Device and method for removing residual polycrystalline diamond on molybdenum support through laser equipment

Abstract

The invention provides a laser device and method for removing residual polycrystalline diamond on the surface of a molybdenum support, the device comprises a shell, a laser and an X-ray diffraction processing device, a scanning head of the laser is arranged at the top of an inner cavity of the shell and is used for emitting laser beams to focus and irradiate the surface of the molybdenum support; the X-ray diffraction processing device is composed of an X-ray emitter and a detector which are arranged on the side of the inner cavity and used for conducting in-situ component analysis on the surface of the molybdenum support in the cleaning process, accurately judging the residual state and the residual area of the polycrystalline diamond and conducting secondary scanning on the residual area to ensure that cleaning is thorough and reaches the standard. The method is efficient and rapid, the surface of the molybdenum support can be effectively protected against damage, the uniformity of the heat conduction performance of the molybdenum support is guaranteed, and the service life is remarkably prolonged.

Description

Technical Field

[0001] The present invention relates to the technical field of laser equipment, and in particular to a device and method for removing residual polycrystalline diamonds on a molybdenum support using laser equipment. Background Art

[0002] Diamond possesses exceptional semiconductor properties, including an ultra-wide bandgap, high electron mobility, high breakdown electric field, high thermal conductivity, and ultra-high hardness, making it an ideal material for manufacturing tools, abrasives, and high-frequency, high-power electronic devices. However, due to its long growth cycle, numerous defects, and rarity, commercially available natural diamonds are often too expensive to be used in various industries. Therefore, synthetic methods are used to produce diamonds to meet current industrial needs. Among the numerous methods for artificially producing diamonds, microwave plasma chemical vapor deposition (MPCVD) has gained widespread favor within the industry due to its high efficiency and ability to provide precise control.

[0003] In the process of growing single-crystal diamond using MPCVD technology, while the plasma deposits single-crystal diamond on the substrate, polycrystalline diamond will also grow on the surface of the molybdenum holder. These polycrystalline diamonds will gradually thicken and tightly connect to the molybdenum holder as the growth time increases, making the cleaning process of the molybdenum holder after the growth is completed very difficult, affecting the repeated growth and use of the molybdenum holder.

[0004] Polycrystalline diamond is chemically very stable, making it difficult to clean with chemical reagents. Using physical or mechanical methods to clean the molybdenum support inevitably damages and deforms the support, affecting its performance. Prior art includes a Chinese patent (publication number: CN117778993A) that discloses a "Method for Cleaning Molybdenum Supports in MPCVD Equipment." This patented technique uses an MPCVD device to etch the molybdenum support at high temperature and then cool it down to separate the polycrystalline diamond from the support. However, this method requires extremely high temperatures, is time-consuming, and inefficient, increasing the growth cycle and cost of synthetic diamonds. Summary of the Invention

[0005] In response to the shortcomings of the existing technology, the present invention provides a device and method for cleaning polycrystalline diamonds on the surface of a molybdenum support with a laser cleaning device, aiming to solve the problems of existing cleaning solutions that easily cause damage and deformation of the molybdenum support surface, take a long time to clean, affect the subsequent use of the molybdenum support, and reduce the durability of the molybdenum support.

[0006] To achieve the above-mentioned purpose, the present invention provides a device and method for cleaning polycrystalline diamond on the surface of a molybdenum support using a laser cleaning device, comprising the following contents: According to a first aspect of an embodiment of the present invention, there is provided a device for removing residual polycrystalline diamond on a molybdenum support by laser, comprising: A housing having a hollow inner cavity with a cleaning platform placed therein; a laser scanning head, located at the top of the hollow inner cavity, for emitting laser light toward the cleaning platform; An X-ray diffraction processing device is arranged on the side of the hollow inner cavity and is used to emit X-rays to detect the composition of the surface of the molybdenum support to be cleaned.

[0007] Preferably, the laser device further comprises: a translation mechanism connected to the cleaning platform, capable of driving the cleaning platform to move horizontally and vertically within the inner cavity.

