and manual rinsing may result in insufficient cleaning.

[0007] Furthermore, manual operation often involves repeatedly moving crucibles between different containers, and the crucibles and their carriers after pickling can easily carry residual acid into subsequent workstations. If there is a lack of effective separation and a reasonable transfer sequence between processing stations, acid mist may also spread to the subsequent cleaning area or operating area, causing equipment corrosion, secondary contamination of workpieces, and personnel exposure to corrosive media.

[0008] Air drying takes a long time, and the crucible is susceptible to environmental particulate contamination during the drying process. Residual moisture on its surface may also evaporate in situ, leaving water stains that can affect subsequent use.

[0009] In summary, existing indium phosphide crucible cleaning methods suffer from low production efficiency, high risk of mechanical damage, insufficient consistency in cleaning quality, and easy diffusion of acid and acid mist. There is a need to provide cleaning methods and equipment that can achieve continuous processing and process control. Summary of the Invention

[0010] In view of this, the purpose of this application is to provide a crucible cleaning method and equipment to solve the problems of low production efficiency, easy damage to crucibles, inconsistent cleaning quality, and easy impact of acid and acid mist on subsequent work stations and operating environment in the existing indium phosphide crucible cleaning methods.

[0011] To achieve the above technical objectives, this application provides a crucible cleaning method, comprising: The material frame containing the indium phosphide crucible to be cleaned is loaded and sent to the front-end processing area for acid washing of the indium phosphide crucible. The pickled material frame is quickly rinsed in the front-end processing area to remove residual acid carried by the material frame and the indium phosphide crucible. After the material frame completes rapid rinsing, the partition between the front treatment area and the rear rinsing area is opened, the material frame is sent into the rear rinsing area for ultrasonic rinsing, and the partition is restored after the material frame passes through. The water resistivity of the rinsing solution at the end of the ultrasonic rinsing is detected, and the detection result is compared with a preset water resistivity threshold. When the detection result is less than the preset water resistivity threshold, the material frame is returned to the front-end processing area for pickling, rapid rinsing and ultrasonic rinsing. When the detection result is greater than or equal to the preset water resistivity threshold, the material frame is sent to the drying station for slow drying, and the dried material frame is unloaded.

[0012] Furthermore, the pickling includes: Place the material frame into the pickling tank containing the pickling solution, and close the automatic tank cover of the pickling tank. The pickling solution is heated and ultrasonically treated, and the material frame is driven to vibrate up and down in the pickling solution to dissolve and remove the adhering substances on the surface of the indium phosphide crucible. After pickling is completed, open the automatic tank cover and remove the material frame from the pickling tank.

[0013] Furthermore, the rapid rinsing is a QDR rapid rinsing performed in a rapid rinsing tank, and the QDR rapid rinsing includes ultrapure water overflow replacement, spray rinsing and rapid drainage; The ultrapure water overflow replacement includes continuously supplying ultrapure water to the rapid rinsing tank, so that the liquid in the rapid rinsing tank is discharged through the overflow structure; The spray rinsing includes spraying ultrapure water onto the material frame and the indium phosphide crucible; The rapid drainage includes draining the liquid from the tank through a rapid drainage valve located at the bottom of the rapid rinsing tank.

[0014] Furthermore, the ultrasonic rinsing includes a first ultrasonic rinsing and a second ultrasonic rinsing performed sequentially in a first ultrasonic tank and a second ultrasonic tank. The water resistivity of the rinsing solution in the second ultrasonic tank is detected by a water resistivity sensor installed in the second ultrasonic tank. When the detection result is less than the preset water resistivity threshold, the material frame is returned to the pickling tank and pickled, QDR rapid rinsing, first ultrasonic rinsing and second ultrasonic rinsing are performed in sequence.

[0015] Furthermore, the slow-pull drying includes: Ultrapure water and isopropanol are supplied to the slow-pull tank through a pure water supply system and an IPA supply system, respectively, and the drying temperature of the slow-pull tank is adjusted by a heating component. The material frame is slowly raised, causing the indium phosphide crucible to gradually detach from the liquid surface. The Marangoni effect is generated by the surface tension gradient formed by isopropanol, which causes the liquid film on the surface of the indium phosphide crucible to retreat from the surface of the indium phosphide crucible.

[0016] This application also discloses a crucible cleaning device, including a frame, a conveying mechanism, a control unit, and a loading station, an acid washing tank, a rapid rinsing tank, an ultrasonic rinsing assembly, a slow pulling tank, and a unloading station arranged in the material frame processing sequence. The pickling tank and the rapid rinsing tank are located in the front treatment area, and the ultrasonic rinsing assembly is located in the rear rinsing area. A first partition is provided between the feeding station and the front processing area, and a second partition is provided between the front processing area and the rear rinsing area. The conveying mechanism is used to transfer material frames between each workstation and each tank, and the material frames are used to load indium phosphide crucibles; The ultrasonic rinsing assembly is equipped with a water resistivity sensor for detecting the water resistivity of the final rinsing solution. The control unit is connected to the conveying mechanism, the first partition, the second partition, and the water resistivity sensor, respectively, and is configured as follows: After the pickled material frame completes rinsing in the rapid rinsing tank, the second partition is opened to allow the material frame to enter the subsequent rinsing area, and the second partition is closed after the material frame has passed through. The detection result of the water resistivity sensor is compared with a preset water resistivity threshold. When the detection result is less than the preset water resistivity threshold, the conveying mechanism is controlled to return the material frame to the pickling tank for re-cleaning. When the detection result is greater than or equal to the preset water resistivity threshold, the conveying mechanism is controlled to send the material frame into the slow-pull trough.

[0017] Furthermore, the pickling tank is equipped with an automatic tank cover, an upper and lower oscillation mechanism, an ultrasonic vibrating plate, and a pickling heating device; The automatic tank cover is flipped relative to the pickling tank by a tank cover drive cylinder; The ultrasonic vibrating plate is disposed at the bottom of the pickling tank, and the pickling heating device is disposed around the pickling tank, including a PFA heater. The up-and-down oscillation mechanism includes a material frame base, a guide rail, an oscillation drive wheel, and an oscillation drive linkage. The material frame base is used to support the material frame and moves up and down under the guidance of the guide rail; One end of the oscillation drive linkage is rotatably connected to the eccentric position of the oscillation drive wheel, and the other end is rotatably connected to the connecting part that drives the material frame base to move up and down.

[0018] Furthermore, the rapid rinsing tank is a QDR rinsing tank, which is equipped with an ultrapure water supply structure, an overflow tank, a spray pipe, and a fast drain valve. The overflow trough is located at the top of the QDR flushing trough and is used to receive the liquid overflowing from the QDR flushing trough. The spray pipe is positioned toward the material frame located inside the QDR rinsing tank; The quick-drain valve is connected to the bottom of the QDR flushing tank.

[0019] Furthermore, the ultrasonic rinsing assembly includes a first ultrasonic tank and a second ultrasonic tank arranged sequentially along the material frame processing sequence, and the water resistivity sensor is disposed in the second ultrasonic tank. The slow-pull tank is equipped with a heating component, an IPA liquid addition system, and a pure water liquid addition system; The pure water dosing system is used to supply ultrapure water to the slow-pull tank, and the IPA dosing system is used to supply isopropanol to the slow-pull tank. The conveying mechanism can drive the material frame to rise slowly relative to the slow-pull trough, so that the indium phosphide crucible gradually detaches from the liquid surface.

[0020] Furthermore, the frame includes a 304 stainless steel skeleton and a PP plate covering the outside of the 304 stainless steel skeleton; An FFU filter is installed on the top of the rack, and exhaust vents connected to the exhaust duct are provided inside the pickling tank and on the side of the tank. The first partition and the second partition are respectively the first automatic lifting door and the second automatic lifting door; The handling mechanism is a handling robot, which includes a horizontal moving component, a vertical lifting component, and a picking and placing part for picking up and placing the material frame, arranged along the direction of each workstation.

