Microstructure influence experiment method for AB double-layer graphene irradiated by fast neutrons with different energies

Abstract

The invention discloses a microstructure influence experiment method for AB double-layer graphene irradiated by fast neutrons with different energies, and particularly relates to the field of material science and nuclear engineering, the experiment steps are as follows: step 1, determining a research target; 2, selecting parameters and setting a control group; 3, selecting and treating a sample; step 4, irradiation control; 5, observing microstructure characterization after irradiation; step 6, data statistics and analysis; and step 7, summarizing. The experimental method disclosed by the invention is simple to operate, according to the experimental method, the fast neutron irradiation has obvious influence on the microstructure of the AB double-layer graphene, the increase of the interlayer distance and the increase of the defect density can be seen, and the change is related to the energy and dosage of the irradiation, which indicates that the modification of the microstructure of the graphene by the irradiation condition has controllability.

Description

Technical Field

[0001] The invention relates to the fields of material science and nuclear engineering, and more specifically to an experimental method for microstructure influence of AB double-layer graphene irradiated by fast neutrons of different energies. Background Art

[0002] In the field of materials science and nuclear engineering, the effect of fast neutron irradiation on material properties has always been a hot topic of research, especially in the study of new two-dimensional materials such as graphene. Fast neutron irradiation can not only reveal the behavioral characteristics of materials under extreme conditions, but also provide important basis for material modification, radiation damage assessment and nuclear energy application.

[0003] Double-layer graphene, as an important structure in the graphene family, has attracted much attention due to its unique electronic, optical and mechanical properties. However, in a nuclear radiation environment, the microstructure and properties of double-layer graphene may change significantly, and these changes have an important impact on its application prospects. Therefore, studying the effect of fast neutron irradiation with different energies on the microstructure of double-layer graphene is of great significance for a deep understanding of its irradiation effect and the development of new nuclear radiation protection materials.

[0004] At present, the research on the effect of fast neutron irradiation on the microstructure of double-layer graphene is still in its infancy. Although some studies have reported the effect of neutron irradiation on single-layer graphene, the behavioral characteristics of double-layer graphene under neutron irradiation may be significantly different from those of single-layer graphene. In addition, most of the existing research focuses on the field of low-energy neutron irradiation, while there are relatively few studies on high-energy fast neutron irradiation. Summary of the invention

[0005] In order to overcome the above-mentioned defects of the prior art, the present invention provides an experimental method for the microstructural influence of AB double-layer graphene irradiated by fast neutrons of different energies.

[0006] To achieve the above object, the present invention provides the following technical solution: an experimental method for the microstructural influence of AB double-layer graphene irradiated by fast neutrons of different energies, the experimental steps are as follows: Step 1: Determine the research objectives and explore the specific effects of fast neutron irradiation with different energies on the microstructure of AB bilayer graphene, including changes in interlayer distance, defect formation, and Raman spectrum changes; Step 2: Select parameters and set up a control group, determine the energy range and irradiation dose of fast neutrons and AB bilayer graphene, that is, the number of neutrons per square centimeter or total energy, ensure that the irradiation conditions are representative and repeatable, and set up a control group; Step 3: Sample selection and processing: selecting high-quality, structurally complete, and defect-free AB double-layer graphene samples, ensuring that their initial state meets the experimental requirements, and then processing the selected AB double-layer graphene samples; Step 4: Irradiation control: Use an accelerator to generate a fast neutron beam of the required energy, accurately control the energy and dose of the fast neutrons, ensure the consistency and repeatability of the irradiation conditions, place the prepared samples in the irradiation room, ensure that the samples are evenly exposed to the neutron beam, and conduct irradiation experiments according to the preset irradiation dose and time; Step 5: Observe the microstructure characterization after irradiation. Use a high-resolution transmission electron microscope (TEM) to observe the microstructure changes of the sample after irradiation, such as changes in interlayer distance and defect morphology. Use a Raman spectrometer to analyze the chemical bond changes and electronic structure changes caused by irradiation. Use an atomic force microscope (AFM) to measure the surface morphology and roughness changes of the sample. Step 6: Data statistics and analysis: Count and analyze the number, type, distribution and other characteristics of defects in the samples after irradiation. Use variance analysis and regression analysis statistical methods to compare the similarities and differences in the microstructure changes of samples under fast neutron irradiation with different energies, and explore the correlation mechanism between irradiation energy and microstructure changes; Step 7: Summarize the data statistics and analysis content.

