Diamond growth in-situ Raman test equipment and Raman test method

By introducing in-situ Raman testing equipment into the diamond growth apparatus, and using height, angle, and distance adjustment mechanisms to achieve precise focusing of the laser beam and real-time monitoring of the Raman signal, the problem of lack of online monitoring during diamond growth is solved, thereby improving film quality and process optimization efficiency.

CN121978075APending Publication Date: 2026-05-05UNIV OF ELECTRONICS SCI & TECH OF CHINA +1
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
UNIV OF ELECTRONICS SCI & TECH OF CHINA
Filing Date
2026-01-23
Publication Date
2026-05-05

AI Technical Summary

Technical Problem

Existing diamond MPCVD growth equipment lacks effective online or in-situ monitoring methods, which makes it difficult to precisely control the process window, resulting in low growth repeatability and a long optimization cycle, seriously hindering the controllable synthesis and industrial scale-up of high-quality diamond.

Method used

Design an in-situ Raman testing device for diamond growth, equipped with a detection window and a Raman laser testing device. Through height adjustment, angle adjustment and distance adjustment mechanisms, the laser beam can be precisely focused on the edge of the diamond sheet, the Raman signal can be collected in real time, and the process parameters can be dynamically optimized.

Benefits of technology

It achieves high signal-to-noise ratio, in-situ, and real-time monitoring in a high-temperature plasma environment, significantly improving the preparation quality and process optimization efficiency of diamond films, and overcoming the technical challenges of background interference and optical path instability.

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Abstract

The invention relates to the technical field of in-situ Raman monitoring microwave plasma chemical vapor deposition devices, and particularly discloses diamond growth in-situ Raman test equipment and a Raman test method, the Raman test equipment comprises a growth device and a Raman laser test device; a detection window is arranged on an upper cover of a reaction chamber of the growth device, and 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 detection window. The three mechanisms cooperate to accurately focus a laser beam on a diamond wafer edge strongest signal area on a deposition table at an optimal incident angle and an optimal working distance; according to the method, in the process of growing the diamond through microwave plasma chemical vapor deposition, Raman spectrums are collected and analyzed in real time, and technological parameters are dynamically fed back and optimized. And finally, high signal-to-noise ratio, in-situ and real-time monitoring and accurate control of the diamond growth process in a high-temperature plasma environment are realized.
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Description

Technical Field

[0001] This invention relates to the field of in-situ Raman monitoring microwave plasma chemical vapor deposition apparatus, and particularly to an in-situ Raman testing device and Raman testing method for diamond growth. Background Technology

[0002] Diamond is valued for its ultra-wide bandgap (5.47 eV) and extremely high thermal conductivity (>2000 W·m). -1 ·K -1 High breakdown electric field (approximately 10 MV·cm) -1 With its superior physical properties such as high carrier mobility, diamond is widely recognized as an ideal semiconductor material for next-generation power electronic devices, quantum information chips, and high-frequency, high-temperature devices. With the maturation of MPCVD technology, research on diamond thin films and single-crystal epitaxy has entered a phase of rapid development.

[0003] However, the carbon bonding structure (sp³ / sp²), defect formation, stress evolution, and growth kinetics of diamond during MPCVD growth are extremely complex and highly sensitive to process parameters such as temperature, plasma power, time, and gas flow rate. Even minute fluctuations in these parameters can directly affect the crystal quality, electrical properties, and device performance of the final product.

[0004] Currently, typical diamond MPCVD growth apparatuses, such as the microwave plasma chemical vapor deposition apparatus disclosed in Chinese Patent Publication No. CN213142184U, focus on improving the physical environment within the reaction chamber (e.g., optimizing substrate temperature uniformity and stability through rotational lifting mechanisms and cooling mechanisms). These apparatuses treat the growth process as a "black box," and their process development and optimization heavily rely on offline characterization methods after growth, such as Raman spectroscopy, scanning electron microscopy, atomic force microscopy, and X-ray diffraction.

[0005] These offline characterization methods have a fundamental flaw: they can only be analyzed after the growth process has completely stopped, the sample has cooled, and the reaction chamber has been removed. Therefore, they cannot capture key structural evolution information that occurs transiently during thin film deposition in real time, such as changes in nucleation rate, the formation and disappearance of sp²-bonded non-diamond carbon phases, the dynamic accumulation process of internal stress in the thin film, the incorporation activity of dopant elements, and the interfacial chemical reaction between plasma and substrate surface.

