CN116145225A - Electrolytic corrosion method for appearance of IN718 nickel-based superalloy crystal grain - Google Patents
Electrolytic corrosion method for appearance of IN718 nickel-based superalloy crystal grain Download PDFInfo
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- 238000005260 corrosion Methods 0.000 title claims abstract description 53
- 230000007797 corrosion Effects 0.000 title claims abstract description 53
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 44
- 238000000034 method Methods 0.000 title claims abstract description 37
- 229910000601 superalloy Inorganic materials 0.000 title claims abstract description 26
- 239000013078 crystal Substances 0.000 title claims abstract description 23
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 22
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims abstract description 57
- 238000005498 polishing Methods 0.000 claims abstract description 23
- 235000006408 oxalic acid Nutrition 0.000 claims abstract description 19
- 238000004140 cleaning Methods 0.000 claims abstract description 14
- 239000008151 electrolyte solution Substances 0.000 claims abstract description 12
- 238000001035 drying Methods 0.000 claims abstract description 8
- 238000000691 measurement method Methods 0.000 claims abstract description 5
- 239000002184 metal Substances 0.000 claims abstract description 5
- 229910052751 metal Inorganic materials 0.000 claims abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 239000008367 deionised water Substances 0.000 claims description 9
- 229910021641 deionized water Inorganic materials 0.000 claims description 9
- 238000011010 flushing procedure Methods 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 238000005868 electrolysis reaction Methods 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 6
- 239000000243 solution Substances 0.000 claims description 5
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 4
- 238000005520 cutting process Methods 0.000 claims description 4
- 238000000227 grinding Methods 0.000 claims description 4
- 229910017604 nitric acid Inorganic materials 0.000 claims description 4
- 229920000742 Cotton Polymers 0.000 claims description 3
- 235000009161 Espostoa lanata Nutrition 0.000 claims description 3
- 240000001624 Espostoa lanata Species 0.000 claims description 3
- 239000011521 glass Substances 0.000 claims description 3
- 230000003287 optical effect Effects 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 239000004576 sand Substances 0.000 claims 2
- 238000005406 washing Methods 0.000 claims 2
- 239000000126 substance Substances 0.000 abstract description 10
- 230000008569 process Effects 0.000 abstract description 8
- 239000003518 caustics Substances 0.000 abstract description 4
- 239000000463 material Substances 0.000 description 5
- 244000137852 Petrea volubilis Species 0.000 description 4
- 230000008901 benefit Effects 0.000 description 4
- 230000009471 action Effects 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 238000005242 forging Methods 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 229910021578 Iron(III) chloride Inorganic materials 0.000 description 1
- 238000012356 Product development Methods 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 238000005275 alloying Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 210000002345 respiratory system Anatomy 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25F—PROCESSES FOR THE ELECTROLYTIC REMOVAL OF MATERIALS FROM OBJECTS; APPARATUS THEREFOR
- C25F3/00—Electrolytic etching or polishing
- C25F3/02—Etching
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
- G01N15/02—Investigating particle size or size distribution
- G01N15/0205—Investigating particle size or size distribution by optical means
- G01N15/0227—Investigating particle size or size distribution by optical means using imaging; using holography
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/84—Systems specially adapted for particular applications
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Abstract
The invention discloses an electrolytic corrosion method for showing the appearance of IN718 nickel-based superalloy crystal grains, belongs to the technical field of metallographic electrolytic polishing corrosion, and particularly relates to an electrolytic corrosion method for showing the appearance of IN718 nickel-based superalloy crystal grains. The invention aims to solve the problems that the traditional chemical corrosion process can not accurately display grain boundaries, and the corrosive agent has short effective time and low success rate. The method comprises the following steps: 1. intercepting an IN718 nickel-based superalloy sample, and mechanically polishing and cleaning to obtain a bright and clean metallographic sample; 2. preparing oxalic acid electrolytic solution; 3. putting the metallographic sample into oxalic acid electrolytic solution for electrolytic corrosion to obtain an electrolytic corrosion sample; 4. cleaning and drying the surface of the electrolytic corrosion sample to obtain an observation sample; 5. the sample was subjected to microscopic observation, and the sample grain size was calculated using a metal average grain size measurement method. The method is used for electrolytic corrosion of the appearance of the IN718 nickel-based superalloy crystal grain.
