CN110346271B - Method for screening radiation damage resistant material by using gradient structure - Google Patents
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- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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- G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
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Abstract
The invention belongs to the field of irradiation damage resistance of materials, and particularly relates to a method for screening irradiation damage resistant materials by using a gradient structure. The method comprises the following steps: step (1): preparing a gradient structure material; step (2): carrying out an irradiation experiment on the surfaces of the gradient structure materials with different grain sizes; and (3): and for the irradiated material, in areas with different grain sizes, performing mechanical property test and automatic preparation of microstructure characterization samples on the samples in the areas with different grain sizes by using nano indentations and converged ion beams. And (4): and (5) carrying out transmission electron microscope and three-dimensional atom probe analysis. The method can realize that different crystal grain sizes are manufactured on one sample, and then the irradiation experiment is carried out, thereby reducing the number of samples required for researching the influence of different crystal grain sizes on irradiation damage, simultaneously improving the sample preparation efficiency of microstructure characterization, and improving the efficiency of screening the irradiation damage resistant material.
Description
Technical Field
The invention belongs to the field of irradiation damage resistance of materials, and particularly relates to a method for screening irradiation damage resistant materials by using a gradient structure.
Background
With energy demand and reduction of CO2The emission problem is increasingly prominent, and the development of nuclear power becomes one of important ways for solving the shortage of human energy. The current nuclear power plant reactor method is mature, but stillThere are a number of difficult process problems that remain. Among them, the problem of radiation damage of reactor materials is particularly prominent. The problem of irradiation damage of nuclear materials is closely related to the safety and economy of a reactor, and is directly related to whether a nuclear reactor can safely operate.
The main mechanisms of radiation damage are mainly: a series of collisions occur between the high-energy particles and lattice atoms of the metal, so that a large number of point defects are generated in the metal, the point defects grow in an aggregation mode to form various structural defects, dislocation movement in the material is prevented, the material is hardened, the ductile-brittle transition temperature of the material is increased, the nuclear power material is converted into a brittle material at the service temperature after long-term irradiation, irradiation hardening and irradiation embrittlement of the material are caused, and the safe operation of a nuclear power station is seriously threatened.
With the development of nuclear power plants, the research on the mechanism of radiation damage is continuously carried out, and the research on nuclear power materials requires advanced research on materials used in next-generation nuclear power plants. The research on the radiation damage effect is helpful for understanding and understanding the basic principle of radiation damage, and lays a foundation for developing the next generation nuclear power material. Factors influencing the performance of the material on the irradiation damage include the microstructure of the material, the types of alloy components, the content of alloy elements, the irradiation dose, the irradiation time, the irradiation temperature and other factors. In the microstructure, the grain size affects the toughness of the material and the sensitivity of the material to radiation, so the grain size is also one of the important factors affecting radiation damage, and needs to be studied.
The research on the influence of the irradiation damage relates to the mechanical property of the irradiation layer and the characterization of the microstructure. In general, mechanical properties can be characterized by nanoindentation or vickers hardness, and microstructures can be characterized by using a transmission electron microscope and a three-dimensional atom probe. However, to study the influence of different grain sizes on irradiation damage, a plurality of samples with different grain sizes need to be prepared respectively, and irradiation experiments are carried out before study. For the representation of the microstructure, samples with different grain sizes need to be repeatedly replaced for sampling, and then the representation of the microstructure is carried out, so that the time is consumed, and the experimental efficiency is low.
Disclosure of Invention
The invention aims to provide a method for screening radiation damage resistant materials by utilizing a gradient structure.
The technical solution for realizing the purpose of the invention is as follows:
a method for screening radiation damage resistant materials by using a gradient structure comprises the following steps:
step (1): preparing a gradient structure material;
step (2): carrying out an irradiation experiment on the surfaces of the gradient structure materials with different grain sizes;
and (3): and for the irradiated material, in areas with different grain sizes, performing mechanical property test and automatic preparation of microstructure characterization samples on the samples in the areas with different grain sizes by using nano indentations and converged ion beams.
And (4): transmission Electron Microscopy (TEM) and three-dimensional Atom Probe (APT) analysis were performed.
Further, the method for preparing the gradient structure material in the step (1) is shot blasting.
Further, the step (1) specifically comprises the following steps:
step (1-1): the raw material adopts a plate-shaped sample, and the cutting traces on the surface and the periphery of the plate-shaped sample are polished completely.