[0006] Due to the lack of effective online or in-situ monitoring methods, precise control of the process window has become extremely difficult, resulting in low growth repeatability and a long optimization cycle, which seriously hinders the controllable and efficient synthesis and industrial scale-up of high-quality diamond. Summary of the Invention

[0007] In view of the shortcomings of the prior art, the purpose of this invention is to provide an in-situ Raman testing device and Raman testing method for diamond growth, so as to solve the above problems.

[0008] An in-situ Raman testing device for diamond growth includes a growth apparatus, which comprises a base, a deposition stage, and an upper cover. The upper cover and the base cooperate to form a reaction chamber. The deposition stage is disposed within the reaction chamber and is used to hold a diamond sheet. The upper cover has a detection window, and a Raman laser testing device is disposed outside the detection window. The Raman laser testing device includes: A laser is used to generate a laser beam, the laser probe of which is located outside the detection window. The laser beam passes through the detection window and enters the reaction chamber, and is focused on the edge of the diamond sheet placed on the deposition stage. A height adjustment mechanism is provided for controlling the vertical movement of the laser. An angle adjustment mechanism, connected to the output end of the height adjustment mechanism, is used to control the detection angle of the laser; A ranging adjustment mechanism, connected to the output end of the angle adjustment mechanism, is used to control the distance between the laser probe of the laser and the detection window.

[0009] Specifically, the growth apparatus further includes a first machine platform, the base is fixed on the first machine platform, and the upper cover is sealed to the base in an openable and closable manner.

[0010] Specifically, the growth device further includes a lifting and opening mechanism and a flipping mechanism, wherein the lifting and opening mechanism includes: The telescopic actuator has its body fixed on the first machine base and its output end connected to a lifting rod. The flip-top mechanism includes: The first rotating seat is fixed to the top of the lifting rod; The swing arm has its middle part rotatably connected to the first rotating seat, and its other end is fixedly connected to the upper cover. The lifting driver has its body fixed to the lifting rod, and its driving end is rotatably connected to the other end of the swing arm.

[0011] Specifically, a lifting controller is provided on the inner side of the base to control the lifting height of the deposition stage within the reaction chamber.

[0012] Specifically, the height adjustment mechanism includes a second machine platform, a scissor lift fixed on the second machine platform, and a tensioning actuator for driving the scissor lift to move up and down; The angle adjustment mechanism includes: The second rotating seat is fixed to the top of the scissor lift; The tray, one end of which is rotatably connected to the second rotating seat; The lead screw module includes a lead screw mounted on the scissor lift via a lead screw seat, a slider threadedly engaged with the lead screw, and a rotary actuator connected to one end of the lead screw for driving its rotation. A connecting rod, one end of which is rotatably connected to the middle of the lower end of the support plate, and the other end of which is rotatably connected to the slider; The ranging adjustment mechanism includes a linear module fixed to the support plate, and the laser is fixed to the slide of the linear module.

[0013] A method for in-situ Raman testing of diamond growth, using the aforementioned Raman testing equipment, includes the following steps: The laser probe of the laser is placed outside the detection window. The laser beam emitted by the laser passes through the detection window and enters the reaction chamber, and is focused on the edge of the diamond sheet placed on the deposition stage to detect the in-situ Raman signal of diamond growth in real time.

[0014] Specifically, before detecting the Raman signal, the position and angle of the laser probe need to be adjusted, including: The height adjustment mechanism, angle adjustment mechanism, and distance adjustment mechanism are used to adjust the incident angle θ of the laser beam to 25° to 45°, and the distance L between the laser probe and the detection window is adjusted to 20mm to 100mm.

[0015] Specifically, the laser used in the laser has a wavelength of 473nm.

[0016] Specifically, the diameter of the detection window is 15mm to 30mm.

[0017] Specifically, the real-time detection of Raman signals also includes the step of adjusting the process parameters of microwave plasma chemical vapor deposition based on the characteristics of the Raman signal to optimize the diamond growth quality.