Description
Technical Field
The invention belongs to the technical field of metallographic electrolytic polishing corrosion, and particularly relates to an electrolytic corrosion method for showing the morphology of IN718 nickel-based superalloy crystal grains.
Background
IN718 nickel-base superalloy as a forging material for various stationary and rotating parts IN aircraft engines and industrial gas turbines; because the workpiece is in long-term service under the high-temperature condition, the workpiece has extremely high requirements on various performance indexes; the structure and performance of the alloy are extremely sensitive to the hot working process, so the quality stability of the material has become a key technology for normal mass production and safety application of the engine. The material has the greatest advantages that various metallurgical products and forgings with different grain sizes and sizes reflecting different performance levels can be obtained by adjusting the thermal deformation process parameters, and then various parts meeting different application requirements in an engine are manufactured, so that the application field of the material is continuously expanded, and the use amount is increasingly increased. Therefore, the detection of the microscopic grain size of the material is one of important key indexes.
Because the IN718 nickel-based alloy material belongs to a precipitation strengthening nickel-based deformation superalloy, the alloying degree is high, the structure morphology is complex and changeable, and it is very difficult to show clear and complete grain boundary lines (grain boundaries) by using a common corrosion method without showing twins. The occurrence of twin crystals affects the evaluation of grain size, which has become a major challenge in the laboratory. Therefore, a new corrosion method is urgently needed to be developed to accurately show the grain morphology, and meanwhile, the accuracy of grain size measurement results can be guaranteed, so that theoretical basis is provided for field process improvement and product development, and the technical requirements of enterprises for developing new products are met.
Disclosure of Invention
The invention aims to solve the problems that the traditional chemical corrosion process can not accurately display grain boundaries, the effective time of the corrosive is short and the success rate is low, and provides an electrolytic corrosion method for displaying the appearance of IN718 nickel-based superalloy grains.
The electrolytic corrosion method for showing the appearance of the IN718 nickel-based superalloy crystal grain specifically comprises the following steps:
1. cutting an IN718 nickel-based superalloy sample, grinding, polishing and cleaning to obtain a bright and clean metallographic specimen;
2. preparing oxalic acid electrolytic solution;
3. placing the bright and clean metallographic sample into oxalic acid electrolytic solution for electrolytic corrosion to obtain an electrolytic corrosion sample;
4. cleaning and drying the surface of the electrolytic corrosion sample to obtain an observation sample;
5. the observation sample was subjected to microscopic observation, and the sample grain size was calculated using a metal average grain size measurement method.
The invention has the beneficial effects that:
the metallographic sample prepared by the method can obtain clear crystal grain morphology, simultaneously reduce or eliminate twin crystals, accurately measure the grain size of the sample and facilitate the grain size grading.
The invention has the advantages of simple implementation, high success rate, safety, cost reduction, synergy, high detection efficiency, accurate assessment result and the like. The prepared electrolyte has long effective time and is easy to store. The invention is also suitable for detecting the grain size of other nickel-based superalloy.
Drawings
FIG. 1 is a photograph of a 200-fold metallographic structure obtained with a conventional chemical etchant;
FIG. 2 is a photograph of a 500-fold metallographic structure obtained by a conventional chemical etchant;
FIG. 3 is a photograph of a 200-fold metallographic structure obtained using the method described in example one;
FIG. 4 is a photograph of a 500-fold metallographic structure obtained using the method described in example one.
Detailed Description
The first embodiment is as follows: the electrolytic corrosion method for showing the morphology of the IN718 nickel-based superalloy crystal grain IN the embodiment is specifically carried out according to the following steps:
1. cutting an IN718 nickel-based superalloy sample, grinding, polishing and cleaning to obtain a bright and clean metallographic specimen;
2. preparing oxalic acid electrolytic solution;
3. placing the bright and clean metallographic sample into oxalic acid electrolytic solution for electrolytic corrosion to obtain an electrolytic corrosion sample;
4. cleaning and drying the surface of the electrolytic corrosion sample to obtain an observation sample;
5. the observation sample was subjected to microscopic observation, and the sample grain size was calculated using a metal average grain size measurement method.
