CN111965205B - Sample preparation method for observing SEM+EBSD of nickel-based powder superalloy in-situ sample micro-area - Google Patents
Sample preparation method for observing SEM+EBSD of nickel-based powder superalloy in-situ sample micro-area Download PDFInfo
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- 238000011065 in-situ storage Methods 0.000 title claims abstract description 41
- 238000001887 electron backscatter diffraction Methods 0.000 title claims abstract description 36
- 239000000843 powder Substances 0.000 title claims abstract description 32
- 229910000601 superalloy Inorganic materials 0.000 title claims abstract description 28
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 26
- 238000005464 sample preparation method Methods 0.000 title claims abstract description 16
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 13
- 238000000227 grinding Methods 0.000 claims abstract description 31
- 238000000034 method Methods 0.000 claims abstract description 22
- 244000137852 Petrea volubilis Species 0.000 claims abstract description 11
- 239000000956 alloy Substances 0.000 claims abstract description 9
- 238000012545 processing Methods 0.000 claims abstract description 9
- 238000005498 polishing Methods 0.000 claims description 29
- 238000005520 cutting process Methods 0.000 claims description 25
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 15
- 238000012360 testing method Methods 0.000 claims description 14
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 10
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 claims description 10
- 235000019441 ethanol Nutrition 0.000 claims description 10
- 238000001878 scanning electron micrograph Methods 0.000 claims description 6
- 238000007598 dipping method Methods 0.000 claims description 5
- 238000011010 flushing procedure Methods 0.000 claims description 5
- 238000003801 milling Methods 0.000 claims description 5
- 229920000742 Cotton Polymers 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- 239000008399 tap water Substances 0.000 claims description 4
- 235000020679 tap water Nutrition 0.000 claims description 4
- 238000005530 etching Methods 0.000 claims 1
- 238000004381 surface treatment Methods 0.000 abstract description 9
- 238000002360 preparation method Methods 0.000 abstract description 6
- 229910045601 alloy Inorganic materials 0.000 abstract description 4
- 230000007246 mechanism Effects 0.000 abstract description 3
- 230000000977 initiatory effect Effects 0.000 abstract description 2
- 230000006399 behavior Effects 0.000 abstract 1
- 239000000523 sample Substances 0.000 description 56
- 239000003518 caustics Substances 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 230000009286 beneficial effect Effects 0.000 description 4
- 239000002904 solvent Substances 0.000 description 4
- 229960003280 cupric chloride Drugs 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000009661 fatigue test Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000001513 hot isostatic pressing Methods 0.000 description 2
- 238000005204 segregation Methods 0.000 description 2
- 230000002159 abnormal effect Effects 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 238000000861 blow drying Methods 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000001192 hot extrusion Methods 0.000 description 1
- 238000010275 isothermal forging Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000004663 powder metallurgy Methods 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
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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
- 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
- G01N23/2206—Combination of two or more measurements, at least one measurement being that of secondary emission, e.g. combination of secondary electron [SE] measurement and back-scattered electron [BSE] measurement
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- General Health & Medical Sciences (AREA)
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Abstract
The invention belongs to the technical field of powder superalloy sample preparation, and relates to a sample preparation method for observing SEM+EBSD of nickel-based powder superalloy in-situ sample micro-areas; the invention adopts a method of processing a powder high-temperature alloy material into an in-situ stretching or low-cycle sample, a sand paper grinding sample and surface treatment to prepare the sample, and then uses a scanning electron microscope and a back scattering electronic device to observe SEM and EBSD; the method is simple and feasible, the prepared in-situ sample surface has no residual stress, the calibration of EBSD is facilitated, the sample surface is clean, the grain boundary can be displayed, the accurate positioning of crack initiation and propagation paths is facilitated, and meanwhile, the method can carry out in-situ tracking and observation on special parts in the alloy and has important significance for analyzing microscopic mechanical behaviors and mechanisms of the powder superalloy.
