CN114509460A - Pretreatment method for zirconium alloy scanning electron microscope sample before neutron irradiation - Google Patents
Pretreatment method for zirconium alloy scanning electron microscope sample before neutron irradiation Download PDFInfo
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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
- G01N1/32—Polishing; Etching
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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
- G01N1/34—Purifying; Cleaning
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E30/00—Energy generation of nuclear origin
- Y02E30/30—Nuclear fission reactors
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Abstract
The invention discloses a pretreatment method of a zirconium alloy scanning electron microscope sample before neutron irradiation, which comprises the steps of grinding and polishing the sample, and then pickling, wherein the grinding and polishing sequentially comprises rough polishing and fine polishing, the rough polishing is that the sample is ground on abrasive paper with different granularities from rough to fine, and the grinding mode is that the sample is rotated by 90 degrees and continuously ground in the vertical direction with the old grinding marks when the abrasive paper is replaced once until the old grinding marks completely disappear and the new grinding marks are uniform and consistent. The method can reduce the roughness and stress layer of the neutron irradiation injection surface to the maximum extent by carrying out grinding and polishing and chemical corrosion (acid washing) on the surface of the sample. In addition, the zirconium alloy sample of the scanning electron microscope prepared by the method can be directly subjected to microscopic structure and component analysis by the scanning electron microscope after neutron irradiation, so that the radioactive threat of oxygen generation after irradiation is avoided.
Description
Technical Field
The invention relates to the technical field of nuclear fuel circulation and irradiation, in particular to a pretreatment method of a zirconium alloy scanning electron microscope sample before neutron irradiation.
Background
The zirconium alloy is the most common mature cladding material in a pressurized water reactor, a boiling water reactor and a heavy water reactor, and is in a complex service environment of high-flux neutron irradiation, high temperature and high pressure and coolant corrosion for a long time, so that the macroscopic heat, force and chemical properties of the zirconium alloy cladding material are easily changed, and the changes of the properties are related to the change of the internal microstructure of the zirconium alloy cladding material caused by the neutron irradiation effect, therefore, the understanding of the specific mechanism of the effect of the irradiation on the microstructure of the zirconium alloy is of great importance for improving the service performance of the zirconium alloy.
The scanning electron microscope, as the most conventional microstructure analysis equipment, can perform analysis tests on the surface morphology, microstructure, element components of sample micro-regions, crystal micro-region orientation and the like. Neutron irradiation means that neutrons generated by a reactor bombard the surface of a sample and interact with atoms near the surface of a material, and the interaction comprises a collision process, a defect formation process and a microstructure evolution process, so that the physical, mechanical potential energy, organization and structure of the material are changed. Because the action depth of neutron irradiation is very limited, and the irradiated zirconium alloy generally has strong radioactivity, in order to analyze the influence of the neutron irradiation on the microstructure and components of the zirconium alloy sample by using a scanning electron microscope, the zirconium alloy sample of the scanning electron microscope before the neutron irradiation needs to be pretreated.
At present, relatively few reports are reported on the pretreatment method of the zirconium alloy sample of the scanning electron microscope before neutron irradiation, so that a pretreatment method for the zirconium alloy sample of the scanning electron microscope before neutron irradiation needs to be designed, the scanning electron microscope is better applied to the microanalysis and characterization of a nuclear structure and a functional material, and theoretical support and technical support are provided for solving the evolution mechanism of the microscopic structure of the zirconium alloy cladding material in the irradiation process and improving the service performance of the zirconium alloy cladding material.
Disclosure of Invention
The invention aims to provide a pretreatment method of a zirconium alloy scanning electron microscope sample before neutron irradiation, which can reduce the roughness and stress layer of a neutron irradiation injection surface to the greatest extent by grinding and polishing and chemical corrosion on the surface of the sample.
