A device and method for preparing a diamond film glass substrate based on laser deposition
By precisely controlling laser parameters and gas flow, and combining machine learning models to optimize the diamond film deposition process, the problem of uneven diamond film deposition on glass substrates was solved, the film quality and substrate performance were improved, making it suitable for high-performance chip manufacturing.
Patent Information
- Application Number
- CN202411722915.3
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2024-11-28
- Publication Date
- 2025-09-30
- Estimated Expiration
- 2044-11-28
AI Technical Summary
In the process of depositing diamond films on glass substrates in existing technologies, the selection and control of laser parameters are not precise enough, resulting in uncertainty in the quality and uniformity of the film layer, affecting the thermal expansion and electrical conductivity of the substrate.
By precisely controlling laser power, pulse frequency, and focal position, combined with a machine learning-based gas flow prediction model and an adaptive frequency adjustment algorithm, the diamond film deposition process is optimized, and the film quality is improved using a segmented annealing method.
The uniform growth and high-quality adhesion of the diamond film are achieved, the performance and stability of the film layer are improved, the thermal expansion and mechanical strength of the substrate are increased, and the reliability of the chip is enhanced.
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Figure CN119753619B_ABST
Abstract
Description
Technical Field
[0001] The present invention relates to the technical field of laser deposition, and in particular to a device and method for preparing a diamond film glass substrate based on laser deposition. Background Art
[0002] With the rapid development of electronic technology, the use of traditional silicon substrates in high-performance chip manufacturing has gradually faced numerous challenges. In recent years, glass substrates have gradually become a new alternative to silicon substrates due to their superior optical properties, thermal stability, and lightweight advantages. However, glass substrates still need to be improved in terms of thermal expansion and electrical conductivity of electronic devices.
[0003] Laser deposition technology, as an emerging thin film fabrication method, has been widely used in the semiconductor and optoelectronic fields by depositing high-quality functional thin films on substrate surfaces. In this process, a laser beam is irradiated onto the substrate surface with high energy density, vaporizing or melting the material and redepositing it to form the desired thin film.
[0004] While existing technologies have enabled the deposition of various thin films on glass substrates, the selection and control of laser parameters remains crucial during diamond film deposition. Laser parameters such as laser power, pulse frequency, and beam focus position are often treated as fixed values, which can lead to uncertainty in film quality and uniformity during deposition. For example, changes in laser power directly affect the growth rate and structural characteristics of diamond films, while laser pulse frequency influences the deposited film thickness and density. Summary of the Invention
[0005] In view of this, the present invention proposes a device and method for preparing a diamond film glass substrate based on laser deposition, which is used to solve the problem of how to improve the quality of the diamond film layer and the performance of the substrate by precisely controlling the precursor gas flow rate and laser parameters.
[0006] The technical solution of the present invention is achieved as follows: The present invention provides a method for preparing a diamond film glass substrate based on laser deposition, comprising the following steps:
[0007] S1, selecting a glass material to prepare a substrate and preparing a diamond film precursor gas mixture;
[0008] S2, placing the substrate in a vacuum environment, delivering a configured diamond film precursor gas mixture into the vacuum environment, and performing laser deposition on the substrate surface to uniformly cover the substrate with a diamond film;
[0009] S3, annealing the diamond film deposited on the substrate and detecting surface properties.
[0010] On the basis of the above technical solutions, preferably, in step S1 , methane and hydrogen are selected as precursor gases, and the mixing ratio of methane and hydrogen is set according to deposition conditions and expected film properties.
[0011] More preferably, in step S2, when the diamond film precursor gas mixture is transported into the vacuum environment where the substrate is located, a gas flow prediction model based on machine learning is introduced. By learning from previous experimental data, the changing trend of the gas flow of methane and hydrogen is predicted and dynamically adjusted to provide an ideal precursor gas environment for laser deposition of diamond film on the substrate surface, so as to avoid sudden gas flow fluctuations affecting the deposition effect.