The second embodiment is as follows: the first difference between this embodiment and the specific embodiment is that: the length of the bright and clean metallographic specimen is 15-20 mm, and the width is 10-15 mm. The other is the same as in the first embodiment.
And a third specific embodiment: the first difference between this embodiment and the specific embodiment is that: the polishing and polishing sequentially comprises coarse sand paper polishing, fine sand paper polishing, coarse flannelette polishing, fine flannelette polishing, clear water flushing and alcohol wiping. The other is the same as in the first embodiment.
The specific embodiment IV is as follows: the first difference between this embodiment and the specific embodiment is that: and step two, adding oxalic acid particles into deionized water, and stirring by using a glass rod until the oxalic acid particles are completely dissolved to obtain the oxalic acid electrolytic solution with the concentration of 7-9%. The other is the same as in the first embodiment.
Fifth embodiment: the first difference between this embodiment and the specific embodiment is that: parameters of electrolytic corrosion: the working voltage is 1.5V-2.0V, the electrolysis current is 4A-6A, and the electrolysis time is 5 min-7 min. The other is the same as in the first embodiment.
Specific embodiment six: the first difference between this embodiment and the specific embodiment is that: and step four, cleaning sequentially comprises the steps of flushing with deionized water, wiping with absorbent cotton balls dipped in a dilute nitric acid solution with the concentration of 23% -27%, flushing with deionized water and wiping with alcohol. The other is the same as in the first embodiment.
The purpose of this embodiment is to wipe the electrolytic corrosion product from the sample surface clean.
Seventh embodiment: the first difference between this embodiment and the specific embodiment is that: and step four, drying the sample by adopting a blower. The other is the same as in the first embodiment.
Eighth embodiment: the first difference between this embodiment and the specific embodiment is that: and fifthly, observing the tissue by adopting a 200-500 times optical microscope. The other is the same as in the first embodiment.
The following examples are used to verify the benefits of the present invention:
embodiment one: the electrolytic corrosion method for showing the appearance of the IN718 nickel-based superalloy crystal grain is specifically carried out according to the following steps:
1. cutting an IN718 nickel-based superalloy sample with the thickness of 25mm multiplied by 15mm, grinding, polishing and cleaning to obtain a bright and clean metallographic specimen; the polishing and cleaning steps comprise coarse sand paper polishing, fine sand paper polishing, coarse flannelette polishing, fine flannelette polishing, clear water flushing and alcohol wiping in sequence;
2. adding 9g of oxalic acid particles into 100mL of deionized water, and stirring by using a glass rod until the oxalic acid particles are completely dissolved to obtain oxalic acid electrolytic solution;
3. placing the bright and clean metallographic sample into oxalic acid electrolytic solution for electrolytic corrosion to obtain an electrolytic corrosion sample; parameters of the electrolytic corrosion: the working voltage is 1.8V, the electrolysis current is 5A, and the electrolysis time is 6min;
4. cleaning and drying the surface of the electrolytic corrosion sample to obtain an observation sample; the cleaning is sequentially carried out by adopting deionized water for flushing, adopting absorbent cotton balls to dip dilute nitric acid solution with the concentration of 23% -27% for wiping, adopting deionized water for flushing and adopting alcohol for wiping;
5. the observation samples were respectively placed on a 100-500-fold optical microscope for tissue observation, a 200-fold enlarged metallographic photograph is shown in fig. 3, a 500-fold enlarged photograph is shown in fig. 4, and the grain size of the samples was calculated using a metal average grain size measurement method.
Embodiment two: metallographic structure samples prepared by using a traditional chemical corrosion method;
the chemical corrosion reagents are: experiments were performed using 5ml HNO3, 200ml HCl and 65g FeCl3 in the etching solution, and finally a 200-fold photograph of the metallographic structure was obtained as shown in FIG. 1, and a 500-fold photograph of the metallographic structure was shown in FIG. 2.
