A method for improving the thickness control accuracy of atomic layer deposition multilayer films

Abstract

The present invention discloses a method for improving the thickness control accuracy of atomic layer deposition multilayer films. The method includes the following steps: S100: placing a sample and a companion film in a reaction chamber; S200: performing atomic layer deposition to obtain a multilayer film sample; S300: obtaining film growth data; S400: comparing the actual film thickness with the theoretical film thickness to obtain an average growth rate; S500 and S600: when the average growth rate does not meet a first growth rate variation trend, eliminating error data and repeating S400-S600; S700: using the average growth rate as the initial growth rate; S800: maintaining process conditions unchanged, adjusting process parameters, and repeating S100-S700; and S900: obtaining a multilayer film device. The method solves the technical problem that prior art research on atomic layer deposition multilayer film thickness control methods is relatively limited, resulting in low control accuracy and an inability to obtain ideal multilayer film thickness control accuracy.

Description

Technical Field

[0001] The present invention relates to the field of precision devices, and in particular to a method for improving the thickness control accuracy of atomic layer deposition multilayer films. Background Art

[0002] Atomic layer deposition (ALD) is a thin film deposition technology based on self-terminating surface reactions. It has the advantages of good uniformity, high conformality, and precise control of film thickness. It has been widely used in optoelectronics, semiconductors, nanotechnology and other fields. However, with the continuous development of precision device preparation technology, high-performance multilayer film devices have increasingly stringent requirements on the thickness control accuracy of their deposited films, especially the control accuracy of thicker multilayer films. For example, in the preparation of X-ray Fresnel lenses and multilayer film mirrors prepared by atomic layer deposition slicing method, small errors in single-layer film thickness often accumulate into large errors in multilayer film thickness, causing device performance degradation or even failure.

[0003] However, in the process of implementing the technical solution of the invention in this application, it was found that the above technology has at least the following technical problems:

[0004] There is relatively little research in the prior art on methods for controlling the thickness of atomic layer deposition multilayer films, resulting in low control accuracy and the technical problem of being unable to obtain ideal multilayer film thickness control accuracy. Summary of the Invention

[0005] The present application provides a method for improving the thickness control accuracy of atomic layer deposition multilayer films, thereby solving the technical problem that the existing technology has relatively little research on the thickness control method of atomic layer deposition multilayer films, resulting in low control accuracy and the inability to obtain ideal multilayer film thickness control accuracy, thereby achieving the technical effect of improving the thickness control accuracy of atomic layer deposition multilayer films.

[0006] In view of the above problems, the present application provides a method for improving the thickness control accuracy of atomic layer deposition multilayer films: S100: placing a sample and a companion film in a reaction chamber; S200: performing atomic layer deposition of the growth material required for the multilayer film in the reaction chamber using first process parameters to obtain a multilayer film sample; S300: performing electron microscope imaging on the multilayer film sample to obtain film growth data; S400: comparing the actual film thickness with the theoretical film thickness to obtain an average growth rate; S500: judging whether the average growth rate meets a first growth rate change trend; S 600: When the average growth rate does not satisfy the first growth rate change trend, eliminate the error data in the average growth rate, and repeat S400-S600 based on the film layer growth data after eliminating the error data until the average growth rate satisfies the first growth rate change trend; S700: Use the average growth rate as the initial growth rate of the thin film material in the next stage; S800: Keep the process conditions unchanged, adjust the process parameters, and repeat S100-S700; S900: Obtain a multilayer film device with high mold thickness control accuracy.

[0007] Preferably, S200 further includes: introducing an inert gas into the reaction chamber for 1-300s to evacuate the reaction chamber to a vacuum degree of 5×10 -3 -9×10 -3 Torr or less; after the reaction chamber, substrate, pipeline and reaction source are heated and stabilized at the set temperature, a precursor source is alternately introduced into the reaction chamber for 0.01-5.00s to perform atomic layer deposition of the growth material required for the multilayer film to obtain a multilayer film sample, and the above process parameters are recorded as the first process parameters.

