CN117783184A - Method for comprehensively representing microstructure change before and after cutting of nickel-based powder superalloy - Google Patents
Method for comprehensively representing microstructure change before and after cutting of nickel-based powder superalloy Download PDFInfo
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 124
- 239000000843 powder Substances 0.000 title claims abstract description 85
- 238000005520 cutting process Methods 0.000 title claims abstract description 81
- 229910000601 superalloy Inorganic materials 0.000 title claims abstract description 78
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 62
- 238000000034 method Methods 0.000 title claims abstract description 32
- 230000008859 change Effects 0.000 title claims description 18
- 230000007797 corrosion Effects 0.000 claims abstract description 65
- 238000005260 corrosion Methods 0.000 claims abstract description 65
- 238000005498 polishing Methods 0.000 claims abstract description 29
- 238000000227 grinding Methods 0.000 claims abstract description 13
- 239000000126 substance Substances 0.000 claims abstract description 9
- 238000012512 characterization method Methods 0.000 claims abstract description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- 239000008367 deionised water Substances 0.000 claims description 13
- 229910021641 deionized water Inorganic materials 0.000 claims description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 10
- 239000003795 chemical substances by application Substances 0.000 claims description 10
- 229910003460 diamond Inorganic materials 0.000 claims description 10
- 239000010432 diamond Substances 0.000 claims description 10
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 6
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 claims description 6
- 238000005530 etching Methods 0.000 claims description 6
- 229910017604 nitric acid Inorganic materials 0.000 claims description 6
- 244000137852 Petrea volubilis Species 0.000 claims description 5
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 5
- 229940117975 chromium trioxide Drugs 0.000 claims description 5
- WGLPBDUCMAPZCE-UHFFFAOYSA-N chromium trioxide Inorganic materials O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 claims description 5
- GAMDZJFZMJECOS-UHFFFAOYSA-N chromium(6+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Cr+6] GAMDZJFZMJECOS-UHFFFAOYSA-N 0.000 claims description 5
- 238000004140 cleaning Methods 0.000 claims description 5
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 4
- 229910000040 hydrogen fluoride Inorganic materials 0.000 claims description 4
- 238000000866 electrolytic etching Methods 0.000 claims description 3
- 238000007517 polishing process Methods 0.000 claims description 2
- 231100001010 corrosive Toxicity 0.000 abstract description 25
- 238000012545 processing Methods 0.000 abstract description 14
- 239000003518 caustics Substances 0.000 abstract description 10
- 239000000463 material Substances 0.000 description 18
- 101000912561 Bos taurus Fibrinogen gamma-B chain Proteins 0.000 description 10
- 230000008569 process Effects 0.000 description 10
- 239000011159 matrix material Substances 0.000 description 9
- 239000000956 alloy Substances 0.000 description 7
- 239000007788 liquid Substances 0.000 description 7
- 229910045601 alloy Inorganic materials 0.000 description 6
- 239000010410 layer Substances 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- 238000005728 strengthening Methods 0.000 description 5
- 230000009471 action Effects 0.000 description 3
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- 238000005516 engineering process Methods 0.000 description 3
- 239000007800 oxidant agent Substances 0.000 description 3
- 239000002244 precipitate Substances 0.000 description 3
- 239000002344 surface layer Substances 0.000 description 3
- 230000002378 acidificating effect Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- KRVSOGSZCMJSLX-UHFFFAOYSA-L chromic acid Substances O[Cr](O)(=O)=O KRVSOGSZCMJSLX-UHFFFAOYSA-L 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 238000001125 extrusion Methods 0.000 description 2
- AWJWCTOOIBYHON-UHFFFAOYSA-N furo[3,4-b]pyrazine-5,7-dione Chemical compound C1=CN=C2C(=O)OC(=O)C2=N1 AWJWCTOOIBYHON-UHFFFAOYSA-N 0.000 description 2
- 238000001513 hot isostatic pressing Methods 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
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- 229910021591 Copper(I) chloride Inorganic materials 0.000 description 1
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- 230000002411 adverse Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
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- 238000007596 consolidation process Methods 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- OXBLHERUFWYNTN-UHFFFAOYSA-M copper(I) chloride Chemical compound [Cu]Cl OXBLHERUFWYNTN-UHFFFAOYSA-M 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
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Abstract
The invention discloses a method for comprehensively representing microstructure changes before and after cutting of nickel-based powder superalloy, which comprises the following steps: grinding and polishing the nickel-based powder superalloy before and after cutting respectively; respectively carrying out chemical corrosion, electrolytic corrosion and chemical corrosion on the sample piece after grinding and polishing by adopting a corrosive A, an electrolytic corrosive B and a corrosive C; microscopic observation is carried out on the corroded sample piece, gamma phase, gamma' phase and PPB images before and after cutting of the nickel-based powder superalloy are obtained, and meanwhile, comprehensive characterization of microstructure morphology before and after cutting of the nickel-based powder superalloy is achieved by means of image analysis software; by providing different corrosives, the invention can successfully observe the changes of gamma phase, gamma' phase and PPB of the nickel-based powder superalloy FGH96 before and after cutting processing, and realize comprehensive characterization of microstructure changes of the nickel-based powder superalloy before and after cutting processing.