The invention is realized by the following technical scheme:
the utility model provides a zirconium alloy scanning electron microscope sample preprocessing method before neutron irradiation, grinds earlier and throws the pickling again to the sample, grind and throw and include in proper order roughly throwing and the essence is thrown, roughly throw and grind by thick to thin in proper order for the sample on the abrasive paper of different granularities, when grinding the mode for every change abrasive paper, rotate 90 with the sample and become the vertical direction with old grinding scar and continue to grind until old grinding scar disappears completely, and new grinding scar is even unanimous.
The method can reduce the roughness and stress layer of the neutron irradiation injection surface to the maximum extent by grinding and polishing and chemical corrosion (acid washing) on the surface of the sample. In addition, the zirconium alloy sample of the scanning electron microscope prepared by the method can be directly subjected to microscopic structure and component analysis by the scanning electron microscope after neutron irradiation, so that the radioactive threat of oxygen generation after irradiation is avoided.
Further, water was sprayed on the sandpaper during rough polishing.
Further, the sand paper used for rough polishing is SiC sand paper.
Further, the fine polishing process comprises the following steps:
and adhering the goose down cloth on a polishing disc, uniformly and lightly pressing the sample on the goose down cloth during polishing, moving the sample back and forth along the diameter direction of the polishing disc, and controlling the humidity of the goose down cloth by using deionized water.
Furthermore, the humidity of the goose down cloth is controlled to ensure that the surface water film is completely evaporated and disappears within 2 s-3 s.
Further, the washing liquid adopted by the acid washing is HF and HNO3、H2SO4And H2O is as follows: 6: 3: 9 mixed solution, or HF, HNO3And H2O is mixed according to the ratio of 2:9: 9.
Further, the acid washing process is to soak the sample in the washing liquid for 30 to 60 seconds.
Further, the method comprises the following steps:
step S1, sample pretreatment;
step S2, sample pre-cleaning: cleaning a sample by using an organic solvent;
step S3, sample inlaying: embedding the cleaned sample into a die or a die sleeve;
step S4, roughly polishing a sample;
step S5, fine polishing of the sample;
step S6, taking the sample after fine polishing out of the mould or the die sleeve;
step S7, pickling a sample: the sample is immersed in the washing solution for 30 to 60 seconds.
In step S1, the sample pretreatment includes sample selection, sample interception, and sample labeling.
Further, in step S3, the sample is inlaid to facilitate polishing and inspecting the edge tissue of the sample. The selected embedding method can not change the original tissue of the sample, the invention takes a cold embedding method and a manual embedding method as specific embodiments, and the embedding die meets the size requirement of a grinding and polishing machine and is marked.
Cold embedding method: the sample is placed into the embedded die sleeve, and when the size of the sample is small, the sample can be clamped by the metal clamp to avoid the inclination of the observation surface. The prepared dissoluble resin is stirred evenly, is fully mixed and then is slowly injected into the embedded die sleeve for solidification.
A manual embedding method comprises the following steps: putting the sample into an embedded mould with the surface to be polished facing downwards, putting the sulfur powder into a beaker for heating and melting, slowly pouring the molten sulfur powder into the mould to exceed the height of the sample, and cooling the sulfur powder.
Compared with the prior art, the invention has the following advantages and beneficial effects:
1. the method can reduce the roughness and stress layer of the neutron irradiation injection surface to the maximum extent by grinding and polishing and chemical corrosion on the surface of the sample. In addition, the zirconium alloy sample of the scanning electron microscope prepared by the method can be directly subjected to microscopic structure and component analysis by the scanning electron microscope after neutron irradiation, so that the radioactive threat of oxygen generation after irradiation is avoided.
2. The method of the invention does not need complex mechanical equipment, is easy to realize and has obvious effect.
3. The sample prepared by the pretreatment method can better apply a scanning electron microscope to the microscopic analysis and characterization of nuclear structures and functional materials, and provides theoretical support and technical support for solving the evolution mechanism of the microscopic structure of the zirconium alloy cladding material in the irradiation process and improving the service performance of the zirconium alloy cladding material.
