Sample preparation method of wire material capable of being used for direct-reading spectrum detection

Abstract

The invention provides a sample preparation method of a wire material for direct-reading spectrum detection, which specifically comprises the following steps: grinding the edge of the wire material until the edge of the wire material has no flying skin, heating until the wire material is completely softened, and then pressing the softened wire material into a sheet to obtain a sheet-shaped wire material; and finally, the surface of the sheet-shaped wire is polished to be smooth, and the wire capable of being used for direct-reading spectrum detection is obtained. The method is suitable for manufacturing direct-reading spectrum detection samples of nickel-based high-temperature alloy wires and iron-based high-temperature alloy wires with the diameter of 4-10 mm. The problem that chemical elements of small wires cannot be directly and accurately detected by a spectrum method due to too small samples and difficult sample preparation is effectively solved, the sample preparation method is simple, and compared with a traditional method that the small wires need to be firstly processed into scrap iron by a lathe, a drilling machine or locking pliers and the like, and then chemical element analysis is carried out by a manual method, the sample preparation method has the advantages that the sample preparation efficiency is greatly improved; when the method is adopted for sample preparation, the detection efficiency can be greatly improved, other impurity elements are not introduced in the whole process, and the detection accuracy is relatively high.

Description

Technical Field

[0001] The invention relates to the technical field of wire element detection and analysis sampling and sample preparation, and in particular to a wire sample preparation method that can be used for direct reading spectrum detection. Background Art

[0002] In order to ensure the quality of wire production, chemical element analysis of wire is a very important link in the production process. When the wire diameter is greater than 10mm, the traditional sampling method is to directly cut a small stick of about 30mm long from the material to be tested, and the rough surface of the cut is machined and polished into a plane, and then the chemical element analysis is directly performed by means such as spectroscopy; however, when the wire diameter is ≤10mm, because the sample is too small, the diameter of the rough surface cut cannot cover the excitation hole on the excitation plate of the spectrometer, and the spectroscopy cannot accurately detect its chemical elements, so manual methods are often used to analyze the chemical element composition. In the field of chemical testing, manual method, also known as wet method, is an extremely common and relatively accurate testing method, but it also has high requirements for the test sample. The sample is too large to be dissolved, and the sample is too small to be operated. Therefore, the test sample of small wire is generally first processed into sample chips by lathe, drilling machine or pliers, and then the element composition of the sample chips is detected by manual method. However, in actual work, there are many types of wire materials, which require frequent clamping, resulting in a cumbersome sample preparation process and difficulty in controlling the particle size of sample chips. These directly affect the sampling efficiency and quality, thereby affecting the length and accuracy of chemical element detection time. Summary of the invention

[0003] In view of the above-mentioned deficiencies in the prior art, the object of the present invention is to provide a method for preparing a sample of a wire that can be used for direct reading spectroscopy detection, so as to solve the problem that in the prior art, the wire with a diameter of ≤10 mm cannot be directly detected accurately by spectroscopy because the sample is too small and the sample preparation is difficult. However, manual detection has the problems of cumbersome sampling steps and poor sampling quality, resulting in low detection efficiency and accuracy.

[0004] In order to solve the above technical problems, the technical solution adopted by the present invention is as follows:

[0005] A method for preparing a sample of a wire material that can be used for direct-reading spectrum detection comprises grinding the wire material until there is no peeling on the wire material edge, heating the wire material until the wire material is completely softened, and then pressing the softened wire material into a sheet to obtain a sheet-like wire material; finally, polishing the surface of the sheet-like wire material to be smooth to obtain the wire material that can be used for direct-reading spectrum detection.

[0006] Furthermore, the diameter of the wire is 4 to 10 mm. The sample preparation method of the present invention is also applicable to wires with a diameter greater than 10 mm, but is more suitable for the preparation of direct reading spectrum detection samples of wires with a small diameter of 4 to 10 mm.

[0007] Furthermore, the length of the wire is 100-120 mm. Since the direct reading spectrometer is used for detection, the sample is required to be excited at least three times, and the three positions cannot overlap (the distance between the three points must be at least 40 mm), so the length of the wire should not be too short. If it is too long, it will cause material waste and increase the detection cost.

[0008] Further, the sheet-like wire material is first bent into a In this way, it is easy to hold the sample steadily to polish the sample surface, and grind the sample surface into the same plane, ensuring that the texture on the sample surface is not disorderly and in the same direction, meeting the requirements of direct reading spectrum detection for sample surface treatment.

