CN110346271A - A method of radiation resistance attacking material is screened using gradient-structure - Google Patents
A method of radiation resistance attacking material is screened using gradient-structure Download PDFInfo
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- CN110346271A CN110346271A CN201910662035.4A CN201910662035A CN110346271A CN 110346271 A CN110346271 A CN 110346271A CN 201910662035 A CN201910662035 A CN 201910662035A CN 110346271 A CN110346271 A CN 110346271A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- 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
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- 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
- G01N1/32—Polishing; Etching
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N17/00—Investigating resistance of materials to the weather, to corrosion, or to light
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N3/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N3/40—Investigating hardness or rebound hardness
- G01N3/42—Investigating hardness or rebound hardness by performing impressions under a steady load by indentors, e.g. sphere, pyramid
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- G—PHYSICS
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- G01Q—SCANNING-PROBE TECHNIQUES OR APPARATUS; APPLICATIONS OF SCANNING-PROBE TECHNIQUES, e.g. SCANNING PROBE MICROSCOPY [SPM]
- G01Q30/00—Auxiliary means serving to assist or improve the scanning probe techniques or apparatus, e.g. display or data processing devices
- G01Q30/20—Sample handling devices or methods
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- 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
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
- G01N2001/2873—Cutting or cleaving
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N2203/0001—Type of application of the stress
- G01N2203/0012—Constant speed test
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- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N2203/0014—Type of force applied
- G01N2203/0016—Tensile or compressive
- G01N2203/0019—Compressive
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N2203/0058—Kind of property studied
- G01N2203/0076—Hardness, compressibility or resistance to crushing
- G01N2203/0078—Hardness, compressibility or resistance to crushing using indentation
- G01N2203/0082—Indentation characteristics measured during load
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N2203/02—Details not specific for a particular testing method
- G01N2203/025—Geometry of the test
- G01N2203/0252—Monoaxial, i.e. the forces being applied along a single axis of the specimen
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N2203/02—Details not specific for a particular testing method
- G01N2203/06—Indicating or recording means; Sensing means
- G01N2203/067—Parameter measured for estimating the property
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Abstract
The invention belongs to material radioresistance injury reinforcing field, especially a kind of method using gradient-structure screening radiation resistance attacking material.Include the following steps: step (1): preparing Gradient Materials；Step (2): there is the surface of various grain sizes to carry out irradiation experiment Gradient Materials；Step (3): the automatic preparation of Mechanics Performance Testing and heterogeneous microstructure characterization sample is carried out using nano impress and convergence ion beam to the sample in various grain sizes region in the region of various grain sizes size to the material after irradiation.Step (4): transmission electron microscope and three-dimensional atom probe analysis are carried out.The present invention may be implemented to produce different crystallite dimensions on one piece of sample by this method, carry out irradiation experiment again later, required sample size is influenced so as to reduce the different grain sizes of research for irradiation damage, it is improved simultaneously in the efficiency for preparing sample for carrying out Microstructure characterization, improves the efficiency of screening radiation resistance attacking material.
Description
Technical field
The invention belongs to material radioresistance injury reinforcing fields, especially a kind of to screen radiation resistance attacking material using gradient-structure
Method.
Background technique
With energy demand and reduce CO2Emission problem becomes increasingly conspicuous, and Nuclear Power Development, which has become, solves mankind's energy
One of important way in short supply.Current nuclear power plant reactor method comparative maturity, but there are still much be difficult to solve
Method problem certainly.Wherein, the irradiation damage of pile materials is particularly problematic.The irradiation damage problem of nuclear material with react
The safety of heap and it is economical have close connection, be directly related to the reactor safety work of nuclear power.
The dominant mechanism of irradiation damage is mainly: a series of collision occurs for the lattice atoms of high energy particle and metal, from
And a large amount of point defect is generated in metal inside, point defect forms various faults of construction in agglomeration, prevents material
In dislocation motion improved so as to cause the ductile-brittle transition temperature of material, so that nuclear material so that material hardens phenomenon
It is transformed into fragile material under its service temperature after long-term irradiation, that is, causes the irradiation hardening and radiation embrittlement of material, seriously
Threaten the safe operation of nuclear power station.
