CN111707513A - Preparation method of NiV alloy metallographic specimen - Google Patents
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- CN111707513A CN111707513A CN202010555893.1A CN202010555893A CN111707513A CN 111707513 A CN111707513 A CN 111707513A CN 202010555893 A CN202010555893 A CN 202010555893A CN 111707513 A CN111707513 A CN 111707513A
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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 a sample: cutting the 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 used for metallographic analysis, and the accuracy of the metallographic analysis is improved.
Description
Technical Field
The invention relates to the technical field of metallographic specimen preparation, in particular to a preparation method of a NiV alloy metallographic specimen.
Background
The NiV alloy target is a novel semiconductor related material developed on the basis of pure nickel and pure vanadium targets. In engineering, NiV alloy target is used to replace original nickel target and vanadium target, so that it can be sputtered to form adhesion layer and barrier layer, and after adding a certain amount of vanadium into nickel, the nickel-base alloy is non-magnetic and is favorable to magnetron sputtering. The metallographic detection is used as an important means for analyzing the performance of the nickel alloy, and the quality of sample preparation is particularly important.
Preparing a metallographic specimen: metallographic analysis is one of the means for examining and analyzing materials, and aims to reveal the true structure of the material. For metallographic analysis, it is necessary to prepare a metallographic specimen which can be used for microscopic examination. In metallographic analysis it is important to select and prepare representative samples. In general, metallographic specimen preparation is carried out by the following steps: sampling, inlaying (sometimes omitted), lapping (rough and fine), polishing, and etching.
The current common methods for preparing metallographic samples are mechanical polishing method and electrolytic polishing method. The single mechanical polishing not only wastes time and labor, but also easily leaves scratches, tails and the like in the grinding and polishing process, and brings interference to tissue observation and analysis. The electrolytic polishing method well overcomes the defects, is suitable for mechanical polishing of 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-based alloy metallographic specimen, belonging to the field of multiphase alloy metallographic preparation. According to the method, a blocky V-based alloy sample is subjected to coarse grinding pretreatment and then is subjected to step-by-step water grinding; preparing an electrolytic polishing solution, and performing electrolytic polishing on the sample; carrying out ultrasonic cleaning on the polished sample, then wiping the sample by using alcohol, and drying the sample; preparing electrolytic corrosion liquid, and performing electrolytic corrosion on the sample; and (4) washing the sample, wiping the sample with alcohol, drying the sample, and then carrying out metallographic observation. According to the invention, different metallographic appearances of the V-based alloy are obtained by adjusting experimental parameters and controlling the preparation of the metallographic sample of the V-based alloy, different metallographic observation requirements are met, more comprehensive information of the microstructure of the V-based alloy is reflected, and experimental support is provided for the research of the V-based alloy.
CN110886010A discloses an aluminum alloy metallographic testThe electrolytic polishing solution for preparation comprises glycerol and hydrochloric acid aqueous solution. The electrolytic polishing solution for the metallographic specimen of the aluminum alloy provided by the invention adopts a combination mode of glycerol and a hydrochloric acid aqueous solution, wherein the hydrochloric acid provides Cl for electrolytic polishing-In an acidic environment, glycerol is used as a reactant to participate in an electrolytic reaction, and simultaneously, 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 after an aluminum alloy sample is polished by the electrolytic polishing solution, the obtained metallographic structure has the excellent performances of clear and accurate imaging of each phase and less shedding of a second phase, and can better meet the requirements of metallographic detection. Moreover, the method for displaying the structure of the aluminum alloy metallographic specimen provided by the invention is simple and convenient to operate, does not need heating, and has high specimen preparation efficiency.
CN109470728A discloses a preparation method of a TC4 titanium alloy swing-grinding piece metallographic specimen, which takes a titanium alloy TC4 swing-grinding piece as a raw material and sequentially comprises the steps of cutting, coarse grinding, fine grinding, electrolytic polishing, corrosion by a corrosive agent and the like. The preparation method of the TC4 titanium alloy swing-grinding piece metallographic specimen can be applied to products which are easy to deform, large in deformation amount, large in stress and irregular in appearance, so that the specimen is in a sub-gloss color after being corroded, good in brightness and good in corrosion uniformity, the corrosion method is high in selectivity, the corroded metallographic structure can be observed by a metallographic microscope to obtain important metal microscopic information of grain morphology and grain structure type, observation is facilitated, observation is more accurate, the preparation method is low in cost, the sample preparation process is simple, the sample preparation period is short, and the preparation method is worthy of market popularization and application.
