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CN-121978075-A - Diamond growth in-situ Raman test equipment and Raman test method

CN121978075ACN 121978075 ACN121978075 ACN 121978075ACN-121978075-A

Abstract

The invention relates to the technical field of in-situ Raman monitoring microwave plasma chemical vapor deposition devices, and particularly discloses a diamond growth in-situ Raman test device and a Raman test method, wherein the Raman test device comprises a growth device and a Raman laser test device; A detection window is arranged on the upper cover of a reaction chamber of the growth device, a Raman laser testing device with a height adjusting mechanism, an angle adjusting mechanism and a distance measuring adjusting mechanism is arranged on the outer side of the reaction chamber, laser beams are precisely focused on the area with the strongest edge signal of a diamond sheet on a deposition table through cooperation of the three mechanisms, and the method is used for acquiring and analyzing Raman spectra in real time and dynamically feeding back and optimizing process parameters in the process of growing diamond by microwave plasma chemical vapor deposition. Finally, high signal-to-noise ratio, in-situ, real-time monitoring and accurate control of the diamond growth process in a high-temperature plasma environment are realized.

Inventors

  • JIAN XIAN
  • XU SHENGYUAN
  • LI SIYING
  • LIU YIFAN
  • ZHANG GUANG
  • LI BEIER

Assignees

  • 电子科技大学
  • 成都腾六光电有限公司

Dates

Publication Date
20260505
Application Date
20260123

Claims (10)

  1. 1. The in-situ Raman testing equipment for diamond growth comprises a growth device (10), wherein the growth device (10) comprises a base (11), a deposition table (12) and an upper cover (13), the upper cover (13) is matched with the base (11) to form a reaction chamber (101), the deposition table (12) is arranged in the reaction chamber (101), the deposition table (12) is used for placing a diamond sheet (20), and the in-situ Raman testing equipment is characterized in that the upper cover (13) is provided with a detection window (131), a Raman laser testing device (30) is arranged outside the detection window (131), and the Raman laser testing device (30) comprises: The laser (31) is used for generating a laser beam, the laser probe of the laser beam is arranged outside the detection window (131), and the laser beam passes through the detection window (131) to enter the reaction chamber (101) and is focused on the edge of the diamond sheet (20) placed on the deposition table (12); a height adjustment mechanism (32) for controlling the laser (31) to move vertically; The angle adjusting mechanism (33) is connected to the output end of the height adjusting mechanism (32) and is used for controlling the detection angle of the laser (31); And the distance measuring and adjusting mechanism (34) is connected to the output end of the angle adjusting mechanism (33) and is used for controlling the distance between the laser probe of the laser (31) and the detection window (131).
  2. 2. A diamond growth in situ raman test device according to claim 1, characterized in that the growth device (10) further comprises a first machine (14), the base (11) is fixed on the first machine (14), and the upper cover (13) is in openable sealing connection with the base (11).
  3. 3. A diamond grown in situ raman test device according to claim 2, wherein the growth means (10) further comprises a lift cap mechanism (15) and a flip mechanism (16), the lift cap mechanism (15) comprising: The telescopic driver (151) is characterized in that the body of the telescopic driver is fixed on the first machine table (14), and the output end of the telescopic driver is connected with a lifting rod (152); The flip mechanism (16) includes: a first rotating seat (161) fixed on the top of the lifting rod (152); The middle part of the swing arm (162) is rotationally connected with the first rotating seat (161), and one end of the swing arm is fixedly connected with the upper cover (13); and the lifting driver (163) is characterized in that the body of the lifting driver is fixed on the lifting rod (152), and the driving end of the lifting driver is rotationally connected with the other end of the swing arm (162).
  4. 4. A diamond growth in situ raman test device according to claim 1, characterized in that a lift controller (17) is provided inside the base (11) for controlling the lift height of the deposition table (12) in the reaction chamber (101).
  5. 5. A diamond grown in situ raman test device according to claim 1, characterized in that said height adjustment mechanism (32) comprises a second table (321), a scissor lift (322) fixed to said second table (321), and a tensioning drive (323) for driving said scissor lift (322) up and down; The angle adjustment mechanism (33) includes: A second rotating seat (331) fixed on the top of the scissor lift (322); a support plate (332) one end of which is rotatably connected with the second rotating seat (331); The screw rod module (333) comprises a screw rod (3331) arranged on the scissor fork type lifter (322) through a screw rod seat, a sliding block (3332) in threaded fit with the screw rod (3331), and a rotation driver (3333) connected to one end of the screw rod (3331) and used for driving the screw rod to rotate; one end of the connecting rod (334) is rotationally connected with the middle part of the lower end of the supporting plate (332), and the other end of the connecting rod is rotationally connected with the sliding block (3332); The distance measuring and adjusting mechanism (34) comprises a linear module (341) fixed on the supporting plate (332), and the laser (31) is fixed on a sliding table of the linear module (341).
  6. 6. A method of in situ raman testing of diamond growth using a raman test apparatus according to any one of claims 1 to 5, comprising the steps of: The laser probe of the laser (31) is arranged outside the detection window (131), and a laser beam emitted by the laser (31) passes through the detection window (131) to enter the reaction chamber (101) and is focused on the edge of the diamond sheet (20) placed on the deposition table (12), so that a Raman signal of the diamond growth in-situ is detected in real time.
  7. 7. The method of in-situ raman detection of diamond growth according to claim 6, wherein before detecting raman signals, the position and angle of the laser probe are adjusted, comprising: The incidence angle theta of the laser beam is adjusted to 25 DEG to 45 DEG by the height adjusting mechanism (32), the angle adjusting mechanism (33) and the distance measuring adjusting mechanism (34), and the distance between the laser probe and the detecting window (131) is adjusted to 20mm to 100mm.
  8. 8. A method of in situ raman testing of diamond growth according to claim 6 or 7, wherein said laser (31) employs a laser wavelength of 473nm.
  9. 9. A method of in situ raman testing of diamond growth according to claim 6, wherein the detection window (131) has a diameter of 15mm to 30mm.
  10. 10. The method of claim 6, further comprising the step of adjusting process parameters of microwave plasma chemical vapor deposition to optimize diamond growth quality based on characteristics of the Raman signal during real-time detection of the Raman signal.

