A real-time control method and system for vacuum glow coating composition
Through the methods of holographic component acquisition and adaptive component adjustment, the vacuum glow coating process is monitored and adjusted in real time, which solves the problem of film unevenness caused by target material consumption, sample loading and temperature changes, and achieves precise control and stability of chromium nitrogen coating.
Patent Information
- Application Number
- CN202510496224.4
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2025-04-21
- Publication Date
- 2025-09-16
- Estimated Expiration
- 2045-04-21
AI Technical Summary
In the existing vacuum glow discharge coating technology, there is a lack of real-time monitoring of target material consumption, which leads to changes in the release of chromium atoms during the coating process, affecting the stability of the film composition; the sample loading density and spatial distribution affect the uniformity of glow discharge, resulting in deviations in film thickness and composition; insufficient control of film thickness affects uniform deposition; and there is a lack of dynamic compensation for temperature dependence, which affects the stability of the plasma state and the mechanical properties of the film.
Using holographic component acquisition, adaptive component adjustment, real-time adjustment strategy and film quality correction methods, multi-dimensional data is collected through sensors, the predicted value of chromium and nitrogen composition is calculated, the coating process parameters are adjusted in real time, the film quality is evaluated and necessary parameter corrections are made.
It achieves precise control of the coating process, improves the uniformity and consistency of the film layer, reduces production fluctuations, ensures product stability and quality meets standards, and improves production efficiency and process stability.
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Figure CN120006243B_ABST
Abstract
Description
Technical Field
[0001] The present invention relates to the technical field of vacuum coating, and in particular to a method and system for real-time control of the composition of vacuum glow coating. Background Art
[0002] Vacuum glow discharge coating technology has a history of several decades of development and has been increasingly widely used in various industries such as semiconductors, molds and dies, and mechanical parts. The industry is also constantly researching new processes and technologies to obtain coatings with better overall performance and wider adaptability.
[0003] The existing vacuum glow discharge excitation coating process has at least the following technical problems: 1. In actual coating production, the impact of target material consumption lacks real-time monitoring of the target material's service life and consumption status, which is not conducive to precise control of the sputtering rate, and will cause changes in the release of chromium atoms during the coating process, thereby affecting the stability of the film composition. The impact of changes in the number of samples in the furnace chamber lacks analysis of the sample loading density and spatial distribution, which is not conducive to ensuring the uniformity of glow discharge, and will lead to large deviations in the film thickness and composition of different batches of products.
[0004] 2. Most existing chromium-nitrogen coating processes lack control over film thickness, which is not conducive to ensuring uniform deposition on different types of substrates. This will lead to large deviations in film thickness on substrates with complex morphologies, affecting the final film performance. In addition, the temperature dependence lacks dynamic compensation for chamber temperature changes during long-term deposition, which is not conducive to maintaining the stability of the plasma state. This will cause the film composition to fluctuate due to temperature changes, thereby affecting the mechanical properties of the final chromium-nitrogen film. Summary of the Invention
[0005] The purpose of the present invention is to provide a method and system for real-time control of the composition of vacuum glow coating, which solves the problems existing in the background technology.
[0006] In order to solve the above technical problems, the present invention adopts the following technical solution: The present invention provides a real-time control method for the composition of vacuum glow coating, including: Step 1, holographic component acquisition: for the coating process of a specified chromium-nitrogen coating, multi-dimensional data of the specified chromium-nitrogen coating process is collected through sensors and monitoring equipment.
[0007] Step 2: Adaptive composition adjustment: Based on the multi-dimensional data of the specified chromium-nitrogen coating process, the predicted value of the chromium-nitrogen composition in the corresponding vacuum chamber during the specified chromium-nitrogen coating process is calculated, and it is evaluated whether the chromium-nitrogen coating needs adaptive composition adjustment.
[0008] Step 3. Real-time adjustment strategy: When the chromium-nitrogen coating requires adaptive composition adjustment, the coating process parameters are adjusted in real time through the designated chromium-nitrogen coating equipment management platform.
[0009] Step 4: Real-time film quality correction: After completing the adaptive adjustment of the coating process parameters, evaluate the film quality of the specified chromium nitrogen coating and analyze whether the coating process parameters need to be corrected.
[0010] In a second aspect, the present invention provides a real-time control system for the composition of vacuum glow coating, including: a holographic component acquisition module for collecting multi-dimensional data of a specified chromium nitrogen coating process through sensors and monitoring equipment.
[0011] The adaptive composition adjustment module is used to calculate the predicted value of the chromium and nitrogen composition in the corresponding vacuum chamber during the specified chromium and nitrogen coating process based on the multi-dimensional data during the specified chromium and nitrogen coating process, and to evaluate whether the chromium and nitrogen coating needs adaptive composition adjustment.
