CN116046825A - Nanometer indentation sample of irradiated dispersion fuel and preparation method thereof - Google Patents
Nanometer indentation sample of irradiated dispersion fuel and preparation method thereof Download PDFInfo
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- CN116046825A CN116046825A CN202310343903.9A CN202310343903A CN116046825A CN 116046825 A CN116046825 A CN 116046825A CN 202310343903 A CN202310343903 A CN 202310343903A CN 116046825 A CN116046825 A CN 116046825A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
- G01N23/2202—Preparing specimens therefor
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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
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
- G01N23/225—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material using electron or ion
- G01N23/2251—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material using electron or ion using incident electron beams, e.g. scanning electron microscopy [SEM]
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- 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
- G01N2001/2866—Grinding or homogeneising
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
The invention discloses a method for preparing a nano indentation sample of irradiated dispersion fuel based on a lapping integrated machine, which belongs to the technical field of preparation of samples after nuclear fuel and material irradiation, and comprises the following steps: acquiring a sample and transferring the sample to a shielding environment in which the lapping integrated machine is arranged; adhering a sample to a sample stage of a nano indentation instrument, and loading the sample stage on a cantilever of a lapping integrated machine; cutting the sample layer by layer until the height of the sample is 0.3-2 mm; grinding and polishing the cut sample sequentially, and electrically connecting the sample with a sample table; and the whole formed by electrically connecting the sample and the sample table falls off from the cantilever of the lapping integrated machine. By adopting the preparation method, the irradiated strong-radioactivity dispersion fuel sample with smooth surface, good conductivity and thickness less than 2mm can be effectively prepared, and the nano indentation test requirement can be met.
Description
Technical Field
The invention relates to a technology for preparing a sample after nuclear fuel and material irradiation, in particular to a method for preparing a nano indentation sample of irradiated dispersion fuel based on a lapping integrated machine and the obtained nano indentation sample of irradiated dispersion fuel.
Background
The nuclear fuel is a key core component of the reactor, the performance of the nuclear fuel is closely related to the safety and reliability of the reactor, but the mechanical performance of the nuclear fuel is inevitably degraded under the service working condition of high temperature, high pressure and strong irradiation in the reactor for a long time. Since the mechanical properties of nuclear fuel during service are directly related to the high-temperature failure behavior, research on the mechanical properties of irradiated fuel is urgently needed.
The fuel phase in the dispersion fuel is unevenly distributed, the mechanical property in the fuel phase after neutron irradiation is heterogeneous, the fuel is often cracked and broken under the action of temperature gradient and fission gas pressure, and the traditional macroscopic mechanical test method is difficult to study. In addition, the irradiated nuclear fuel has strong radioactivity, samples are extremely precious, the traditional macroscopic mechanical testing mode is usually destructive detection, the number of the samples is large, the size of the tested samples is large, the radioactivity is stronger, and the testing is difficult.
Nano indentation is an effective means for researching the mechanical properties of nuclear fuel after irradiation, but the distance from the nano indentation pressure head to a sample is only 2mm, so that the thickness of the sample is required to be less than 2mm, and meanwhile, the nano indentation test also requires that the surface of the sample is smooth and has low stress. The existing preparation method of the nuclear fuel electron microscope sample after strong radioactive irradiation is to inlay the fuel sample in a hot room, then grind and polish the inlaid sample by an automatic grinding and polishing machine, but the thickness of the inlaid sample is about 20mm, and the nano indentation test requirement cannot be met.
Disclosure of Invention
The invention aims to provide a preparation method of a nano indentation sample of irradiated dispersion fuel, which aims to solve the problems of nano indentation sample preparation.
The invention provides a method for preparing a nano indentation sample of irradiated dispersion fuel based on a lapping integrated machine, which comprises the following steps:
acquiring a sample and transferring the sample to a shielding environment provided with a lapping integrated machine;
adhering a sample to a sample stage of a nano indentation instrument, and loading the sample stage on a cantilever of a lapping integrated machine;
cutting the sample layer by layer until the thickness of the sample is 0.3-2 mm;
grinding and polishing the cut sample in sequence, and then electrically connecting the sample with the sample table;
and the whole formed by electrically connecting the sample and the sample table falls off from the cantilever of the lapping all-in-one machine.
The invention has the beneficial effects that: firstly, adhering a sample to a sample table of a nano indentation instrument for preparation, so that the situation that the sample is not adhered to the sample table well after the preparation of the sample is finished can be avoided; secondly, the lapping integrated machine is adopted to cut the sample layer by layer, so that the excessive acting force of the blade on the sample can be avoided, the sample falls off, and the thickness of the sample can be thinned to be below 2 mm; finally, grinding, polishing, ultrasonic cleaning and conductive slurry connection are combined, so that the obtained sample surface is smooth enough, the conductivity of the sample is good, and the subsequent measurement result is accurate; the sample prepared by the invention can meet the requirements of nano indentation test.
