CN113418770A - Electrolytic polishing solution for preparing molybdenum-rhenium alloy metallographic specimen and method thereof - Google Patents
Electrolytic polishing solution for preparing molybdenum-rhenium alloy metallographic specimen and method thereof Download PDFInfo
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- 238000005498 polishing Methods 0.000 title claims abstract description 137
- 229910000691 Re alloy Inorganic materials 0.000 title claims abstract description 43
- YUSUJSHEOICGOO-UHFFFAOYSA-N molybdenum rhenium Chemical compound [Mo].[Mo].[Re].[Re].[Re] YUSUJSHEOICGOO-UHFFFAOYSA-N 0.000 title claims abstract description 37
- 238000000034 method Methods 0.000 title claims abstract description 36
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 32
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 20
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 16
- 239000008367 deionised water Substances 0.000 claims abstract description 13
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 13
- 238000000227 grinding Methods 0.000 claims description 23
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 13
- 238000005520 cutting process Methods 0.000 claims description 10
- 239000004744 fabric Substances 0.000 claims description 10
- 244000137852 Petrea volubilis Species 0.000 claims description 7
- 239000003795 chemical substances by application Substances 0.000 claims description 7
- 229910003460 diamond Inorganic materials 0.000 claims description 7
- 239000010432 diamond Substances 0.000 claims description 7
- 239000000314 lubricant Substances 0.000 claims description 7
- 239000007921 spray Substances 0.000 claims description 7
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 6
- 238000004140 cleaning Methods 0.000 claims description 4
- 239000000243 solution Substances 0.000 abstract description 30
- 239000011259 mixed solution Substances 0.000 abstract description 8
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 abstract description 8
- 238000002360 preparation method Methods 0.000 abstract description 7
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 abstract description 6
- LELOWRISYMNNSU-UHFFFAOYSA-N hydrogen cyanide Chemical compound N#C LELOWRISYMNNSU-UHFFFAOYSA-N 0.000 abstract description 6
- 230000007797 corrosion Effects 0.000 abstract description 5
- 238000005260 corrosion Methods 0.000 abstract description 5
- 238000009776 industrial production Methods 0.000 abstract description 4
- 239000002253 acid Substances 0.000 abstract description 2
- 229910045601 alloy Inorganic materials 0.000 description 8
- 239000000956 alloy Substances 0.000 description 8
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 6
- 238000003760 magnetic stirring Methods 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 229910052750 molybdenum Inorganic materials 0.000 description 5
- 239000011733 molybdenum Substances 0.000 description 5
- 238000007517 polishing process Methods 0.000 description 5
- 238000005070 sampling Methods 0.000 description 5
- 239000007788 liquid Substances 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 230000003287 optical effect Effects 0.000 description 4
- 230000007547 defect Effects 0.000 description 2
- 235000019441 ethanol Nutrition 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 229910052702 rhenium Inorganic materials 0.000 description 2
- WUAPFZMCVAUBPE-UHFFFAOYSA-N rhenium atom Chemical compound [Re] WUAPFZMCVAUBPE-UHFFFAOYSA-N 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000006056 electrooxidation reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000009499 grossing Methods 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 238000005191 phase separation Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 229910000753 refractory alloy Inorganic materials 0.000 description 1
- 239000003870 refractory metal Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 229920001169 thermoplastic Polymers 0.000 description 1
- 239000004416 thermosoftening plastic Substances 0.000 description 1
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Classifications
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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
Abstract
The invention belongs to the technical field of metallographic sample preparation, and relates to an electrolytic polishing method for preparing a molybdenum-rhenium alloy metallographic sample. According to the invention, the metallographic specimen is prepared by adopting electrolytic polishing, and the mixed solution of sulfuric acid, phosphoric acid and deionized water is used as the electrolytic polishing solution, so that the use of acid corrosion samples with strong oxidizability and strong corrosivity such as hydrocyanic acid, hydrofluoric acid, perchloric acid and the like is avoided, and the potential safety hazard in the process of preparing the molybdenum-rhenium alloy metallographic specimen is reduced. The molybdenum-rhenium alloy metallographic specimen prepared by the method can observe clear and obvious metallographic microstructure, is more controllable in operation process and higher in efficiency, and is very suitable for industrial production.