However, in the method for preparing the metallographic specimen of the alloy material, the adopted electrolytic polishing solution and corrosive solution are only suitable for the corresponding alloy material and are not suitable for preparing the metallographic specimen of the NiV alloy, so that the analysis result is inaccurate when the metallographic specimen of the NiV alloy is analyzed.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide the preparation method of the NiV alloy metallographic specimen, and the NiV alloy metallographic specimen prepared by the preparation method can clearly and correctly observe the metallographic microstructure of the material when being used for metallographic analysis, thereby being beneficial to improving the accuracy of the metallographic analysis.
In order 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 a sample: cutting the 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 be used for clearly and correctly observing the metallographic microstructure of the material when being used for metallographic analysis through sample cutting, grinding, electrolytic polishing and corrosion treatment, and the accuracy of the metallographic analysis is improved.
In the step 2), the rough grinding is to perform rough grinding on the small sample obtained in the step 1) through 200# sand paper, 500# sand paper and 800# sand paper in sequence, and the fine grinding is to perform fine grinding on the small sample subjected to the rough grinding through 1000# sand paper and 2000# sand paper in sequence.
In the step 3), the polishing solution for electrolytic polishing comprises the following components in parts by volume:
5-7 parts of ethanol, for example, 5 parts, 6 parts or 7 parts of ethanol by volume.
2-4 parts of ethylene glycol butyl ether, for example, the volume parts of the ethylene glycol butyl ether are 2 parts, 3 parts or 4 parts, and the like.
10-15 parts of distilled water, for example, 10 parts, 11 parts, 12 parts, 13 parts, 14 parts or 15 parts by volume of distilled water.
4-6 parts of perchloric acid, for example, 4 parts, 5 parts or 6 parts of perchloric acid by volume.
In step 3), the parameters of the electrolytic polishing are as follows: the voltage of the electrolytic polishing is 30-50V, for example, the voltage of the electrolytic polishing is 30V, 31V, 32V, 33V, 34V, 35V, 36V, 37V, 38V, 39V, 40V, 41V, 42V, 43V, 44V, 45V, 46V, 47V, 48V, 49V or 50V, etc.; the time of the electrolytic polishing is 30-50 s, for example, the time of the electrolytic polishing is 30s, 31s, 32s, 33s, 34s, 35s, 36s, 37s, 38s, 39s, 40s, 41s, 42s, 43s, 44s, 45s, 46s, 47s, 48s, 49s or 50s, and the like.
In the step 4), firstly, etching for 20-30 s by using a nitric acid aqueous solution, for example, the etching time is 20s, 21s, 22s, 23s, 24s, 25s, 26s, 27s, 28s, 29s or 30 s; and then etching with an aqueous solution of nitric acid and hydrofluoric acid for 1-2 min, for example, etching time is 1min, 1.1min, 1.2min, 1.3min, 1.4min, 1.5min, 1.6min, 1.7min, 1.8min, 1.9min or 2 min.
The nitric acid aqueous solution is a mixed solution of nitric acid and water, the volume ratio of the nitric acid to the water is 1: 4-1: 1, for example, the volume ratio of the nitric acid to the water is 1:4, 1:3, 1:2 or 1:1, and the like.
The nitric acid and hydrofluoric acid aqueous solution is a mixed solution of nitric acid, hydrofluoric acid and water, and the volume ratio of the nitric acid to the hydrofluoric acid to the 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, the preparation method of the NiV alloy metallographic specimen comprises the following steps:
1) cutting a sample: cutting the NiV alloy material into small blocks of 20 multiplied by 5 mm;
2) grinding: carrying out coarse grinding on the sample obtained in the step 1) by using 200# abrasive paper, 500# abrasive paper and 800# abrasive paper and fine grinding on 1000# abrasive paper and 2000# abrasive paper in sequence;
3) electrolytic polishing: putting the sample ground in the step 2) into a polishing solution, and performing electrolytic polishing treatment for 30-50 s at the voltage of 30-50V;
4) and (3) corrosion: and (3) putting the sample subjected to the electrolytic polishing treatment in the step 3) into a corrosive liquid for corrosion treatment, firstly corroding for 20-30 s by using an aqueous solution of nitric acid, and then corroding for 1-2 min by using an aqueous solution of nitric acid and hydrofluoric acid to obtain the NiV alloy metallographic sample.
