Vacuum glow coating component real-time control method and system
By adopting real-time component control method in vacuum glow coating technology, the problems of insufficient monitoring of target service life and consumption status and insufficient compensation of film thickness and temperature dependence are solved, real-time and precise control of coating components is achieved, and the controllability of the coating process and the stability of film quality are improved.
Patent Information
- Application Number
- CN202510496224.4
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-04-21
- Publication Date
- 2025-05-16
- Estimated Expiration
- 2045-04-21
AI Technical Summary
The existing vacuum glow coating technology lacks real-time monitoring of the service life and consumption state of the target material, which leads to changes in the release of chromium atoms during the coating process, affecting the stability of the film layer composition; at the same time, there is a lack of dynamic compensation for the film layer thickness and temperature dependence, resulting in unstable film layer performance.
The real-time component control method of vacuum glow coating is adopted, and real-time precise control of coating components is achieved through steps such as holographic component acquisition, adaptive component adjustment, real-time adjustment strategy and film layer quality correction. Specifically, it includes: collecting multi-dimensional data through sensors, calculating the predicted value of chromium nitrogen components, evaluating whether adaptive adjustment of process parameters is required, and evaluating and correcting the membrane layer quality.
A comprehensive monitoring of the coating environment in the vacuum cavity is achieved, ensuring the accuracy of process data, improving the controllability of the coating process, avoiding unstable film quality caused by parameter drift, and improving coating uniformity and consistency.
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Figure CN120006243A_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 components 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 excited coating process has at least the following technical problems: 1. In actual coating production, the impact of target consumption lacks real-time monitoring of target service life and consumption status, which is not conducive to precise control of 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 sample loading density and spatial distribution, which is not conducive to ensuring the uniformity of glow discharge, and will lead to large deviations in film thickness and composition of different batches of products.
[0004] 2. Most of the existing chromium-nitrogen coating processes lack control over the film thickness, which is not conducive to ensuring uniform deposition on different types of substrates. It will lead to large deviations in the film thickness on substrates with complex morphologies, affecting the final film performance. In addition, the temperature dependence lacks dynamic compensation for changes in chamber temperature during long-term deposition, which is not conducive to maintaining the stability of the plasma state. It 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 solutions: The present invention provides a method for real-time control of the composition of vacuum glow coating, including: 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.
[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 needs to be adaptively adjusted in composition, 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 a vacuum glow coating, comprising: a holographic composition acquisition module for acquiring 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-nitrogen composition in the corresponding vacuum chamber during the specified chromium-nitrogen coating process according to the multi-dimensional data during the specified chromium-nitrogen coating process, and to evaluate whether the chromium-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 specified 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 as follows: 1. A method and system for real-time control of the composition of a vacuum glow coating provided by an embodiment of the present invention, in the process of holographic component collection, 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. In the process of adaptive component adjustment, the chromium and nitrogen components are predicted and calculated, and it is evaluated whether they need to be adjusted, which is conducive to early detection of coating composition deviations and avoiding unstable film quality due to parameter drift during the deposition process.
[0015] 2. In the process of real-time adjustment strategy, 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, and the coating uniformity and consistency are improved. In the process of film quality evaluation, the comprehensive quantitative calculation of film hardness, adhesion and surface roughness is passed, 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.
[0016] 3. In the process of predicting chromium nitrogen concentration, the embodiment of the present invention adopts spectral measurement, plasma temperature monitoring and gas pressure measurement, which is beneficial to improving the accuracy of composition prediction and avoiding inaccurate regulation 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 beneficial to accurately correct the process differences under different batches and different cavity loading conditions, reduce fluctuations in the production process, and improve 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 evaluating the roughness of the film layer, 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 monitoring the plasma parameters, 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 the 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 drawings required for use in the embodiments or the description of the prior art will be briefly introduced below. 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 creative work.
[0019] Figure 1 It is a schematic flow chart of the implementation steps of the present invention.
