Metallographic corrosion method of Ti-Ag alloy and Ti-Ag alloy

By machining, grinding, and polishing Ti-Ag alloys, and then treating them with a corrosion solution of ammonium bifluoride, hydrofluoric acid, and water, the problem of poor metallographic corrosion of Ti-Ag alloys was solved, resulting in clear corrosion of microstructures and improved detection efficiency.

CN121783659APending Publication Date: 2026-04-03西安汉唐分析检测有限公司
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-12-16
Publication Date
2026-04-03

AI Technical Summary

Technical Problem

In existing technologies, the metallographic corrosion effect of Ti-Ag alloys is poor, resulting in low detection efficiency and accuracy.

Method used

A combination of machining, grinding, polishing and etching solution treatment was used to perform planar microstructure observation of Ti-Ag alloy. The etching solution consisted of ammonium hydrogen fluoride, hydrofluoric acid and water, with a ratio of (5~10)g:(10~20)mL:100mL.

Benefits of technology

The microstructure is clear and uniform, which improves the efficiency and accuracy of metallographic testing. The operation is simple, stable and repeatable.

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Abstract

The invention provides a metallographic corrosion method of a Ti-Ag alloy and the Ti-Ag alloy, and relates to the technical field of metallographic detection. The metallographic corrosion method comprises the following steps: machining Ti-Ag alloy so as to form a microscopic structure observation plane on the Ti-Ag alloy; the microscopic structure observation plane is ground on a metallographic phase pre-grinding machine, and the ground microscopic structure observation plane is placed on a polishing machine to be subjected to mechanical polishing; etching the mechanically polished microscopic structure observation plane by using an etchant solution to obtain a microscopic structure observation plane to be observed; wherein the corrosion solution comprises ammonium hydrogen fluoride, hydrofluoric acid and water, and the ratio of the ammonium hydrogen fluoride to the hydrofluoric acid to the water is (5-10) g: (10-20) mL: 100 mL. According to the method, the metallographic corrosion effect of the Ti-Ag alloy can be improved.
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Description

Technical Field

[0001] This disclosure relates to the field of metallographic testing technology, and more specifically, to a metallographic corrosion method for Ti-Ag alloys and Ti-Ag alloys. Background Technology

[0002] Ti-Ag alloys are important biomedical metallic materials, and their excellent properties also have applications in other industrial fields. Ti-Ag alloys are not a single alloy with a fixed composition, but rather an alloy system in which the amount of silver added can be adjusted to obtain different properties. Its core characteristic is that the addition of silver significantly enhances the antibacterial properties of titanium while maintaining the excellent biocompatibility and mechanical properties of titanium itself.

[0003] Currently, etchants specifically designed for Ti are commonly used to perform metallographic etching on Ti-Ag alloys. However, this method suffers from poor metallographic etching results.

[0004] It should be noted that the information disclosed in the background section above is only used to enhance the understanding of the background of this disclosure, and therefore may include information that does not constitute prior art known to those skilled in the art. Summary of the Invention

[0005] The purpose of this disclosure is to provide a metallographic corrosion method for Ti-Ag alloys and a Ti-Ag alloy, thereby overcoming, at least to some extent, the problem of poor metallographic corrosion effect of Ti-Ag alloys.

[0006] According to a first aspect of this disclosure, a metallographic etching method for Ti-Ag alloys is provided, comprising: machining the Ti-Ag alloy to form a microstructure observation plane on the Ti-Ag alloy; grinding the microstructure observation plane on a metallographic pre-grinding machine and then mechanically polishing the ground microstructure observation plane on a polishing machine; etching the mechanically polished microstructure observation plane with an etching solution to obtain the microstructure observation plane to be observed; wherein the etching solution contains ammonium bifluoride, hydrofluoric acid and water, and the ratio of ammonium bifluoride, hydrofluoric acid and water is (5~10)g:(10~20)mL:100mL.

[0007] Optionally, grinding the microstructure observation plane on a metallographic pre-grinding machine includes: grinding the microstructure observation plane on the metallographic pre-grinding machine using metallographic wet sandpaper of different mesh sizes; wherein, each time the metallographic wet sandpaper is changed, the grinding direction is rotated by 90°.

