CN114509327A - Display method of metallographic structure of tantalum target material - Google Patents

Display method of metallographic structure of tantalum target material Download PDF

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CN114509327A
CN114509327A CN202111446198.2A CN202111446198A CN114509327A CN 114509327 A CN114509327 A CN 114509327A CN 202111446198 A CN202111446198 A CN 202111446198A CN 114509327 A CN114509327 A CN 114509327A
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tantalum target
target material
grinding
polishing
metallographic structure
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丁跃跃
童培云
行卫东
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Leading Film Materials Anhui Co ltd
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Pilot Film Materials Co ltd
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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
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34—Sputtering
    • C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
    • C23C14/3414—Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy

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Abstract

The invention discloses a display method of a metallographic structure of a tantalum target material, and belongs to the technical field of preparation of metallographic samples. According to the method, the semiconductor tantalum target material with a clear and distinct metallographic structure of crystal grain boundaries is obtained by a reasonable grinding and polishing method, a corrosion liquid proportion and control of time of each stage, the approximate size and uniformity of observable crystal grains are set by an optical mirror ruler, and the crystal grain size and average grain size of the tantalum target material can be calculated by software.

Description

Display method for metallographic structure of tantalum target material
Technical Field
The invention relates to a display method of a metallographic structure of a tantalum target material, belonging to the technical field of preparation of metallographic samples.
Background
The pure tantalum target material is mainly used for preparing a diffusion barrier layer of a copper interconnection line and a silicon substrate in the advanced semiconductor technology and is a key material in a copper interconnection process. At present, a super-large-scale integrated circuit is gradually developed into a Cu/Ta sputtering target material, and along with the rapid development of the integrated circuit towards the direction of super-large scale and high operation speed, the tantalum sputtering target material becomes a key raw material of the semiconductor industry, has irreplaceability and has a very wide application prospect. In the sputtering process of the tantalum target material, the grain size and the texture orientation of the tantalum target material seriously affect the sputtering rate and the uniformity of a sputtered film, the internal structure of the material has direct and close relation with the material performances such as the hardness, the strength, the ductility and the like of the material, and metallographic observation is the most direct and effective method for researching the internal structure of the metal material.
CN101699253B discloses a display method of a metallographic structure of a target, which comprises providing a target, wherein the target is tantalum or a tantalum alloy; cutting a part of the target material to be used as a sample; carrying out surface treatment on the sample to form at least one polished surface; carrying out first corrosion treatment on the sample by using a first etching solution; then using a second etching solution to carry out second corrosion treatment on the sample; and observing the corroded sample by using a metallographic microscope. In the method, etching treatment with different proportions is required twice, so that the operation is complicated, the preparation time is long, the detection progress is influenced, and the detection cost is increased.
CN109738444A discloses a method for rapidly detecting metallographic structures of tantalum, niobium and alloys thereof, which comprises the following steps of (1) grinding a sample, namely grinding the plane of a tantalum, niobium and alloys thereof to be detected by a handheld grinding machine, (2) corroding the sample by adopting a soaking or pouring method, wherein a corrosive liquid is a mixed solution of hydrofluoric acid, concentrated nitric acid and concentrated sulfuric acid, then washing the mixed solution by water, and drying the residual water on the surface of the sample by blowing, and (3) observing the sample under a portable microscope. In the method, only the product with large sample size is macroscopically detected or directly detected, the processing and detection of the sample with smaller size cannot be met, the polishing procedure of the sample is omitted, the surface quality and the definition effect of a metallographic structure are poor, and the measurement precision of crystal grains is influenced.
In conclusion, the grain size and the texture orientation of the tantalum target are strictly controlled in the research and production processes of the tantalum target, the internal structure of the metal material is researched, the metallographic structure detection is particularly important, and the development of the display method of the metallographic structure of the semiconductor tantalum target is more important.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a display method of a metallographic structure of a tantalum target material, which comprises the steps of taking a picture and measuring the grain size from polishing to corrosion through an optical mirror, obtaining a semiconductor tantalum target material with a metallographic structure with clear grain boundaries through a reasonable polishing method, corrosion liquid proportioning and time control, setting the approximate size and uniformity of observable grains through an optical mirror ruler, and calculating the grain size and average grain size through software.