[0018] The beneficial effects of this invention are: This invention discloses an in-situ Raman testing device and method for diamond growth. The Raman testing device includes a growth apparatus and a Raman laser testing device. A detection window is provided on the reaction chamber of the growth apparatus, and a Raman laser testing device with height adjustment, angle adjustment, and distance adjustment mechanisms is configured outside the window. Through the coordinated operation of these three mechanisms, a 473nm laser is precisely focused onto the region with the strongest signal at the edge of the diamond sheet on the deposition stage at an optimal incident angle of 25° to 45° and an optimal working distance of 20mm to 100mm. The method involves real-time acquisition and analysis of Raman spectra during microwave plasma chemical vapor deposition growth, dynamically feeding back and optimizing process parameters. Ultimately, this achieves high signal-to-noise ratio, in-situ, real-time monitoring and precise control of the diamond growth process under high-temperature plasma conditions, effectively overcoming technical challenges such as strong background interference and unstable optical paths, and significantly improving the preparation quality and process optimization efficiency of diamond films. Attached Figure Description

[0019] Figure 1 A three-dimensional view of the in-situ Raman testing equipment for diamond growth according to this application; Figure 2 This is a perspective view of the Raman laser testing apparatus of this application; Figure 3 The three-dimensional growth apparatus of this application Figure 1 ; Figure 4 The three-dimensional growth apparatus of this application Figure 2 ; Figure 5 This is a top view of the in-situ Raman testing equipment for diamond growth according to this application; Figure 6 for Figure 5 A three-dimensional sectional view along line AA; Figure 7 This is a schematic diagram of the laser used in this application to perform Raman laser testing on a diamond sheet. The diagram also shows a simulated reaction process in which a solid film is formed on the surface of a diamond sheet by using plasma as an energy source and reacting gases undergoing a series of chemical and plasma reactions. Figure 8 This is the Raman spectrum of diamond. The horizontal axis represents the Raman shift, and the unit is cm. -1 The vertical axis represents light intensity, and the unit "au" represents "any unit". In the spectral analysis of this application, we mainly focus on the relative level and peak position of light intensity, rather than the absolute value. Figure 9 The image shows the in-situ Raman diffraction peaks of diamond measured at 300-800℃ with 10-minute intervals.

[0020] The attached figures are labeled as follows: growth device 10, base 11, deposition stage 12, upper cover 13, reaction chamber 101, diamond sheet 20, solid film 21, detection window 131, first machine base 14, lifting and opening mechanism 15, telescopic actuator 151, lifting rod 152, flip-top mechanism 16, first rotating seat 161, swing arm 162, lifting actuator 163, lifting controller 17, Raman laser testing device 30, laser 31, height adjustment mechanism 32, second machine base 321, scissor lift 322, tension actuator 323, angle adjustment mechanism 33, second rotating seat 331, support plate 332, lead screw module 333, lead screw 3331, slider 3332, rotation actuator 3333, connecting rod 334, distance adjustment mechanism 34, linear module 341, reaction gas 41, plasma 42. Detailed Implementation

[0021] This invention provides an in-situ Raman spectroscopy testing device and method for diamond growth. To make the objectives, technical solutions, and effects of this invention clearer and more explicit, the invention will be further described in detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are only for explaining the invention and are not intended to limit the invention.

[0022] In the description of this invention, it should be understood that the orientation descriptions, such as up, down, front, back, left, right, etc., are based on the orientation or positional relationship shown in the accompanying drawings. They are only for the convenience of describing this invention 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 limiting this invention.

[0023] Please refer to Figure 1-7As shown, this embodiment discloses an in-situ Raman testing device for diamond growth, including a growth apparatus 10. The growth apparatus 10 includes a base 11, a deposition stage 12, and an upper cover 13. The upper cover 13 and the base 11 cooperate to form a reaction chamber 101. The deposition stage 12 is disposed in the reaction chamber 101 and is used to place a diamond sheet 20. The upper cover 13 is provided with a detection window 131, and a Raman laser testing device 30 is provided outside the detection window 131. The Raman laser testing device 30 includes a laser 31, a height adjustment mechanism 32, an angle adjustment mechanism 33, and a distance adjustment mechanism 34. The laser 31 is used for the production of diamond sheets 20. A laser beam is generated. The laser probe of the laser 31 is located outside the detection window 131. The laser beam passes through the detection window 131 and enters the reaction chamber 101, and is focused on the edge of the diamond sheet 20 placed on the deposition stage 12. The height adjustment mechanism 32 is used to control the vertical movement of the laser 31. The angle adjustment mechanism 33 is connected to the output end of the height adjustment mechanism 32 and is used to control the detection angle of the laser 31. The distance adjustment mechanism 34 is connected to the output end of the angle adjustment mechanism 33 and is used to control the distance between the laser probe of the laser 31 and the detection window 131.