Description
Technical Field
The invention relates to the technical field of nickel-based superalloy metallographic corrosion, in particular to a method for comprehensively representing microstructure changes before and after cutting of nickel-based powder superalloy.
Background
The powder superalloy is a high-temperature alloy produced and prepared by a powder metallurgy process, and is subjected to the technological processes of prealloy powder preparation, powder consolidation, post-treatment and the like, so that the powder superalloy can work for a long time at the high temperature of 600 ℃ and above under the action of certain stress, and has the advantages of fine powder particles, uniform alloy structure, high mechanical property of the material, high reliability and the like. The microstructure of the powder is composed of a matrix phase gamma phase and a strengthening phase gamma ' phase, the quantity and the size of the gamma ' phases have great influence on the material in the precipitation strengthening powder high-temperature alloy material, and the larger the size of the gamma ' phase (smaller than the critical size), the better the strengthening effect and the higher the alloy strength (the opposite effect when exceeding the critical size). The primary grain boundary (PPB) is one of three defects in powder superalloys, and refers to a layer of second phase continuous web film which is different from the matrix plasticity and is precipitated at the primary powder grain boundary during powder preparation and during initial heating of hot isostatic pressing, and the layer of precipitates is believed to prevent diffusion bonding among powder grains during hot isostatic pressing, and stress concentration is generated in the layer of precipitates under the action of stress, so that the layer of precipitates becomes a potential crack source and a crack propagation channel in the alloy, and has adverse effects on the performance of the alloy.
Metal cutting is an important means of achieving certain geometric and surface integrity requirements, and is the most common machining method in the manufacturing industry. In the material removal process, due to complex processes such as extrusion, shearing, friction and the like occurring between a cutter and a workpiece, serious plastic deformation occurs on the surface layer and the subsurface layer of the workpiece, the microstructure of the material evolves under the action of a thermo-mechanical load, and the microstructure evolution of the surface layer and the subsurface layer of the material caused by cutting processing has a critical decisive effect on the final use performance of the part, so that the research on the microstructure evolution process of the material in the cutting processing process has been paid attention to by various students.
There have been some successful cases for nickel-base powder superalloy microstructure observations, which also include those in which nickel-base powder superalloys have been successfully observed. However, the specific corrosion effects of the different corrosion schemes are not clearly shown in these schemes at present, nor are the different corrosion schemes laterally compared. Regarding observation schemes for changes in the nickel-based powder superalloy PPB, it is generally known that the kaling reagent: 5g CuCl 2 +100ml HCl+10ml CH 3 CH 2 OH was examined, but it was found that PPB was rarely developed through practical operation, and observation of PPB changes before and after cutting was not mentioned.