[0007] As a further improvement of the technical solution of the present invention, when determining the energy range of fast neutrons in step 2, multiple energy points are selected according to research needs, such as 1MeV, 5MeV and 10MeV, and the area of ​​AB double-layer graphene is 8.385×10 -15 cm 2 .

[0008] As a further improvement of the technical solution of the present invention, in the step 2, the control group selects an unirradiated AB double-layer graphene sample as the control group so as to be directly compared with the irradiated sample.

[0009] As a further improvement of the technical solution of the present invention, the processing of the AB double-layer graphene sample in step three includes cleaning to remove surface impurities to ensure that no other influencing factors are introduced during the irradiation process, and marking or fixing the sample as needed so that it can be accurately identified and analyzed after irradiation.

[0010] As a further improvement of the technical solution of the present invention, when performing irradiation control in step 4, environmental parameters such as temperature, humidity, and pressure during the irradiation process are recorded so that the influence of these factors can be considered in subsequent analysis.

[0011] As a further improvement of the technical solution of the present invention, the specific steps of irradiation control in step 4 are as follows: S1. Operate the accelerator: select the appropriate accelerator type (including linear accelerator or cyclotron accelerator), adjust the accelerator parameters (including voltage, current, magnetic field strength) to produce a fast neutron beam with the required energy, and use a neutron energy measurement device (neutron spectrometer) to monitor the energy distribution of the neutron beam in real time; S2. Dose control: Calculate the required neutron flux and irradiation time according to the preset irradiation dose and time, use a neutron dosimeter or neutron detector to monitor the irradiation dose in real time to ensure the consistency and repeatability of the dose, and use a rotating sample stage or a moving neutron beam to ensure that the sample is evenly exposed to the neutron beam; S3. Irradiation chamber design: Select an irradiation chamber with good sealing and radiation shielding capabilities. The irradiation chamber is equipped with a sample stage and a neutron beam guide device to accurately control the relative position of the sample and the neutron beam.

[0012] As a further improvement of the technical solution of the present invention, in step six, image processing software is used to identify and count defects in the TEM image, and the defect density calculation formula is: ρ=VN, where ρ is the defect density, N is the number of defects, and V is the volume of the observation area; the irradiation dose calculation formula is: D=AN×E, where D is the irradiation dose (unit: MeV / cm² or number of neutrons / cm²), N is the number of neutrons, E is the neutron energy (unit: MeV), and A is the sample area (unit: cm²).

[0013] Beneficial effects of the present invention: The experimental method for the influence of fast neutron irradiation of AB double-layer graphene on the microstructure of different energies is simple to operate. According to the experimental method, it can be seen that with the increase of irradiation energy, the change amount of interlayer distance also shows an increasing trend; with the increase of irradiation dose, the change amount of interlayer distance also increases; the defect density increases with the increase of irradiation energy and dose, high energy and high dose irradiation leads to the highest defect density, even at lower energy and dose, the formation of defects can be observed, but the density is relatively low; with the increase of irradiation energy and dose, the degree of defects intensifies, and there are few defects in the non-irradiated samples of the set control group; that is, it can be concluded that fast neutron irradiation has a significant effect on the microstructure of AB double-layer graphene, including the increase of interlayer distance and the increase of defect density, and these changes are related to the energy and dose of irradiation, indicating that the irradiation conditions are controllable for the microstructure modification of graphene. BRIEF DESCRIPTION OF THE DRAWINGS