Drawings
The accompanying drawings, which are included to provide a further understanding of the embodiments of the invention and are incorporated in and constitute a part of this application, illustrate embodiment(s) of the invention and together with the description serve to explain the principles of the invention. In the drawings:
FIG. 1 is a macroscopic view of a zirconium alloy sample for a scanning electron microscope prepared by the method;
FIG. 2 is a metallographic image of a zirconium alloy sample for a scanning electron microscope prepared by the method.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail below with reference to examples and accompanying drawings, and the exemplary embodiments and descriptions thereof are only used for explaining the present invention and are not meant to limit the present invention.
Example 1:
according to the test requirements of the sample of the scanning electron microscope equipment, the test area of the sample size is not less than 100mm2The thickness of the zirconium alloy sample is preferably 1 mm-2 mm (smaller than the transverse dimension), and the inspection area of the sample can meet the requirement of a neutron irradiation test. The invention takes zirconium alloy samples with the size of 10mm multiplied by 15mm multiplied by 1mm and 10mm multiplied by 20mm multiplied by 1.5mm as specific examples, and the following is a specific implementation mode of the zirconium alloy microscopic analysis pretreatment method of the example.
1) Sample selection
In order to meet the requirement of effective inspection, the selection of the sample should represent the structural characteristics of the whole zirconium alloy block body as objectively and comprehensively as possible, and the intercepting direction, the intercepting part and the intercepting quantity of the sample should be cut according to the manufacturing method, the inspection purpose and the relevant standard specification of the sample.
2) Cutting of the sample
The method comprises the steps of cutting a zirconium alloy sample by a precision cutting machine, a wire cut electric discharge machine and the like, avoiding the influence (such as deformation, overheating and the like) of the cutting method on the zirconium alloy structure as much as possible when the sample is cut, removing an influence layer caused by cutting operation by using methods such as grinding with a grinding wheel and the like in the subsequent sample preparation process, and taking preventive measures (such as using cooling liquid and the like) when the sample is cut to prevent the structure from changing.
3) Specimen marking
And immediately marking other parts except the test surface of the sample after the sample is intercepted, so as to ensure that the sample is not disordered in the subsequent pretreatment process.
4) Sample cleaning
The cut sample has more greasy dirt on the surface, so the sample needs to be pre-cleaned. The cleaning solvent is an organic solvent capable of dissolving oil stains, the morphology and the structure of the zirconium alloy sample are not damaged, and acetone and absolute ethyl alcohol are selected in the embodiment. The specific operation comprises the steps of sequentially putting a zirconium alloy sample into acetone and an alcohol solvent (absolute ethyl alcohol), respectively carrying out ultrasonic treatment for 15min by using an ultrasonic cleaning agent, then washing the sample by using deionized water, and finally drying the sample.
5) Sample inlay
In order to conveniently polish and inspect the edge tissue of the sample, the sample needs to be embedded. The selected embedding method can not change the original tissue of the sample, the invention takes a cold embedding method and a manual embedding method as specific embodiments, and the embedding die meets the size requirement of a grinding and polishing machine and is marked.
The present embodiment adopts a cold-mosaic method: the sample is placed into the embedded die sleeve, and when the size of the sample is small, the sample can be clamped by the metal clamp to avoid the inclination of the observation surface. The prepared soluble epoxy resin is stirred evenly, is injected into the embedded die sleeve slowly after being fully mixed, and is cured.
6) Rough polishing of test sample
Preparing 220#, 600#, 800#, 1200#, 1500#, 3000#, 5000# SiC sand paper, flat glass or metal plate, and deionized water. Sequentially spreading the SiC sand paper on a glass or metal plate with a flat surface. And (4) sequentially grinding the embedded samples on sand paper with different granularity from coarse to fine. Before grinding, in order to avoid deeper scratches and better slow down the resistance in the grinding process, some deionized water needs to be sprinkled on the sand paper. The grinding mode is that each time the sand paper is replaced, the sample is rotated by 90 degrees and continuously ground in the direction vertical to the old grinding mark until the old grinding mark completely disappears and the new grinding mark is uniform and consistent. The sample was rinsed clean with deionized water before each sandpaper change.