Disclosure of Invention
Aiming at the problems existing in the prior art, the invention provides a method for comprehensively representing the microstructure change of the nickel-based powder superalloy before and after cutting, and by providing different corrosives, the change of gamma phase, gamma' phase and PPB of the nickel-based powder superalloy FGH96 before and after cutting can be successfully observed, so that the comprehensive representation of the microstructure change of the nickel-based powder superalloy before and after cutting is realized.
The technical scheme of the invention is as follows:
in a first aspect of the invention, there is provided a method for comprehensively characterizing microstructure changes of a nickel-based powder superalloy before and after cutting, comprising the steps of:
grinding and polishing the nickel-based powder superalloy before and after cutting respectively;
respectively carrying out chemical corrosion, electrolytic corrosion and chemical corrosion on the sample piece after grinding and polishing by adopting a corrosive A, an electrolytic corrosive B and a corrosive C;
and (3) microscopic observation is carried out on the corroded sample piece to obtain gamma phase, gamma' phase and PPB images before and after cutting of the nickel-based powder superalloy, and meanwhile, comprehensive characterization of microstructure morphology before and after cutting of the nickel-based powder superalloy is achieved by means of image analysis software.
In the embodiment, various corrosion schemes are used for corroding the nickel-based powder superalloy, and the aim of comprehensively characterizing microstructure changes (including gamma phase, gamma' phase and PPB) before and after cutting processing of the nickel-based powder superalloy is fulfilled by observing the nickel-based powder superalloy by means of a confocal microscope and a Scanning Electron Microscope (SEM) technology.
One or more of the technical schemes of the invention has the following beneficial effects:
(1) The method for comprehensively representing the microstructure change before and after cutting of the nickel-based powder superalloy can help more researchers to study the microstructure of the nickel-based powder superalloy. Through the technical scheme, the change conditions of gamma and gamma' phases, the size and shape of the material PPB and the like before and after the cutting processing of the nickel-based powder superalloy can be comprehensively and multi-angle observed, a researcher is helped to comprehensively describe the microscopic characteristics of the nickel-based powder superalloy, the observation efficiency and the observation accuracy are greatly improved, and meanwhile, the deep research on the microscopic structure evolution rule in the cutting processing process of the nickel-based powder superalloy is also helped.
(2) The invention aims at the changes of gamma phase, gamma 'phase and PPB in the microstructure before and after the cutting processing of the nickel-based powder superalloy, uses different types of corrosive liquids for corrosion, and observes by means of a confocal microscope and a Scanning Electron Microscope (SEM) technology to achieve the aim of comprehensively characterizing the changes of the microstructure (comprising gamma phase, gamma' phase and PPB) before and after the cutting processing of the nickel-based powder superalloy.
(3) According to the corrosion solution A, the electrolytic corrosion solution B and the corrosion solution C provided by the invention, after the corrosion of the corrosion solution to the nickel-based powder superalloy is found through practical verification, the changes of gamma phase, gamma' phase and PPB of the nickel-based powder superalloy before and after cutting processing can be successfully observed, and the corrosion results of the corrosion solution A and the electrolytic corrosion solution B used in the observation scheme are opposite.
(4) After microstructure observation data are collected, the microstructure change condition can be quantitatively and comprehensively characterized by further using Image analysis software Image Pro Plus or Image J, and meanwhile, the used corrosive liquid has better corrosion control capability.
Drawings
FIG. 1 is a flow chart of a method for comprehensively characterizing microstructure changes before and after cutting of a nickel-based powder superalloy provided by the invention;
FIG. 2 is a graph showing the corrosion comparison of the nickel-base powder superalloy before and after cutting after corrosion using corrosive agent A in example 1 of the present invention;
FIG. 3 is a graph showing the corrosion comparison of the nickel-base powder superalloy before and after cutting after corrosion using electrolytic corrosive B in example 1 of the present invention;
FIG. 4 is a graph comparing corrosion results of example 1 of the present invention on nickel-based powder superalloy FGH96 using corrosive A and electrolytic corrosive B;
FIG. 5 is a graph showing the corrosion comparison of the nickel-base powder superalloy before and after cutting after corrosion using corrosive liquid C in example 1 of the present invention;
fig. 6 is an image of the gamma prime phase and PPB before and after cutting of the nickel-base powder superalloy obtained in example 1 of the present invention, after post-treatment with Fiji software.
