A rapid detection method for two-dimensional nanomaterials

Abstract

The invention discloses a rapid detection method for two-dimensional nanomaterials, and relates to the technical field of two-dimensional nanomaterial detection; in order to improve the detection efficiency; comprising the following steps: using modified inorganic substances as a basis, combining graphene or reduced graphene oxide, and performing functional modification to be charged; using X-ray diffraction and transmission electron microscopy to determine the crystal structure of the basic inorganic substance and the number of layers and morphology of graphene / rGO; using an electrochemical workstation to perform cyclic voltammetry monitoring, using a pH meter and an ion chromatograph to monitor solution changes, and performing conductivity testing. The present invention can quickly and accurately determine the crystal structure, number of layers and morphology of two-dimensional nanomaterials, as well as the elemental composition and chemical state of the surface, and improve the detection efficiency by means of technical means such as X-ray diffraction (XRD), transmission electron microscopy (TEM) and X-ray photoelectron spectroscopy (XPS).

Description

Technical Field

[0001] The present invention relates to the technical field of two-dimensional nanomaterial detection, and in particular to a method for rapid detection of two-dimensional nanomaterials. Background Art

[0002] In the existing technology, with the rapid development of nanotechnology, two-dimensional nanomaterials have shown great application potential in many fields such as electronics, optoelectronics, energy, and biomedicine due to their unique physical and chemical properties. Graphene and reduced graphene oxide (rGO), as typical two-dimensional nanomaterials, have become the focus of scientific research and industry due to their excellent conductivity, thermal stability and mechanical strength. However, the performance and application effect of two-dimensional nanomaterials are often affected by many factors such as their structure, morphology, surface chemical state, and response behavior to external stimuli. Therefore, how to quickly and accurately detect and analyze these characteristics of two-dimensional nanomaterials has become a key issue restricting their further application.

[0003] Traditional two-dimensional nanomaterial detection methods, such as scanning electron microscopy (SEM) and atomic force microscopy (AFM), can provide high-resolution images of materials, but the operation is complex and time-consuming, and it is difficult to fully reflect the physical and chemical properties and stimulus response behavior of the materials;

[0004] In order to overcome these shortcomings, the present invention proposes a rapid detection method for two-dimensional nanomaterials. By integrating multiple detection technologies, it is possible to comprehensively and quickly analyze various performance parameters of two-dimensional nanomaterials and achieve efficient detection of two-dimensional nanomaterials. Summary of the invention

[0005] The purpose of the present invention is to solve the shortcomings of the prior art and to propose a rapid detection method for two-dimensional nanomaterials.

[0006] In order to achieve the above object, the present invention adopts the following technical solutions:

[0007] A rapid detection method for two-dimensional nanomaterials comprises the following steps:

[0008] S1: Using modified inorganic substances as a basis, combining graphene or reduced graphene oxide, and functionalizing and modifying them to be charged;

[0009] S2: Determine the crystal structure of the underlying inorganic material and the number and morphology of graphene / rGO layers using X-ray diffraction and transmission electron microscopy;

[0010] S3: Cyclic voltammetry monitoring using an electrochemical workstation, monitoring solution changes using a pH meter and ion chromatograph, and conductivity testing;

[0011] S4: Set trigger conditions, precisely control trigger conditions, observe morphological changes, and monitor electrochemical signal changes;

[0012] S5: Comprehensive evaluation and data analysis.

[0013] Preferably: in step S1, the functional modification is achieved by adding different chemical groups so that the two-dimensional material is charged after protonation or deprotonation.

[0014] Further: In step S2, the operation steps of X-ray diffraction (XRD) include:

[0015] Place the sample in an X-ray diffractometer;

[0016] Adjust the X-ray source, sample position and detector to collect the diffraction pattern.

[0017] Further: In step S2, the operation steps of the transmission electron microscope (TEM) include:

[0018] The sample is dispersed in an appropriate solvent and dropped onto a TEM grid for high-resolution imaging.

[0019] As a preferred solution of the present invention: in step S3, the step of performing cyclic voltammetry monitoring by the electrochemical workstation includes using the material to be tested as a working electrode, forming a three-electrode system with a reference electrode and an auxiliary electrode, immersing the electrode in a solution, and starting the experiment after setting CV parameters.

