Graphene in-situ characterization method and system
Patent Information
- Application Number
- CN202411383107.9
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-09-30
- Publication Date
- 2024-12-13
Smart Images
Figure CN119124067A_ABST
Abstract
Description
Technical Field
[0001] The present invention belongs to the technical field of graphene quality detection, and in particular relates to a graphene in-situ characterization method and system. Background Art
[0002] In 2018, my country launched a special plan for the development and application of standards for carbon-based nanomaterials such as graphene, focusing on the research of graphene detection technology. In recent years, a series of structural-related detection standards and methods for graphene materials have emerged. However, among these standards, only GB / T40066-2021 "Nanotechnology Graphene Oxide Thickness Measurement by Atomic Force Microscopy" and GB / T40066-2021 "Nanotechnology Graphene-related Two-dimensional Materials Layer Number Measurement by Raman Spectroscopy" have been published as national standards, and other standards are still under preparation. In addition, these standards and methods are mostly aimed at a certain parameter of graphene materials and cannot evaluate the overall properties of graphene materials. Some foreign standards such as ISO TS21356-1-2021 "Graphene Powder and Dispersion Detection", PAS1201-2018 "Properties of Graphene Sheets", and "Good Practice Guide for Graphene Structural Characterization" expect to comprehensively evaluate graphene materials through a variety of instruments, and provide guidance on the macroscopic analysis of a certain aspect of the properties of graphene by combining multiple parameters. However, multiple instruments cannot accurately characterize samples at the same location, the test data cannot be accurately matched, and multi-parameter comprehensive analysis cannot be performed, so the test results lack credibility and comprehensiveness.
[0003] In-situ characterization technology is a very important means of characterizing nanomaterials. For the study of material structure and performance, as well as the qualitative determination of samples, accurate characterization of the same area and the same position is far more accurate and reliable than the results of statistical measurements. In-situ characterization technology has been developed for many years and is often used in scientific research, but rarely used in production and testing. At present, there are two main in-situ characterization schemes: SEM-based in-situ characterization function module expansion and software-based multi-instrument coordinate correlation.
[0004] The large space of SEM provides more possibilities for functional expansion. Equipping SEM with other characterization instruments can realize the in-situ characterization function of graphene. Its functional feature is to adjust the focus of SEM and other characterization instruments to the same position, so that each instrument can be characterized in turn, and the sample does not need to be moved or transferred. Equipping SEM with other characterization instruments is a better method for in-situ characterization, but it is prone to the following problems: the concentration of various characterization instruments in one will seriously weaken the functional diversity, working stability, and parameter adjustability; secondly, the expansion of these accessories is expensive, complex in structure, difficult to maintain, and has a high failure rate, so it is not currently popularized.
[0005] Software-based multi-instrument coordinate association is a new technology in the past five years. The working principle is to install the same coordinate control software for multiple instruments that want to achieve in-situ characterization functions, and pre-position the universal sample stage in each instrument. For samples at a specific location, the coordinates are recorded and positioned in one of the instruments, and the universal sample stage is transferred to other instruments equipped with the software. By entering the coordinates, it can automatically move to the position recorded by the previous instrument, thereby realizing joint characterization. However, due to the universality of the software, the software of different instrument manufacturers is not open to authorization or is not compatible with the software, so it can only be used in conjunction with a limited number of devices from the same manufacturer. Instruments that want to be used in conjunction need to use a universal sample stage, but most old instruments and instruments of different brands cannot be used with the universal sample stage. Therefore, there is currently no coordinate software and hardware that can be used between different brands and different systems. Summary of the invention
[0006] The object of the present invention is to provide a method and system capable of in-situ characterization of a graphene sample, which can enable each detection instrument to be accurately positioned on the graphene sample for joint detection.
[0007] The above-mentioned purpose is achieved by the following technical solutions.