[0021] As can be seen from the above technical solutions, the crucible cleaning method and equipment designed in this application have the following beneficial effects: 1. By connecting the feeding, pickling, rapid rinsing, ultrasonic rinsing, slow drying and unloading, and using a conveying mechanism to automatically transfer the material frame loading the crucible, the cleaning process can be carried out continuously in a set sequence, reducing manual repeated handling and tank-by-tank operation, and improving batch cleaning efficiency.

[0022] 2. For indium phosphide microcrystals, phosphides, indium oxide and other adhering residues, the adhering residues are removed and the chemical solution is replaced step by step through pickling, rapid rinsing and ultrasonic rinsing. Among them, the heating, ultrasonic action and up-and-down vibration during pickling can promote the contact between the chemical solution and the adhering residues, and the water resistivity detection of the final rinsing solution can provide process criteria for rewashing control and improve the repeatability of residual pollution control.

[0023] 3. Cleaning is completed by using the action of the liquid, controlled up-and-down vibration, and ultrasonic treatment adapted to the crucible. This reduces manual knocking and direct scraping operations, lowers the risk of mechanical damage such as scratches and micro-cracks on the crucible, and helps extend the service life of the crucible.

[0024] 4. By combining the treatment area partition, pickling tank cover, top clean air supply and tank interior and side exhaust, the entry of external particles and acid mist overflow are reduced; the pickled material frame is first quickly rinsed in the front treatment area and then enters the rear rinsing area, which can reduce the strong acid residue carried to the rear work station; combined with slow pull drying, the risk of water stain residue and secondary pollution is reduced.

[0025] 5. The cleaning time, temperature, ultrasonic power, chemical solution ratio, and number of rinsing cycles are set electronically, so that similar crucibles can be processed according to the corresponding process parameters; the water resistivity test results trigger rewashing or subsequent drying, reducing the differences caused by relying solely on human experience, and improving the consistency of batch cleaning and the controllability of the process. Attached Figure Description

[0026] To more clearly illustrate the technical solutions in the embodiments of this application or the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments of this application. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0027] Figure 1 This is a schematic flowchart of a crucible cleaning method provided in this application; Figure 2 This is a schematic diagram of the overall layout structure of a crucible cleaning device provided in this application; Figure 3 This is a side view of a crucible cleaning device provided in this application; Figure 4 This is a schematic diagram of the structure of the loading and unloading section and the material frame of a crucible cleaning device provided in this application; Figure 5 This is a schematic diagram of the pickling tank of a crucible cleaning device provided in this application; Figure 6 for Figure 5 Sectional view of position AA in the middle; Figure 7 The crucible cleaning device provided in this application In the diagram: 1. Frame; 2. Loading station; 3. First partition; 4. Pickling tank; 5. Rapid rinsing tank; 6. Second partition; 7. First ultrasonic tank; 8. Second ultrasonic tank; 9. Slow pull tank; 10. Unloading station; 11. Transport mechanism; 12. FFU filter; 13. Water resistivity sensor; 14. Automatic tank cover; 15. Up and down vibration mechanism; 16. Ultrasonic vibrating plate; 17. PFA heater; 18. Material frame base; 19. 20. Guide rail; 21. Vibration drive wheel; 22. Vibration drive linkage; 23. Overflow trough; 24. Spray pipe; 25. Quick drain valve; 26. Horizontal moving assembly; 27. Vertical lifting assembly; 28. Picking and placing part; 29. ​​Water inlet; 30. Drain valve; 31. Material frame; 32. Connecting part; 33. Tank side exhaust port; 34. Exhaust duct; 35. Medicine tank; 36. Electrical cabinet; 37. Piping area; 38. Tank cover drive cylinder; 39. Pickling tank exhaust port. Detailed Implementation

[0028] The technical solutions of the embodiments of this application will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the embodiments of this application, and not all embodiments. Based on the embodiments of this application, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the protection scope of the embodiments of this application.

[0029] In the description of the embodiments of this application, it should be noted that the terms "center," "upper," "lower," "left," "right," "vertical," "horizontal," "inner," and "outer," etc., indicate the orientation or positional relationship based on the orientation or positional relationship shown in the accompanying drawings. They are only for the convenience of describing the embodiments of this application and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation. Therefore, they should not be construed as limitations on the embodiments of this application. In addition, the terms "first," "second," and "third" are used for descriptive purposes only and should not be construed as indicating or implying relative importance.

[0030] In the description of the embodiments of this application, it should be noted that, unless otherwise explicitly specified and limited, the terms "installation," "connection," and "linking" should be interpreted broadly. For example, they can refer to a fixed connection, a replaceable connection, or an integral connection; they can refer to a mechanical connection or an electrical connection; they can refer to a direct connection or an indirect connection through an intermediate medium; and they can refer to the internal connection of two components. Those skilled in the art can understand the specific meaning of the above terms in the embodiments of this application based on the specific circumstances.

[0031] The indium phosphide crucible described in this application refers to a crucible used in processes such as indium phosphide crystal growth, and its body can be made of materials such as quartz or silicon carbide. The cleaning targets include residual indium phosphide microcrystals, indium oxide, elemental phosphorus, other phosphides, and deposits formed at high temperatures on the crucible.

[0032] The water resistivity mentioned in this application is a parameter used to characterize the electrical conductivity of the rinsing solution, and in this application, it serves as a process criterion for determining whether to proceed to the rewashing process or the subsequent drying process. The slow-pull drying refers to a drying process in which the crucible is gradually lifted off the liquid surface through controlled, slow lifting, thus removing the surface liquid film.

[0033] This application discloses a crucible cleaning method and equipment.

[0034] Please see Figure 1 as well as Figure 2 An embodiment of a crucible cleaning method provided in this application includes the following steps: S1, the material frame 30 containing the indium phosphide crucible to be cleaned is loaded and sent to the front-end processing area to perform acid washing on the indium phosphide crucible.

[0035] Specifically, this step involves loading and pickling. The indium phosphide crucible to be cleaned is loaded into the material frame 30, which supports the crucible. The material frame 30 is then sent to the pre-processing area for pickling.

[0036] The material frame 30 is used to enable the crucible to be transferred as a transport unit between different workstations. The same material frame 30 can load a corresponding number of crucibles according to its load-bearing capacity and crucible size. During loading, the surface to be cleaned can be in contact with the cleaning medium, and the obstruction between crucibles can be avoided to prevent the cleaning medium from reaching the relevant surface.

[0037] Pickling is used to bring the pickling solution into contact with residues on the crucible, promoting the dissolution or loosening of residues that can react with the selected pickling solution, and creating conditions for subsequent rinsing and washing. The choice of pickling solution should be compatible with the crucible material and the deposits to be removed, so that the cleaning action is concentrated on the residues that need to be removed.

[0038] The pretreatment area is used to accommodate the pickling and rapid rinsing processes after pickling. Arranging the above two processes in the same pretreatment area allows the pickled material frame 30 to complete the removal of residual chemicals before being transferred to the subsequent rinsing area.

[0039] S2, the pickled material frame 30 is quickly rinsed in the front-end processing area to remove residual acid carried by the material frame 30 and the indium phosphide crucible.

[0040] Specifically, this step involves a rapid rinsing process in the pretreatment area. After pickling, the material frame 30 is transferred to the rapid rinsing position in the pretreatment area for a rapid rinse of both the material frame 30 and the crucible.

[0041] When the material frame 30 and the crucible leave the pickling solution, their surfaces and local gaps may carry acid. Rapid rinsing involves contacting the rinsing medium with the aforementioned carryover solution to reduce the concentration of residual acid and remove loose residues and particles from the corresponding surfaces.

[0042] The material frame 30 itself is also subject to rapid rinsing. The material frame 30 carries the crucible between different workstations, and if a significant amount of acid remains on its surface, it may carry acid into subsequent workstations. Therefore, rinsing the material frame 30 simultaneously with rinsing the crucible can reduce the amount of acid carried over by the carrying tool.

