CN115436134A - Metallographic structure characterization method of high-purity yttrium target material - Google Patents
Metallographic structure characterization method of high-purity yttrium target material Download PDFInfo
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- 229910052727 yttrium Inorganic materials 0.000 title claims abstract description 61
- 239000013077 target material Substances 0.000 title claims abstract description 45
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- 238000012360 testing method Methods 0.000 claims abstract description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 57
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 42
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 22
- 229910017604 nitric acid Inorganic materials 0.000 claims description 22
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 21
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 11
- 150000002910 rare earth metals Chemical class 0.000 claims description 11
- 244000137852 Petrea volubilis Species 0.000 claims description 10
- 239000003518 caustics Substances 0.000 claims description 9
- 239000000243 solution Substances 0.000 claims description 9
- 239000003795 chemical substances by application Substances 0.000 claims description 7
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 7
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 7
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- 239000000463 material Substances 0.000 description 13
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- 229910052751 metal Inorganic materials 0.000 description 7
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- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
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- 229910052759 nickel Inorganic materials 0.000 description 3
- 239000010936 titanium Substances 0.000 description 3
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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
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/32—Polishing; Etching
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- 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
- G01N1/34—Purifying; Cleaning
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/84—Systems specially adapted for particular applications
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Abstract
The invention belongs to the technical field of metallographic analysis and test, and particularly relates to a metallographic structure characterization method of a high-purity yttrium target material. The yttrium target is processed by a method with a specific proportion, the traditional process that metallographic sample preparation needs five steps of sampling → embedding → grinding → polishing → corrosion is broken through, and the yttrium target metallographic sample which has good contrast, obvious grain boundary profile and clear crystal grain appearance and is convenient to observe and analyze under a microscope can be prepared by directly corroding after embedding and grinding.
Description
Technical Field
The invention belongs to the technical field of metallographic analysis and test, and particularly relates to a metallographic structure characterization method of a high-purity yttrium target sample.
Background
Yttrium (Yttrium) is a gray-black metal, the crystal structure of which belongs to the hexagonal system. As the first rare earth metal to be discovered, yttrium, a rare earth, has been widely used in the fields of integrated circuits, novel displays, sputtering targets for 5G communication electronic information, and the like. The internal microstructure of the material can directly influence the service performance of a product, for a high-purity yttrium target, the grain size and the texture orientation seriously influence the sputtering rate and the uniformity of a sputtered film, the internal structure of the material has direct and close relation with the material properties such as hardness, strength, ductility and the like of the material, and metallographic analysis is the most direct and effective method for researching the internal structure of a metal material.
The preparation of the high-quality metallographic sample is the basis for developing the observation and research on the microstructure morphology of the high-purity yttrium target material, and the quality of the prepared sample directly influences the representativeness and the accuracy of the material structure. The rare earth yttrium target is soft, and is easy to embed particles during grinding and polishing so as to generate a deformation interference layer; the chemical activity is high, the polishing process is easy to oxidize, and when metallographic corrosion occurs, the reaction is fast and over corrosion is easy to occur, so that a clear and real microstructure is difficult to obtain.
So far, the existing material microstructure research technology at home and abroad does not relate to the metallographic sample preparation technology of the yttrium target material. The sample prepared by the metallographic sample preparation method of other metal materials disclosed in the prior art inevitably has cracks and deformation interference layers, and the surface of the material is seriously oxidized and corroded, so that a real tissue cannot be obtained. The high-purity yttrium target material is a key raw material for developing high and new technical materials. In the document of the New Material industry development guide, it is clearly pointed out that the high-purity metal sputtering target material needs to be developed vigorously. The development of the microstructure research of the high-purity yttrium target material accords with the development direction of high-end new materials, and the microscopic sample preparation method is a key technology for ensuring the quality improvement of the rare earth yttrium target material product and needs to carry out new research and exploration.
Disclosure of Invention
In order to solve the problems, the invention provides an efficient and convenient preparation method of a high-purity yttrium target material sample for metallographic structure characterization, which adopts four steps of sampling → embedding → grinding → corroding, and can prepare the high-purity yttrium target material metallographic sample with good contrast and clear structure display without metallographic polishing.