Description
Technical Field
The invention relates to the technical field of metallographic sample preparation, in particular to an electrolytic polishing method for preparing a molybdenum-rhenium alloy metallographic sample.
Background
The molybdenum (Mo) has high melting point, small expansion coefficient, high electric conductivity and good thermal conductivity, and has good application prospect in important fields of metallurgy, agricultural electrical and chemical industry, aerospace and the like. However, since molybdenum atoms have a strong bonding force, the strength and hardness at both normal and high temperatures are particularly high, thereby limiting the workability and the range of applications to some extent. In the actual production process, a method of adding alloy elements is generally adopted to achieve the purpose of improving the plasticity of the molybdenum. The addition of rhenium (Re) to pure molybdenum can improve the strength of molybdenum and the plasticity to a great extent. Research shows that the molybdenum-rhenium alloy obtained by adding 35% of rhenium into molybdenum has the deformation amount reaching 90% at room temperature. The Mo-Re alloy has excellent high-temperature mechanical property, radiation resistance and ductility, so that the Mo-Re alloy is widely applied to high-tech fields such as aerospace, medical treatment, nuclear industry and the like. As a refractory alloy, the preparation and subsequent processing of the molybdenum-rhenium alloy are extremely complex, and the performance is very sensitive to the structural structure and composition segregation. In industrial production, the microstructure of the product is regulated and controlled by combining thermoplastic deformation with annealing treatment, so that the effect of improving the alloy performance is achieved. Therefore, there is a need for an adequate understanding and appreciation of the structure of the alloy during its manufacturing process. The metallographic detection is one of important means for analyzing the tissue structure of the material, and has great significance for guiding the production and processing of the molybdenum-rhenium alloy.
The preparation process of the conventional metallographic specimen comprises sampling, inlaying, grinding, polishing, corroding and the like, wherein the polishing and corroding steps are crucial to obtaining a metallographic structure. The metallographic structure of the alloy is usually subjected to chemical corrosion or electrochemical corrosion, the former usually adopts acidic mixed liquor containing hydrocyanic acid, hydrofluoric acid, nitric acid and the like with strong oxidizability and strong corrosiveness to corrode a polished metallographic sample, and the method has the defects of high corrosion speed, difficulty in controlling the process, low success rate, poor effect and the like, and can bring great potential safety hazards to the environment and the health of operators. The electrolytic polishing method can effectively overcome the defects, and the electrolytic polishing method has the advantages of simple equipment, convenience in operation and low cost, and is very suitable for being applied to industrial production. At present, for the electrolytic polishing of a refractory metal metallographic specimen such as a molybdenum-rhenium alloy, the adopted electrolyte is usually a mixed solution of perchloric acid and ethanol, but if the electrolytic process is not operated properly, the perchloric acid and ethanol solution has the risk of explosion. In addition, there is often a phase separation problem during electrolysis.
Disclosure of Invention
The invention aims to provide an electrolytic polishing method for preparing a molybdenum-rhenium alloy metallographic specimen, which is used for preparing the molybdenum-rhenium alloy metallographic specimen for metallographic analysis. The method disclosed by the invention can reduce the potential safety hazard in the polishing process of the molybdenum-rhenium alloy metallographic specimen and improve the display effect of the metallographic structure.
The invention realizes the aim through the following technical scheme:
an electrolytic polishing method for preparing a molybdenum-rhenium alloy metallographic specimen specifically comprises the step of adopting a special electrolytic polishing solution, wherein the electrolytic polishing solution is a mixed solution of sulfuric acid, phosphoric acid and deionized water.
The mass fraction concentration of the sulfuric acid is more than 95%.
The mass fraction concentration of the phosphoric acid is more than 85 percent.
The volume ratio of sulfuric acid to phosphoric acid to deionized water in the electrolytic polishing solution is (10-30): (40-60): (20-40).