[0024] The in-situ Raman spectroscopy equipment for diamond growth in this embodiment is used in the microwave plasma chemical vapor deposition process. During growth, a carbon-containing reactive gas 41 (such as a mixture of methane and hydrogen) is introduced into the reaction chamber 101, and a high-temperature microwave plasma 42 is generated under microwave energy excitation. The plasma 42 activates the reactive gas 41, and a chemical reaction occurs on the surface of the diamond sheet 20 under a set temperature and pressure, resulting in the deposition and growth of a solid film 21 layer by layer.

[0025] The Raman laser testing device 30 emits a laser beam through the detection window 131 toward the edge of the growing solid film 21. The laser interacts with the material molecules to generate Raman scattered light, which is collected and analyzed, thereby enabling in-situ, real-time monitoring of the growth process of the solid film 21 on the surface of the diamond sheet 20.

[0026] This application, through the coordinated adjustment of the height adjustment mechanism 32, the angle adjustment mechanism 33, and the distance adjustment mechanism 34, can precisely control the laser beam to focus at the edge of the diamond sheet 20 with the strongest signal at the optimal incident angle of 25° to 45°, and ensure that the laser probe and the detection window 131 maintain the optimal working distance of 20mm to 100mm, effectively overcoming the interference of strong plasma background light and optical path transmission loss, and significantly improving the signal-to-noise ratio of the Raman signal.

[0027] In a preferred embodiment, the growth apparatus 10 further includes a first stage 14, with a base 11 fixed on the first stage 14, and an upper cover 13 sealed to the base 11 in an openable and closable manner. The first stage 14 provides a stable support foundation for the entire growth apparatus 10, ensuring that the reaction chamber 101 remains stable under vacuum or specific pressure conditions. The openable and closable sealed connection between the upper cover 13 and the base 11 facilitates the clamping, cleaning, and maintenance of the deposition stage 12, while ensuring the sealing required for the growth process.

[0028] In a preferred embodiment, the growth apparatus 10 further includes a lifting and opening mechanism 15 and a flipping mechanism 16. The lifting and opening mechanism 15 includes a telescopic actuator 151, the body of which is fixed on the first machine base 14, and the output end of which is connected to a lifting rod 152. The lifting and opening mechanism 15 drives the lifting rod 152 to move vertically through the telescopic actuator 151 (such as a hydraulic cylinder or an electric push rod), thereby realizing the overall lifting and lowering of the upper cover 13, providing space for the operation of the flipping mechanism 16, making the opening operation more labor-saving and safer.

[0029] In a preferred embodiment, the flip-top mechanism 16 includes a first rotating seat 161, a swing arm 162, and a lifting actuator 163. The first rotating seat 161 is fixed to the top of the lifting rod 152. The middle part of the swing arm 162 is rotatably connected to the first rotating seat 161, and one end of the swing arm 162 is fixedly connected to the upper cover 13. The body of the lifting actuator 163 is fixed to the lifting rod 152, and the driving end of the lifting actuator 163 is rotatably connected to the other end of the swing arm 162. The flip-top mechanism 16 drives the swing arm 162 to rotate around the first rotating seat 161 via the lifting actuator 163, thereby causing the upper cover 13 to open or close around the hinge point. This design enables the upper cover 13 to open and close at a large angle, greatly facilitating comprehensive operation and observation of the interior of the reaction chamber 101, especially the deposition stage 12.

[0030] In a preferred embodiment, a lifting controller 17 is provided inside the base 11 to control the lifting height of the deposition stage 12 within the reaction chamber 101. The lifting controller 17 (such as a lead screw mechanism driven by a stepper motor) can precisely adjust the height position of the deposition stage 12 within the reaction chamber 101. This helps to place the diamond sheet 20 in the optimal area of ​​the plasma torch 42 to control the deposition rate and uniformity of the thin film 21, which is a key means of optimizing process parameters.

[0031] In other embodiments, a rotation controller can be provided inside the base 11 to control the rotation of the deposition stage 12. By adding a rotation controller (such as a servo motor-driven rotary table), the deposition stage 12 can rotate at a uniform speed during the growth process. This can further promote the uniform distribution of the reactive gas 41 on the surface of the diamond wafer 20, effectively improve the local non-uniformity that may exist in the plasma 42, thereby obtaining a solid film 21 with more uniform thickness and properties.