The specific technical scheme of the invention is as follows:
1. sampling: cutting out a sample by linear cutting to prepare a cubic sample with a smooth and flat ground surface and a side length of (15-25) mm;
2. inlaying: weighing 90-120g of liquid epoxy resin and 10-20g of epoxy curing agent, fully and uniformly stirring to prepare a cold embedding material, putting a sample into a cold embedding mold with a ground surface facing downwards, adding the embedding material into the mold to completely immerse the sample, vacuumizing, curing at room temperature for 8-24h, and demolding to prepare a cold embedding sample;
3. grinding: sequentially grinding cold-inlaid samples on silicon carbide abrasive paper of different models from coarse to fine step by step, dripping lubricating oil on the abrasive paper to prevent false images caused by sand embedding, grinding each step in the same direction, and rotating the samples by 45-135 degrees in the next grinding process until scratches of the previous step are removed;
4. and (3) corrosion: and performing metallographic corrosion on the sample by adopting a mixed solution of acetic acid, nitric acid and phosphoric acid.
Preferably, the cold insert in the second step is prepared from 100g of liquid epoxy resin and 15g of epoxy curing agent.
Preferably, a vacuum impregnation device is adopted for vacuumizing in the second step, the vacuum pressure is 90kPa, and the required time is 2min.
Further, the sand paper in the third step is 800 meshes, 1000 meshes, 2500 meshes or 4000 meshes of silicon carbide water sand paper.
Furthermore, the sample grinding medium in the third step is absolute ethyl alcohol, and when the sample is ground and the sand paper is replaced, the sample is immediately immersed into the absolute ethyl alcohol solution to prevent oxidation.
Further, the proportion of acetic acid, nitric acid and phosphoric acid in the four corrosive agents is (5-50) mL: (5-15) mL: (5-40) mL, wherein the mass percentage concentration of the acetic acid is 99.8%, the mass percentage concentration of the nitric acid is 65%, and the mass percentage concentration of the phosphoric acid is 85%. Preferably, acetic acid (10 mL), nitric acid (10 mL) and phosphoric acid (10 mL) are mixed.
Furthermore, the corrosion mode is that absorbent cotton is dipped in the corrosive agent and the surface of the sample is wiped for 5-30s at the temperature of 15-35 ℃, and the room temperature is preferred.
The invention has the beneficial effects that:
1. the method breaks through the traditional process that metallographic sample preparation needs five steps of sampling → embedding → grinding → polishing → corroding, directly corrodes after sampling, embedding and grinding, and does not need polishing, so that the high-purity yttrium target metallographic structure characterization sample can be prepared, the process flow is simple and convenient, a polishing disc and a polishing agent are not needed, the operation efficiency is improved, and meanwhile, metallographic experiment consumables are effectively saved.
2. The metallographic corrosive disclosed by the invention corrodes the yttrium target material through the synergistic effect of acetic acid and nitric acid in a specific proportion, and in consideration of the fact that the yttrium target material is active in property, phosphoric acid is added as a corrosion inhibitor, phosphate precipitates generated by the reaction of the phosphoric acid and high-purity metal yttrium are attached to the surface of a matrix to form a passivation film, the corrosion capability of the corrosive is controlled, the corrosion capability of the corrosive is prevented from being too strong, and the corrosion time is not easy to control.
3. The method can effectively fill up the gap of the metallographic sample preparation technology of the high-purity yttrium target material.
4. The invention adopts a cold-inlaid mode, effectively protects the edge and simultaneously avoids the tissue change and the false image caused by heating the rare earth yttrium target material.
5. According to the method, absolute ethyl alcohol is used as cooling liquid instead of water cooling during sample grinding, and when the sand paper is replaced during sample grinding, the sample is immersed in the absolute ethyl alcohol, so that the reaction of the high-purity yttrium target material with water and air during sample grinding is effectively prevented, and the real tissue of the rare earth yttrium target material is further influenced.
6. According to the invention, the silicon carbide abrasive paper with a fineness of 500 meshes or more is selected as a sample grinding medium for the first pass, so that the problems of over deep scratch, thickening of a deformation layer and the like caused by the soft rare earth yttrium target material in the sample grinding of 80 meshes or 120 meshes or 240 meshes are avoided.
Drawings
FIG. 1 is a microstructure image of the high purity yttrium target prepared in example 1;
FIG. 2 is a microstructure image of the high purity yttrium target prepared in example 2;
3.1-3.4 are microstructure images of the high purity yttrium target prepared in example 3;
FIGS. 4.1-4.4 are microstructure images of the high purity yttrium target prepared in example 4;
FIGS. 5.1-5.3 are microstructure images of the high purity yttrium target prepared in example 5;
FIGS. 6.1-6.3 are microstructure images of the high purity yttrium target prepared in example 6;
FIGS. 7.1-7.3 are microstructure images of the high purity yttrium target prepared in example 7;
FIG. 8 is a flow chart of a sample preparation method of the present invention.
