Method for observing macro structure of niobium-tungsten alloy

By mechanical processing and corrosion of niobium tungsten alloy, the problems of complex and long periods of observation plane preparation in the prior art are solved, and clear observation and efficient inspection of macroscopic structures are achieved.

CN119574542APending Publication Date: 2025-03-07西安汉唐分析检测有限公司
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Patent Information

Application Number
CN202411651220.0
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-11-19
Publication Date
2025-03-07

AI Technical Summary

Technical Problem

The observation plane preparation of the macrostructure observation method of niobium tungsten alloy in the prior art is complex and has a long period, making it difficult to meet the demand for large sample volume.

Method used

By mechanically processing and corrosion of niobium tungsten alloy, a macroscopic tissue plane can be prepared that can be observed by the naked eye or a magnifying glass, simplifying the preparation process of the observation plane and shortening the preparation cycle.

Benefits of technology

The simplicity and efficiency of observation plane preparation are achieved, and the macrostructure obtained is clear and there are no obvious corrosion pits, meeting the needs of macrostructure inspection.

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Abstract

The invention discloses an observation method for a niobium-tungsten alloy macrostructure. The method comprises the following steps: step 1, machining a niobium-tungsten alloy to form an observation plane; 2, wiping the observation plane machined in the step 1 with alcohol cotton, and then immersing the observation plane into a corrosion solution to erode for 2-10 minutes; and 3, directly observing the observation plane corroded in the step 2 by naked eyes or observing the macrostructure through a magnifying lens. According to the observation method, the niobium-tungsten alloy is machined and corroded, a plane for observing the macroscopic structure through naked eyes or a magnifying lens can be obtained, the macroscopic structure of the niobium-tungsten alloy on the observation platform is clear and free of obvious corrosion pits, and the observation method is suitable for the technical field of metal material macroscopic structure observation.
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Description

Technical Field

[0001] The invention belongs to the technical field of macroscopic structure observation of metal materials, and in particular relates to a method for observing the macroscopic structure of a niobium-tungsten alloy. Background Art

[0002] The Nb521 niobium-tungsten alloy developed in my country can be used in the manufacture of the thrust chamber of a two-element liquid rocket engine. Under the protection of the high-temperature oxidation-resistant coating of molybdenum silicide, the working temperature of the thrust chamber can reach about 1550°C, which greatly reduces the propellant flow used to cool the combustion chamber, which is beneficial to improving the performance of the engine. With the needs of rocket model development, the use of Nb521 niobium-tungsten alloy in my country's aerospace field has become more extensive, not only in two-element liquid rocket engines, but also in some high-temperature components of other high-speed aircraft.

[0003] In order to study the performance of Nb521 niobium tungsten alloy, it is necessary to observe the macroscopic structure of the alloy to determine the structure type and its uniformity, so as to lay the foundation for improving the performance of Nb521 alloy. At present, there are only studies on the observation methods of alloy microstructure. The preparation of the observation plane of these microstructure observation methods is relatively complicated, and usually requires fine grinding after mechanical processing, which increases the preparation cycle of the observation plane. Since the purpose of macroscopic structure observation is to determine the structure type and uniformity of the alloy, the required sample size is large, so an observation method with simple process and short preparation cycle is needed. Summary of the invention

[0004] The purpose of the present invention is to overcome the shortcomings of the above-mentioned prior art and provide a method for observing the macroscopic structure of niobium-tungsten alloy. The observation method can obtain a plane for observing the macroscopic structure through the naked eye or a magnifying glass by corroding the niobium-tungsten alloy after mechanical processing, effectively simplifying the preparation process of the observation plane, shortening the preparation cycle, and solving the problem of complex process and long cycle of preparing the observation plane in the prior art.

[0005] To achieve the above object, the technical solution adopted by the present invention is: a method for observing the macroscopic structure of niobium tungsten alloy, characterized in that the method comprises the following steps:

[0006] Step 1: machining the niobium tungsten alloy into an observation plane;

[0007] Step 2: Wipe the observation plane machined in step 1 with alcohol cotton, and then immerse it in the corrosion solution for 2 minutes to 10 minutes;

[0008] Step 3: Observe the macroscopic structure of the observation plane after corrosion in step 2 directly with the naked eye or through a magnifying glass.

[0009] The above-mentioned method for observing the macrostructure of niobium tungsten alloy is characterized in that the niobium tungsten alloy in step 1 is Nb521 niobium tungsten alloy.

[0010] The above-mentioned method for observing the macrostructure of niobium tungsten alloy is characterized in that the mechanical processing in step one adopts lathe turning or grinder grinding, and the processing parameters of the lathe turning are: speed 360r / min, cutting depth 1mm, feed rate 0.2mm.

[0011] The present invention can effectively avoid tool sticking during machining by controlling machining parameters of a lathe, and can obtain a suitable machining plane, which can be directly used for macroscopic structure observation after corrosion treatment.