In order to achieve the purpose, the invention adopts the technical scheme that: a display method of a metallographic structure of a tantalum target material comprises the following steps:
(1) grinding: sequentially using abrasive paper with gradually increased granularity to perform coarse grinding, fine grinding and fine grinding on the surface of the tantalum target sample until the ground surface can observe a mirror surface, thus obtaining the ground tantalum target, wherein the direction of the coarse grinding and the fine grinding is 90 degrees, and the grinding direction of the fine grinding and the fine grinding is 90 degrees;
(2) polishing and cleaning: mechanically polishing and cleaning the ground tantalum target material to obtain a cleaned tantalum target material;
(3) and (3) corrosion: corroding the cleaned tantalum target material by adopting a soaking or pouring method for 2-40s, wherein the corrosion liquid is a mixed solution of hydrofluoric acid, nitric acid and sulfuric acid, then washing the tantalum target material by using pure water and absolute ethyl alcohol, and drying the surface of the sample by blowing, and the volume ratio of the hydrofluoric acid to the nitric acid to the sulfuric acid is 4:2: 1;
(4) and (4) observing the sample prepared in the step (3) under a metallographic microscope.
According to the invention, through a reasonable grinding and polishing method, corrosion liquid proportion and time control, the crystal phase structure display of the tantalum target material is realized, the metallographic microstructure of the tantalum target material is clear and visible, the grain boundary lines are clear and have no coarsening and overlapping, the approximate size and uniformity of observable grains are set through an optical mirror ruler, and the grain size and average grain size can be calculated through software.
According to the invention, a mixed solution of hydrofluoric acid, nitric acid and sulfuric acid is used as an etching solution, and the etching time is controlled, so that the etching solution can properly etch the surface of the tantalum target material, the crystal phase structure of the etched tantalum target material is clear and visible, and the grain boundary lines are clear and have no coarsening and overlapping.
Tantalum can be rapidly dissolved in mixed acid of hydrofluoric acid and nitric acid, and brownish red pungent gas is generated, and the reaction formula is as follows: 3Ta +5HNO3+21HF＝3H2[TaF7]+5NO↑+10H2O；2NO+O2＝2NO2↑。
If the corrosivity of the corrosive liquid is too high and the corrosion time is too long, the tantalum target material can be subjected to transitional corrosion and even completely dissolved, so that the coarsening and overlapping of crystal boundaries of crystal phase tissues of the tantalum target material are caused, the distinguishing effect is poor, and larger errors exist in the measurement of the grain size and the average grain size; if the corrosiveness of the corrosive liquid is too low, the surface of the tantalum target material is not corroded sufficiently, and the metallographic structure of the tantalum target material cannot be completely displayed.
As a preferable embodiment of the method for displaying the metallographic structure of the tantalum target material, the concentration of the hydrofluoric acid is more than or equal to 40%, the concentration of the nitric acid is 70-72%, and the concentration of the sulfuric acid is 95-98%.
According to the invention, by reasonably configuring the volume ratio and the mass percentage concentration of hydrofluoric acid, nitric acid and sulfuric acid in the corrosive liquid, if the content or the mass percentage concentration of any acid in the corrosive liquid is too small, the crystal phase structure on the surface of the tantalum target material is not clear due to insufficient corrosivity of the corrosive liquid, and the complete crystal phase structure with clear crystal boundaries cannot be observed; if the content or mass percentage concentration of any acid in the corrosive liquid is too large, the surface of the tantalum target is corroded and transited due to the too strong corrosivity of the corrosive liquid, and the crystalline phase structure of the tantalum target is damaged, so that the tantalum target cannot be observed. The inventor finds that the corrosive liquid prepared by hydrofluoric acid, nitric acid and hydrochloric acid according to the volume ratio of 4:2:1 under the mass percentage concentration has stable speed of corroding the tantalum target material, and the crystal phase structure and the crystal boundary of the corroded tantalum target material are clear.
In a preferred embodiment of the method for displaying the metallographic structure of the tantalum target material according to the invention, the sandpaper is 400# silicon carbide sandpaper, 1000# silicon carbide sandpaper or 2000# silicon carbide sandpaper.
The grinding method comprises the following specific steps: and (3) roughly grinding the surface of the tantalum target sample by using 400# silicon carbide abrasive paper along the same direction, finely grinding by using 1000# silicon carbide abrasive paper, and finally finely grinding by using 2000# silicon carbide abrasive paper until the mirror surface can be observed on the ground surface, so that the ground tantalum target can be obtained, wherein the directions of rough grinding and fine grinding form 90 degrees, and the grinding directions of fine grinding and fine grinding form 90 degrees.
