Film growth surface temperature measuring device and method in magnetron sputtering process
By combining an X-type multilayer NiCr/NiSi thin film thermocouple with a standard K-type wire thermocouple, the temperature of the thin film growth surface during magnetron sputtering is directly measured, solving the deviation problem of traditional indirect measurement methods and realizing high-precision, real-time temperature measurement, which is suitable for magnetron sputtering processes.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2026-01-28
- Publication Date
- 2026-04-10
AI Technical Summary
Traditional temperature measurement methods cannot directly obtain the actual temperature of the thin film growth surface during magnetron sputtering, resulting in a large deviation between the measurement results and the actual temperature, and thus failing to provide accurate temperature data for process optimization.
By combining an X-type multilayer NiCr/NiSi thin-film thermocouple with a standard K-type wire thermocouple, the thermoelectric potential signal of the thin-film growth surface is directly measured. Combined with a data processing system for temperature conversion and error correction, accurate measurement of the thin-film growth surface is achieved.
It enables direct measurement of the surface temperature of thin film growth with an accuracy of up to ±0.5℃, strong real-time performance, adaptability to the vacuum environment of magnetron sputtering, simple operation, and does not affect the efficiency of thin film preparation.
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Figure CN121829796A_ABST
Abstract
Description
Technical Field
[0001] This invention belongs to the field of thin film preparation technology, specifically relating to a device and method for measuring the surface temperature of thin film growth during magnetron sputtering. Background Technology
[0002] In thin film fabrication, the temperature of the film growth surface is a key parameter affecting the film's crystallinity, density, adhesion, and microstructure, directly determining its final quality and performance. However, traditional temperature measurement methods have significant limitations: since magnetron sputtering is typically performed in a vacuum environment, and the bombardment of sputtered particles leads to uneven temperature distribution, traditional measurement methods cannot directly obtain the actual temperature of the film growth surface. Most methods can only indirectly infer the film surface temperature by measuring the substrate temperature. This indirect measurement method ignores the temperature differences caused by factors such as sputtered particle energy conversion and thermal resistance between the film and the substrate during film growth, resulting in a large deviation between the measured results and the true temperature of the film growth surface. This fails to provide accurate temperature data for process optimization and hinders the fabrication and development of high-performance thin films. Therefore, developing a device and method that can directly measure the surface temperature of thin films during magnetron sputtering has become an urgent technical problem to be solved in this field. Summary of the Invention
[0003] To address the aforementioned technical problems, this invention provides a device and method for measuring the surface temperature of thin films during magnetron sputtering, thereby resolving the issues in the prior art. The technical solution adopted by this invention is as follows: A device for measuring the surface temperature of thin film growth during magnetron sputtering includes an X-type glass substrate, an X-type multilayer NiCr / NiSi thin film thermocouple, a standard K-type wire thermocouple, a DC pulse magnetron sputtering device, a multimeter, and a data processing system. The X-type multilayer NiCr / NiSi thin film thermocouple is prepared on the surface of an X-type glass substrate by magnetron sputtering, with its hot junction exposed in the sputtering area and its cold junction connected to a multimeter via wires. The hot junction of the standard K-type wire thermocouple is embedded inside the X-type glass substrate, and the cold junction is connected to a multimeter via a wire. The DC pulse magnetron sputtering equipment includes a sputtering cavity, a target material, a vacuum system, and a power supply system. An X-shaped glass substrate is fixed inside the sputtering cavity as a sample stage, and the hot junction of an X-shaped multilayer NiCr / NiSi thin film thermocouple is directly opposite the sputtering center region of the target material. The data processing system has a built-in temperature conversion algorithm for converting and storing temperature data.