An electrolytic polishing method for preparing a molybdenum-rhenium alloy metallographic specimen specifically comprises the following steps:
(1) cutting a sample: cutting the molybdenum-rhenium alloy plate into small blocky samples;
(2) grinding: carrying out coarse grinding and fine grinding on the small sample obtained in the step (1) by using abrasive paper;
(3) mechanical polishing: placing the sample finely ground in the step (2) on a polishing machine, and performing mechanical polishing treatment;
(4) electrolytic polishing: and (4) putting the mechanically polished sample obtained in the step (3) into an electrolytic polishing solution for electrolytic polishing treatment to obtain the molybdenum-rhenium alloy metallographic sample.
Preferably, in the step (2), the sample is ground by using metallographic sandpaper of W50, W28, W14, W10 and W5 in sequence; when the sample is ground, the sample is pushed in one direction by hand, and after the sand paper is replaced once, the sample is replaced by 90 degrees in the vertical direction until no cross scratch is formed.
Preferably, in the step (3), the rotation speed of the mechanical polishing disk is 600-.
Preferably, in the step (3), the polishing agent uses a diamond spray with the specification of W3.5, the polishing cloth is made of velvet cloth, and the lubricant is water.
Preferably, in the step (4), the polishing pool is provided with magnetic stirring to enable the polishing solution to flow, and the rotating speed is 80-120 rad/min;
preferably, in the step (4), the temperature of the electrolytic polishing solution is room temperature, the voltage of the electrolytic polishing is 5-20V, and the polishing time is 10-30 s.
Preferably, in the step (4), after the electrolytic polishing is finished, the sample is placed into absolute ethyl alcohol for ultrasonic cleaning for 5-10min, the sample is dried by a blower, and the sample is placed under a metallographic microscope for observing metallographic structures.
The invention has the beneficial effects that: due to the adoption of the technical scheme, the mixed solution of sulfuric acid, phosphoric acid and deionized water is adopted as the electrolytic polishing solution, the phosphoric acid is used as the main component of the polishing solution, the higher viscosity of the phosphoric acid is favorable for preferentially dissolving the convex part on the surface of the sample, the corrosion to the sample is lower, and the effect of smoothing the surface is achieved; the deionized water improves the dispersing capacity of the electrolytic polishing solution and improves the conductivity; the strong oxidizing and corrosive nature of sulfuric acid promotes dissolution of the sample surface, which is corroded out due to the irregular arrangement of grain atoms, which has a higher free energy than the grain boundaries. The method avoids using strong oxidizing and corrosive acids such as hydrocyanic acid, hydrofluoric acid, perchloric acid and the like, improves the safety of the metallographic sample preparation process, and has small harm to operators and environment. The molybdenum-rhenium alloy metallographic specimen prepared by the electrolytic polishing method improves the corrosion effect of the molybdenum-rhenium alloy structure, enables the process for preparing the molybdenum-rhenium alloy metallographic specimen to be more controllable and has higher efficiency, and is more suitable for being used in industrial production.
Drawings
FIG. 1 is a schematic view of metallographic structure observed under a metallographic microscope of a molybdenum-rhenium alloy metallographic specimen of example 1 after being treated by the electrolytic polishing solution of the invention.
FIG. 2 is a schematic view of metallographic structure observed under a metallographic microscope of a molybdenum-rhenium alloy metallographic specimen of example 2 after being treated by the electrolytic polishing solution of the present invention.
FIG. 3 is a schematic view of metallographic structure observed under a metallographic microscope of a molybdenum-rhenium alloy metallographic specimen of example 3 after being treated by the electrolytic polishing solution of the present invention.
FIG. 4 is a schematic view of metallographic structure observed under a metallographic microscope of a molybdenum-rhenium alloy metallographic specimen of example 4 after being treated by the electrolytic polishing solution of the present invention.
Detailed Description
The invention relates to an electrolytic polishing method for preparing a molybdenum-rhenium alloy metallographic specimen, which is further described by combining specific embodiments and drawings without limiting the invention.