After the step 4), a step of cleaning is also included, and the cleaning is performed by using water.
Compared with the prior art, the invention has the beneficial effects that:
according to the preparation method of the NiV alloy metallographic specimen, the prepared NiV alloy metallographic specimen can be used for clearly and correctly observing the metallographic microstructure of the material when being used for metallographic analysis through sample cutting, grinding, electrolytic polishing and corrosion treatment, and the accuracy of the metallographic analysis is favorably improved.
Drawings
FIG. 1 is an electron micrograph after metallographic microscopic analysis of example 1 of the present invention;
FIG. 2 is an electron micrograph after metallographic microscopic analysis according to example 2 of the present invention;
FIG. 3 is an electron micrograph after metallographic microscopic analysis according to example 7 of the present invention;
FIG. 4 is an electron micrograph after metallographic microscopic analysis of example 8 of the present invention.
Detailed Description
The technical solution of the present invention is further explained by the following embodiments.
Unless otherwise specified, various starting materials of the present invention are commercially available or prepared according to conventional methods in the art.
Example 1
The preparation method of the NiV alloy metallographic specimen of the embodiment comprises the following steps:
1) cutting a sample: cutting the NiV alloy material into small blocks of 20 multiplied by 5 mm;
2) grinding: carrying out coarse grinding on the sample obtained in the step 1) by using 200# abrasive paper, 500# abrasive paper and 800# abrasive paper and fine grinding by using 1000# abrasive paper and 2000# abrasive paper;
3) electrolytic polishing: putting the sample ground in the step 2) into polishing solution, and performing electrolytic polishing treatment for 50s at the voltage of 40V;
the polishing solution for electrolytic polishing comprises the following components in parts by volume:
4) and (3) corrosion: and (3) putting the sample subjected to the electrolytic polishing treatment in the step 3) into a corrosive liquid for corrosion treatment, firstly corroding for 25s by using a nitric acid aqueous solution, and then corroding for 1.5min by using a nitric acid and hydrofluoric acid aqueous solution, wherein the nitric acid aqueous solution is a mixed solution of nitric acid and water, the volume ratio of nitric acid to water is 1:1, the nitric acid and hydrofluoric acid aqueous solution 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 metallographic specimen of the NiV alloy prepared in this example was used for metallographic analysis, and an electron micrograph after metallographic microscopic analysis is shown in fig. 1.
As can be seen from figure 1, the grain boundary of each grain is clearly shown, 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 a sample: cutting the NiV alloy material into small blocks of 20 multiplied by 5 mm;
2) grinding: carrying out coarse grinding on the sample obtained in the step 1) by using 200# abrasive paper, 500# abrasive paper and 800# abrasive paper and fine grinding by using 1000# abrasive paper and 2000# abrasive paper;
3) electrolytic polishing: putting the sample ground in the step 2) into polishing solution, and performing electrolytic polishing treatment for 40s at the voltage of 40V;
the polishing solution for electrolytic polishing comprises the following components in parts by volume:
4) and (3) corrosion: putting the sample subjected to the electrolytic polishing treatment in the step 3) into a corrosive liquid for corrosion, firstly corroding for 25s by using a nitric acid aqueous solution, and then corroding for 2min by using a nitric acid and hydrofluoric acid aqueous solution, wherein the nitric acid aqueous solution is a mixed solution of nitric acid and water, the volume ratio of nitric acid to water is 1:1, the nitric acid and hydrofluoric acid aqueous solution 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 metallographic specimen of the NiV alloy prepared in this example was used for metallographic analysis, and an electron micrograph 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 a sample: cutting the NiV alloy material into small blocks of 20 multiplied by 5 mm;
2) grinding: carrying out coarse grinding on the sample obtained in the step 1) by using 200# abrasive paper, 500# abrasive paper and 800# abrasive paper and fine grinding by using 1000# abrasive paper and 2000# abrasive paper;
3) electrolytic polishing: putting the sample ground in the step 2) into polishing solution, and performing electrolytic polishing treatment for 40s at the voltage of 40V;
the polishing solution for electrolytic polishing comprises the following components in parts by volume:
4) and (3) corrosion: putting the sample subjected to the electrolytic polishing treatment in the step 3) into a corrosive liquid for corrosion, firstly corroding for 20s by using a nitric acid aqueous solution, and then corroding for 1min by using a nitric acid and hydrofluoric acid aqueous solution, wherein the nitric acid aqueous solution is a mixed solution of nitric acid and water, the volume ratio of nitric acid to water is 1:4, the nitric acid and hydrofluoric acid aqueous solution 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 metallographic phase gold-testing micrograph of the NiV alloy prepared by the embodiment is clear, and the metallographic analysis accuracy can be well improved.