[0008] Optionally, the microstructure observation plane is ground using metallographic wet sandpaper of different grits, including: grinding the microstructure observation plane with 120#, 800#, 1200# and 2000# metallographic wet sandpaper in sequence.

[0009] Optionally, during the mechanical polishing process, the polishing slurry used is SiO2 polishing slurry with a particle size of 0.25μm, and the polishing cloth is metallographic damping polishing cloth.

[0010] Optionally, etching the mechanically polished microstructure observation plane with an etching solution includes immersing the mechanically polished microstructure observation plane in an etching solution using an etching method.

[0011] Optionally, the corrosion time is 5~10s.

[0012] Optionally, the water is one or a mixture of tap water, purified water, deionized water, and distilled water.

[0013] Optionally, the metallographic etching method further includes: in the process of generating the etching solution, the order of preparation is water, ammonium bifluoride, and hydrofluoric acid added in sequence.

[0014] Optionally, hydrofluoric acid is an analytical grade reagent.

[0015] According to a second aspect of this disclosure, a Ti-Ag alloy is provided, including a microstructure observation plane prepared by the metallographic etching method of the above-described Ti-Ag alloy.

[0016] In the exemplary embodiment of this disclosure, a etching solution prepared by mixing (5-10) g ammonium bifluoride, (10-20) mL hydrofluoric acid, and 100 mL water is used to etch the surface of the Ti-Ag alloy. This rapidly etches a clear and uniform microstructure, improving the metallographic etching effect and thus enhancing detection efficiency and accuracy. Furthermore, this method requires no special equipment, is simple to operate, provides stable etching results, and exhibits high repeatability.

[0017] It should be understood that the above general description and the following detailed description are exemplary and explanatory only, and are not intended to limit this disclosure. Attached Figure Description

[0018] The accompanying drawings, which are incorporated in and form part of this specification, illustrate embodiments consistent with this disclosure and, together with the description, serve to explain the principles of this disclosure. It is obvious that the drawings described below are merely some embodiments of this disclosure, and those skilled in the art can obtain other drawings based on these drawings without any inventive effort.

[0019] Figure 1The results of metallographic etching of Ti-Ag alloys using some techniques are shown.

[0020] Figure 2 A flowchart illustrating the metallographic corrosion method for Ti-Ag alloys according to embodiments of the present disclosure is shown.

[0021] Figure 3 A schematic diagram of the microstructure of the Ti-Ag alloy of Example 1 of this disclosure is shown.

[0022] Figure 4 A schematic diagram of the microstructure of the Ti-Ag alloy of Example 2 of this disclosure is shown.

[0023] Figure 5 The microstructure of the Ti-Ag alloy of Example 3 of this disclosure is schematically shown.

[0024] Figure 6 A schematic diagram of the microstructure of the Ti-Ag alloy of Example 4 of this disclosure is shown.

[0025] Figure 7 A schematic diagram of the microstructure of the Ti-Ag alloy of Example 5 of this disclosure is shown.

[0026] Figure 8 A schematic diagram of the microstructure of the Ti-Ag alloy of Example 6 of this disclosure is shown. Detailed Implementation

[0027] Exemplary embodiments will now be described more fully with reference to the accompanying drawings. However, these exemplary embodiments can be implemented in many forms and should not be construed as limited to the examples set forth herein; rather, these embodiments are provided to make this disclosure more comprehensive and complete, and to fully convey the concept of the exemplary embodiments to those skilled in the art. The described features, structures, or characteristics can be combined in any suitable manner in one or more embodiments. In the following description, numerous specific details are provided to give a full understanding of embodiments of this disclosure. However, those skilled in the art will recognize that the technical solutions of this disclosure can be practiced with one or more of these specific details omitted, or other methods, processes, steps, etc., can be employed. In other instances, well-known technical solutions are not shown or described in detail to avoid obscuring various aspects of this disclosure.

