CN111707513B - Preparation method of NiV alloy metallographic specimen - Google Patents

Preparation method of NiV alloy metallographic specimen Download PDF

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CN111707513B
CN111707513B CN202010555893.1A CN202010555893A CN111707513B CN 111707513 B CN111707513 B CN 111707513B CN 202010555893 A CN202010555893 A CN 202010555893A CN 111707513 B CN111707513 B CN 111707513B
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nitric acid
sample
electrolytic polishing
abrasive paper
metallographic
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CN111707513A (en
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姚力军
潘杰
边逸军
王学泽
龚润泽
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Ningbo Jiangfeng Electronic Material Co Ltd
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Ningbo Jiangfeng Electronic Material Co Ltd
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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
    • G01N1/286Preparing 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
    • G01N1/32Polishing; Etching

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  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
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  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
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  • Pathology (AREA)
  • Sampling And Sample Adjustment (AREA)
  • Investigating And Analyzing Materials By Characteristic Methods (AREA)

Abstract

The invention discloses a preparation method of a NiV alloy metallographic specimen. The preparation method of the NiV alloy metallographic specimen comprises the following steps: 1) Cutting: cutting a NiV alloy material into small blocks; 2) Grinding: coarse grinding and fine grinding are carried out on the small sample obtained in the step 1); 3) Electrolytic polishing: carrying out electrolytic polishing treatment on the sample ground in the step 2); 4) And (3) corrosion: and 3) carrying out corrosion treatment on the sample subjected to the electrolytic polishing treatment in the step 3) to obtain the NiV alloy metallographic sample. According to the preparation method of the NiV alloy metallographic specimen, the prepared NiV alloy metallographic specimen can clearly and correctly observe the metallographic microstructure of the material when being used for metallographic analysis, and is beneficial to improving the accuracy of metallographic analysis.

Description

Preparation method of NiV alloy metallographic specimen
Technical Field
The invention relates to the technical field of metallographic sample preparation, in particular to a preparation method of a NiV alloy metallographic sample.
Background
The NiV alloy target material is a novel semiconductor associated material developed on the basis of pure nickel and pure vanadium targets. The NiV alloy target is adopted to replace the original nickel target and vanadium target in engineering, so that an adhesion layer and a barrier layer can be formed by one-time sputtering, and meanwhile, after a certain amount of vanadium is added into nickel, the nickel-based alloy is nonmagnetic and is favorable for magnetron sputtering. The metallographic detection is an important means for analyzing the performance of the nickel alloy, and the quality of sample preparation is particularly important.
Preparing a metallographic sample: metallographic analysis is one of the means of examining the analytical material, aimed at revealing the true structure of the material. For metallographic analysis, a metallographic specimen, which is a sample that can be used for microscopic observation and inspection, must be prepared. In metallographic analysis, it is important to select and prepare representative samples. In general, the preparation of metallographic specimens involves the following steps: sampling, embedding (which may sometimes be omitted), buffing (coarse and fine), polishing and etching.
The current common methods for preparing metallographic specimens are a mechanical polishing method and an electrolytic polishing method. The single mechanical polishing is time-consuming and labor-consuming, and scratches, tails and the like are extremely easy to leave in the grinding and polishing process, so that the tissue observation and analysis are interfered. The electrolytic polishing method well overcomes the defects, is suitable for mechanically polishing metal materials difficult to eliminate scratches, and has the advantages of low equipment cost, easy operation and simple preparation process.
CN103884566a discloses a preparation method of a V-base alloy metallographic specimen, which belongs to the field of multiphase alloy metallographic preparation. The method comprises the steps of carrying out rough grinding pretreatment on a block-shaped V-based alloy sample, and then carrying out step-by-step water grinding; preparing electrolytic polishing solution, and performing electrolytic polishing on a sample; ultrasonically cleaning the polished sample, then wiping with alcohol, and drying; preparing electrolytic corrosion liquid, and carrying out electrolytic corrosion on the sample; and (3) washing the sample, wiping with alcohol, drying, and then carrying out metallographic observation. According to the invention, through the steps of adjusting experimental parameters and controlling preparation of the V-based alloy metallographic sample, different metallographic morphologies of the V-based alloy are obtained, different metallographic observation requirements are met, more comprehensive information of the V-based alloy microstructure is reflected, and experimental support is provided for research of the V-based alloy.