[0012] More preferably, the prediction model for the gas flow rate change trend of methane and hydrogen is,
[0013] ,
[0014] Where t is time, and are the predicted flow rates of methane and hydrogen at the next time step at time t, X ( t ) is the input feature matrix of the model. The input features of the model include historical gas flow data of methane and hydrogen, environmental conditions and equipment parameters. h t-1 is the hidden state at time t-1, θ are the trainable parameters of the model;
[0015] The adjustment formulas for dynamically adjusting the gas flow rates of methane and hydrogen are:
[0016] ,
[0017] ,
[0018] in, and are the gas flow rates of methane and hydrogen after adjustment in the next time step, and is the gas flow rate of methane and hydrogen in the current time step, α is the adjustment coefficient and is used to smooth the change of gas flow rate. The value range of α is between 0 and 1.
[0019] On the basis of the above technical solution, preferably, in step S2, the deposition rate of the diamond film on the substrate is adjusted by adjusting the laser power and pulse frequency. The calculation formula of the deposition rate is:
[0020] R=( f ×A) / D,
[0021] Where R is the deposition rate, f is the pulse frequency, A is the thickness of material deposited per pulse, and D is the effective area of the substrate.
[0022] More preferably, in step S2, the deposition rate and the deposition thickness of the diamond film are monitored during the laser deposition process, and an adaptive frequency adjustment algorithm based on machine learning is introduced to optimize the pulse frequency. The adjustment algorithm formula is:
[0023] f new = f old +β×(R target -R measured ),
[0024] Among them, β is the pulse frequency adjustment coefficient, R target is the target deposition rate, R measured The deposition rate is monitored in real time. Through adaptive adjustment, the optimal frequency control is achieved under different film thicknesses.
[0025] On the basis of the above technical solution, preferably, in step S2, the focus of the laser is adjusted so that the laser is focused on the surface of the glass substrate. The calculation formula of the spot diameter D of the laser focus is:
[0026] D = (2 × λ × F) / (π × D0),
[0027] Wherein, λ is the laser wavelength, F is the focal length of the focusing lens, F ranges from 50 mm to 100 mm, D0 is the input diameter of the laser beam, and D ranges from 50 μm to 200 μm.
[0028] On the basis of the above technical solution, preferably, in step S3, the diamond film is annealed by a segmented annealing method, and the temperature distribution formula during annealing can be expressed as:
[0029] T(t)=T0+ΔT×sin(πt / t f ),
[0030] Where T0 is the initial temperature, ΔT is the temperature variation range, t is the deposition time, t f is the end time of the annealing process.
[0031] On the basis of the above technical solution, preferably, in step S3, when detecting the surface characteristics of the diamond film, an ellipsometer or a step meter is used to measure the thickness of the diamond film, and confirm whether the thickness of the diamond film meets the design requirements; and the uniformity of the film layer is evaluated by detecting multiple positions of the diamond film, and the tolerance range of the film thickness is ±10%.
[0032] On the other hand, the present invention provides a device for preparing a diamond film glass substrate based on laser deposition, which is used for the above-mentioned method for preparing a diamond film glass substrate based on laser deposition, including a vacuum chamber in which a substrate is arranged; a laser device, which emits laser into the vacuum chamber and is used to laser deposit a diamond film on the surface of the substrate; a gas delivery system, which delivers a configured diamond film precursor gas mixture into the vacuum chamber; a control unit, which is electrically connected to the vacuum chamber, the laser device and the gas delivery system, the control unit monitors and adjusts the power, pulse frequency and focal position of the laser device in real time, the control unit adjusts the flow rate and proportion of the diamond film precursor gas mixture delivered by the gas delivery system, and the control unit monitors the vacuum degree and environmental parameters of the vacuum chamber.
[0033] The device and method for preparing a diamond film glass substrate based on laser deposition of the present invention have the following beneficial effects compared with the prior art:
[0034] (1) During the deposition process, key parameters such as laser power, pulse frequency, and laser focus position are monitored. By precisely controlling these parameters of the laser system, the laser energy is ensured to be accurately focused on the surface of the glass substrate, achieving uniform growth and high-quality adhesion of the diamond film, and significantly improving the performance and stability of the film layer.