Description
The invention belongs to the technical field of preparation of powder superalloy samples, and relates to a sample preparation method for observing SEM+EBSD of nickel-based powder superalloy in-situ samples.
Background
The nickel-based powder superalloy is a precipitation strengthening superalloy prepared by a powder metallurgy process, and compared with the traditional casting superalloy and deformation superalloy, the powder superalloy can limit element segregation in one powder particle, further eliminate macro segregation of the element and improve the hot workability of the alloy; meanwhile, the powder superalloy can be subjected to superplastic hot working, so that the utilization rate of materials is improved, and raw materials are saved. The powder superalloy has the characteristics of uniform structure, fine grains and excellent mechanical properties, and has become the first choice material of an advanced aeroengine turbine disk.
The turbine disk is one of the most important core hot end components of the aero-engine and is used under high temperature, thermal shock, large load and variable load; with the development of high thrust-weight ratio, high power-weight ratio and high combustion efficiency engines, higher requirements are put on the comprehensive mechanical properties, reliability and durability of the turbine disk. At present, in order to improve the comprehensive mechanical property of the turbine disk, the development of new materials is advanced, and meanwhile, the preparation process of the turbine disk is greatly improved, namely, the original direct hot isostatic pressing and heat treatment is changed into the existing hot isostatic pressing, hot extrusion, isothermal forging and heat treatment, so that the uniformity of the disk structure and the more excellent mechanical property are improved.
However, during master alloy melting, powder preparation and a series of hot working processes, nonmetallic inclusions are introduced into the disc and abnormal grain structures are generated, and these special parts become weak points of the whole disc, and during the service of the disc, the parts become crack sources, so that failure and fracture of the disc are caused. Therefore, deep research on the evolution rule and micromechanics behavior of the tissue of the special part in the in-situ stretching or fatigue process is needed, so that the residual life and failure mechanism of the special part are mastered, and the data support is improved for the normal use of the turbine disk of the engine.
For a long time, the surface treatment method for simultaneously carrying out SEM+EBSD observation on the powder superalloy in-situ sample has conflict: SEM observation needs to keep the original shape of the surface, and usually adopts a sand paper flat grinding and water polishing method, but the surface of a sample has stress, and an EBSD image cannot be obtained; EBSD observation requires that the surface of the sample be flat and stress-free, and the surface treatment is usually carried out by adopting an electrolytic polishing method, but the surface morphology is changed; both observed surface treatments are not compatible. The surface treatment method for simultaneously carrying out SEM+EBSD observation on the in-situ sample abroad adopts a sand paper flat grinding and water polishing method, the in-situ sample is required to be gradually ground from 400-mesh sand paper to 4000-mesh sand paper, the requirement on grinding sample is extremely high, the sample preparation process is complex, and the success rate is low. The method is simple and feasible, the prepared in-situ sample surface has no residual stress, the calibration of the EBSD is facilitated, the grain boundary can be displayed on the basis of retaining the surface morphology, the accurate positioning of crack initiation and propagation paths is facilitated, and the method has important significance for analyzing the micromechanics behavior and mechanism of the powder superalloy.
Disclosure of Invention
The technical problems to be solved by the invention are as follows: the method for preparing the nickel-based powder superalloy in-situ sample by observing SEM+EBSD in a micro-area is provided, and the prepared in-situ sample can obtain a clear SEM image and an EBSD image with high acquisition rate, so that the microstructure change and mechanical behavior of the alloy at a special part in the in-situ stretching or fatigue process can be accurately observed.
The technical scheme of the invention is as follows: the sample preparation method for observing SEM+EBSD of nickel-based powder superalloy in-situ sample micro-area is characterized by comprising the following steps: firstly, cutting a block-shaped test block from a powder high-temperature alloy material, carrying out flat grinding, polishing and water polishing on the plane of the test block to obtain a test block with a flat surface and no scratch, and observing and marking a part to be observed under a metallographic microscope; secondly, processing the sample by taking the observation part as the center; then preparing corrosive agent, dipping the solution by using a cotton swab, slightly wiping the observed part of a working area, corroding for 3-4 seconds, sequentially flushing with clear water and alcohol, drying, and observing the observed part by SEM+EBSD to obtain SEM images and EBSD images with grain boundaries.