CN110886010a discloses an electrolytic polishing solution for preparing an aluminum alloy metallographic specimen, which comprises glycerol and aqueous hydrochloric acid. The aluminum alloy metallographic specimen electrolytic polishing solution provided by the invention adopts a combination mode of glycerol and aqueous solution of hydrochloric acid, wherein the hydrochloric acid provides Cl for electrolytic polishing - And the glycerol is taken as a reactant to participate in the electrolytic reaction in the acidic environment, and meanwhile, the water can also improve the conductivity of the electrolytic polishing solution. The electrolytic polishing solution provided by the invention has low hydrochloric acid content and no explosion hazard, and the obtained metallographic structure has the excellent performances of clear and accurate imaging of each phase and less falling of the second phase after the aluminum alloy sample is polished by the electrolytic polishing solution, so that the metallographic detection requirement can be better met. In addition, the structure display method of the aluminum alloy metallographic specimen provided by the invention is simple and convenient to operate, does not need heating, and is preparedThe sample efficiency is high.
CN109470728A discloses a preparation method of a metallographic specimen of a TC4 titanium alloy swinging and grinding piece, which takes the titanium alloy TC4 swinging and grinding piece as a raw material and sequentially comprises the steps of segmentation, coarse grinding, fine grinding, electrolytic polishing, corrosion by corrosive agents and the like. The preparation method of the TC4 titanium alloy swinging and grinding piece metallographic sample can be applied to products which are easy to deform, large in deformation, large in stress and irregular in appearance, so that the sample is in a matte color after being corroded, good in brightness, good in corrosion uniformity, high in selectivity, and capable of obtaining important metal microscopic information of crystal grain morphology and crystal grain structure type through metallographic microscopic observation of the corroded metallographic structure, more beneficial to observation, more accurate in observation, low in cost, simple in sample preparation process, short in sample preparation period and worthy of market popularization and application.
However, in the preparation method of the alloy material metallographic specimen, the electrolytic polishing solution and the corrosive solution are only suitable for the corresponding alloy material, and are not suitable for the preparation of the NiV alloy metallographic specimen, so that the analysis result is inaccurate when the metallographic analysis of the NiV alloy is performed.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a preparation method of a NiV alloy metallographic specimen, which can clearly and correctly observe the metallographic microstructure of a material when being used for metallographic analysis and is beneficial to improving the accuracy of metallographic analysis.
To achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a NiV alloy metallographic specimen comprises the following steps:
1) Cutting: cutting a NiV alloy material into small blocks;
2) Grinding: coarse grinding and fine grinding are carried out on the small sample obtained in the step 1);
3) Electrolytic polishing: carrying out electrolytic polishing treatment on the sample ground in the step 2);
4) And (3) corrosion: and 3) carrying out corrosion treatment on the sample subjected to the electrolytic polishing treatment in the step 3) to obtain the NiV alloy metallographic sample.
According to the preparation method of the NiV alloy metallographic specimen, through sample cutting, grinding, electrolytic polishing and corrosion treatment, the prepared NiV alloy metallographic specimen can clearly and correctly observe the metallographic microstructure of a material when being used for metallographic analysis, and is beneficial to improving the accuracy of metallographic analysis.
In the step 2), the coarse grinding is to sequentially grind the sample obtained in the step 1) by 200# abrasive paper, 500# abrasive paper and 800# abrasive paper, and the fine grinding is to sequentially grind the sample after the coarse grinding by 1000# abrasive paper and 2000# abrasive paper.
In the step 3), the polishing solution for electrolytic polishing comprises the following components in parts by volume:
5 to 7 parts of ethanol, for example, 5 parts, 6 parts, 7 parts or the like by volume of ethanol.
2 to 4 parts of ethylene glycol butyl ether, for example, 2 parts, 3 parts or 4 parts by volume of ethylene glycol butyl ether, etc.
10 to 15 parts of distilled water, for example, 10 parts, 11 parts, 12 parts, 13 parts, 14 parts, 15 parts or the like by volume of distilled water.
4 to 6 parts of perchloric acid, for example, 4 parts, 5 parts or 6 parts by volume of perchloric acid.