[0035] (2) By setting specific laser parameters, the effects of laser power, spot diameter, wavelength, and pulse frequency on the growth of diamond films were taken into account. By utilizing the optimized combination of these parameters, the crystal structure and thickness of the diamond film were more accurately controlled. Through inverse process simulation and adjustment, high precision and consistency of the film layer were achieved. This enabled the substrate to have better thermal expansion and mechanical strength, thereby improving the performance and reliability of the chip.
[0036] (3) During the deposition process, a precisely configured precursor gas mixture is used and laser deposition is performed in a vacuum environment, which reduces the generation of impurities and defects. At the same time, by annealing the deposited diamond film and testing its surface properties, dynamic changing factors such as time and temperature are taken into account, and the crystal quality and surface flatness of the film layer are improved more accurately, thereby improving the overall performance and application prospects of the substrate. BRIEF DESCRIPTION OF THE DRAWINGS
[0037] In order 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. Obviously, the drawings described below are only some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying any creative work.
[0038] Figure 1 is a flow chart of the preparation method of the present invention;
[0039] Figure 2 Schematic diagram of the preparation device of the present invention. DETAILED DESCRIPTION
[0040] The following will be combined with the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the embodiments described 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.
[0041] like Figure 1 As shown, the present invention provides a method for preparing a diamond film glass substrate based on laser deposition, comprising the following steps:
[0042] S1. Prepare substrate 1 from a glass material and clean its surface to remove contaminants. Simultaneously, prepare a diamond film precursor gas mixture. The type of glass substrate is selected based on application requirements. Common materials include: 1) Borosilicate glass (e.g., Corning 7740): offers excellent thermal stability and chemical resistance. 2) Aluminosilicate glass (e.g., Corning 7059): offers high transmittance and a low thermal expansion coefficient. 3) Soda-lime glass: economical and practical for general applications. Select an appropriate glass substrate thickness based on equipment requirements and final product performance, typically between 0.5 mm and 2 mm. Thicker substrates offer improved thermal stability and mechanical strength. Depending on the degree of contamination on the glass substrate, select an appropriate cleaning method. These methods include: ultrasonic cleaning using an ultrasonic cleaner, immersing substrate 1 in deionized water or a cleaning agent, typically at an ultrasonic frequency of 40 kHz for 5-10 minutes; and chemical cleaning using ethanol or acetone, immersing and wiping substrate 1 to remove organic matter and oil. After cleaning is completed, use an optical microscope or a scanning electron microscope (SEM) to check the cleaning effect on the surface of the substrate 1 to ensure that there is no obvious dirt or particles remaining on the surface.
[0043] Before laser deposition, the surface roughness of the glass substrate 1 can be adjusted through mechanical polishing or chemical mechanical polishing (CMP), depending on the requirements for diamond film deposition. The target roughness is generally Ra < 5nm to ensure uniform thin film deposition. Plasma treatment or flame treatment techniques are also used to create highly active sites on the substrate 1 surface, enhancing the adhesion of the diamond film. The cleaned surface topography is examined using an atomic force microscope (AFM) or scanning electron microscope (SEM) to assess surface flatness and roughness to ensure that it meets deposition requirements. A contact angle meter can also be used to measure the contact angle of a water droplet on the substrate 1 surface to assess its surface hydrophilicity and energy, ensuring suitability for subsequent diamond film deposition.
[0044] S2, placing substrate 1 in a vacuum environment, delivering the configured diamond film precursor gas mixture into the vacuum environment, and performing laser deposition on the surface of substrate 1, so that the diamond film is evenly covered on substrate 1. Specific steps include: ensuring that the laser parameters (power, frequency, and focus) are adjusted to appropriate values (e.g., power: 500mW, frequency: 2kHz); starting the delivery of the gas mixture, ensuring a stable gas flow rate, typically setting the methane (CH4) flow rate to 100sccm and the hydrogen (H2) flow rate to 900sccm; and setting the deposition time based on the required film thickness. Common deposition time ranges are: 30 minutes to 1 hour for thin films, with target thicknesses between 500nm and 1µm; and 1 to 3 hours for thick films, with target thicknesses between 1µm and 5µm.
