CN115753291A - Method for preparing gradient tissue structure material by laser remelting - Google Patents
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Abstract
The invention relates to the technical field of material irradiation damage resistance, in particular to a method for preparing a gradient tissue structure material by laser remelting, which comprises the following steps of S1, laser remelting: preparing a gradient tissue structure material by laser remelting; s2, irradiation experiment: carrying out an irradiation experiment on the surface of the gradient tissue structure material; s3, performance test and structural characterization preparation: and for the irradiated material microstructure gradient change area, performing mechanical property test and microstructure characterization sample preparation on the sample of the microstructure gradient change area by using a nanoindenter and a converged ion beam. The method for preparing the gradient structure material by laser remelting provided by the embodiment of the invention generates various microstructures in one alloy sample, can realize the performance test and the structure characterization of the various microstructures through the irradiation experiment of one alloy sample, and saves a large amount of personnel, time, experiment expenses and other costs.
Description
Technical Field
The invention relates to the technical field of irradiation damage resistance of materials, in particular to a method for preparing a gradient tissue structure material by laser remelting.
Background
With the rapid development of the nuclear power industry in China, higher requirements are put forward on advanced nuclear energy material equipment. Besides the environment of high temperature, high pressure and strong corrosion, the material is subjected to irradiation of neutrons and other high-energy particles for a long time in a nuclear reactor, and a large amount of atomic displacement and helium atom impurities are generated inside the nuclear reactor, so that the problems of swelling, deformation, element segregation and the like of the material are caused, and the mechanical property, the corrosion resistance and the like of the material are influenced. Therefore, ensuring that the nuclear power material has good radiation resistance is a key problem in the field of advanced nuclear power materials.
Due to long-term exposure to energy-carrying particle irradiation, a large number of irradiation defects are generated in the material, so that the microstructure and chemical composition of the material are changed. The properties of the radiation-resistant material such as radiation resistance, mechanics, corrosion resistance and the like of the microstructure have a great influence, so that intensive research on the properties is necessary.
Neutron irradiation is adopted in the traditional irradiation experiment of the irradiation-resistant material, but the neutron irradiation period is long, the equipment is rare, and the experiment cost is high. Therefore, in order to reduce the experiment period, the experiment cost and the irradiation time of personnel, a preparation method of the anti-irradiation gradient tissue needs to be developed, various microstructures are generated in one alloy sample, the performance test and the structural characterization of the various microstructures can be realized through the irradiation experiment of the alloy sample, and the purpose of high-throughput development of the anti-irradiation damage sample is further realized.
Disclosure of Invention
The invention aims to provide a method for preparing a gradient structure material by laser remelting, which can generate a plurality of microstructures in an alloy sample, can realize the performance test and the structure characterization of the plurality of microstructures through the irradiation experiment of the alloy sample, and save a large amount of personnel, time, experiment expenses and other costs so as to solve the problems in the background art.
In order to achieve the purpose, the invention provides the following technical scheme:
a method of preparing a gradient texture material using laser remelting, the method comprising the steps of:
s1, laser remelting: preparing a gradient tissue structure material by laser remelting;
s2, irradiation experiment: carrying out an irradiation experiment on the surface of the gradient tissue structure material;
s3, performance test and structural characterization preparation: for the irradiated material microstructure gradient change area, a nano indenter and a converged ion beam are utilized to perform mechanical property test on a sample in the microstructure gradient change area and prepare a microstructure characterization sample;
s4, tissue structure characterization: and carrying out analysis by a scanning electron microscope, a transmission electron microscope and a three-dimensional atom probe.
Preferably, the S1 includes the steps of:
s1-1, cutting an alloy material into samples with the size of 10 multiplied by 15mm, respectively grinding the samples by sand paper of 150#, 320#, 600#, 1000# and the like, and then polishing the surfaces of the ground samples;
s1-2, loading the sample processed in the step S1-1 into laser remelting equipment, and carrying out laser remelting treatment on the polished surface;
and S1-3, performing line cutting on the sample of the S1-2 in parallel to the laser remelting surface, and sequentially forming a laser remelting area, a heat affected zone and an original casting area from the cut surface close to the laser remelting surface downwards.
Preferably, the preparation of the gradient structure material by laser remelting in S1 comprises:
and (3) selecting the laser scanning speed of 200mm/min and the laser output power of 250W, and carrying out laser cladding until the thickness of the cladding layer is not less than 300 mu m, thus finishing the preparation of the material with the gradient tissue structure.
Preferably, the wire cutting of the sample of S1-2 parallel to the laser remelting face in S1-3 comprises:
the cut samples were less than 18mm by 18mm in length and width and not more than 2mm in thickness.