[0008] A first aspect of the present invention provides a graphene in-situ characterization method, comprising the following steps:
[0009] Placing the sample to be tested on a base; wherein the base is provided with a plurality of identification areas, each of which has a different identifier;
[0010] Placing the base in the working area of a scanning electron microscope for scanning processing to obtain the microscopic morphology of the sample to be tested, and locating the identification area where the sample to be tested is located to obtain an identifier of the corresponding position of the sample to be tested;
[0011] The base is transferred to the working area of the Raman spectrometer, and according to the identifier of the identification area where the sample to be tested is located, the sample to be tested is moved to the focal position of the Raman spectrometer, and the Raman spectrum of the sample to be tested is measured and recorded;
[0012] The base is transferred to the working area of the atomic force microscope, and the sample to be tested is moved to the needle tip position of the atomic force microscope according to the identifier of the identification area where the sample to be tested is located, and the surface morphology image and edge thickness of the sample to be tested are measured and recorded.
[0013] In some of these embodiments, the identification area includes a first area and a second area, and the identifier includes a first identifier and a second identifier;
[0014] The base is provided with a plurality of regularly arranged first areas, each of which is marked with a different first identifier, and each of the first areas is divided into a plurality of regularly arranged second areas, each of which is marked with a different second identifier.
[0015] In some embodiments, the first region is rectangular, and the first regions are arranged in an array on the base.
[0016] In some embodiments, the second region is rectangular, and the second regions are arranged in an array within the first region.
[0017] In some of the embodiments, there is a space between two adjacent first regions.
[0018] In some of the embodiments, when the scanning electron microscope is scanning the microscopic morphology of the sample to be tested, the acceleration voltage of the scanning electron microscope is 2kV-5kV, and the beam current is 10μA-30μA.
[0019] In some embodiments, the wavelength of the scanning laser of the Raman spectrometer is 532nm or 633nm, and the scanning range is 1100cm -1 -3000cm -1 , the laser power on the sample surface is ≤1mW.
[0020] In some embodiments, the base is one of a silicon wafer, a quartz wafer, and a sapphire wafer, and the identifier is engraved on the base by engraving.
[0021] In some of the embodiments, the method for preparing the sample to be tested is: placing the sample to be tested in a dispersant for ultrasonic dispersion to obtain a graphene dispersion liquid, and dripping the graphene dispersion liquid onto the base and performing a drying process.
[0022] The second aspect of the present invention provides a system for the graphene in-situ characterization method as described above, comprising a base, a scanning electron microscope, a Raman spectrometer, an atomic force microscope and a mobile platform; the scanning electron microscope, the Raman spectrometer and the atomic force microscope are arranged in sequence;
[0023] The mobile platform is arranged below the base and can drive the base to move below the scanning electron microscope, the Raman spectrometer and the atomic force microscope; a plurality of identification areas are arranged on the base, and each identification area has a different identifier.
[0024] In the present invention, a plurality of identification areas are provided on the base, and each identification area has a different identifier. Therefore, according to the different positions of the sample to be tested on the base, the corresponding identifier can be obtained according to the identification area at the position where the sample is located. Therefore, the sample to be tested can be accurately located by the identifier. In combination with the use of a scanning electron microscope, a Raman spectrometer and an atomic force microscope, the microscopic morphology characterization, Raman spectrum characterization, surface morphology image and edge thickness of the same sample can be characterized and measured. The data of the three characterization methods are for the same sample piece, and the data can correspond to each other, so that the sample can be accurately and comprehensively qualitatively analyzed, the position of the characterization is precise, and the data credibility is high. BRIEF DESCRIPTION OF THE DRAWINGS
[0025] Figure 1 It is a schematic diagram of the enlarged structure of a local marking area of a base according to an embodiment of the present invention;
[0026] Figure 2 This is a SEM microscopic morphology of the mechanically exfoliated graphene in the unit cell A5-b5 of the base in Example 1;
[0027] Figure 3 The 500x microscope image and Raman spectrum image of the mechanically exfoliated graphene in the unit cell A5-b5 of the base in Example 1, wherein Figure 3 (a) is a 500x microscope image. Figure 3 (b) is the Raman spectrum;
[0028] Figure 4 The AFM image and edge thickness of the mechanically exfoliated graphene in the unit cell A5-b5 of the base in Example 1;
[0029] Figure 5 The SEM microscopic morphology of graphene oxide in the unit cell A5-f5 of the base in Example 2;
[0030] Figure 6 The 500x optical image and Raman spectrum of graphene oxide in the unit cell A5-f5 of the base in Example 2 are shown in FIG. Figure 6 (a) is a 500x microscope image. Figure 6 (b) is the Raman spectrum;
[0031] Figure 7 The AFM image and edge thickness of graphene oxide in the unit cell A5-f5 of the base in Example 2. DETAILED DESCRIPTION
[0032] In order to facilitate the understanding of the present invention, the present invention will be described more fully below. The present invention can be implemented in many different forms and is not limited to the embodiments described herein. On the contrary, the purpose of providing these embodiments is to make the understanding of the disclosure of the present invention more thorough and comprehensive.
