Nickel-vanadium target metallographic etchant for semiconductor and metallographic structure display method

By using specific configurations of hydrofluoric acid and nitric acid corrosion liquid, combined with mechanical grinding and polishing treatment, the clarity of the metallographic structure of the nickel-vana target is significantly improved, the problem of unclear grain boundaries in the prior art is solved, and effective monitoring of the nickel-vana target preparation process is achieved.

CN119958944APending Publication Date: 2025-05-09PIONEER FILM MATERIALS (ANHUI) CO LTD
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Patent Information

Application Number
CN202510235678.6
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-02-28
Publication Date
2025-05-09

AI Technical Summary

Technical Problem

The prior art is difficult to effectively display the metallographic structure of nickel-vana targets, resulting in unclear grain boundaries, difficult to observe and analyze, and commonly used corrosion liquids are prone to volatilization, increasing operational risks.

Method used

The metallographic corrosion liquid of a specific concentration configured of hydrofluoric acid, nitric acid and water is used to flatten the surface of the nickel-vana target through mechanical grinding and polishing. The target material is then corroded with the gradient water flow flushing and hot air flow drying, which significantly improves the clarity of the grain boundary.

Benefits of technology

It realizes a clear display of the grain boundaries of nickel-vana targets, avoids excessive corrosion, reduces operational risks, and improves the observation and analysis effect of metallographic structure.

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Abstract

The invention discloses a nickel-vanadium target metallographic etchant for a semiconductor and a metallographic structure display method, and belongs to the technical field of metal surface treatment. The metallographic etchant is prepared from hydrofluoric acid, nitric acid and water according to the volume ratio of 1: 1: (6-10); wherein the mass fraction of hydrofluoric acid is greater than or equal to 40%, and the mass fraction of nitric acid is 70%-72%. The target material is mechanically ground through abrasive paper with different mesh numbers, then mechanically polished, uniformly infiltrated by adopting the metallographic phase corrosive liquid, and washed by gradient water flow after corrosion; under the reasonable grinding and polishing method, corrosive liquid ratio and time control, clear and non-coarsened and overlapped nickel-vanadium target crystal boundary lines can be observed through a metallographic microscope, crystal grains are clear and uniform, the metallographic display method is convenient to observe and analyze, and the nickel-vanadium target preparation process can be monitored in real time.
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Description

Technical Field

[0001] The invention belongs to the technical field of metal surface treatment, and in particular relates to a metallographic etching solution for a nickel-vanadium target material for semiconductors and a metallographic structure display method. Background Art

[0002] Nickel-vanadium sputtering target is made by adding vanadium to nickel melt during the preparation of nickel-vanadium alloy, so that the prepared alloy is more conducive to magnetron sputtering. It combines the advantages of nickel sputtering target and vanadium sputtering target, and can complete the sputtering of nickel layer (bonding layer) and vanadium layer (barrier layer) at one time. Nickel-vanadium alloy is non-magnetic, which is conducive to magnetron sputtering. In the electronics and information industry, it has completely replaced pure nickel sputtering target. Nickel-vanadium target has a wide range of applications. In chip manufacturing, it is used to prepare bonding layer and barrier layer to prevent diffusion between different metal layers and improve chip performance and stability. Not only that, it also has many application scenarios in the fields of optics, aerospace and mechanical manufacturing. It is mainly used for surface coating of parts and components to improve the high temperature resistance and corrosion resistance of parts and components and increase their service life. The prepared sputtering nickel-vanadium target requires high purity, less impurities, uniform chemical composition, no segregation, no pores, uniform grain structure, and grain size of micrometer-millimeter level. The grain size difference in a single sputtering target is as small as possible. In this way, discharge is not likely to occur during magnetron sputtering, and the magnetron sputtered film is uniform.