[0008] Preferably, S300 also includes: waiting for the multilayer film sample to cool to room temperature and then taking it out; imaging the multilayer film sample with an electron microscope, measuring the film thickness layer by layer, and performing an average calculation to obtain the growth rate of the growing material; using the growth rate as the starting rate, and according to the designed thickness of each film layer, calculating the cycles sample table required for thin film growth, and using it as the film layer growth data.

[0009] Preferably, S400 further includes:

[0010] A silicon substrate is prepared, ultrasonically cleaned with acetone, ethanol, and deionized water for 10-20 minutes respectively, and blown with high-purity nitrogen until the moisture meets the first predetermined requirement; the cleaned silicon substrate is cut into n small silicon wafers and placed around the multilayer film sample, and the cycles value of the process recipe is changed, while other parameters remain unchanged, to grow the multilayer film; when the multilayer film deposition meets the predetermined thickness, the n small silicon wafers are taken out, imaged by an electron microscope, and the film thickness is measured sample by sample and layer by layer, and the actual film thickness data of each film layer is obtained, and the average growth rate is obtained based on the film thickness data of each film layer.

[0011] Preferably, S500 also includes: preliminarily eliminating error data of the thickness data of each layer of the membrane to obtain first processed data; calculating the average growth rate based on the first processed data; obtaining a stage error change curve based on the average growth rate calculation, and judging whether the stage error change curve meets the first growth rate change trend; when the stage error change curve does not meet the first growth rate change trend, data is eliminated according to the error percentage in the first processed data, and iterative calculation is continued until the stage error change curve calculated after the iteration meets the first growth rate change trend.

[0012] Preferably, the growth material includes a simple substance, a nitride, or an oxide.

[0013] Preferably, the precursor source comprises trimethylaluminum, tetrahafnium and deionized water.

[0014] Preferably, the heating temperature range of the pipeline is 20-300°C, the heating temperature range of the reaction chamber is 20-300°C, the heating temperature range of the reaction source is 20-200°C, and the heating temperature range of the precursor source is 70-80°C.

[0015] Preferably, the adjustment range of the process vacuum is 0.10 Torr-1.00 Torr.

[0016] One or more technical solutions provided in this application have at least the following technical effects or advantages:

[0017] Due to the adoption of S100: placing the sample and the companion film in the reaction chamber; S200: performing atomic layer deposition of the growth material required for the multilayer film in the reaction chamber through the first process parameters to obtain a multilayer film sample; S300: performing electron microscope imaging on the multilayer film sample to obtain film layer growth data; S400: comparing the actual film thickness with the theoretical film thickness to obtain the average growth rate; S500: judging whether the average growth rate meets the first growth rate change trend; S600: when the average growth rate does not meet the first growth rate change trend, eliminating the error data in the average growth rate, and repeating S400-S600 based on the film layer growth data after eliminating the error data until the average growth rate meets the first growth rate change trend; S700: using the average growth rate as the initial growth rate of the thin film material in the next stage; S800: keeping the process conditions unchanged, adjusting the process parameters, and repeating S100-S700; S900: obtaining a multilayer film device with high mold thickness control accuracy. During the thin film growth process, the process parameters are easy to control and the data adjustment range is small. Through limited data processing and changes in simple process parameters, the technical effect of achieving high-precision layer-by-layer control of thicker multi-layer films is achieved.

[0018] The above description is only an overview of the technical solution of the present application. In order to more clearly understand the technical means of the present application, it can be implemented in accordance with the contents of the specification. In order to make the above and other purposes, features and advantages of the present application more obvious and easy to understand, the specific implementation methods of the present application are listed below. BRIEF DESCRIPTION OF THE DRAWINGS

[0019] Figure 1 A schematic flow chart of a method for improving the thickness control accuracy of atomic layer deposition multilayer films according to the present application;

[0020] Figure 2 This is a comparison curve between the actual film thickness and the theoretical film thickness of a multilayer film structure in a method for improving the film thickness control accuracy of atomic layer deposition multilayer films in this application. DETAILED DESCRIPTION