[0012] The real-time adjustment strategy module is used to adjust the coating process parameters in real time through the designated chromium nitrogen coating equipment management platform when the chromium nitrogen coating needs to be adaptively adjusted in composition.
[0013] The real-time film quality correction module is used to evaluate the film quality of the specified chromium nitrogen coating after completing the adaptive adjustment of the coating process parameters, and analyze whether the coating process parameters need to be corrected.
[0014] The beneficial effects of the present invention are: 1. A real-time control method and system for the composition of a vacuum glow coating provided by an embodiment of the present invention, during the holographic composition collection process, realizes real-time collection of multi-dimensional data, including spectral signals, film thickness, surface roughness and other parameters, which is conducive to comprehensive monitoring of the coating environment in the vacuum chamber, ensuring the accuracy of process data, and improving the controllability of the coating process. During the adaptive composition adjustment process, the chromium and nitrogen composition is predicted and calculated, and whether it needs to be adjusted is evaluated, which is conducive to early detection of coating composition deviations and avoidance of unstable film quality due to parameter drift during the deposition process.
[0015] 2. In the real-time strategy adjustment process, the embodiment of the present invention optimizes the process parameters based on the calculation results, which is conducive to the dynamic correction of nitrogen flow, target current and bias voltage, so that the coating composition can be maintained within the set range in real time, improving the uniformity and consistency of the coating. In the film quality evaluation process, the film hardness, adhesion and surface roughness are comprehensively quantitatively calculated, which is conducive to the accurate characterization of the film performance. It can also be combined with the target threshold to determine whether further process adjustment is needed to ensure that the final product meets the quality standards.
[0016] 3. In the process of predicting chromium and nitrogen concentration, the embodiment of the present invention adopts spectral measurement, plasma temperature monitoring, and gas pressure measurement, which is conducive to improving the accuracy of composition prediction and avoiding inaccurate control of coating composition due to single parameter measurement error. In the process of correcting coating process parameters, feedback control based on the quantitative value of film quality is adopted, which is conducive to accurate correction for process differences under different batches and different cavity loading conditions, reducing fluctuations in the production process, and improving product consistency and stability.
[0017] 4. In the process of optimizing the calculation formula, the embodiment of the present invention uses mathematical analysis of the nitrogen flow rate, bias voltage, and target current adjustment, which is conducive to accurately calculating the required adjustment amount, making the coating process more intelligent, reducing human intervention, and improving production efficiency. In the process of film roughness evaluation, electron microscope scanning and multi-point measurement calculation are used, which is conducive to accurately obtaining the morphological characteristics of the coating surface, optimizing deposition parameters, and improving the mechanical properties and optical quality of the film. In the process of plasma parameter monitoring, the plasma temperature and experimental calibration coefficient are calculated, which is conducive to better understanding the influence of the plasma environment on the coating composition, optimizing the coating process, and improving process stability. BRIEF DESCRIPTION OF THE DRAWINGS
[0018] 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.
[0019] Figure 1 Schematic diagram of the implementation steps of the present invention.
[0020] Figure 2 This is a schematic diagram of the system structure connection of the present invention.
[0021] Figure 3 This is a schematic diagram of the principle of the real-time composition control system for vacuum glow discharge excitation coating according to the present invention. DETAILED DESCRIPTION
[0022] 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.
[0023] See also Figure 1As shown, the present invention provides a real-time control method for the composition of vacuum glow coating, which includes: step 1, holographic component acquisition: for a specified chromium nitrogen coating process, multi-dimensional data of the specified chromium nitrogen coating process is collected through sensors and monitoring equipment.
[0024] It should be noted that the present invention uses chromium nitrogen coating as an example for detailed analysis and explanation, but the method and system are not limited to chromium nitrogen coating, but are applicable to various vacuum glow coating processes, including but not limited to titanium nitride coating, aluminum nitride coating and aluminum oxide coating. Through the steps of holographic component acquisition, adaptive component adjustment, real-time adjustment strategy and film quality correction, real-time and precise control of the coating composition is achieved. Therefore, the method of the present invention has universal applicability and can be extended to other coating materials and processes.
[0025] In a specific embodiment, the multi-dimensional data includes spectral signal intensity, film thickness and surface roughness.