7) Sample fine polishing
Preparing goose down cloth, diamond grinding paste (W1.5/6000 mesh) and deionized water, and sticking the goose down cloth on a polishing disc. When polishing, the sample is evenly lightly pressed on the goose down cloth, the sample is moved back and forth along the diameter direction of the polishing disc, the deionized water is utilized to control the humidity of the goose down cloth, the polishing quality is prevented from being affected (the tail is dragged due to too large humidity, and black spots are generated due to too small humidity), and when the sample is taken down from the disc to be observed due to the humidity of the goose down cloth, the surface water film is completely evaporated and disappears within 2-3 s. The sample is polished until the wear marks are completely removed and the surface is mirror-finished. If the polishing effect is not good, the polishing time can be properly increased until the polished surface is a mirror surface.
7) Sample removal
And selecting a proper solvent to take the polished sample out of the mosaic mold, wherein the solvent is selected to dissolve the mosaic reagent and take the shape and the structure of the zirconium alloy sample as the reference without damaging. In the embodiment, the inlaying reagent is epoxy resin, and epoxy resin dissolving liquid is selected to dissolve the epoxy resin, so that a zirconium alloy sample is taken out; if the mosaic reagent is selected from sulfur powder, CS is selected2Dissolving the zirconium alloy by using a solvent, and taking out a zirconium alloy sample (if other dissolving reagents are selected, the zirconium alloy sample is in the protection scope of the invention). The procedure 4 cleaning was repeated after the sample was removed. And replacing other inspection surfaces of the sample, and repeatedly carrying out the processes 5-6 to ensure that other 5 surfaces of the sample are flat.
8) Sample pickling
In order to reduce the influence of the stress layer in the sample preparation process and the roughness of the polished sample on the inspection of the zirconium alloy scanning electron microscope sample after ion irradiation as much as possible, a clamping tool is adopted to clamp the sample, and the sample moves back and forth in the pickling solution for pickling. Immediately cleaning the sample after acid washing with alcohol, sucking or drying the alcohol, and performing subsequent tests in time.
The acid washing solution is HF HNO3:H2SO4:H2O is 2: 6: 3: 9, HF, HNO may also be used3:H2The etching time is 30-60 s, and can be adjusted according to the solution temperature and the actual acid washing effect when necessary. The process was repeated for a further 4 washes after the acid wash. FIG. 1 is a graph showing the effect of the zirconium alloy sample after pickling and cleaning.
9) Examination of a sample
The microscopic appearance of the prepared sample is observed by adopting metallographic phase microscopy, the overall appearance of the sample is generally observed at low magnification, then the sample is inspected at different magnifications according to the test purpose, and different illumination observation modes can be adopted according to the research requirement, and the observation is usually carried out by adopting a bright field observation mode. And selecting a proper magnification factor and an illumination observation mode for an area needing to acquire an image, adjusting parameters such as a field diaphragm and an aperture diaphragm to ensure that the image observed under the objective lens is clearest and has the best contrast, and acquiring the image to determine whether the prepared sample meets the analysis requirement of the scanning electron microscope after ion irradiation. If the prepared sample is not qualified (obvious scratches, pollutants, oxides or reaction product layers exist on the surface of the sample), the preparation process of the analysis sample readjusts the test parameters to prepare the sample, and if necessary, the sample can be re-sampled to prepare the sample according to the test requirements until the prepared sample meets the analysis requirements of the scanning electron microscope after ion irradiation, as shown in fig. 2.
10) Sample preservation
The qualified prepared samples are properly stored, the numbers, the quantity and the storage positions of the samples are recorded, the stored samples are required to be traceably rechecked so as to ensure that the subsequent tests of the samples can be smoothly carried out, the samples of different types are stored separately, and necessary measures are taken to prevent sample mixing.