The flat grinding and the water polishing are that firstly, a grinding machine is used for carrying out flat grinding on the sample plane, the roughness is less than or equal to 0.8, then, the flat grinding is carried out on a grinding machine, and then, polishing and the water polishing are carried out on a polishing machine with the thickness of 2.5 mu m and a polishing machine with the thickness of 1.5 mu m, so as to obtain a test block with a flat surface and no scratch.
The sample grinding machine is used for grinding with 600-mesh, 800-mesh, 1000-mesh, 1200-mesh and 1500-mesh sand paper.
The sample is an in situ sample.
The processing method of the sample comprises the steps of firstly linearly cutting a flat sample with a certain thickness, then processing the flat sample with a milling cutter taking an observation part as a center according to an in-situ sample drawing, gradually thinning the flat sample with linear cutting in the thickness direction, slowly moving wires with linear cutting when the thickness direction approaches to the thickness required by the sample, and then cleaning the processed sample with tap water and alcohol in sequence.
The wire cutting current of the wire cutting slow-moving wire is less than or equal to 0.5mA.
The corrosive agent is 10g of copper chloride, 50ml of absolute ethyl alcohol and 50ml of hydrochloric acid.
And the observation of SEM and EBSD is carried out by adopting a scanning electron microscope and a back scattering electron device to observe the observation part simultaneously.
The invention has the advantages and beneficial effects that: the invention provides a sample preparation method for observing SEM+EBSD of a nickel-based powder superalloy in-situ sample, which has the following advantages and beneficial effects.
(1) The in-situ sample prepared by the sample preparation method can prevent the sample from buckling and deforming in the processing process, so that the surface of the sample is flat.
(2) A clear SEM image containing grain boundaries is obtained, which is beneficial to observing the tissue change of a working area in an in-situ process;
(3) The EBSD image with high acquisition rate is obtained, which is beneficial to observing the tissue change of the working area in the in-situ process;
(4) The method has the advantages that the tissue change and micromechanics behavior of a special part in the in-situ process are mastered, the service life prediction of the powder disc is facilitated, and the use safety and reliability of the engine are improved.
Description of the drawings:
FIG. 1 is a flow chart for preparing an SEM+EBSD in-situ sample
(a) Sand paper flat grinding, polishing by polishing machine, water polishing and calibrating observation part
(b) Wire cutting
(c) Milling machine
(d) Wire-electrode cutting layer-by-layer thinning
(e) Corrosive wiping working area
(f) Water + alcohol rinse + blow-dry
FIG. 2 example 1 in situ drawing sheet
FIG. 3 example 1SEM image and EBSD image
FIG. 4 example 2 in situ drawing
FIG. 5 example 2SEM image and EBSD image
Detailed Description
The invention is further illustrated by the following examples in conjunction with the accompanying drawings:
firstly cutting a block-shaped sample from a powder high-temperature alloy material, carrying out flat grinding on the sample plane by a grinding machine, then carrying out flat grinding on a sample grinding machine by sand paper, then sequentially carrying out polishing by a polishing agent and water polishing to obtain a test block with a flat surface and no scratch, and observing and marking a part to be observed under a metallographic microscope; secondly, processing according to a sample drawing by taking an observation part as a center; then preparing a surface treatment corrosive agent, wherein the preparation ratio of the corrosive agent is 10g of copper chloride, 50ml of absolute ethyl alcohol and 50ml of hydrochloric acid, dipping the solvent with a cotton swab, slightly wiping the observed part of a working area, after corroding for 3-4 seconds, flushing the observed part with clear water and alcohol, and drying the washed part by a blower; and finally, observing an observation part by using a scanning electron microscope and a back scattering electron probe device to obtain a clear SEM image containing a grain boundary and an EBSD image with high acquisition rate.