The invention relates to an electrolytic polishing solution for preparing a molybdenum-rhenium alloy metallographic specimen, which comprises the following components in part by weight: sulfuric acid, phosphoric acid and deionized water; the volume ratio of sulfuric acid to phosphoric acid to deionized water in the electrolytic polishing solution is (10-30): 40-60): 20-40.
The invention relates to a method for preparing a molybdenum-rhenium alloy metallographic specimen by using the electrolytic polishing solution, which comprises the following steps:
s1) cutting: cutting the molybdenum-rhenium alloy plate into small blocky samples;
s2) grinding: carrying out coarse grinding and fine grinding on the small sample obtained in the step S1) by using abrasive paper;
s3) mechanical polishing: placing the sample finely ground in the step S2) on a polishing machine, and performing mechanical polishing treatment;
s4) electropolishing: and (4) placing the mechanically polished sample of S3) into an electrolytic polishing solution for electrolytic polishing treatment, and cleaning to obtain a molybdenum-rhenium alloy metallographic sample.
The process of coarse grinding and fine grinding of the sand paper in the step S2) comprises the following steps: and grinding the sample by using the metallographic abrasive paper of W50, W28, W14, W10 and W5 in sequence.
The rotation speed of the mechanical polishing in the S3) is 600- & lt1000 rad/min, and the polishing time is 5-10 min.
The polishing agent in the S3) is a diamond spray with the specification of W3.5, the polishing cloth is made of velvet cloth, and the lubricant is water.
The temperature of the electrolytic polishing solution in the step S4) is room temperature, the polishing tank is provided with magnetic stirring, and the polishing solution flows at a rotating speed of 80-120 rad/min.
The voltage of the electrolytic polishing in the step S4) is 5-20V, and the polishing time is 10-30S.
The cleaning process in the step S4) comprises the following steps: and (3) placing the sample into absolute ethyl alcohol for ultrasonic cleaning for 5-10min, drying the sample by using a blower, and placing the sample under a metallographic microscope to observe metallographic structures.
Example 1
The electrolytic polishing method for preparing the molybdenum-rhenium alloy metallographic specimen comprises the following steps:
(1) cutting a sample: sampling on a rolled Mo-47.5 wt% Re alloy plate, wherein the size of the sampled sample is 10mm multiplied by 5mm multiplied by 3 mm;
(2) grinding: sequentially grinding the sample by adopting W50, W28, W14, W10 and W5 metallographic abrasive paper; when the sample is ground, the sample is pushed in one direction by hand, and after the sand paper is replaced once, the sample is replaced by 90 degrees in the vertical direction to be continuously ground until no obvious scratch is formed.
(3) Mechanical polishing: and (3) carrying out mechanical polishing treatment on the ground sample, wherein the rotating speed of a mechanical polishing disk is 600rad/min, and the polishing time is 10 min. In the mechanical polishing process, water is used as a lubricant, the polishing cloth is made of velvet materials and matched with a W3.5 diamond spray to be used as a polishing agent, the surface of a sample is polished to be flat and bright, and no obvious cross scratch can be observed under an optical microscope of 200 times.
(4) Electrolytic polishing: a mixed solution of sulfuric acid, phosphoric acid and deionized water in a volume ratio of 1:5:4 is used as an electrolytic polishing solution, and the polishing solution flows at a rotation speed of 100rad/min by magnetic stirring in a polishing tank. And (3) putting the alloy sample after mechanical polishing into an electrolytic cell as an anode, wherein the temperature of electrolytic polishing liquid is room temperature, the voltage of electrolytic polishing is 15V, and the polishing time is 10 s. And after the electrolytic polishing is finished, putting the sample into absolute ethyl alcohol for ultrasonic cleaning for 10min, drying the sample by using a blower, and placing the sample under a metallographic microscope to observe metallographic structures. As shown in fig. 1, a clearly evident grain structure can be seen.