Example 4
The preparation method of the NiV alloy metallographic specimen of the embodiment comprises the following steps:
1) cutting a sample: cutting the NiV alloy material into small blocks of 20 multiplied by 5 mm;
2) grinding: carrying out coarse grinding on the sample obtained in the step 1) by using 200# abrasive paper, 500# abrasive paper and 800# abrasive paper and fine grinding by using 1000# abrasive paper and 2000# abrasive paper;
3) electrolytic polishing: putting the sample ground in the step 2) into polishing solution, and performing electrolytic polishing treatment for 50s at the voltage of 40V;
the polishing solution for electrolytic polishing comprises the following components in parts by volume:
4) and (3) corrosion: putting the sample subjected to the electrolytic polishing treatment in the step 3) into a corrosive liquid for corrosion, firstly corroding for 25s by using a nitric acid aqueous solution, and then corroding for 1.5min by using a nitric acid and hydrofluoric acid aqueous solution, wherein the nitric acid aqueous solution is a mixed solution of nitric acid and water, the volume ratio of nitric acid to water is 1:1, the nitric acid and hydrofluoric acid aqueous solution 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 by the embodiment is used for metallographic analysis, the image is clear, the organizational structure information of the material can be well reflected, and the accuracy of the metallographic analysis is improved.
Example 5
This example is different from example 1 in that the polishing liquid used in the electrolytic polishing treatment was sulfuric acid: perchloric acid: alcohol: water 1:2:1:20, the rest being the same as in example 1.
When the NiV alloy metallographic specimen prepared by the embodiment is used for metallographic analysis, the microstructure of the material cannot be clearly and truly reflected, and interference is caused on 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.
When the NiV alloy metallographic specimen prepared by the embodiment is used for metallographic analysis, the microstructure of the material cannot be clearly and truly reflected, and interference is caused on subsequent analysis and judgment.
Example 7
This example differs from example 1 in that the parameters of the electropolishing process were: the polishing voltage was 30V and the time was 30s, and the rest was the same as in example 1.
The metallographic specimen of the NiV alloy prepared in this example was used for metallographic analysis, and an electron micrograph after metallographic microscopic analysis is shown in fig. 3.
As can be seen from FIG. 3, the grain boundary of the grain in the metallographic phase is not completely corroded, and meanwhile, due to the excessively short electropolishing time, the surface of the sample has more scratches, so that the texture structure of the material cannot be truly reflected, and the subsequent analysis is wrongly judged.
Example 8
The present embodiment is different from embodiment 1 in that the parameters of the etching treatment are: and corroding for 30s by using an aqueous solution of nitric acid, and corroding for 2min by using an aqueous solution of nitric acid and hydrofluoric acid, wherein the aqueous solution of nitric acid (the volume ratio is 1:1) and the aqueous solution of nitric acid and hydrofluoric acid (the volume ratio is 2:1:20) to obtain the NiV alloy metallographic specimen. The rest is the same as in example 1.
The metallographic specimen of the NiV alloy prepared in this example was used for metallographic analysis, and an electron micrograph after metallographic microscopic analysis is shown in fig. 4.
As can be seen from FIG. 4, the crystal phase structure tends to be corroded for too long, and many small black spots appear on the crystal grains, which do not well reflect the correct structure of the material.
The present invention is illustrated by the above-mentioned examples, but the present invention is not limited to the above-mentioned detailed process equipment and process flow, i.e. it is not meant to imply that the present invention must rely on the above-mentioned detailed process equipment and process flow to be practiced. It should be understood by those skilled in the art that any modification of the present invention, equivalent substitutions of the raw materials of the product of the present invention, addition of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.