[0004] A method for measuring the surface temperature of thin film growth during magnetron sputtering includes the following steps: Step 1, Pretreatment of the apparatus: The X-type glass substrate is ultrasonically cleaned with acetone and ethanol for 15 min each, rinsed with deionized water, and dried at 80-120℃ for 20-40 min; X-type multilayer NiCr / NiSi thin film thermocouples are prepared on the substrate by magnetron sputtering; a standard K-type wire thermocouple is embedded inside the substrate, and after the wire connection is completed, the insulation performance of the entire substrate is tested to ensure that there is no leakage. Step 2, Equipment Assembly and Vacuum Environment Setup: Fix the pretreated X-shaped glass substrate onto the sample stage of the DC pulsed magnetron sputtering equipment. Adjust the position of the sample stage so that the distance between the thin-film thermocouple hot junction and the target material is 8-12 cm and directly faces the sputtering center area. Close the sputtering chamber, start the vacuum system, and evacuate the vacuum level inside the chamber to 1×10⁻⁶. -3 Below Pa; Step 3, Temperature measurement system start-up: Turn on the multimeter, set the sampling frequency to 1-10Hz, perform zero-point calibration on the X-type multilayer NiCr / NiSi thin film thermocouple and the standard K-type wire thermocouple, and record the thermoelectric potential signals of the two thermocouples in the initial state. Step 4, Magnetron Sputtering and Real-time Temperature Measurement: Start the DC pulse magnetron sputtering equipment and deposit a thin film on the surface of the X-type glass substrate using a Ti target or a TiO2 target. If a Ti target is used, the sputtering parameters are set as follows: argon flow rate 25-35 sccm, sputtering power 130-170 W, sputtering time 40-80 min; if a TiO2 target is used, the sputtering parameters are set as follows: argon flow rate 20-30 sccm, oxygen flow rate 3-7 sccm, sputtering power 160-200 W, sputtering time 30-60 min. During sputtering, the hot junction of the X-type multilayer NiCr / NiSi thin film thermocouple directly receives the bombardment of sputtered particles, and the thermoelectric potential signal of the film growth surface is collected in real time. The standard K-type wire thermocouple synchronously collects the thermoelectric potential signal of the substrate. Both signals are transmitted to a multimeter and converted into temperature values by the temperature conversion algorithm of the data processing system to generate a temperature-time curve. Step 5, Measurement completion and data processing: After the sputtering process is completed, first turn off the magnetron sputtering equipment, and after the cavity has cooled naturally to room temperature, turn off the vacuum system and temperature measurement system, export the measurement data, and correct the measurement results by comparing and analyzing the thin film surface temperature and the substrate temperature.
[0005] Furthermore, the temperature conversion algorithm includes the following steps: Thermoelectric potential signal preprocessing: Signal filtering: A moving average filtering method is used to reduce noise in the two raw thermoelectric potential signals acquired by the multimeter, eliminating high-frequency interference. The formula is as follows: ; in, Let N be the thermoelectric potential at time t after filtering, and N be the length of the sliding window. Zero-point correction: Based on the zero-point calibration data, the initial thermoelectric potential offset is subtracted to obtain the corrected thermoelectric potential; Preliminary temperature calculation based on the scale table: Thin-film thermocouple temperature calculation: The thermoelectric potential-temperature relationship of NiCr / NiSi thermocouples follows a polynomial fitting law, and the fitting formula is based on experimental calibration data. ; in, , , , These are the weighting coefficients; Standard K-type thermocouple temperature calculation: Temperature T2 is calculated using linear interpolation, with the following formula: ; Where EL and EH are the lower and upper limits of thermoelectric potential adjacent to the correction in the calibration table, respectively, and TL and TH are the corresponding temperature values; Dual-channel signal error correction: Temperature difference compensation model: A fixed temperature difference exists between the thin film surface temperature and the substrate temperature. The temperature difference compensation coefficient k is established through experimental calibration. ; The surface temperature of the thin film was measured using a high-precision infrared thermometer. These are measurements taken by a type K thermocouple during the same period. The average temperature difference from multiple calibration experiments; Final temperature calculation: ; illustrate: The initial temperature is the initial temperature of the substrate before sputtering begins. The system has a fixed systematic error.