[0028] Furthermore, the accompanying drawings are merely illustrative of this disclosure and are not necessarily drawn to scale. The same reference numerals in the drawings denote the same or similar parts, and therefore repeated descriptions of them will be omitted. The flowcharts shown in the drawings are merely exemplary illustrations and do not necessarily include all steps. For example, some steps may be broken down, while others may be combined or partially combined; therefore, the actual order of execution may change depending on the specific circumstances.

[0029] In some techniques, a etching solution prepared with, for example, 10 mL of hydrofluoric acid, 30 mL of nitric acid, and 50 mL of water is used to etch the surface of Ti-Ag alloys. For example, etching for 10 seconds can yield results such as... Figure 1 The microscopic results are shown. From Figure 1 As can be seen, the microstructure of the Ti-Ag alloy is blurry and invisible, resulting in poor performance.

[0030] In order to clearly etch out the microstructure of Ti-Ag alloys and thus improve the accuracy of the test results, this disclosure provides a new metallographic etching method for Ti-Ag alloys.

[0031] Figure 2 A flowchart illustrating the metallographic corrosion method for Ti-Ag alloys according to embodiments of the present disclosure is shown schematically. (Reference) Figure 2 The metallographic etching method for Ti-Ag alloys according to the present disclosure may include the following steps: S22. Machining the Ti-Ag alloy to form a microstructure observation plane on the Ti-Ag alloy.

[0032] The embodiments disclosed herein do not limit the machining process. In addition, the microstructure observation plane is the basis of metallographic testing, and this disclosure does not limit it either.

[0033] S24. Grind the microstructure observation plane on a metallographic pre-grinding machine, and then place the ground microstructure observation plane on a polishing machine for mechanical polishing.

[0034] According to some embodiments of this disclosure, the microstructure observation plane is ground on a metallographic pre-grinding machine using metallographic wet sandpaper of different grits. Each time the metallographic wet sandpaper is changed, the grinding direction is rotated by 90° to ensure that the grinding marks from the previous grinding are completely eliminated. For example, 120#, 800#, 1200#, and 2000# metallographic wet sandpaper are used sequentially to grind the microstructure observation plane.

[0035] After grinding, rinse away the sand particles on the microscopic tissue observation plane.

[0036] During the mechanical polishing process, a SiO2 polishing slurry with a particle size of 0.25 μm was used, and a metallographic damping polishing cloth was employed. After the polishing process, care should be taken to ensure that no liquid droplets remain on the microstructure observation surface after mechanical polishing, and that the surface remains clean and dry.

[0037] According to some embodiments of this disclosure, mechanical polishing is performed until the surface of the microstructure observation plane is smooth, shiny, and free of scratches and drag.

[0038] S26. The mechanically polished microstructure observation plane is etched with an etching solution to obtain the microstructure observation plane to be observed.

[0039] In an exemplary embodiment of this disclosure, the corrosion solution comprises ammonium bifluoride, hydrofluoric acid, and water, wherein the ratio of ammonium bifluoride, hydrofluoric acid, and water is (5~10) g:(10~20) mL:100 mL. That is, the ratio of ammonium bifluoride, hydrofluoric acid, and water can be (5~10):(10~20):100, wherein ammonium bifluoride is expressed in g, and hydrofluoric acid and water are expressed in mL.

[0040] Specifically, the water used in the embodiments of this disclosure can be one or a mixture of tap water, purified water, deionized water, and distilled water. Hydrofluoric acid is an analytical grade reagent.

[0041] In the process of generating the corrosive solution, the order of preparation is as follows: water, ammonium bifluoride, and hydrofluoric acid are added sequentially.

[0042] For a mechanically polished microstructure observation plane, an etching method can be used to immerse the mechanically polished microstructure observation plane in an etching solution for a time of 5-10 seconds. The etching time mentioned in the embodiments of this disclosure refers to the immersion time of the plane in the etching solution.

[0043] For example, the mechanically polished microstructure observation plane can be immersed in the etching solution using an inverted suspension method. This disclosure does not limit the etching method; simply placing the microstructure observation plane in the etching solution is sufficient.

[0044] Furthermore, this disclosure also provides a Ti-Ag alloy, which includes a microstructure observation plane prepared by the above method.