Develop with nuclear power station, the research of irradiation damage mechamism is ongoing, and the research of nuclear material requires
Advanced research goes out next-generation nuclear power station material therefor.Radiation damage effect is studied, the base for being appreciated and understood by irradiation damage is facilitated
Present principles lay the foundation to develop next-generation nuclear material.Influence material for irradiation damage performance because being known as material
Heterogeneous microstructure, alloying component type, alloying element content, irradiation dose, irradiation time, the factors such as irradiation temperature.?
In microstructure, the toughness and material that crystallite dimension will affect material are to the sensibility of irradiation, so crystallite dimension is also to influence
One of important factor in order of irradiation damage needs to study it.
The influence of research irradiation damage is related to irradiating the mechanical property of layer and the characterization of microstructure.Under normal conditions,
Mechanical property can be characterized by nano impress or Vickers hardness, and transmission electron microscope, Three-dimensional atom can be used in microstructure
Probe is characterized.But the influence for various grain sizes to be studied for irradiation damage needs to prepare muti-piece difference respectively
The sample of crystallite dimension carries out irradiation experiment, can just be studied later.It is duplicate more for the characterization needs of microstructure
The sample for changing various grain sizes is sampled, then carries out the characterization of microstructure, expends the time, and conventional efficient is low.
Summary of the invention
Technical problem solved by the invention is to provide a kind of side using gradient-structure screening radiation resistance attacking material
Method.
The technical solution for realizing the aim of the invention is as follows:
A method of radiation resistance attacking material being screened using gradient-structure, is included the following steps:
Step (1): Gradient Materials are prepared；
Step (2): there is the surface of various grain sizes to carry out irradiation experiment Gradient Materials；
Step (3): to the material after irradiation, in the region of various grain sizes size, using nano impress and converge from
Beamlet carries out the automatic preparation of Mechanics Performance Testing and heterogeneous microstructure characterization sample to the sample in various grain sizes region.
Step (4): transmission electron microscope (TEM) and three-dimensional atom probe (APT) analysis are carried out.
Further, the method that Gradient Materials are prepared in the step (1) is shot-peening.
Further, the step (1) specifically comprises the following steps:
Step (1-1): raw material uses plaques, the revolution mark of plaques surface and surrounding is polished clean.
Step (1-2): the technological parameter of bead is determined；
Step (1-3): plaques are fitted into rotation shot blasting equipment, are carried out bead to bead face (4), are hung down
Nanometer crystalline region I, ultra-fine crystalline region II and coarse grain zone III directly are sequentially formed from bead face in the surface of bead face (4), is examined
Look into deformation layer thickness (nanometer crystalline region I, ultra-fine crystalline region II)；
Step (1-4): the sample in step (1-3) is taken out and is cut, cut surface is perpendicular to bead face (4).
Further, the step (1-2) specifically: first determine that hoodle diameter is 1mm, speed 70m/s.
Further, the step (1-3) specifically: after being disposed, check deformation layer (nanometer crystalline region I, ultra-fine crystalline region
II) thickness does not need adjustment bullet diameter and velocity of shot if reaching 300 μm, if less than needing to adjust bullet diameter
1.0mm, 1.5mm, 2.0mm, 5mm) and velocity of shot (30m/s~90m/s), until deformation layer thickness reaches 300 μm, completion ladder
Spend the preparation of sample.
Further, in the step (1-4), the length and width of the sample after cutting are less than 18mm*18mm, and thickness is no more than
2mm, when to guarantee to carry out irradiation experiment, sample is completely covered by the beam spot of ion beam.
Further, the step (3) specifically comprises the following steps:
Step (3-1): nano-indenter test；
Step (3-2): transmission electron microscope sample preparation；
Step (3-3): three-dimensional atom probe sample preparation；
Step (3-4): it is Zone switched, it repeats step (3-1) to (3-3).