[0021] This application provides a method for improving the thickness control accuracy of atomic layer deposition multilayer films, which solves the problem that the existing technology has relatively little research on the thickness control method of atomic layer deposition multilayer films, resulting in low control accuracy and the inability to obtain ideal multilayer film thickness control accuracy, thereby achieving the technical effect of improving the thickness control accuracy of atomic layer deposition multilayer films. The embodiments of this application are described below in conjunction with the accompanying drawings. It is known to those skilled in the art that with the development of technology and the emergence of new scenarios, the technical solutions provided by this application are also applicable to similar technical problems.

[0022] The terms "first", "second", etc. in the specification and claims of this application and the above-mentioned drawings are used to distinguish similar objects, and are not necessarily used to describe a specific order or sequence. It should be understood that the terms used in this way can be interchanged under appropriate circumstances. This is merely a way of distinguishing when describing objects with the same properties in the embodiments of the present application. In addition, the terms "including" and "having" and any variations thereof are intended to cover non-exclusive inclusions, so that a process, method, system, product or apparatus that includes a series of units is not necessarily limited to those units, but may include other units not expressly listed or inherent to these processes, methods, products or apparatuses.

[0023] Application Overview

[0024] Atomic layer deposition (ALD) is a thin film deposition technology based on self-terminating surface reactions. It has the advantages of good uniformity, high conformality, and precise control of film thickness. It has been widely used in optoelectronics, semiconductors, nanotechnology and other fields. However, with the continuous development of precision device preparation technology, high-performance multilayer film devices have increasingly stringent requirements on the thickness control accuracy of their deposited films, especially the control accuracy of thicker multilayer films. For example, in the preparation of X-ray Fresnel lenses and multilayer film mirrors prepared by atomic layer deposition slicing method, small errors in single-layer film thickness often accumulate into large errors in multilayer film thickness, causing device performance degradation or even failure.

[0025] At present, there are relatively few studies on the thickness control methods of atomic layer deposition multilayer films. Most of them focus on examining the influence of single process conditions (temperature, vacuum degree, etc.) on the thickness of thin film deposition. It is difficult to form a systematic control scheme, and it is unable to solve important issues affecting film thickness in actual applications, such as environmental changes in the thin film growth chamber, uncertainty in thin film growth rate, increased device preparation time, and real-time adjustment of process parameters. As a result, it is difficult to improve control accuracy and has caused certain limitations on the development of device performance.

[0026] Therefore, how to determine the film thickness control scheme of atomic layer deposition technology and obtain ideal multilayer film thickness control accuracy is a technical problem that needs to be solved urgently.

[0027] In response to the above technical problems, the overall idea of ​​the technical solution provided by this application is as follows:

[0028] S100: placing a sample and a companion film in a reaction chamber; S200: performing atomic layer deposition of the growth material required for the multilayer film in the reaction chamber using the first process parameters to obtain a multilayer film sample; S300: performing electron microscope imaging on the multilayer film sample to obtain film layer growth data; S400: comparing the actual film thickness with the theoretical film thickness to obtain an average growth rate; S500: judging whether the average growth rate satisfies a first growth rate change trend; S600: when the average growth rate does not satisfy the first growth rate change trend, eliminating error data in the average growth rate, and repeating S400-S600 based on the film layer growth data after eliminating the error data until the average growth rate satisfies the first growth rate change trend; S700: using the average growth rate as the initial growth rate of the thin film material in the next stage; S800: keeping the process conditions unchanged, adjusting the process parameters, and repeating S100-S700; S900: obtaining a multilayer film device with high mold thickness control accuracy.

[0029] After introducing the basic principles of the present application, various non-limiting implementation methods of the present application will be specifically introduced in conjunction with the drawings in the specification.