[0026] In a specific embodiment, the multi-dimensional data of the specified chromium nitrogen coating process is collected by sensors and monitoring equipment. The specific process is as follows: the partial pressure of nitrogen is measured by the pressure sensor in the vacuum chamber. The distance between the target material on the target material holder in the vacuum chamber and the spectrum probe is measured by the distance measuring device and recorded as , the plasma temperature is measured by the plasma diagnostic instrument and recorded as The experimental coefficients of chromium and nitrogen, as well as the reaction rates of chromium and nitrogen in plasma were obtained through calibration experiments, and the experimental coefficients of chromium and nitrogen were recorded as and , the reaction rates of chromium and nitrogen in plasma are recorded as and , and then calculated by the formula: and , and the spectral signal intensities of chromium and nitrogen are obtained respectively and , is a positive number, Expressed as the equivalent partial pressure of chromium in the plasma.
[0027] Obtain the coating deposition time using the timing system of a specified chromium-nitrogen coating equipment , the plasma temperature was determined by experiment. The corresponding coating deposition time is The film growth rate , and the corresponding temperature dependence coefficient of the specified chromium nitrogen coating process is obtained through experimental determination , and then calculated by the formula: , the plasma temperature during the specified chromium nitrogen coating process is obtained The corresponding coating deposition time is The film thickness inside .
[0028] The surface of the sample to be coated is fixed on the sample holder and each monitoring point is set. The surface height corresponding to each monitoring point is obtained by scanning with an electron microscope. , It represents the number of each monitoring point. , is the total number of monitoring points, and is a positive integer, and the average height of the surface of the sample to be coated is obtained by calculating the mean value, which is recorded as , and then calculated by the formula: , get the surface roughness of the sample to be coated fixed on the sample holder .
[0029] It should be noted that the plasma temperature The unit is Kelvin, and Kelvin is recorded as , temperature dependence coefficient The unit is ,so It is a dimensionless quantity.
[0030] It should be noted that the process of estimating the equivalent partial pressure of chromium in the plasma based on the effective partial pressure of chromium obtained by combining spectral measurement based on the sputtering power, the volume of the vacuum chamber and the target area is an estimation process of the prior art and will not be elaborated on here.
[0031] It should also be noted that the specific process of obtaining the experimental coefficients of chromium and nitrogen, as well as the reaction rates of chromium and nitrogen in plasma respectively, through calibration experiments is as follows: in a certain experiment, first, under known gas pressure and temperature conditions, chromium and nitrogen in a vacuum chamber are glow discharged, and the emission spectrum intensity at different wavelengths is measured using a spectrometer. Then, by changing the nitrogen flow rate and target current, the changes in the spectral signal are observed, and the plasma density and electron temperature are measured using a spectral probe. Then, the measured spectral intensity, gas partial pressure and plasma temperature data are substituted into the theoretical model, and the experimental coefficients of chromium and nitrogen are calculated using the least squares fitting method. Their deposition rates are measured under different plasma powers and gas flow rates, and the results are calculated in combination with the reaction kinetics model. For example, at a gas pressure of 0.5 Pascals and a sputtering power of 500 W, the growth rate of the chromium nitrogen film layer is measured to be 2 nanometers per minute, and the corresponding reaction rates of chromium and nitrogen are calculated by the ratio of the deposition amount to the plasma composition.
[0032] It should also be noted that the plasma temperature is determined by experimental The corresponding coating deposition time is The film growth rate , and the specific process of obtaining the temperature dependence coefficient corresponding to the specified chromium nitrogen coating process through experimental determination is as follows: in the actual experiment, the deposition time of the coating is recorded by the timing system of the chromium nitrogen coating equipment. For example, the coating time is set to 30 minutes, and the coating is carried out at a plasma temperature of 573.15K, 673.15K, and 773.15K under a gas pressure of 0.5 Pascal, a sputtering power of 500 watts, and a substrate bias of -50 volts. The thickness of the film after deposition is measured using an ellipsometer or an X-ray reflectometer, for example For example, the film thickness measured at 573.15K is 100 nanometers, 120 nanometers at 673.15K, and 140 nanometers at 773.15K. The film growth rate at the corresponding temperature is calculated, that is, the thickness divided by time, which is 3.33 nanometers per minute, 4 nanometers per minute, and 4.67 nanometers per minute, respectively. Subsequently, these data are fitted to the relationship curve between film growth rate and temperature, for example, using a linear fitting method to obtain the temperature dependence coefficient, which is used to reflect the change pattern of film growth rate with temperature.
[0033] In the process of real-time strategy adjustment, the embodiment of the present invention optimizes the process parameters based on the calculation results, which is conducive to the dynamic correction of nitrogen flow, target current and bias voltage, so that the coating composition can be maintained within the set range in real time, thereby improving the uniformity and consistency of the coating. In the process of film quality evaluation, the comprehensive quantitative calculation of film hardness, adhesion and surface roughness is carried out, which is conducive to the accurate characterization of thin film performance, and can be combined with the target threshold to determine whether further process adjustment is needed to ensure that the final product meets the quality standards.