[0003] During the sputtering process, the grain size and texture orientation of the nickel-vanadium target seriously affect the sputtering rate and the uniformity of the sputtered film. The internal structure of the material has a direct and close relationship with the material properties such as hardness, strength, and ductility. The coating quality is closely related to the study of nickel-vanadium metallography. Metallographic observation is the most direct and effective method to study the internal structure of metal materials. Through metallographic analysis, it can be observed whether the grains are uniform and further detect the grain size, and the perfection of the process preparation can also be explored. From the literature that can be consulted at present, it is known that there are very few metallographic corrosion methods for nickel-vanadium alloy targets, and the corrosion resistance of nickel-vanadium alloys makes it difficult for ordinary corrosive liquids to make the grain boundaries clearly displayed. More research is done on the metallographic phase of pure nickel with similar properties to nickel-vanadium. For example, in the patent document CN114199657A "A metallographic etchant and a method for displaying metallographic structures", the pure nickel target is hot-mounted and ground on sandpaper of different particle sizes in a handheld manner, and finally polished with a polyurethane polishing pad and three types of aluminum oxide polishing agents of different particle sizes, and then polished with glycerin as a polishing agent and then placed in an etchant for corrosion. The preparation process of this method is cumbersome, the operation time is long, which affects the progress of detection and increases time costs. Patent document CN 104878389 A "A pure nickel metallographic etchant and its corrosion method" mentions a pure nickel metallographic etchant and its corrosion method. The mechanical grinding of the sample is time-consuming and demanding, and volatile nitric acid is also used, which increases the risk to personnel during the preparation of the etchant.

[0004] There is no reference literature on the metallographic development of nickel-vanadium alloys. Therefore, a metallographic etching solution for nickel-vanadium target materials for semiconductors and a metallographic structure display method are urgently needed to determine the perfection of the nickel-vanadium alloy target preparation process. Summary of the invention

[0005] One of the purposes of the present invention is to provide a nickel-vanadium target metallographic etching solution for semiconductors to solve the problem that the metallographic structure of the nickel-vanadium target is not clear and difficult to observe and distinguish;

[0006] The second object of the present invention is to provide a method for displaying the metallographic structure of a nickel-vanadium target for semiconductors, by which the uniformity of the nickel-vanadium target grains can be observed at any time through metallographic analysis, thereby monitoring the nickel-vanadium target preparation process.

[0007] The purpose of the present invention can be achieved by the following technical solutions:

[0008] In the first aspect, a metallographic etching solution for a nickel-vanadium target for semiconductors is prepared by mixing hydrofluoric acid, nitric acid and water in a volume ratio of 1:1:(6-10); wherein the mass fraction of hydrofluoric acid is ≥40%, and the mass fraction of nitric acid is 70%-72%.

[0009] In a second aspect, a method for displaying the metallographic structure of a nickel-vanadium target for semiconductors adopts the metallographic etching solution described in the first aspect, comprising the following steps:

[0010] Step 1, mechanical grinding: the nickel-vanadium target is grinded with 240#, 400#, 1000#, 2000#, and 3000# silicon carbide water-abrasive sandpaper in sequence until the grinding surface presents a mirror surface. Each time the sandpaper is changed, the grinding direction is kept perpendicular to the previous grinding direction to obtain the ground nickel-vanadium target;

[0011] Step 2, mechanical polishing: Use cashmere polishing cloth and polishing agent to mechanically polish the ground nickel-vanadium target material until the ground surface is a smooth mirror surface without scratches;

[0012] Step 3, metallographic etching liquid etching: evenly drop the metallographic etching liquid on the surface to be tested of the polished nickel-vanadium target material to make it in a complete contact state;

[0013] Step 4, cleaning and drying: After the corrosion is completed, the corrosion surface is rinsed according to the gradient water flow flushing procedure, and then dried with hot air flow;

[0014] Step 5: Inspection: Observation and inspection under a metallographic microscope.

[0015] As a further solution of the present invention, in step 1, the nickel-vanadium target material is a three-dimensional regular shape, including a cube, a cuboid, and a cylinder, and has a thickness of 5-30 mm.

[0016] As a further solution of the present invention, in step 1, when grinding with 240# silicon carbide water-abrasive sandpaper, the grinding speed is 250-350 r / min, and the grinding time is 4-8 min.