In the whole grinding process, the correct grinding direction is kept, the smoothness of a grinding surface is ensured, multiple surfaces are avoided, the display of the crystal phase structure of the tantalum target material is influenced, the surface of the tantalum target material and the surface of new silicon carbide abrasive paper need to be cleaned before each abrasive paper is replaced, impurities on the surfaces of the tantalum target material and the new silicon carbide abrasive paper are prevented from being brought into the grinding process of the next stage, dirt on the surface of the tantalum target material can be removed through grinding, serious surface defects of an oxidant are eliminated, and preparation can be made for polishing of the next stage.
In addition, the rotating speed and time in the grinding process can influence the display result of the crystal phase structure of the tantalum target material, the rotating speed and time are too small, surface defects such as a deformation processing layer, scratches, oxidation and the like on the surface of the tantalum target material are not cleaned, and subsequent corrosion is influenced, so that the crystal phase structure of the tantalum target material cannot be completely displayed; the surface of the tantalum target material is seriously abraded due to overhigh rotating speed and overlong time, excessive corrosion can be caused during corrosion, and the display result of a crystalline phase structure is further influenced.
As a preferred embodiment of the method for displaying the metallurgical structure of the tantalum target material, the rotation speed of the coarse grinding is 250-350r/min, and the time t1 is 2-8 min.
As a preferred embodiment of the method for displaying the metallurgical structure of the tantalum target material, the rotation speed of the fine grinding is 300-400r/min, and the time t2 is 1-6 min.
As a preferred embodiment of the method for displaying the metallurgical structure of the tantalum target material, the rotation speed of the fine grinding is 300-400r/min, and the time t3 is 1-6 min.
As a preferred embodiment of the method for displaying the metallurgical structure of the tantalum target material, the mechanical polishing comprises the following steps: and mechanically polishing the ground tantalum target sample by using cashmere polishing cloth and a gold diamond spraying polishing agent.
And after the grinding, fine scratches and a surface deformation layer on the surface of the tantalum target material can be removed by mechanical polishing, and the rotation direction needs to be continuously removed in the mechanical polishing process, so that the surface of the tantalum target material becomes a scratch-free smooth mirror surface.
In addition, the rotation speed and time of the mechanical polishing can also have an influence on the subsequent processing of the tantalum target material. When the rotating speed and the time are too small, surface defects such as a deformation layer, scratches and the like on the surface of the tantalum target material are not well treated, and subsequent corrosion is influenced, so that the crystalline phase structure of the tantalum target material cannot be completely displayed; the surface of the tantalum target material is seriously abraded due to overhigh rotating speed and overlong time, excessive corrosion can be caused during corrosion, and the display result of a crystalline phase structure is further influenced.
As a preferred embodiment of the method for displaying the metallurgical structure of the tantalum target material, the rotation speed of the mechanical polishing is 350-450r/min, and the time t4 is 1-3 min.
Compared with the prior art, the invention has the beneficial effects that: according to the invention, through a reasonable grinding and polishing method, corrosion liquid proportion and time control, the crystal phase structure display of the tantalum target material is realized, the metallographic microstructure of the tantalum target material is clear and visible, the grain boundary lines are clear and have no coarsening and overlapping, the approximate size and uniformity of observable grains are set through an optical mirror ruler, and the grain size and average grain size can be calculated through software.
Drawings
FIG. 1 is a crystal phase structure diagram of a tantalum target according to example 1;
FIG. 2 is a crystal phase structure diagram of a tantalum target according to example 2;
FIG. 3 is a crystal phase structure diagram of a tantalum target according to example 3;
FIG. 4 is a crystal phase structure diagram of a tantalum target material in comparative example 1;
FIG. 5 is a structural diagram showing the crystal phase of a tantalum target material in comparative example 2;
FIG. 6 is a structural diagram showing the crystal phase of a tantalum target material in comparative example 3;
FIG. 7 is a structural diagram showing the crystal phase of the tantalum target material of comparative example 4.
Detailed Description
To better illustrate the objects, aspects and advantages of the present invention, the present invention will be further described with reference to the following detailed description and accompanying drawings.
The tantalum target material sample of the invention is preferably a sample with a regular shape, such as a cuboid, a cube, a cylinder and the like, and the thickness of the tantalum target material sample is 5-30 mm.