In step 3), the parameters of the electrolytic polishing are as follows: the electropolishing voltage is 30-50V, for example, the electropolishing voltage is 30V, 31V, 32V, 33V, 34V, 35V, 36V, 37V, 38V, 39V, 40V, 41V, 42V, 43V, 44V, 45V, 46V, 47V, 48V, 49V, 50V, or the like; the electropolishing time is 30 to 50s, for example 30s, 31s, 32s, 33s, 34s, 35s, 36s, 37s, 38s, 39s, 40s, 41s, 42s, 43s, 44s, 45s, 46s, 47s, 48s, 49s or 50s, etc.
In the step 4), the etching treatment is performed for 20 to 30 seconds by using a nitric acid aqueous solution, for example, etching time is 20 seconds, 21 seconds, 22 seconds, 23 seconds, 24 seconds, 25 seconds, 26 seconds, 27 seconds, 28 seconds, 29 seconds or 30 seconds, etc.; and then etching for 1-2 min by aqueous solution of nitric acid and hydrofluoric acid, for example, etching for 1min, 1.1min, 1.2min, 1.3min, 1.4min, 1.5min, 1.6min, 1.7min, 1.8min, 1.9min or 2min, etc.
The aqueous solution of nitric acid is a mixed solution of nitric acid and water, the volume ratio of nitric acid to water is 1:4-1:1, for example, the volume ratio of nitric acid to water is 1:4, 1:3, 1:2 or 1:1, etc.
The aqueous solution of nitric acid and hydrofluoric acid is a mixed solution of nitric acid, hydrofluoric acid and water, and the volume ratio of nitric acid to hydrofluoric acid to water is 1:1:20-2:1:20.
The nitric acid is commercially available analytically pure nitric acid, and the hydrofluoric acid is commercially available analytically pure hydrofluoric acid.
As a preferred scheme of the invention, a preparation method of a NiV alloy metallographic specimen comprises the following steps:
1) Cutting: cutting NiV alloy material into block-shaped small samples with the size of 20 multiplied by 5 mm;
2) Grinding: sequentially carrying out rough grinding on 200# abrasive paper, 500# abrasive paper and 800# abrasive paper and fine grinding on 1000# abrasive paper and 2000# abrasive paper on the small sample obtained in the step 1);
3) Electrolytic polishing: placing the sample ground in the step 2) into polishing solution, and carrying out electrolytic polishing treatment for 30-50 s at the voltage of 30-50V;
4) And (3) corrosion: and 3) placing the sample subjected to the electrolytic polishing treatment in the step 3) into an etching solution for etching treatment, etching for 20-30 s by using an aqueous solution of nitric acid, and then etching for 1-2 min by using an aqueous solution of nitric acid and hydrofluoric acid to obtain the NiV alloy metallographic sample.
After step 4), a step of washing with water is further included.
Compared with the prior art, the invention has the beneficial effects that:
according to the preparation method of the NiV alloy metallographic specimen, through sample cutting, grinding, electrolytic polishing and corrosion treatment, the prepared NiV alloy metallographic specimen can clearly and correctly observe the metallographic microstructure of a material when being used for metallographic analysis, and the accuracy of metallographic analysis is facilitated to be improved.
Drawings
FIG. 1 is an electron microscopic image after analysis of a metallographic microscope according to example 1 of the present invention;
FIG. 2 is an electron microscopic image after analysis of the metallographic microscope of example 2 of the present invention;
FIG. 3 is an electron microscopic image after analysis of the metallographic microscope of example 7 of the present invention;
FIG. 4 is an electron micrograph of the invention after analysis with a metallographic microscope of example 8.
Detailed Description
The technical scheme of the invention is further described by the following specific embodiments.
The various starting materials of the present invention are commercially available, or may be prepared according to methods conventional in the art, unless specifically indicated.