[0012] The above-mentioned method for observing the macrostructure of niobium-tungsten alloy is characterized in that the roughness Ra of the observation plane after mechanical processing in step 1 is not greater than 1.6 μm.

[0013] The above-mentioned method for observing the macroscopic structure of niobium tungsten alloy is characterized in that the corrosion solution in step 2 is composed of the following components in volume percentage: 10% to 20% HF solution, 10% to 30% HNO3 solution, 10% to 24% H2SO4 solution, and the balance is water.

[0014] The above-mentioned method for observing the macroscopic structure of niobium-tungsten alloy is characterized in that the mass concentration of the HF solution is 40%, the mass concentration of the HNO3 solution is 65%, and the mass concentration of the H2SO4 solution is 95%.

[0015] The above-mentioned method for observing the macrostructure of niobium tungsten alloy is characterized in that the illumination of the observation plane in step three is not less than 2153Lx.

[0016] Compared with the prior art, the present invention has the following advantages:

[0017] 1. The present invention mechanically processes and corrodes the niobium tungsten alloy, and then observes the macroscopic structure of the niobium tungsten alloy after corrosion with the naked eye or a magnifying glass. The macroscopic structure of the niobium tungsten alloy on the observation platform is clear without obvious corrosion pits. Compared with the prior art in which pseudo-structures are easily produced when preparing the observation platform, this method can obtain a clearer observation platform.

[0018] 2. The present invention adopts a method of etching after mechanical processing when preparing the observation platform. Compared with the method of polishing or grinding the sample and then etching to display the structure in the prior art, the operation is simpler. Combined with the etching liquid with high corrosion efficiency, it can display a clear macroscopic structure to meet the needs of macroscopic structure inspection.

[0019] 3. The method of the present invention is simple to operate, the corrosion solution used is non-toxic, the macroscopic structure of the niobium tungsten alloy can be clearly observed, and no special equipment is required, and the macroscopic structure type and uniformity of the niobium tungsten alloy can be checked at any time.

[0020] The technical solution of the present invention is further described in detail below through the accompanying drawings and embodiments. BRIEF DESCRIPTION OF THE DRAWINGS

[0021] Figure 1 This is a macroscopic structure diagram of the observation plane of the Nb521 alloy of Example 1 of the present invention.

[0022] Figure 2 This is a macroscopic structure diagram of the observation plane of the Nb521 alloy of Example 2 of the present invention.

[0023] Figure 3 This is a macroscopic structure diagram of the observation plane of the Nb521 alloy of Example 3 of the present invention.

[0024] Figure 4 This is a macroscopic structure diagram of the observation plane of the Nb521 alloy of Example 4 of the present invention.

[0025] Figure 5 This is a macroscopic structure diagram of the observation plane of the Nb521 alloy of Example 5 of the present invention. DETAILED DESCRIPTION

[0026] Example 1

[0027] The method of this embodiment includes the following steps:

[0028] Step 1: lathe the Nb521 alloy to form an observation plane with a surface roughness Ra not greater than 1.6 μm; the lathe machining parameters are: speed 360 r / min, cutting depth 1 mm, feed rate 0.2 mm;

[0029] Step 2: Wipe the observation plane machined in step 1 with alcohol cotton, and then immerse it in a corrosion solution for 2 minutes; the corrosion solution consists of 20.0 mL of 40% HF, 20.0 mL of 65% HNO3 solution, 20.0 mL of 95% H2SO4 solution and 60.0 mL of water;

[0030] Step 3: Observe the macroscopic structure of the observation plane after corrosion in step 2 directly with the naked eye or through a magnifying glass.

[0031] The observation plane after corrosion in this embodiment is macroscopically observed, such as Figure 1 As shown, the macroscopic structure of the observation plane is clear, without obvious corrosion pits; after testing, the illumination of the observation plane is not less than 2153Lx.

[0032] Example 2

[0033] The method of this embodiment includes the following steps:

[0034] Step 1: lathe the Nb521 alloy to form an observation plane with a surface roughness Ra not greater than 1.6 μm; the lathe machining parameters are: speed 360 r / min, cutting depth 1 mm, feed rate 0.2 mm;

[0035] Step 2: Wipe the observation plane machined in step 1 with alcohol cotton, and then immerse it in a corrosion solution for 2 minutes; the corrosion solution consists of 20.0 mL of 40% HF, 30.0 mL of 65% HNO3 solution, 40.0 mL of 95% H2SO4 solution and 80.0 mL of water;

[0036] Step 3: Observe the macroscopic structure of the observation plane after corrosion in step 2 directly with the naked eye or through a magnifying glass.

[0037] The observation plane after corrosion in this embodiment is macroscopically observed, such as Figure 2 As shown, the macroscopic structure of the observation plane is clear, without obvious corrosion pits; after testing, the illumination of the observation plane is not less than 2153Lx.

