CN111077004A - High-efficiency metallographic sample corrosion process for high-temperature-resistant alloy sample of gas turbine - Google Patents
High-efficiency metallographic sample corrosion process for high-temperature-resistant alloy sample of gas turbine Download PDFInfo
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- CN111077004A CN111077004A CN201911381905.7A CN201911381905A CN111077004A CN 111077004 A CN111077004 A CN 111077004A CN 201911381905 A CN201911381905 A CN 201911381905A CN 111077004 A CN111077004 A CN 111077004A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/32—Polishing; Etching
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Abstract
The invention discloses a high-efficiency metallographic specimen corrosion process for a high-temperature-resistant alloy specimen of a gas turbine, which comprises the steps of sampling and polishing metals, manufacturing the polished specimens into corresponding samples, polishing, corroding the metals by adopting a method combining electric corrosion and chemical corrosion, and detecting the corrosion surface of the metals.
Description
Technical Field
The invention relates to the field of metal detection, in particular to a high-efficiency metallographic specimen corrosion process for a high-temperature-resistant alloy specimen of a gas turbine.
Background
The metallographic examination is mainly to determine the three-dimensional space morphology of an alloy structure by adopting a quantitative metallographic principle and applying the measurement and calculation of a metallographic microstructure of a two-dimensional metallographic specimen ground surface or a film, thereby establishing the quantitative relation among alloy components, structures and performances.
Disclosure of Invention
The invention aims to solve the defects of the prior art, and provides a high-efficiency metallographic sample corrosion process for a high-temperature-resistant alloy sample of a gas turbine, so that the corrosion efficiency is improved, an oxalic acid solution can be recycled, and the metal corrosion effect is improved.
The technical scheme is that the high-efficiency metallographic specimen corrosion process for the high-temperature-resistant alloy specimen of the gas turbine comprises the following process steps:
a. sampling, namely intercepting a metal sample from target metal, polishing one surface of the metal sample by adopting coarse sand paper to flatten the cover surface, wherein the surface is a surface to be observed, and removing scraps;
b. preparing a sample: d, embedding and wrapping the sample polished in the step a by cold embedding or hot embedding, shaping and wrapping the sample by using a hot embedding equipment embedding cylinder or a cold embedding mould, placing and fixing the observation surface of the sample downwards at the bottom of the hot embedding cylinder or the cold embedding mould, pouring resin into the hot embedding cylinder or the cold embedding mould for fixing and shaping, and taking out the shaped sample;
c. polishing: b, grinding the sample in the step b, grinding and polishing one surface of the sample, which is provided with the metal sample, by using a metallographic sample grinding and polishing machine, grinding and polishing by using abrasive paper rotating along with an abrasive paper fixing disc on the grinding and polishing machine, and grinding the surface with the metal until the mesh number is 1150-plus-1200, wherein the metal surface is smooth and is mirror gloss;
d. and (3) corrosion: c, corroding the polished sample in the step C, putting the sample into 5% -15% oxalic acid solution, keeping the oxalic acid solution at 16-30 ℃, connecting a cathode of a 1-5V direct current power supply with the solution through a lead, putting the sample into the oxalic acid solution to enable the liquid to submerge the sample, connecting an anode of the 1-5V direct current power supply with a metal rod through a lead, pressing the metal rod on the metal sample on the sample, applying certain pressure to ensure that the metal rod is in close contact with the metal sample, and observing that the surface of the corroded sample has a mirror surface which is changed into a fog surface;
e. and (3) detection: according to the detection standard, the thickness of residual coating on the surface of a sample, the thickness of intergranular corrosion layer, grain boundary precipitation, carbide in crystal grains and the like are detected, a measuring tool is an Olympus GX51 optical microscope, and an experimenter compares a microstructure image seen by the microscope with a microstructure picture typical of metal and evaluates the microstructure picture to obtain the conclusion of the test.
