CN114526978A - Metallographic corrosive liquid of vanadium alloy and preparation method of metallographic sample of vanadium alloy - Google Patents

Metallographic corrosive liquid of vanadium alloy and preparation method of metallographic sample of vanadium alloy Download PDF

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CN114526978A
CN114526978A CN202210175543.1A CN202210175543A CN114526978A CN 114526978 A CN114526978 A CN 114526978A CN 202210175543 A CN202210175543 A CN 202210175543A CN 114526978 A CN114526978 A CN 114526978A
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metallographic
vanadium alloy
alloy
polishing
acid
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CN114526978B (en
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曲凤盛
刘学
马如茹
王震宏
董鲜峰
陈道明
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Institute of Materials of CAEP
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/32Polishing; Etching
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/286Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/44Sample treatment involving radiation, e.g. heat
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/286Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
    • G01N2001/2866Grinding or homogeneising
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/20Recycling

Abstract

The invention provides a metallographic corrosive liquid of a vanadium alloy, which is prepared from 98.3% by mass of concentrated sulfuric acid, 68% by mass of concentrated nitric acid, 36.5% by mass of concentrated hydrochloric acid and distilled water. The metallographic corrosive liquid of the vanadium alloy is convenient to obtain, low in cost and easy to prepare, and the surface of the metallographic specimen of the vanadium alloy prepared by the method has a metal mirror surface effect, is free of scratches, continuous polishing and throwing points, an oxide layer, smooth, bright and clean in surface, clear in corrosion structure, high in grain boundary contrast, good in stability of a corrosion method, high in corrosion speed and high in corrosion efficiency.

Description

Metallographic corrosive liquid of vanadium alloy and preparation method of metallographic sample of vanadium alloy
Technical Field
The invention belongs to the technical field of metal surface treatment, and particularly relates to a metallographic corrosive liquid for a vanadium alloy and a preparation method of a metallographic sample of the vanadium alloy.
Background
The vanadium alloy has good high-temperature strength and plasticity, low irradiation activation, high thermal conductivity, low thermal expansion coefficient, high creep strength and good irradiation swelling resistance, so that the vanadium alloy is selected as a candidate first wall structure material of fusion energy, the mechanical property of the structure material is mainly determined by microstructure, and the development of the microstructure research of the vanadium alloy has great significance. At present, more techniques are used for observing the structure, such as SEM, TEM, EBSD and the like, but the metallographic phase is still one of the most important means for analyzing the structure. The method has the characteristics of direct observation, good macroscopic effect, more reaction information and the like. The vanadium alloy metallographic corrosive liquid disclosed at home and abroad at present comprises a mixed liquid of nitric acid, hydrofluoric acid and water and a mixed liquid of nitric acid, lactic acid and water, but both of the two types of metallographic corrosive liquids have the defect of low corrosion contrast, the vanadium alloy is mainly a quasi-single-phase alloy, and mainly has an aging precipitation phase except a matrix, so that the corrosion is difficult due to the composition, the crystal boundary is difficult to be clear, and the observation effect is influenced.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a metallographic etchant for vanadium alloy and a preparation method of a metallographic specimen of vanadium alloy, aiming at the defects of the prior art, the metallographic etchant for vanadium alloy is convenient to obtain, low in cost and easy to prepare, and the metallographic etchant for vanadium alloy prepared by the invention has the advantages of no scratch, continuous polishing and throwing, no oxide layer, smooth and bright and clean surface, clear corrosion structure, high grain boundary contrast, good stability of a corrosion method, high corrosion speed and high corrosion efficiency, and the surface of the metallographic specimen of vanadium alloy has a metal mirror effect.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows: a metallographic corrosive liquid of vanadium alloy is prepared from the following raw materials in percentage by volume: the material is prepared from the following raw materials in percentage by volume: 25-50% of concentrated sulfuric acid, 15-30% of concentrated nitric acid, 0.5-2% of concentrated hydrochloric acid and the balance of distilled water; the mass fraction of the concentrated sulfuric acid is 98.3%, the mass fraction of the concentrated nitric acid is 68%, and the mass fraction of the concentrated hydrochloric acid is 36.5%; the concentrated sulfuric acid, the concentrated nitric acid and the concentrated hydrochloric acid are analytically pure.