[0008] Preferably, the laser device further includes: the X-ray diffraction processing device further includes a controller, a display, an X-ray emitter and an X-ray receiver, the display is electrically connected to the controller, the controller is electrically connected to the X-ray receiver, the controller is used to receive the intensity information of the X-ray receiving device and perform automatic peak analysis and residual judgment on the diffraction pattern, and feed back the judgment result to the laser scanning head, the controller is also used to send it to the display, and the display is used to display the diffraction pattern of the surface of the molybdenum support to be cleaned.

[0009] According to another aspect of an embodiment of the present invention, a method for removing residual polycrystalline diamonds on a molybdenum support using a laser device is provided, comprising: placing the molybdenum support to be cleaned on a cleaning platform of a laser cleaning machine and positioning the laser above the molybdenum support to be cleaned; setting parameters of the laser cleaning machine, starting the laser cleaning machine, and moving the laser beam across the surface of the molybdenum support for scanning; during the scanning process, using an X-ray diffraction processing device to monitor, analyze, and determine the residual polycrystalline diamond area and using an exhaust device to remove polycrystalline diamond debris stripped by the laser; turning off the laser cleaning machine and removing the molybdenum support, ultrasonically cleaning it with acetone, alcohol, and deionized water, drying it with nitrogen, and storing it in a drying oven.

[0010] Preferably, the moving scanning range of the laser cleaning machine is adjusted by vertical movement and horizontal movement, and the moving range is 0-500 mm.

[0011] Preferably, the mobile scanning is divided into two scans: the first scan is a low-power coarse scan, the scanning power of the coarse scan is 200W, the scanning range covers the entire molybdenum support surface, and the scanning speed is 10mm / s; the second scan is a high-power fine scan, the scanning power of the fine scan is 300-500W, the scanning speed is 5mm / s, and the residual area is removed.

[0012] Preferably, the first scan is specifically: forward spiral scanning along a first direction; when the laser moves to the first edge area of ​​the molybdenum holder, switching to forward spiral scanning in a second direction that intersects the first direction at 90°; when the laser reaches the second edge area of ​​the molybdenum holder, switching to forward spiral scanning in a third direction that is 180° parallel to the first direction; when the laser reaches the third edge area of ​​the molybdenum holder, switching to forward spiral scanning in a fourth direction that is 180° parallel to the second direction.

[0013] The second scan is specifically as follows: focusing the laser beam on the polycrystalline residual area, setting the laser spiral scan to spread from the inside to the outside, and ending when approaching the raised edge position for limiting the placement of diamonds. When the laser beam reaches the edge of the edge area, the scan is completed.

[0014] Preferably, after performing the first scan, the polycrystalline diamond residual area is analyzed and determined by an X-ray diffraction processing device, and then a second scan is performed on the residual area.

[0015] Preferably, the step of cleaning the molybdenum holder with acetone, alcohol and deionized water includes: placing the molybdenum holder in containers containing acetone, alcohol and deionized water respectively for ultrasonic cleaning to remove oil stains remaining on the molybdenum holder during the laser cleaning process, drying it with nitrogen after cleaning, and placing it in a drying oven for drying and storage.

[0016] Preferably, the switching of the first direction, the second direction, the third direction and the fourth direction is automatically performed by the numerical control system of the laser cleaning machine, and the path planning covers more than 95% of the surface area of ​​the molybdenum support.

[0017] The present invention provides a method for removing residual polycrystalline diamond from a molybdenum support using a laser device. The method involves placing the molybdenum support to be cleaned in a laser cleaning machine, then activating the laser cleaning machine to focus the laser beam on the surface of the molybdenum support to be cleaned. The interaction between the laser and the polycrystalline diamond on the molybdenum support surface generates high temperature and energy, causing the polycrystalline diamond to instantly heat up and expand, reducing its binding force with the molybdenum support surface and ultimately falling off the surface of the molybdenum support to be cleaned. The method is simple to operate, does not damage the molybdenum support surface, and is time-efficient. It achieves rapid and efficient cleaning of the polycrystalline diamond, ensures the roughness of the molybdenum support surface, does not reduce the thermal conductivity of the molybdenum support, and extends the service life of the molybdenum support. The present invention also utilizes an X-ray diffraction processing device to monitor the cleaning surface in real time, accurately determining the residual state of the polycrystalline diamond and ensuring thorough removal to the required standard. This method is efficient and quick, effectively protecting the molybdenum support surface from damage, ensuring the uniformity of the molybdenum support's thermal conductivity, and significantly extending its service life. BRIEF DESCRIPTION OF THE DRAWINGS

[0018] To more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the following briefly introduces the drawings required for use in the embodiments or the description of the prior art. Meanwhile, the drawings described below are merely some embodiments of the present invention. A person of ordinary skill in the art can, without inventive effort, derive other drawings based on the structures shown in these drawings.