Detailed Description
The invention will be further described with reference to the drawings and examples.
A method for comprehensively characterizing microstructure changes before and after cutting of nickel-based powder superalloy comprises the following steps:
grinding and polishing the nickel-based powder superalloy before and after cutting respectively;
respectively carrying out chemical corrosion, electrolytic corrosion and chemical corrosion on the sample piece after grinding and polishing by adopting a corrosive A, an electrolytic corrosive B and a corrosive C;
and (3) microscopic observation is carried out on the corroded sample piece to obtain gamma phase, gamma' phase and PPB images before and after cutting of the nickel-based powder superalloy, and meanwhile, comprehensive characterization of microstructure morphology before and after cutting of the nickel-based powder superalloy is achieved by means of image analysis software.
Specifically, different corrosive liquids are used for the nickel-based powder superalloy material, the change condition of microstructure before and after cutting is observed from different angles in all aspects, after corrosion is completed and observation is finished, confocal and SEM observation results are collected, images are processed and measured by means of Image analysis software Image-Pro Plus or Image J, the morphology of microstructure structure of the material before and after cutting is obtained, comparison is carried out, and the morphology and the size change of PPB are measured.
In some embodiments of the invention, the lapping and polishing process comprises first mechanically lapping with 1000-3000 mesh sand paper, then rough polishing with 2.5-0.5 μm diamond polish, and finish polishing with 0.25 μm diamond polish until the surface of the sample is polished to a mirror surface free of scratches.
In some embodiments of the present invention, the etchant A comprises 1.4-1.6 g of anhydrous copper chloride, 28-35 ml of concentrated hydrochloric acid, 28-35 ml of anhydrous ethanol, and 28-35 ml of deionized water, wherein the purity of the anhydrous copper chloride is 98%, and the mass fraction of the concentrated hydrochloric acid is 37%.
In some embodiments of the invention, the etching is performed with etchant A for a period of 28-33 seconds at a temperature of 20-25 ℃.
The corrosive liquid A provides an acidic environment, can carry out metallographic corrosion more quickly, and is added with Cu 2+ As an oxidizing agent, the dissolution of elements such as Fe, mo and the like can be promoted.
In some embodiments of the invention, the electrolytic etchant B comprises 3-5 g of chromium trioxide, 160-180 ml of concentrated phosphoric acid and 8-12 ml of concentrated hydrochloric acid, wherein the purity of the chromium trioxide is 99%, the mass fraction of the concentrated phosphoric acid is 85%, and the mass fraction of the concentrated hydrochloric acid is 37%.
The acid electrolysis environment is provided in the corrosive liquid B to accelerate the electrolytic corrosion process, chromic acid formed by dissolving chromium trioxide serving as a strong oxidant in water is also an oxidant, and the chromic acid can be reduced in the electrolytic process, so that elements in a nickel-based powder superalloy matrix phase are corroded more quickly, and the distribution and the morphology of a strengthening phase are clearly seen.
In some embodiments of the present invention, the electrolytic etching using electrolytic etchant B comprises: and (3) taking the sample to be corroded as an anode, carrying out electrolytic corrosion on the sample by using an electrolytic polishing corrosion instrument through using an electrolytic corrosion agent B, controlling the voltage to be 6V, carrying out electrolytic corrosion for 15-20 s at the corrosion temperature of 20-25 ℃, and cleaning and wiping the surface by using deionized water and absolute ethyl alcohol after the corrosion is finished.
In some embodiments of the invention, the etchant C comprises 2.5-3.5 ml hydrogen fluoride, 4.5-6 ml concentrated nitric acid, and 92ml deionized water, wherein the concentrated hydrogen fluoride has a purity of 99% and the concentrated nitric acid has a mass fraction of 65%.
The corrosive agent C provides an acidic environment, nitric acid reacts on elements such as Fe, cr and the like, and meanwhile, the contained F-permeability and coordination capacity are strong, so that the corrosive agent C is easy to coordinate with high-valence ions, thereby accelerating the effective corrosion of the nickel-based powder superalloy and showing the matrix phase distribution and morphology of the nickel-based powder superalloy.