[0006] The present invention has the following beneficial effects: (1) Direct temperature measurement: The hot junction of the thin film thermocouple is directly exposed to the sputtering area, and the surface temperature of the thin film is directly measured, avoiding the temperature deviation between the substrate and the thin film surface in traditional indirect temperature measurement, and the measurement result is closer to the true value. (2) High measurement accuracy: By combining the comparative calibration of standard K-type wire thermocouples, the environmental interference and system error are corrected through the data processing system. The corrected temperature measurement error is controlled within ±0.5℃, which meets the precise temperature measurement requirements of thin film preparation process. (3) Strong real-time performance: The thin film thermocouple has a fast response speed, and the sampling frequency of the data acquisition system can be adjusted in the range of 1-10Hz. It can capture the dynamic changes of temperature during the thin film growth process in real time and generate temperature-time curves to provide real-time data support for process optimization. (4) Good adaptability: The device has a compact structure and the wires are protected by a ceramic insulation layer with a thickness of 0.1-0.3mm, which can be adapted to the vacuum working environment of magnetron sputtering. The X-type substrate (size 40-60mm×40-60mm, thickness 1-3mm) and thermocouple structure design are compatible with the sample stage and target layout of the magnetron sputtering equipment, and the installation is convenient. (5) Simple operation: The entire measurement process does not require complex auxiliary equipment. The pretreatment, assembly and measurement steps are simple and can be carried out simultaneously with the magnetron sputtering process without affecting the thin film preparation efficiency. Attached Figure Description
[0007] Figure 1 This is a schematic diagram of the overall structure of the present invention; Figure 2 This is a schematic diagram of a temperature measurement system for TiO2 thin film deposition. Detailed Implementation
[0008] The following will be described in conjunction with embodiments of the present invention. Figures 1-2 The technical solutions in the embodiments of the present invention will be clearly and completely described. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Unless otherwise specified, the technical means used in the embodiments are conventional means well known to those skilled in the art.
[0009] This invention fabricates an X-type multilayer NiCr / NiSi thin-film thermocouple on an X-type glass substrate, directly exposing its hot junction to the magnetron sputtering region. This allows the hot junction to directly receive the bombardment of sputtered particles, enabling real-time sensing of temperature changes on the thin-film growth surface. Simultaneously, a standard K-type wire thermocouple is used to measure the substrate temperature as a comparative reference. Through collaborative analysis of the two temperature data streams, measurement errors are corrected. This approach eliminates the need for indirect inference from the substrate temperature, directly obtaining the temperature information of the thin-film growth surface. Furthermore, the NiCr / NiSi thin-film thermocouple features fast response speed and a temperature range suitable for magnetron sputtering processes (-200℃ to 1300℃). The X-type structure design ensures effective contact between the hot junction and the sputtering region, and the ceramic insulating wire avoids short-circuit problems in the vacuum sputtering environment. The overall device is compact and adaptable to the vacuum operating environment of magnetron sputtering equipment.
[0010] This invention proposes a device for measuring the surface temperature of thin film growth during magnetron sputtering, comprising an X-type glass substrate, an X-type multilayer NiCr / NiSi thin film thermocouple, a standard K-type wire thermocouple, a DC pulse magnetron sputtering device, a multimeter, and a data processing system; The X-shaped glass substrate is made of quartz glass, with dimensions of 40-60mm × 40-60mm and a thickness of 1-3mm, serving as the thermocouple integration carrier. The X-shaped multilayer NiCr / NiSi thin-film thermocouple is fabricated on the surface of the X-shaped glass substrate using magnetron sputtering. The X-shaped structure is formed by the intersection of NiCr alloy thin films and NiSi alloy thin films, with a 50-100μm hot junction exposed in the sputtering area. The cold junction is led out to the edge of the substrate and connected to a multimeter via a high-temperature insulated wire. The hot junction of the standard K-type wire thermocouple is embedded inside the X-shaped glass substrate, 1-2mm from the substrate surface, and the cold junction is connected to the multimeter via a compensating wire. The multimeter is connected to a standard K-type wire thermocouple. Its measurement accuracy is ±0.5℃, and the temperature range is -200℃ to 1300℃. The DC pulse magnetron sputtering equipment includes a sputtering chamber, a Ti or TiO2 target, a vacuum system, and a power supply system. An X-shaped glass substrate is fixed inside the sputtering chamber on a sample stage. The hot junction of the thin-film thermocouple is directly opposite the sputtering center area of the target, and the distance between the target and the substrate is 8-12cm. The multimeter is a high-precision digital multimeter with millivolt-level signal acquisition capability, and it connects to both the thin-film thermocouple and the standard K-type wire thermocouple. The data processing system has a built-in temperature conversion algorithm, which can display, store, and export temperature data in real time. The sampling frequency can be adjusted within the range of 1-10Hz.