[0019] Figure 1 Mechanical diagram of the laser device provided by the present invention; Figure 2 A movable cleaning platform inside the laser equipment provided by the present invention; Figure 3 Flowchart of the laser equipment provided by the present invention for removing residual polycrystalline diamond from a molybdenum support; Figure 4 This is a before and after comparison of using laser cleaning equipment to remove polycrystalline diamonds from the surface of a molybdenum support in the present invention. DETAILED DESCRIPTION

[0020] The following will clearly and completely describe the technical solutions in the embodiments of the present invention in conjunction with the accompanying drawings. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative efforts are within the scope of protection of the present invention.

[0021] Figure 1 The mechanical diagram of the laser equipment provided by the present invention is as follows: Figure 1 As shown, the laser device includes a housing 101, a laser 102, an X-ray diffraction processing device 103, a cleaning platform 104, a testing device 106 and an exhaust device 107, wherein: the laser 102 is installed directly above the housing 101, located at the top of the hollow inner cavity, and is used to emit laser light toward the cleaning platform so that the laser beam can vertically hit the middle of the cleaning platform; the X-ray diffraction processing device 103 is configured on the upper side of the housing 101, passing through the side of the hollow inner cavity. The optical transmitter of the X-ray diffraction processing device 103 is used to emit X-rays to detect the composition of the surface of the molybdenum support to be cleaned. In this way, the surface polycrystals are blown away while the laser is scanning, and whether the surface composition of the molybdenum support contains residual carbon peaks can be directly detected.

[0022] The interior of the laser device also includes a cleaning platform 104, such as Figure 2 As shown, Figure 2The movable cleaning platform inside the laser device provided by the present invention is located in the hollow cavity of the shell 101. At the same time, the molybdenum holder bracket 105 is installed on the cleaning platform 104 and moves in the left and right directions and the front and back directions under the drive of the cleaning platform 104. This makes it easy to adjust the position where the laser hits the surface of the molybdenum holder to be cleaned, and also facilitates X-ray diffraction detection.

[0023] The cleaning platform of the laser device also includes a translation mechanism, which is connected to the cleaning platform and drives the cleaning platform to move left and right and front and back in the shell cavity. Specifically, the cleaning platform 104 includes two rods and four track grooves. The two rods are distributed in the track grooves of the cleaning platform and move back and forth and left and right along the track grooves. The molybdenum support bracket 105 is located on the two rods and moves back and forth and left and right with the two rods.

[0024] The X-ray diffraction processing device 103 also includes a controller, a display and a light receiver. The display is electrically connected to the controller, and the controller is electrically connected to the light receiving device. The controller is used to receive the intensity information of the X-ray receiving device and perform automatic peak analysis and residual judgment on the diffraction pattern, and feed the judgment result back to the laser and send it to the display. The display is used to display the diffraction pattern of the surface of the molybdenum support to be cleaned.

[0025] The function of the testing device 106 is to detect whether the surface composition of the molybdenum support contains residual carbon peaks. Specifically, the two-dimensional detection data of the diffracted X-rays with the largest X-ray intensity is extracted from the two-dimensional detection data of the diffracted X-rays obtained at multiple scanning angles. The two-dimensional detection data is the peak two-dimensional detection data; the position with the largest X-ray intensity is determined according to the peak two-dimensional detection data, and the maximum position is the peak position; and data processing is performed using the position information of the peak position determined by the peak two-dimensional detection data.

[0026] The function of the exhaust device 107 is to extract the polycrystals cleaned by the laser.