[0020] As a further solution of the present invention: in step S3, the step of using a pH meter and an ion chromatograph to monitor changes in the solution includes measuring the initial pH value of the solution, stirring after adding the material to be tested, and measuring the pH value and ion concentration at regular intervals.

[0021] As a further solution of the present invention: in step S3, the conductivity test, its operating steps include preparing the material to be tested into a thin film or coating, and placing it between measuring electrodes; setting measurement conditions, such as temperature and humidity, and then starting the experiment; recording conductivity data, and analyzing the conductivity changes of the material under different conditions; based on the conductivity data, evaluating the performance of the material as a two-dimensional electrolyte.

[0022] Based on the above scheme: In step S4, the step of setting the trigger condition includes analyzing the material properties, determining the sensitive range of the material, selecting suitable experimental equipment and connecting equipment, setting the experimental program, and setting the experimental program on the equipment according to the experimental design.

[0023] On the basis of the above scheme: in step S4, the step of observing morphological changes includes selecting appropriate microscopy technology, taking an initial morphological image of the material, observing and recording the morphological changes of the material in real time during the triggering process, taking the morphological image again after the triggering condition ends, and monitoring the changes in electrochemical signals, which includes preparing an electrochemical workstation; setting electrochemical measurement parameters; and monitoring electrochemical signals.

[0024] On the basis of the above scheme: In step S5, the comprehensive evaluation and data analysis step includes integrating all the test data into the database, processing the test data using a machine learning algorithm, predicting the performance of the material and optimizing its design, evaluating the performance of the material based on the test results, and optimizing the material preparation process and triggering conditions based on the evaluation results.

[0025] The beneficial effects of the present invention are:

[0026] 1. A rapid detection method for two-dimensional nanomaterials, which can quickly and accurately determine the crystal structure, number of layers and morphology, as well as the elemental composition and chemical state of the surface of two-dimensional nanomaterials through advanced technical means such as X-ray diffraction (XRD), transmission electron microscopy (TEM) and X-ray photoelectron spectroscopy (XPS).

[0027] 2. A rapid detection method for two-dimensional nanomaterials, using an electrochemical workstation for cyclic voltammetry (CV) monitoring, a pH meter and an ion chromatograph to monitor solution changes, and conductivity testing, can provide a comprehensive understanding of the charge changes of the material during protonation or deprotonation, changes in the pH value and ion concentration of the solution, and the conductivity characteristics of the material.

[0028] 3. A rapid detection method for two-dimensional nanomaterials. By setting precise trigger conditions, selecting suitable experimental equipment and precisely controlling the experimental process, it can accurately evaluate the response behavior of materials under different conditions, and use microscopy technology and electrochemical workstations to monitor the morphological changes and electrochemical signal changes of materials in real time.

[0029] 4. A rapid detection method for two-dimensional nanomaterials integrates all detection data into a database and processes the detection data using machine learning algorithms. It can predict the performance of the material and optimize its design, which can not only improve the performance of the material, but also shorten the R&D cycle and reduce R&D costs. BRIEF DESCRIPTION OF THE DRAWINGS

[0030] Figure 1 It is a schematic flow chart of a rapid detection method for two-dimensional nanomaterials proposed by the present invention. DETAILED DESCRIPTION

[0031] The technical solution of this patent is further described in detail below in conjunction with specific implementation methods.

[0032] The embodiments of the present invention are described in detail below, and examples of the embodiments are shown in the accompanying drawings, wherein the same or similar reference numerals throughout represent the same or similar elements or elements having the same or similar functions. The embodiments described below with reference to the accompanying drawings are exemplary and are only used to explain the present invention, and cannot be understood as limiting the present invention.

[0033] Embodiment 1:

[0034] A rapid detection method for two-dimensional nanomaterials comprises the following steps:

[0035] S1: Material preparation:

[0036] Using modified inorganic substances as a basis, combined with two-dimensional materials such as graphene or reduced graphene oxide (rGO); functionalizing graphene or rGO, adding different chemical groups, so that it undergoes protonation or deprotonation to become positive ions (2D cations) or negative ions (2D anions) and carry a charge;

[0037] S2: Material properties analysis:

[0038] (1) Determine the crystal structure of the basic inorganic material and the number and morphology of graphene / rGO layers using X-ray diffraction (XRD) and transmission electron microscopy (TEM):

[0039] The steps of X-ray diffraction (XRD) include:

[0040] Place the sample in an X-ray diffractometer;

[0041] Adjust the X-ray source, sample position and detector to collect diffraction patterns;

[0042] The operation steps of transmission electron microscopy (TEM) include:

[0043] The sample is dispersed in an appropriate solvent and dropped onto a TEM grid for high-resolution imaging;

[0044] (2) X-ray photoelectron spectroscopy (XPS) is used to analyze the elemental composition and chemical state of the material surface. The operation steps include:

[0045] Place the sample in the XPS instrument, adjust the X-ray source, energy range and detection conditions, and collect the energy spectrum; the purpose is to analyze the elemental composition and chemical state of the material surface;

[0046] S3: Stimulus response behavior detection:

[0047] (1) Cyclic voltammetry (CV) monitoring is performed using an electrochemical workstation, the steps of which include:

[0048] The material to be tested is used as the working electrode, and forms a three-electrode system with the reference electrode and the auxiliary electrode;

[0049] Immerse the three-electrode system in an acidic or alkaline solution, making sure the solution fully covers the working electrode;

[0050] Set CV parameters, such as scan rate and frequency range, and start the experiment;

[0051] Monitor and record electrochemical behavior curves to analyze charge changes during protonation or deprotonation;

[0052] (2) Using a pH meter and an ion chromatograph to monitor solution changes, the operating steps include:

[0053] Use a pH meter to measure the initial pH value of the solution and record it;

[0054] Add the material to be tested into the solution and start stirring to ensure full contact between the material and the solution;

[0055] At regular intervals, use a pH meter to measure the pH value of the solution and record it;

[0056] At the same time, the concentration changes of specific ions in the solution are measured and recorded using an ion chromatograph;

[0057] Analyze changes in pH and ion concentration to infer the protonation / deprotonation state of the material;

[0058] (3) Conductivity test, the operation steps include:

[0059] The material to be tested is prepared into a thin film or coating and placed between the measuring electrodes;

[0060] Set the measurement conditions, such as temperature and humidity, and start the experiment;

[0061] Record conductivity data and analyze conductivity changes of materials under different conditions;

[0062] Based on the conductivity data, the performance of the material as a two-dimensional electrolyte is evaluated;

[0063] S4: Trigger mechanism and response behavior assessment, which includes:

[0064] (1) Set the trigger conditions, including:

[0065] Analytical material properties:

[0066] Understand the physicochemical properties of the material, including its response characteristics to different triggering conditions; determine the sensitive range of the material, such as a specific pH range, temperature range, light intensity, or concentration of a specific chemical;

[0067] (2) Precise control of trigger conditions

[0068] Select experimental equipment:

[0069] According to the experimental requirements, choose suitable programmable automated experimental equipment, such as pH controller, temperature controller, light controller or chemical injection system;

[0070] Connect the experimental equipment:

[0071] Connect the experimental equipment to the material to be tested and ensure that the equipment can accurately control the triggering conditions;

[0072] Set up the experimental procedure:

[0073] According to the experimental design, set the experimental program on the equipment, including the start time, duration, change rate, etc. of the trigger conditions;

[0074] (3) Observe morphological changes

[0075] Prepare the microscope:

[0076] Selection of appropriate microscopy techniques, such as electron microscopy;

[0077] Observe the material form:

[0078] Before the trigger condition is activated, the initial morphological image of the material is first captured. During the triggering process, the morphological changes of the material are observed and recorded in real time. After the trigger condition ends, the morphological image of the material is captured again and compared with the initial image.

[0079] (4) Monitoring changes in electrochemical signals, including:

[0080] (1) Prepare the electrochemical workstation:

[0081] Ensure that the electrochemical workstation is working properly, the electrode system is connected correctly, and the material to be tested is used as the working electrode to form a three-electrode system with the reference electrode and the auxiliary electrode;

[0082] (2) Set electrochemical measurement parameters:

[0083] According to experimental requirements, set electrochemical measurement parameters, such as the scan rate of cyclic voltammetry and the frequency range of electrochemical impedance spectroscopy;

[0084] (3) Monitoring electrochemical signals:

[0085] Before the trigger condition is initiated, the initial value of the electrochemical signal is recorded first. During the trigger process, the changes of the electrochemical signal are monitored and recorded in real time. After the trigger condition ends, the monitoring continues for a period of time.