[0032] In a preferred embodiment, the height adjustment mechanism 32 includes a second platform 321, a scissor lift 322 fixed on the second platform 321, and a tensioning actuator 323 for driving the scissor lift 322 to move up and down. The height adjustment mechanism 32 drives the scissor lift 322 to move up and down through the tensioning actuator 323 (such as a lead screw module), thereby causing the entire upper angle adjustment mechanism 33, the distance adjustment mechanism 34, and the laser 31 to move in the vertical direction, realizing coarse and fine adjustment of the laser beam focus in the vertical direction, ensuring that it can be accurately aligned with diamond sheet 20 samples at different heights.

[0033] In a preferred embodiment, the angle adjustment mechanism 33 includes a second rotating seat 331, a support plate 332, a lead screw module 333, and a connecting rod 334. The second rotating seat 331 is fixed to the top of the scissor lift 322. One end of the support plate 332 is rotatably connected to the second rotating seat 331. The lead screw module 333 includes a lead screw 3331 mounted on the scissor lift 322 via a lead screw seat, a slider 3332 threadedly engaged with the lead screw 3331, and a rotation driver 3333 connected to one end of the lead screw 3331 for driving its rotation. One end of the connecting rod 334 is rotatably connected to the lower middle part of the support plate 332, and the other end of the connecting rod 334 is rotatably connected to the slider 3332. The rotation driver 3333 drives the lead screw 3331 to rotate, causing the slider 3332 to move linearly along the lead screw 3331. The slider 3332 pushes or pulls the support plate 332 via the connecting rod 334, causing it to rotate around the second rotating seat 331, thereby changing the pitch angle of the laser 31 fixed on the support plate 332. This is the key mechanism for achieving the laser beam incident at the optimal angle (25°-45°).

[0034] In a preferred embodiment, the ranging adjustment mechanism 34 includes a linear module 341 fixed on the support plate 332, and a laser 31 fixed on the slide of the linear module 341. The ranging adjustment mechanism 34 drives the laser 31 to move back and forth in the horizontal direction via the linear module 341 (such as a lead screw module or a linear motor module), directly adjusting the distance (20-100mm) between the laser probe and the detection window 131. Controlling this distance optimizes the size of the laser focused spot at the edge of the diamond sheet 20, achieving the collection of high-intensity Raman signals.

[0035] This embodiment also discloses an in-situ Raman testing method for diamond growth, which uses Raman testing equipment and includes the following steps: S1. Equipment preparation and process parameter initialization A circular molybdenum stage with a diameter of 10 mm is used as the deposition stage 12, and a diamond sheet 20 is placed on the deposition stage 12.

[0036] Close the upper cover 13 and the base 11 to create a sealed environment in the reaction chamber 101.

[0037] like Figure 7 As shown, reaction gas 41 is introduced into reaction chamber 101, wherein hydrogen is used as carrier gas and plasma source gas, and methane is used as carbon source. The flow ratio of hydrogen to methane is preferably 100:1 to 500:1.

[0038] The microwave plasma chemical vapor deposition system is activated, and the microwave power is adjusted to generate a stable microwave plasma 42 within the reaction chamber 101. The pressure within the chamber is controlled to be between 5 kPa and 15 kPa, and the temperature is raised to the diamond growth temperature range of 800°C to 1200°C. During this process, the plasma 42 activates the reactive gas 41, causing it to undergo a chemical reaction on the surface of the diamond sheet 20, thus initiating the deposition and growth of a solid thin film 21.

[0039] S2. Laser Path Alignment and Parameter Optimization This step is accomplished collaboratively by three adjustment mechanisms of the Raman laser testing device 30 to ensure that the laser beam can be effectively incident and focused on the optimal signal region, specifically including: S21. Coarse height adjustment and angle setting: The scissor lift 322 is driven by the tensioning driver 323 of the height adjustment mechanism 32 to adjust the laser 31 to the approximate height.

[0040] S22, Operating angle adjustment mechanism 33: Start the rotation driver 3333 to drive the lead screw 3331 to rotate, which drives the slider 3332 to move. The slider 3332 pushes the support plate 332 to rotate around the second rotating seat 331 through the connecting rod 334, thereby accurately adjusting the detection angle θ of the laser 31 to the optimal incident angle range of 25° to 45°.