[0043] The rapid rinsing is completed in the pre-treatment area, leaving the unrinsed pickling material frames 30 in the pre-treatment area. This spatial arrangement, coordinated with the rinsing sequence, provides a basis for controlling the separation between the pre-treatment area and the subsequent rinsing area.

[0044] S3. After the material frame 30 completes the rapid rinsing, open the partition between the front treatment area and the rear rinsing area, send the material frame 30 into the rear rinsing area for ultrasonic rinsing, and restore the partition after the material frame 30 passes through.

[0045] Specifically, this step involves completing a rapid rinse and then transferring the material to the subsequent rinsing zone. A partition that can be opened and closed is installed between the pre-treatment zone and the subsequent rinsing zone. After the pickled material frame 30 completes a rapid rinse, the partition is opened, and the material frame 30 is sent to the subsequent rinsing zone. The partition is then closed after the material frame 30 has passed through.

[0046] The partition here restricts direct communication between two areas when the material frame 30 does not need to move across areas, and opens the corresponding passage when the material frame 30 needs to be transferred across areas. By connecting the opening of the partition with the completion of rapid rinsing, the situation where unrinsed pickling material frames 30 directly enter the subsequent workstations can be reduced.

[0047] The aforementioned pre-rinsing and subsequent transfer control refers to the forward transfer of the pickled material frame 30 to the subsequent rinsing zone. After the material frame 30 enters the subsequent rinsing zone, the partition is restored, thus suppressing the diffusion of acid mist generated during the preceding pickling process into the subsequent zone.

[0048] S4, detect the water resistivity of the rinsing solution at the end of ultrasonic rinsing, and compare the detection result with the preset water resistivity threshold.

[0049] Specifically, this step involves ultrasonic rinsing. The material frame 30 is placed in the rinsing solution in the subsequent rinsing zone, and the crucible is ultrasonically rinsed.

[0050] When ultrasound is applied to the rinsing solution, it promotes contact between the rinsing solution and the crucible surface, and facilitates localized liquid renewal, further treating particles and contaminants remaining after acid washing and rapid rinsing. The rinsing solution also replaces residual chemicals on the crucible surface, seamlessly connecting the initial decontamination process with the subsequent fine rinsing.

[0051] Pickling, rapid rinsing, and ultrasonic rinsing serve to treat adhering substances, initially remove residual acid and loose particles, and further remove subsequent residues, respectively. These steps, in the order of processing, work together to improve the cleanliness of the crucible.

[0052] S5. When the test result is less than the preset water resistivity threshold, the material frame 30 is returned to the front-end processing area for pickling, quick rinsing and ultrasonic rinsing.

[0053] Specifically, this step involves detecting the water resistivity and determining the subsequent processing path. At the end of the ultrasonic rinsing, the water resistivity of the rinsing solution is measured, and the result is compared with a preset water resistivity threshold.

[0054] The preset water resistivity threshold is a process judgment value determined based on the rinsing process and cleaning requirements adopted. The water resistivity data used during testing should have corresponding measurement conditions with this judgment value so that the comparison results can be used for process judgment.

[0055] Ionic contaminants in the rinsing solution can affect its electrical conductivity. Under given rinsing process conditions, water resistivity detection can provide feedback for the control of residual conductive contaminants. This application combines this feedback with the already performed pickling, rapid rinsing, and ultrasonic rinsing processes to determine the subsequent processing path of the material frame 30.

[0056] When the test result is less than the preset water resistivity threshold, the control box 30 returns to the front-end processing area and restarts the pickling process, sequentially completing pickling, rapid rinsing, and ultrasonic rinsing again. After the re-rinsing is completed, the subsequent processing is determined based on the corresponding test results.

[0057] During the rewashing process, the crucible is returned to the pickling process to allow it to be treated again for any remaining residues. After that, the residual chemicals are replaced and rinsed, forming a cleaning process with feedback.

[0058] When the test result is greater than or equal to the preset water resistivity threshold, the material frame 30 is allowed to enter the subsequent drying process. In this way, the process release is linked to the readable test result, reducing the discrepancies caused by relying solely on manual observation or experience.

[0059] S6. When the detection result is greater than or equal to the preset water resistivity threshold, the material frame 30 is sent to the drying station for slow drying, and the dried material frame 30 is unloaded.

[0060] Specifically, this step involves slow drying and unloading. The material frame 30, having met the set process criteria, is fed into the drying station. The crucible is gradually lifted off the liquid surface, and the surface liquid film is removed during this process. After drying is complete, the material frame 30 is moved to the unloading position.

[0061] Slow lifting allows for controlled relative movement between the crucible surface and the liquid surface, enabling the liquid film removal process to proceed gradually along the crucible surface. When combined with appropriate drying media and conditions, the lifting process helps reduce surface water carryover and residual water stains.

[0062] The drying process is arranged after rinsing and inspection, so that the material frame 30 that does not meet the set process criteria is returned to the cleaning process first, reducing the situation where unqualified material frames 30 directly enter the drying station.

[0063] Following the steps described above, the material frame 30 can complete the cleaning process from loading to unloading in a predetermined processing sequence, and perform a rewashing branch based on the water resistivity detection results. Figure 1 The main process flow through each step is shown, and the rewashing branch is implemented through detection and return control in this embodiment.

[0064] like Figure 2 as well as Figure 3As shown, this embodiment also provides a crucible cleaning device, including a frame 1, a conveying mechanism 11, a control unit, a loading station 2, an acid pickling tank 4, a rapid rinsing tank 5, an ultrasonic rinsing assembly, a slow pull tank 9, and a unloading station 10.

[0065] The frame 1 provides the mounting foundation for each process tank and related mechanism, enabling the equipment to form a cohesive whole. The loading station 2 receives the material frame 30 containing the crucibles to be cleaned, and the unloading station 10 receives the material frame 30 after cleaning and drying.

[0066] Pickling tank 4 is used to contain the pickling solution and provide space for the crucible to perform pickling. Rapid rinsing tank 5 is located at the post-processing position of pickling tank 4 and is used to receive the pickled material frame 30 and remove residual solution and loose particles carried on it.

[0067] Pickling tank 4 and rapid rinsing tank 5 are located in the front-end treatment area, while the ultrasonic rinsing assembly is located in the rear-end rinsing area. This division between the front-end treatment area and the rear-end rinsing area allows the initial removal of pickling and residual chemicals after pickling to be completed in the front-end, while the rear-end rinsing assembly handles the subsequent rinsing.

[0068] The slow-pull tank 9 is located at the post-processing position of the ultrasonic rinsing assembly and is used to complete the slow-pull drying of the crucible. The material frame 30 is transferred between each station and between each tank via the conveying mechanism 11, reducing manual handling of each tank.

[0069] A first partition 3 is installed between the loading station 2 and the front processing area, and a second partition 6 is installed between the front processing area and the rear rinsing area. The first partition 3 is used to restrict the direct connection between the front processing area and the loading station, and the second partition 6 is used to restrict the direct connection between the front processing area and the rear rinsing area.

[0070] Two partitions are located on the feed side and discharge side of the front-end processing area, respectively, placing the pickling tank 4 and the rapid rinsing tank 5 between the two partitions. When the material frame 30 is transferred between zones, the corresponding partition opens; after the transfer is completed, the corresponding partition closes.

[0071] The conveying mechanism 11 has the capability to remove the material frame 30 from one processing position and send it to another processing position. It can move the material frame 30 in the normal process direction and return the material frame 30 to the pickling tank 4 when rewashing is required. The material frame 30 carries the crucible during conveying, reducing the need for repeated gripping of the crucible body.

[0072] The ultrasonic rinsing assembly is equipped with a water resistivity sensor 13, which is used to detect the water resistivity of the final rinsing solution. The final rinsing solution refers to the rinsing solution used in the last stage of rinsing before the material frame 30 completes ultrasonic rinsing and is ready to enter the drying process.