In some embodiments of the invention, the etching is performed with etchant C for a period of time ranging from 65 to 75 seconds and at a temperature ranging from 20 to 25 ℃.
In some embodiments of the present invention, the etched sample is cleaned and wiped with deionized water and absolute ethanol, respectively, prior to microscopic observation of the etched sample.
In some embodiments of the invention, the gamma phase and gamma' phase changes before and after cutting of the nickel-based powder superalloy are observed by a scanning electron microscope, and the changes in the PPB before and after cutting of the nickel-based powder superalloy are observed by a confocal microscope.
Example 1
In an exemplary embodiment of the present invention, a method for comprehensively characterizing microstructure changes before and after cutting of a nickel-based powder superalloy is provided, and as shown in fig. 1, the method is divided into three parts: the first part is the comparison observation before and after cutting the gamma phase, the second part is the comparison observation before and after cutting the gamma 'phase, the third part is the comparison observation before and after cutting the PPB material, the corrosion observation is carried out by taking FGH96 as an example in the embodiment, the main components of FGH96 are shown in table 1, and according to the related study, elements such as Ti, nb and the like in the FGH96 alloy are mainly distributed in the gamma' phase, and elements such as Cr, co and the like are mainly distributed in the matrix phase.
TABLE 1 FGH96 chemical composition
1. The specific operation steps of the comparison observation before and after gamma phase cutting are as follows:
(1) Cutting the FGH96 matrix and the cut FGH96 material into a sample with a certain size by a wire;
(2) After two sample pieces are inlaid, sequentially using 1000-mesh, 1500-mesh, 2000-mesh, 2500-mesh and 3000-mesh sand paper for mechanical grinding, and finally, respectively using 0.5 mu m diamond polishing agent for rough polishing and 0.25 mu m diamond polishing agent for fine polishing until the surface of the sample piece is polished until no scratches exist on the surface of the sample piece;
(3) Preparing an etchant A:1.5g of anhydrous copper chloride+33 ml of HCl+33ml of absolute ethyl alcohol+33 ml of deionized water, wherein the purity of the anhydrous copper chloride is 98%, and the mass fraction of concentrated hydrochloric acid is 37%;
(4) And (3) corroding the FGH96 sample by using a corrosive agent A for 28-33s at the temperature of 25 ℃, and cleaning and wiping the surface by using deionized water and absolute ethyl alcohol after the corrosion is finished.
After etching with etchant a, SEM observation shows that etchant a can etch the gamma ' phase, and the remainder is gamma phase, and etching before and after cutting is performed on the gamma ' phase, such as shown in fig. 2, where holes of different sizes are gamma ' phases of different sizes, and the remainder is gamma phase. Therefore, in summary, the corrosion scheme can successfully compare the change condition of gamma phase before and after cutting of the nickel-based powder superalloy FGH 96.
2. The specific operation steps for comparison observation before and after gamma' phase cutting are as follows:
(1) Cutting the FGH96 matrix and the cut FGH96 material into a sample with a certain size by a wire;
(2) After two sample pieces are inlaid, sequentially using 1000-mesh, 1500-mesh, 2000-mesh, 2500-mesh and 3000-mesh sand paper for mechanical grinding, and finally, respectively using 0.5 mu m diamond polishing agent for rough polishing and 0.25 mu m diamond polishing agent for fine polishing until the surface of the sample piece is polished until no scratches exist on the surface of the sample piece;
(3) Manufacturing the polished sample into an electrode by using a cold mosaic technology;
(4) Preparing an electrolytic corrosive agent B: 3-5 g CrO 3 +160～180ml H 3 PO 4 +8 to 12ml of HCl, wherein CrO 3 The purity of (2) is 99%, the mass fraction of the concentrated phosphoric acid is 85%, and the mass fraction of the concentrated hydrochloric acid is 37%;
(5) And (3) using an EP-06 type electrolytic polishing corrosion instrument to take a sample to be corroded as an anode, using an electrolytic corrosive agent B to carry out electrolytic corrosion on the FGH96 sample, controlling the voltage to be 6V, carrying out electrolytic corrosion for 15-20 s at the corrosion temperature of 25 ℃, and respectively using deionized water and absolute ethyl alcohol to clean and wipe the surface after the corrosion is finished.