[0017] As a further solution of the present invention, in step 1, when 400# silicon carbide water-abrasive sandpaper is used for grinding, the grinding speed is 350-450 r / min and the grinding time is 4-6 min.

[0018] As a further solution of the present invention, in step 1, when 1000#, 2000#, 3000# silicon carbide water-abrasive sandpaper is used for grinding, the grinding speed is 300-400r / min, and the grinding time is 4-6min.

[0019] As a further solution of the present invention, in step 2, the polishing agent is aluminum oxide with a particle size of 1-3 μm.

[0020] As a further solution of the present invention, in step 2, the polishing rotation speed is 500-800 r / min, and the polishing time is 2-5 min.

[0021] As a further solution of the present invention, in step 3, the etching time of the metallographic etching solution is 120-150s.

[0022] As a further solution of the present invention, in step 4, the gradient water flow flushing degree is first flushing at a water flow rate of 2-6 m / s for 5-8 s, and then flushing at a water flow rate of 14-20 m / s for 10-15 s.

[0023] As a further solution of the present invention, in step 4, the hot air flow drying time is 3-5 minutes.

[0024] Compared with the prior art, the present invention has the following beneficial effects:

[0025] 1. The present invention provides a metallographic etching solution for a nickel-vanadium target material for semiconductors. The metallographic display of the nickel-vanadium target material is performed by using an etching solution of a specific concentration prepared from hydrofluoric acid, nitric acid and water. During the etching process, the hydrofluoric acid initially protects the metal surface by generating a fluoride film, but the corrosion rate at a high concentration will increase significantly, and the nitric acid further aggravates the corrosion process through oxidation. Through the coordinated cooperation of conditions such as the etching time, the grain boundaries of the nickel-vanadium target material can be corroded so that the grain boundaries are clearly displayed, the excessive corrosion is not easy, the erosion to the inside of the grain is small, the grain boundary lines are clear and there is no coarsening and overlap, which is convenient for observation and analysis. In addition, the etching solutions used are all conventional laboratory reagents with low cost, low concentration and high configuration safety.

[0026] 2. In the process of metallographic structure display of nickel-vanadium target material for semiconductor using metallographic etching liquid, the present invention firstly uses silicon carbide water-abrasive paper with increasing particle size for grinding through continuous metallographic display exploration. Among them, when grinding with 240# silicon carbide water-abrasive paper, the bottom is flattened by coarse grinding, and it is evenly pressed and fixed in the grinding disc of the grinding and polishing machine, and the grinding direction is adjusted to be perpendicular to the previous grinding direction. The 400# silicon carbide water-abrasive paper is replaced, and the scratches produced by the previous stage of grinding are removed by fine grinding, and then 1000#, 2000#, and 3000# silicon carbide water-abrasive paper are used for fine grinding three times in sequence. After five times of grinding with gradient particle size water-abrasive paper, the grinding surface presents a mirror effect and a clear portrait; secondly, mechanical polishing is used to remove the fine grinding residues remaining on the grinding surface after fine grinding. marks and surface deformation layer, so as to avoid scratches affecting the subsequent corrosion effect and the clarity of metallographic presentation; in addition, due to the sequential grinding of gradient particle size ink sandpaper, the electrolytic polishing step is omitted in this step, and a good polishing effect is also obtained, which effectively saves costs; in the corrosion stage, the metallographic corrosion liquid is evenly dripped and infiltrated to fully contact with the nickel-vanadium target material. Compared with completely placing the target material to be tested in the corrosion liquid, the corrosion intensity can be fully controlled and the detection effect is more accurate; by flushing with water at a gradient flow rate, the corrosion liquid is slowly flushed and diluted in a short time, and the residual corrosion liquid after dilution continues to corrode and deepen the grain boundary line, and then the residual corrosion liquid is washed away by rapid water flow for a long time, so that it is completely removed, and a clear grain boundary can be obtained after observation after drying. During the entire corrosion period, no wiping method is used. BRIEF DESCRIPTION OF THE DRAWINGS

[0027] The present invention will be further described below in conjunction with the accompanying drawings.