[0020] Figure 2 It is a schematic diagram of the system structure connection of the present invention.
[0021] Figure 3 The figure is a schematic diagram of the principle of the real-time control system of components for vacuum glow discharge excitation coating according to the present invention. DETAILED DESCRIPTION
[0022] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. 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 creative work 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, the method comprising: step one, holographic component acquisition: for a coating process of a specified chromium-nitrogen coating, multi-dimensional data of the specified chromium-nitrogen coating process is acquired 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 components can be 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 on the target 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 , and the experimental coefficients of chromium and nitrogen, as well as the reaction rates of chromium and nitrogen in plasma were obtained through calibration experiments. The experimental coefficients of chromium and nitrogen were recorded as and , the reaction rates of chromium and nitrogen in the plasma are recorded as and , and then through the calculation 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] Obtaining the deposition time of the coating through the timing system of a specified chrome-nitrogen coating equipment , the plasma temperature is 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 by experimental determination , and then through the calculation formula: , the plasma temperature during the specified chromium-nitrogen coating process is 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 surface height of the sample to be coated is obtained by averaging, which is recorded as , and then through the calculation 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 Is a dimensionless quantity.
[0030] It should be noted that the process of estimating the equivalent partial pressure of chromium in plasma based on the effective partial pressure of chromium obtained by combining spectral measurement according to 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 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, the chromium and nitrogen in the 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 are calculated in combination with the reaction kinetics model. For example, under a gas pressure of 0.5 Pascal 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 deposition amount to plasma composition.
[0032] It should also be noted that the plasma temperature is determined by experimental measurements. The corresponding coating deposition time is The film growth rate , and the specific process of obtaining the corresponding temperature dependence coefficient in 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 0.5 Pascal gas pressure, 500 W sputtering power, -50 V substrate bias, and plasma temperatures of 573.15 K, 673.15 K, and 773.15 K respectively, and the thickness of the film after deposition is measured using an ellipsometer or an X-ray reflectometer, for example For example, the film thickness is measured to be 100 nanometers at 573.15K, 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 the time, which is 3.33 nanometers per minute, 4 nanometers per minute, and 4.67 nanometers per minute, respectively. Subsequently, these data are fit 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 adjustment strategy, the embodiment of the present invention optimizes the process parameters based on the calculation results, which is conducive to dynamically correcting the nitrogen flow rate, target current and bias voltage, so that the coating composition can be maintained within the set range in real time, and the coating uniformity and consistency are improved. In the process of film quality evaluation, the comprehensive quantitative calculation of film hardness, adhesion and surface roughness is passed, which is conducive to accurately characterizing the performance of the thin film, and can determine whether further process adjustment is needed in combination with the target threshold 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-nitrogen composition in the corresponding vacuum chamber during the chromium-nitrogen coating process, and the specific process is as follows: using the chromium-nitrogen concentration prediction formula: , , respectively obtain 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 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 needs to be adaptively adjusted in composition is performed as follows: according to the setting of the target film layer composition of the specified chromium-nitrogen coating equipment as a chromium-nitrogen coating in which the ratio of the number of chromium atoms to the number of nitrogen atoms is 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 need to be adaptively adjusted in composition, otherwise, it indicates that the chromium-nitrogen coating needs to be adaptively adjusted in composition.
[0038] It should be noted that, for example, in a specified chromium-nitrogen coating device, the target film layer 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 the chromium nitrogen concentration, the embodiment of the present invention adopts spectral measurement, plasma temperature monitoring and gas pressure measurement, which is beneficial to improving the accuracy of composition prediction and avoiding inaccurate regulation of coating composition due to single parameter measurement error. In the process of correcting the coating process parameters, feedback control based on the quantified value of the film quality is adopted, which is beneficial to accurately correct the process differences under different batches and different cavity loading conditions, reduce fluctuations in the production process, and improve product consistency and stability.