Example 1
The tantalum target material sample used in this example was a cuboid with a thickness of 20 mm.
The embodiment provides a method for displaying a crystalline phase structure of a tantalum target, which comprises the following steps:
(1) grinding: and (3) placing the 400# silicon carbide water grinding abrasive paper in a grinding disc of a grinding and polishing machine, operating the grinding and polishing machine to drive the grinding disc, setting the rotating speed at 300r/min, and setting the grinding time t1 to be 5 min. Starting a machine, placing the sample on sand paper in one direction for coarse grinding, and grinding off a deeper grinding mark and a surface processing deformation layer; then, 1000# silicon carbide abrasive paper is replaced for grinding, the rotating speed is set to be 350r/min, and the grinding time t2 is 3 min. At the moment, the grinding direction of the sample is rotated to form an angle of 90 degrees with the previous direction, so that scratches generated in the previous process are removed, the sample is ground until the ground surface is smooth, the scratches are further reduced, and stress generated in the previous process is reduced; and finally, replacing 2000# silicon carbide sand paper for continuous grinding, setting the rotating speed at 350r/min, and setting the grinding time t3 to be 2 min. Then the grinding direction is rotated to form a 90-degree direction with the last time until the ground surface has no scratch and the mirror surface can be observed, and the detection method is that the human image can be observed through the ground surface.
(2) Polishing and cleaning: using cashmere polishing cloth and a diamond spray polishing agent (W1.5 mu m), removing fine grinding marks and surface deformation layers left by fine grinding on a grinding surface, and continuously removing the rotation direction to enable the grinding surface to be a smooth mirror surface without scratches, wherein the rotation speed is set to 450r/min, and the polishing time t4 is 2 min; and (4) washing the grinding fluid and the polishing agent on the surface of the sample by using pure water, then washing by using alcohol, and drying the surface by using a blower.
(3) And (3) corrosion: immersing the cleaned tantalum target material into a corrosive liquid or corroding by adopting a pouring mode, and simultaneously, timing by pressing a stopwatch and observing the reaction rate; taking out the sample, quickly putting the sample into pure water for washing, then washing with alcohol and drying; wherein the corrosive liquid is prepared from hydrofluoric acid with the mass percentage concentration of 42%, nitric acid with the mass percentage concentration of 71% and sulfuric acid with the mass percentage concentration of 96% according to the volume ratio of 4:2: 1.
(4) And (4) observing the sample prepared in the step (3) under a metallographic microscope.
Example 2
The tantalum target material sample used in this example was a cuboid with a thickness of 30 mm.
The embodiment provides a method for displaying a crystalline phase structure of a tantalum target, which comprises the following steps:
(1) grinding: and (3) placing the 400# silicon carbide water grinding abrasive paper in a grinding disc of a grinding and polishing machine, operating the grinding and polishing machine to drive the grinding disc, setting the rotating speed at 250r/min, and setting the grinding time t1 to be 8 min. Starting a machine, placing the sample on sand paper in one direction for coarse grinding, and grinding off a deeper grinding mark and a surface processing deformation layer; then, the sample is ground by using 1000# silicon carbide abrasive paper, the rotating speed is set to be 300r/min, and the grinding time t2 is 6 min. At the moment, the grinding direction of the sample is rotated to form an angle of 90 degrees with the previous direction, so that scratches generated in the previous process are removed, the sample is ground until the ground surface is smooth, the scratches are further reduced, and stress generated in the previous process is reduced; and finally, replacing 2000# silicon carbide sand paper for continuous grinding, setting the rotating speed at 300r/min, and setting the grinding time t3 to be 6 min. Then the grinding direction is rotated to form a 90-degree direction with the last time until the ground surface has no scratch and the mirror surface can be observed, and the detection method is that the human image can be observed through the ground surface.
(2) Polishing and cleaning: using cashmere polishing cloth and a diamond spray polishing agent (W1-3 mu m), removing fine grinding marks and surface deformation layers left by fine grinding on a grinding surface, and continuously removing the rotation direction to enable the grinding surface to be a smooth mirror surface without scratches, wherein the rotation speed is set to 350r/min, and the polishing time t4 is 3 min; and (4) washing the grinding fluid and the polishing agent on the surface of the sample by using pure water, then washing by using alcohol, and drying the surface by using a blower.