The invention also provides a method for preparing the vanadium alloy metallographic specimen by using the metallographic corrosive liquid for the vanadium alloy, which comprises the following steps:
s1, adopting an automatic metallographic grinder to perform rough grinding on the surface of the vanadium alloy sample by using 200-mesh, 400-mesh, 600-mesh and 800-mesh metallographic abrasive paper in sequence under the condition that the pressure is 15N-25N, stopping the rough grinding time of each type of metallographic abrasive paper in the rough grinding when the scratch of the previous type of metallographic abrasive paper cannot be seen by naked eyes, and then using 2000-mesh metallographic abrasive paper to perform final finish grinding under the same pressure condition to obtain a finish-ground alloy sample;
s2, pre-polishing the fine-ground alloy sample obtained in the step S1 by using a polishing agent through a mechanical polishing method under the condition that the pressure is 20N, and then performing mechanochemical polishing through a polishing solution to obtain an alloy sample to be corroded;
and S3, soaking the alloy sample to be corroded obtained in the step S2 in a metallographic corrosive liquid of the vanadium alloy at the temperature of 10-35 ℃ to corrode for 2-4 min, taking out the alloy sample, washing the alloy sample with clear water for 2-3 times, washing the alloy sample with absolute ethyl alcohol for 2-3 times, and drying the alloy sample to obtain the metallographic sample of the vanadium alloy.
Preferably, the refining time in S1 is 5min to 8 min.
Preferably, the polishing agent in S2 is a diamond spray polishing agent having a particle size of 2.5 to 5 μm.
Preferably, the polishing solution in S2 is a mixed solution of concentrated nitric acid, hydrofluoric acid and distilled water in a volume ratio of 1:0.5: 8; the mass fraction of the concentrated nitric acid is 68 percent; the mass fraction of the hydrofluoric acid is 40%; the concentrated nitric acid and the hydrofluoric acid are analytically pure.
Preferably, the pre-polishing time in S2 is 5min to 10 min.
Preferably, the time for the mechanochemical polishing in S2 is 5 min.
Compared with the prior art, the invention has the following advantages:
the metallographic corrosive liquid of the vanadium alloy is convenient to obtain, low in cost and easy to prepare, and the surface of the metallographic specimen of the vanadium alloy prepared by the method has a metal mirror surface effect, is free of scratches, continuous polishing and throwing points, free of an oxide layer, smooth, bright and clean in surface, clear in corrosion structure, high in grain boundary contrast, good in stability of a corrosion method, high in corrosion speed and high in corrosion efficiency.
The present invention will be described in further detail with reference to the accompanying drawings and examples.
Drawings
FIG. 1 is a metallographic specimen of a vanadium alloy according to example 1 of the present invention.
FIG. 2 is a metallographic specimen of a vanadium alloy according to example 2 of the present invention.
FIG. 3 is a metallographic specimen of a vanadium alloy according to example 3 of the present invention.
Detailed Description
Example 1
The metallographic corrosive liquid of the vanadium alloy is prepared from the following raw materials in percentage by volume: 50% of concentrated sulfuric acid, 30% of concentrated nitric acid, 2% of concentrated hydrochloric acid and the balance of distilled water; the mass fraction of the concentrated sulfuric acid is 98.3%, the mass fraction of the concentrated nitric acid is 68%, and the mass fraction of the concentrated hydrochloric acid is 36.5%; the concentrated sulfuric acid, the concentrated nitric acid and the concentrated hydrochloric acid are analytically pure.