[0028] Figure 1 is a metallographic structure diagram of the nickel-vanadium target in Example 4 of the present invention;

[0029] Figure 2 is a metallographic structure diagram of the nickel-vanadium target in Example 5 of the present invention;

[0030] Figure 3 is a metallographic structure diagram of the nickel-vanadium target in Example 6 of the present invention;

[0031] Figure 4 is the metallographic structure diagram of the nickel-vanadium target in Comparative Example 3 of the present invention;

[0032] Figure 5 is the metallographic structure diagram of the nickel-vanadium target in Comparative Example 4 of the present invention;

[0033] Figure 6 is the metallographic structure diagram of the nickel-vanadium target in Comparative Example 5 of the present invention;

[0034] Figure 7 is the metallographic structure diagram of the nickel-vanadium target in Comparative Example 6 of the present invention;

[0035] Figure 8 is the metallographic structure diagram of the nickel-vanadium target in Comparative Example 7 of the present invention;

[0036] Fig. 9 is the metallographic structure diagram of the nickel-vanadium target in Comparative Example 8 of the present invention;

[0037] Fig.10 It is the metallographic structure diagram of the nickel-vanadium target in comparative example 9 of the present invention. DETAILED DESCRIPTION

[0038] The following will be combined with the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0039] Example 1

[0040] A metallographic etching solution for a nickel-vanadium target for semiconductors is prepared by the following steps:

[0041] In a fume hood, use a clean measuring cup to prepare HF:HNO3:H2O in a volume ratio of 2mL:2mL:16mL, where the mass fraction of HF is 50% and the mass fraction of HNO3 is 72%.

[0042] Example 2

[0043] A metallographic etching solution for a nickel-vanadium target for semiconductors is prepared by the following steps:

[0044] In a fume hood, use a clean measuring cup to prepare HF:HNO3:H2O in a volume ratio of 2mL:2mL:20mL, where the mass fraction of HF is 50% and the mass fraction of HNO3 is 72%.

[0045] Example 3

[0046] A metallographic etching solution for a nickel-vanadium target for semiconductors is prepared by the following steps:

[0047] In a fume hood, use a clean measuring cup to prepare HF:HNO3:H2O in a volume ratio of 2mL:2mL:12mL, where the mass fraction of HF is 50% and the mass fraction of HNO3 is 72%.

[0048] Example 4

[0049] A method for displaying the metallographic structure of a nickel-vanadium target material for semiconductors, using the metallographic etching solution configured in Example 1, comprises the following steps:

[0050] Step 1: Mechanical grinding: The nickel-vanadium target (N i-7wt% V) is processed into a cube with a thickness of 10mm, and 240# silicon carbide water-abrasive paper is placed in the grinding disc of the grinding and polishing machine, and the grinding and polishing machine is operated to drive the grinding disc, the speed is set to 300r / min, and the grinding time is t=6min; then 400# silicon carbide water-abrasive paper is replaced for grinding, the speed is set to 400r / min, and the grinding time is t=5min; at this time, the grinding direction of the sample is rotated to be perpendicular to the last grinding direction, the purpose is to remove the scratches generated in the previous process, and it is ground until the grinding surface is flat and the scratches are further reduced; then 1000# silicon carbide water-abrasive paper, 2000# silicon carbide water-abrasive paper, and 3000# silicon carbide water-abrasive paper are replaced in turn, the speed is set to 350r / min, the grinding time is t=5min, and they are ground separately, and the grinding direction of each time is perpendicular to the last grinding and polishing direction, until there are no scratches on the grinding surface and a mirror surface can be observed, and the detection method is that a clear portrait can be seen through the grinding surface;

[0051] Step 2, mechanical polishing: Use cashmere polishing cloth with aluminum oxide spray polishing agent (particle size is 1-3μm) to remove the fine wear marks and surface deformation layer left by mechanical grinding of the grinding surface. During the polishing process, continuously change the polishing direction to make the grinding surface a smooth mirror without scratches. Set the speed to 650r / min and the polishing time to 4min.