[0030] Example 1

[0031] The present application provides a method for improving the thickness control accuracy of atomic layer deposition multilayer films, such as Figure 1 As shown, the method includes:

[0032] S100: placing a sample and a companion piece in a reaction chamber;

[0033] S200: performing atomic layer deposition of a material required for growing the multilayer film in the reaction chamber using first process parameters to obtain a multilayer film sample;

[0034] The step S200 of the present application further includes: introducing an inert gas into the reaction chamber for 1-300 seconds, evacuating the reaction chamber to a vacuum degree of 5×10 -3 -9×10 -3 Torr or less; after the reaction chamber, substrate, pipeline and reaction source are heated and stabilized at the set temperature, a precursor source is alternately introduced into the reaction chamber for 0.01-5.00s to perform atomic layer deposition of the growth material required for the multilayer film to obtain a multilayer film sample, and the above process parameters are recorded as the first process parameters.

[0035] Specifically, a substrate such as silicon, sapphire, or glass is placed in an atomic layer deposition reaction chamber, and an inert gas is introduced for 1-300 seconds to evacuate the reaction chamber to a pressure of 5×10 -3 -9×10 -3Torr or less, and start heating the substrate, reaction chamber, pipeline, reaction source, etc.; after the reaction chamber, substrate, pipeline and reaction source are heated and stabilized at the set temperature (the heating temperature range of the pipeline is 20-300°C, the heating temperature range of the reaction chamber is 20-300°C, the heating temperature range of the reaction source is 20-200°C, and the heating temperature range of the precursor source is 70-80°C), the precursor source is alternately introduced into the reaction chamber for 0.01-5.00s to perform atomic layer deposition of the growth material required for the multilayer film to obtain a stacked structure, and the process parameters such as the vacuum degree, carrier gas value, and process recipe are recorded.

[0036] S300: performing electron microscope imaging on the multilayer film sample to obtain film growth data;

[0037] S300 of the present application also includes: waiting for the multilayer film sample to cool to room temperature and then taking it out; imaging the multilayer film sample with an electron microscope, measuring the film thickness layer by layer, and performing an average calculation to obtain the growth rate of the growing material; using the growth rate as the starting rate, and calculating the cycles sample table required for thin film growth based on the designed thickness of each film layer, and using it as the film layer growth data.

[0038] Specifically, after the deposition process is completed, the multilayer film sample is cooled to room temperature in a vacuum and then taken out for electron microscopy imaging. The thickness of each layer is measured using measurement software, and the average calculation is performed to obtain the growth rate of the growing material (unit: ) as the starting rate, and according to the designed thickness of each film layer, the cycles sample table required for thin film growth is calculated.

[0039] S400: Compare the actual film thickness with the theoretical film thickness to obtain the average growth rate;

[0040] S400 of the present application also includes: preparing a silicon substrate, ultrasonically cleaning it with acetone, ethanol, and deionized water for 10-20 minutes respectively, and blowing it with high-purity nitrogen until the moisture meets the first predetermined requirement; cutting the cleaned silicon substrate into n small silicon wafers and placing them around the multilayer film sample, changing the cycles value of the process recipe, and keeping the other parameters unchanged to grow the multilayer film; when the multilayer film deposition meets the predetermined thickness, taking out the n small silicon wafers, performing electron microscope imaging, and measuring the film thickness sample by sample and layer by layer, collating the actual film thickness data of each film layer, and obtaining the average growth rate based on the film thickness data of each film layer.

[0041] Specifically, a substrate is prepared for cutting, and a small-sized substrate is ultrasonically cleaned with acetone, ethanol, and deionized water for 5-20 minutes to remove impurities that may exist on the surface, and then blown dry with high-purity inert gas. The multilayer film sample is fixed in an atomic layer reaction chamber, and a cleaned substrate is placed around the multilayer film sample as a companion film. The growth of the film is monitored, and the experimental parameters are set to the parameter values ​​set in the initial experiment. After the experimental conditions are met, the film growth is carried out alternately. After depositing 5000-15000 cycles of film thickness, the process experiment is suspended, and the multilayer film sample is cooled to room temperature in a vacuum. The film in the chamber is cleaned, the companion film is taken out, and the cross-sectional imaging is performed by an electron microscope. The companion films are measured layer by layer to obtain the actual film thickness data of each layer.