[0073] The control unit receives the detection signal from the water resistivity sensor 13 and outputs corresponding control signals to the conveying mechanism 11 and the partition. The control unit can move the material frame 30 in the sequence of feeding, pickling, rapid rinsing, ultrasonic rinsing, slow drying and unloading according to the preset processing program.

[0074] For the second partition 6, the control unit sets the rapid rinsing of the material frame 30 as a process condition for its forward entry into the subsequent rinsing zone. After the pickled material frame 30 is rinsed in the rapid rinsing tank 5, the second partition 6 opens, the conveying mechanism 11 drives the material frame 30 into the subsequent rinsing zone, and then the second partition 6 closes.

[0075] To determine the cleaning results, the control unit compares the detection result of the water resistivity sensor 13 with a preset threshold. When the detection result is lower than the preset threshold, the control conveying mechanism 11 returns the material frame 30 to the pickling tank 4 and re-executes the corresponding cleaning procedure; when the detection result reaches the preset threshold, the control conveying mechanism 11 sends the material frame 30 into the slow pull trough 9.

[0076] Therefore, the equipment in this embodiment can realize the forward processing flow and rewashing flow in the cleaning method through workstation layout, partition control, automatic handling, and water resistivity feedback. The spatial partition of the front-end processing area, combined with the pre-rinse and post-transfer mechanism, reduces the impact of acid and acid mist on the subsequent rinsing area; the detection results, combined with the handling path, enable the rewashing to be completed inside the equipment.

[0077] The above is Embodiment 1 of a crucible cleaning method and apparatus provided in this application. The following is Embodiment 2 of a crucible cleaning method and apparatus provided in this application. Please refer to the following for details. Figures 2 to 7 .

[0078] Based on the solution of Embodiment 1 above: Furthermore, such as Figure 2 as well as Figure 5 As shown, during the pickling process, the material frame 30 is placed into the pickling tank 4 so that the pickling solution contacts the surface of the crucible to be cleaned, and the automatic tank cover 14 of the pickling tank 4 is closed.

[0079] After the automatic tank cover 14 is closed, the pickling solution is heated and ultrasonically treated, while the material frame 30 vibrates up and down. Heating improves the treatment conditions of the corresponding solution on the deposits, ultrasonic waves promote local cleaning, and up-and-down vibration causes relative movement between the crucible and the surrounding solution, promoting the renewal of the liquid near the crucible surface.

[0080] For firmly attached microcrystalline residues and oxides on the inner wall of the crucible, the liquid first comes into contact with them, and the residues are loosened by heating and ultrasound. Then, the loosened parts are separated from the crucible surface by the up-and-down reciprocating motion of the material frame 30, and new liquid continues to contact the corresponding position.

[0081] The up-and-down oscillation causes controlled displacement of the entire crucible via the material frame 30. The oscillation amplitude and operating state are adapted to the crucible's load-bearing method, keeping the crucible stable within the material frame 30 and reducing mutual collisions. The ultrasonic power and processing time are also set according to the crucible material and deposits to achieve a cleaning effect suitable for the corresponding crucible.

[0082] The automatic tank cover 14 covers the tank opening during pickling, which helps to reduce the direct escape of acid mist from the tank opening during heating and liquid movement. After pickling is completed, the automatic tank cover 14 is opened, and the conveying mechanism 11 removes the material frame 30 from the pickling tank 4 and then transfers it to the rapid rinsing tank 5.

[0083] Furthermore, such as Figure 2 as well as Figure 7 As shown, the rapid rinsing adopts QDR rapid rinsing. QDR rapid rinsing removes acid and particles carried on the surface of the crucible and material frame 30 through a combination of ultrapure water supply, overflow replacement, spraying and rapid liquid drainage.

[0084] After the material frame 30 enters the rapid rinsing tank 5, ultrapure water is supplied into the tank, allowing the ultrapure water to contact the inner and outer surfaces of the crucible and the surface of the material frame 30. As ultrapure water is continuously supplied, the liquid in the tank is discharged through the overflow structure at the top, thereby continuously replacing the liquid in the tank.

[0085] During the overflow replacement process, ultrapure water is sprayed onto the material frame 30 and the crucible through a spray structure. The spray can rinse all accessible surfaces and gaps, and in conjunction with the liquid replacement in the tank, it reduces the retention of residual chemicals in certain areas.

[0086] When performing the rapid drainage action, the quick-drain valve 24 located at the bottom of the tank is opened to quickly drain the liquid in the tank carrying acid and particles. According to the set process, the corresponding water supply, spraying and drainage actions can be performed in one rapid rinsing process, and the rinsing can be completed according to the set number of times.

[0087] Overflow displacement continuously reduces the concentration of residual reagent in the tank; spraying promotes the removal of surface-carrying liquid; and rapid drainage shortens the residence time of contaminated liquid in the tank. These combined effects improve reagent displacement in localized areas of the crucible and within the gaps of the material frame 30.

[0088] After the material frame 30 completes the set QDR rapid rinsing program, the second partition 6 is opened to allow it to enter the subsequent rinsing area. This sequence creates a clear process connection between pickling, rapid rinsing, and subsequent rinsing.

[0089] Furthermore, such as Figure 2 As shown, ultrasonic rinsing includes a first ultrasonic rinsing and a second ultrasonic rinsing, which are performed in the first ultrasonic tank 7 and the second ultrasonic tank 8, respectively.

[0090] After being quickly rinsed by QDR, the material frame 30 first enters the first ultrasonic tank 7. The first ultrasonic tank 7 rinses away the particles and other materials remaining after the previous treatment. Then, the material frame 30 enters the second ultrasonic tank 8 for another ultrasonic rinse.

[0091] The two-stage rinsing is carried out in different tanks, allowing the material frame 30 to enter the subsequent rinsing environment after completing the first stage of treatment. Through this tiered treatment, the impact of surface residues and carried-over substances on subsequent processes can be gradually reduced.

[0092] The ultrasonic rinsing in this embodiment targets the removal of tiny particles, including cleaning impurities with a particle size of 0.1 micrometers or larger. The specific removal effect is related to the particle adhesion state, crucible geometry, ultrasonic parameters, rinsing time, and water quality conditions, and appropriate parameters can be determined according to the actual process.

[0093] A water resistivity sensor 13 is installed in the second ultrasonic tank 8 to obtain the water resistivity of the liquid used in the second ultrasonic rinsing. The object of detection is the rinsing liquid after the subsequent rinsing stage, so that the detection result corresponds to the rinsing state before drying.

[0094] If the test result does not reach the preset water resistivity threshold after the second ultrasonic rinsing is completed, the rewashing program is started, and the material frame 30 is returned to the pickling tank 4 for pickling, QDR rapid rinsing, first ultrasonic rinsing and second ultrasonic rinsing again.

[0095] After being washed, the material frame 30 still needs to be tested at the second ultrasonic tank 8, and the subsequent path is determined based on the test results. Through this process, the material frame 30 entering the slow-pull drying process is judged by the corresponding rinsing process each time.

[0096] Furthermore, slow drying is carried out in slow drying tank 9, and the process media used include ultrapure water and IPA.

[0097] IPA stands for isopropanol. The pure water supply system provides ultrapure water to the slow-pull tank 9, the IPA supply system provides isopropanol to the slow-pull tank 9, and the heating element is used to regulate the drying temperature of the slow-pull tank 9.

[0098] During slow-pull drying, the material frame 30 is placed in the processing position of the slow-pull tank 9, and then the material frame 30 is slowly raised so that the surface of the crucible gradually passes over the liquid surface. Utilizing the effect of isopropanol on the surface tension near the liquid surface, a surface tension gradient is formed in the corresponding interface region, thereby generating the Marangoni effect, which causes the attached liquid film to retreat into the tank.

[0099] The lifting speed during the slow-pull process is coordinated with the medium supply and temperature conditions, allowing the liquid film removal process to be completed gradually as the crucible is raised. This drying process helps reduce water stains formed by in-situ evaporation of residual moisture on the crucible surface and reduces environmental exposure caused by prolonged natural drying.