[0033] The experimental methods in the following examples without specifying specific conditions are usually carried out under conventional conditions or conditions recommended by the manufacturers. The various commonly used chemical reagents used in the examples are all commercially available products.
[0034] Unless otherwise defined, all technical and scientific terms used in the present invention have the same meaning as those commonly understood by those skilled in the art to which the present invention belongs. The terms used in the specification of the present invention are only for the purpose of describing specific embodiments and are not intended to limit the present invention. The term "and / or" used in the present invention includes any and all combinations of one or more of the related listed items.
[0035] The embodiment of the present invention provides a graphene in-situ characterization method, comprising the following steps:
[0036] Placing the sample to be tested on a base; wherein the base is provided with a plurality of identification areas, each of which has a different identifier;
[0037] Placing the base in the working area of a scanning electron microscope for scanning processing to obtain the microscopic morphology of the sample to be tested, and locating the identification area where the sample to be tested is located to obtain an identifier of the corresponding position of the sample to be tested;
[0038] The base is transferred to the working area of the Raman spectrometer, and according to the identifier of the identification area where the sample to be tested is located, the sample to be tested is moved to the focal position of the Raman spectrometer, and the Raman spectrum of the sample to be tested is measured and recorded;
[0039] The base is transferred to the working area of the atomic force microscope, and the sample to be tested is moved to the needle tip position of the atomic force microscope according to the identifier of the identification area where the sample to be tested is located, and the surface morphology image and edge thickness of the sample to be tested are measured and recorded.
[0040] Among them, since a plurality of identification areas are arranged on the base, and each identification area has a different identifier, according to the different positions of the sample to be tested on the base, the corresponding identifier can be obtained according to the identification area at the position where the sample to be tested is located, so the sample to be tested can be accurately located by the identifier, and combined with the coordinated use of the scanning electron microscope, the Raman spectrometer and the atomic force microscope, when the scanning electron microscope scans the microscopic morphology of the sample to be tested, the identification area where the sample to be tested is located can be located at the same time, and the identifier of the corresponding position of the sample to be tested can be obtained, and when the Raman spectrometer and the atomic force microscope are measured in the next step, the position of the sample to be tested can be accurately obtained according to the identifier, wherein the Raman spectrometer obtains the Raman spectrum of the sample to be tested, and the atomic force microscope obtains the surface morphology image and edge thickness of the sample to be tested, so according to the joint in-situ characterization of the scanning electron microscope, the Raman spectrometer and the atomic force microscope, the sample is qualitatively determined, wherein the microscopic morphology of the sample to be tested is measured to be flaky, the Raman spectrum has an obvious G peak, and the edge thickness measured by AFM is ≤3.4nm, that is, the sample is considered to be graphene, otherwise it is not graphene.
[0041] In summary, by setting up multiple identification areas on the base, and each identification area has a different identifier, according to the different positions of the sample to be tested on the base, the corresponding identifier can be obtained according to the identification area at its position, so the sample to be tested can be accurately located by the identifier, and combined with the use of a scanning electron microscope, a Raman spectrometer and an atomic force microscope, it is possible to characterize and measure the microscopic morphology, Raman spectrum, surface morphology image and edge thickness of the same sample. The data of the three characterization methods are for the same sample piece, and the data can correspond to each other, so the sample can be comprehensively qualitatively analyzed, the characterization position is accurate, and the data credibility is high.