[0034] Step 2: Adaptive composition adjustment: Based on the multi-dimensional data of the specified chromium-nitrogen coating process, the predicted value of the chromium-nitrogen composition in the corresponding vacuum chamber during the specified chromium-nitrogen coating process is calculated, and it is evaluated whether the chromium-nitrogen coating needs adaptive composition adjustment.
[0035] In a specific embodiment, the calculation specifies the predicted value of the chromium and nitrogen composition in the vacuum chamber during the chromium and nitrogen coating process. The specific process is as follows: using the chromium and nitrogen concentration prediction formula: 、 , respectively get the predicted value of chromium concentration in the corresponding vacuum chamber during the specified chromium nitrogen coating process , nitrogen concentration prediction value ,in 、 They are respectively represented by the influence coefficient of temperature on chromium concentration and the influence coefficient of temperature on nitrogen concentration measured by spectral experiments.
[0036] It should be noted that, assuming that the experiment is conducted at different plasma temperatures, such as 600 Kelvin, 700 Kelvin and 800 Kelvin, the spectral signal intensities of chromium are measured to be 200, 250 and 310, respectively, and the spectral signal intensities of nitrogen are 180, 230 and 290, respectively. Subsequently, the nonlinear fitting method is used to obtain the influence coefficient of temperature on chromium concentration and the influence coefficient of temperature on nitrogen concentration. If the fitting results show that for every 100 Kelvin increase in temperature, the chromium concentration increases by 15% and the nitrogen concentration increases by 12%, then the influence coefficient of temperature on chromium concentration is set to 0.15, that is, for every 1 Kelvin increase in temperature, the chromium concentration increases by 0.0015, and the influence coefficient of temperature on nitrogen concentration is set to 0.12, that is, for every 1 Kelvin increase in temperature, the nitrogen concentration increases by 0.0012.
[0037] In a specific embodiment, the evaluation of whether the chromium-nitrogen coating requires adaptive composition adjustment is performed as follows: based on a set target film composition of a specified chromium-nitrogen coating device, a chromium-nitrogen coating having a ratio of chromium atoms to nitrogen atoms of 1:1, a predicted chromium concentration value and a predicted nitrogen concentration value in a vacuum chamber corresponding to the specified chromium-nitrogen coating process are compared with set chromium concentration threshold range intervals and nitrogen concentration threshold range intervals, respectively. If the predicted chromium concentration value and the predicted nitrogen concentration value in the vacuum chamber corresponding to the specified chromium-nitrogen coating process are both within the set chromium concentration threshold range intervals and nitrogen concentration threshold range intervals, it indicates that the chromium-nitrogen coating does not require adaptive composition adjustment; otherwise, it indicates that the chromium-nitrogen coating requires adaptive composition adjustment.
[0038] It should be noted that, for example, in a specified chromium-nitrogen coating device, the target film composition is set to a ratio of chromium atoms to nitrogen atoms of 1:1. Experimental measurements show that under optimal coating conditions, the average chromium concentration and nitrogen concentration in the vacuum chamber are 5.0 mol per cubic meter, respectively. Taking into account factors such as experimental errors, gas flow fluctuations, and sputtering rate changes, the threshold range can be set to ±5%, that is, the chromium concentration threshold range is 4.75-5.25 mol per cubic meter, and the nitrogen concentration threshold range is 4.75-5.25 mol per cubic meter. Then, according to the above comparison process, it can be determined whether the chromium-nitrogen coating needs adaptive composition adjustment.
[0039] In the process of predicting chromium and nitrogen concentration, the embodiment of the present invention adopts spectral measurement, plasma temperature monitoring and gas pressure measurement, which is conducive to improving the accuracy of composition prediction and avoiding inaccurate control of coating composition due to single parameter measurement error. In the process of correcting coating process parameters, feedback control based on the quantitative value of film quality is adopted, which is conducive to accurate correction for process differences under different batches and different cavity loading conditions, reducing fluctuations in the production process, and improving product consistency and stability.
[0040] Step 3. Real-time adjustment strategy: When the chromium-nitrogen coating requires adaptive composition adjustment, the coating process parameters are adjusted in real time through the designated chromium-nitrogen coating equipment management platform.