[0100] In this embodiment, the effect of isopropanol is related to the surface tension gradient near the liquid surface, and the specific supply state should be adapted to the drying mechanism. The temperature, isopropanol dosage, and lifting speed of the slow-pull tank 9 are determined based on the actual crucible and drying process.

[0101] When loading the crucible, it should be designed to allow for drainage of the liquid inside, enabling the surface liquid film treated during the slow pulling process to recede and reducing the impact of liquid accumulation inside the crucible on drying. The specific placement of the crucible is determined based on its shape and the structure of the material frame 30.

[0102] By combining slow drying with a clean environment inside the equipment, the risk of water stains and secondary pollution can be reduced, and the changes in surface condition caused by long-term residual moisture can be minimized.

[0103] Furthermore, such as Figure 5 as well as Figure 6 As shown, the pickling tank 4 includes a tank body and an automatic tank cover 14 that cooperates with the tank body, an up-and-down oscillation mechanism 15, an ultrasonic vibration plate 16, and a pickling heating device.

[0104] The tank is used to hold the pickling solution and provides space for the material frame 30 to enter, soak, and agitate vertically. The tank's capacity is adapted to the size of the material frame 30 and its vertical movement range, allowing the material frame 30 to move to the required cleaning position.

[0105] The automatic tank cover 14 is driven by the tank cover drive cylinder 37 to flip relative to the pickling tank 4. In the illustrated structure, flip-able tank cover parts are respectively provided on both sides of the tank opening, and the corresponding tank cover drive cylinder 37 drives the tank cover part to open or close through telescopic movement.

[0106] When the tank cover is open, it provides a passage for the material frame 30 to enter and exit the pickling tank 4; after the material frame 30 is placed in place, the tank cover closes, covering the upper opening of the pickling tank 4. The tank cover drive cylinder 37 enables the opening and closing action to be coordinated with the handling and pickling process, reducing the need for manual operation near the tank opening.

[0107] The opening and closing of the trough cover and the placement and removal of the material frame 30 are coordinated in time. When placing the material frame 30, the trough cover is opened first, and then the conveying mechanism 11 places the material frame 30 in the bearing position inside the trough; after the conveying mechanism 11 completes the placement and withdraws from the area affecting the closing of the trough cover, the trough cover is closed. When removing the material frame 30, the trough cover is opened first, and then the material is removed.

[0108] The ultrasonic transducer 16 is located at the bottom of the pickling tank 4. The ultrasonic waves it generates act on the pickling solution in the tank, allowing the ultrasonic waves in the solution to be transmitted to the surface of the crucible. The bottom arrangement separates the ultrasonic transducer 16 from the upper and lower transport channels of the material frame 30, facilitating the loading and unloading operations above the tank.

[0109] The pickling heating device is located around the pickling tank 4 and includes a PFA heater 17. The PFA heater 17 is used to heat the pickling solution under suitable conditions. The arrangement around the tank facilitates the supply of heat to the solution around the material frame 30.

[0110] The heating device and the ultrasonic vibrating plate 16 provide thermal and ultrasonic effects, respectively, while the upper and lower oscillation mechanism 15 provides relative motion between the material frame 30 and the chemical solution. These three components work together in the same pickling process, ensuring controllable processing conditions.

[0111] The up-and-down oscillation mechanism 15 includes a material frame 30 base 18, a guide rail 19, an oscillation drive wheel 20, and an oscillation drive linkage 21. The material frame 30 base 18 is located inside the pickling tank 4 and is used to support the material frame 30 from below, so that the material frame 30 and the material frame 30 base 18 move up and down together.

[0112] The guide rail 19 is used to constrain the movement direction of the relevant bearing parts of the base 18 of the material frame 30, so that it mainly reciprocates in the vertical direction. Through the guiding constraint, the uncontrolled lateral swaying of the material frame 30 during oscillation is reduced, so that the material frame 30 and the crucible maintain a relatively stable motion state.

[0113] The oscillating drive wheel 20 is connected to a corresponding drive source and can rotate around its own axis of rotation. One end of the oscillating drive linkage 21 is connected to the eccentric position of the oscillating drive wheel 20, and the other end is connected to the connecting part 31 that drives the material frame 30 base 18 to move up and down.

[0114] When the oscillation drive wheel 20 rotates, its eccentric connection position moves around the rotation axis, the oscillation drive connecting rod 21 moves accordingly, and pushes or pulls the connecting part 31 to move up and down along the guide rail 19, thereby driving the base 18 of the material frame 30 and the material frame 30 to oscillate up and down.

[0115] Through the cooperation of the oscillating drive wheel 20, the oscillating drive linkage 21, and the guide rail 19, the rotational motion is converted into a guided reciprocating motion. The base 18 of the material frame 30 bears the weight and motion transmission of the material frame 30, so that the crucible in the material frame 30 can receive the corresponding oscillation action along with the material frame 30.

[0116] The relevant oscillation drive components are arranged on the outside of the pickling tank 4, and drive the base 18 of the material frame 30 inside the tank through a connecting structure. This arrangement facilitates the formation of a drive and guide installation space on the outside of the tank, while reserving space for the treatment of the chemical solution inside the tank.

[0117] The travel of the base 18 of the material frame 30 is adapted to the internal space of the pickling tank 4, so that the material frame 30 maintains the necessary distance between itself and the ultrasonic vibrating plate 16 and the tank body during the vibration process. The base 18 of the material frame 30 is mainly used to support and transmit motion. The liquid-passing structure of the material frame 30 allows the liquid to enter the interior of the material frame 30 and contact the crucible.

[0118] Pickling tank 4 is also equipped with a water inlet 28 and a drain valve 29. The water inlet 28 is used to replenish the tank with the water required for the corresponding process, and the drain valve 29 is used to drain the liquid in the tank during liquid change or tank maintenance. The above interfaces are coordinated with the piping layout of the equipment to ensure that liquid replenishment and drainage of the tank can be carried out in accordance with process requirements.

[0119] Furthermore, such as Figure 7 As shown, the rapid rinsing tank 5 is a QDR rinsing tank, which includes a tank body for accommodating the material frame 30, an ultrapure water supply structure, an overflow tank 22, a spray pipe 23, and a rapid drain valve 24.

[0120] The ultrapure water supply structure is used to deliver ultrapure water into the tank. As the liquid level in the tank rises, the liquid enters the overflow tank 22 from the upper overflow position and leaves the rapid rinsing tank 5 through the corresponding discharge passage.

[0121] An overflow tank 22 is located at a corresponding position on the upper periphery of the tank body to receive overflowing liquid. By continuously supplying ultrapure water and discharging the overflow liquid, the liquid in the tank is renewed, and the residual acid around the material frame 30 and crucible is gradually replaced.

[0122] The spray pipe 23 is located at the top of the tank and faces the material frame 30 inside the tank. In the illustrated structure, there are spray positions on both sides of the material frame 30 facing the material frame 30, so that the spray water can enter the area where the material frame 30 is located from the side and above.

[0123] The spray water acts on the material frame 30 and the reachable crucible surface, helping to remove adhering liquid and allowing detached particles to enter the tank liquid with the rinsing water. The liquid passage openings on the side wall of the material frame 30 provide a path for both the spray water and the tank liquid.

[0124] The quick-drain valve 24 is located on the drainage passage at the bottom of the tank. When the quick-drain valve 24 is opened, the liquid in the tank is discharged through the bottom passage, allowing residual medicine and particles to leave the tank with the discharged liquid.

[0125] By combining top overflow with rapid bottom drainage, both continuous replacement and rapid overall drainage according to a program can be achieved. The spray structure provides supplementary rinsing to the surface during the corresponding rinsing stages, thus combining the renewal of the liquid inside the tank with the removal of surface-carrying liquid.

[0126] Both the rapid rinsing tank 5 and the pickling tank 4 are located between the first partition 3 and the second partition 6. When the material frame 30 is transferred from the pickling tank 4 to the rapid rinsing tank 5, it does not need to enter the subsequent rinsing area first, thus the initial removal of residual acid can be completed while maintaining the separation between the front and rear areas.