[0011] Specifically, the data processing system of this invention incorporates a temperature conversion algorithm. Its core is based on the thermoelectric effect principle of thermocouples, combined with the collaborative calibration logic of two temperature measurement signals, to achieve accurate conversion from thermoelectric potential to temperature and error correction. Specifically, it includes: 1. Using the known calibration tables of NiCr / NiSi thin film thermocouples and standard K-type wire thermocouples, establish a one-to-one correspondence between thermoelectric potential (E) and temperature (T), and realize continuous temperature calculation through interpolation algorithm.
[0012] 2. Using the measurement value of a standard K-type thermocouple (measurement accuracy ±0.5℃) as a reference, correct the systematic errors of the thin-film thermocouple (such as material property drift, vacuum environment interference, etc.) to improve the overall measurement accuracy.
[0013] The specific steps of the temperature conversion algorithm include: S1: Thermoelectric potential signal preprocessing: Signal filtering: A moving average filtering method is used to reduce noise in the two raw thermoelectric potential signals (E1 is the thin-film thermocouple signal, and E2 is the K-type thermocouple signal) acquired by the multimeter, eliminating high-frequency interference. The formula is as follows: ; in, Let N be the thermoelectric potential at time t after filtering, and N be the length of the sliding window (values range from 5 to 10, adapted to sampling frequencies of 1 to 10 Hz). Δt = 1 / fs (where fs is the sampling frequency).
[0014] Zero-point correction: Based on the zero-point calibration data, the initial thermoelectric potential offset is subtracted to obtain the corrected thermoelectric potential; S2: Preliminary temperature calculation based on the scale table: Temperature calculation for thin-film thermocouples (NiCr / NiSi): The thermoelectric potential-temperature relationship of NiCr / NiSi thermocouples follows a polynomial fitting law, and the fitting formula is based on experimental calibration data. ; in, , , , These are the weighting coefficients; the coefficient values are: a0 = -0.12 (℃), a1 = 42.35 (℃ / mV), a2 = -1.87 (℃ / (mV²)), a3 = 0.32 (℃ / (mV³)). The coefficients are obtained through standard constant temperature bath calibration experiments and cover key temperature points in the target temperature measurement range (such as -200℃, 0℃, 500℃, 1000℃, 1300℃).
[0015] Standard K-type thermocouple temperature calculation: Using the K-type thermocouple calibration table specified in international standard IEC 60584-1, the temperature T2 is calculated using linear interpolation. The formula is as follows: ; Wherein, EL and EH are the lower and upper limits of the thermoelectric potential adjacent to the correction in the calibration table, respectively, and TL and TH are the corresponding temperature values, with an interpolation error ≤ 0.1℃.
[0016] S3: Dual-channel signal error correction: Temperature difference compensation model: A fixed temperature difference exists between the thin film surface temperature and the substrate temperature (caused by factors such as sputtered particle energy conversion and thermal resistance). The temperature difference compensation coefficient k is established through experimental calibration. ; -The surface temperature of the thin film measured by a high-precision infrared thermometer (calibration reference). - These are measurements taken by a K-type thermocouple during the same period. - This represents the average temperature difference from multiple calibration experiments. k ranges from 1.0 to 1.2 (dynamically adjusted based on sputtering power and target type).
[0017] Final temperature calculation: ; illustrate: -Initial temperature is the initial temperature of the substrate before sputtering begins. - The system has a fixed systematic error (obtained through long-term experimental statistics, with a value of 0.2-0.3℃), and the measurement error after correction is ≤±0.5℃.
[0018] The initial temperature is the initial temperature of the substrate before sputtering begins. The system has a fixed systematic error (obtained through long-term experimental statistics, with a value of 0.2-0.3℃). After correction, the measurement error is ≤ ±0.5℃.
[0019] S4: Real-time data output and storage: Temperature-time curve generation: By setting the sampling frequency (1-10Hz), the final result of each calculation is associated with the corresponding timestamp to generate a continuous curve.
[0020] Outlier removal: When the temperature exceeds ℃ (outside the normal temperature range), it is determined to be an abnormal signal, and the temperature value from the previous moment is used to replace it to ensure data continuity.