The embodiment also provides a method for preparing the vanadium alloy metallographic specimen by using the metallographic corrosive liquid for the vanadium alloy, which comprises the following steps:
s1, under the condition that the pressure is 25N, using metallographic abrasive paper with the models of 200 meshes, 400 meshes, 600 meshes and 800 meshes to perform rough grinding on the surface of the vanadium alloy sample in sequence, stopping the rough grinding time of each metallographic abrasive paper in the rough grinding when the scratch of the previous metallographic abrasive paper cannot be seen by naked eyes, and then performing fine grinding for 8min by using the metallographic abrasive paper with the model of 2000 meshes under the same pressure condition to obtain a fine-ground alloy sample; the vanadium alloy sample is a V-5Cr-5Ti alloy;
s2, pre-polishing the fine-ground alloy sample obtained in the S1 for 7.5min by using a diamond spray polishing agent with the granularity of 2.5-5 microns by using a mechanical polishing method under the condition that the pressure is 20N, and then performing mechanical chemical polishing for 5min by using polishing liquid to obtain an alloy sample to be corroded; the polishing solution is a mixed solution of concentrated nitric acid, hydrofluoric acid and distilled water in a volume ratio of 1:0.5: 8; the mass fraction of the concentrated nitric acid is 68 percent; the mass fraction of the hydrofluoric acid is 40%; the concentrated nitric acid and the hydrofluoric acid are analytically pure;
and S3, soaking the alloy sample to be corroded obtained in the step S2 in a metallographic corrosive liquid of the vanadium alloy at the temperature of 22 ℃ to corrode for 3min, taking out the alloy sample, washing the alloy sample with clear water for 3 times, washing the alloy sample with absolute ethyl alcohol for 3 times, and drying the alloy sample to be corroded to obtain the metallographic sample of the vanadium alloy.
FIG. 1 is a metallographic graph of a metallographic specimen of a vanadium alloy according to the example, and it can be seen that a matrix structure (indicated by an arrow a in the figure) and a precipitated phase (indicated by an arrow b in the figure) of the metallographic specimen of the vanadium alloy are clearly shown.
The metallographic corrosive liquid of the vanadium alloy of the embodiment is convenient to obtain, low in cost and easy to prepare, the surface of the metallographic specimen of the vanadium alloy prepared by the embodiment has a metal mirror effect, no scratch, no oxide layer, smooth, bright and clean surface, clear corrosion structure, high grain boundary contrast, good stability of a corrosion method, high corrosion speed and high corrosion efficiency, and is continuously polished and thrown away.
Example 2
The metallographic corrosive liquid of the vanadium alloy is prepared from the following raw materials in percentage by volume: 25% of concentrated sulfuric acid, 15% of concentrated nitric acid, 0.5% of concentrated hydrochloric acid and the balance of distilled water; the mass fraction of the concentrated sulfuric acid is 98.3%, the mass fraction of the concentrated nitric acid is 68%, and the mass fraction of the concentrated hydrochloric acid is 36.5%; the concentrated sulfuric acid, the concentrated nitric acid and the concentrated hydrochloric acid are analytically pure.
The embodiment also provides a method for preparing the vanadium alloy metallographic specimen by using the metallographic corrosive liquid for the vanadium alloy, which comprises the following steps:
s1, under the condition that the pressure is 15N, using metallographic abrasive paper with the models of 200 meshes, 400 meshes, 600 meshes and 800 meshes to perform rough grinding on the surface of the vanadium alloy sample in sequence, stopping the rough grinding time of each metallographic abrasive paper in the rough grinding when the scratch of the previous metallographic abrasive paper cannot be seen by naked eyes, and then performing fine grinding for 5min by using the metallographic abrasive paper with the model of 2000 meshes under the same pressure condition to obtain a fine-ground alloy sample; the vanadium alloy sample is a V-4Cr-4Ti alloy;
s2, pre-polishing the fine-ground alloy sample obtained in S1 for 10min by using a diamond spray polishing agent with the granularity of 2.5-5 mu m by using a mechanical polishing method under the condition that the pressure is 20N, and then performing mechanical chemical polishing for 5min by using polishing liquid to obtain an alloy sample to be corroded; the polishing solution is a mixed solution of concentrated nitric acid, hydrofluoric acid and distilled water in a volume ratio of 1:0.5: 8; the mass fraction of the concentrated nitric acid is 68 percent; the mass fraction of the hydrofluoric acid is 40%; the concentrated nitric acid and the hydrofluoric acid are analytically pure;
and S3, soaking the alloy sample to be corroded obtained in the step S2 in a metallographic corrosive liquid of the vanadium alloy at the temperature of 35 ℃ to corrode for 2min, taking out the alloy sample, washing the alloy sample with clear water for 2 times, washing the alloy sample with absolute ethyl alcohol for 2 times, and drying the alloy sample to be corroded to obtain the metallographic sample of the vanadium alloy.