Example 2
The electrolytic polishing method for preparing the molybdenum-rhenium alloy metallographic specimen comprises the following steps:
(1) cutting a sample: sampling on a rolled Mo-47.5 wt% Re alloy plate, wherein the size of the sampled sample is 10mm multiplied by 5mm multiplied by 3 mm;
(2) grinding: sequentially grinding the sample by adopting W50, W28, W14, W10 and W5 metallographic abrasive paper; when the sample is ground, the sample is pushed in one direction by hand, and after the sand paper is replaced once, the sample is replaced by 90 degrees in the vertical direction to be continuously ground until no obvious scratch is formed.
(3) Mechanical polishing: and (3) carrying out mechanical polishing treatment on the ground sample, wherein the rotating speed of a mechanical polishing disk is 800rad/min, and the polishing time is 8 min. In the mechanical polishing process, water is used as a lubricant, the polishing cloth is made of velvet materials and matched with a W3.5 diamond spray to be used as a polishing agent, the surface of a sample is polished to be flat and bright, and no obvious cross scratch can be observed under an optical microscope of 200 times.
(4) Electrolytic polishing: a mixed solution of sulfuric acid, phosphoric acid and deionized water in a volume ratio of 2:5:3 is used as an electrolytic polishing solution, and the polishing solution flows at a rotation speed of 120rad/min by magnetic stirring in a polishing tank. And (3) putting the alloy sample after mechanical polishing into an electrolytic cell as an anode, wherein the temperature of electrolytic polishing liquid is room temperature, the voltage of electrolytic polishing is 10V, and the polishing time is 15 s. And after the electrolytic polishing is finished, putting the sample into absolute ethyl alcohol for ultrasonic cleaning for 5min, drying the sample by using a blower, and placing the sample under a metallographic microscope to observe metallographic structures. As shown in fig. 2, a clearly evident grain structure can be seen.
Example 3
The electrolytic polishing method for preparing the molybdenum-rhenium alloy metallographic specimen comprises the following steps:
(1) cutting a sample: sampling on a rolled Mo-47.5 wt% Re alloy plate, wherein the size of the sampled sample is 10mm multiplied by 5mm multiplied by 3 mm;
(2) grinding: sequentially grinding the sample by adopting W50, W28, W14, W10 and W5 metallographic abrasive paper; when the sample is ground, the sample is pushed in one direction by hand, and after the sand paper is replaced once, the sample is replaced by 90 degrees in the vertical direction to be continuously ground until no obvious scratch is formed.
(3) Mechanical polishing: and (3) carrying out mechanical polishing treatment on the ground sample, wherein the rotating speed of a mechanical polishing disk is 1000rad/min, and the polishing time is 5 min. In the mechanical polishing process, water is used as a lubricant, the polishing cloth is made of velvet materials and matched with a W3.5 diamond spray to be used as a polishing agent, the surface of a sample is polished to be flat and bright, and no obvious cross scratch can be observed under an optical microscope of 200 times.
(4) Electrolytic polishing: a mixed solution of sulfuric acid, phosphoric acid and deionized water in a volume ratio of 2:4:4 is used as an electrolytic polishing solution, and the polishing solution flows at a rotation speed of 110rad/min by magnetic stirring in a polishing tank. And (3) putting the alloy sample after mechanical polishing into an electrolytic cell as an anode, wherein the temperature of electrolytic polishing liquid is room temperature, the voltage of electrolytic polishing is 5V, and the polishing time is 30 s. And after the electrolytic polishing is finished, putting the sample into absolute ethyl alcohol for ultrasonic cleaning for 8min, drying the sample by using a blower, and placing the sample under a metallographic microscope to observe metallographic structures. As shown in fig. 3, a clearly evident grain structure can be seen.
Example 4
The electrolytic polishing method for preparing the molybdenum-rhenium alloy metallographic specimen comprises the following steps:
(1) cutting a sample: sampling on a rolled Mo-47.5 wt% Re alloy plate, wherein the size of the sampled sample is 10mm multiplied by 5mm multiplied by 3 mm;
(2) grinding: sequentially grinding the sample by adopting W50, W28, W14, W10 and W5 metallographic abrasive paper; when the sample is ground, the sample is pushed in one direction by hand, and after the sand paper is replaced once, the sample is replaced by 90 degrees in the vertical direction to be continuously ground until no obvious scratch is formed.