[0041] In a specific embodiment, the coating process parameters are adjusted in real time by specifying a chromium nitrogen coating equipment management platform. The specific process is as follows: the coating process parameter adjustment includes nitrogen flow adjustment, bias adjustment and target current adjustment. The corresponding nitrogen concentration in the current vacuum chamber is obtained by specifying a chromium nitrogen coating equipment management platform. , and according to the target film composition of chromium and nitrogen atoms with a ratio of 1 to 1, the corresponding target nitrogen concentration in the vacuum chamber is obtained ,when Greater than When the nitrogen supply is reduced, Less than When the nitrogen supply is increased, equal When the current nitrogen supply is maintained, the corresponding chromium concentration in the current vacuum chamber is obtained by specifying the chromium nitrogen coating equipment management platform. , and the corresponding target chromium concentration in the vacuum chamber is recorded as ,when Greater than When the bias voltage setting value and the target current setting value are increased, Less than When the bias voltage and target current are lowered, equal When , the current bias voltage and target current setting values are maintained without adjustment, and the required adjustment amount of the current nitrogen supply amount, the required adjustment amount of the bias voltage and the required adjustment amount of the target current are calculated by the calculation formula.
[0042] It should be noted that, for example, assuming that a chromium nitrogen coating equipment adopts a magnetron sputtering PVD process, the substrate temperature is set to 500°C, the working pressure is 0.5 Pascal, and the target film thickness is 2 microns. Under such conditions, experimental data show that when the ratio of chromium and nitrogen atomic concentrations in the cavity is maintained at 1:1, the composition of the chromium-nitrogen film layer finally deposited on the substrate is closest to a ratio of chromium atoms to nitrogen atoms of 1:1. In order to achieve this ratio, it is first necessary to determine the concentrations of chromium atoms and nitrogen atoms in the plasma region of the vacuum chamber, which depends on the nitrogen flow rate and the sputtering rate of the chromium target. Through experimental measurements, at a pressure of 0.5 Pascals, when the nitrogen flow rate is set to 30 standard milliliters per minute, the concentration of nitrogen atoms in the plasma is approximately 5 mol per cubic meter, and the sputtering rate of chromium atoms corresponds to a plasma chromium atom concentration of 5 mol per cubic meter. At this time, the target nitrogen concentration can be set to 5 mol per cubic meter and the target chromium concentration can be set to 5 mol per cubic meter as the benchmark value for subsequent feedback control. In the actual coating process, if the nitrogen atom concentration measured by the spectrum is lower than 5 mol per cubic meter, the nitrogen flow rate needs to be increased, and vice versa. Similarly, if the chromium atom concentration is too low, the sputtering rate of chromium atoms can be increased by increasing the target current or reducing the substrate bias voltage, so that the ratio of chromium atom concentration to nitrogen atom concentration in the plasma is always stable at 1:1, thereby ensuring that the composition of the chromium nitrogen film finally deposited on the substrate meets the expected requirements.
[0043] In a specific embodiment, the calculation to obtain the current nitrogen supply amount, the bias voltage and the target current required adjustment is as follows: by the calculation formula: 、 and , respectively get the required adjustment amount of the current nitrogen supply , Bias voltage adjustment amount and target current need to be adjusted ,in 、 They are the influence coefficient of the set nitrogen concentration on the chromium nitrogen film layer and the influence coefficient of the plasma temperature on the nitrogen flow adjustment. 、 They are the influence coefficient of the set bias voltage on chromium atom deposition and the influence coefficient of the chromium nitrogen film thickness on the bias voltage adjustment. 、 They are the influence coefficient of the set target current on the release of chromium atoms and the influence coefficient of the plasma temperature on the target current regulation.
[0044] It should be noted that the setting process of the influence coefficient of nitrogen concentration on the chromium nitrogen film layer and the influence coefficient of plasma temperature on nitrogen flow adjustment is as follows; obtained through experimental measurement and data fitting, first, under different nitrogen flow conditions, such as 10 standard milliliters per minute, 15 standard milliliters per minute, and 20 standard milliliters per minute, the composition change of the chromium nitrogen film layer after coating is measured, and then, under different plasma temperatures, other process parameters are kept unchanged, the change of film layer composition after nitrogen flow adjustment is measured, and the response degree of temperature change to nitrogen flow adjustment is analyzed to obtain the temperature influence coefficient. For example, the experiment found that for every 100 Kelvin increase in temperature, the nitrogen flow rate needs to increase by 5% to maintain the same chromium-nitrogen atomic ratio, so the influence coefficient of plasma temperature on nitrogen flow adjustment is set to 0.05. 、 、 、 The setting process and 、 The setting process is the same as , so I will not go into details here.