[0041] S23. Working distance fine adjustment: Start the linear module 341 of the ranging adjustment mechanism 34 to drive the laser 31 to move in the horizontal direction, and precisely adjust the distance L between the laser probe and the detection window 131 to the range of 20mm to 100mm to ensure that the laser spot can be minimized and clearly focused on the edge area of ​​the diamond sheet 20 (after multiple tests, the signal at the edge area of ​​the diamond sheet 20 is the best).

[0042] S24. Wavelength Selection: Activate laser 31, using a 473nm wavelength laser as the excitation source. This wavelength was selected after analyzing the microwave plasma interference spectrum, effectively avoiding the strong luminous background interference of plasma 42.

[0043] S3. Real-time acquisition and monitoring of in-situ Raman signals While maintaining the above MPCVD growth conditions (such as temperature 900℃, pressure 10kPa, microwave power 3000W), the laser beam is continuously irradiated with optimized parameters (θ=30°, L=50mm) at the edge of the growing solid film 21.

[0044] Raman scattering signals are acquired and recorded in real time. This process continues throughout the entire growth cycle (e.g., for several hours, with spectra acquired every 10 minutes), thereby enabling dynamic monitoring of the entire deposition process.

[0045] S4. Test Result Analysis and Characterization The collected Raman spectra were analyzed, and the specific characterization results are as follows: S41. Diamond phase identification and quality assessment: such as... Figure 8 As shown, at a Raman displacement of approximately 1332 cm -1 A sharp characteristic peak was observed, which is a hallmark of the diamond sp³ bond structure. The high intensity and sharp shape of this peak indicate that the in-situ grown solid film 21 has good crystallinity. By monitoring the changes in the peak position (reflecting stress), peak width (reflecting crystallinity), and intensity of this characteristic peak over time, the growth quality and structural evolution of the solid film 21 can be evaluated in real time.

[0046] S42. Real-time tracking of the growth process: such as Figure 9 As shown, a series of in-situ Raman spectra measured at 10-minute intervals within a growth temperature range of 300-900℃ clearly demonstrate the evolution of the diamond characteristic peaks (peaks shown in the figure) over growth time. Although at 800 cm⁻¹... -1 While there may be interfering peaks from gases such as methane in the vicinity, the diamond characteristic peaks remain clearly visible and have the highest intensity. This demonstrates that the testing system can effectively capture the diamond growth signal in the complex MPCVD process environment, enabling in-situ online detection.

[0047] S5. Process Parameter Feedback and Optimization Based on the Raman signal characteristics obtained from the real-time analysis in step S4 (e.g., 1332 cm⁻¹), -1 The process parameters of MPCVD are dynamically adjusted to optimize growth quality, including peak intensity, full width at half maximum (FWHM), and peak position.

[0048] For example: if the Raman spectrum is at 1350 cm⁻¹ -1and 1580 cm -1 The presence of a non-diamond carbon phase (sp² carbon, i.e., D and G bands) signal nearby indicates a tendency for graphitization in the solid film 21. In this case, the concentration of methane in the reaction gas 41 can be reduced promptly, or the plasma power 42 can be adjusted. Conversely, if the diamond characteristic peaks are strong and sharp, parameters can be maintained or fine-tuned to ensure stable, high-quality growth. This real-time feedback mechanism significantly shortens the process optimization cycle and improves the repeatability and controllability of the growth process.

[0049] In summary, this invention, through the above-described method, deeply integrates Raman spectroscopy detection with the MPCVD growth process, and successfully solves the problem of in-situ monitoring in a high-temperature plasma environment by utilizing specific equipment structures and optimized test parameters, providing strong technical support for the controllable preparation of high-quality diamonds.

[0050] The preferred embodiments of the present invention have been described in detail above, but the present invention is not limited to the embodiments described. Those skilled in the art can make various equivalent modifications or substitutions without departing from the spirit of the present invention, and these equivalent modifications or substitutions are all included within the scope defined by the claims of the present invention.