Detailed Description
The invention is described in further detail below with reference to the figures and specific examples. The technical solution of the present invention is not limited to the following embodiments, but includes any combination between the embodiments.
Referring to fig. 8, a short-flow, environment-friendly microscopy sample preparation method for high-purity rare earth metal Er comprises the following steps:
example 1
1) Sampling: and cutting out the high-purity yttrium target material with the purity of 99.999% by adopting linear cutting to obtain a rare earth yttrium metal sample with smooth and flat ground surface and the thickness of 15mm.
2) Cold inlaying: weighing 100g of liquid epoxy resin and 15g of epoxy curing agent, fully stirring uniformly, placing a sample in a cold-insert mold with a ground surface facing downwards, adding a cold-insert material uniformly stirred into the mold to completely immerse the sample, vacuumizing by adopting a vacuum impregnation device under the pressure of 90kPa, keeping the vacuum for 2min, curing at room temperature for 18h, and demolding to obtain the cold-insert sample.
3) Grinding: the method is characterized in that absolute ethyl alcohol is used as a grinding sample cooling medium, lubricating oil is dripped on the abrasive paper, cold embedded samples are sequentially ground on 800-mesh, 1000-mesh, 2500-mesh and 4000-mesh silicon carbide abrasive paper from coarse to fine step by step, a sample is immersed in the absolute ethyl alcohol when the abrasive paper is replaced, after the next time of abrasive paper fixation, the sample is taken out and is rotated by 90 degrees to continue grinding, after the last time of abrasive paper grinding, the grinding surface has a good light reflecting effect, and fine scratches can be uniformly arranged.
4) And (3) corrosion: performing metallographic corrosion on the yttrium metal sample by using a corrosive agent; the corrosive agent is prepared from acetic acid: nitric acid: phosphoric acid =10mL:10mL of: 10mL, wherein the mass percent concentrations of the used acid solvent are respectively as follows: 99.8 percent of acetic acid, 65 percent of nitric acid and 85 percent of phosphoric acid; and (3) dipping absorbent cotton into the corrosive agent, wiping the surface of the sample for 15s, immediately washing the surface of the sample by absolute ethyl alcohol, drying by cold air, and observing under a microscope.
Fig. 1 is a microstructure image obtained by the present embodiment, in which the yttrium target material has an obvious grain boundary profile and a distinct grain morphology.
Example 2
This embodiment differs from example 1 in that: the liquid epoxy resin in the step 2): the proportion of the epoxy curing agent is 120g: and 20g, vacuumizing by using a vacuum impregnation device under the pressure of 90kPa, curing at room temperature for 12h, and demolding to obtain a cold-inlaid sample. The rest is the same as in example 1.
Fig. 2 is a microstructure image obtained by the present embodiment, in which the yttrium target material has an obvious grain boundary profile and a clear and identifiable grain morphology.
Example 3
The time of the wiping corrosion is controlled to be 5-30 s; the etching time was changed from 15s of the wiping etching time in example 1; the method is changed as follows:
example 3-method 1: etching time =5s;
example 3-method 2: etch time =30s;
example 3-method 3: etching time =2s;
example 3-method 4: etch time =60s;
the other process steps were kept in accordance with example 1, and the samples obtained were observed under a microscope, the results being shown in FIGS. 3.1 to 3.4.
From the above results, it is understood that when the etching time is controlled to 5 to 30 seconds in examples 1 and 3-methods 1 to 2, a real and clear microstructure of the yttrium target can be obtained, and when the sample is etched at other times such as in examples 3-methods 3 to 4, it is difficult to obtain an ideal metallographic structure. When the method 3 is adopted for corrosion, because the time is too short, the reaction time of the yttrium target and the corrosive agent is short, the scratches on the surface of the sample are more remained, and the metallographic structure of the sample cannot be completely shown; when the method 4 is adopted for corrosion, the corrosion of the surface of the yttrium target is serious and the metallographic structure is blurred after a long time.