[0040] Step 3: Real-time adjustment strategy: When the chromium-nitrogen coating needs to be adaptively adjusted in composition, 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 being 1:1, 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 is lowered and the target current is 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.
[0042] It should be noted that, for example, assuming that a chromium-nitrogen coating device adopts a magnetron sputtering PVD process, the substrate temperature is set to 500°C, the working gas pressure is 0.5 Pascal, and the target film thickness is 2 microns. Under this condition, experimental data show that when the ratio of chromium to nitrogen atom 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 reference 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, otherwise it needs to be reduced. Similarly, if the concentration of chromium atoms 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 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 calculating the formula: , and , respectively get the required adjustment amount of the current nitrogen supply 、Bias voltage adjustment amount The target current needs 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 respectively 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 the nitrogen flow adjustment is 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. Secondly, at different plasma temperatures, other process parameters are kept unchanged, and the change of film layer composition after nitrogen flow adjustment is measured. 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 needs to increase by 5% to maintain the same chromium-nitrogen atomic number ratio. 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] In the process of optimizing the calculation formula, the embodiment of the present invention adopts mathematical modeling 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 evaluating the roughness of the film layer, electron microscope scanning and multi-point measurement calculation are adopted, which is conducive to accurately obtaining the morphological characteristics of the coating surface, optimizing the deposition parameters, and improving the mechanical properties and optical quality of the film. In the process of monitoring the plasma parameters, the plasma temperature and the 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 the 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 specific process of evaluating the film quality of the specified chromium-nitrogen coating is as follows: by calculating the formula: , get the quantitative value of the film quality of the specified chromium nitrogen coating ,in It is expressed as the hardness of the film layer. Expressed as the adhesion of the film, It 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 the roughness of the film layer on the quality in a specified chromium-nitrogen coating.
[0048] It should be noted that in 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, a hard probe is used to apply a gradually increasing load to the film layer, and the critical load when the film layer peels off is measured. The load at which the film layer starts to peel off is recorded, 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 of 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 it is necessary to correct the coating process parameters is as follows: comparing the specified chromium-nitrogen coating film quality quantification value with the set target film quality quantification value threshold. If the specified chromium-nitrogen coating film quality quantification value is greater than the set target film quality quantification value threshold, it indicates that the film hardness is too large and the coating process parameters need to be corrected. If the specified chromium-nitrogen coating film quality quantification value is approximately equal to the set target film quality quantification value threshold, it indicates that the film quality meets the requirements and the coating process parameters do not need to be corrected. If the specified chromium-nitrogen coating film quality quantification value is less than the set target film quality quantification 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 process of parameter correction is the analysis process of step three above.
[0051] See also Figure 2 As shown, a real-time control system for the composition of vacuum glow coating 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-nitrogen composition in the corresponding vacuum chamber during the specified chromium-nitrogen coating process according to the multi-dimensional data during the specified chromium-nitrogen coating process, and to evaluate whether the chromium-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 specified 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, the schematic 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. The chromium target is fixed on the target material holder. The target material holder is installed on the side wall or the top of the vacuum chamber, directly opposite to the sample holder. The sample holder is used to fix the sample to be coated. A spectrum probe is arranged in the vacuum chamber. The collected spectral parameters are transmitted to the spectrum analysis device via optical fiber. The light intensity signal of the spectrum analysis processing device is converted into an electronic signal and then enters the terminal controller. The whole process is completed through PC analysis. PC represents the control computer.
[0058] The embodiments of the present invention provide a method and system for real-time control of the composition of vacuum glow coating. In the process of holographic component collection, multi-dimensional data is collected in real time, 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. In the process of adaptive component adjustment, the chromium and nitrogen components are predicted and calculated, and whether they need to be adjusted is evaluated, which is conducive to discovering the deviation of the coating composition in advance and avoiding unstable film quality due to parameter drift during the deposition process.