[0042] In some embodiments, the identification area includes a first area and a second area, and the identifier includes a first identifier and a second identifier; wherein the base is provided with a plurality of regularly arranged first areas, each of which is marked with a different first identifier, and each of the first areas is divided into a plurality of regularly arranged second areas, each of which is marked with a different second identifier. wherein a large first area is provided on the base and marked with different first identifiers, for example, a coordinate number can be engraved on the upper left corner of the outer side of the first area as the first identifier, such as Figure 1As shown, for example, capital letters plus numbers can be used, such as A1, A2, A3...A8 in the first column, B1, B2, B3...B8 in the second column, and H1, H2, H3...H8 in the eighth column. Each first area is divided into multiple second areas, for example, 8×8 to 10×10 cells, and the cells are marked with coordinates in rows and columns. The row coordinates are 1, 2, 3...8, and the column coordinates are lowercase letters a, b, c...h. For example, the coordinate of the first cell in the first row is a1, the coordinate of the third cell in the second row is b3, and so on. By coordinating the first area and the second area and the first identifier and the second identifier, when the base is placed in the working area of the scanning electron microscope for scanning processing, the first identifier of the first area and the second identifier of the second area where the sample to be tested is located are obtained. After the base is transferred to the working area of the Raman spectrometer, the first area is first found in the low-power microscope according to the first identifier, and then the second area is found in the high-power microscope according to the second identifier, so that the sample is accurately matched with the focal position of the Raman spectrometer, so as to facilitate the measurement of the Raman spectrometer. Similarly, after the base is transferred to the working area of the atomic force microscope, the first area is first found in the low-power microscope according to the first identifier, and then the second area is found in the high-power microscope according to the second identifier, so that the sample is accurately matched with the needle tip position of the atomic force microscope, so as to facilitate the scanning of the atomic force microscope. Therefore, by setting the structure of the first area and the second area on the base, the position of the sample can be quickly and accurately located.
[0043] In some embodiments, the first area is rectangular, and each of the first areas is arranged in an array on the base. Preferably, there is a spacing between two adjacent first areas; wherein the spacing between the two adjacent first areas is used to engrave a coordinate number as a first identifier, specifically, the coordinate number is engraved on the upper left corner of the outer side of the first area as the first identifier. More preferably, the spacing between two adjacent first areas is 80μm to 150μm.
[0044] In some embodiments, the second region is rectangular, and each of the second regions is arranged in an array within the first region.
[0045] Among them, the rectangular array is arranged regularly, which can quickly locate the graphene sample according to the identifier of the location.
[0046] In some embodiments, when the scanning electron microscope is scanning the microscopic morphology of the sample to be tested, the acceleration voltage of the scanning electron microscope is 2kV-5kV, and the beam current is 10μA-30μA.
[0047] In some embodiments, the wavelength of the scanning laser of the Raman spectrometer is 532nm or 633nm, and the scanning range is 1100cm -1 -3000cm -1 , the laser power on the sample surface is ≤1mW. Specifically, the Raman spectrometer can be a microscopic Raman spectrometer, which has both the function of microscope imaging and the function of Raman spectrum analysis.
[0048] In some embodiments, the base is one of a silicon wafer, a quartz wafer, and a sapphire wafer. Specifically, the first region, the second region, the first identifier, and the second identifier may be engraved on the base by photolithography.
[0049] In some embodiments, the preparation method of the sample to be tested is: placing the sample to be tested in a dispersant for ultrasonic dispersion to obtain a graphene dispersion, and dripping the graphene dispersion onto the base and performing a drying process. The dispersant may be anhydrous ethanol.