[0042] S500: Determine whether the average growth rate meets a first growth rate change trend;

[0043] S400 of the present application also includes: preliminarily eliminating error data of the thickness data of each layer of the membrane to obtain first processed data; calculating the average growth rate based on the first processed data; calculating a stage error change curve based on the average growth rate, and judging whether the stage error change curve meets the first growth rate change trend; when the stage error change curve does not meet the first growth rate change trend, data is eliminated according to the error percentage in the first processed data, and iterative calculation is continued until the stage error change curve calculated after the iteration meets the first growth rate change trend.

[0044] S600: When the average growth rate does not satisfy the first growth rate variation trend, eliminating error data in the average growth rate, and repeating S400-S600 based on the film growth data after eliminating the error data until the average growth rate satisfies the first growth rate variation trend;

[0045] S700: using the average growth rate as the initial growth rate of the thin film material in the next stage;

[0046] Specifically, the measured data is processed, and the error data is first eliminated, that is: the error data of the thickness data of each layer of the film is preliminarily eliminated to obtain the first processed data, and the average actual growth rates of the two materials are calculated respectively; secondly, the error between the actual film thickness and the theoretical film thickness is solved, so as to obtain the error change curve of this stage; then it is judged whether the average growth rate conforms to the change trend. If not, the error percentage is used as the judgment basis, and the data with a larger error percentage is continued to be eliminated for iterative calculation; if the average growth rate conforms to the change trend, it is regarded as the initial rate of the next stage.

[0047] S800: keep the process conditions unchanged, adjust the process parameters, and repeat S100-S700;

[0048] S900: Obtain multilayer film devices with high mold thickness control accuracy.

[0049] Specifically, the process parameters, including the calculated cycles and the size of the carrier gas flowmeter, are adjusted to keep the process conditions stable, and the above steps are repeated until the deposition of the stacked structure is completed, thereby obtaining a multilayer film device with high mold thickness control accuracy.

[0050] The growth materials described in this application can be various types of thin films, such as single substances (Co, Cu, Ta, Ti, W, Ge, Pt, Ru, Ni, Fe, Ir, etc.), nitrides (TiN, SiN, AlN, TaN, ZrN, HfN, WN, etc.), oxides (TiO2, HfO2, SiO2, ZnO, ZrO2, Al2O3, La2O3, SnO2, Ta2O5, etc.) and other compounds (GaAs, AlP, InP, GaP, InAs, LaHfxOy , SrTiO3, SrTaO6, etc.), the grown thin film materials are aluminum oxide and hafnium oxide; the precursor sources include trimethylaluminum (TMA), tetrakis(dimethylamine)hafnium (TDMAH) and deionized water; the heating temperature range of the pipeline is 20-300°C, the heating temperature range of the reaction chamber is 20-300°C, the heating temperature range of the reaction source is 20-200°C, and the heating temperature range of the precursor source is 70-80°C; the adjustment range of the process vacuum is 0.10Torr-1.00Torr.

[0051] Example 2

[0052] 1) Place the silicon substrate in an atomic layer deposition reaction chamber, evacuate the reaction chamber, and reduce the vacuum degree of the chamber to 5×10 -3 -9×10 -3 Torr or less, and set the heating temperature of the substrate, reaction chamber, pipeline, reaction source, etc. at the same time. After the actual temperature reaches the set temperature, keep it warm for 1-2 hours, set the gas flow value, and maintain the process vacuum degree at 0.10Torr-0.25Torr.