Further, step (3-1) nano-indenter test specifically: after sample is put into instrument, selected under light microscopic
Satisfactory region is taken to do mark, every piece of sample takes 6 points, while guaranteeing that the linear distance of adjacent point-to-point transmission is greater than pressure
Enter 20 times of depth, after choosing a little, shut instrument, ram movement is tested to marked region, and in test process, pressure head is being marked
Note region moves 2000nm, speed of service 10nm/s into sample, after reaching 2000nm, will be slow unloading, and pressure head is slowly
Surface is received out again, and at regular intervals, system records the value of a depression depths and hardness, finally forms depth with firmness change
Curve.
Further, step (3-2) the transmission electron microscope sample preparation specifically: so that sample stage verts 54 °, it is emerging feeling
The region of interest plates protective Pt, then digs respectively to after enough depth, sample stage is tilted in 52 ° and 56 ° progress groovings
15 ° carry out interrupting behaviour and do, so that sample bottom is separated from block；Then will be stained on the left of sample with nanometer hand, later again from
Right side cutting, so that area-of-interest is completely separated from sample, then takes out and is transferred on Special sample table, then subtracted
Thin operation, direct thickness of sample reach 100nm hereinafter, completing transmission electron microscope sample preparation.
Further, step (3-3) the three-dimensional atom probe sample preparation specifically: so that sample stage verts 54 °,
Interested region plates protective Pt, then starts grooving, so that area-of-interest is separated in block sample, then with receiving
Rice hand is drawn off, and is placed on Special sample pedestal, carries out annular cutting, it is below in 100nm to finally obtain top end diameter
Needle-shaped specimen.
Further, in the step step (3-4) it is Zone switched pass through control system mobile example platform complete.
Further, transmission electron microscope (TEM) described in step (4) and three-dimensional atom probe (APT) analysis are carried out.
Compared with prior art, the present invention its remarkable advantage is as follows:
The microstructure of different grain sizes is obtained on same sample, carries out irradiation experiment again later, so as to
With reduce study different grain sizes irradiation damage influenced needed for sample size, while can be same using this method
The region of the various grain sizes of product carries out sample and prepares automatically, improves the effect in the sample preparation for carrying out Microstructure characterization
Rate, saves funds and the time of the cost of irradiation experiment, to improve the testing efficiency of evaluation material anti-radiation performance, more
Material that is good, more effectively filtering out radiation resistance damage.
Detailed description of the invention
Fig. 1 the application gradient-structure and cut direction schematic diagram.
Fig. 2 the application sample preparation position view.
Description of symbols:
I-nanometer crystalline region, II-ultra-fine crystalline region, III-coarse grain zone, 1- transmission electron microscope sample, 2- atom probe specimens, 3- nanometers
Impression test, 4- bead face.
Specific embodiment
The purpose of the present invention is to provide it is a kind of using gradient-structure screening radiation resistance attacking material experimental method, so as to
In reducing laboratory sample quantity, the efficiency of material microstructure characterization is improved, to improve the effect of screening radioresistance injury reinforcing material
Rate.
Realize the method scheme of the object of the invention, the following steps are included:
Step 1: the revolution mark of plaques surface and surrounding being polished clean.
Step 2: first determining that hoodle diameter is 1mm, speed 70m/s.
Step 3: sample clamping being entered in the equipment (rotation shot blasting equipment) of making Nano surface, the bullet that diameter is 1mm is added
Pearl, starting device, latency speed reach 70m/s, start to carry out bead to sample, until reaching processing time 10min
Stop processing and take out sample, after being disposed, check deformation layer (nanometer crystalline region I, ultra-fine crystalline region II) thickness, if reaching 300 μm
Adjusting parameter is not needed then, needs to adjust bullet diameter (1.0mm, 1.5mm, 2.0mm, 5mm) and velocity of shot if being less than
(30m/s~90m/s), until deformation layer thickness reaches 300 μm.