[0050] The embodiment of the present invention also provides a system for the graphene in-situ characterization method as described above, the system comprising a base, a scanning electron microscope, a Raman spectrometer, an atomic force microscope and a mobile platform; the scanning electron microscope, the Raman spectrometer and the atomic force microscope are arranged in sequence;
[0051] The mobile platform is arranged below the base and can drive the base to move below the scanning electron microscope, the Raman spectrometer and the atomic force microscope; a plurality of identification areas are arranged on the base, and each identification area has a different identifier. Specific implementation method:
[0053] Embodiment 1:
[0054] This embodiment provides a graphene in-situ characterization method, comprising the following steps:
[0055] (1) Select the base structure
[0056] A single-sided polished silicon wafer was selected as the base material, and the base was a rectangle with a side length of 1.2 cm.
[0057] The surface of the base is engraved with 8×8 independent large rectangular cells as the first area. The large cells are 250μm apart; the large cell width is 1000μm, the engraved line width is 10μm, and the coordinate engraved line depth is 3μm. The coordinate number is engraved in the upper left corner of the outer side of the large cell. The number is in the form of capital letters plus numbers, such as A1, A2, A3...A8 in the first column, B1, B2, B3...B8 in the second column, and H1, H2, H3...H8 in the eighth column.
[0058] Each large cell is engraved with 9×9 small rectangular cells as the second area. Each small cell is 90μm wide, the line width is 10μm, and the coordinate line depth is 3μm. The cells are divided into rows and columns to engrave coordinates. The first row coordinates are numbers 1, 2, 3...8, and the first column coordinates are lowercase letters a, b, c...h. The coordinates of the first row and the first cell are a1, the coordinates of the second row and the third cell are b3, and so on.
[0059] (2) Sample preparation
[0060] Take an appropriate amount of mechanically exfoliated graphene powder sample and place it in anhydrous ethanol, ultrasonically disperse it for 30 minutes to make a dispersion of appropriate concentration, use a pipette to drop an appropriate amount of the dispersion on the surface of the base, dry it naturally, and obtain a base with a sample on the surface.
[0061] (3) SEM examination of samples
[0062] The base with the sample on the surface was placed in a scanning electron microscope (SEM), and the acceleration voltage was set to 2 kV and the beam current to 25 μA. The flake sample was found and the microscopic morphology of the sample was obtained under an appropriate magnification. Figure 2 Take the SEM microscopic morphology image, appropriately reduce the magnification and record the coordinate f of the small cell where the sample is located, and then appropriately reduce the magnification and record the large cell A5 where the small cell is located.
[0063] (4) Raman spectroscopy of samples
[0064] Transfer the base with the sample to the Raman spectrometer. First, find the large cell A5 where the sample is located in step (3) under the 50x microscope. Figure 3 a. Find the small cell f where the sample is located in step (3) under a 500x microscope. Finally, move the sample to the focal position of the Raman spectrometer and use a 532nm laser with a scanning range of 1100-3000cm. -1 , the laser power on the sample surface is ≤1mW, measure and record the Raman spectrum, see Figure 3 b, observe the Raman spectrum at 1580cm -1 There is an obvious G peak.
[0065] (5) AFM testing of samples
[0066] Transfer the base with the sample to an atomic force microscope (AFM). First, find the large cell A5 where the sample is located in step (3) under a 50x microscope. Then find the small cell f where the sample is located in step (3) under a 500x microscope. Finally, move the sample to the tip of the AFM. Set the scanning range to 5μm and the mode to smart scanning according to the sample size. See Figure 4 , and obtain the sample surface morphology image and edge thickness.
[0067] (6) Qualitative determination of samples
[0068] The qualitative judgment criteria of the samples are shown in Table 1 below.
[0069] Table 1 Qualitative analysis standards / judgment criteria for graphene materials
[0070]
[0071] Depend on Figures 2 to 4 It can be seen that the SEM microstructure of the sample is flake-like. The Raman spectrum shows an obvious -1 The presence of a G peak at , indicating that the sample is a carbon material. The edge thickness measured by AFM is 2.589nm, which is less than the theoretical thickness of 10 layers of graphene, 3.4nm. Therefore, the sample is graphene.
[0072] Embodiment 2:
[0073] This embodiment provides a graphene in-situ characterization method, comprising the following steps:
[0074] (1) Select the base structure
[0075] A single-sided polished silicon wafer was selected as the base material, and the base was a rectangle with a side length of 1.2 cm.