After electrolytic etching using electrolytic etchant B, it was found that gamma phase was etched and residual gamma 'phase was etched, and as shown in FIG. 3, gamma' phases of different sizes were clearly seen from the drawing, gamma 'phases of the material before cutting were uniformly distributed in the material, and deformation such as elongation, extrusion and partial phase transformation were generated in gamma' phases of the surface layer after cutting. Therefore, in summary, the corrosion scheme can successfully compare the change condition of gamma' phase before and after cutting of the nickel-based powder superalloy FGH 96.
The comparison of the corrosion results of the corrosive A and the electrolytic corrosive B on the nickel-based powder superalloy FGH96 is shown in FIG. 4, and the corrosion results of the corrosive A and the electrolytic corrosive B are clearly proved to be opposite from the graph, so that the change conditions of gamma and gamma' phases before and after the cutting process of the nickel-based powder superalloy can be complementarily verified.
3. The specific operation steps for comparison observation before and after PPB cutting are as follows:
the specific operation steps for comparison observation before and after PPB cutting are as follows:
(1) Cutting the FGH96 matrix and the cut FGH96 material into a sample with a certain size by a wire;
(2) After two sample pieces are inlaid, sequentially using 1000-mesh, 1500-mesh, 2000-mesh, 2500-mesh and 3000-mesh sand paper for mechanical grinding, and finally, respectively using 0.5 mu m diamond polishing agent for rough polishing and 0.25 mu m diamond polishing agent for fine polishing until the surface of the sample piece is polished until no scratches exist on the surface of the sample piece;
(3) Preparing corrosive agent C:3ml HF+5ml HNO 3 +92ml deionized water, wherein the purity of the concentrated HF is 99% and the mass fraction of the concentrated nitric acid is 65%;
(4) And (3) corroding the FGH96 sample by using a corrosive agent C for 65-75s at the temperature of 25 ℃, and cleaning and wiping the surface by using deionized water and absolute ethyl alcohol after the corrosion is finished.
The change of the PPB in the nickel-based powder superalloy before and after cutting can be clearly found by using a confocal microscope after corrosion by using the corrosive liquid C, and corrosion pairs before and after cutting are shown in fig. 5, for example, the distribution of PPB with different sizes in the material before cutting can be seen from the graph, the deformation of the PPB is larger when the material PPB is deformed after cutting and is closer to the processing surface, and the dissolution of the PPB occurs when the surface is processed. Therefore, in summary, the corrosion scheme can successfully compare the change condition of the PPB before and after cutting of the nickel-based powder superalloy FGH 96.
The obtained gamma' phase and PPB images before and after cutting the nickel-based powder superalloy are subjected to post-treatment by adopting Fiji software, as shown in FIG. 6, the morphology of a matrix phase, a strengthening phase and PPB can be observed more clearly, and quantitative characterization data can be obtained.
The characterization method for the microstructure change before and after the cutting processing of the nickel-based powder superalloy provided by the invention can comprehensively and multi-angle observe the change conditions of gamma and gamma' phases, the size and shape of a material PPB and the like before and after the cutting processing of the nickel-based powder superalloy, helps researchers to comprehensively describe the microstructure characteristics of the nickel-based powder superalloy more quickly, greatly improves the observation efficiency and the observation accuracy, and is also beneficial to deep study on the microstructure evolution rule in the cutting processing process of the nickel-based powder superalloy.
While the foregoing description of the embodiments of the present invention has been presented in conjunction with the drawings, it should be understood that it is not intended to limit the scope of the invention, but rather, it is intended to cover all modifications or variations within the scope of the invention as defined by the claims of the present invention.