[0052] Step 3: Metallographic etching liquid corrosion:

[0053] Place the polished nickel-vanadium target in a vacuum drying oven, dry until the surface is dry, cool to room temperature (25-30°C), drop the metallographic etching solution evenly on the surface to be tested, so that it is infiltrated and in full contact. Start timing from the moment of contact, and the etching is completed after 130 seconds.

[0054] Step 4, cleaning and drying: After the corrosion is completed, place it under the flushing device and flush it for 6 seconds at a water flow rate of 4 m / s according to the preset gradient flushing program, and then flush it for 12 seconds at a water flow rate of 16 m / s. After the flushing is completed, use the built-in hot air drying device to blow the sample dry again within 3 minutes;

[0055] Step 5: Inspection: Use metallographic microscope to observe and inspect. The metallographic structure is as follows: Figure 1 shown.

[0056] Example 5

[0057] A method for displaying the metallographic structure of a nickel-vanadium target material for semiconductors, which is different from the method of embodiment 4 in that the metallographic etching solution configured in embodiment 2 is used and a metallographic microscope is used for observation and detection. Figure 2 shown.

[0058] Example 6

[0059] A method for displaying the metallographic structure of a nickel-vanadium target material for semiconductors, which is different from the method of embodiment 4 in that the metallographic etching solution configured in embodiment 3 is used and a metallographic microscope is used for observation and detection. Figure 3 shown.

[0060] from Figure 1 — Figure 3 It can be seen that after being corroded by metallographic etching liquid at a certain volume ratio, the nickel-vanadium target shows clear lines of grain boundaries, the metallographic structure is clearly visible, the grains are distinct, the grain boundary lines are clear without coarsening and overlap, and the use of concentration and volume ratio within this range can present the best metallographic effect.

[0061] Comparative Example 1

[0062] A metallographic etching solution for a nickel-vanadium target for semiconductors is prepared by the following steps:

[0063] In a fume hood, use a clean measuring cup to prepare HF:HNO3:H2O in a volume ratio of 2mL:2mL:5mL, where the mass fraction of HF is 50% and the mass fraction of HNO3 is 72%.

[0064] Comparative Example 2

[0065] A metallographic etching solution for a nickel-vanadium target for semiconductors is prepared by the following steps:

[0066] In a fume hood, use a clean measuring cup to prepare HF:HNO3:H2O in a volume ratio of 2mL:2mL:25mL, where the mass fraction of HF is 50% and the mass fraction of HNO3 is 72%.

[0067] Comparative Example 3

[0068] A method for displaying the metallographic structure of a nickel-vanadium target material for semiconductors, which is different from Example 4 in that the metallographic etching solution configured in Comparative Example 1 is used, and a metallographic microscope is used for observation and detection, and the metallographic structure is as follows Figure 4 shown.

[0069] Comparative Example 4

[0070] A method for displaying the metallographic structure of a nickel-vanadium target material for semiconductors, which is different from Example 4 in that the metallographic etching solution configured in Comparative Example 2 is used, and a metallographic microscope is used for observation and detection, and the metallographic structure is as follows Figure 5 shown.

[0071] pass Figure 4 and Figure 5 and Figure 1 — Figure 3By comparison, it can be seen that when the concentration of the etching solution is too low, the corrosion effect is poor, the grain boundary lines are unclear, and there is overlapping; when the concentration of the etching solution is too high, the corrosion phenomenon is serious, and then the interior of the grain is eroded.

[0072] Comparative Example 5

[0073] A method for displaying the metallographic structure of a nickel-vanadium target for semiconductors, using the metallographic etching solution configured in Example 1, is different from Example 4 in that, during the mechanical grinding process in step 1, 240#, 400# and 2000# silicon carbide water-abrasive paper are used in sequence for grinding, and step 1 is specifically as follows:

[0074] Step 1, mechanical grinding: the nickel-vanadium target (Ni-7wt%V) to be ground is processed into a cube with a thickness of 10mm, and 240# silicon carbide water-abrasive paper is placed in the grinding disc of the grinding and polishing machine, and the grinding and polishing machine is operated to drive the grinding disc, the speed is set to 300r / min, and the grinding time is t=6min; then 400# silicon carbide water-abrasive paper is replaced for grinding, the speed is set to 400r / min, and the grinding time is t=5min; at this time, the grinding direction of the sample is rotated perpendicular to the last grinding direction, the purpose is to remove the scratches generated in the previous process, and it is ground until the grinding surface is flat and the scratches are further reduced; then 2000# silicon carbide water-abrasive paper is replaced, the speed is set to 350r / min, and the grinding time is t=15min;

[0075] The remaining steps and parameters are the same as those in Example 4;

[0076] The metallographic microscope was used to observe and detect the metallographic structure. Figure 6 shown.