[0045] The scheme of Embodiment 1 of this disclosure will be described below.

[0046] First, the Ti-Ag alloy is machined to form a microstructure observation plane on the Ti-Ag alloy. The microstructure observation plane is then ground on a metallographic pre-grinding machine, and finally mechanically polished on a polishing machine. This process is as described in steps S22 and S24 above, and will not be repeated here.

[0047] Next, the mechanically polished microstructure observation plane was etched using an etching solution to obtain the microstructure observation plane to be observed. The ratio of ammonium bifluoride, hydrofluoric acid, and water in the etching solution was 5 g:10 mL:100 mL, and the etching time was 5 seconds.

[0048] Figure 3 A schematic diagram illustrating the microstructure of the Ti-Ag alloy of Example 1 of this disclosure shows the metallographic corrosion results. Compared to Figure 1 , Figure 3 The results show that the microstructure obtained by the scheme of Example 1 of this disclosure is clear and uniform, which improves the effect of metallographic corrosion and helps to improve the efficiency and accuracy of metallographic detection.

[0049] The scheme of Embodiment 2 of this disclosure will be described below.

[0050] The difference between Example 2 and Example 1 is that the ratio of ammonium bifluoride, hydrofluoric acid and water in the corrosion solution is 5g:10mL:100mL, and the corrosion time is 10s.

[0051] Figure 4 A schematic diagram illustrating the microstructure of the Ti-Ag alloy of Example 2 of this disclosure shows the metallographic corrosion results. Compared to Figure 1 , Figure 4 The results show that the microstructure obtained by the scheme of Example 2 of this disclosure is clear and uniform, which improves the effect of metallographic corrosion and helps to improve the efficiency and accuracy of metallographic detection.

[0052] The scheme of Embodiment 3 of this disclosure will be described below.

[0053] The difference between Example 3 and Example 1 is that the ratio of ammonium bifluoride, hydrofluoric acid and water in the corrosion solution is 5g:20mL:100mL, and the corrosion time is 5s.

[0054] Figure 5 A schematic diagram illustrating the microstructure of the Ti-Ag alloy of Example 3 of this disclosure shows the metallographic corrosion results. Compared to Figure 1 , Figure 5 The results show that the microstructure obtained by the scheme of Example 3 of this disclosure is clear and uniform, which improves the effect of metallographic corrosion and helps to improve the efficiency and accuracy of metallographic detection.

[0055] The scheme of Embodiment 4 of this disclosure will be described below.

[0056] The difference between Example 4 and Example 1 is that the ratio of ammonium bifluoride, hydrofluoric acid and water in the corrosion solution is 5g:20mL:100mL, and the corrosion time is 10s.

[0057] Figure 6 A schematic diagram illustrating the microstructure of the Ti-Ag alloy of Example 4 of this disclosure shows the metallographic corrosion results. Compared to Figure 1 , Figure 6 The results show that the microstructure obtained by the scheme of Example 4 of this disclosure is clear and uniform, which improves the effect of metallographic corrosion and helps to improve the efficiency and accuracy of metallographic detection.

[0058] The scheme of Embodiment 5 of this disclosure will be described below.

[0059] The difference between Example 5 and Example 1 is that the ratio of ammonium bifluoride, hydrofluoric acid and water in the corrosion solution is 10g:20mL:100mL, and the corrosion time is 5s.

[0060] Figure 7 A schematic diagram of the microstructure of the Ti-Ag alloy of Example 5 of this disclosure is shown. Compared to Figure 1 , Figure 7 The results show that the microstructure obtained by the scheme of Example 5 of this disclosure is clear and uniform, which improves the effect of metallographic corrosion and helps to improve the efficiency and accuracy of metallographic detection.

[0061] The scheme of Embodiment 6 of this disclosure will be described below.

[0062] The difference between Example 6 and Example 1 is that the ratio of ammonium bifluoride, hydrofluoric acid and water in the corrosion solution is 10g:20mL:100mL, and the corrosion time is 10s.