(3) And (3) corrosion: immersing the cleaned tantalum target material into a corrosive liquid or corroding by adopting a pouring mode, and simultaneously, timing by pressing a stopwatch and observing the reaction rate; the corrosion time t is 25s, the sample is taken out, quickly placed into pure water for washing, washed by alcohol and dried; the corrosive liquid is prepared from 40% by mass of hydrofluoric acid, 70% by mass of nitric acid and 95% by mass of sulfuric acid according to the volume ratio of 4:2: 1.
(4) And (4) observing the sample prepared in the step (3) under a metallographic microscope.
Example 3
The tantalum target material sample used in this example was a cuboid with a thickness of 5 mm.
The embodiment provides a method for displaying a crystalline phase structure of a tantalum target, which comprises the following steps:
(1) grinding: and (3) placing the 400# silicon carbide water grinding abrasive paper in a grinding disc of a grinding and polishing machine, operating the grinding and polishing machine to drive the grinding disc, setting the rotating speed at 350r/min, and setting the grinding time t1 to be 5 min. Starting a machine, placing the sample on sand paper in one direction for coarse grinding, and grinding off a deeper grinding mark and a surface processing deformation layer; then, the sample is ground by using 1000# silicon carbide abrasive paper, the rotating speed is set to be 400r/min, and the grinding time t2 is 2 min. At the moment, the grinding direction of the sample is rotated to form a 90-degree angle with the last direction, so that scratches generated in the last process are removed, the sample is ground until the ground surface is flat, the scratches are further reduced, and stress generated in the last process is reduced; and finally, continuously grinding by replacing 2000# silicon carbide sand paper, setting the rotating speed at 400r/min, and setting the grinding time t3 to be 1 min. Then the grinding direction is rotated to form a 90-degree direction with the last time until the ground surface has no scratch and the mirror surface can be observed, and the detection method is that the human image can be observed through the ground surface.
(2) Polishing and cleaning: using cashmere polishing cloth and a diamond spray polishing agent (W1-3 mu m), removing fine grinding marks and surface deformation layers left by fine grinding on a grinding surface, and continuously removing the rotation direction to enable the grinding surface to be a smooth mirror surface without scratches, wherein the rotation speed is set to be 450r/min, and the polishing time t4 is 1 min; and (4) washing the grinding fluid and the polishing agent on the surface of the sample by using pure water, then washing by using alcohol, and drying the surface by using a blower.
(3) And (3) corrosion: immersing the cleaned tantalum target material into a corrosive liquid or corroding by adopting a pouring mode, and simultaneously, timing by pressing a stopwatch and observing the reaction rate; the corrosion time t is 5s, the sample is taken out, quickly placed into pure water for washing, washed by alcohol and dried; the corrosive liquid is prepared from 44% hydrofluoric acid, 72% nitric acid and 98% sulfuric acid according to the volume ratio of 4:2: 1.
(4) And (4) observing the sample prepared in the step (3) under a metallographic microscope.
Fig. 1 is a structural diagram of a crystal phase of a tantalum target according to example 1, fig. 2 is a structural diagram of a crystal phase of a tantalum target according to example 2, and fig. 3 is a structural diagram of a crystal phase of a tantalum target according to example 3, clear lines of grain boundaries of the tantalum target under different multiples can be observed from fig. 1-3, the structure of the crystal phase is clear, the grains are clear, and the lines of the grain boundaries are clear and have no coarsening and overlapping.
Comparative example 1
The only difference between the comparative example and the example 1 is the continuous rotation direction during the grinding process.
FIG. 4 is a structural diagram of the crystal phase of the tantalum target of the comparative example, which shows that the tantalum target has many scratches, which indicates that the continuous rotation direction during the grinding process can cause the surface defects such as scratches and oxidation on the surface of the tantalum target to be not completely eliminated, and the scratches are more and more, which affects the subsequent optical mirror image-taking effect and the grain size calculation; stress is increased when the direction is continuously rotated, and the later corrosion effect is influenced; the direction of the rotation is continuous, deviation is easy to generate, the sample is ground into multiple surfaces, and a bright and scratch-free mirror surface cannot be formed.
Comparative example 2
As a method for showing the crystal phase structure of the tantalum target material in the comparative example of the present invention, the only difference between the present comparative example and the example 1 is that the etching time is 45 s.