Preferably, the cathode and the anode in the step d are made of metal copper, the lower end of the cathode is spiral, and the spiral part of the cathode is immersed in the solution.
Preferably, the metal in the step d can be corroded discontinuously, that is, the metal rod is continuously pressed to be far away from the metal surface, so that the surface of the corroded sample is observed, the mirror surface is changed into a fog surface, and different tissues are distinguished more obviously.
The high-efficiency metallographic sample corrosion process for the high-temperature-resistant alloy sample of the gas turbine, disclosed by the invention, has the beneficial effects that through the corrosion method in the step d, the same solution can be adopted to corrode various metals, the practicability of the process is improved, the corrosion efficiency is increased, the metal rod is pressed on the metal surface to be electrified and chemically corroded, so that different structures of the corrosion surface of the metal are more obviously distinguished, a corrosion area can meet the detection process requirement in the step e, the microstructure state is conveniently evaluated, the detection efficiency of the process is improved, the corrosion solution can be recycled, the waste of the solution is reduced, and the cost is further reduced.
Detailed Description
The technical content of the invention is explained in detail with reference to the following specific examples:
a high-efficiency metallographic specimen corrosion process for a high-temperature-resistant alloy specimen of a gas turbine comprises the following process steps:
a. sampling, namely cutting a sample from the high-temperature-resistant alloy of the gas turbine, polishing one surface of the metal sample by using coarse sand paper to flatten the cover surface, wherein the surface is a surface to be observed, and removing fragments;
b. preparing a sample: d, embedding and wrapping the sample polished in the step a by cold embedding or hot embedding, shaping and wrapping the sample by using a hot embedding equipment embedding cylinder or a cold embedding mould, placing and fixing the observation surface of the sample downwards at the bottom of the hot embedding cylinder or the cold embedding mould, pouring resin into the hot embedding cylinder or the cold embedding mould for fixing and shaping, and taking out the shaped sample;
c. polishing: b, grinding the sample in the step b, grinding and polishing one surface of the sample, which is provided with the metal sample, by using a metallographic sample grinding and polishing machine, grinding and polishing by using abrasive paper rotating along with an abrasive paper fixing disc on the grinding and polishing machine, and grinding the surface with the metal until the mesh number is 1150-plus-1200, wherein the metal surface is smooth and is mirror gloss;
d. and (3) corrosion: c, corroding the polished sample in the step C, putting the sample into 5% -15% oxalic acid solution, keeping the oxalic acid solution at 16-30 ℃, connecting a cathode of a 1-5V direct current power supply with the solution through a lead, putting the sample into the oxalic acid solution to enable the liquid to submerge the sample, connecting an anode of the 1-5V direct current power supply with a metal rod through a lead, pressing the metal rod on the metal sample on the sample, applying certain pressure to ensure that the metal rod is in close contact with the metal sample, and observing that the surface of the corroded sample has a mirror surface which is changed into a fog surface;
e. and (3) detection: according to the detection standard, the thickness of residual coating on the surface of a sample, the thickness of intergranular corrosion layer, grain boundary precipitation, carbide in crystal grains and the like are detected, a measuring tool is an Olympus GX51 optical microscope, and an experimenter compares a microstructure image seen by the microscope with a microstructure picture typical of metal and evaluates the microstructure picture to obtain the conclusion of the test.
The oxalic acid solution is prepared by dissolving solid oxalic acid in water, the cathode and the anode in the step d are made of metal copper, the lower end of the cathode is spiral, the spiral part at the lower end of the cathode is immersed in the solution, and a direct current power supply is arranged to work under a constant voltage state; and d, in the step d, metal corrosion can be performed discontinuously, namely, the metal rod is continuously pressed to be far away from the metal surface, so that the surface of a sample to be observed is changed into a fog surface from a mirror surface, and different tissues are distinguished more obviously.