[0045] S3, annealing and surface characterization of the diamond film deposited on substrate 1 to improve film quality and performance. X-ray diffraction (XRD) analysis is performed to evaluate the crystal structure and quality of the film, with the goal of improving the crystallinity and purity of the film. The XRD pattern should show obvious diamond characteristic peaks, indicating good film quality. The interplanar spacing d is calculated using Bragg's law as 2dsin θ =nλ, where θ is the diffraction angle; λ is the X-ray wavelength (typically 0.15406 nm); and n is the diffraction order, usually 1. Scanning electron microscopy (SEM) or atomic force microscopy (AFM) is used to observe the surface morphology of the film and assess grain size and surface roughness, with a roughness Ra of less than 10 nm being ideal. Raman spectroscopy is used to assess the quality of diamond films. Diamond has a characteristic peak at 1332 cm⁻¹, and its peak intensity and full width at half maximum can be used to assess crystal quality.
[0046] When evaluating the annealing effect of diamond films, comparing XRD and Raman spectra before and after annealing reveals an increase in the intensity of characteristic peaks and a decrease in the full width at half maximum, indicating improved crystal quality. The film internal stress, σ, is calculated as (E / (1-ν))×(Δd / d), where E is the Young's modulus (approximately 1050 GPa for diamond). νis the Poisson's ratio (about 0.1); Δd / d represents the relative change in the interplanar spacing. According to the stress and crystal quality, adjust the annealing temperature and time. For example, when the stress is too large, the annealing temperature can be reduced to 650°C or the cooling time can be extended. Record the experimental data in the database to establish a relationship model between annealing parameters and film properties. Linear regression or machine learning methods can be used for model fitting to obtain the model y=β0+β1T+β2t+β3σ+ϵ, where y is the film property (such as hardness, thermal conductivity, etc.), T is the annealing temperature, t is the annealing time, σ is the stress in the film, and ϵ is the error term. Nanoindentation test is performed on the diamond film to determine the hardness 𝐻 and Young's modulus 𝐸 of the film. The hardness calculation formula is H=P max / A, where P max is the maximum load, and A is the contact area. The thermal diffusivity α of the diamond film is tested using the laser flash method, and then the thermal conductivity κ is calculated as α×ρ× C p , ρ is the density (diamond is about 3.51g / cm³), C p The specific heat capacity is approximately 0.52 J / g·K. The four-probe method was used to measure the resistivity of the diamond film: ρ = (V / I) × (π / ln²), where V is voltage and I is current. Mechanical, thermal, and electrical properties were comprehensively evaluated to assess whether the diamond film meets application requirements. Compared with traditional substrate materials, the advantages of diamond-coated glass substrates, such as high thermal conductivity, high hardness, and electrical insulation, were highlighted. By combining multiphysics simulation with experimental data, mechanical, thermal, and electrical performance models of the film were constructed to predict its performance in different applications.
[0047] exist Figure 1 In a preferred embodiment shown, in step S1, methane and hydrogen are selected as precursor gases, and the mixing ratio of methane and hydrogen is set according to deposition conditions and desired film properties. Methane (CH4) is the primary precursor gas, suitable for diamond film deposition, with its concentration typically ranging from 1% to 10%. Hydrogen (H2) is used to dilute the methane and provide a reducing environment to ensure diamond film quality, and its concentration can exceed 90% of the mixed gas. Other gases, such as ethylene (C2H4), are often included to adjust film properties, but their proportions must be carefully controlled.
[0048] A methane to hydrogen volume ratio of 1:9 is typically suitable for depositing most diamond films. Adjusting the methane concentration can optimize the film's hardness and conductivity, while higher methane concentrations can increase the film's growth rate.