[0086] S5: Comprehensive evaluation and data analysis includes the following steps:

[0087] Integrate all test data into a database for statistical analysis;

[0088] Use machine learning algorithms to process test data to predict material performance and optimize its design;

[0089] Evaluate material performance, such as sensitivity, selectivity, and reproducibility, based on test results;

[0090] The material preparation process and triggering conditions are optimized based on the evaluation results.

[0091] The above is a preferred specific implementation manner of the present invention, and the protection scope of the present invention is not limited thereto. Any modification, equivalent substitution and improvement made by any technician familiar with the field within the technical scope disclosed by the present invention in combination with the prior art or public common sense, within the spirit and principle of the present invention, shall be covered by the protection scope of the present invention.

Claims

1. A rapid detection method for two-dimensional nanomaterials, characterized in that: The following steps are involved: S1: Using modified inorganic substances as a basis, combining graphene or reduced graphene oxide, and functionalizing and modifying them to be charged; S2: Determine the crystal structure of the underlying inorganic material and the number and morphology of graphene / rGO layers using X-ray diffraction and transmission electron microscopy; S3: Cyclic voltammetry monitoring using an electrochemical workstation, monitoring solution changes using a pH meter and ion chromatograph, and conductivity testing; S4: Set trigger conditions, precisely control trigger conditions, observe morphological changes, and monitor electrochemical signal changes; S5: Comprehensive evaluation and data analysis.

2. A rapid detection method for two-dimensional nanomaterials according to claim 1, characterized in that: In step S1, the functional modification is achieved by adding different chemical groups so that the two-dimensional material is charged after protonation or deprotonation.

3. A rapid detection method for two-dimensional nanomaterials according to claim 2, characterized in that: In step S2, the operation steps of X-ray diffraction (XRD) include: Place the sample in an X-ray diffractometer; Adjust the X-ray source, sample position and detector to collect the diffraction pattern.

4. A rapid detection method for two-dimensional nanomaterials according to claim 3, characterized in that: In step S2, the operation steps of the transmission electron microscope (TEM) include: The sample is dispersed in an appropriate solvent and dropped onto a TEM grid for high-resolution imaging.

5. A rapid detection method for two-dimensional nanomaterials according to claim 4, characterized in that: In step S3, the electrochemical workstation performs cyclic voltammetry monitoring, including using the material to be tested as a working electrode, forming a three-electrode system with a reference electrode and an auxiliary electrode, immersing the electrode in a solution, and starting the experiment after setting CV parameters.

6. A rapid detection method for two-dimensional nanomaterials according to claim 5, characterized in that: In step S3, the step of monitoring the solution change using a pH meter and an ion chromatograph includes measuring the initial pH value of the solution, stirring after adding the material to be tested, and measuring the pH value and ion concentration at regular intervals.

7. A rapid detection method for two-dimensional nanomaterials according to claim 6, characterized in that: In step S3, the conductivity test is performed, and the operating steps include preparing the material to be tested into a thin film or coating and placing it between measuring electrodes; setting measurement conditions, such as temperature and humidity, and then starting the experiment; recording conductivity data and analyzing the conductivity changes of the material under different conditions; and evaluating the performance of the material as a two-dimensional electrolyte based on the conductivity data.

8. A rapid detection method for two-dimensional nanomaterials according to claim 7, characterized in that: In step S4, the step of setting the trigger condition includes analyzing the material properties, determining the sensitive range of the material, selecting suitable experimental equipment and connecting equipment, setting the experimental program, and setting the experimental program on the equipment according to the experimental design.

9. A rapid detection method for two-dimensional nanomaterials according to claim 8, characterized in that: In step S4, the step of observing morphological changes includes selecting a suitable microscope technology, taking an initial morphological image of the material, observing and recording the morphological changes of the material in real time during the triggering process, taking the morphological image again after the triggering condition ends, and monitoring the changes in electrochemical signals, which includes preparing an electrochemical workstation; setting electrochemical measurement parameters; and monitoring electrochemical signals.

10. A rapid detection method for two-dimensional nanomaterials according to claim 9, characterized in that: In step S5, the comprehensive evaluation and data analysis step includes integrating all the test data into a database, processing the test data using a machine learning algorithm, predicting the performance of the material and optimizing its design, evaluating the performance of the material based on the test results, and optimizing the material preparation process and triggering conditions based on the evaluation results.

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