Preferably, the S3 includes:
and (3) nano indentation testing: after a sample is put into a nano-indenter, an area meeting the requirement is selected under an optical lens to be marked, 8 points are taken for each sample, meanwhile, the linear distance between two adjacent points is guaranteed to be larger than 20 times of the indentation depth, after the points are selected, the instrument is closed, a pressure head moves to a nano-indentation test mark area to be tested, in the test process, the pressure head moves 2000nm into the sample in the nano-indentation test mark area, the running speed is 10nm/s, the pressure head can be slowly unloaded after the running speed reaches 2000nm, the surface is slowly collected again, the system records the values of the indentation depth and the hardness once at intervals, and finally a curve of the depth changing along with the hardness is formed.
Preferably, the S4 includes:
s4-1, scanning electron microscope analysis: after the sample is irradiated, the sample can be directly placed into a scanning electron microscope device for testing.
Preferably, the S4 further includes:
s4-2, transmission electron microscope analysis: 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 special sample table, then carrying out thinning operation, directly enabling the thickness of the sample to reach below 100nm, completing the preparation of the transmission electron microscope sample, and carrying out transmission electron microscope analysis after the preparation.
Preferably, the S4 further includes:
s4-3, three-dimensional atom probe analysis: 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 block sample by using a nanometer hand, placing the block sample on a special sample base, carrying out annular cutting to obtain a needle-shaped sample with the diameter of the top end below 100nm, and carrying out three-dimensional atom probe analysis after preparation.
Compared with the prior art, the invention has the beneficial effects that:
the method for preparing the gradient structure structural material by laser remelting provided by the embodiment of the invention adopts laser remelting to prepare the irradiation-resistant material of the gradient structure, and then irradiation experiments are carried out, so that the influence of irradiation on different structures can be researched.
Drawings
Fig. 1 is a schematic view of a laser remelting partition of a method for preparing a gradient structural material by laser remelting according to an embodiment of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, belong to the protection scope of the present invention.
The embodiment of the invention provides a method for preparing a gradient tissue structure material by laser remelting, which comprises the following steps:
s1, laser remelting: preparing a gradient tissue structure material by laser remelting;
s2, irradiation experiment: carrying out an irradiation experiment on the surface of the gradient tissue structure material;
s3, performance test and structural characterization preparation: for the irradiated material microstructure gradient change area, a sample in the microstructure gradient change area is subjected to mechanical property test and microstructure structure characterization sample preparation by using a nanoindenter and a converged ion beam;
s4, tissue structure characterization: and carrying out analysis by a scanning electron microscope, a transmission electron microscope and a three-dimensional atom probe.
The method for preparing the gradient structure material by laser remelting provided by the embodiment of the invention generates various microstructures in one alloy sample, can realize the performance test and the structure characterization of the various microstructures through the irradiation experiment of one alloy sample, and saves a large amount of personnel, time, experiment expenses and other costs.
Fig. 1 is a schematic view of a laser remelting partition of a method for preparing a gradient structural material by laser remelting according to an embodiment of the present invention. As shown in fig. 1, in one embodiment of the present invention, S1 includes the steps of:
s1-1, cutting an alloy material into samples with the size of 10 multiplied by 15mm, respectively grinding the samples by sand paper of 150#, 320#, 600#, 1000# and the like, and then polishing the surfaces of the ground samples;
s1-2, loading the sample processed in the step S1-1 into laser remelting equipment, and carrying out laser remelting treatment on the polished surface;
and S1-3, performing line cutting on the sample of the S1-2 in parallel to the laser remelting surface, and sequentially forming a laser remelting area 1, a heat affected area 2 and an original casting area 3 from the cut surface close to the laser remelting surface downwards.
After cutting, nano indentation test, scanning electron microscope analysis, transmission electron microscope sample analysis and three-dimensional atom probe analysis are respectively carried out on the laser remelting area 1, the heat affected area 2 and the original casting area 3, so that the influence of irradiation on different tissues can be researched.
Specifically, the step of preparing the gradient structure material by laser remelting in the step S1 comprises the following steps:
selecting the laser scanning speed of 200mm/min and the laser output power of 250W, and carrying out laser cladding until the thickness of the cladding layer is not less than 300 mu m, thereby completing the preparation of the gradient structure material and ensuring that the cladding layer has no obvious defects such as cavities, cracks and the like.
In an embodiment of the present invention, the wire cutting of the sample of S1-2 in S1-3 parallel to the laser remelting plane comprises:
the length and width of the cut sample are less than 18mm < 18mm, and the thickness of the cut sample is not more than 2mm, so that the sample is completely covered by the beam spot of the ion beam when an irradiation experiment is carried out.
The S3 of the method for preparing the gradient structure material by laser remelting comprises the following steps:
and (3) nano indentation testing: after a sample is put into a nano-indenter, an area meeting the requirement is selected under an optical lens to be marked, 8 points are taken for each sample, meanwhile, the linear distance between two adjacent points is guaranteed to be larger than 20 times of the indentation depth, after the points are selected, the instrument is closed, a pressure head moves to a nano-indentation test mark area to be tested, in the test process, the pressure head moves 2000nm into the sample in the nano-indentation test mark area, the running speed is 10nm/s, the pressure head can be slowly unloaded after the running speed reaches 2000nm, the surface is slowly collected again, the system records the values of the indentation depth and the hardness once at intervals, and finally a curve of the depth changing along with the hardness is formed.