[0049] Use the following formula to calculate the required gas volumes of methane and hydrogen:
[0050] V (CH4) =Vtotal ×C (CH4) / (C (CH4) +C (H2) ),
[0051] V (H2) =V total ×C (H2) / (C (CH4) +C (H2) ),
[0052] Among them, V total is the total gas volume, C (CH4) with C (H2) are the concentrations of methane and hydrogen, respectively.
[0053] Based on this calculation, combined with the real-time feedback control system, the time function of gas flow is introduced to dynamically calculate and adjust the gas flow. The time function is,
[0054] V (CH4) (t)=V total (t)×C (CH4) (t) / (C (CH4) (t)+C (H2) (t)),
[0055] The gas flow rate can be adjusted in real time as a function of time to optimize the deposition rate of the film layer.
[0056] exist Figure 1 In a preferred embodiment shown, in step S2, when the diamond film precursor gas mixture is transported into the vacuum environment where the substrate 1 is located, a gas flow prediction model based on machine learning is introduced to predict the changing trend of the gas flow of methane and hydrogen and dynamically adjust it to provide an ideal precursor gas environment for laser deposition of diamond film on the surface of the substrate 1.
[0057] exist Figure 1 In a preferred embodiment shown, a time series prediction model, such as a long short-term memory network (LSTM) or a regression model, can be used to predict the changing trend of gas flow. The following is a detailed description of using a machine learning model to predict gas flow and dynamically adjust it:
[0058] 1) Determine the model's data input type and preprocess the data. The input data includes: historical gas flow data (e.g., methane and hydrogen flow); environmental conditions (such as temperature and pressure), set as E(t); and device parameters (such as current laser power and gas mixture ratio), set as P(t). We combine these data into an input feature matrix X(t) = [V (CH4) (t),V (H2) (t), E(t), P(t)], where t represents time.
[0059] 2) LSTM (Long Short-Term Memory) is used as the prediction model. LSTM is suitable for processing time series data and can learn time dependencies. The basic structure of the LSTM model is as follows:
[0060] h t =LSTM(X(t), h t-1 ),
[0061] in, h t It is the hidden state (memory state) at time t, which is obtained by inputting the feature X(t) and the previous hidden state h t-1 Joint decision.
[0062] The predicted output is the gas flow at the next time step t+1 ,
[0063] ,
[0064] in, f () is the traffic prediction function obtained through the LSTM network.
[0065] 3) Using mean square error (MSE) as the loss function, calculate the difference between the predicted value and the actual gas flow rate,
[0066] ,
[0067] Where N is the time step of the prediction, is the predicted value of the model at the t+i time step, V ( t + i ) is the actual gas flow rate. The loss function is optimized through backpropagation and gradient descent, and the parameters of the LSTM model are updated to make the prediction results more accurate.
[0068] 4) The prediction model for the gas flow rate change trend of methane and hydrogen is:
[0069] ,
[0070] Where t is time, and are the predicted flow rates of methane and hydrogen at the next time step at time t, X ( t ) is the input feature matrix of the model. The input features of the model include historical gas flow data of methane and hydrogen, environmental conditions and equipment parameters. h t-1is the hidden state at time t-1; θ This is a trainable parameter of the model, updated with each new data input, making the model more adaptable to dynamic changes in gas flow. This machine learning-based gas flow prediction model allows the system to predict gas flow trends in advance and dynamically adjust based on the predicted results, thereby minimizing the impact of gas flow fluctuations on the deposition process and ensuring high-quality diamond film deposition.
[0071] 5) Based on the predicted gas flow, the closed-loop control algorithm is used to dynamically adjust the gas flow of methane and hydrogen. The adjustment formulas are:
[0072] ,
[0073] ,
[0074] in, and are the gas flow rates of methane and hydrogen after adjustment in the next time step, and is the gas flow rate of methane and hydrogen at the current time step, α is the adjustment coefficient and is used to smooth the change of gas flow rate, and the value range of α is between 0 and 1.