Step (1-2): determining the technological parameters of shot blasting;
step (1-3): loading a plate-shaped sample into rotary shot blasting equipment, carrying out shot blasting on a shot blasting surface (4), forming a nanocrystalline region I, an ultrafine grain region II and a coarse grain region III in sequence from the shot blasting surface perpendicular to the surface of the shot blasting surface (4), and inspecting the thickness of a deformation layer (the nanocrystalline region I and the ultrafine grain region II);
step (1-4): and (4) taking out and cutting the sample in the step (1-3), wherein the cutting surface is vertical to the shot blasting surface (4).
Further, the step (1-2) is specifically: the diameter of the marble was determined to be 1mm and the speed was 70 m/s.
Further, the step (1-3) is specifically: and after the treatment is finished, the thickness of the deformation layer (the nanocrystalline area I and the ultrafine grain area II) is checked, if the thickness reaches 300 mu m, the diameter and the speed of the shot are not required to be adjusted, and if the thickness is less than 300 mu m, the diameter of the shot is required to be adjusted to be 1.0mm,1.5mm,2.0mm and 5mm) and the speed of the shot is required to be adjusted to be 30-90 m/s until the thickness of the deformation layer reaches 300 mu m, and the preparation of the gradient sample is finished.
Further, in the steps (1-4), the length and width of the cut sample are less than 18mm by 18mm, and the thickness is not more than 2mm, so that the sample is completely covered by the beam spot of the ion beam when the irradiation experiment is carried out.
Further, the step (3) specifically includes the following steps:
step (3-1): carrying out nano indentation test;
step (3-2): preparing a transmission electron microscope sample;
step (3-3): preparing a three-dimensional atom probe sample;
step (3-4): and (4) switching the region, and repeating the steps (3-1) to (3-3).
Further, the nano indentation test in the step (3-1) is specifically as follows: after a sample is placed in an instrument, an area meeting the requirement is selected under an optical lens to be marked, 6 points are taken for each sample, meanwhile, the linear distance between two adjacent points is guaranteed to be larger than 20 times of the pressing depth, after the points are selected, the instrument is closed, a pressure head moves to a marking area to be tested, in the testing process, the pressure head moves 2000nm towards the inside of the sample in the marking area, the running speed is 10nm/s, the pressure head is slowly unloaded after the running speed reaches 2000nm, the surface is slowly withdrawn, the system records the values of the pressing depth and the hardness once every other period of time, and finally a curve of the depth changing along with the hardness is formed.
Further, the preparation of the transmission electron microscope sample in the step (3-2) specifically comprises the following steps: the sample platform is tilted by 54 degrees, protective Pt is coated on the interested area, then grooves are dug at 52 degrees and 56 degrees respectively, after the grooves are dug to enough depth, the sample platform is tilted to 15 degrees to interrupt the operation, so that the bottom of the sample is separated from the block body; and then, adhering the left side of the sample by using a nanometer hand, then cutting off the sample from the right side to completely separate the region of interest from the sample, then taking out the sample and transferring the sample to a special sample table, and then performing thinning operation to directly reduce the thickness of the sample to be less than 100nm, thereby completing the preparation of the transmission electron microscope sample.
Further, the three-dimensional atom probe sample preparation in the step (3-3) is specifically as follows: and (3) tilting the sample platform by 54 degrees, plating protective Pt on the interested area, then beginning to dig a groove to separate the interested area from the block sample, taking out the interested area by using a nanometer hand, placing the interested area on a special sample base, and performing annular cutting to obtain a needle-shaped sample with the diameter of the top end below 100 nm.
Further, the switching area in the step (3-4) is completed by the control system moving the sample stage.
Further, Transmission Electron Microscopy (TEM) and three-dimensional Atom Probe (APT) analysis described in step (4) were performed.
Compared with the prior art, the invention has the following remarkable advantages:
the method has the advantages that the microstructures with different grain sizes are obtained on the same sample, and then the irradiation experiment is carried out, so that the number of samples required for researching the influence of different grain sizes on the irradiation damage can be reduced.
Drawings
FIG. 1 is a schematic view of the gradient structure and cutting direction of the present application.
FIG. 2 is a schematic illustration of a sample preparation site of the present application.
Description of reference numerals:
i-nanocrystalline region, II-ultrafine crystalline region, III-coarse crystalline region, 1-transmission electron microscope sample, 2-atom probe sample, 3-nano indentation test and 4-shot blasting surface.
Detailed Description
The invention aims to provide an experimental method for screening an irradiation damage resistant material by using a gradient structure, so that the number of experimental samples is reduced, the microstructure characterization efficiency of the material is improved, and the irradiation damage resistant material screening efficiency is improved.