Example 1
The preparation method of the NiV alloy metallographic specimen of the embodiment comprises the following steps:
1) Cutting: cutting NiV alloy material into block-shaped small samples with the size of 20 multiplied by 5 mm;
2) Grinding: carrying out rough grinding on the 200# abrasive paper, the 500# abrasive paper and the 800# abrasive paper and fine grinding on the 1000# abrasive paper and the 2000# abrasive paper on the small sample obtained in the step 1);
3) Electrolytic polishing: placing the sample ground in the step 2) into polishing solution, and carrying out electrolytic polishing treatment for 50s at the voltage of 40V;
wherein, the polishing solution for electrolytic polishing comprises the following components in parts by volume:
4) And (3) corrosion: and 3) placing the sample subjected to the electrolytic polishing treatment in an etching solution for etching treatment, wherein the sample is firstly subjected to etching treatment by an aqueous solution of nitric acid for 25 seconds, and then subjected to etching treatment by an aqueous solution of nitric acid and an aqueous solution of hydrofluoric acid for 1.5 minutes, wherein the aqueous solution of nitric acid is a mixed solution of nitric acid and water, the volume ratio of nitric acid to water is 1:1, the aqueous solution of nitric acid and hydrofluoric acid is a mixed solution of nitric acid, hydrofluoric acid and water, and the volume ratio of nitric acid to hydrofluoric acid to water is 1:1:20, so as to obtain the NiV alloy metallographic sample.
The NiV alloy metallographic specimen prepared in the embodiment is used for metallographic analysis, and an electron microscope diagram after metallographic microscopic analysis is shown in FIG. 1.
As can be seen from FIG. 1, the grain boundary of each grain is clearly shown, so that the metallographic microstructure of the material can be clearly observed, and the accuracy of metallographic analysis is facilitated.
Example 2
The preparation method of the NiV alloy metallographic specimen of the embodiment comprises the following steps:
1) Cutting: cutting NiV alloy material into block-shaped small samples with the size of 20 multiplied by 5 mm;
2) Grinding: carrying out rough grinding on the 200# abrasive paper, the 500# abrasive paper and the 800# abrasive paper and fine grinding on the 1000# abrasive paper and the 2000# abrasive paper on the small sample obtained in the step 1);
3) Electrolytic polishing: placing the sample ground in the step 2) into polishing solution, and carrying out electrolytic polishing treatment for 40s at a voltage of 40V;
wherein, the polishing solution for electrolytic polishing comprises the following components in parts by volume:
4) And (3) corrosion: and 3) placing the sample subjected to the electrolytic polishing treatment in a corrosive liquid for corrosion, wherein the sample is corroded for 25 seconds by an aqueous solution of nitric acid, and then is corroded for 2 minutes by an aqueous solution of nitric acid and hydrofluoric acid, wherein the aqueous solution of nitric acid is a mixed solution of nitric acid and water, the volume ratio of nitric acid to water is 1:1, the aqueous solution of nitric acid and hydrofluoric acid is a mixed solution of nitric acid, hydrofluoric acid and water, and the volume ratio of nitric acid to hydrofluoric acid to water is 1:1:20, so that the NiV alloy metallographic sample is obtained.
The NiV alloy metallographic specimen prepared in the embodiment is used for metallographic analysis, and an electron microscope diagram after metallographic microscopic analysis is shown in FIG. 2.
Example 3
The preparation method of the NiV alloy metallographic specimen of the embodiment comprises the following steps:
1) Cutting: cutting NiV alloy material into block-shaped small samples with the size of 20 multiplied by 5 mm;
2) Grinding: carrying out rough grinding on the 200# abrasive paper, the 500# abrasive paper and the 800# abrasive paper and fine grinding on the 1000# abrasive paper and the 2000# abrasive paper on the small sample obtained in the step 1);
3) Electrolytic polishing: placing the sample ground in the step 2) into polishing solution, and carrying out electrolytic polishing treatment for 40s at a voltage of 40V;
wherein, the polishing solution for electrolytic polishing comprises the following components in parts by volume:
4) And (3) corrosion: and 3) placing the sample subjected to the electrolytic polishing treatment in the step 3) into a corrosive liquid for corrosion, wherein the sample is corroded for 20 seconds by an aqueous solution of nitric acid, and then is corroded for 1min by an aqueous solution of nitric acid and hydrofluoric acid, wherein the aqueous solution of nitric acid is a mixed solution of nitric acid and water, the volume ratio of nitric acid to water is 1:4, the aqueous solution of nitric acid and hydrofluoric acid is a mixed solution of nitric acid, hydrofluoric acid and water, and the volume ratio of nitric acid to hydrofluoric acid to water is 1:1:20, so that the NiV alloy metallographic sample is obtained.