As a possible implementation, the sample size obtained should be as small as possible in order to make the radioactivity low and easy to prepare. But receive the restriction of hot indoor cutting sampling precision, and the sample size is too little, and the unable centre gripping of manipulator, consequently the sample length that usually obtains is 2mm ~6mm, and width is 1mm ~3mm, highly is the primitive thickness (2 mm ~3 mm) of fuel plate.
As a possible implementation mode, the thickness of each cut in the layer-by-layer cutting process is 90-110 mu m, preferably 98-102 mu m, so that the safety accident caused by overlarge interaction force between a blade and a sample in the cutting process and the falling of the sample from a sample table of the nano indentation instrument can be effectively prevented.
As a possible implementation manner, in the layer-by-layer cutting process, the rotating speed of the cutting blade is 10000-15000 r/min, preferably 12000 r/min; the water flow speed in the cutting process is 12-16 ml/min, preferably 15 ml/min.
As a possible implementation, during the grinding process, at least two grinding discs of different diameters, preferably three, are used for the grinding.
As one possible implementation, when the abrasive disc is 3 in type, the three abrasive discs have diameters of 9 μm, 2 μm, and 0.5 μm in order.
As one possible implementation, during polishing, the polishing liquid is a diamond suspension of 0.02 μm; preferably, the rotation speed of the polishing shaft is 200-300 r/min.
As one possible implementation manner, the conductive paste is adopted to realize electrical connection in the step of electrically connecting the surface of the sample obtained after polishing with the sample stage, so that good sample conductivity is realized, and the scanning electron microscope is adopted to observe the indentation position and morphology in the nanoindentation test process, and adverse effects of charge deposition on the nanoindentation test process are avoided.
Drawings
FIG. 1 is a schematic illustration of the nano-indentation of the irradiated strong-radioactivity U-Mo dispersion fuel in example 1.
Description of the embodiments
In order to make the technical problems, technical schemes and beneficial effects to be solved more clear, the invention is further described in detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
The inventor of the invention discovers that the fuel phase in the dispersion fuel is unevenly distributed, the mechanical property in the fuel phase after neutron irradiation is heterogeneous, and the fuel is often cracked and broken under the action of temperature gradient and fission gas pressure, so that the traditional macroscopic mechanical testing method is difficult to study. In addition, the irradiated nuclear fuel has strong radioactivity, and the sample is extremely precious, and the traditional macroscopic mechanical testing mode is usually destructive detection, so that the number of the samples is large, the size of the tested samples is large, the radioactivity is stronger, and the testing is difficult.
The inventors of the present invention have thus found that, in solving the above-described problems, the nanoindenter can study the mechanical properties (including hardness, young's modulus, etc.) of various local locations within the fuel sample on a smaller scale. The volume of a sample required by nano indentation is small, so that the radioactivity of the sample is low, and the detection is convenient; the nano indentation test can not destroy the sample, so that the sample is saved, multiple groups of data can be obtained by testing in the same sample, the test is accurate, convenient and efficient, and the method is a powerful means for researching the mechanical properties of the irradiated nuclear fuel.
However, the nanoindentation test requires that the sample surface be flat, smooth, and the sample thickness cannot exceed this value since the nanoindenter indenter is only 2mm from the sample stage. Meanwhile, the nano indentation test needs to be combined with the in-situ observation and positioning of a scanning electron microscope, and the sample conductivity is also good.
The existing electron microscope sample preparation process after neutron irradiation is to put a sample into a sample tube in a hot chamber, insert epoxy resin into the sample tube, and grind and polish the embedded sample by an automatic grinding and polishing machine. However, the thickness of the sample tube is about 20mm, which is far more than 2mm required by the nanoindentation instrument, and the requirements cannot be met.
The invention provides a method for preparing a nano indentation sample of irradiated dispersion fuel based on a lapping integrated machine, which comprises the following steps:
s1, acquiring a sample and transferring the sample to a shielding environment in which the lapping integrated machine is arranged;
in the present invention, the sample obtaining method may be: and selecting and cutting in the hot chamber through a milling machine. The "hot cell" is a shielded cell that performs high-emissivity tests and operations; and (3) in the cutting and sampling process, personnel are completed outside the hot chamber through a mechanical arm. The size of the samples that can be cut and clamped out with a manipulator in a hot cell is typically 6mm x 3mm x 3mm due to the difficulty of handling.