FIG. 2 is a gold phase diagram of a metallographic specimen of a vanadium alloy according to the present embodiment, in which a V-4Cr-4Ti alloy is a high-purity electrolytic dendritic vanadium, and thus the vanadium alloy has fewer precipitated phases but still can be seen clearly; as can be seen from the figure, the matrix structure (indicated by arrow a in the figure) and the precipitation phase (indicated by arrow b in the figure) of the metallographic specimen of the vanadium alloy are clearly shown.
The metallographic corrosive liquid of the vanadium alloy of the embodiment is convenient to obtain, low in cost and easy to prepare, the surface of the metallographic specimen of the vanadium alloy prepared by the embodiment has a metal mirror effect, no scratch, no oxide layer, smooth, bright and clean surface, clear corrosion structure, high crystal boundary contrast, good stability of a corrosion method, high corrosion speed and high corrosion efficiency, and is continuously polished and thrown away.
Example 3
The metallographic corrosive liquid of the vanadium alloy is prepared from the following raw materials in percentage by volume: 30% of concentrated sulfuric acid, 20% of concentrated nitric acid, 1% of concentrated hydrochloric acid and the balance of distilled water; the mass fraction of the concentrated sulfuric acid is 98.3%, the mass fraction of the concentrated nitric acid is 68%, and the mass fraction of the concentrated hydrochloric acid is 36.5%; the concentrated sulfuric acid, the concentrated nitric acid and the concentrated hydrochloric acid are analytically pure.
The embodiment also provides a method for preparing the vanadium alloy metallographic specimen by using the metallographic corrosive liquid for the vanadium alloy, which comprises the following steps:
s1, under the condition that the pressure is 25N, using metallographic abrasive paper with the models of 200 meshes, 400 meshes, 600 meshes and 800 meshes to perform rough grinding on the surface of the vanadium alloy sample in sequence, stopping the rough grinding time of each metallographic abrasive paper in the rough grinding when the scratch of the previous metallographic abrasive paper cannot be seen by naked eyes, and then performing fine grinding for 8min by using the metallographic abrasive paper with the model of 2000 meshes under the same pressure condition to obtain a fine-ground alloy sample; the vanadium alloy sample is a V-5Cr-15Ti alloy, and C is added into the V-5Cr-15Ti alloy;
s2, spraying a polishing agent by using diamond with the grain size of 2.5-5 mu m by adopting a mechanical polishing method under the condition that the pressure is 20N; pre-polishing the fine-ground alloy sample obtained in the step S1 for 10min, and then performing mechanochemical polishing on the fine-ground alloy sample by using a polishing solution for 5min to obtain an alloy sample to be corroded; the polishing solution is a mixed solution of concentrated nitric acid, hydrofluoric acid and distilled water in a volume ratio of 1:0.5: 8; the mass fraction of the concentrated nitric acid is 68 percent; the mass fraction of the hydrofluoric acid is 40%; the concentrated nitric acid and the hydrofluoric acid are analytically pure;
and S3, soaking the alloy sample to be corroded obtained in the step S2 in a metallographic corrosive liquid of the vanadium alloy at the temperature of 10 ℃ to corrode for 4min, taking out the alloy sample, washing the alloy sample with clear water for 3 times, washing the alloy sample with absolute ethyl alcohol for 3 times, and drying the alloy sample to be corroded to obtain the metallographic sample of the vanadium alloy.