1. Firstly cutting a powder superalloy material into a block-shaped sample (the plane size is larger than that of an in-situ sample) which is convenient to manually hold, carrying out flat grinding on the large plane of the block-shaped sample, wherein the roughness is less than or equal to 0.8, then carrying out flat grinding on a grinding machine by using 600-mesh, 800-mesh, 1000-mesh, 1200-mesh and 1500-mesh sand paper, then polishing by using 2.5 mu m and 1.5 mu m polishing agents and water polishing to obtain a test block with a flat surface and no scratches, and observing and marking the part to be observed by using SEM+EBSD under a metallographic microscope. As shown in fig. 1 (a).
2. Processing according to a sample drawing by taking an observation part as a center: firstly, wire cutting a flat sample with a certain thickness (the smaller the thickness is, the better the thickness is under the condition that the sample is not deformed), then processing the flat sample by using a milling cutter with an observation part as the center according to an in-situ sample drawing, and then gradually thinning the flat sample by using wire cutting in the thickness direction to prevent the in-situ sample from buckling deformation, when the thickness direction is close to the thickness required by the sample, the wire cutting is slowly carried out, the wire cutting current is less than or equal to 0.5mA, the surface of a working area is prevented from being polluted by the wire cutting, and then the wire cut sample is washed by using tap water and alcohol, as shown in the (c) and (d) of fig. 1.
3. Preparing a surface treatment solvent, namely preparing a solvent with a ratio of 10g of cupric chloride to 50ml of absolute ethyl alcohol to 50ml of hydrochloric acid, dipping the cupric chloride in the solvent to perform surface treatment after the cupric chloride is completely dissolved and the solution is completely mixed, slightly wiping an observation part of a working area after corrosion for 3-4 seconds, flushing the observation part with clear water and alcohol, and blow-drying the observation part by a blower, thereby obtaining an in-situ sample with a clean surface and no stress, as shown in fig. 1 (e) and (f).
4. And (3) respectively observing the observed part by adopting a scanning electron microscope and a back scattering electronic device, so as to obtain a clear SEM image and an EBSD image with high acquisition rate of the observed part.
Embodiment one: SEM+EBSD image observation of inclusions at the surface of in-situ tensile sample of powder superalloy
And (3) preparing an in-situ tensile sample of the powder superalloy material, and observing SEM+EBSD images. Firstly cutting a 50mm multiplied by 20mm test block from a high-temperature alloy material, carrying out flat grinding on a large plane of the test block, wherein the roughness is less than or equal to 0.8, then carrying out flat grinding on a sample grinding machine by using 600-mesh, 800-mesh, 1000-mesh, 1200-mesh and 1500-mesh sand paper, then carrying out polishing and water polishing by using a 2.5-mu m and 1.5-mu m polishing machine to obtain a test block with a flat surface and no scratch, and observing and marking surface inclusions to be observed by SEM+EBSD under a metallographic microscope; secondly, taking the inclusion as a center, firstly linearly cutting a 50mm multiplied by 10mm flat sample, then taking the inclusion as a sample working area center, processing by using a milling cutter according to an in-situ sample drawing, as shown in figure 2, gradually thinning by linear cutting in the thickness direction, slowly feeding the wire by linear cutting when the thickness direction is close to the thickness required by the sample, wherein the current of the linear cutting is less than or equal to 0.5mA, and then cleaning the linearly cut sample by using tap water and alcohol; the corrosive agent is prepared from the following components in proportion: 10g of copper chloride, 50ml of absolute ethyl alcohol and 50ml of hydrochloric acid, dipping the solution with a cotton swab for surface treatment, slightly wiping the observation part of a working area, after corroding for 3-4 seconds, flushing with clear water and alcohol, and drying with a blower; finally, SEM+EBSD photo shooting is carried out by adopting a scanning electron microscope+back scattering flaw detection, and the picture is shown in figure 3.