In the invention, the transportation of the sample can be carried out by adopting a lead tank and other equipment with shielding effect; as used herein, the "shielded environment" refers to an enclosed environment having shielded radiation, which may be provided by a shielded glove box in the present invention.
S2, adhering the sample to a sample stage of a nano indentation instrument and loading the sample stage on a cantilever of the fine grinding integrated machine;
in the invention, the sample is adhered to the sample stage of the nanoindentation instrument and the sample stage is loaded on the cantilever of the lapping integrated machine, the sequence of the sample stage and the cantilever can be any sequence, and the sample stage is loaded on the cantilever of the lapping integrated machine and then adhered to the sample stage of the nanoindentation instrument, so that the condition that the sample is carelessly dropped when the sample is adhered and loaded at first can be avoided.
In the invention, the sample can be adhered to a sample stage of the nano indentation instrument through 3M AB glue; in the invention, the sample table can be fixed on a cylindrical sample fixing clamp of the lapping integrated machine, and then the cylindrical sample fixing clamp can be fixed on a cantilever of the lapping integrated machine.
S3, cutting the sample layer by layer;
as used herein, the "layer-by-layer cleavage" refers to a layer-by-layer cleavage of the sample; in the invention, the thickness of each cutting is generally 90-110 mu m, suitably 98-102 mu m, more suitably 100 mu m, and the safety accident caused by overlarge interaction force between a cutting tool and a sample in the cutting process can be effectively prevented from falling off from a sample table of the nano indentation instrument.
In the present invention, the cutting tool used in the cutting process may be made of any material that is insulating and has a microhardness greater than 7200, such as: a cutter.
In the invention, the height of the sample is generally 0.3-2 mm when cutting is completed, and is suitably 1mm, the height can meet the requirement that the distance between the indenter of the nanoindenter and the sample stage can be measured under the condition of only 2mm, and a sufficient space is reserved, so that the sample stage can be conveniently loaded onto the nanoindenter subsequently.
In the invention, the rotating speed of the cutting tool is generally 10000-15000 r/min, suitably 12000 r/min; the water flow speed in the cutting process is generally 12-16 ml/min, and is suitably 15 ml/min, and the heat generated in the cutting process can be timely taken away by spraying water on the blade, so that the cutting process is ensured to be carried out smoothly.
S4, grinding and polishing the sample obtained after cutting;
in the invention, the number of the grinding discs is three, so that the diameter of one grinding disc is about 9 mu m, the diameter of the second grinding disc can be about 2 mu m, and the diameter of the last grinding disc can be 0.5 mu m; in the present invention, the abrasive disc used in the grinding process may be made of diamond.
In the grinding process, the rotating speeds of the grinding discs with different diameters are generally 1800-2200 r/min, suitably 1800-2000 r/min, more suitably 2000 r/min; because heat and generated scraps are taken away by spraying water in the grinding process, the flow rate of the water can be correspondingly adjusted according to the rotating speed of the grinding disc, and is generally 3-6 ml/min, suitably 4-6 ml/min, more suitably 4 ml/min.
In order to obtain a flat plane with stable conductivity, the polishing liquid is adopted for polishing after grinding, so that a flatter plane can be obtained, heat and generated dust in the polishing process can be taken away, an additional water spraying process is not required, and the cost is saved; in the invention, the solute in the polishing solution can be diamond, and the grain diameter of the diamond is 0.02 mu m; in the invention, the polishing speed in the polishing process can be 200-300 r/min, and is suitably 280-300 r/min.
S5, electrically connecting a sample with the sample table;
in the present invention, the sample and the sample stage may be connected by any material capable of achieving an electrically conductive connection between the two, such as conductive silver paste; in the invention, when the conductive material is slurry, the surface of the sample can be connected with the sample platform in a coating mode; in the invention, the tool used in the coating process can be any tool capable of completing coating, such as a toothpick, and the invention does not limit the coating tool; in the present invention, the conductive material need only be coated on a region of the sample surface, suitably less than 20% of the sample surface area, so as not to interfere with subsequent nanoindentation testing (nanoindentation testing should be performed with the uncoated location selected).
S6, the whole formed by electrically connecting the sample and the sample table falls off from the cantilever of the lapping all-in-one machine.
The invention has the beneficial effects that:
firstly, adhering a sample to a sample table of a nano indentation instrument and then carrying out surface treatment, so that the situation that the sample is difficult to adhere after the surface treatment is finished can be avoided; secondly, adopt lapping all-in-one to carry out the layer by layer cutting to the sample, can effectively prevent that the interact power between blade and the sample from too big in the cutting process from leading to strong radioactivity sample to drop from nanometer indentation appearance sample stage and causing the incident. Finally, by adopting the preparation method, the surface of the prepared sample is smooth enough, the conductivity is good, the thickness is less than 2mm, and the nano indentation test requirement can be met.