Step 4: sample being cut (as shown in dotted line in attached drawing 1) along the direction perpendicular to shot-peening face, is cut into ruler
Very little suitable size (sample of maximum 18mm*18mm size, thickness are no more than 2mm, when to guarantee to carry out irradiation experiment,
Sample can be completely covered by the beam spot of ion beam).
Step 5: the surface that will be perpendicular to peened surface is polished, until guaranteeing that surface does not have scratch and stress
Stop, being then transferred on irradiation experiment platform later and carry out irradiation experiment.
Step 6: after completing irradiation experiment, to the sample after irradiation in the region of various grain sizes size, utilizing nanometer
The equipment such as impression and convergence ion beam carry out Mechanics Performance Testing and heterogeneous microstructure to the sample in various grain sizes region
Characterize the automatic preparation (transmission electron microscope sample preparation and the preparation of three-dimensional atom probe sample) of sample.Between different zones
Switching is completed by control system mobile example platform, is repeated 6.1-6.3 step later and is completed test and sample preparation.
Step 6.1: the nanometer of model Nano Indenter G200 nano-indenter test process: is used in experimentation
Impression instrument is tested.After sample is put into instrument, first satisfactory region is chosen under light microscopic does upper mark, every piece of sample
6 points are taken, while guaranteeing that the linear distance of adjacent point-to-point transmission is greater than 20 times (40 μm) of compression distance.After choosing a little, shut
Instrument, pressure head can move to marked region and be tested.Test the pressure head model Berkovich tip pressing chosen, test
In the process, pressure head can move 2000nm, speed of service 10nm/s into sample in marked region, after reaching 2000nm, can delay
Slow unloading, pressure head can slowly receive out surface again, and at regular intervals, system will record the value of a depression depths and hardness,
Depth is finally formed with the curve of firmness change.After pressure head is received out, next point can be moved to, carries out the test of next point.
Step 6.2: transmission electron microscope sample preparation process: making sample stage vert 54 ° first, plates in interested region
Then protective Pt is dug to after enough depth, sample stage is tilted to 15 ° and is interrupted in 52 ° and 56 ° progress groovings respectively
Behaviour does, so that sample bottom is separated from block.Then it will be stained on the left of sample with nanometer hand, cut off, make from right side again later
It obtains sample to be completely separated from sample, then takes out and be transferred on Special sample table, then carry out thinning operation, direct sample is thick
Degree reaches 100nm once, completes transmission electron microscope sample preparation.
Step 6.3: three-dimensional atom probe sample preparation procedure: making sample stage vert 54 ° first, in interested region
Protective Pt is plated, grooving is then started, so that area-of-interest is separated in block sample, is then taken with nanometer hand
Out, it is placed on Special sample pedestal, carries out annular cutting, finally obtain the needle-shaped specimen of top end diameter once in 100nm.
Step 7: the transmission electron microscope sample and three-dimensional atom probe sample that have prepared are analyzed.
Claims (10)
1. a kind of method using gradient-structure screening radiation resistance attacking material, which comprises the steps of:
Step (1): Gradient Materials are prepared；
Step (2): there is the surface of various grain sizes to carry out irradiation experiment Gradient Materials；
Step (3): nano impress and convergence ion beam are utilized in the region of various grain sizes size to the material after irradiation
The automatic preparation of Mechanics Performance Testing and heterogeneous microstructure characterization sample is carried out to the sample in various grain sizes region；
Step (4): transmission electron microscope (TEM) and three-dimensional atom probe (APT) analysis are carried out.
2. the method according to claim 1, wherein the method for preparing Gradient Materials in the step (1)
For shot-peening.