[0127] Furthermore, such as Figure 2 As shown, the ultrasonic rinsing assembly includes a first ultrasonic tank 7 and a second ultrasonic tank 8, which are arranged sequentially along the normal processing order of the material frame 30.

[0128] The first ultrasonic tank 7 receives the material frame 30 after QDR rapid rinsing, and the second ultrasonic tank 8 receives the material frame 30 after the first ultrasonic rinsing. The two tanks respectively provide the corresponding rinsing space and ultrasonic action conditions.

[0129] Each ultrasonic tank promotes the detachment of residual particles through ultrasonic waves, and further replaces the surface-carrying liquid with rinsing solution. This two-stage treatment allows any residues that may remain after the initial cleaning to be continuously rinsed.

[0130] A water resistivity sensor 13 is installed in the second ultrasonic tank 8, and its detection part is in contact with the rinsing liquid in the second ultrasonic tank 8, and is used to output the water resistivity signal of the rinsing liquid to the control unit.

[0131] The water resistivity sensor 13 is positioned corresponding to the object it detects, so that the signal it acquires reflects the state of the rinsing liquid after the first rinsing of the material frame 30. The control unit performs process judgment based on this signal and controls the conveying mechanism 11 to select either returning to the pickling tank 4 or transferring to the slow-pulling tank 9.

[0132] The second ultrasonic tank 8 is used as the detection location, ensuring that the process judgment occurs after the two-stage rinsing. The material frame 30 only enters the slow-pulling tank 9 after undergoing the predetermined rinsing process and meeting the set process criteria.

[0133] Furthermore, the slow-pull tank 9 is equipped with a heating component, an IPA dispensing system, and a pure water dispensing system, which are used to provide drying temperature conditions, isopropanol, and ultrapure water, respectively.

[0134] The pure water addition system supplies ultrapure water to the slow-pull tank 9, creating a liquid environment for the slow-pull process in the feed frame 30 and crucible. The IPA addition system provides isopropanol to the slow-pull tank 9, allowing it to participate in the surface tension regulation near the liquid surface.

[0135] The heating element is used to regulate the temperature conditions of the slow-pull trough 9 to adapt it to the corresponding medium supply and slow-pull process. The operating parameters of the heating element are set according to the specific process and together with the material frame 30 lifting process determine the drying state.

[0136] The conveying mechanism 11 can feed the material frame 30 into the slow-pull trough 9 and drive the material frame 30 to rise at a speed suitable for slow-pull drying. By performing controlled lifting on the same conveying mechanism, the transfer of the material frame 30 and the slow-pull lifting can be connected in a unified motion system.

[0137] As the material frame 30 rises slowly, the surface of the crucible gradually passes over the liquid surface, and the liquid film recedes under the action of the surface tension gradient. After the lifting and corresponding drying processes are completed, the conveying mechanism 11 moves the material frame 30 to the unloading station 10.

[0138] This structure allows the rinsed crucible to continue drying inside the equipment, reducing the need for manual transfer to an external drying location after rinsing and helping to maintain the surface condition after cleaning.

[0139] Furthermore, such as Figure 3 As shown, frame 1 is made of 304 stainless steel and is covered with PP board on the outside of the frame.

[0140] The 304 stainless steel frame provides support for the tank, the handling mechanism 11, and other components, ensuring the rigidity required for the overall installation and operation of the equipment. The PP sheet, made of polypropylene, forms the outer protective structure, providing the metal frame and related internal components with protection suitable for the cleaning environment.

[0141] The frame and the outer PP sheet together constitute the overall support and enclosure structure of the equipment. The process tanks are arranged in the corresponding areas of the frame 1, and the conveying mechanism 11 is set along the arrangement direction of the workstations, so that each process can be connected within the same equipment.

[0142] The first partition 3 is the first automatic lifting door, and the second partition 6 is the second automatic lifting door. The first automatic lifting door is located between the loading station 2 and the pickling tank 4, and the second automatic lifting door is located between the rapid rinsing tank 5 and the first ultrasonic tank 7.

[0143] The lifting door opens or closes the area through which the material frame 30 passes by moving up and down. When closed, it creates a barrier between adjacent areas; when open, it allows the material frame 30 and the relevant pick-and-place parts of the conveying mechanism 11 to pass through their respective positions.

[0144] The first automatic lifting door reduces gas exchange between the pickling area and the feeding area, while the second automatic lifting door reduces the impact of the pickling area on the subsequent ultrasonic rinsing area. The two lifting doors, in conjunction with the external enclosure structure, provide a relatively independent processing environment for the front-end treatment area.

[0145] During normal forward processing, after the material frame 30 enters the front processing area, the first automatic lifting door closes; the material frame 30 first completes pickling and QDR rapid rinsing, and then enters the rear rinsing area through the second automatic lifting door. After the material frame 30 passes through, the second automatic lifting door closes again.

[0146] During the rewashing process, the material frame 30 needs to return to the pickling tank 4 from the second ultrasonic tank 8. At this time, according to the return transport requirements, the second automatic lifting door is opened to allow the material frame 30 to pass through in reverse, and then closed after passing through. After the material frame 30 completes pickling again, it is first subjected to QDR rapid rinsing, and then enters the subsequent rinsing area according to the forward transfer procedure.

[0147] Therefore, the requirement to perform QDR quick rinsing before opening the second automatic lifting door corresponds to the forward release of the pickled material frame 30 to the rear rinsing area; the rewash return is completed according to the reverse transport procedure, and the two together achieve a repeatable cleaning process.

[0148] Furthermore, such as Figure 3 As shown, a (ultra-high efficiency) FFU filter 12 is installed on the top of rack 1. The FFU is a fan filter unit that supplies filtered air to the interior of the equipment through filtered air supply.

[0149] The filtered airflow enters the process area from the top of the equipment downwards, so that the material frame 30, crucible and related processing positions are in a controlled clean air supply environment, which helps to reduce the entry of environmental suspended particles and their adhesion to the cleaned surface.

[0150] like Figure 6 As shown, the pickling tank 4 is equipped with a pickling tank exhaust vent 38, such as... Figure 3 As shown, side exhaust vents 32 are provided on the side of the relevant water tanks, and each exhaust vent is connected to an exhaust duct 33. The exhaust vent 38 of the pickling tank is connected to the gas space above the liquid surface in the tank, and is used to collect acid mist generated during the pickling process.

[0151] The side exhaust vent 32 is used to guide gas from around the corresponding process tank into the exhaust duct 33. The top-filtered air supply, together with the exhaust vents inside and on the side of the tank, ensures that the process area receives clean air and promptly removes locally generated acid mist and moisture.

[0152] The FFU filter 12 is responsible for filtering air particles and providing clean air supply, while the exhaust structure is responsible for guiding and discharging acid mist and moisture. The two work together to control the internal environment of the equipment.

[0153] The automatic tank cover 14 reduces acid mist escaping directly from the pickling tank opening, while the first and second automatic lifting doors reduce the cross-area diffusion of acid mist. The exhaust vent and exhaust duct 33 guide the acid mist away from the corresponding area. Through the coordinated structure of the above, the corrosion of equipment by acid mist and its impact on operators can be reduced.

[0154] Furthermore, such as Figures 2 to 4 As shown, the handling mechanism 11 employs a handling robot, which includes a horizontal moving component 25, a vertical lifting component 26, and a picking and placing section 27 for picking and placing the material frame 30.

[0155] The horizontal moving component 25 extends along the arrangement direction of each station and tank in the equipment, corresponding to the X-axis of the robot arm, and is used to enable the pick-and-place unit 27 to reach the corresponding positions of the loading station 2, pickling tank 4, rapid rinsing tank 5, first ultrasonic tank 7, second ultrasonic tank 8, slow pull tank 9 and unloading station 10.