[0059] The above contents are merely examples and explanations of the concept of the present invention. Those skilled in the art may make various modifications or additions to the specific embodiments described 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 shall all fall within the protection scope 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 the 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: Calculate the predicted chromium-nitrogen composition in the corresponding vacuum chamber during the specified chromium-nitrogen coating process based on the multi-dimensional data during the specified chromium-nitrogen coating process, and evaluate whether the chromium-nitrogen coating needs to be adaptively adjusted; Step 3: Real-time adjustment strategy: When the chromium-nitrogen coating needs to be adaptively adjusted, 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.
2. A method for real-time control of composition of vacuum glow coating according to claim 1, characterized in that: The multi-dimensional data includes spectral signal intensity, film thickness and surface roughness.
3. The method for real-time control of composition of vacuum glow coating according to claim 1, characterized in that: 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 on the target 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 , and the experimental coefficients of chromium and nitrogen, as well as the reaction rates of chromium and nitrogen in plasma were obtained through calibration experiments. The experimental coefficients of chromium and nitrogen were recorded as and , the reaction rates of chromium and nitrogen in the plasma are recorded as and , and then through the calculation 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 plasma; Obtaining the deposition time of the coating through the timing system of a specified chrome-nitrogen coating equipment , the plasma temperature is 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 by experimental determination , and then through the calculation formula: , the plasma temperature during the specified chromium-nitrogen coating process is 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 the mean calculation, which is recorded as , and then through the calculation formula: , and obtain the surface roughness of the sample to be coated fixed on the sample holder .
4. A method for real-time control of composition of vacuum glow coating according to claim 3, characterized in that: The specific process of calculating the predicted value of the chromium and nitrogen composition in the corresponding vacuum chamber during the chromium and nitrogen coating process is as follows: The chromium nitrogen concentration is predicted by the formula: , , respectively obtain 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.
5. A method for real-time control of composition of vacuum glow coating according to claim 4, 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 need to be adaptively adjusted in composition; otherwise, it indicates that the chromium-nitrogen coating needs to be adaptively adjusted in composition.
6. A method for real-time control of composition of vacuum glow coating according to claim 5, characterized in that: 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 the chromium nitrogen coating equipment management platform. , and according to the target film composition of chromium and nitrogen atoms being 1:1, 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 is lowered and the target current is 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.
7. A method for real-time control of composition of vacuum glow coating according to claim 6, characterized in that: 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 The target current needs 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 respectively 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.
8. A method for real-time control of composition of vacuum glow coating according to claim 7, 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 It is expressed as the hardness of the film layer. Expressed as the adhesion of the film, It 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 the roughness of the film layer on the quality in a specified chromium-nitrogen coating.
9. A method for real-time control of composition of vacuum glow coating according to claim 8, characterized in that: The analysis of whether the coating process parameters need to be corrected is as follows: The film quality quantification value of the specified chromium-nitrogen coating is compared with the set target film quality quantification value threshold. If the film quality quantification value of the specified chromium-nitrogen coating is greater than the set target film quality quantification value threshold, it indicates that the film hardness is too large and the coating process parameters need to be corrected. If the film quality quantification value of the specified chromium-nitrogen coating is approximately equal to the set target film quality quantification value threshold, it indicates that the film quality meets the requirements and no coating process parameters need to be corrected. If the film quality quantification value of the specified chromium-nitrogen coating is less than the set target film quality quantification value threshold, it indicates that the film quality does not meet the requirements and the coating process parameters need to be corrected.
10. A real-time control system for the composition of vacuum glow coating that implements the real-time control method for the composition of vacuum glow coating according to any one of claims 1 to 9, characterized in that: Includes the following modules: Holographic component acquisition module, used for acquiring 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 value of the chromium and nitrogen composition in the corresponding vacuum chamber during the specified chromium and nitrogen coating process according to the multi-dimensional data during the specified chromium and nitrogen coating process, and to evaluate whether the chromium and nitrogen coating needs to be adaptively adjusted in composition; Real-time adjustment strategy module, 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; 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.
Citation Information
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