[0038] Example 3

[0039] The method of this embodiment includes the following steps:

[0040] Step 1: lathe the Nb521 alloy to form an observation plane with a surface roughness Ra not greater than 1.6 μm; the lathe machining parameters are: speed 360 r / min, cutting depth 1 mm, feed rate 0.2 mm;

[0041] Step 2: Wipe the observation plane machined in step 1 with alcohol cotton, and then immerse it in a corrosion solution for 3.5 minutes; the corrosion solution consists of 30.0 mL of 40% HF, 45.0 mL of 65% HNO3 solution, 22.5 mL of 95% H2SO4 solution and 120.0 mL of water;

[0042] Step 3: Observe the macroscopic structure of the observation plane after corrosion in step 2 directly with the naked eye or through a magnifying glass.

[0043] The observation plane after corrosion in this embodiment is macroscopically observed, such as Figure 3 As shown, the macroscopic structure of the observation plane is clear, without obvious corrosion pits; after testing, the illumination of the observation plane is not less than 2153Lx.

[0044] Example 4

[0045] The method of this embodiment includes the following steps:

[0046] Step 1: Grind the Nb521 niobium tungsten alloy to obtain an observation plane with a surface roughness Ra not greater than 1.6 μm;

[0047] Step 2: Wipe the observation plane machined in step 1 with alcohol cotton, and then immerse it in a corrosion solution for 10 minutes; the corrosion solution consists of 10.0 mL of 40% HF, 10.0 mL of 65% HNO3 solution, 10 mL of 95% H2SO4 solution and 70.0 mL of water;

[0048] Step 3: Observe the macroscopic structure of the observation plane after corrosion in step 2 directly with the naked eye or through a magnifying glass.

[0049] The observation plane after corrosion in this embodiment is macroscopically observed, such as Figure 4 As shown, the macroscopic structure of the observation plane is clear, without obvious corrosion pits; after testing, the illumination of the observation plane is not less than 2153Lx.

[0050] Example 5

[0051] The method of this embodiment includes the following steps:

[0052] Step 1: Grind the Nb521 niobium tungsten alloy to obtain an observation plane with a surface roughness Ra not greater than 1.6 μm;

[0053] Step 2: Wipe the observation plane machined in step 1 with alcohol cotton, and then immerse it in a corrosion solution for 2 minutes; the corrosion solution consists of 20.0 mL of 40% HF, 30.0 mL of 65% HNO3 solution, 24.0 mL of 95% H2SO4 solution and 26.0 mL of water;

[0054] Step 3: Observe the macroscopic structure of the observation plane after corrosion in step 2 directly with the naked eye or through a magnifying glass.

[0055] The observation plane after corrosion in this embodiment is macroscopically observed, such as Figure 5 As shown, the macroscopic structure of the observation plane is clear, without obvious corrosion pits; after testing, the illumination of the observation plane is not less than 2153Lx.

[0056] The above description is only a preferred embodiment of the present invention and does not limit the present invention in any way. Any simple modification, change and equivalent structural transformation made to the above embodiment based on the technical essence of the present invention still falls within the protection scope of the technical solution of the present invention.

Claims

1. A method for observing the macrostructure of niobium tungsten alloy, characterized in that: The method comprises the following steps: Step 1: machining the niobium tungsten alloy into an observation plane; Step 2: Wipe the observation plane machined in step 1 with alcohol cotton, and then immerse it in the corrosion solution for 2 minutes to 10 minutes; Step 3: Observe the macroscopic structure of the observation plane after corrosion in step 2 directly with the naked eye or through a magnifying glass.

2. The method for observing the macrostructure of niobium-tungsten alloy according to claim 1, characterized in that: The niobium tungsten alloy in step 1 is Nb521 niobium tungsten alloy.

3. The method for observing the macrostructure of niobium-tungsten alloy according to claim 1, characterized in that: The mechanical processing in step one adopts lathe turning or grinder grinding, and the processing parameters of the lathe turning are: speed 360r / min, cutting depth 1mm, feed rate 0.2mm.

4. The method for observing the macrostructure of niobium-tungsten alloy according to claim 1, characterized in that: The roughness Ra of the observation plane after mechanical processing is not greater than 1.6 μm.

5. The method for observing the macrostructure of niobium-tungsten alloy according to claim 1, characterized in that: The etching solution in step 2 is composed of the following components in volume percentage: 10% to 20% HF solution, 10% to 30% HNO3 solution, 10% to 24% H2SO4 solution, and the balance is water.

6. The method for observing the macrostructure of niobium-tungsten alloy according to claim 5, characterized in that: The mass concentration of the HF solution is 40%, the mass concentration of the HNO3 solution is 65%, and the mass concentration of the H2SO4 solution is 95%.

7. The method for observing the macrostructure of niobium-tungsten alloy according to claim 1, characterized in that: The illumination of the observation plane in step 3 is not less than 2153Lx.