Example 4
The corrosive of the invention comprises the following components: nitric acid: phosphoric acid = (5-50) mL: (5-15) mL: (5-40) mL; the dosage of each acid solvent in the corrosive is changed, and the proportion of the corrosive in the example 1 is that acetic acid: nitric acid: phosphoric acid =10mL:10mL of: 10mL; the method is changed into the following steps:
example 4-method 1: acetic acid: nitric acid: phosphoric acid =5mL:15mL of: 40mL;
example 4-method 2: acetic acid: nitric acid: phosphoric acid =50mL:5mL of: 5mL;
example 4-method 3: acetic acid: nitric acid: phosphoric acid =55mL:2mL of: 3mL;
example 4-method 4: acetic acid: nitric acid: phosphoric acid =3mL:12mL of: 45mL;
the other process steps were kept in accordance with example 1, and the obtained samples were observed under a microscope, and the results are shown in FIGS. 4.1 to 4.4.
From the above results, the etchant ratio directly affects the texture display effect of the yttrium target. Example 1 and example 4-methods 1-2 the ratio of the controlled corrosive was acetic acid: nitric acid: phosphoric acid = (5-50) mL: (5-15) mL: (5-40) mL, and a metallographic structure photograph with an obvious grain boundary profile and clear and distinguishable crystal grain morphology can be obtained by observing under a microscope. Other proportions are adopted, the selective corrosion action on the grain boundary and the grain interior of the sample is poor, and the ideal yttrium target metallographic structure is difficult to obtain. Wherein, the yttrium target material is corroded according to the proportion of the corrosive agent in the embodiment 4-the method 3, the grain boundary of the sample is not completely shown, and the appearance of the grain is fuzzy; when the corrosion is carried out according to the proportion of the embodiment 4 to the method 4, the crystal face of the sample is seriously corroded, the metallographic structure is blackened and darkened, and the related analytical research work cannot be effectively carried out.
Example 5
In the corrosive of the invention, the mixed solution of acetic acid, nitric acid and phosphoric acid is used as the corrosive, the type of the corrosive is changed, and the acetic acid is controlled by the embodiment 1: nitric acid: phosphoric acid =10mL:10mL of: 10mL; the method is changed as follows:
example 5-method 1: corroding the sample by using a 4% nitric acid alcohol solution;
example 5-method 2: corroding the sample by using a solution prepared from 2mL of hydrofluoric acid (20 wt%), 3mL of nitric acid (65 wt%), 5mL of hydrochloric acid (37 wt%) and 190mL of water;
example 5-method 3: the sample is corroded with 10 to 20% NaOH aqueous solution.
The other process steps were in accordance with example 1, and the samples obtained were observed under a microscope, the results being shown in FIGS. 5.1 to 5.3.
From the above results, it is known that, when the method 1-3 of the present embodiment is used for etching, the obtained structures all have the problems of fuzzy grain boundary profile and unclear grain morphology, and it is difficult to obtain a relatively ideal metallographic etching effect.
Example 6
When the yttrium target material is ground, the used sand paper is not coarser than 500 meshes, the grinding medium is liquid which does not react with the yttrium target material and comprises absolute ethyl alcohol, and when the sand paper is replaced, the sample is immediately immersed into the absolute ethyl alcohol solution to prevent oxidation. The sample grinding mode of the yttrium target material is changed as follows:
example 6-method 1: in the grinding process, the silicon carbide sand paper is sequentially 800 meshes, 2500 meshes and 4000 meshes.
Example 6-method 2: in the grinding process, the used sand paper is 120-mesh, 240-mesh, 500-mesh, 1000-mesh and 2500-mesh silicon carbide water sand paper in sequence.
Example 6-method 3: in the grinding process, the grinding sample cooling medium is water.
The other process steps were in accordance with example 1, and the samples obtained were observed under a microscope, the results being shown in FIGS. 6.1 to 6.3.
Therefore, the grinding process parameters can obviously influence the tissue display effect of the yttrium target material. When the sandpaper which is not thicker than 500 meshes and the grinding cooling medium which is corresponding to the sandpaper of the embodiment 1 and the embodiment 6-the method 1 are adopted, the sample preparation effect can be more satisfactory; when the 120-mesh, 240-mesh, 500-mesh, 1000-mesh and 2500-mesh sandpaper described in the embodiment 6-method 2 is used for grinding, the scratches generated by the high-purity yttrium target material are too deep and are difficult to effectively remove in the subsequent process, and finally, when the high-purity yttrium target material is observed under a mirror, the scratches on the surface of the sample are more and the metallographic structure is blurred, so that the effective development of the microstructure analysis work of the high-purity yttrium target material is influenced. When water described in embodiment 6-method 3 is used as a cooling medium, the property of the high-purity yttrium target material is active, and the surface of a sample reacts with water in the grinding process, so that an oxide layer is generated on the surface of the sample after final corrosion, the metallographic structure is blurred, and the effective development of the microscopic structure analysis work of the yttrium target material is influenced.