[0077] contrast Figure 1 and Figure 6 By using sandpaper of different mesh sizes for grinding in the fine grinding stage, surface defects such as scratches on the surface of the nickel-vanadium target can be further eliminated, which is beneficial to the uniform infiltration of the corrosive liquid, and thus to the imaging effect of the metallographic microscope, thereby realizing real-time detection of the nickel-vanadium target preparation process.

[0078] Comparative Example 6

[0079] A method for displaying the metallographic structure of a nickel-vanadium target for semiconductors, using the metallographic etching solution configured in Example 1, which is different from Example 4 in that in step 3, the etching time is 180 seconds;

[0080] The remaining steps and parameters are the same as those in Example 4;

[0081] The metallographic microscope was used to observe and detect the metallographic structure. Figure 7 shown.

[0082] Comparative Example 7

[0083] A method for displaying the metallographic structure of a nickel-vanadium target for semiconductors, using the metallographic etching solution configured in Example 1, which is different from Example 4 in that in step 3, the etching time is 100 seconds;

[0084] The remaining steps and parameters are the same as those in Example 4;

[0085] The metallographic microscope was used to observe and detect the metallographic structure. Figure 8 shown.

[0086] contrast Figure 7 , Figure 8 and Figure 1 If the etching time is too short, the etching effect is not good and the grain boundary lines are not clear; if the etching time is too long, the grain boundaries will coarsen and the crystal phase structure will be destroyed, making it impossible to accurately measure the grain size.

[0087] Comparative Example 8

[0088] A method for displaying the metallographic structure of a nickel-vanadium target for semiconductors, using the metallographic etching solution configured in Example 1, which is different from Example 4 in that, in step 3, the polished nickel-vanadium target is etched by immersing it in the metallographic etching solution for 130 seconds;

[0089] The remaining steps and parameters are the same as those in Example 4;

[0090] The metallographic microscope was used to observe and detect the metallographic structure. Fig. 9 shown.

[0091] contrast Fig. 9 and Figure 1 Completely immersing the nickel-vanadium target in the metallographic etching solution will lead to excessive corrosion and coarse metallographic grain boundaries, affecting the detection accuracy.

[0092] Comparative Example 9

[0093] A method for displaying the metallographic structure of a nickel-vanadium target for semiconductors, using the metallographic etching solution configured in Example 1, which is different from Example 4 in that, in step 4, a water flow with a flow rate of 10 m / s is used for flushing for 15 seconds;

[0094] The remaining steps and parameters are the same as those in Example 4;

[0095] The metallographic microscope was used to observe and detect the metallographic structure. Fig.10 shown.

[0096] contrast Fig.10 and Figure 1By flushing with gradient water flow, the degree of corrosion can be further controlled, and the residual amount of dilution liquid can be controlled to deepen the grain boundary lines of the nickel-vanadium target. Rapid water flow flushing can take away the residual corrosive liquid so that it can be completely removed. After drying, clear grain boundaries can be observed.

[0097] The invention mechanically grinds the target material by sandpapers of different meshes, and then mechanically polishes it, and then uses the metallographic etching liquid to uniformly infiltrate it, and then washes it with gradient water flow after etching; under reasonable grinding and polishing methods, etching liquid ratio and time control, a metallographic microscope can observe clear nickel-vanadium target grain boundary lines without coarsening and overlap, and the grains are clear and uniform. The metallographic display method is convenient for observation and analysis, and can realize real-time monitoring of the nickel-vanadium target preparation process.