[0027] like Figure 3 As shown in FIG, the flow chart of the laser device provided in this embodiment for removing residual polycrystalline diamond from a molybdenum support includes: Step S100: Place the molybdenum holder to be cleaned on the sample cleaning platform of the laser cleaning machine so that the laser is located above the molybdenum holder; Step S200, setting the parameters of the laser cleaning machine, then starting the laser cleaning machine to move and scan the laser beam on the surface of the molybdenum support; Step S300: During the scanning process, an X-ray diffraction processing device is used to monitor and analyze the remaining polycrystalline diamond area and an exhaust device is used to remove the polycrystalline diamond cleaned by the laser; Step S400: turn off the laser cleaning machine and take out the molybdenum holder, and clean the pollutants remaining on the surface of the molybdenum holder with acetone, alcohol and deionized water.

[0028] To non-destructively remove polycrystalline diamonds from a molybdenum support, the molybdenum support to be cleaned must first be placed on the cleaning platform of a laser cleaning machine. Laser cleaning parameters are then set, and the laser cleaning machine is activated to emit a laser beam that scans the polycrystalline diamonds on the molybdenum support. The interaction between the laser and the polycrystalline diamonds on the molybdenum support generates high temperatures and energy within the polycrystalline diamonds, causing them to instantly heat up and expand, weakening the bond between the polycrystalline diamonds and the molybdenum support surface, ultimately causing them to fall off the molybdenum support. This method requires no additional equipment or tools, is simple to operate, is time-efficient, and does not damage the molybdenum support, thereby improving its durability.

[0029] The laser cleaning machine's cleaning scan width is adjustable through vertical and horizontal movement, with a range of 0-100mm. The laser cleaning machine performs two scans: the first is a low-power, coarse scan at a power of 200W, covering the entire molybdenum support surface at a speed of 10mm / s; the second is a high-power, fine scan at a power of 300-500W and a speed of 5mm / s.

[0030] The first scan specifically involves a forward spiral scan along a first direction. When the laser reaches the first edge of the molybdenum support, it switches to a forward spiral scan in a second direction that intersects the first direction at 90 degrees. When the laser reaches the second edge of the molybdenum support, it switches to a forward spiral scan in a third direction that is 180 degrees parallel to the first direction. When the laser reaches the third edge of the molybdenum support, it switches to a forward spiral scan in a fourth direction that is 180 degrees parallel to the second direction. Switching between the first, second, third, and fourth directions is automatically performed by the laser cleaning machine's CNC system, and the path planning covers more than 95% of the molybdenum support's surface area.

[0031] After the first scan is performed, the polycrystalline diamond residual area is analyzed and determined by the X-ray diffraction processing device, and then a second scan is performed on the residual area.

[0032] The second scan is specifically as follows: focusing the laser beam on the polycrystalline residual area, setting the laser spiral scan to spread from the inside to the outside, and ending when approaching the raised edge position for limiting the placement of diamonds. When the laser beam reaches the edge of the edge area, the scan is completed.

[0033] The flowchart of the laser device provided in this embodiment for removing residual polycrystalline diamond from a molybdenum support is as follows: First, place the molybdenum holder to be cleaned on the sample cleaning platform of the laser cleaning machine so that the laser is above the molybdenum holder, and then perform the following steps: S210: Set the laser output power to 200W; S220: Setting the cleaning scanning width of the laser cleaning machine to be able to move vertically and horizontally 0-100 mm, preferably 100 mm; S230: Setting the scanning speed of the laser cleaning machine to 10 mm / s; S240: Setting the scanning path of the laser cleaning machine to forward spiral scanning along a first direction; when the laser moves to a first edge region of the molybdenum support to be cleaned, switching to forward spiral scanning along a second direction, the second direction intersecting the first direction at 90°; when the laser is located at a second edge region of the molybdenum support to be cleaned, switching to forward spiral scanning along a third direction, the third direction being 180° parallel to the first direction; when the laser is located at a third edge region of the molybdenum support to be cleaned, switching to forward spiral scanning along a fourth direction, the fourth direction being 180° parallel to the second direction; S250: Set the laser output power to 500W and the scanning speed of the laser cleaning machine to 5mm / s.