[0045] During the calculation formula optimization process, the embodiment of the present invention uses mathematical modeling of nitrogen flow, bias voltage, and target current adjustment, which is conducive to accurately calculating the required adjustment amount, making the coating process more intelligent, reducing human intervention, and improving production efficiency. During the film roughness evaluation process, electron microscope scanning and multi-point measurement calculation are used, which is conducive to accurately obtaining the morphological characteristics of the coating surface, optimizing deposition parameters, and improving the mechanical properties and optical quality of the film. During the plasma parameter monitoring process, the plasma temperature and experimental calibration coefficient are calculated, which is conducive to better understanding the influence of the plasma environment on the coating composition, optimizing the coating process, and improving process stability.
[0046] Step 4: Real-time film quality correction: After completing the adaptive adjustment of the coating process parameters, evaluate the film quality of the specified chromium nitrogen coating and analyze whether the coating process parameters need to be corrected.
[0047] In a specific embodiment, the evaluation of the film quality of a specified chromium-nitrogen coating is performed as follows: by calculating the formula: , get the quantitative value of the film quality of the specified chromium nitrogen coating ,in Expressed as the hardness of the film, Expressed as the adhesion of the film, Indicates the standard adhesion of the film required by the specified chromium nitrogen coating process. Indicates the standard hardness and It is expressed as the influence coefficient of film roughness on quality in a specified chromium-nitrogen coating.
[0048] It should be noted that, through the nanoindentation test, an increasing load is applied to the surface of the film layer, a diamond probe is pressed into the film, the maximum load and the corresponding indentation area are recorded, and the maximum load is divided by the indentation area to obtain the result. , through the scratch test, use a hard probe to apply a gradually increasing load to the film layer, measure the critical load when the film layer peels off, and record the load at which the film layer begins to peel off, which is , obtained from the recommended process parameter settings provided by the corresponding supplier of the specified chromium nitrogen coating equipment and The setting range value, The setting process and 、 The setting process is the same as , so I will not go into details here.
[0049] In a specific embodiment, the analysis of whether the coating process parameters need to be corrected is as follows: the film quality quantization value of the specified chromium-nitrogen coating is compared with the set target film quality quantization value threshold. If the film quality quantization value of the specified chromium-nitrogen coating is greater than the set target film quality quantization value threshold, it indicates that the film hardness is too large and the coating process parameters need to be corrected. If the film quality quantization value of the specified chromium-nitrogen coating is approximately equal to the set target film quality quantization value threshold, it indicates that the film quality meets the requirements and the coating process parameters do not need to be corrected. If the film quality quantization value of the specified chromium-nitrogen coating is less than the set target film quality quantization value threshold, it indicates that the film quality does not meet the requirements and the coating process parameters need to be corrected.
[0050] It should be noted that the parameter correction process is the analysis process of step three above.
[0051] See also Figure 2 As shown, a real-time control system for vacuum glow coating composition includes the following modules: a holographic composition acquisition module, an adaptive composition adjustment module, a real-time adjustment strategy module and a real-time film quality correction module.
[0052] The holographic component acquisition module is connected to the adaptive component adjustment module, the adaptive component adjustment module is connected to the real-time adjustment strategy module, and the real-time adjustment strategy module is connected to the real-time film quality correction module.
[0053] The holographic component acquisition module is used to collect multi-dimensional data of the specified chromium-nitrogen coating process through sensors and monitoring equipment.
[0054] The adaptive composition adjustment module is used to calculate the predicted value of the chromium and nitrogen composition in the corresponding vacuum chamber during the specified chromium and nitrogen coating process based on the multi-dimensional data during the specified chromium and nitrogen coating process, and to evaluate whether the chromium and nitrogen coating needs adaptive composition adjustment.
[0055] The real-time adjustment strategy module is used to adjust the coating process parameters in real time through the designated chromium nitrogen coating equipment management platform when the chromium nitrogen coating needs to be adaptively adjusted in composition.
[0056] The real-time film quality correction module is used to evaluate the film quality of the specified chromium nitrogen coating after completing the adaptive adjustment of the coating process parameters, and analyze whether the coating process parameters need to be corrected.
[0057] See also Figure 3 As shown in the figure, the principle diagram of the real-time control system of vacuum glow discharge excitation coating composition based on optical emission spectrum is shown. A chromium target is arranged in the specified chromium nitrogen coating equipment and fixed on the target material holder. The target material holder is installed on the side wall or top of the vacuum chamber, directly opposite the sample holder. The sample holder is used to fix the sample to be coated. A spectrum probe is set in the vacuum chamber, and the collected spectral parameters are transmitted to the spectrum analysis device via optical fiber. The light intensity signal of the spectrum analysis and processing device is converted into an electronic signal and then enters the terminal controller. The whole process is completed by PC analysis. PC represents the control computer.