[0075] exist Figure 1 In a preferred embodiment shown in FIG. 1 , in step S2, the deposition rate of the diamond film on the substrate 1 is adjusted by adjusting the laser power and pulse frequency. The deposition rate is calculated as follows: R=( f ×A) / D, where R is the deposition rate, f is the pulse frequency, A is the thickness of material deposited per pulse, and D is the active area of substrate 1. The pulse frequency range is 1 Hz to 10 kHz, which facilitates adjustment of deposition rate and film quality. Specifically, low frequencies (1-500 Hz) are suitable for thick film deposition, allowing sufficient material cooling; medium frequencies (500 Hz-2 kHz) are suitable for depositing films of moderate thickness; and high frequencies (2 kHz-10 kHz) are suitable for rapid thin film deposition.
[0076] exist Figure 1In a preferred embodiment shown, in step S2, the deposition rate and the deposition thickness of the diamond film are monitored during the laser deposition process. Specifically, a monitoring device (such as an optical microscope, RHEED) is used to monitor the growth of the film layer in real time to ensure the uniformity and quality of the film layer. The growth rate of the film layer is R=D / t, where R is the deposition rate (in nm / s), D is the film thickness (in nm), and t is the deposition time (in s). For example, if the film thickness target is 1µm and the deposition time is 1 hour (3600s), then the deposition rate R=1000nm / 3600s≈0.28nm / s. An adaptive frequency adjustment algorithm based on machine learning is introduced to optimize the pulse frequency, and the adjustment algorithm formula is,
[0077] f new = f old +β×(R target -R measured ),
[0078] Among them, β is the pulse frequency adjustment coefficient, R target is the target deposition rate, R measured is the deposition rate monitored in real time.
[0079] A power meter and frequency meter can also be installed to monitor the laser power and frequency in real time to ensure their stability. The monitoring values can be set: power monitoring range: 0-1500mW; frequency monitoring range: 1Hz-10kHz.
[0080] At the same time, a feedback mechanism is set to ensure real-time adjustment of laser parameters. PID control algorithm can be used to adjust to keep laser parameters stable. The algorithm formula is:
[0081] ,
[0082] Among them, u(t) is the control output, e(t) is the current error, K p , K i , K d are proportional, integral, and differential gains respectively.
[0083] exist Figure 1 In a preferred embodiment shown in FIG. 1 , in step S2 , the focus of the laser is adjusted so that the laser is focused on the surface of the glass substrate 1 . The calculation formula for the spot diameter D of the laser focus is:
[0084] D = (2 × λ × F) / (π × D0),
[0085] Wherein, λ is the laser wavelength, F is the focal length of the focusing lens, F ranges from 50 mm to 100 mm, D0 is the input diameter of the laser beam, and D ranges from 50 μm to 200 μm.
[0086] exist Figure 1 In a preferred embodiment shown, in step S3, the common annealing temperature range is 500°C to 800°C. The annealing time depends on the film thickness and the required crystal quality. Generally, the annealing time is 30 minutes to 2 hours. For example, for a film with a thickness of 1µm, the annealing time can be set to 1 hour. Annealing should be carried out in an inert gas (such as argon) or a high vacuum (<10⁻ 4 Pa) environment to prevent film oxidation. The gas purity should reach 99.999% to ensure a clean environment. The heating and cooling rates are controlled to prevent the film from cracking due to thermal stress. The heating and cooling rate is 5°C / min. The diamond film is annealed using the segmented annealing method. The temperature distribution formula during annealing can be expressed as:
[0087] T(t)=T0+ΔT×sin(πt / t f ),
[0088] Where T0 is the initial temperature, ΔT is the temperature variation range, t is the deposition time, t f is the end time of the annealing process.