[0034] S260: Focus the laser beam at the center of the residual polycrystal area. Set the laser spiral scan to diffuse from the inside out, ending when approaching the edge. The laser pitch is 100µm. The scan is complete when the laser beam reaches the edge of the target area. If the polycrystals on the molybdenum support surface have not yet fallen off, the motion control system will move the laser head to the initial center position and continue scanning. If there are multiple concentrated areas of residual polycrystals on the molybdenum support surface, scan and clean them in batches at different center locations.

[0035] S270: Adjust the position of the cleaning platform so that the X-ray diffraction processing device can detect the surface composition information of the molybdenum support.

[0036] In this embodiment, after the molybdenum support to be cleaned is placed on the cleaning platform of the laser cleaning machine, the laser cleaning output power is set to 200W and 500W, the laser cleaning scan width is set to 100mm, the scan speed is set to 10mm / s and 5mm / s, and the rough cleaning scan path is set to a forward spiral scan in a first direction. When the laser moves to the first edge area of ​​the molybdenum support to be cleaned, it switches to a forward spiral scan in a second direction, which intersects the first direction at 90°. When the laser is located at the second edge area of ​​the molybdenum support to be cleaned, it switches to a forward spiral scan in a third direction, which is 180° parallel to the first direction. When the laser is located at the third edge area of ​​the molybdenum support to be cleaned, it switches to a forward spiral scan in a fourth direction, which is 180° parallel to the second direction. The fine cleaning scan path is set to the position of the polycrystalline residual area. Because the molybdenum support surface has a raised edge designed to limit the placement of the diamond, to avoid damaging the edge, the position must avoid the edge and be as close to the center of the polycrystalline residual area as possible. The laser spiral scanning was set to spread from the inside to the outside and end when approaching the edge position. The laser pitch was 100µm.

[0037] In this embodiment, the switching between the first, second, third, and fourth directions is automatically performed by the laser cleaning machine's CNC system, and the path planning covers more than 95% of the molybdenum support surface area. In some embodiments, the output power of the laser cleaning can be controlled within a range of 200-500W. The laser cleaning scan width can be set within a range of 10-110mm, and the laser beam scanning speed can be set at 3mm / s, 5mm / s, or 15mm / s.

[0038] In this embodiment, the step of cleaning the molybdenum holder with acetone, alcohol, and deionized water includes: placing the molybdenum holder in containers containing acetone, alcohol, and deionized water, respectively, and performing ultrasonic cleaning to remove oil stains remaining on the molybdenum holder during the laser cleaning process; after cleaning, drying it with nitrogen gas, and drying it in a drying oven for storage.

[0039] like Figure 4 As shown in the before and after comparison diagram of using laser cleaning equipment to remove polycrystalline diamonds on the surface of a molybdenum support with raised edges provided in this embodiment, it can be seen that the method of using laser equipment to remove residual polycrystalline diamonds on a molybdenum support of the present invention has an obvious cleaning effect, and the residual polycrystalline diamonds on the molybdenum support have been cleaned up.

[0040] This patent places the molybdenum support to be cleaned in a laser cleaning machine, then starts the laser cleaning machine to focus the laser beam on the surface of the molybdenum support to be cleaned. Through the interaction between the laser and the polycrystalline diamond on the surface of the molybdenum support, high temperature and high energy are generated, causing the polycrystalline diamond to instantly heat up and expand, reducing the bonding force with the surface of the molybdenum support, and eventually falling off from the surface of the molybdenum support to be cleaned without damaging the surface of the molybdenum support, and taking a short time, thereby achieving fast and efficient cleaning of the polycrystalline, ensuring the thermal conductivity of the molybdenum support, and extending the service life of the molybdenum support.

[0041] It should be noted that the technical features in the above embodiments can be combined in any way, and the technical solutions formed by the combination all fall within the scope of protection of this application. In this article, terms such as "including", "comprising" or any other variants thereof are intended to cover non-exclusive inclusion, so that the process, method, article or device including a series of elements includes not only those elements, but also includes other elements that are not explicitly listed, or also includes elements inherent to such process, method, article or device. In the absence of further restrictions, the elements defined by the sentence "including a..." do not exclude the presence of other identical elements in the process, method, article or device including the elements.