Example 7
The preparation method is suitable for the high-purity metal yttrium target material, changes the type of the metal material, and adopts the high-purity yttrium target material with the purity of 99.999 percent in the embodiment 1; the method is changed as follows:
example 7-method 1: high-purity yttrium target material with the purity of 99.99 percent;
example 7-method 2: the purity of the high-purity titanium target material is 99.999 percent;
example 7-method 3: the purity of the high-purity nickel target material is 99.999 percent.
The other process steps were in accordance with example 1, and the obtained samples were observed under a microscope, and the results are shown in FIGS. 7.1 to 7.3, respectively.
It can be seen that the yttrium target materials described in example 1 and example 7-method 1 can obtain a satisfactory metallographic sample preparation effect by using the sample preparation process of the present invention, and the obtained metallographic structure has good contrast and clear crystal grain morphology. After the type of the metal material is changed, by adopting the sample preparation process, the surface of the titanium target material has obvious deformation interference layers and scratches, the surface of the nickel target material is densely provided with uniform and fine scratches, and the metallographic structures of the two metals are not shown. It can be known that the invention can not realize synchronous chemical polishing and metallographic corrosion to high-purity titanium target material, nickel target material, etc., and can not make metallographic structure successfully show.
The results show that the method is suitable for preparing the metallographic specimen of the high-purity yttrium target material, and the same test effect cannot be achieved by simply replacing other metal materials.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention, and not for limiting the same. Although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (5)
1. The preparation method of the high-purity yttrium target metallographic sample is characterized by comprising the following steps:
(1) Sampling: cutting out a rare earth yttrium target material sample by adopting linear cutting to obtain a cubic sample with a smooth and flat ground surface and a side length of (15-25) mm;
(2) Inlaying: weighing liquid epoxy resin and an epoxy curing agent, uniformly stirring, adding into a cold embedding mold with a prepared sample grinding surface facing downwards, vacuumizing, curing at room temperature for 8-24h, and demolding to obtain a cold embedding sample;
(3) Grinding: sequentially grinding the test sample on non-coarse 500-mesh silicon carbide abrasive paper, grinding each stage in the same direction, and rotating the sample by 45-135 degrees at the next stage until scratches of the previous stage are removed;
(4) And (3) corrosion: and performing metallographic corrosion on the sample by adopting a mixed solution of acetic acid, nitric acid and phosphoric acid.
2. The method of claim 1, wherein: the purity of the rare earth yttrium target material is more than or equal to 99.99 percent.
3. The method of claim 1, wherein: when the step (2) is inlaid, the ratio of the liquid epoxy resin to the epoxy curing agent is 90-120g:10-20g.
4. The method of claim 1, wherein: when in grinding, the used sand paper is not thicker than 500 meshes; the sample grinding medium is liquid which does not react with the yttrium target material chemically and comprises absolute ethyl alcohol; when the sandpaper was replaced, the sample was immediately immersed in an absolute ethanol solution to prevent oxidation.