Claims (10)
1. The method for comprehensively characterizing the microstructure change before and after cutting of the nickel-based powder superalloy is characterized by comprising the following steps:
grinding and polishing the nickel-based powder superalloy before and after cutting respectively;
respectively carrying out chemical corrosion, electrolytic corrosion and chemical corrosion on the sample piece after grinding and polishing by adopting a corrosive A, an electrolytic corrosive B and a corrosive C;
and (3) microscopic observation is carried out on the corroded sample piece to obtain gamma phase, gamma' phase and PPB images before and after cutting of the nickel-based powder superalloy, and meanwhile, comprehensive characterization of microstructure morphology before and after cutting of the nickel-based powder superalloy is achieved by means of image analysis software.
2. The method for comprehensively characterizing microstructure variation before and after cutting of nickel-base powder superalloy according to claim 1, wherein the grinding and polishing process comprises the steps of mechanically grinding by using 1000-3000 mesh sand paper, coarse polishing by using 2.5-0.5 μm diamond polishing agent, and fine polishing by using 0.25 μm diamond polishing agent until the surface of a sample is polished until the surface of the sample has no scratches.
3. The method for comprehensively characterizing microstructure variations of a nickel-base powder superalloy before and after cutting as recited in claim 1, wherein the etchant a comprises: 1.4-1.6 g of anhydrous copper chloride, 28-35 ml of concentrated hydrochloric acid, 28-35 ml of anhydrous ethanol and 28-35 ml of deionized water, wherein the purity of the anhydrous copper chloride is 98%, and the mass fraction of the concentrated hydrochloric acid is 37%.
4. The method for comprehensively characterizing microstructure variations before and after cutting of a nickel-base powder superalloy according to claim 1, wherein the etching is performed with an etchant A for 28-33s at 20-25deg.C.
5. The method for comprehensively characterizing microstructure variations of a nickel-base powder superalloy before and after cutting as recited in claim 1, wherein the electrolytic etchant B comprises: 3-5 g of chromium trioxide, 160-180 ml of concentrated phosphoric acid and 8-12 ml of concentrated hydrochloric acid, wherein the purity of the chromium trioxide is 99%, the mass fraction of the concentrated phosphoric acid is 85%, and the mass fraction of the concentrated hydrochloric acid is 37%.
6. The method for comprehensively characterizing microstructure variations of a nickel-base powder superalloy before and after cutting as recited in claim 1, wherein the electrolytic etching with electrolytic etchant B comprises: and (3) taking the sample to be corroded as an anode, carrying out electrolytic corrosion on the sample by using an electrolytic polishing corrosion instrument through using an electrolytic corrosion agent B, controlling the voltage to be 6V, carrying out electrolytic corrosion for 15-20 s at the corrosion temperature of 20-25 ℃, and cleaning and wiping the surface by using deionized water and absolute ethyl alcohol after the corrosion is finished.
7. The method for comprehensively characterizing microstructure variations of a nickel-base powder superalloy before and after cutting as recited in claim 1, wherein the etchant C comprises: 2.5-3.5 ml of hydrogen fluoride, 4.5-6 ml of concentrated nitric acid and 92ml of deionized water, wherein the purity of the concentrated hydrogen fluoride is 99%, and the mass fraction of the concentrated nitric acid is 65%.
8. The method for comprehensively characterizing microstructure variations of a nickel-base powder superalloy before and after cutting as recited in claim 1, wherein the etching is performed with an etchant C for 65-75s at 20-25 ℃.
9. The method for comprehensively characterizing microstructure variations of a nickel-based powder superalloy before and after cutting according to claim 1, wherein deionized water and absolute ethyl alcohol are used for cleaning and wiping the surface of the corroded sample piece before microscopic observation is carried out on the corroded sample piece.
10. The method for comprehensively characterizing microstructure changes before and after cutting of the nickel-based powder superalloy according to claim 1, wherein the gamma phase and gamma' phase changes before and after cutting of the nickel-based powder superalloy are observed by a scanning electron microscope, and the changes of the PPB before and after cutting of the nickel-based powder superalloy are observed by a confocal microscope.
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