[0021] The temperature conversion algorithm of this invention is designed for different sputtering parameters (such as gas flow rate and power) of Ti and TiO2 targets. The algorithm has a built-in parameter library and automatically matches the corresponding temperature difference compensation coefficient k and filter window N. This is applicable in vacuum conditions ≤1×10⁻⁶. - 3 Under a vacuum environment of Pa, the algorithm compensates for the slight influence of vacuum on thermoelectric potential through a preset vacuum environment correction term (vacuum, P being the vacuum level). The algorithm employs lightweight computational logic, with a single-step computation time of ≤1ms, meeting the real-time requirements of a maximum sampling frequency of 10Hz.
[0022] Furthermore, the surface of the cold junction lead wire of the X-type multilayer NiCr / NiSi thin film thermocouple is covered with a ceramic insulating layer, the thickness of which is 0.1-0.3 mm.
[0023] This invention also proposes a method for measuring the surface temperature of thin film growth during magnetron sputtering, comprising the following steps: Step 1, Pretreatment of the apparatus: The X-type glass substrate is ultrasonically cleaned with acetone and ethanol for 15 minutes each, rinsed with deionized water, and then dried at 80-120℃ for 20-40 minutes. An X-type multilayer NiCr / NiSi thin-film thermocouple is fabricated on the substrate using magnetron sputtering. The NiCr target power is 70-90W, and the NiSi target power is 60-80W. The sputtering time is 10-20 minutes to ensure the hot junction is intact and undamaged, and the cold junction lead wires are reliably connected. A standard K-type wire thermocouple is embedded inside the substrate. After the wire connections are completed, the insulation performance of the entire substrate is tested to ensure there is no leakage. Step 2, Equipment Assembly and Vacuum Environment Setup: Fix the pretreated X-shaped glass substrate onto the sample stage of the DC pulsed magnetron sputtering equipment. Adjust the position of the sample stage so that the distance between the thin-film thermocouple hot junction and the target material is 8-12 cm and directly faces the sputtering center area. Close the sputtering chamber, start the vacuum system, and evacuate the vacuum level inside the chamber to 1×10⁻⁶. -3 Below Pa; Step 3, Temperature measurement system startup: Turn on the multimeter and data processing system, set the sampling frequency to 1-10Hz (preferably 5Hz), perform zero-point calibration on the thin-film thermocouple and the standard K-type wire thermocouple, and record the thermoelectric potential signals of the two thermocouples in the initial state; Step 4, Magnetron Sputtering and Real-time Temperature Measurement: Start the DC pulse magnetron sputtering equipment and deposit a thin film on the X-type glass substrate where the thin film thermocouple is located using a Ti target or TiO2 target. If a Ti target is used, the sputtering parameters are set as follows: argon flow rate 25-35 sccm, sputtering power 130-170 W, sputtering time 40-80 min; if a TiO2 target is used, the sputtering parameters are set as follows: argon flow rate 20-30 sccm, oxygen flow rate 3-7 sccm, sputtering power 160-200 W, sputtering time 30-60 min. During sputtering, the hot junction of the thin film thermocouple directly receives the bombardment of sputtered particles, and the thermoelectric potential signal of the film growth surface is collected in real time. The standard K-type wire thermocouple synchronously collects the thermoelectric potential signal of the substrate. Both signals are transmitted to a multimeter and converted into temperature values by the temperature conversion algorithm of the data processing system to generate a temperature-time curve. Step 5, Measurement Completion and Data Processing: After the sputtering process is completed, first turn off the magnetron sputtering equipment. After the cavity cools naturally to room temperature, turn off the vacuum system and temperature measurement system, export the measurement data, and correct the measurement results by comparing and analyzing the thin film surface temperature and the substrate temperature. The corrected temperature measurement error is controlled within ±0.5℃.
[0024] Specific embodiments of the present invention are as follows: Example 1: Temperature Measurement of TiO2 Thin Films Based on Ti Target Magnetron Sputtering Pretreatment of the device: A quartz glass with a size of 50mm×50mm and a thickness of 2mm was selected as the X-type substrate. It was ultrasonically cleaned with acetone and ethanol for 15min each, rinsed with deionized water, and then dried in a 100℃ oven for 30min. NiCr / NiSi thin film thermocouples were prepared on the substrate surface by magnetron sputtering. The NiCr target power was 80W and the NiSi target power was 70W. The sputtering time was 15min to form an X-type structure with a hot junction size of about 80μm. The cold junction lead wire was treated with a ceramic insulation layer with a thickness of 0.2mm. A standard K-type wire thermocouple was embedded in the substrate, 1.5mm away from the surface. After connecting the wire, an insulation test was performed to ensure no leakage.