The metallographic structure obtained by the traditional chemical corrosive agent has the advantages that the whole color of an image is darkened to influence the observation, the grain boundary is not completely displayed, a large number of twin crystals appear, the twin crystals seriously interfere the evaluation of the grain, the corrosion is uneven in the corrosion process, the success rate is low, the storage effective time of the corrosive agent is short, the strong pungent smell is associated, and the human respiratory system is influenced when the chemical corrosive agent is used for a long time.
The metallographic structure obtained by the electrolytic corrosion mode has high overall saturation of the image color, brightness and definition, basically, clearly and completely show crystal grains, clean matrix, no twin crystals, obvious sample corrosion effect, and more environment-friendly use process, and meanwhile, the electrolyte is a dilute oxalic acid solution with little influence on human bodies.
The electrolytic corrosion method is a chemical dissolution process under the action of an electric field, and is characterized in that the atomic arrangement at the grain boundary is disordered, the energy is higher, the grains are easy to erode to form grooves, and the positions of the atoms are different and the erosion degree is different, so that the reflection of the parts into the light rays is different under the irradiation of vertical light rays, and the grains with different grain boundaries are shown as dark. Under the action of an external power supply, the micro-current low voltage can accelerate grain boundary corrosion, the boundary between grains can be quickly displayed within a certain time, the matrix can still be kept bright, and meanwhile, the twin crystal can be inhibited or reduced, compared with the electrolytic corrosion method, the electrolytic corrosion method is obviously superior to the chemical corrosion method.
Claims (8)
1. The electrolytic corrosion method for showing the appearance of the IN718 nickel-based superalloy crystal grain is characterized by comprising the following steps of:
1. cutting an IN718 nickel-based superalloy sample, grinding, polishing and cleaning to obtain a bright and clean metallographic specimen;
2. preparing oxalic acid electrolytic solution;
3. placing the bright and clean metallographic sample into oxalic acid electrolytic solution for electrolytic corrosion to obtain an electrolytic corrosion sample;
4. cleaning and drying the surface of the electrolytic corrosion sample to obtain an observation sample;
5. the observation sample was subjected to microscopic observation, and the sample grain size was calculated using a metal average grain size measurement method.
2. The electrolytic corrosion method for developing the morphology of IN718 nickel-base superalloy crystal grains according to claim 1, wherein the bright and clean metallographic specimen IN the step one has a length of 15-20 mm and a width of 10-15 mm.
3. The electrolytic corrosion method for developing the morphology of the IN718 nickel-based superalloy crystal grain according to claim 1, wherein the polishing IN the step one is sequentially coarse sand polishing, fine sand polishing, coarse flannelette polishing, fine flannelette polishing, clear water flushing and alcohol wiping.
4. The electrolytic corrosion method for showing the morphology of IN718 nickel-based superalloy crystal grains according to claim 1, wherein IN the second step, oxalic acid particles are added into deionized water, and a glass rod is adopted to stir until the oxalic acid particles are completely dissolved, so that an oxalic acid electrolytic solution with the concentration of 7% -9% is obtained.
5. An electrolytic corrosion method for developing morphology of IN718 nickel-base superalloy grains according to claim 1 wherein step three is defined by: the working voltage is 1.5V-2.0V, the electrolysis current is 4A-6A, and the electrolysis time is 5 min-7 min.
6. The electrolytic corrosion method for showing the morphology of the IN718 nickel-based superalloy crystal grain according to claim 1, wherein the cleaning IN the fourth step is sequentially washing with deionized water, wiping with absorbent cotton balls dipped IN a dilute nitric acid solution with a concentration of 23% -27%, washing with deionized water, and wiping with alcohol.
7. The electrolytic corrosion method for developing the morphology of an IN718 nickel-base superalloy grain according to claim 1, wherein the step four of drying is drying the sample with a blower.
8. The electrolytic corrosion method for appearance of IN718 nickel-base superalloy crystal grain morphology according to claim 1, wherein IN step five the observation of the structure is performed by using a 100-500 times optical microscope.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211690145.XA CN116145225A (en) | 2022-12-27 | 2022-12-27 | Electrolytic corrosion method for appearance of IN718 nickel-based superalloy crystal grain |
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| CN202211690145.XA CN116145225A (en) | 2022-12-27 | 2022-12-27 | Electrolytic corrosion method for appearance of IN718 nickel-based superalloy crystal grain |
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