The method scheme for realizing the aim of the invention comprises the following steps:
step 1: and (4) polishing the cutting traces on the surface and around the plate-shaped sample.
Step 2: the diameter of the marble was determined to be 1mm and the speed was 70 m/s. .
And step 3: clamping a sample into a device (rotary shot blasting device) with a nano-surface, adding a marble with the diameter of 1mm, starting the device, waiting for the speed to reach 70m/s, starting shot blasting on the sample, stopping processing until the processing time reaches 10min, taking out the sample, checking the thickness of a deformation layer (a nanocrystalline area I and an ultrafine grain area II) after processing, wherein if the thickness reaches 300 mu m, the parameter does not need to be adjusted, and if the thickness is less than 300 mu m, the diameter (1.0mm,1.5mm,2.0mm and 5mm) and the speed (30 m/s-90 m/s) of the marble are required to be adjusted until the thickness of the deformation layer reaches 300 mu m. .
And 4, step 4: the sample is cut in a direction perpendicular to the shot blasting surface (as shown by a dotted line in fig. 1), and cut into a proper size (the sample with the size of 18mm at the maximum and the thickness of not more than 2mm so as to ensure that the sample can be completely covered by the beam spot of the ion beam when the irradiation experiment is carried out).
And 5: and polishing the surface vertical to the shot blasting surface until the surface is free of scratches and stress, and then transferring the surface to an irradiation experiment platform for irradiation experiment.
Step 6: after the irradiation experiment is finished, mechanical property testing and automatic preparation of microstructure characterization samples (transmission electron microscope sample preparation and three-dimensional atom probe sample preparation) are carried out on the samples in the areas with different grain sizes after the irradiation by utilizing equipment such as nano indentation and converged ion beams. The switching among different areas is completed by the control system moving the sample stage, and then the steps of 6.1-6.3 are repeated to complete the test and the sample preparation.
Step 6.1: and (3) nano indentation testing process: the test was carried out using a nanoindenter model Nano index G200 during the experiment. After the samples are put into the instrument, areas meeting the requirements are selected under a light mirror to be marked, 6 points are taken for each sample, and meanwhile, the linear distance between two adjacent points is ensured to be more than 20 times (40 mu m) of the pressing depth. After the point is selected, the instrument is closed and the indenter moves to the marking area for testing. The model of the pressure head selected in the experiment is a Berkovich tip pressure pin, in the testing process, the pressure head can move 2000nm towards the inside of a sample in a marking area, the running speed is 10nm/s, the pressure head can be slowly unloaded after reaching 2000nm, the pressure head can be slowly withdrawn from the surface, the system can record the values of the pressing depth and the hardness once every other period of time, and finally a curve of the depth changing along with the hardness is formed. After the pressure head is withdrawn, the pressure head moves to the next point to perform the test of the next point.
Step 6.2: the preparation process of the transmission electron microscope sample comprises the following steps: the sample stage is first tilted 54 ° to plate the area of interest with protective Pt, then trenched at 52 ° and 56 °, respectively, and after digging to a sufficient depth, the stage is tilted 15 ° to interrupt the operation, causing the sample bottom to separate from the block. And then, adhering the left side of the sample by using a nanometer hand, then cutting off the sample from the right side to ensure that the sample is thoroughly separated from the sample, then taking out the sample and transferring the sample to a special sample table, and then carrying out thinning operation until the thickness of the sample reaches 100nm, thereby completing the preparation of the transmission electron microscope sample.
Step 6.3: the preparation process of the three-dimensional atom probe sample comprises the following steps: firstly, the sample platform is tilted by 54 degrees, protective Pt is plated on the interested area, then the groove digging is started to separate the interested area from the block sample, then the interested area is taken out by a nanometer hand and placed on a special sample base to carry out annular cutting, and finally the needle-shaped sample with the diameter of the top end of 100nm is obtained.
And 7: and analyzing the prepared transmission electron microscope sample and the prepared three-dimensional atom probe sample.