[0089] exist Figure 1 In a preferred embodiment shown in FIG. 1 , in step S3 , when detecting the surface characteristics of the diamond film, an ellipsometer or a step profiler is used to measure the thickness of the diamond film, and the calculation formula is:
[0090] ,
[0091] And confirm whether the thickness of the diamond film meets the design requirements; and evaluate the uniformity of the film layer (for example, 1µm) by testing multiple locations of the diamond film. The tolerance range of the film thickness is ±10%.
[0092] like Figure 2 As shown, a diamond film glass substrate preparation device based on laser deposition of the present invention is used in a diamond film glass substrate preparation method based on laser deposition of any of the above embodiments, including a vacuum chamber 2, a laser device 3, a gas delivery system 4 and a control unit 5.
[0093] The substrate 1 is placed in the vacuum chamber 2. The vacuum chamber 2 is usually made of high-temperature and corrosion-resistant materials, such as stainless steel. The volume of the vacuum chamber is between 50L and 200L to accommodate deposition of different scales; its vacuum degree is required to reach 10⁻ 5 to 10⁻ 6 Torr high vacuum environment to reduce the impact of gas molecules on the deposited film.
[0094] Use vacuum pumps (such as mechanical pumps and turbomolecular pumps) to establish a vacuum environment. Specifically, start the mechanical pump to perform initial vacuuming until the vacuum reaches 10⁻³Torr; switch to the turbomolecular pump to further increase the vacuum to the target value (10⁻³Torr). 5 to 10⁻ 6 Torr).
[0095] Laser device 3 emits laser light into vacuum chamber 2 and is used to deposit a diamond film on substrate 1. A pulsed laser (such as a Nd laser) is used as the laser emitter. Its wavelength is 1064 nm, and its peak power is adjustable from 100 mW to 1500 mW, typically set based on the required film thickness. Laser device 3 has three power levels: low power (100-300 mW), suitable for initial film growth; medium power (500-800 mW), suitable for accelerated film growth; and high power (1000-1500 mW), suitable for rapid deposition. The power required for deposition can be calculated using the formula P=E / t, where P is the power (in W), E is the required energy (in J), and t is the deposition time (in seconds).
[0096] The gas delivery system 4 delivers the configured diamond film precursor gas mixture into the vacuum chamber 2. High-precision gas flow valves are used in the gas delivery system 4 to ensure the stability and adjustability of the flow rates of each gas. A mass flow meter (MFC) is typically used for real-time monitoring and adjustment, with an accuracy of ±0.5% FS. Before the mixed gas is delivered, methane and hydrogen are introduced into a premixed gas tank and mixed evenly according to the configured ratio. A stirring device can be used to improve mixing uniformity and ensure that the mixed gas is free of external contamination. After mixing, the mixed gas is analyzed for composition using analytical techniques such as gas chromatography (GC) or mass spectrometry (MS) to ensure that the gas ratios meet expectations. Based on the test results, the gas flow rates are adjusted appropriately to ensure the stability and suitability of the gas mixture, providing an ideal precursor gas environment for subsequent laser deposition.
[0097] The control unit 5 is electrically connected to the vacuum chamber 2, the laser device 3, and the gas delivery system 4. The control unit 5 monitors and adjusts the power, pulse frequency, and focal position of the laser device 3 in real time. The control unit 5 also adjusts the flow rate and ratio of the diamond film precursor gas mixture delivered by the gas delivery system 4. The control unit 5 also monitors the vacuum level and environmental parameters of the vacuum chamber 2.
[0098] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present invention should be included in the scope of protection of the present invention.