In conclusion, by the corrosion method in the step d, multiple metals can be corroded by the same solution, the practicability of the process is improved, the corrosion efficiency is improved, the metal rod is pressed on the surface of the metal to be electrified and chemically corroded, different structures of the corrosion surface of the metal are distinguished more obviously, the corrosion area meets the detection process requirement in the step e, the microstructure state is conveniently evaluated, the detection efficiency of the process is improved, the corrosion solution can be recycled, the waste of the solution is reduced, and the cost is further reduced.
The above description is the preferred embodiment of the present invention, and the scope of the claims of the present invention should not be limited thereto. It should be noted that modifications and equivalents may be made to the technical solution of the present invention by those skilled in the art without departing from the scope of the present invention.
Claims (3)
1. The high-efficiency metallographic specimen corrosion process for the high-temperature-resistant alloy specimen of the gas turbine is characterized by comprising the following process steps of:
a. sampling, namely intercepting a metal sample from target metal, polishing one surface of the metal sample by adopting coarse sand paper to flatten the cover surface, wherein the surface is a surface to be observed, and removing scraps;
b. preparing a sample: d, embedding and wrapping the sample polished in the step a by cold embedding or hot embedding, shaping and wrapping the sample by using a hot embedding equipment embedding cylinder or a cold embedding mould, placing and fixing the observation surface of the sample downwards at the bottom of the hot embedding cylinder or the cold embedding mould, pouring resin into the hot embedding cylinder or the cold embedding mould for fixing and shaping, and taking out the shaped sample;
c. polishing: b, grinding the sample in the step b, grinding and polishing one surface of the sample, which is provided with the metal sample, by using a metallographic sample grinding and polishing machine, grinding and polishing by using abrasive paper rotating along with an abrasive paper fixing disc on the grinding and polishing machine, and grinding the surface with the metal until the mesh number is 1150-plus-1200, wherein the metal surface is smooth and is mirror gloss;
d. and (3) corrosion: c, corroding the polished sample in the step C, putting the sample into 5% -15% oxalic acid solution, keeping the oxalic acid solution at 16-30 ℃, connecting a cathode of a 1-5V direct current power supply with the solution through a lead, putting the sample into the oxalic acid solution to enable the liquid to submerge the sample, connecting an anode of the 1-5V direct current power supply with a metal rod through a lead, pressing the metal rod on the metal sample on the sample, applying certain pressure to ensure that the metal rod is in close contact with the metal sample, and observing that the surface of the corroded sample has a mirror surface which is changed into a fog surface;
e. and (3) detection: according to the detection standard, the thickness of the residual coating on the surface of the sample, the thickness of intergranular corrosion layer, grain boundary precipitates, carbides in crystal grains and the like are detected, the measuring tool is an optical microscope, and an experimenter compares a structure image seen by the microscope with a typical microstructure picture of metal and evaluates the structure picture to obtain the conclusion of the test.
2. The process for efficiently corroding the metallographic specimen of the high-temperature-resistant alloy specimen of the gas turbine as claimed in claim 1, wherein the cathode and the anode in the step d are made of copper metal, the lower end of the cathode is spiral, and the spiral part of the cathode is immersed in the solution.
3. The process for efficiently corroding the metallographic specimen of the high-temperature-resistant alloy specimen of the gas turbine as claimed in claim 1, wherein the metal corrosion in the step d can be performed discontinuously, that is, the metal rod is continuously pressed to be away from the metal surface, so that the surface of the corroded specimen is observed to have a mirror surface and is changed into a fog surface, and the different tissues are distinguished more obviously.
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| CN112255526A (en) * | 2020-09-09 | 2021-01-22 | 北京航天控制仪器研究所 | Preparation method and test method of copper-filled silicon through hole electromigration test structure |
| CN113138157A (en) * | 2021-04-08 | 2021-07-20 | 北京科技大学 | Nondestructive evaluation method for stress corrosion sensitivity of aluminum alloy extruded section |
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