[0098] It should be noted that, in this article, relational terms such as first and second, etc. are only used to distinguish one entity or operation from another entity or operation, and do not necessarily require or imply any such actual relationship or order between these entities or operations. Moreover, the terms "include", "comprises" or any other variations thereof are intended to cover non-exclusive inclusion, so that a process, method, article or device including a series of elements includes not only those elements, but also other elements not explicitly listed, or also includes elements inherent to such process, method, article or device.

[0099] Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and variations may be made to the embodiments without departing from the principles and spirit of the present invention, and that the scope of the present invention is defined by the appended claims and their equivalents.

Claims

1. A nickel-vanadium target metallographic etching solution for semiconductor, characterized in that: It is prepared by mixing hydrofluoric acid, nitric acid and water in a volume ratio of 1:1:(6-10); wherein the mass fraction of hydrofluoric acid is ≥40%, and the mass fraction of nitric acid is 70%-72%.

2. A method for displaying the metallographic structure of a nickel-vanadium target for semiconductors, characterized in that: Using the metallographic etching solution according to claim 1, comprising the following steps: Step 1, grinding the nickel-vanadium target material with 240#, 400#, 1000#, 2000#, and 3000# silicon carbide water-abrasive sandpaper in sequence until the grinding surface presents a mirror surface, and each time the sandpaper is changed, the grinding direction is kept perpendicular to the previous grinding direction to obtain the ground nickel-vanadium target material; Step 2, using cashmere polishing cloth and polishing agent to mechanically polish the ground nickel-vanadium target material until the ground surface is a smooth mirror surface without scratches; Step 3, evenly drop the metallographic etching solution on the surface to be tested of the polished nickel-vanadium target material to make it in a complete contact state; Step 4: After the corrosion is completed, the corrosion surface is rinsed according to the gradient water flow flushing procedure, and then dried with hot air flow; Step 5: Observe and inspect under a metallographic microscope.

3. A method for displaying the metallographic structure of a nickel-vanadium target for semiconductor according to claim 2, characterized in that: In the step 1, the nickel-vanadium target material is a three-dimensional regular shape with a thickness of 5-30 mm.

4. A method for displaying the metallographic structure of a nickel-vanadium target for semiconductor according to claim 2, characterized in that: In the step 1, when 240# silicon carbide water-abrasive sandpaper is used for grinding, the grinding speed is 250-350 r / min and the grinding time is 4-8 min.

5. The method for displaying the metallographic structure of a nickel-vanadium target for semiconductor according to claim 2, characterized in that: In the step 1, when 400# silicon carbide water-abrasive sandpaper is used for grinding, the grinding speed is 350-450 r / min and the grinding time is 4-6 min.

6. A method for displaying the metallographic structure of a nickel-vanadium target for semiconductor according to claim 2, characterized in that: In the step 1, when 1000#, 2000#, 3000# silicon carbide water-abrasive sandpaper is used for grinding, the grinding speed is 300-400r / min, and the grinding time is 4-6min.

7. A method for displaying the metallographic structure of a nickel-vanadium target for semiconductor according to claim 2, characterized in that: In the step 2, the polishing agent is aluminum oxide with a particle size of 1-3 μm.

8. A method for displaying the metallographic structure of a nickel-vanadium target for semiconductor according to claim 2, characterized in that: In the step 2, the polishing speed is 500-800 r / min, and the polishing time is 2-5 min.

9. A method for displaying the metallographic structure of a nickel-vanadium target for semiconductor according to claim 2, characterized in that: In step 3, the etching time of the metallographic etching solution is 120-150s.

10. The method for displaying the metallographic structure of a nickel-vanadium target for semiconductor according to claim 2, characterized in that: In step 4, the gradient water flow flushing degree is first flushing at a water flow rate of 2-6 m / s for 5-8 s, and then flushing at a water flow rate of 14-20 m / s for 10-15 s.

Citation Information

Patent Citations

  • Pure-nickel metallographic etchant and corroding method using same

    CN104878389A

  • Metallographic etchant and display method of metallographic structure

    CN114199657A