[0053] 2) Set the substrate heating temperature to 100-200°C, the pipeline heating temperature to 80-150°C, the aluminum source and oxygen source to room temperature, and the hafnium source to saturated vapor pressure at room temperature. The source bottle needs to be heated because the saturated vapor pressure is low. Therefore, the temperature is set to 70-75°C. After the reaction conditions are stable, the carrier gas N2 is introduced into the reaction chamber as the first precursor aluminum source trimethylaluminum for 0.02-0.80s, purged for 10-60s, and then the oxygen source deionized water is introduced for 0.015-0.80s, purged for 10-6 0s, after completing the growth of the set cycles, an aluminum oxide film is obtained; then, the second precursor, hafnium source tetrakis(dimethylamine) hafnium, is introduced for 0.08-0.80s, purged for 15-60s, and then the oxygen source, deionized water, is introduced for 0.015-0.80s, purged for 10-60s, and after completing the growth of the set cycles, a hafnium oxide film is obtained. The two films are grown alternately in a cycle to obtain the initial stacked structure, and the process vacuum is recorded to be 0.19-0.20Torr.

[0054] 3) After the deposition is completed and cooled to room temperature, the multilayer film sample is taken out and the initial growth rate of aluminum oxide is obtained by cross-sectional measurement using an electron microscope. Growth rate of hafnium oxide According to the designed multilayer film structure, the cycles sample table required for growth is calculated.

[0055] 4) Prepare a silicon substrate, ultrasonically clean it with acetone, ethanol, and deionized water for 15 minutes each, and blow dry it with high-purity nitrogen gas.

[0056] 5) Cut the cleaned silicon substrate into multiple small silicon wafers and place them around the sample. Change the cycles value of the process recipe while keeping other parameters unchanged to grow the multilayer film sample.

[0057] 6) After depositing a film with a thickness of 8000 cycles, the multilayer film sample was cooled to room temperature, the small silicon wafer was taken out, and electron microscope imaging was performed. The film thickness of the multilayer film sample was measured layer by layer, and a comparison table of the theoretical film thickness and the actual film thickness was obtained, as shown in FIG. Figure 2 .

[0058] 7) Process the measured data. Taking the 65-98 layers of the zone plate structure as an example, the average growth rates of the aluminum oxide and hafnium oxide layers in the previous stage (41-64) are 0.712 and

[0059] First, the actual average growth rate is solved. After excluding the data with obvious differences (generally the error percentage is 25% or above), the average growth rates of the two materials are calculated to be and Secondly, the variation curve of the film thickness error percentage is obtained. The analysis shows that the growth rate of aluminum oxide in this stage shows a decreasing trend, while the variation trend of hafnium oxide is the opposite. Therefore, the calculated result is not accurate. Therefore, the data with large errors (20% and above) are further excluded, and the calculated results are 0.707 and This group of results is consistent with the growth rate change trend of the two materials. Therefore, it can be used as the initial rate for the next stage to update the cycles value of the sample table.

[0060] 8) Change the obtained cycles numerical parameter in the process recipe and adjust other process parameters to maintain the process conditions unchanged to obtain an optimized high-precision film structure. Repeat steps 4-7 to complete the deposition of the multilayer film structure.

[0061] In summary, the method of the present invention proposes for the first time a method for improving the thickness control accuracy of atomic layer deposition multilayer films. The method is simple to operate and can be used for a large number of repeatable experiments. The ALD multilayer film structure prepared by the method is extremely close to the theoretical stacked structure, fully leveraging the advantage of precise controllable ALD film thickness. The present invention is of great significance for improving the performance of thicker multilayer film devices prepared by atomic layer deposition technology in fields such as biological detection, flexible panels, and microscopic spectroscopy.

[0062] Based on the above technical solution and the test results of the samples prepared according to this method, the present invention has the following beneficial effects:

[0063] 1) During the thin film growth process, the process parameters are easy to control and the data adjustment range is small. Through limited data processing and simple changes in process parameters, high-precision layer-by-layer control of thicker multilayer films can be achieved.

[0064] 2) It does not affect the growth of the multilayer film and has little impact on the preparation time of the multilayer film device.

[0065] 3) The preparation method has a high success rate and can be repeated many times.