The present invention is illustrated by the above-mentioned examples, but the present invention is not limited to the above-mentioned detailed process equipment and process flow, i.e. it is not meant to imply that the present invention must rely on the above-mentioned detailed process equipment and process flow to be practiced. It should be understood by those skilled in the art that any modification of the present invention, equivalent substitutions of the raw materials of the product of the present invention, addition of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.
The preferred embodiments of the present invention have been described in detail, however, the present invention is not limited to the specific details of the above embodiments, and various simple modifications may be made to the technical solution of the present invention within the technical idea of the present invention, and these simple modifications are within the protective scope of the present invention.
It should be noted that the various technical features described in the above embodiments can be combined in any suitable manner without contradiction, and the invention is not described in any way for the possible combinations in order to avoid unnecessary repetition.
In addition, any combination of the various embodiments of the present invention is also possible, and the same should be considered as the disclosure of the present invention as long as it does not depart from the spirit of the present invention.
Claims (10)
- The preparation method of the NiV alloy metallographic specimen is characterized by comprising the following steps:1) cutting a sample: cutting the 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.
- 2. The preparation method according to claim 1, wherein in the step 2), the rough grinding is carried out by carrying out rough grinding on the sample obtained in the step 1) by using 200# sand paper, 500# sand paper and 800# sand paper in sequence, and the fine grinding is carried out by carrying out fine grinding on the sample after the rough grinding by using 1000# sand paper and 2000# sand paper in sequence.
- 3. The production method according to claim 1 or 2, wherein in the step 3), the polishing solution for electrolytic polishing comprises the following components in parts by volume:
- 4. the method according to any one of claims 1 to 3, wherein the parameters of the electropolishing in step 3) are: the voltage of the electrolytic polishing is 30-50V, and the time of the electrolytic polishing is 30-50 s.
- 5. The preparation method according to any one of claims 1 to 4, wherein in the step 4), the etching treatment is performed for 20 to 30 seconds by using an aqueous solution of nitric acid, and then for 1 to 2 minutes by using an aqueous solution of nitric acid and hydrofluoric acid.
- 6. The preparation method according to claim 5, wherein the aqueous solution of nitric acid is a mixed solution of nitric acid and water, and the volume ratio of the nitric acid to the water is 1: 4-1: 1.
- 7. The method according to claim 5, wherein the aqueous solution of nitric acid and hydrofluoric acid is a mixed solution of nitric acid, hydrofluoric acid and water.
- 8. The preparation method according to claim 7, wherein the volume ratio of the nitric acid to the hydrofluoric acid and the water is 1:1:20 to 2:1: 20.
- 9. The method according to any one of claims 1 to 8, comprising the steps of:1) cutting a sample: cutting the NiV alloy material into small blocks of 20 multiplied by 5 mm;2) grinding: carrying out coarse grinding on the sample obtained in the step 1) by using 200# abrasive paper, 500# abrasive paper and 800# abrasive paper and fine grinding on 1000# abrasive paper and 2000# abrasive paper in sequence;3) electrolytic polishing: putting the sample ground in the step 2) into a polishing solution, and performing electrolytic polishing treatment for 30-50 s at the voltage of 30-50V;4) and (3) corrosion: and (3) putting the sample subjected to the electrolytic polishing treatment in the step 3) into a corrosive liquid for corrosion treatment, firstly corroding for 20-30 s by using an aqueous solution of nitric acid, and then corroding for 1-2 min by using an aqueous solution of nitric acid and hydrofluoric acid to obtain the NiV alloy metallographic sample.
- 10. The method according to any one of claims 1 to 9, further comprising a washing step after the step 4).
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| CN114113043A (en) * | 2021-12-13 | 2022-03-01 | 宁波江丰电子材料股份有限公司 | Method for measuring nickel and vanadium content in NiV alloy by using inductively coupled plasma emission spectrometer |
| CN114526978A (en) * | 2022-02-25 | 2022-05-24 | 中国工程物理研究院材料研究所 | Metallographic corrosive liquid of vanadium alloy and preparation method of metallographic sample of vanadium alloy |
| CN115078049A (en) * | 2022-08-19 | 2022-09-20 | 深圳市聚鑫视科技有限公司 | Automatic sample preparation and grinding method and system for metallographic sample |
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