[0063] Figure 8 A schematic diagram of the microstructure of the Ti-Ag alloy of Example 6 of this disclosure, showing the metallographic corrosion results, is shown. Compared to Figure 1 , Figure 8 The results show that the microstructure obtained by the scheme of Example 6 of this disclosure is clear and uniform, which improves the effect of metallographic corrosion and helps to improve the efficiency and accuracy of metallographic detection.

[0064] It should be noted that although the steps of the method in this disclosure are described in a specific order in the accompanying drawings, this does not require or imply that the steps must be performed in that specific order, or that all the steps shown must be performed to achieve the desired result. Additional or alternative steps may be omitted, multiple steps may be combined into one step, and / or a step may be broken down into multiple steps.

[0065] Furthermore, the above figures are merely illustrative of the processes included in the method according to exemplary embodiments of this disclosure and are not intended to be limiting. It is readily understood that the processes shown in the above figures do not indicate or limit the temporal order of these processes. Additionally, it is readily understood that these processes may be executed synchronously or asynchronously, for example, in multiple modules.

[0066] Other embodiments of this disclosure will readily occur to those skilled in the art upon consideration of the specification and practice of the disclosure herein. This application is intended to cover any variations, uses, or adaptations of this disclosure that follow the general principles of this disclosure and include common knowledge or customary techniques in the art not disclosed herein. The specification and examples are to be considered exemplary only, and the true scope and spirit of this disclosure are indicated by the claims.

[0067] It should be understood that this disclosure is not limited to the precise structures described above and shown in the accompanying drawings, and various modifications and changes can be made without departing from its scope. The scope of this disclosure is limited only by the appended claims.

Claims

1. A metallographic etching method for Ti-Ag alloys, characterized in that, include: The Ti-Ag alloy is machined to form a microstructure observation plane on the Ti-Ag alloy; The microstructure observation plane was ground on a metallographic pre-grinding machine, and then the ground microstructure observation plane was placed on a polishing machine for mechanical polishing. The mechanically polished microstructure observation plane is etched with an etching solution to obtain the microstructure observation plane to be observed. The corrosion solution contains ammonium hydrogen fluoride, hydrofluoric acid, and water, and the ratio of ammonium hydrogen fluoride, hydrofluoric acid, and water is (5~10)g:(10~20)mL:100mL.

2. The metallographic etching method according to claim 1, characterized in that, Grinding the microstructure observation plane on a metallographic pre-grinding machine includes: On a metallographic pre-grinding machine, metallographic wet sandpaper of different mesh sizes was used to grind the microstructure observation plane; Each time the metallographic wet sandpaper is changed, the grinding direction is rotated 90°.

3. The metallographic etching method according to claim 2, characterized in that, The microstructure observation plane was ground using metallographic wet sandpaper of different grits, including: The microstructure observation plane was ground sequentially using metallographic wet sandpaper of 120#, 800#, 1200# and 2000#.

4. The metallographic etching method according to claim 1, characterized in that, During the mechanical polishing process, the polishing slurry used is SiO2 polishing slurry with a particle size of 0.25μm, and the polishing cloth is metallographic damping polishing cloth.

5. The metallographic etching method according to claim 1, characterized in that, Etching of the microstructure observation plane after mechanical polishing using an etching solution includes: The mechanically polished microstructure observation plane was immersed in an etching solution using an etching method.

6. The metallographic etching method according to claim 1 or 5, characterized in that, The corrosion time is 5~10s.

7. The metallographic etching method according to claim 1, characterized in that, The water is one or more of tap water, pure water, deionized water, and distilled water.

8. The metallographic etching method according to claim 1, characterized in that, The metallographic etching method further includes: In the process of generating the corrosive solution, the order of preparation is as follows: water, ammonium bifluoride, and hydrofluoric acid are added sequentially.

9. The metallographic etching method according to claim 8, characterized in that, The hydrofluoric acid was an analytical grade reagent.

10. A Ti-Ag alloy, characterized in that, The Ti-Ag alloy includes a microstructure observation plane prepared by the metallographic etching method of Ti-Ag alloy as described in any one of claims 1 to 9.