Claims
1. A method for preparing a diamond film glass substrate based on laser deposition, characterized in that: The following steps are included: S1, selecting a glass material to prepare a substrate (1), and preparing a diamond film precursor gas mixture, selecting methane and hydrogen as precursor gases, and setting the mixing ratio of methane and hydrogen according to deposition conditions and expected film properties; S2, placing the substrate (1) in a vacuum environment, delivering the configured diamond film precursor gas mixture into the vacuum environment, and performing laser deposition on the surface of the substrate (1) so that the diamond film is evenly covered on the substrate (1); when delivering the diamond film precursor gas mixture into the vacuum environment where the substrate (1) is located, introducing a gas flow prediction model based on machine learning to predict the changing trend of the gas flow of methane and hydrogen and dynamically adjust it to provide an ideal precursor gas environment for laser deposition of diamond film on the surface of the substrate (1); the prediction model for the changing trend of the gas flow of methane and hydrogen is, , Where t is time, and are the predicted flow rates of methane and hydrogen at the next time step at time t, X ( t ) is the input feature matrix of the model. The input features of the model include historical gas flow data of methane and hydrogen, environmental conditions and equipment parameters. h t-1 is the hidden state at time t-1, θ are the trainable parameters of the model; The adjustment formulas for dynamically adjusting the gas flow rates of methane and hydrogen are: , , in, and are the gas flow rates of methane and hydrogen after adjustment in the next time step, and is the gas flow rate of methane and hydrogen at the current time step, α is the adjustment coefficient and is used to smooth the change of gas flow rate, and the value range of α is between 0 and 1; The deposition rate of the diamond film on the substrate (1) is adjusted by adjusting the laser power and pulse frequency. The calculation formula of the deposition rate is: R=( f ×A) / D, Where R is the deposition rate, f is the pulse frequency, A is the thickness of the material deposited per pulse, and D is the effective area of the substrate (1); During the laser deposition process, the deposition rate and the thickness of the diamond film are monitored, and an adaptive frequency adjustment algorithm based on machine learning is introduced to optimize the pulse frequency. The adjustment algorithm formula is: f new = f old +β×(R target -R measured ), Among them, β is the pulse frequency adjustment coefficient, R target is the target deposition rate, R measured is the deposition rate monitored in real time; S3, annealing the diamond film deposited on the substrate (1) and detecting its surface properties.
2. The method for preparing a diamond film glass substrate based on laser deposition according to claim 1, characterized in that: In step S2, the focus of the laser is adjusted so that the laser is focused on the surface of the glass substrate (1). The calculation formula for the spot diameter D of the laser focus is: D = (2 × λ × F) / (π × D0), Wherein, λ is the laser wavelength, F is the focal length of the focusing lens, F ranges from 50 mm to 100 mm, D0 is the input diameter of the laser beam, and D ranges from 50 μm to 200 μm.
3. The method for preparing a diamond film glass substrate based on laser deposition according to claim 1, wherein: In step S3, the diamond film is annealed by a segmented annealing method. The temperature distribution formula during annealing can be expressed as: T(t)=T0+ΔT×sin(πt / t f ), Where T0 is the initial temperature, ΔT is the temperature variation range, t is the deposition time, t f is the end time of the annealing process.
4. The method for preparing a diamond film glass substrate based on laser deposition according to claim 1, wherein: In step S3, when detecting the surface characteristics of the diamond film, the thickness of the diamond film is measured using an ellipsometer or a step profiler to confirm whether the thickness of the diamond film meets the design requirements; The uniformity of the diamond film is evaluated by inspecting multiple locations of the film, with a film thickness tolerance of ±10%.
5. A device for preparing a diamond film on a glass substrate based on laser deposition, characterized in that: A method for preparing a diamond film glass substrate based on laser deposition according to any one of claims 1 to 4, include, a vacuum chamber (2), in which the substrate (1) is arranged; A laser device (3) emits laser light into the vacuum chamber (2) and is used to laser-deposit a diamond film on the surface of the substrate (1); A gas delivery system (4) delivers the configured diamond film precursor gas mixture into the vacuum chamber (2); The control unit (5) is electrically connected to the vacuum chamber (2), the laser device (3) and the gas delivery system (4). The control unit (5) monitors and adjusts the power, pulse frequency and focus position of the laser device (3) in real time. The control unit (5) adjusts the flow rate and proportion of the diamond film precursor gas mixture delivered by the gas delivery system (4). The control unit (5) monitors the vacuum degree and environmental parameters of the vacuum chamber (2).
Citation Information
Patent Citations
Laser chemical gas-phase deposition process of diamond film
CN1122378A