The microscopic photograph of the metallographic gold test phase of the NiV alloy prepared by the embodiment is clear, and the metallographic analysis accuracy can be improved well.
Example 4
The preparation method of the NiV alloy metallographic specimen of the embodiment comprises the following steps:
1) Cutting: cutting NiV alloy material into block-shaped small samples with the size of 20 multiplied by 5 mm;
2) Grinding: carrying out rough grinding on the 200# abrasive paper, the 500# abrasive paper and the 800# abrasive paper and fine grinding on the 1000# abrasive paper and the 2000# abrasive paper on the small sample obtained in the step 1);
3) Electrolytic polishing: placing the sample ground in the step 2) into polishing solution, and carrying out electrolytic polishing treatment for 50s at the voltage of 40V;
wherein, the polishing solution for electrolytic polishing comprises the following components in parts by volume:
4) And (3) corrosion: and 3) placing the sample subjected to the electrolytic polishing treatment in a corrosive liquid for corrosion, wherein the sample is corroded for 25 seconds by an aqueous solution of nitric acid, and then is corroded for 1.5 minutes by an aqueous solution of nitric acid and hydrofluoric acid, wherein the aqueous solution of nitric acid is a mixed solution of nitric acid and water, the volume ratio of nitric acid to water is 1:1, the aqueous solution of nitric acid and hydrofluoric acid is a mixed solution of nitric acid, hydrofluoric acid and water, and the volume ratio of nitric acid to hydrofluoric acid to water is 1:1:20, so that the NiV alloy metallographic sample is obtained.
The NiV alloy metallographic specimen prepared by the embodiment is used for metallographic analysis, and the image is clear, so that the structural information of the material can be well reflected, and the accuracy of metallographic analysis can be improved.
Example 5
This example differs from example 1 in that the polishing liquid used for the electrolytic polishing treatment is sulfuric acid: perchloric acid: alcohol: water=1:2:1:20, otherwise the same as in example 1.
The NiV alloy metallographic specimen prepared by the embodiment is used for metallographic analysis, can not clearly and truly reflect the structure of the material, and causes interference to subsequent analysis and judgment.
Example 6
The difference between this example and example 1 is that the etching solution used for etching is hydrochloric acid: nitric acid: water=2:1:15, otherwise the same as in example 1.
The NiV alloy metallographic specimen prepared by the embodiment is used for metallographic analysis, can not clearly and truly reflect the structure of the material, and causes interference to subsequent analysis and judgment.
Example 7
The present example differs from example 1 in that the parameters of the electropolishing process are: the polishing voltage was 30V and the time was 30s, and the same as in example 1 was repeated.
The NiV alloy metallographic specimen prepared in the embodiment is used for metallographic analysis, and an electron microscope diagram after metallographic microscopic analysis is shown in FIG. 3.
As can be seen from FIG. 3, the grain boundaries of the grains in the metallographic phase are not completely corroded, and meanwhile, as the electrolytic polishing time is too short, more scratches exist on the surface of the sample, so that the structure of the material cannot be truly reflected, and the subsequent analysis is wrongly judged.
Example 8
The difference between this embodiment and embodiment 1 is that the parameters of the etching process are: etching for 30s by using aqueous solution of nitric acid, and then etching for 2min by using aqueous solution of nitric acid and hydrofluoric acid, wherein the volume ratio of the aqueous solution of nitric acid is 1:1, and the volume ratio of the aqueous solution of nitric acid and hydrofluoric acid is 2:1:20, so as to obtain the NiV alloy metallographic sample. Otherwise, the same as in example 1 was used.
The NiV alloy metallographic specimen prepared in the embodiment is used for metallographic analysis, and an electron microscope diagram after metallographic microscopic analysis is shown in FIG. 4.
As can be seen from fig. 4, the crystal phase structure has a tendency of excessively long etching time, and many small black spots appear on the crystal grains, which cannot well reflect the correct structure condition of the material.
The detailed process equipment and process flow of the present invention are described by the above embodiments, but the present invention is not limited to, i.e., it does not mean that the present invention must be practiced depending on the detailed process equipment and process flow. It should be apparent to those skilled in the art that any modification of the present invention, equivalent substitution of raw materials for the product of the present invention, addition of auxiliary components, selection of specific modes, etc., falls within the scope of the present invention and the scope of disclosure.