[0156] The vertical lifting component 26 corresponds to the Z-axis of the robot arm and is used to move the pick-and-place section 27 and the material frame 30 up and down, so that the material frame 30 can enter the trough, leave the trough, and be slowly lifted at the slow pull trough 9.

[0157] The pick-and-place section 27 extends from the carrying part of the handling robot to the location of the material frame 30 and cooperates with the corresponding receiving part on the upper part of the material frame 30 to form support or lift from both sides of the material frame 30, so that the material frame 30 remains stable during lifting and horizontal transfer.

[0158] The material frame 30 has an internal space for accommodating the crucible, and its side walls are provided with multiple liquid passage openings. The liquid passage openings allow pickling solution, rinsing water and washing solution to pass through the side walls of the material frame 30 into the interior, and allow the liquid to drain when the material frame 30 is removed, reducing the obstruction of the material frame 30 wall to the flow of the medium.

[0159] The receiving part at the top of the material frame 30 cooperates with the robotic arm's pick-and-place part 27, enabling the robotic arm to transport the entire material frame 30. After the material frame 30 enters the pickling tank 4, it can be supported by the base 18 of the material frame 30 and subjected to up-and-down vibration; when the material frame 30 leaves the pickling tank 4, it is then taken out by the handling robotic arm.

[0160] The horizontal moving component 25 and the vertical lifting component 26 work together to form a cross-station transport path. During transport, the vertical lifting component 26 first moves the material frame 30 away from the current tank and its surrounding structure, then the horizontal moving component 25 moves the material frame 30 to the target position, and then the vertical lifting component 26 puts the material frame 30 into the target tank.

[0161] During slow-pull drying, the vertical lifting assembly 26 operates at the corresponding slow-pull speed; during normal pick-and-place and cross-tank transport, it operates according to the corresponding transport program. Through motion control of different processes, the same transport robot can adapt to the needs of inter-tank transfer and slow-pull drying.

[0162] Furthermore, such as Figure 2 As shown, the equipment is equipped with a chemical solution tank to hold the required process chemicals and is coordinated with the relevant chemical solution supply layout. The equipment also includes an electrical cabinet 35 and a piping area 36, ​​with the electrical cabinet 35 located at the top and the piping area 36 located at the bottom.

[0163] The electrical cabinet 35 is used to house control and electrical connection components, while the piping area 36 is used to arrange corresponding pipelines for liquid supply and drainage. This layout allows the process tank, handling robot, and electrical and piping components to form corresponding installation areas within the frame 1, facilitating connection and maintenance between various systems.

[0164] The control unit can control the time and actions of each process according to the cleaning procedure, including material frame 30 handling, tank cover opening and closing, lifting door opening and closing, pickling heating, ultrasonic treatment, up and down vibration, QDR rinsing, rinsing detection and slow pull lifting.

[0165] Cleaning time, temperature, ultrasonic power, chemical solution ratio, and rinsing cycles are settable process parameters and managed electronically. Different batches of the same type of crucible can use the same parameter configuration to maintain consistent process conditions; for crucibles of different materials, sizes, or residual states, appropriate parameter configurations can be used.

[0166] Among them, the setting of the drug solution ratio is matched with the drug solution supply configuration adopted by the equipment, the cleaning temperature is matched with the heating device, the ultrasonic power is matched with the ultrasonic action component, and the number of rinsing cycles is matched with the execution program of rapid rinsing and ultrasonic rinsing.

[0167] A preset water resistivity threshold is used to control the destination of the final rinse. This threshold is adapted to the actual rinsing process and is set in conjunction with predetermined detection conditions so that the detection results can be stably used for rewashing and drying release judgment.

[0168] In general, the crucible cleaning equipment of this embodiment can be operated according to the following process.

[0169] First, the indium phosphide crucible to be cleaned is loaded into the material frame 30, and the material frame 30 is placed at the loading station 2. The equipment operates according to the set program, with top-filtered air supply and corresponding exhaust, to create a suitable environment for cleaning in the process area.

[0170] The first automatic lifting door opens, and the handling robot picks up the material frame 30 from the loading station 2. Through the cooperation of the horizontal moving component 25 and the vertical lifting component 26, the material frame 30 is sent into the front-end processing area. After the material frame 30 enters, the first automatic lifting door closes.

[0171] The automatic tank cover 14 of the pickling tank 4 opens, and the handling robot places the material frame 30 onto the material frame 30 base 18 inside the pickling tank 4, and then exits the area that affects the opening and closing of the tank cover and vibration. After the automatic tank cover 14 closes, pickling heating and ultrasonic treatment are carried out according to the set conditions.

[0172] The oscillating drive wheel 20 rotates, which drives the base 18 of the material frame 30 to move up and down along the guide rail 19 via the eccentrically connected oscillating drive linkage 21. The material frame 30 and the crucible inside it then oscillate in the liquid medicine. The action of the liquid medicine, the action of ultrasound, and the up-and-down motion work together to promote the removal of the attached substances.

[0173] After pickling is completed, the up-and-down oscillation mechanism 15 is stopped at a suitable position for material picking, the automatic tank cover 14 is opened, the material frame 30 is taken out by the handling robot, and the material frame 30 is moved into the QDR rinsing tank.

[0174] The QDR rinsing tank supplies ultrapure water to the material frame 30 and crucible, removing residual acid and loose particles through continuous overflow replacement, spraying, and rapid drainage. This process is completed in the front-end treatment area, and the second automatic lifting door maintains a corresponding isolation state until the material frame 30 has completed its rapid rinsing.

[0175] After the set QDR rinsing is completed, the second automatic lifting door opens. The handling robot sends the material frame 30 into the subsequent rinsing area, and then the second automatic lifting door closes.

[0176] The material frame 30 sequentially enters the first ultrasonic tank 7 and the second ultrasonic tank 8 to complete two-stage ultrasonic rinsing. The water resistivity sensor 13 in the second ultrasonic tank 8 acquires the water resistivity of the corresponding rinsing solution and sends the detection result to the control unit.

[0177] If the test result is less than the preset water resistivity threshold, the control unit initiates the rewashing procedure. The handling robot removes the material frame 30 from the second ultrasonic tank 8, follows the return path through the second automatic lifting door into the pre-treatment area, and then sends it back into the pickling tank 4. Afterward, pickling, QDR rapid rinsing, and two-stage ultrasonic rinsing are performed sequentially.

[0178] If the detection result is greater than or equal to the preset water resistivity threshold, the control unit allows the material frame 30 to enter the slow-pull tank 9. The slow-pull tank 9 provides the corresponding drying conditions through a pure water addition system, an IPA addition system, and a heating component. The handling robot slowly lifts the material frame 30, causing the crucible to gradually detach from the liquid surface, and the surface liquid film is removed by utilizing the Marangoni effect.

[0179] After drying, the handling robot sends the material frame 30 to the unloading station 10 to complete the processing of the crucible loaded in the material frame 30.

[0180] During the above process, the material frame 30 is automatically transferred between the pickling, rinsing, washing and drying stations, reducing manual operation in each tank; the material frame 30 that needs to be washed again returns to the front-end processing area according to the test results, and the material frame 30 that has been washed again still performs the same rinsing, washing and testing procedures.

[0181] This embodiment aims to replace the step-by-step operations of manual knocking to remove slag, manual soaking, manual rinsing, and natural air drying, and its design goal is to improve cleaning efficiency by more than 3 times compared to the corresponding manual treatment methods. The actual efficiency is related to the batch loading quantity, the time of each process, the state of crucible residue, the frequency of rewashing, and the connection between workstations, and can be determined according to the actual production cycle.

[0182] In terms of crucible protection, damage caused by direct impact is reduced through the use of chemical solutions, controlled mechanical vibration, and appropriate ultrasonic treatment. In terms of cleanliness control, the impact of external particles and acid mist is reduced through enclosure, isolation, filtered air supply and exhaust, and continuous treatment within the equipment. In terms of process control, the consistency of the processing of similar crucibles is improved through parameter setting and final rinsing detection.