Claims

1. A diamond growth in-situ Raman testing device, comprising a growth apparatus (10), the growth apparatus (10) comprising a base (11), a deposition stage (12), and an upper cover (13), the upper cover (13) cooperating with the base (11) to form a reaction chamber (101), the deposition stage (12) being disposed within the reaction chamber (101), the deposition stage (12) being used to place a diamond sheet (20); characterized in that, The upper cover (13) is provided with a detection window (131), and a Raman laser testing device (30) is provided outside the detection window (131). The Raman laser testing device (30) includes: A laser (31) is used to generate a laser beam. Its laser probe is located outside the detection window (131). The laser beam passes through the detection window (131) and enters the reaction chamber (101), and is focused on the edge of the diamond sheet (20) placed on the deposition stage (12). A height adjustment mechanism (32) is used to control the laser (31) to move vertically; An angle adjustment mechanism (33) is connected to the output end of the height adjustment mechanism (32) and is used to control the detection angle of the laser (31); The ranging adjustment mechanism (34) is connected to the output end of the angle adjustment mechanism (33) and is used to control the distance between the laser probe of the laser (31) and the detection window (131).

2. The in-situ Raman testing equipment for diamond growth according to claim 1, characterized in that, The growth device (10) also includes a first machine base (14), the base (11) is fixed on the first machine base (14), and the upper cover (13) is sealed to the base (11) in an openable and closable manner.

3. The in-situ Raman testing equipment for diamond growth according to claim 2, characterized in that, The growth device (10) further includes a lifting and opening mechanism (15) and a flipping mechanism (16), wherein the lifting and opening mechanism (15) includes: The telescopic actuator (151) has its body fixed on the first machine base (14) and its output end is connected to a lifting rod (152). The flip-top mechanism (16) includes: The first rotating seat (161) is fixed to the top of the lifting rod (152); The swing arm (162) has its middle part rotatably connected to the first rotating seat (161), and one end of it is fixedly connected to the upper cover (13); The lifting drive (163) is fixed to the lifting rod (152), and its driving end is rotatably connected to the other end of the swing arm (162).

4. The in-situ Raman testing equipment for diamond growth according to claim 1, characterized in that, The base (11) is provided with a lifting controller (17) on its inner side, which is used to control the lifting height of the deposition stage (12) in the reaction chamber (101).

5. The in-situ Raman testing equipment for diamond growth according to claim 1, characterized in that, The height adjustment mechanism (32) includes a second machine base (321), a scissor lift (322) fixed on the second machine base (321), and a tensioning driver (323) for driving the scissor lift (322) to rise and fall. The angle adjustment mechanism (33) includes: The second rotating seat (331) is fixed to the top of the scissor lift (322); The tray (332) has one end rotatably connected to the second rotating seat (331); The lead screw module (333) includes a lead screw (3331) mounted on the scissor lift (322) via a lead screw seat, a slider (3332) threadedly engaged with the lead screw (3331), and a rotary actuator (3333) connected to one end of the lead screw (3331) for driving its rotation. The connecting rod (334) has one end rotatably connected to the middle of the lower end of the support plate (332), and the other end rotatably connected to the slider (3332); The ranging adjustment mechanism (34) includes a linear module (341) fixed on the tray (332), and the laser (31) is fixed on the slide of the linear module (341).

6. A method for in-situ Raman testing of diamond growth, characterized in that, The method of using the Raman testing apparatus as described in any one of claims 1-5 includes the following steps: The laser probe of the laser (31) is set outside the detection window (131). The laser beam emitted by the laser (31) passes through the detection window (131) and enters the reaction chamber (101), and is focused on the edge of the diamond sheet (20) placed on the deposition stage (12) to detect the in-situ Raman signal of diamond growth in real time.

7. The in-situ Raman spectroscopy method for diamond growth according to claim 6, characterized in that, Before detecting the Raman signal, the position and angle of the laser probe need to be adjusted, specifically including: The incident angle θ of the laser beam is adjusted to 25° to 45° by means of the height adjustment mechanism (32), the angle adjustment mechanism (33) and the distance adjustment mechanism (34), and the distance L between the laser probe and the detection window (131) is adjusted to 20mm to 100mm.

8. The in-situ Raman spectroscopy method for diamond growth according to claim 6 or 7, characterized in that, The laser (31) uses a laser wavelength of 473nm.

9. The in-situ Raman testing method for diamond growth according to claim 6, characterized in that, The diameter of the detection window (131) is 15 mm to 30 mm.

10. The in-situ Raman spectroscopy method for diamond growth according to claim 6, characterized in that, The real-time detection of Raman signals also includes the step of adjusting the process parameters of microwave plasma chemical vapor deposition based on the characteristics of the Raman signal to optimize the diamond growth quality.

Citation Information

Patent Citations

  • Microwave plasma chemical vapor deposition device

    CN213142184U