[0014] Figure 1 The present invention is a flow chart of the experimental method. DETAILED DESCRIPTION

[0015] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0016] As attached Figure 1 The experimental method for the microstructural effects of AB bilayer graphene irradiated by fast neutrons of different energies is shown in the figure. The experimental steps are as follows: Step 1: Determine the research objectives and explore the specific effects of fast neutron irradiation with different energies on the microstructure of AB bilayer graphene, including changes in interlayer distance, defect formation, and Raman spectrum changes; Step 2: Select parameters and set up a control group, determine the energy range and irradiation dose of fast neutrons and AB bilayer graphene, that is, the number of neutrons per square centimeter or total energy, ensure that the irradiation conditions are representative and repeatable, and set up a control group; Step 3: Sample selection and processing: selecting high-quality, structurally complete, and defect-free AB double-layer graphene samples, ensuring that their initial state meets the experimental requirements, and then processing the selected AB double-layer graphene samples; Step 4: Irradiation control: Use an accelerator to generate a fast neutron beam of the required energy, accurately control the energy and dose of the fast neutrons, ensure the consistency and repeatability of the irradiation conditions, place the prepared samples in the irradiation room, ensure that the samples are evenly exposed to the neutron beam, and conduct irradiation experiments according to the preset irradiation dose and time; Step 5: Observe the microstructure characterization after irradiation. Use a high-resolution transmission electron microscope (TEM) to observe the microstructure changes of the sample after irradiation, such as changes in interlayer distance and defect morphology. Use a Raman spectrometer to analyze the chemical bond changes and electronic structure changes caused by irradiation. Use an atomic force microscope (AFM) to measure the surface morphology and roughness changes of the sample. Step 6: Data statistics and analysis: Count and analyze the number, type, distribution and other characteristics of defects in the samples after irradiation. Use variance analysis and regression analysis statistical methods to compare the similarities and differences in the microstructure changes of samples under fast neutron irradiation with different energies, and explore the correlation mechanism between irradiation energy and microstructure changes; Step 7: Summarize the data statistics and analysis content.

[0017] Preferably, when determining the energy range of fast neutrons in step 2, multiple energy points are selected according to research needs, such as 1MeV, 5MeV and 10MeV, and the area of ​​AB double-layer graphene is 8.385×10 -15 cm 2 .

[0018] Preferably, in step 2, the control group selects an unirradiated AB double-layer graphene sample as the control group so as to be directly compared with the irradiated sample.

[0019] Preferably, the processing of the AB double-layer graphene sample in step three includes cleaning to remove surface impurities to ensure that no other influencing factors are introduced during the irradiation process, and marking or fixing the sample as needed so that it can be accurately identified and analyzed after irradiation.

[0020] Preferably, during the irradiation control in the fourth step, environmental parameters such as temperature, humidity, and pressure during the irradiation process are recorded so that the influence of these factors can be considered in subsequent analysis.

[0021] Preferably, the specific steps of irradiation control in step 4 are as follows: S1. Operate the accelerator: select the appropriate accelerator type (including linear accelerator or cyclotron accelerator), adjust the accelerator parameters (including voltage, current, magnetic field strength) to produce a fast neutron beam with the required energy, and use a neutron energy measurement device (neutron spectrometer) to monitor the energy distribution of the neutron beam in real time; S2. Dose control: Calculate the required neutron flux and irradiation time according to the preset irradiation dose and time, use a neutron dosimeter or neutron detector to monitor the irradiation dose in real time to ensure the consistency and repeatability of the dose, and use a rotating sample stage or a moving neutron beam to ensure that the sample is evenly exposed to the neutron beam; S3. Irradiation chamber design: Select an irradiation chamber with good sealing and radiation shielding capabilities. The irradiation chamber is equipped with a sample stage and a neutron beam guide device to accurately control the relative position of the sample and the neutron beam.