[0058] An embodiment of the present invention provides a real-time control method and system for the composition of vacuum glow coating. During the holographic composition acquisition process, multi-dimensional data is collected in real time, including spectral signals, film thickness, surface roughness and other parameters. This is conducive to comprehensive monitoring of the coating environment in the vacuum chamber, ensuring the accuracy of process data, and improving the controllability of the coating process. During the adaptive composition adjustment process, the chromium and nitrogen composition is predicted and calculated, and whether it needs to be adjusted is evaluated. This is conducive to discovering deviations in the coating composition in advance and avoiding unstable film quality due to parameter drift during the deposition process.
[0059] The above content is merely an example and explanation of the concept of the present invention. Those skilled in the art may make various modifications or additions to the described specific embodiments or replace them in a similar manner. As long as they do not deviate from the concept of the invention or exceed the scope defined in this specification, they should all fall within the scope of protection of the present invention.
Claims
1. A method for real-time control of the composition of vacuum glow coating, characterized in that: include: Step 1: Holographic component collection: For the coating process of a specified chromium-nitrogen coating, multi-dimensional data of the specified chromium-nitrogen coating process is collected through sensors and monitoring equipment; Step 2: Adaptive composition adjustment: Based on the multi-dimensional data of the specified chromium-nitrogen coating process, the predicted value of the chromium-nitrogen composition in the vacuum chamber corresponding to the specified chromium-nitrogen coating process is calculated, and it is evaluated whether the chromium-nitrogen coating needs adaptive composition adjustment; Step 3: Real-time adjustment strategy: When the chromium-nitrogen coating requires adaptive composition adjustment, the coating process parameters are adjusted in real time through the designated chromium-nitrogen coating equipment management platform; Step 4: Real-time film quality correction: After completing the adaptive adjustment of the coating process parameters, evaluate the film quality of the specified chromium nitrogen coating and analyze whether the coating process parameters need to be corrected; The multi-dimensional data collected during the specified chromium nitrogen coating process by sensors and monitoring equipment includes: measuring the partial pressure of nitrogen by the pressure sensor in the vacuum chamber , and according to the sputtering power and target area, the effective partial pressure of chromium is estimated The distance between the target material on the target material holder in the vacuum chamber and the spectrum probe is measured by the distance measuring device and recorded as , the plasma temperature is measured by the plasma diagnostic instrument and recorded as The experimental coefficients of chromium and nitrogen, as well as the reaction rates of chromium and nitrogen in plasma were obtained through calibration experiments, and the experimental coefficients of chromium and nitrogen were recorded as and , the reaction rates of chromium and nitrogen in plasma are recorded as and , and then calculated by the formula: and , and the spectral signal intensities of chromium and nitrogen are obtained respectively and , is a positive number; Obtain the coating deposition time using the timing system of a specified chromium-nitrogen coating equipment , the plasma temperature was determined by experiment. The corresponding coating deposition time is The film growth rate , and the corresponding temperature dependence coefficient of the specified chromium nitrogen coating process is obtained through experimental determination , and then calculated by the formula: , the plasma temperature during the specified chromium nitrogen coating process is obtained The corresponding coating deposition time is The film thickness inside ; The surface of the sample to be coated is fixed on the sample holder and each monitoring point is set. The surface height corresponding to each monitoring point is obtained by scanning with an electron microscope. , It represents the number of each monitoring point. , is the total number of monitoring points, and is a positive integer, and the average height of the surface of the sample to be coated is obtained by calculating the mean value, which is recorded as , and then calculated by the formula: , get the surface roughness of the sample to be coated fixed on the sample holder ; The multi-dimensional data includes spectral signal intensity, film thickness and surface roughness; The specific process of calculating the predicted value of the chromium and nitrogen composition in the vacuum chamber during the specified chromium and nitrogen coating process is as follows: The chromium nitrogen concentration is predicted by the formula: 、 , respectively get the predicted value of chromium concentration in the corresponding vacuum chamber during the specified chromium nitrogen coating process , nitrogen concentration prediction value ,in 、 They are respectively the influence coefficients of temperature on chromium concentration and nitrogen concentration determined by spectral experiments; The coating process parameters are adjusted in real time by specifying a chromium nitrogen coating equipment management platform. The specific process is as follows: Coating process parameter adjustment includes nitrogen flow adjustment, bias adjustment and target current adjustment. The corresponding nitrogen concentration in the current vacuum chamber is obtained by specifying the chromium nitrogen coating equipment management platform. , and according to the target film composition of chromium and nitrogen atoms with a ratio of 1 to 1, the corresponding target nitrogen concentration in the vacuum chamber is obtained ,when Greater than When the nitrogen supply is reduced, Less than When the nitrogen supply is increased, equal When the current nitrogen supply is maintained, the corresponding chromium concentration in the current vacuum chamber is obtained by specifying the chromium nitrogen coating equipment management platform. , and the corresponding target chromium concentration in the vacuum chamber is recorded as ,when Greater than When the bias voltage setting value and the target current setting value are increased, Less than When the bias voltage and target current are lowered, equal When the current bias voltage and target current setting values are maintained without adjustment, the required adjustment amount of the current nitrogen supply amount, the required adjustment amount of the bias voltage and the required adjustment amount of the target current are calculated by the calculation formula; The calculation obtains the required adjustment amount of the current nitrogen supply amount, the required adjustment amount of the bias voltage, and the required adjustment amount of the target current. The specific process is as follows: By calculation formula: 、 and , respectively get the required adjustment amount of the current nitrogen supply , Bias voltage adjustment amount and target current need to be adjusted ,in 、 They are the influence coefficient of the set nitrogen concentration on the chromium nitrogen film layer and the influence coefficient of the plasma temperature on the nitrogen flow adjustment. 、 They are the influence coefficient of the set bias voltage on chromium atom deposition and the influence coefficient of the chromium nitrogen film thickness on the bias voltage adjustment. 、 They are the influence coefficient of the set target current on the release of chromium atoms and the influence coefficient of the plasma temperature on the target current regulation.