Embodiment two: SEM+EBSD image observation of inclusions at the surface of in-situ fatigue test sample of powder superalloy
The procedure of example one was repeated to prepare an in-situ fatigue test specimen as shown in FIG. 4, after which the working area was observed by SEM+EBSD image, and the test results are shown in FIG. 5.
Claims (5)
1. The sample preparation method for observing SEM+EBSD of nickel-based powder superalloy in-situ sample micro-area is characterized by comprising the following steps: firstly, cutting a block-shaped test block from a powder high-temperature alloy material, carrying out flat grinding, polishing and water polishing on the plane of the test block to obtain a test block with a flat surface and no scratch, and observing and marking surface inclusions to be observed by SEM+EBSD under a metallographic microscope; secondly, processing a sample by taking the inclusion as a center; firstly wire-cutting a 50mm multiplied by 10mm flat sample, then using a milling cutter to process the flat sample according to an in-situ sample drawing by taking inclusions as the center of a sample working area, then using wire-cutting to gradually thin the flat sample in the thickness direction, and when the thickness direction is close to the required thickness of the sample, then using tap water and alcohol to clean the wire-cut sample; then preparing an etchant, dipping the solution by using a cotton swab, slightly wiping the observed part of a working area, etching for 3-4 seconds, sequentially flushing and drying by using clear water and alcohol, and observing the observed part by SEM+EBSD to obtain SEM images and EBSD images with grain boundaries, wherein the etchant is 10g of copper chloride+50 ml of absolute ethyl alcohol+50 ml of hydrochloric acid.
2. The sample preparation method of nickel-based powder superalloy in-situ sample micro-area observation sem+ebsd according to claim 1, wherein the sample preparation method is characterized by: the flat grinding and the water polishing are that firstly, a grinding machine is used for carrying out flat grinding on the sample plane, the roughness is less than or equal to 0.8, then, the flat grinding is carried out on a grinding machine, and then, polishing and the water polishing are carried out on a polishing machine with the thickness of 2.5 mu m and a polishing machine with the thickness of 1.5 mu m, so as to obtain a test block with a flat surface and no scratch.
3. The sample preparation method of nickel-based powder superalloy in-situ sample micro-area observation sem+ebsd according to claim 2, wherein the sample preparation method is characterized by: the sample grinding machine is used for grinding with 600-mesh, 800-mesh, 1000-mesh, 1200-mesh and 1500-mesh sand paper.
4. The sample preparation method of nickel-based powder superalloy in-situ sample micro-area observation sem+ebsd according to claim 1, wherein the sample preparation method is characterized by: the wire cutting current of the wire cutting slow-moving wire is less than or equal to 0.5mA.
5. The sample preparation method of nickel-based powder superalloy in-situ sample micro-area observation sem+ebsd according to claim 1, wherein the sample preparation method is characterized by: and the observation of SEM and EBSD is carried out by adopting a scanning electron microscope and a back scattering electron device to observe the observation part simultaneously.
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| CN110514683B (en) * | 2019-08-16 | 2022-05-13 | 西北工业大学 | Sample for capturing crack initiation of block material in mesoscopic scale and manufacturing method |
| CN113976888A (en) * | 2021-12-29 | 2022-01-28 | 中国航发北京航空材料研究院 | Preparation method of powder alloy disc with detectable inclusions, powder alloy disc and method for verifying the detectability of inclusions therein |
| CN115372135B (en) * | 2022-08-10 | 2023-06-16 | 国标（北京）检验认证有限公司 | Method for measuring rotation angle of high-temperature alloy crystal grain |
| CN115128109B (en) * | 2022-09-02 | 2022-11-25 | 北京化工大学 | EBSD sample stage based on orientation calibration and correction and image acquisition method |
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