Claims (8)
1. A method for screening radiation damage resistant materials by utilizing a gradient structure is characterized by comprising the following steps:
step (1): preparing a gradient structure material;
step (2): carrying out an irradiation experiment on the surfaces of the gradient structure materials with different grain sizes;
and (3): for the irradiated material, in areas with different grain sizes, carrying out mechanical property test and automatic preparation of microstructure characterization samples on the samples in the areas with different grain sizes by utilizing nano-indentation and converged ion beams;
the step (3) specifically comprises the following steps:
step (3-1): carrying out nano indentation test; the nano indentation test in the step (3-1) is specifically as follows: after a sample is placed in an instrument, an area meeting the requirement is selected under an optical lens to be marked, 6 points are taken for each sample, the linear distance between two adjacent points is guaranteed to be larger than 20 times of the pressing depth, after the points are selected, the instrument is closed, a pressure head moves to a marking area to be tested, in the testing process, the pressure head moves 2000nm towards the inside of the sample in the marking area, the running speed is 10nm/s, the pressure head is slowly unloaded after reaching 2000nm, the surface is slowly withdrawn, the system records the values of the pressing depth and the hardness once every other period of time, and finally a curve of which the depth changes along with the hardness is formed;
step (3-2): preparing a transmission electron microscope sample;
step (3-3): preparing a three-dimensional atom probe sample;
step (3-4): switching the region, repeating the steps (3-1) to (3-3)
And (4): and (5) carrying out transmission electron microscope and three-dimensional atom probe analysis.
2. The method according to claim 1, wherein the method for preparing the gradient structure material in the step (1) is shot blasting.
3. The method according to claim 2, characterized in that said step (1) comprises in particular the steps of:
step (1-1): the raw material adopts a plate-shaped sample, and the cutting traces on the surface and the periphery of the plate-shaped sample are polished clean;
step (1-2): determining the technological parameters of shot blasting;
step (1-3): loading the plate-shaped sample into a rotary shot blasting device, carrying out shot blasting on the shot blasting surface (4), and forming a nanocrystalline region I, an ultrafine grain region II and a coarse grain region III in sequence from the shot blasting surface perpendicular to the surface of the shot blasting surface (4);
step (1-4): and (4) taking out and cutting the sample in the step (1-3), wherein the cutting surface is vertical to the shot blasting surface (4).
4. The method according to claim 3, wherein the steps (1-3) are in particular: firstly, determining the diameter of the marble to be 1mm and the speed to be 70m/s, after the treatment is finished, checking the thickness of a deformation layer, namely the nanocrystalline region I and the superfine crystalline region II, if the thickness reaches 300 mu m, the diameter and the speed of the marble do not need to be adjusted, if the thickness is less than 300 mu m, the diameter and the speed of the marble need to be adjusted until the thickness of the deformation layer reaches 300 mu m, and finishing the preparation of the gradient sample.
5. The method according to claim 3, wherein in the step (1-4), the cut sample has a length and width of less than 18mm x 18mm and a thickness of no more than 2mm, so as to ensure that the sample is completely covered by the beam spot of the ion beam when the irradiation experiment is performed.
6. The method according to claim 1, wherein the step (3-2) of preparing the transmission electron microscope sample comprises: the sample platform is tilted by 54 degrees, protective Pt is plated on the interested area, then grooves are dug at 52 degrees and 56 degrees respectively, after the grooves are dug to the required depth, the sample platform is tilted to 15 degrees to interrupt the operation, so that the bottom of the sample is separated from the block body; and then, adhering the left side of the sample by using a nanometer hand, then cutting off the sample from the right side to completely separate the region of interest from the sample, then taking out the sample and transferring the sample to a sample table, and then performing thinning operation to directly enable the thickness of the sample to reach below 100nm, thereby completing the preparation of the transmission electron microscope sample.
7. The method according to claim 1, wherein the step (3-3) of preparing the three-dimensional atom probe sample is specifically: and (3) tilting the sample platform by 54 degrees, plating protective Pt on the region of interest, then beginning to dig a groove to separate the region of interest from the block sample, taking out the block sample by using a nanometer hand, placing the block sample on a sample base, and performing annular cutting to obtain a needle-shaped sample with the diameter of the top end below 100 nm.
8. The method of claim 1, wherein the switching region of step (3-4) is accomplished by moving the sample stage via a control system.
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| CN112432968B (en) * | 2020-10-21 | 2022-08-30 | 中国核动力研究设计院 | Preparation method of irradiated reactor structure material thermal conductivity test sample and test sample box |
| CN112858150A (en) * | 2021-01-11 | 2021-05-28 | 南京理工大学 | Method for screening nuclear power reactor pressure vessel alloy irradiation-resistant material |
| CN116046825B (en) * | 2023-04-03 | 2023-06-27 | 中国核动力研究设计院 | Nanometer indentation sample of irradiated dispersion fuel and preparation method thereof |
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| US6568239B1 (en) * | 2001-07-03 | 2003-05-27 | Jack Champaigne | Test strip and method for confirming shot peening coverage |
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