[0076] The surface of the base is engraved with 8×8 independent large rectangular cells as the first area. The large cells are 250μm apart; the large cell width is 1000μm, the engraved line width is 10μm, and the coordinate engraved line depth is 3μm. The coordinate number is engraved in the upper left corner of the outer side of the large cell as the first identifier. The number is in the form of uppercase letters plus numbers, such as A1, A2, A3.......A8 in the first column, B1, B2, B3.......B8 in the second column, and H1, H2, H3.......H8 in the eighth column.
[0077] Each large cell is engraved with 9×9 small rectangular cells as the second area. Each small cell is 90μm wide, the line width is 10μm, and the coordinate line depth is 3μm. The coordinates of the cells are engraved in rows and columns as the second identifier. The first row coordinates are numbers 1, 2, 3...8, and the first column coordinates are lowercase letters a, b, c...h. The coordinates of the first row and the first cell are a1, the coordinates of the second row and the third cell are b3, and so on.
[0078] (2) Sample preparation
[0079] Take an appropriate amount of graphene oxide powder sample and place it in anhydrous ethanol, ultrasonically disperse it for 30 minutes to make a dispersion of appropriate concentration, use a pipette to take an appropriate amount of the dispersion and drop it on the surface of the base, dry it naturally, and obtain a base with the sample on the surface.
[0080] (3) SEM examination of samples
[0081] Place the base with the sample on the surface into the SEM, set the acceleration voltage to 2kV, the beam current to 25μA, and look for the flake sample. The microscopic morphology at an appropriate magnification is obtained. Figure 5 Take the SEM microscopic morphology image, appropriately reduce the magnification and record the coordinate f5 of the small cell where the sample is located, and then appropriately reduce the magnification and record the large cell A5 where the small cell is located.
[0082] (4) Raman spectroscopy of samples
[0083] Transfer the base with the sample to the Raman spectrometer. First, find the large cell A5 where the sample is located in step (3) under the 50x microscope. Figure 6 a. Find the small cell f5 where the sample is located in step (3) under a 500x microscope. Finally, move the sample to the focal position of the Raman spectrometer and use a 532nm laser with a scanning range of 1100-3000cm. -1 , the laser power on the sample surface is ≤1mW, measure and record the Raman spectrum, see Figure 6 b, observe the Raman spectrum at 1580cm -1 There is an obvious G peak.
[0084] (5) AFM testing of samples
[0085] Transfer the base with the sample to an atomic force microscope (AFM). First, find the large cell A5 where the sample is located in step (3) under a 50x microscope. Then find the small cell f5 where the sample is located in step (3) under a 500x microscope. Finally, move the sample to the tip position of the AFM. Set the scanning range to 5μm and the mode to smart scanning according to the sample size. See Figure 7 , and obtain the sample surface morphology image and edge thickness.
[0086] (6) Qualitative determination of samples
[0087] The qualitative determination of the samples is shown in Table 1.
[0088] Depend on Figures 5 to 7 It can be seen that the SEM microscopic morphology of the sample in this embodiment is flake-shaped. The Raman spectrum has an obvious -1 The presence of a G peak at , indicating that the sample is a carbon material. The edge thickness measured by AFM is 1.426nm, which is less than the theoretical thickness of 10 layers of graphene, 3.4nm. Therefore, the sample is graphene.
[0089] In summary, by engraving the first area on a flat base and forming a first identifier, and engraving the second area in the first area to form a second identifier, first find a sample piece that meets the characteristics of graphene under the SEM, gradually reduce the magnification, and record the second identifier and the first identifier of the sample position in turn. Transfer to the Raman spectrometer and atomic force microscope successively, first move to the first area position corresponding to the first identifier under the low-power microscope, then move to the second area position corresponding to the second identifier under the high-power microscope, and finally move the sample to the focus position of the Raman spectrometer or the tip position of the atomic force microscope. According to this method, the sample piece you want to observe can be gradually found, and the SEM, Raman spectroscopy, and AFM can accurately locate the same sample piece, and the same sample piece can be jointly characterized in situ, so that the sample piece can be comprehensively qualitatively analyzed, and the characterization position is accurate and the data credibility is high.