(3) Mechanical polishing: and (3) carrying out mechanical polishing treatment on the ground sample, wherein the rotating speed of a mechanical polishing disk is 900rad/min, and the polishing time is 7 min. In the mechanical polishing process, water is used as a lubricant, the polishing cloth is made of velvet materials and matched with a W3.5 diamond spray to be used as a polishing agent, the surface of a sample is polished to be flat and bright, and no obvious cross scratch can be observed under an optical microscope of 200 times.
(4) Electrolytic polishing: a mixed solution of sulfuric acid, phosphoric acid and deionized water in a volume ratio of 2:5:3 is used as an electrolytic polishing solution, and the polishing solution flows at a rotating speed of 80rad/min by magnetic stirring in a polishing tank. And (3) putting the alloy sample after mechanical polishing into an electrolytic cell as an anode, wherein the temperature of electrolytic polishing liquid is room temperature, the voltage of electrolytic polishing is 20V, and the polishing time is 10 s. And after the electrolytic polishing is finished, putting the sample into absolute ethyl alcohol for ultrasonic cleaning for 10min, drying the sample by using a blower, and placing the sample under a metallographic microscope to observe metallographic structures. As shown in fig. 4, a clearly evident grain structure can be seen.
The above description is a preferred embodiment of the present invention, and the present invention is not limited to the above description, but only to illustrate the detailed sample preparation process of the present invention, and the present invention is not limited to the above sample preparation process. It should be understood by those skilled in the art that any simple modification and content modification to the technology of the present invention can be made without departing from the technical scope of the present invention, and the technical scope of the present invention is covered.
Claims (9)
1. The electrolytic polishing solution for preparing the molybdenum-rhenium alloy metallographic specimen is characterized by comprising the following components in parts by weight: sulfuric acid, phosphoric acid and deionized water; the volume ratio of sulfuric acid to phosphoric acid to deionized water in the electrolytic polishing solution is (10-30): 40-60): 20-40.
2. The electrolytic polishing solution according to claim 1, wherein the concentration of the sulfuric acid is 95% or more; the concentration of the phosphoric acid is more than 85 percent.
3. A method for preparing a molybdenum-rhenium alloy metallographic specimen by using the electrolytic polishing solution as defined in claim 1, wherein the method comprises the following steps:
s1) cutting: cutting the molybdenum-rhenium alloy plate into small blocky samples;
s2) grinding: carrying out coarse grinding and fine grinding on the small sample obtained in the step S1) by using abrasive paper;
s3) mechanical polishing: placing the sample finely ground in the step S2) on a polishing machine, and performing mechanical polishing treatment;
s4) electropolishing: and (4) placing the mechanically polished sample of S3) into an electrolytic polishing solution for electrolytic polishing treatment, and cleaning to obtain a molybdenum-rhenium alloy metallographic sample.
4. The method as claimed in claim 3, wherein the process of coarse and fine grinding of the sand paper in S2) is as follows: and grinding the sample by using the metallographic abrasive paper of W50, W28, W14, W10 and W5 in sequence.
5. The method as claimed in claim 3, wherein the rotation speed of the mechanical polishing in S3) is 600-1000rad/min, and the polishing time is 5-10 min.
6. The method as claimed in claim 3, wherein the polishing agent in S3) is diamond spray with specification W3.5, the polishing cloth is velvet cloth, and the lubricant is water.
7. The method as claimed in claim 3, wherein the electropolishing solution in S4) is cooled to room temperature, and the polishing solution is stirred by magnetic force and flowed at a rotation speed of 80-120 rad/min.
8. The method as claimed in claim 3, wherein the electropolishing in S4) is performed at a voltage of 5-20V and for a polishing time of 10-30S.
9. The method as claimed in claim 3, wherein the cleaning in S4) comprises the following steps: and (3) placing the sample into absolute ethyl alcohol for ultrasonic cleaning for 5-10min, drying the sample by using a blower, and placing the sample under a metallographic microscope to observe metallographic structures.
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