[0066] It should be noted that the steps and methods employed in the claims of the present invention are the same as those in the above-described embodiments. To avoid redundancy, the present invention describes preferred embodiments. However, those skilled in the art may make additional changes and modifications to these embodiments once they understand the basic inventive concepts. Therefore, the appended claims are intended to be interpreted as covering the preferred embodiments and all changes and modifications that fall within the scope of the present invention.

[0067] Obviously, those skilled in the art may make various changes and modifications to the present invention without departing from the spirit and scope of the present invention. Thus, if such changes and modifications fall within the scope of the claims and their equivalents, the present invention is intended to include such changes and modifications.

Claims

1. A method for improving the thickness control accuracy of atomic layer deposition multilayer films, characterized in that: The method comprises: S100: placing a sample and a companion piece in a reaction chamber; S200: performing atomic layer deposition of a material required for growing the multilayer film in the reaction chamber using first process parameters to obtain a multilayer film sample; S300: performing electron microscope imaging on the multilayer film sample to obtain film growth data; S400: Compare the actual film thickness with the theoretical film thickness to obtain the average growth rate; S500: Determine whether the average growth rate meets a first growth rate change trend; S600: When the average growth rate does not satisfy the first growth rate variation trend, eliminating error data in the average growth rate, and repeating S400-S600 based on the film growth data after eliminating the error data until the average growth rate satisfies the first growth rate variation trend; S700: using the average growth rate as the initial growth rate of the thin film material in the next stage; S800: keep the process conditions unchanged, adjust the process parameters, and repeat S100-S700; S900: Obtain multilayer film devices with high film thickness control accuracy.

2. The method according to claim 1, wherein The method S200 further includes: The reaction chamber was purged with inert gas for 1-300s, and the reaction chamber was evacuated to a vacuum degree of 5×10 -3 -9×10 -3 Torr below; After the reaction chamber, substrate, pipeline and reaction source are heated and stabilized at the set temperature, the precursor source is alternately introduced into the reaction chamber for 0.01-5.00s to perform atomic layer deposition of the growth material required for the multilayer film to obtain a multilayer film sample, and the above process parameters are recorded as the first process parameters.

3. The method according to claim 1, wherein The method S300 further includes: Waiting for the multilayer film sample to cool to room temperature and then taking it out; Taking electron microscope images of the multilayer film sample, measuring the film thickness layer by layer, and performing average calculation to obtain the growth rate of the growing material; The growth rate is used as the starting rate, and according to the designed thickness of each film layer, a cycles sample table required for thin film growth is calculated and obtained, which is used as the film layer growth data.

4. The method according to claim 1, wherein The method S400 further includes: When the multilayer film deposition meets the predetermined thickness, n small silicon wafers are taken out, imaged by an electron microscope, and the film thickness is measured sample by sample and layer by layer. The actual film thickness data of each film layer is sorted out, and the average growth rate is obtained based on the film thickness data of each film layer.

5. The method according to claim 4, wherein The method S500 further includes: Preliminarily eliminating error data from the thickness data of each film layer to obtain first processed data; Calculate the average growth rate according to the first processed data; Calculating a stage error change curve based on the average growth rate, and determining whether the stage error change curve satisfies the first growth rate change trend; When the stage error change curve does not satisfy the first growth rate change trend, data is eliminated according to the error percentage in the first processed data, and iterative calculation is continued until the stage error change curve calculated after iteration satisfies the first growth rate change trend.

6. The method according to claim 1, wherein The growth material includes simple substance, nitride and oxide.

7. The method according to claim 2, wherein The precursor source includes trimethylaluminum, tetrakis(dimethylamine)hafnium (TDMAH) and deionized water.

8. The method according to claim 2, wherein The heating temperature range of the pipeline is 20-300°C, the heating temperature range of the reaction chamber is 20-300°C, the heating temperature range of the reaction source is 20-200°C, and the heating temperature range of the precursor source is 70-80°C.

9. The method according to claim 1, wherein The adjustment range of process vacuum is 0.10Torr-1.00Torr.

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