The above-mentioned embodiments are intended to illustrate the objects, technical solutions and advantages of the present invention in further detail, and it should be understood that the above-mentioned embodiments are merely exemplary embodiments of the present invention, and are not intended to limit the scope of the present invention, and any modifications, equivalent substitutions, improvements and the like made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (10)
1. The utility model provides a zirconium alloy scanning electron microscope sample pretreatment methods before neutron irradiation, its characterized in that, grinds the polishing earlier to the sample and carries out the pickling, grind and throw and include in proper order roughly throwing and finely polishing, roughly throw and grind by thick to thin in proper order for the sample on the abrasive paper of different granularities, when the mode of grinding is for every change abrasive paper, with the sample rotatory 90 with old wear scar one-tenth vertical direction continue to grind, until old wear scar disappears completely, and new wear scar is even unanimous.
2. The pretreatment method for the zirconium alloy scanning electron microscope sample before neutron irradiation according to claim 1, characterized in that water is sprayed on sand paper during rough polishing.
3. The pretreatment method for the zirconium alloy scanning electron microscope sample before neutron irradiation according to claim 1, characterized in that the sand paper used for rough polishing is SiC sand paper.
4. The pretreatment method for the zirconium alloy scanning electron microscope sample before neutron irradiation according to claim 1, characterized in that the fine polishing process comprises the following steps:
and adhering the goose down cloth on a polishing disc, uniformly and lightly pressing the sample on the goose down cloth during polishing, moving the sample back and forth along the diameter direction of the polishing disc, and controlling the humidity of the goose down cloth by using deionized water.
5. The pretreatment method for the zirconium alloy scanning electron microscope sample before neutron irradiation according to claim 4, characterized in that the humidity of the goose down cloth is controlled to ensure that the surface water film is completely evaporated and disappears within 2 s-3 s.
6. The method for pretreating a zirconium alloy scanning electron microscope sample before neutron irradiation according to claim 1, wherein washing liquids adopted by acid washing are HF and HNO3、H2SO4And H2O is as follows: 6: 3: 9 mixed solution, or HF, HNO3And H2O is mixed according to the ratio of 2:9: 9.
7. The method for pretreating a zirconium alloy scanning electron microscope sample before neutron irradiation according to claim 1, wherein the pickling process comprises soaking the sample in a washing solution for 30-60 s.
8. The pretreatment method for the zirconium alloy scanning electron microscope sample before neutron irradiation according to claim 1, characterized by comprising the following steps:
step S1, sample pretreatment;
step S2, sample pre-cleaning: cleaning a sample by using an organic solvent;
step S3, sample inlaying: embedding the cleaned sample into a die or a die sleeve;
step S4, roughly polishing the sample;
step S5, fine polishing of the sample;
step S6, taking the sample after fine polishing out of the mould or the die sleeve;
step S7, pickling a sample: the sample is soaked in the washing solution for 30 to 60 seconds.
9. The method for pretreating a zirconium alloy scanning electron microscope sample before neutron irradiation according to claim 8,
in step S1, the sample preprocessing includes sample selection, sample interception, and sample labeling.
10. The method for pretreating a zirconium alloy scanning electron microscope sample before neutron irradiation according to claim 8, wherein in step S3, the sample embedding comprises a cold embedding method and a manual embedding method, the cold embedding method is to put the sample into an embedding mold, stir the prepared soluble resin uniformly, mix the resin sufficiently, slowly inject the resin into the embedding mold, and cure the resin; the manual embedding method comprises the steps of putting a sample into an embedding die with a polished surface facing downwards, putting sulfur powder into a beaker for heating and melting, slowly pouring the molten sulfur powder into the die to exceed the height of the sample, and cooling the sulfur powder.
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| CN202210151374.8A CN114509460A (en) | 2022-02-18 | 2022-02-18 | Pretreatment method for zirconium alloy scanning electron microscope sample before neutron irradiation |
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