[0183] The above provides a detailed description of a crucible cleaning method and apparatus provided in this application. For those skilled in the art, based on the ideas of the embodiments of this application, there will be changes in the specific implementation methods and application scope. Therefore, the content of this specification should not be construed as a limitation of this application.

Claims

1. A crucible cleaning method, characterized in that, include: The material frame (30) containing the indium phosphide crucible to be cleaned is loaded and sent to the front-end processing area to pickle the indium phosphide crucible. The pickled material frame (30) is quickly rinsed in the front-end processing area to remove residual acid carried by the material frame (30) and the indium phosphide crucible. After the material frame (30) has completed a quick rinse, the partition between the front treatment area and the rear rinsing area is opened, the material frame (30) is sent into the rear rinsing area for ultrasonic rinsing, and the partition is restored after the material frame (30) has passed through. The water resistivity of the rinsing solution at the end of the ultrasonic rinsing is detected, and the detection result is compared with a preset water resistivity threshold. When the detection result is less than the preset water resistivity threshold, the material frame (30) is returned to the front-end processing area for pickling, rapid rinsing and ultrasonic rinsing. When the detection result is greater than or equal to the preset water resistivity threshold, the material frame (30) is sent to the drying station for slow drying, and the dried material frame (30) is unloaded.

2. The crucible cleaning method according to claim 1, characterized in that, The pickling includes: Place the material frame (30) into the pickling tank containing the pickling solution and close the automatic tank cover (14) of the pickling tank. The pickling solution is heated and ultrasonically treated, and the material frame (30) is driven to vibrate up and down in the pickling solution to dissolve and remove the adhering substances on the surface of the indium phosphide crucible. After pickling is completed, open the automatic tank cover (14) and remove the material frame (30) from the pickling tank.

3. The crucible cleaning method according to claim 1, characterized in that, The rapid rinsing is a QDR rapid rinsing performed in a rapid rinsing tank, which includes ultrapure water overflow replacement, spray rinsing and rapid drainage; The ultrapure water overflow replacement includes continuously supplying ultrapure water to the rapid rinsing tank, so that the liquid in the rapid rinsing tank is discharged through the overflow structure; The spray rinsing includes spraying ultrapure water onto the material frame (30) and the indium phosphide crucible; The rapid drainage includes draining the liquid in the tank through a rapid drain valve (24) located at the bottom of the rapid flushing tank.

4. The crucible cleaning method according to claim 1, characterized in that, The ultrasonic rinsing includes a first ultrasonic rinsing and a second ultrasonic rinsing performed sequentially in a first ultrasonic tank and a second ultrasonic tank. The water resistivity of the rinsing liquid in the second ultrasonic tank is detected by a water resistivity sensor (13) installed in the second ultrasonic tank. When the detection result is less than the preset water resistivity threshold, the material frame (30) is returned to the pickling tank and pickled, QDR quick rinse, first ultrasonic rinse and second ultrasonic rinse are performed in sequence.

5. The crucible cleaning method according to claim 1, characterized in that, The slow-pull drying includes: Ultrapure water and isopropanol are supplied to the slow-pull tank through a pure water supply system and an IPA supply system, respectively, and the drying temperature of the slow-pull tank is adjusted by a heating component. The material frame (30) is slowly raised so that the indium phosphide crucible gradually detaches from the liquid surface. The Marangoni effect is generated by the surface tension gradient formed by isopropanol, which causes the liquid film on the surface of the indium phosphide crucible to retreat from the surface of the indium phosphide crucible.

6. A crucible cleaning device, characterized in that, It includes a frame (1), a conveying mechanism (11), a control unit, and a loading station (2), a pickling tank (4), a rapid rinsing tank (5), an ultrasonic rinsing assembly, a slow pull tank (9), and a unloading station (10) arranged in the processing sequence along the material frame (30). The pickling tank (4) and the rapid rinsing tank (5) are located in the front treatment area, and the ultrasonic rinsing assembly is located in the rear rinsing area. A first partition (3) is provided between the feeding station (2) and the front processing area, and a second partition (6) is provided between the front processing area and the rear rinsing area. The conveying mechanism (11) is used to transfer the material frame (30) between each work station and each tank, and the material frame (30) is used to load the indium phosphide crucible; The ultrasonic rinsing assembly is equipped with a water resistivity sensor (13) for detecting the water resistivity of the final rinsing liquid. The control unit is connected to the conveying mechanism (11), the first partition (3), the second partition (6), and the water resistivity sensor (13), and is configured as follows: After the pickled material frame (30) has completed rinsing in the rapid rinsing tank (5), the second partition (6) is opened to allow the material frame (30) to enter the downstream rinsing area, and the second partition (6) is closed after the material frame (30) has passed through. The detection result of the water resistivity sensor (13) is compared with the preset water resistivity threshold. When the detection result is less than the preset water resistivity threshold, the conveying mechanism (11) is controlled to return the material frame (30) to the pickling tank (4) for re-cleaning. When the detection result is greater than or equal to the preset water resistivity threshold, the conveying mechanism (11) is controlled to send the material frame (30) into the slow pull tank (9).

7. The crucible cleaning equipment according to claim 6, characterized in that, The pickling tank (4) is equipped with an automatic tank cover (14), an up-and-down oscillation mechanism (15), an ultrasonic vibrating plate (16), and a pickling heating device. The automatic tank cover (14) is driven by the tank cover drive cylinder (37) to flip relative to the pickling tank (4); The ultrasonic vibrating plate (16) is disposed at the bottom of the pickling tank (4), and the pickling heating device is disposed around the pickling tank (4) and includes a PFA heater (17). The up-and-down oscillation mechanism (15) includes a material frame (30) base (18), a guide rail (19), an oscillation drive wheel (20), and an oscillation drive linkage (21). The base (18) of the material frame (30) is used to support the material frame (30) and moves up and down under the guidance of the guide rail (19); One end of the oscillation drive linkage (21) is rotatably connected to the eccentric position of the oscillation drive wheel (20), and the other end is rotatably connected to the connecting part (31) that drives the material frame (30) base (18) to move up and down.

8. The crucible cleaning equipment according to claim 6, characterized in that, The rapid rinsing tank (5) is a QDR rinsing tank, which is equipped with an ultrapure water supply structure, an overflow tank (22), a spray pipe (23) and a fast drain valve (24). The overflow tank (22) is located at the top of the QDR flushing tank and is used to receive the liquid overflowing from the QDR flushing tank; The spray pipe (23) is positioned toward the material frame (30) located inside the QDR rinsing tank; The quick-drain valve (24) is connected to the bottom of the QDR flushing tank.

9. The crucible cleaning equipment according to claim 6, characterized in that, The ultrasonic rinsing assembly includes a first ultrasonic tank (7) and a second ultrasonic tank (8) arranged sequentially along the processing order of the material frame (30), and the water resistivity sensor (13) is disposed in the second ultrasonic tank (8). The slow-pull tank (9) is equipped with a heating component, an IPA liquid addition system and a pure water liquid addition system; The pure water dosing system is used to supply ultrapure water to the slow-pull tank (9), and the IPA dosing system is used to supply isopropanol to the slow-pull tank (9); The conveying mechanism (11) can drive the material frame (30) to rise slowly relative to the slow pull trough (9) so that the indium phosphide crucible gradually leaves the liquid surface.

10. A crucible cleaning device according to claim 6, characterized in that, The frame (1) includes a 304 stainless steel skeleton and a PP plate covering the outside of the 304 stainless steel skeleton. An FFU filter (12) is provided on the top of the frame (1), and an exhaust port connected to the exhaust duct (33) is provided inside the pickling tank (4) and on the side of the tank. The first partition (3) and the second partition (6) are respectively the first automatic lifting door and the second automatic lifting door; The handling mechanism (11) is a handling robot, which includes a horizontal moving component (25), a vertical lifting component (26), and a picking and placing part (27) for picking up and placing the material frame (30) arranged along the direction of each workstation.

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