5. The method of claim 1, wherein: the proportion of acetic acid, nitric acid and phosphoric acid in the corrosive agent is (5-50) mL: (5-15) mL: (5-40) mL, wherein the mass percentage concentration of acetic acid is 99.8%, the mass percentage concentration of nitric acid is 65%, the mass percentage concentration of phosphoric acid is 85%, and acetic acid is preferably: nitric acid: phosphoric acid =10mL:10mL of: 10mL; the corrosion mode is that absorbent cotton is dipped in the corrosive agent and the surface of the sample is wiped for 5-30s.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116930230A (en) * | 2023-06-15 | 2023-10-24 | 珠海市公安局刑事警察支队 | Pretreatment method for fire disaster bead electron microscope image acquisition |
| CN117907055A (en) * | 2024-01-17 | 2024-04-19 | 东北大学 | Preparation method of metallographic specimen of rare earth dysprosium |
Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0116483A1 (en) * | 1983-01-17 | 1984-08-22 | Rhone-Poulenc Chimie | Process for recovering uranium, yttrium, thorium and rare earth metals from an organic phase |
| CN102912302A (en) * | 2012-10-11 | 2013-02-06 | 厦门大学 | Method for preparing yttrium/silicon nitride compound coating material on surface of magnesium alloy |
| CN103698193A (en) * | 2013-12-16 | 2014-04-02 | 电子科技大学 | Application of corrosive liquid and corrosion method |
| CN104120299A (en) * | 2014-08-07 | 2014-10-29 | 大连理工大学 | Preparation method of yttrium-containing high-plasticity red copper |
| CN107976443A (en) * | 2017-11-24 | 2018-05-01 | 西北有色金属研究院 | A kind of observational technique of pure magnesium metallographic structure |
| CN109738444A (en) * | 2019-03-01 | 2019-05-10 | 株洲硬质合金集团有限公司 | A kind of method of quick detection tantalum, niobium and its alloy microstructure |
| CN110172612A (en) * | 2019-05-10 | 2019-08-27 | 河北工业大学 | A kind of high-strength corrosion-resistant erosion titanium zirconium-base alloy and preparation method thereof |
| CN110592457A (en) * | 2019-09-27 | 2019-12-20 | 太原理工大学 | Rare earth element high-entropy alloy material and preparation method thereof |
| CN111074279A (en) * | 2018-10-22 | 2020-04-28 | 宁波江丰电子材料股份有限公司 | Target corrosive agent and application method thereof |
| CN113234978A (en) * | 2021-05-08 | 2021-08-10 | 合肥诺瓦新材料科技有限公司 | Extruded magnesium-yttrium alloy and preparation method thereof |
| CN114509327A (en) * | 2021-11-26 | 2022-05-17 | 先导薄膜材料有限公司 | Display method of metallographic structure of tantalum target material |
-
2022
- 2022-09-23 CN CN202211164138.6A patent/CN115436134A/en active Pending
Patent Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0116483A1 (en) * | 1983-01-17 | 1984-08-22 | Rhone-Poulenc Chimie | Process for recovering uranium, yttrium, thorium and rare earth metals from an organic phase |
| CN102912302A (en) * | 2012-10-11 | 2013-02-06 | 厦门大学 | Method for preparing yttrium/silicon nitride compound coating material on surface of magnesium alloy |
| CN103698193A (en) * | 2013-12-16 | 2014-04-02 | 电子科技大学 | Application of corrosive liquid and corrosion method |
| CN104120299A (en) * | 2014-08-07 | 2014-10-29 | 大连理工大学 | Preparation method of yttrium-containing high-plasticity red copper |
| CN107976443A (en) * | 2017-11-24 | 2018-05-01 | 西北有色金属研究院 | A kind of observational technique of pure magnesium metallographic structure |
| CN111074279A (en) * | 2018-10-22 | 2020-04-28 | 宁波江丰电子材料股份有限公司 | Target corrosive agent and application method thereof |
| CN109738444A (en) * | 2019-03-01 | 2019-05-10 | 株洲硬质合金集团有限公司 | A kind of method of quick detection tantalum, niobium and its alloy microstructure |
| CN110172612A (en) * | 2019-05-10 | 2019-08-27 | 河北工业大学 | A kind of high-strength corrosion-resistant erosion titanium zirconium-base alloy and preparation method thereof |
| CN110592457A (en) * | 2019-09-27 | 2019-12-20 | 太原理工大学 | Rare earth element high-entropy alloy material and preparation method thereof |
| CN113234978A (en) * | 2021-05-08 | 2021-08-10 | 合肥诺瓦新材料科技有限公司 | Extruded magnesium-yttrium alloy and preparation method thereof |
| CN114509327A (en) * | 2021-11-26 | 2022-05-17 | 先导薄膜材料有限公司 | Display method of metallographic structure of tantalum target material |
Non-Patent Citations (1)
| Title |
|---|
| 姚素娟等: "钇对AZ91镁合金微观组织及腐蚀性能影响的研究", 中国稀土学报, vol. 25, no. 03, 30 June 2007 (2007-06-30) * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116930230A (en) * | 2023-06-15 | 2023-10-24 | 珠海市公安局刑事警察支队 | Pretreatment method for fire disaster bead electron microscope image acquisition |
| CN117907055A (en) * | 2024-01-17 | 2024-04-19 | 东北大学 | Preparation method of metallographic specimen of rare earth dysprosium |
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