The detailed process equipment and process flow of the present invention are described by the above embodiments, but the present invention is not limited to, i.e., it does not mean that the present invention must be practiced depending on the detailed process equipment and process flow. It should be apparent to those skilled in the art that any modification of the present invention, equivalent substitution of raw materials for the product of the present invention, addition of auxiliary components, selection of specific modes, etc., falls within the scope of the present invention and the scope of disclosure.
The preferred embodiments of the present invention have been described in detail above, but the present invention is not limited to the specific details of the above embodiments, and various simple modifications can be made to the technical solution of the present invention within the scope of the technical concept of the present invention, and all the simple modifications belong to the protection scope of the present invention.
In addition, the specific features described in the above embodiments may be combined in any suitable manner, and in order to avoid unnecessary repetition, various possible combinations are not described further.
Moreover, any combination of the various embodiments of the invention can be made without departing from the spirit of the invention, which should also be considered as disclosed herein.

Claims (5)

1. The preparation method of the NiV alloy metallographic specimen is characterized by comprising the following steps of:
1) Cutting: cutting a NiV alloy material into small blocks;
2) Grinding: coarse grinding and fine grinding are carried out on the small sample obtained in the step 1);
3) Electrolytic polishing: carrying out electrolytic polishing treatment on the sample ground in the step 2); the polishing solution for electrolytic polishing comprises the following components in parts by volume: 5-7 parts of ethanol, 2-4 parts of ethylene glycol butyl ether, 10-15 parts of distilled water and 4-6 parts of perchloric acid;
4) And (3) corrosion: carrying out corrosion treatment on the sample subjected to the electrolytic polishing treatment in the step 3) to obtain a NiV alloy metallographic sample; the corrosion treatment is carried out by firstly corroding for 20-30 s by aqueous solution of nitric acid, and then corroding for 1-2 min by aqueous solution of nitric acid and hydrofluoric acid; the aqueous solution of nitric acid is a mixed solution of nitric acid and water, and the volume ratio of nitric acid to water is 1:4-1:1; the aqueous solution of nitric acid and hydrofluoric acid is a mixed solution of nitric acid, hydrofluoric acid and water; the volume ratio of the nitric acid to the hydrofluoric acid to the water is 1:1:20-2:1:20.
2. The method according to claim 1, wherein in the step 2), the coarse grinding is to sequentially grind the sample obtained in the step 1) with 200# abrasive paper, 500# abrasive paper and 800# abrasive paper, and the fine grinding is to sequentially grind the sample after the coarse grinding with 1000# abrasive paper and 2000# abrasive paper.
3. The method according to claim 1, wherein in step 3), the parameters of the electropolishing are: the voltage of the electrolytic polishing is 30-50V, and the time of the electrolytic polishing is 30-50 s.
4. A method of preparation according to any one of claims 1 to 3, characterized in that the method of preparation comprises the steps of:
1) Cutting: cutting NiV alloy material into block-shaped small samples with the size of 20 multiplied by 5 mm;
2) Grinding: sequentially carrying out rough grinding on 200# abrasive paper, 500# abrasive paper and 800# abrasive paper and fine grinding on 1000# abrasive paper and 2000# abrasive paper on the small sample obtained in the step 1);
3) Electrolytic polishing: placing the sample ground in the step 2) into polishing solution, and carrying out electrolytic polishing treatment for 30-50 s at the voltage of 30-50V;
4) And (3) corrosion: and 3) placing the sample subjected to the electrolytic polishing treatment in the step 3) into an etching solution for etching treatment, etching for 20-30 s by using an aqueous solution of nitric acid, and then etching for 1-2 min by using an aqueous solution of nitric acid and hydrofluoric acid to obtain the NiV alloy metallographic sample.
5. The method of claim 4, further comprising a step of washing after step 4).
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Electrochemical Polarization Behaviour of Electroless Ni-P Deposits with Different Chromium-Free Pre-Treatment on Magnesium Alloy;Jothi Sudagar et al.;International Journal of ELECTROCHEMICAL SCIENCE;第6卷;第2767-2788页 *

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