FIG. 5 is a structural diagram of the crystal phase of the tantalum target of the present comparative example, which shows that the corrosion liquid has too strong corrosivity and the corrosion time is long, so that the crystal phase structure of the tantalum target is destroyed due to the corrosion transition on the surface of the tantalum target, the grain boundary is coarsened and has a stereoscopic impression, and further the crystal phase structure cannot be observed, and the size of the crystal grain cannot be accurately measured.
Comparative example 3
The only difference between this comparative example and example 1 is that during the grinding process, the angle between the coarse grinding direction and the fine grinding direction is 120 °, and the angle between the fine grinding direction and the fine grinding direction is 120 °.
FIG. 6 is a structural diagram of the crystal phase of the tantalum target material of the comparative example, which shows that the grinding angle is 120 degrees, which always causes the crossing of the front and rear scratches, so that the scratches cannot be better processed, and the display effect of the corroded grain boundary is poor.
Comparative example 4
The only difference between the comparative example and the example 1 is that the mass percentage concentration of the nitric acid is 68%.
FIG. 7 is a crystal phase structure diagram of the tantalum target of this comparative example, in which the grain boundaries of the tantalum target are unclear and cannot be observed because the concentration of the etchant is low, and therefore, the size of the crystal grains cannot be accurately measured.
Finally, it should be noted that the above embodiments are intended to illustrate the technical solutions of the present invention and not to limit the scope of the present invention, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications and equivalent substitutions can be made to the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.

Claims (8)

1. A display method of a metallurgical structure of a tantalum target material is characterized by comprising the following steps:
(1) grinding: sequentially using abrasive paper with gradually increased granularity to perform coarse grinding, fine grinding and fine grinding on the surface of the tantalum target sample until the ground surface can observe a mirror surface, thus obtaining the ground tantalum target, wherein the direction of the coarse grinding and the fine grinding is 90 degrees, and the grinding direction of the fine grinding and the fine grinding is 90 degrees;
(2) polishing and cleaning: mechanically polishing and cleaning the ground tantalum target material to obtain a cleaned tantalum target material;
(3) and (3) corrosion: corroding the cleaned tantalum target material by adopting a soaking or pouring method for 2-40s, wherein the corrosion liquid is a mixed solution of hydrofluoric acid, nitric acid and sulfuric acid, then washing the tantalum target material by using pure water and absolute ethyl alcohol, and drying the surface of the sample by blowing, and the volume ratio of the hydrofluoric acid to the nitric acid to the sulfuric acid is 4:2: 1;
(4) and (4) observing the sample prepared in the step (3) under a metallographic microscope.
2. The method for displaying the metallographic structure of the tantalum target material as recited in claim 1, wherein a concentration of said hydrofluoric acid is not less than 40%, a concentration of said nitric acid is 70% -72%, and a concentration of said sulfuric acid is 95% -98%.
3. The method for displaying the metallographic structure of the tantalum target material according to claim 1, wherein the sandpaper is 400# silicon carbide sandpaper, 1000# silicon carbide sandpaper or 2000# silicon carbide sandpaper.
4. The method for displaying the metallographic structure of the tantalum target material as defined in claim 1, wherein the rotation speed of the rough grinding is 250-350r/min, and the time is t 1-2-8 min.
5. The method for displaying the metallographic structure of the tantalum target material as recited in claim 1, wherein the rotation speed of the fine grinding is 300-.
6. The method for displaying the metallographic structure of the tantalum target material as recited in claim 1, wherein the rotation speed of the fine grinding is 300-.
7. The method for displaying the metallographic structure of the tantalum target material according to claim 1, wherein the mechanical polishing comprises the following steps: and mechanically polishing the ground tantalum target sample by using cashmere polishing cloth and a gold diamond spraying polishing agent.
8. The method for displaying the metallographic structure of a tantalum target material as claimed in claim 6, wherein the rotation speed of the mechanical polishing is 350-450r/min, and the time is t 4-1-3 min.
CN202111446198.2A 2021-11-26 2021-11-26 Display method of metallographic structure of tantalum target material Pending CN114509327A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115436134A (en) * 2022-09-23 2022-12-06 国标（北京）检验认证有限公司 Metallographic structure characterization method of high-purity yttrium target material

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115436134A (en) * 2022-09-23 2022-12-06 国标（北京）检验认证有限公司 Metallographic structure characterization method of high-purity yttrium target material

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