[0022] Preferably, in step six, image processing software is used to identify and count defects in the TEM image, and the defect density calculation formula is: ρ=VN, where ρ is the defect density, N is the number of defects, and V is the volume of the observation area; the irradiation dose calculation formula is: D=AN×E, where D is the irradiation dose (unit: MeV / cm² or number of neutrons / cm²), N is the number of neutrons, E is the neutron energy (unit: MeV), and A is the sample area (unit: cm²).

[0023] According to the above experimental method, the samples are numbered as S1, S2, S3, S4, S5, S6 and S7, and then the irradiation experiment is carried out to obtain the following table: Sample No. Irradiation energy (MeV) Radiation dose (×10-2) Irradiation time (min) Change of interlayer distance (A) Defect density (×10-2) Raman spectrum changes (I_D / I_G ratio) Remark S1 0 (Control) 0 0 0 0 0.05 Unirradiated samples S2 1 1 10 +0.02 0.5 0.10 Slight interlayer expansion, few defects S3 1 5 10 +0.05 2.0 0.15 The distance between layers increases significantly, and defects increase S4 5 1 10 +0.03 1.0 0.20 At medium energy, there are changes in layers and defects S5 5 5 10 +0.10 4.0 0.30 Significant changes at high doses S6 10 1 10 +0.04 1.5 0.25 Under high energy, the interlayer and defect changes are obvious S7 10 5 10 +0.15 6.0 0.40 Drastic changes at very high doses and energies In the above table: In this hypothetical table: Sample number: S1 was used as the control group and was not irradiated; Irradiation energy: Three energy points of 1MeV, 5MeV and 10MeV were selected; Radiation dose: For each energy point, 1×10 -2 and 5×10 -2 Two doses.

[0024] Irradiation time: The irradiation time for all samples was 10 minutes; Interlayer distance change: in Å (angstroms), the increase in interlayer distance after irradiation is statistically analyzed; Defect density: ×10 -2 The unit is , and the number of defects in the sample after irradiation is counted; Raman spectrum changes: expressed as the ratio of I_D / I_G (the intensity ratio of the D peak to the G peak), the changes in the Raman spectrum after irradiation are statistically analyzed to evaluate the degree of defects in graphene; Notes: The characteristics of the microstructural changes after irradiation of each sample are described; According to the above table, it can be seen that with the increase of irradiation energy, the change of interlayer distance also shows an increasing trend. For example, at the same dose, the samples irradiated with 10 MeV (S6 and S7) show a greater increase in interlayer distance than the samples irradiated with 1 MeV and 5 MeV (S2 ​​to S5); at the same energy, with the increase of irradiation dose, the change of interlayer distance also increases. For example, at 5 MeV energy, 5×10 -2 Dose (S5) ratio 1×10 -2 dose (S4) leads to a greater increase in the interlayer distance; the defect density increases with the increase of irradiation energy and dose. High energy and high dose irradiation (such as S7) leads to the highest defect density. Even at lower energy and dose (such as S2 and S4), the formation of defects can be observed, but the density is relatively low; the change in the I_D / I_G ratio in the Raman spectrum reflects the increase in the degree of defects in graphene. With the increase of irradiation energy and dose, the I_D / I_G ratio increases, indicating that the degree of defects is aggravated. The I_D / I_G ratio of the control group (S1) is the lowest, indicating that there are few defects in the unirradiated sample; that is, it can be concluded that fast neutron irradiation has a significant effect on the microstructure of AB bilayer graphene, including the increase of interlayer distance and the increase of defect density. These changes are related to the energy and dose of irradiation, indicating that the irradiation conditions are controllable for the microstructural modification of graphene.