FIG. 3 is a metallographic graph of a metallographic specimen of a vanadium alloy according to the example, and it can be seen that a matrix structure (indicated by an arrow a in the figure) and a precipitated phase (indicated by an arrow b in the figure) of the metallographic specimen of the vanadium alloy are clearly shown.
The metallographic corrosive liquid of the vanadium alloy of the embodiment is convenient to obtain, low in cost and easy to prepare, the surface of the metallographic specimen of the vanadium alloy prepared by the embodiment has a metal mirror effect, no scratch, no oxide layer, smooth, bright and clean surface, clear corrosion structure, high crystal boundary contrast, good stability of a corrosion method, high corrosion speed and high corrosion efficiency, and is continuously polished and thrown away.
The above description is only for the preferred embodiment of the present invention, and is not intended to limit the present invention in any way. Any simple modification, change and equivalent changes of the above embodiments according to the technical essence of the invention are still within the protection scope of the technical solution of the invention.

Claims (7)

1. The metallographic corrosive liquid of the vanadium alloy is characterized by being prepared from the following raw materials in percentage by volume: the material is prepared from the following raw materials in percentage by volume: 25-50% of concentrated sulfuric acid, 15-30% of concentrated nitric acid, 0.5-2% of concentrated hydrochloric acid and the balance of distilled water; the mass fraction of the concentrated sulfuric acid is 98.3%, the mass fraction of the concentrated nitric acid is 68%, and the mass fraction of the concentrated hydrochloric acid is 36.5%; the concentrated sulfuric acid, the concentrated nitric acid and the concentrated hydrochloric acid are analytically pure.
2. The method for preparing the metallographic specimen of the vanadium alloy by using the metallographic corrosive liquid of the vanadium alloy as described in claim 1, which is characterized by comprising the following steps:
s1, adopting an automatic metallographic grinder to perform rough grinding on the surface of the vanadium alloy sample by using 200-mesh, 400-mesh, 600-mesh and 800-mesh metallographic abrasive paper in sequence under the condition that the pressure is 15N-25N, stopping the rough grinding time of each type of metallographic abrasive paper in the rough grinding when the scratch of the previous type of metallographic abrasive paper cannot be seen by naked eyes, and then using 2000-mesh metallographic abrasive paper to perform final finish grinding under the same pressure condition to obtain a finish-ground alloy sample;
s2, pre-polishing the fine-ground alloy sample obtained in the step S1 by using a polishing agent through a mechanical polishing method under the condition that the pressure is 20N, and then performing mechanochemical polishing through a polishing solution to obtain an alloy sample to be corroded;
s3, soaking the alloy sample to be corroded obtained in the step S2 in a metallographic corrosive solution of the vanadium alloy at the temperature of 10-35 ℃ to corrode for 2-4 min, taking out the alloy sample, washing the alloy sample with clear water for 2-3 times, washing the alloy sample with absolute ethyl alcohol for 2-3 times, and drying the alloy sample to obtain the metallographic sample of the vanadium alloy.
3. The method according to claim 2, wherein the refining time in S1 is 5min to 8 min.
4. The method of claim 2, wherein the polishing slurry of S2 is a diamond spray polishing slurry having a particle size of 2.5 μm to 5 μm.
5. The method according to claim 2, wherein the polishing solution in S2 is a mixed solution of concentrated nitric acid, hydrofluoric acid and distilled water in a volume ratio of 1:0.5: 8; the mass fraction of the concentrated nitric acid is 68 percent; the mass fraction of the hydrofluoric acid is 40%; the concentrated nitric acid and the hydrofluoric acid are analytically pure.
6. The method of claim 2, wherein the pre-polishing time in S2 is 5min to 10 min.
7. The method of claim 2, wherein the mechanochemical polishing in S2 is performed for 5 min.
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