The method for preparing the nano indentation sample of the irradiated dispersion fuel based on the lapping integrated machine comprises the following steps:
(1) Selecting and cutting a sample of 6mm ×3× 3mm ×3× 3mm (length×width×height) in a hot chamber by a milling machine;
(2) Transferring the sample into a shielding glove box with a lapping integrated machine through a lead tank;
(3) Fixing a sample stage of the nanoindentation instrument by a cylindrical sample fixing clamp of the lapping integrated machine, loading the sample stage onto a cantilever of the lapping integrated machine, placing the cantilever into an auxiliary tool for autonomous design and processing, and finally adhering a sample to the sample stage of the nanoindentation instrument by 3M AB structural adhesive;
(4) Loading a cutter on a motor spindle, cutting the surface of a sample layer by layer according to set cutting parameters (the rotating speed is 15000r/min, the water flow speed is 15 ml/min) after cutting, so as to achieve the purpose of thinning, wherein the thickness of each cut is 100 mu m, and the thickness of the sample is thinned to 1 mm;
(5) According to the set grinding parameters (the rotating speed is 2000 r/min, the water flow speed is 4 ml/min), the surfaces of the samples are sequentially ground by using diamond grinding discs with the particle diameters of 9 mu m, 2 mu m and 0.5 mu m respectively;
(6) Taking down the millstone on the main shaft, replacing the millstone with a polishing disc, using diamond polishing liquid with the thickness of 0.02 mu m, and polishing the surface of the sample according to set polishing parameters (300 r/min, closing water flow);
(7) And dipping the conductive silver paste with a toothpick, coating the sample, connecting the sample surface with a sample stage with nano indentation, and taking the sample stage with the sample out of the fixed clamp to be used for the test of the nano indentation instrument.
A schematic diagram of the strong-radioactivity U-Mo dispersion fuel nanoindentation after irradiation is shown in figure 1; as can be seen from fig. 1, the method for preparing a sample disclosed by the invention successfully prepares a nano indentation sample of the irradiated strong-radioactivity dispersion fuel, which has a bright and clean surface, good conductivity and a thickness of less than 2mm, and successfully realizes analysis of the sample through a nano indentation instrument.
The foregoing description of the embodiments has been provided for the purpose of illustrating the general principles of the invention, and is not meant to limit the scope of the invention, but to limit the invention to the particular embodiments, and any modifications, equivalents, improvements, etc. that fall within the spirit and principles of the invention are intended to be included within the scope of the invention.
Claims (10)
1. The preparation method of the nano indentation sample of the irradiated strong-radioactivity dispersion fuel based on the lapping integrated machine is characterized by comprising the following steps of:
acquiring a sample and transferring the sample to a shielding environment in which the lapping integrated machine is arranged;
adhering the sample to a sample stage of a nano indentation instrument, and loading the sample stage on a cantilever of the lapping integrated machine;
cutting the sample layer by layer until the thickness of the sample is 0.3-2 mm;
sequentially grinding and polishing the cut sample, and cleaning by an ultrasonic cleaner;
electrically connecting a sample with the sample stage;
and the whole formed by electrically connecting the sample and the sample table is taken down from the cantilever of the lapping all-in-one machine.
2. The method of claim 1, wherein the sample is 2mm to 6mm in length, 1mm to 3mm in width, and 2mm to 3mm in height.
3. The method according to claim 1, wherein the thickness of each cut during the layer-by-layer cutting is 90 μm to 110 μm.
4. The method according to claim 1, wherein the rotation speed of the cutting blade is 10000-15000 r/min in the layer-by-layer cutting process; the water flow speed in the cutting process is 12-16 ml/min.
5. The method of claim 1, wherein during grinding, at least two grinding discs of different diameters are used for grinding.
6. The method of claim 5, wherein when the abrasive discs are 3 in a category, the three abrasive discs have diameters of 9 μm, 2 μm, and 0.5 μm in that order.
7. The method of claim 1, wherein during polishing, the polishing liquid is a diamond suspension of 0.02 μm; the rotation speed of the polishing shaft is 200-300 r/min.
8. The method according to claim 1, wherein the ultrasonic cleaning is performed for 3 to 5 minutes using absolute ethanol during the ultrasonic cleaning.
9. The method of claim 1, wherein the step of electrically connecting the sample obtained after polishing to the sample stage is accomplished by using a conductive paste.
10. A nano-indentation sample of irradiated dispersion fuel prepared by the method of any one of claims 1-9.
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