[0025] Equipment Assembly and Vacuum Construction: Fix the pretreated substrate onto the sample stage of the magnetron sputtering equipment, adjust the target-substrate distance to 10 cm, and ensure the thermocouple hot junction is aligned with the Ti target sputtering center; close the sputtering chamber and evacuate through the vacuum system interface until the vacuum level inside the chamber reaches 5 × 10⁻⁶. -4 Pa.
[0026] Temperature measurement system startup: Turn on the high-precision digital multimeter and data processing system, set the sampling frequency to 5Hz, perform zero-point calibration on the two thermocouples, record the initial thermoelectric potential signal, and ensure that the measurement system works normally.
[0027] Magnetron sputtering and temperature measurement: Start the magnetron sputtering equipment and set the Ti target sputtering parameters as follows: argon flow rate 30 sccm, sputtering power 150W, sputtering time 60min; during the sputtering process, the thin film thermocouple collects the thermoelectric potential signal of the thin film surface in real time, and the standard K-type wire thermocouple collects the substrate signal simultaneously. The data processing system converts the thermoelectric potential into temperature value and generates two temperature-time curves in real time.
[0028] Measurement completion and data processing: After sputtering, the magnetron sputtering equipment was turned off. After the cavity cooled to room temperature (about 30°C), the vacuum system and temperature measurement system were turned off, and the data was exported. Analysis showed that the surface temperature of the thin film stabilized at 285-290°C 10 minutes after sputtering, and the substrate temperature stabilized at 260-265°C. The temperature difference between the two was about 25°C. After correction, the error of the measured value of the thin film surface temperature was ±0.3°C, which is within the error control range of ±0.5°C.
[0029] Example 2: Temperature Measurement of TiO2 Thin Films Based on TiO2 Target Magnetron Sputtering The difference from Example 1 is that the target material was changed to a TiO2 target, and the sputtering parameters were adjusted to: argon flow rate 25 sccm, oxygen flow rate 5 sccm, sputtering power 180 W, and sputtering time 45 min; the sampling frequency was set to 8 Hz. Measurement results show that the surface temperature of the grown film stabilized at 310-315℃ after 8 min of sputtering, and the substrate temperature stabilized at 280-285℃, with a temperature difference of approximately 30℃. The corrected measurement error was ±0.4℃, meeting the error control requirement of ±0.5℃.
[0030] The above embodiments are merely descriptions of preferred embodiments of the present invention and are not intended to limit the scope of the present invention. Any modifications, alterations, alterations, or substitutions made by those skilled in the art to the technical solutions of the present invention without departing from the spirit of the present invention should fall within the protection scope defined by the claims of the present invention.
Claims
1. A device for measuring the surface temperature of thin film growth during magnetron sputtering, characterized in that, Includes X-type glass substrate, X-type multilayer NiCr / NiSi thin film thermocouple, standard K-type wire thermocouple, DC pulse magnetron sputtering equipment, multimeter and data processing system; The X-type multilayer NiCr / NiSi thin film thermocouple is prepared on the surface of an X-type glass substrate by magnetron sputtering, with its hot junction exposed in the sputtering area and its cold junction connected to a multimeter via wires. The hot junction of the standard K-type wire thermocouple is embedded inside the X-type glass substrate, and the cold junction is connected to a multimeter via a wire. The DC pulse magnetron sputtering equipment includes a sputtering cavity, a target material, a vacuum system, and a power supply system. An X-shaped glass substrate is fixed inside the sputtering cavity as a sample stage, and the hot junction of an X-shaped multilayer NiCr / NiSi thin film thermocouple is directly opposite the sputtering center region of the target material. The data processing system has a built-in temperature conversion algorithm for converting and storing temperature data.