The S4 of the method for preparing the gradient structure material by laser remelting comprises the following steps:
s4-1, scanning electron microscope analysis: after the sample is irradiated, the sample can be directly placed into a scanning electron microscope device for testing;
s4-2, transmission electron microscope analysis: 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; 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, then carrying out thinning operation, directly finishing the preparation of the transmission electron microscope sample when the thickness of the sample reaches below 100nm, and carrying out transmission electron microscope analysis after the preparation;
s4-3, three-dimensional atom probe analysis: 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 block sample by using a nanometer hand, placing the block sample on a special sample base, carrying out annular cutting to obtain a needle-shaped sample with the diameter of the top end below 100nm, and carrying out three-dimensional atom probe analysis after preparation.
The method for preparing the gradient structure material by laser remelting provided by the embodiment of the invention adopts laser remelting to prepare the irradiation-resistant material of the gradient structure, and then irradiation experiments are carried out, so that the influence of irradiation on different structures can be researched.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (8)
1. A method for preparing a gradient structure material by laser remelting, comprising the steps of:
s1, laser remelting: preparing a gradient tissue structure material by laser remelting;
s2, irradiation experiment: carrying out an irradiation experiment on the surface of the gradient tissue structure material;
s3, performance test and structural characterization preparation: for the irradiated material microstructure gradient change area, a sample in the microstructure gradient change area is subjected to mechanical property test and microstructure structure characterization sample preparation by using a nanoindenter and a converged ion beam;
s4, tissue structure characterization: and carrying out analysis by a scanning electron microscope, a transmission electron microscope and a three-dimensional atom probe.
2. The method according to claim 1, wherein S1 comprises the steps of:
s1-1, cutting an alloy material into samples with the size of 10 multiplied by 15mm in a wire mode, respectively grinding the samples through sand paper such as 150#, 320#, 600#, 1000#, and the like, and then polishing the surfaces of the ground samples;
s1-2, loading the sample treated in the step S1-1 into laser remelting equipment, and performing laser remelting treatment on the polished surface;
and S1-3, performing line cutting on the sample of the S1-2 in parallel to the laser remelting surface, and sequentially forming a laser remelting area (1), a heat affected area (2) and an original casting area (3) from the cut surface close to the laser remelting surface downwards.
3. The method of claim 2, wherein the step of preparing the gradient structure material by laser remelting in S1 comprises:
and (3) selecting the laser scanning speed of 200mm/min and the laser output power of 250W, and carrying out laser cladding until the thickness of the cladding layer is not less than 300 mu m, thus finishing the preparation of the material with the gradient tissue structure.
4. The method of claim 3, wherein the wire cutting a sample of S1-2 parallel to the laser remelting surface in S1-3 comprises:
the cut samples were less than 18mm by 18mm in length and width and not more than 2mm in thickness.
5. The method according to any one of claims 1 to 4, wherein the step S3 comprises:
and (3) nano indentation testing: after a sample is put into a nano-indenter, an area meeting the requirement is selected under an optical lens to be marked, 8 points are taken for each sample, meanwhile, the linear distance between two adjacent points is guaranteed to be larger than 20 times of the indentation depth, after the points are selected, the instrument is closed, a pressure head moves to a nano-indentation test mark area to be tested, in the test process, the pressure head moves 2000nm into the sample in the nano-indentation test mark area, the running speed is 10nm/s, the pressure head can be slowly unloaded after the running speed reaches 2000nm, the surface is slowly collected again, the system records the values of the indentation depth and the hardness once at intervals, and finally a curve of the depth changing along with the hardness is formed.
6. The method of claim 5, wherein the step S4 comprises:
s4-1, scanning electron microscope analysis: after the sample is irradiated, the sample can be directly placed into a scanning electron microscope device for testing.
7. The method according to claim 6, wherein the step S4 further comprises:
s4-2, transmission electron microscope analysis: 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 special sample table, then carrying out thinning operation, directly enabling the thickness of the sample to reach below 100nm, completing the preparation of the transmission electron microscope sample, and carrying out transmission electron microscope analysis after the preparation.
8. The method according to claim 7, wherein the step S4 further comprises:
s4-3, three-dimensional atom probe analysis: 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 block sample by using a nanometer hand, placing the block sample on a special sample base, carrying out annular cutting to obtain a needle-shaped sample with the diameter of the top end below 100nm, and carrying out three-dimensional atom probe analysis after preparation.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN116519727A (en) * | 2023-03-21 | 2023-08-01 | 浙江大学 | Scanning electron microscope and observation method for microstructure evolution of sample thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116519727A (en) * | 2023-03-21 | 2023-08-01 | 浙江大学 | Scanning electron microscope and observation method for microstructure evolution of sample thereof |
| CN116519727B (en) * | 2023-03-21 | 2024-03-26 | 浙江大学 | Scanning electron microscope and observation method for microstructure evolution of sample thereof |
| 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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