Description

Diamond growth in-situ Raman test equipment and Raman test method Technical Field The invention relates to the technical field of in-situ Raman monitoring microwave plasma chemical vapor deposition devices, in particular to diamond growth in-situ Raman testing equipment and a Raman testing method. Background Diamond is recognized as an ideal semiconductor material for next-generation power electronics, quantum information chips, and high-frequency high-temperature devices due to its excellent physical properties such as ultra-wide forbidden band (5.47 eV), extremely high thermal conductivity (> 2000W ·m -1·K-1), high breakdown electric field (about 10mv·cm -1), and high carrier mobility. As MPCVD technology matures, research into diamond thin films and single crystal epitaxy has entered a rapid development stage. However, diamond has extremely complex bond formation (sp 3/sp 2), defect formation, stress evolution and growth kinetics mechanisms during MPCVD growth, and is highly sensitive to process parameters such as temperature, plasma power, time, gas flow, etc. Small fluctuations in these parameters directly affect the crystal quality, electrical properties, and device performance of the final product. Currently, a typical MPCVD growth device for diamond, such as a microwave plasma chemical vapor deposition device disclosed in chinese patent publication No. CN213142184U, is designed with a focus on improving the physical environment in the reaction chamber (e.g., optimizing the temperature uniformity and stability of the substrate by rotating the lifting mechanism and the cooling mechanism). The device treats the growth process as a 'black box', and the process development and optimization of the device are seriously dependent on offline characterization methods after the growth is finished, such as Raman spectrum, a scanning electron microscope, an atomic force microscope, X-ray diffraction and the like. The offline characterization methods have the fundamental defects that the offline characterization methods can only be analyzed after the growth process is completely stopped, a sample is cooled and a reaction cavity is taken out, so that key structural evolution information, such as nucleation rate change, generation and disappearance of sp2 bonded non-diamond carbon phases, dynamic accumulation process of internal stress of the film, doping element doping activity, interface chemical reaction of plasma and the surface of a substrate and the like, which occur in a transient state in the thin film deposition process cannot be captured in real time. Because of the lack of effective on-line or in-situ monitoring means, accurate control of a process window becomes extremely difficult, so that the growth repeatability is low, the optimization period is long, and the controllable, efficient synthesis and industrialization amplification of high-quality diamond are seriously hindered. Disclosure of Invention In view of the above-mentioned shortcomings of the prior art, the present invention aims to provide a raman testing device and a raman testing method for diamond growth in situ, so as to solve the above-mentioned problems. The in-situ Raman testing equipment for diamond growth comprises a growth device, wherein the growth device comprises a base, a deposition table and an upper cover, the upper cover is matched with the base to form a reaction chamber, the deposition table is arranged in the reaction chamber and is used for placing a diamond sheet, the upper cover is provided with a detection window, a Raman laser testing device is arranged outside the detection window, and the Raman laser testing device comprises: The laser is used for generating a laser beam, a laser probe of the laser beam is arranged outside the detection window, and the laser beam passes through the detection window, enters the reaction chamber and is focused on the edge of the diamond sheet placed on the deposition table; The height adjusting mechanism is used for controlling the laser to move vertically; the angle adjusting mechanism is connected to the output end of the height adjusting mechanism and used for controlling the detection angle of the laser; And the distance measuring and adjusting mechanism is connected to the output end of the angle adjusting mechanism and used for controlling the distance between the laser probe of the laser and the detection window. Specifically, the growth device further comprises a first machine table, the base is fixed on the first machine table, and the upper cover is in openable sealing connection with the base. Specifically, the growing device still includes lift uncapping mechanism and flip mechanism, lift uncapping mechanism includes: the body of the telescopic driver is fixed on the first machine table, and the output end of the telescopic driver is connected with a lifting rod; The flip mechanism includes: the first rotating seat is fixed at the top of the lifting rod; The middle part of