2. A method for measuring the surface temperature of thin film growth during magnetron sputtering, applied to the device for measuring the surface temperature of thin film growth during magnetron sputtering as described in claim 1, characterized in that, Includes the following steps: Step 1, Pretreatment of the apparatus: The X-type glass substrate is ultrasonically cleaned with acetone and ethanol for 15 min each, rinsed with deionized water, and dried at 80-120℃ for 20-40 min; X-type multilayer NiCr / NiSi thin film thermocouples are prepared on the substrate by magnetron sputtering; a standard K-type wire thermocouple is embedded inside the substrate, and after the wire connection is completed, the insulation performance of the entire substrate is tested to ensure that there is no leakage. Step 2, Equipment Assembly and Vacuum Environment Setup: Fix the pretreated X-shaped glass substrate onto the sample stage of the DC pulsed magnetron sputtering equipment. Adjust the position of the sample stage so that the distance between the thin-film thermocouple hot junction and the target material is 8-12 cm and directly faces the sputtering center area. Close the sputtering chamber, start the vacuum system, and evacuate the vacuum level inside the chamber to 1×10⁻⁶. -3 Below Pa; Step 3, Temperature measurement system start-up: Turn on the multimeter, set the sampling frequency to 1-10Hz, perform zero-point calibration on the X-type multilayer NiCr / NiSi thin film thermocouple and the standard K-type wire thermocouple, and record the thermoelectric potential signals of the two thermocouples in the initial state. Step 4, Magnetron Sputtering and Real-time Temperature Measurement: Start the DC pulse magnetron sputtering equipment and deposit a thin film on the surface of the X-type glass substrate using a Ti target or a TiO2 target. If a Ti target is used, the sputtering parameters are set as follows: argon flow rate 25-35 sccm, sputtering power 130-170 W, sputtering time 40-80 min; if a TiO2 target is used, the sputtering parameters are set as follows: argon flow rate 20-30 sccm, oxygen flow rate 3-7 sccm, sputtering power 160-200 W, sputtering time 30-60 min. During sputtering, the hot junction of the X-type multilayer NiCr / NiSi thin film thermocouple directly receives the bombardment of sputtered particles, and the thermoelectric potential signal of the film growth surface is collected in real time. The standard K-type wire thermocouple synchronously collects the thermoelectric potential signal of the substrate. Both signals are transmitted to a multimeter and converted into temperature values by the temperature conversion algorithm of the data processing system to generate a temperature-time curve. Step 5, Measurement completion and data processing: After the sputtering process is completed, first turn off the magnetron sputtering equipment, and after the cavity has cooled naturally to room temperature, turn off the vacuum system and temperature measurement system, export the measurement data, and correct the measurement results by comparing and analyzing the thin film surface temperature and the substrate temperature.
3. The method for measuring the surface temperature of thin film growth during magnetron sputtering according to claim 2, characterized in that, The temperature conversion algorithm includes the following steps: Thermoelectric potential signal preprocessing: Signal filtering: A moving average filtering method is used to reduce noise in the two raw thermoelectric potential signals acquired by the multimeter, eliminating high-frequency interference. The formula is as follows: ; in, Let N be the thermoelectric potential at time t after filtering, and N be the length of the sliding window. Zero-point correction: Based on the zero-point calibration data, the initial thermoelectric potential offset is subtracted to obtain the corrected thermoelectric potential; Preliminary temperature calculation based on the scale table: Thin-film thermocouple temperature calculation: The thermoelectric potential-temperature relationship of NiCr / NiSi thermocouples follows a polynomial fitting law, and the fitting formula is based on experimental calibration data. ; in, , , , These are the weighting coefficients; Standard K-type thermocouple temperature calculation: Temperature T2 is calculated using linear interpolation, with the following formula: ; Where EL and EH are the lower and upper limits of thermoelectric potential adjacent to the correction in the calibration table, respectively, and TL and TH are the corresponding temperature values; Dual-channel signal error correction: Temperature difference compensation model: A fixed temperature difference exists between the thin film surface temperature and the substrate temperature. The temperature difference compensation coefficient k is established through experimental calibration. ; The surface temperature of the thin film was measured using a high-precision infrared thermometer. These are measurements taken by a type K thermocouple during the same period. The average temperature difference from multiple calibration experiments; Final temperature calculation: ; illustrate: The initial temperature is the initial temperature of the substrate before sputtering begins. The system has a fixed systematic error.