[0090] The technical features of the above-described embodiments may be arbitrarily combined. To make the description concise, not all possible combinations of the technical features in the above-described embodiments are described. However, as long as there is no contradiction in the combination of these technical features, they should be considered to be within the scope of this specification.
[0091] The above-mentioned embodiments only express several implementation methods of the present invention, and the descriptions thereof are relatively specific and detailed, but they cannot be understood as limiting the scope of the invention patent. It should be pointed out that, for ordinary technicians in this field, several variations and improvements can be made without departing from the concept of the present invention, and these all belong to the protection scope of the present invention. Therefore, the protection scope of the patent of the present invention shall be subject to the attached claims.
Claims
1. A graphene in-situ characterization method, characterized in that: The steps include: Placing the sample to be tested on a base; wherein the base is provided with a plurality of identification areas, each of which has a different identifier; Placing the base in the working area of a scanning electron microscope for scanning processing to obtain the microscopic morphology of the sample to be tested, and locating the identification area where the sample to be tested is located to obtain an identifier of the corresponding position of the sample to be tested; The base is transferred to the working area of the Raman spectrometer, and according to the identifier of the identification area where the sample to be tested is located, the sample to be tested is moved to the focal position of the Raman spectrometer, and the Raman spectrum of the sample to be tested is measured and recorded; The base is transferred to the working area of the atomic force microscope, and the sample to be tested is moved to the needle tip position of the atomic force microscope according to the identifier of the identification area where the sample to be tested is located, and the surface morphology image and edge thickness of the sample to be tested are measured and recorded.
2. The graphene in-situ characterization method according to claim 1, characterized in that: The identification area includes a first area and a second area, and the identifier includes a first identifier and a second identifier; The base is provided with a plurality of regularly arranged first areas, each of which is marked with a different first identifier, and each of the first areas is divided into a plurality of regularly arranged second areas, each of which is marked with a different second identifier.
3. The graphene in-situ characterization method according to claim 2, characterized in that: The first regions are rectangular, and the first regions are arranged in an array on the base.
4. The graphene in-situ characterization method according to claim 2, characterized in that: The second region is rectangular, and the second regions are arranged in an array within the first region.
5. The graphene in-situ characterization method according to claim 3, characterized in that: There is a space between two adjacent first areas.
6. The graphene in-situ characterization method according to any one of claims 1 to 5, characterized in that: During the process of scanning the microscopic morphology of the sample to be tested by the scanning electron microscope, the acceleration voltage of the scanning electron microscope is 2kV-5kV, and the beam current is 10μA-30μA.
7. The graphene in-situ characterization method according to any one of claims 1 to 5, characterized in that: The wavelength of the scanning laser of the Raman spectrometer is 532nm or 633nm, and the scanning range is 1100cm -1 -3000cm -1 , the laser power on the sample surface is ≤1mW.
8. The graphene in-situ characterization method according to any one of claims 1 to 5, characterized in that: The base is one of a silicon wafer, a quartz wafer and a sapphire wafer, and the identifier is engraved on the base by engraving.
9. The graphene in-situ characterization method according to any one of claims 1 to 5, characterized in that: The preparation method of the sample to be tested is: placing the sample to be tested in a dispersant for ultrasonic dispersion to obtain a graphene dispersion liquid, and dripping the graphene dispersion liquid onto the base and performing a drying process.
10. A system for the graphene in-situ characterization method according to any one of claims 1 to 9, characterized in that: It includes a base, a scanning electron microscope, a Raman spectrometer, an atomic force microscope and a mobile platform; the scanning electron microscope, the Raman spectrometer and the atomic force microscope are arranged in sequence; The mobile platform is arranged below the base and can drive the base to move below the scanning electron microscope, the Raman spectrometer and the atomic force microscope; a plurality of identification areas are arranged on the base, and each identification area has a different identifier.