2. The method for real-time control of the composition of vacuum glow coating according to claim 1, characterized in that: The specific process of evaluating whether the chromium nitrogen coating needs to be adaptively adjusted is as follows: According to the set target film layer composition of the specified chromium-nitrogen coating equipment, which is a chromium-nitrogen coating with a ratio of chromium atoms to nitrogen atoms of 1:1, the predicted chromium concentration value and the predicted nitrogen concentration value in the corresponding vacuum chamber during the specified chromium-nitrogen coating process are compared with the set chromium concentration threshold range interval and the nitrogen concentration threshold range interval, respectively. If the predicted chromium concentration value and the predicted nitrogen concentration value in the corresponding vacuum chamber during the specified chromium-nitrogen coating process are both within the set chromium concentration threshold range interval and the nitrogen concentration threshold range interval, it indicates that the chromium-nitrogen coating does not require adaptive composition adjustment; otherwise, it indicates that the chromium-nitrogen coating requires adaptive composition adjustment.
3. The method for real-time control of the composition of vacuum glow coating according to claim 1, characterized in that: The specific process of evaluating the film quality of a specified chromium-nitrogen coating is as follows: By calculation formula: , get the quantitative value of the film quality of the specified chromium nitrogen coating ,in Expressed as the hardness of the film, Expressed as the adhesion of the film, Indicates the standard adhesion of the film required by the specified chromium nitrogen coating process. Indicates the standard hardness and It is expressed as the influence coefficient of film roughness on quality in a specified chromium-nitrogen coating.
4. The method for real-time control of the composition of vacuum glow coating according to claim 3, characterized in that: The analysis of whether the coating process parameters need to be corrected is as follows: The film quality quantization value of the specified chromium-nitrogen coating is compared with the set target film quality quantization value threshold. If the film quality quantization value of the specified chromium-nitrogen coating is greater than the set target film quality quantization value threshold, it indicates that the film hardness is too large and the coating process parameters need to be corrected. If the film quality quantization value of the specified chromium-nitrogen coating is equal to the set target film quality quantization value threshold, it indicates that the film quality meets the requirements and no coating process parameter correction is required. If the film quality quantization value of the specified chromium-nitrogen coating is less than the set target film quality quantization value threshold, it indicates that the film quality does not meet the requirements and the coating process parameters need to be corrected.
5. A real-time control system for the composition of a vacuum glow coating that implements the real-time control method for the composition of a vacuum glow coating according to any one of claims 1 to 4, characterized in that: Includes the following modules: Holographic component acquisition module, used for collecting multi-dimensional data of the specified chromium-nitrogen coating process through sensors and monitoring equipment; An adaptive composition adjustment module is used to calculate the predicted chromium and nitrogen composition in the vacuum chamber during the specified chromium and nitrogen coating process based on multi-dimensional data during the specified chromium and nitrogen coating process, and to evaluate whether the chromium and nitrogen coating needs adaptive composition adjustment; A real-time adjustment strategy module is used to adjust the coating process parameters in real time through the designated chromium nitrogen coating equipment management platform when the chromium nitrogen coating requires adaptive composition adjustment; The real-time film quality correction module is used to evaluate the film quality of the specified chromium nitrogen coating after completing the adaptive adjustment of the coating process parameters, and analyze whether the coating process parameters need to be corrected.
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