[0042] While embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions, and variations may be made to these embodiments without departing from the principles and spirit of the invention, and that the scope of the invention is defined by the appended claims and their equivalents.

Claims

1. A laser device, characterized in that include: A housing having a hollow inner cavity with a cleaning platform placed therein; a laser scanning head, located at the top of the hollow inner cavity, for emitting laser light toward the cleaning platform; An X-ray diffraction processing device is arranged on the side of the hollow inner cavity and is used to emit X-rays to detect the composition of the surface of the molybdenum support to be cleaned.

2. The laser device according to claim 1, wherein The laser device further comprises: a translation mechanism connected to the cleaning platform and capable of driving the cleaning platform to move horizontally and vertically within the inner cavity.

3. The laser device according to claim 1, wherein The laser device further comprises: The X-ray diffraction processing device also includes a controller, a display, an X-ray emitter and an X-ray receiver. The display is electrically connected to the controller, and the controller is electrically connected to the X-ray receiver. The controller is used to receive the intensity information of the X-ray receiving device and perform automatic peak analysis and residual judgment on the diffraction pattern, and feed back the judgment result to the laser scanning head. The controller is also used to send it to the display, and the display is used to display the diffraction pattern of the surface of the molybdenum support to be cleaned.

4. A method for removing residual polycrystalline diamond from a molybdenum support using a laser device, characterized in that: The following steps are involved: Placing the molybdenum support to be cleaned on the cleaning platform of the laser cleaning machine so that the laser is located above the molybdenum support to be cleaned; Set the parameters of the laser cleaning machine, start the laser cleaning machine, and move the laser beam to scan the surface of the molybdenum support; During the scanning process, an X-ray diffraction processing device is used to monitor and analyze the residual area of ​​polycrystalline diamond and an exhaust device is used to remove the polycrystalline diamond debris stripped by the laser; Turn off the laser cleaning machine and take out the molybdenum holder, clean it ultrasonically with acetone, alcohol, and deionized water, blow it dry with nitrogen, and store it in a drying oven.

5. The method according to claim 4, characterized in that The moving scanning range of the laser cleaning machine is adjusted by vertical movement and horizontal movement, and the moving range is 0-500mm.

6. The method according to claim 5, characterized in that The mobile scan is divided into two scans: The first scan is a low-power coarse scan with a scanning power of 200 W, a scanning range covering the entire molybdenum support surface, and a scanning speed of 10 mm / s; The second scan is a high-power fine scan with a scanning power of 300-500W and a scanning speed of 5mm / s to remove the residual area.

7. The method according to claim 6, characterized in that The first scan is specifically as follows: forward spiral scanning along a first direction; when the laser moves to the first edge area of ​​the molybdenum support, switching to forward spiral scanning in a second direction intersecting the first direction at 90°; when the laser reaches the second edge area of ​​the molybdenum support, switching to forward spiral scanning in a third direction parallel to the first direction at 180°; when the laser reaches the third edge area of ​​the molybdenum support, switching to forward spiral scanning in a fourth direction parallel to the second direction at 180°; The second scan is specifically as follows: focusing the laser beam on the polycrystalline residual area, setting the laser spiral scan to spread from the inside to the outside, and ending when approaching the raised edge position for limiting the placement of diamonds. When the laser beam reaches the edge of the edge area, the scan is completed.

8. The method according to claim 7, characterized in that After the first scan is performed, the polycrystalline diamond residual area is analyzed and determined by the X-ray diffraction processing device, and then a second scan is performed on the residual area.

9. The method according to claim 4, characterized in that The step of cleaning the molybdenum support includes: placing the molybdenum support in containers containing acetone, alcohol, and deionized water for ultrasonic cleaning to remove oil stains remaining on the molybdenum support during the laser cleaning process, drying it with nitrogen after cleaning, and placing it in a drying oven for drying and storage.

10. The method according to claim 7, characterized in that The switching among the first direction, the second direction, the third direction and the fourth direction is automatically performed by the numerical control system of the laser cleaning machine, and the path planning covers more than 95% of the surface area of ​​the molybdenum support.

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