3. according to the method described in claim 2, it is characterized in that, the step (1) specifically comprises the following steps:
Step (1-1): raw material uses plaques, the revolution mark of plaques surface and surrounding is polished clean.；
Step (1-2): the technological parameter of bead is determined；
Step (1-3): plaques are fitted into rotation shot blasting equipment, carry out bead to bead face (4), perpendicular to
The surface in bead face (4) sequentially forms nanometer crystalline region I, ultra-fine crystalline region II and coarse grain zone III from bead face；
Step (1-4): the sample in step (1-3) is taken out and is cut, cut surface is perpendicular to bead face (4).
4. according to the method described in claim 3, it is characterized in that, the step (1-3) specifically: first determine that hoodle diameter is
1mm, speed 70m/s after being disposed, check deformation layer (nanometer crystalline region I, ultra-fine crystalline region II) thickness, if 300 μm of arrival
Adjustment bullet diameter and velocity of shot are not needed, needs to adjust bullet diameter (1.0mm, 1.5mm, 2.0mm, 5mm) if being less than
The preparation of gradient sample is completed until deformation layer thickness reaches 300 μm with velocity of shot (30m/s~90m/s).
5. according to the method described in claim 3, it is characterized in that, in the step (1-4), the length and width of the sample after cutting
Less than 18mm*18mm, thickness is no more than 2mm, and when to guarantee to carry out irradiation experiment, sample is covered completely by the beam spot of ion beam
Lid.
6. according to the method described in claim 3, it is characterized in that, the step (3) specifically comprises the following steps:
Step (3-1): nano-indenter test；
Step (3-2): transmission electron microscope sample preparation；
Step (3-3): three-dimensional atom probe sample preparation；
Step (3-4): it is Zone switched, it repeats step (3-1) to (3-3).
7. according to the method described in claim 6, it is characterized in that, the step (3-1) nano-indenter test specifically: by sample
After product are put into instrument, satisfactory region is chosen under light microscopic and does upper mark, every piece of sample takes 6 points, while guaranteeing adjacent
The linear distance of point-to-point transmission be greater than 20 times of compression distance, after choosing a little, shut instrument, ram movement to marked region progress
It tests, in test process, pressure head moves 2000nm into sample in marked region, and speed of service 10nm/s reaches 2000nm
Afterwards, will be slow unloading, pressure head slowly receive out surface again, at regular intervals, system records a depression depths and hardness
Value finally forms depth with the curve of firmness change.
8. according to the method described in claim 6, it is characterized in that, prepared by the step (3-2) transmission electron microscope sample specifically:
So that sample stage verts 54 °, protective Pt is plated in interested region, is then dug respectively in 52 ° and 56 ° progress groovings
To after enough depth, sample stage, which is tilted to 15 °, to carry out interrupting behaviour and does, so that sample bottom is separated from block；Then nanometer is used
Hand will be stained on the left of sample, be cut off again from right side later, so that area-of-interest is completely separated from sample, is then taken out and is turned
It moves on on Special sample table, then carries out thinning operation, direct thickness of sample reaches 100nm hereinafter, the transmission electron microscope sample system of completion
It is standby.
9. according to the method described in claim 6, it is characterized in that, the step (3-3) three-dimensional atom probe sample preparation has
Body are as follows: so that sample stage verts 54 °, plate protective Pt in interested region, then start grooving, so that region of interest
Domain is separated in block sample, is then drawn off, is placed on Special sample pedestal with nanometer hand, carries out annular cutting, finally
Top end diameter is obtained in 100nm needle-shaped specimen below.
10. according to the method described in claim 6, it is characterized in that, Zone switched in the step step (3-4) passes through control
System mobile example platform processed is completed.
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Cited By (3)
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| CN112432968A (en) * | 2020-10-21 | 2021-03-02 | 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 |
| CN116046825A (en) * | 2023-04-03 | 2023-05-02 | 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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| CN112432968A (en) * | 2020-10-21 | 2021-03-02 | 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 |
| CN116046825A (en) * | 2023-04-03 | 2023-05-02 | 中国核动力研究设计院 | Nanometer indentation sample of irradiated dispersion fuel and preparation method thereof |
| 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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