[0025] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims

1. Experimental method for the microstructural effects of AB double-layer graphene irradiated by fast neutrons of different energies, characterized in that: The experimental steps are as follows: Step 1: Determine the research objectives and explore the specific effects of fast neutron irradiation with different energies on the microstructure of AB bilayer graphene, including changes in interlayer distance, defect formation, and Raman spectrum changes; Step 2: Select parameters and set a control group, determine the energy range and irradiation dose of fast neutrons and AB double-layer graphene, and set a control group; Step 3: Sample selection and processing: selecting high-quality, structurally complete, and defect-free AB double-layer graphene samples, and then processing the selected AB double-layer graphene samples; Step 4: Irradiation control: Use an accelerator to generate a fast neutron beam with the required energy, accurately control the energy and dose of the fast neutrons, place the prepared samples in the irradiation room, expose the samples evenly to the neutron beam, and perform irradiation experiments according to the preset irradiation dose and time; Step 5: Observe the microstructure characterization after irradiation. Use a high-resolution transmission electron microscope (TEM) to observe the microstructure changes of the sample after irradiation, including the change in interlayer distance and defect morphology. Use a Raman spectrometer to analyze the chemical bond changes and electronic structure changes caused by irradiation. Use an atomic force microscope (AFM) to measure the surface morphology and roughness changes of the sample. Step 6: Data statistics and analysis: Count and analyze the number, type, and distribution characteristics of defects in the samples after irradiation. Use variance analysis and regression analysis statistical methods to compare the similarities and differences in the microstructure changes of samples under fast neutron irradiation with different energies, and explore the correlation mechanism between irradiation energy and microstructure changes; Step 7: Summarize the data statistics and analysis content.

2. The experimental method for the microstructural influence of AB double-layer graphene irradiated by fast neutrons of different energies according to claim 1 is characterized by: When determining the energy range of fast neutrons in step 2, multiple energy points are selected according to research needs, such as 1MeV, 5MeV and 10MeV. The area of ​​AB double-layer graphene is 8.385×10 -15 cm 2 .

3. The experimental method for the microstructural influence of AB double-layer graphene irradiated by fast neutrons of different energies according to claim 1, characterized in that: In the step 2, the control group selects an unirradiated AB double-layer graphene sample as the control group for direct comparison with the irradiated sample.

4. The experimental method for the microstructural influence of AB double-layer graphene irradiated by fast neutrons of different energies according to claim 1, characterized in that: The treatment of the AB double-layer graphene sample in step three includes cleaning to remove surface impurities, and marking or fixing the sample as needed.

5. The experimental method for the microstructural influence of AB double-layer graphene irradiated by fast neutrons of different energies according to claim 1, characterized in that: When performing irradiation control in step 4, the temperature, humidity, and pressure environmental parameters during the irradiation process are recorded to consider the influence of these factors in subsequent analysis.

6. The experimental method for the microstructural influence of AB double-layer graphene irradiated by fast neutrons of different energies according to claim 1, characterized in that: The specific steps of irradiation control in step 4 are as follows: S1. Operate the accelerator: select the appropriate accelerator type (including linear accelerator or cyclotron accelerator), adjust the accelerator parameters (including voltage, current, magnetic field strength) to produce a fast neutron beam with the required energy, and use a neutron energy measurement device (neutron spectrometer) to monitor the energy distribution of the neutron beam in real time; S2. Dose control: Calculate the required neutron flux and irradiation time according to the preset irradiation dose and time, use a neutron dosimeter or neutron detector to monitor the irradiation dose in real time, and use a rotating sample stage or a moving neutron beam to expose the sample evenly to the neutron beam; S3. Irradiation chamber design: Select an irradiation chamber with good sealing and radiation shielding capabilities. The irradiation chamber is equipped with a sample stage and a neutron beam guide device to accurately control the relative position of the sample and the neutron beam.

7. The experimental method for the microstructural influence of AB double-layer graphene irradiated by fast neutrons of different energies according to claim 1, characterized in that: In step six, image processing software is used to identify and count defects in the TEM image. The defect density calculation formula is: ρ=VN, where ρ is the defect density, N is the number of defects, and V is the volume of the observation area; the irradiation dose calculation formula is: D=AN×E, where D is the irradiation dose (unit: MeV / cm² or number of neutrons / cm²), N is the number of neutrons, E is the neutron energy (unit: MeV), and A is the sample area (unit: cm²).

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