[0009] Further, the sheet-like wire is polished into After type, The length of the two vertical parts of the type is 30 to 40 mm. The two vertical parts of the model are the hand-held parts when the sample is polished. The length is set in this way to facilitate steady hand-held sample polishing of the sample surface. The length of the hand-held sample should not be too long. Too long will make the surface polishing force uneven, so that the surface forms multiple planes, resulting in poor fit between the sample surface and the excitation table surface of the direct reading spectrometer. When the direct reading spectrometer is used for detection, it will not only cause leakage of high-purity argon gas, but also strong light leakage when igniting discharge burning, which will make the signal collection incomplete and the converted detection data inaccurate. And the length of the hand-held sample should not be too short, otherwise the hand is prone to mechanical damage during the polishing process.

[0010] Furthermore, the heating temperature is 800-1200°C. Because the samples have different brands and physical properties, the softening temperatures are different. Below 800°C, the softening degree of the sample is not enough, and the sample is easy to break during the tableting process; above 1200°C, the chromium, aluminum, and titanium elements in the sample will be consumed, making the data detected by the direct reading spectrometer lower.

[0011] Furthermore, the width of the sheet wire is 4 to 12 mm, and the thickness is not less than 1.0 mm. The inner diameter of the excitation hole on the small sample excitation plate of the direct reading spectrometer is 4 mm, and the outer diameter is 10 mm. The width of the sample must cover the inner diameter of the excitation to ensure the integrity of the direct reading spectrometer signal acquisition. The sample thickness must be greater than 1.0 mm to ensure that the direct reading spectrometer will not be punctured when burning the sample and cause environmental pollution.

[0012] Furthermore, the sheet-like wire material has a width of 6 mm and a thickness greater than 1 mm.

[0013] Furthermore, after the surface is polished and smooth, the surface particle size of the wire is 0.124-0.25mm. The hardness of the wire material varies with different grades. According to the different hardness, the sandpaper wheel particle size (80-120 mesh) selected on the spectrum grinder can meet the requirements of the direct reading spectrometer to quickly ignite and burn during sample detection and keep the distance between the excitation electrodes unchanged. When the particle size is greater than 0.25mm, the texture is too deep, and the distance between the excitation electrodes changes, which affects the detection data; when the particle size is less than 0.124mm, the sample surface is not easy to polish and the surface is easy to turn blue, which affects the detection data.

[0014] Furthermore, the wire is a nickel-based high-temperature alloy wire or an iron-based high-temperature alloy wire.

[0015] The present invention discloses a method for preparing a sample of a wire material for direct-reading spectrum detection. The wire material sample is subjected to edge grinding, high-temperature treatment, sheet pressing treatment and surface grinding treatment in sequence, thereby obtaining a wire material that can be used for direct-reading spectrum detection. The method removes the flying skin at the edge of the sample by edge grinding, thereby preventing the flying skin from melting and falling off when the wire material is subjected to direct-reading spectrum detection, thereby affecting the accuracy of the detection result; the wire material is then transformed into a thin sheet state that is easy to measure by high-temperature and sheet pressing treatment, and finally the particle size of the wire material surface is controlled by surface grinding, thereby obtaining a wire material that can be used for accurate direct-reading spectrum detection. The method is also applicable to small wire materials with a diameter of 4 to 10 mm, thereby solving the problem that the small wire material cannot be directly and accurately detected for chemical elements by spectroscopy because the sample is too small and the sample preparation is difficult. The sample preparation method is simple, the detection efficiency is high, other impurity elements are not introduced in the whole process, and the detection accuracy is also high.

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

[0017] The present invention is a method for preparing a sample of a wire for direct-reading spectrum detection. The wire sample is subjected to edge grinding, high-temperature treatment, sheet pressing treatment and surface polishing treatment in sequence, thereby obtaining a wire that can be used for direct-reading spectrum detection. The method is suitable for preparing samples for direct-reading spectrum detection of 4-10 mm nickel-based high-temperature alloy wires and iron-based high-temperature alloy wires. The method effectively solves the problem that small wires cannot be accurately detected by spectroscopy directly because the sample is too small and the sample preparation is difficult. The sample preparation method is simple. Compared with the traditional method that requires first processing the small wire into sample chips using a lathe, a drill press or pliers, and then using a manual method to perform chemical element analysis, the sample preparation method of the present invention can greatly improve the detection efficiency, and no other impurity elements are introduced in the whole process, and the detection accuracy is also high. DETAILED DESCRIPTION

[0018] The specific implementation modes of the present invention are further described in detail below in conjunction with specific examples.

[0019] Example 1

[0020] This embodiment provides a method for preparing a sample of a silk material that can be used for direct reading spectroscopy detection, comprising the following steps:

[0021] (1) Sampling: Take 120 mm of GH4033 nickel-based high-temperature alloy wire with a diameter of 4.0 mm and grind the wire edge until there is no flying skin on the wire edge;

[0022] (2) high temperature treatment: heating the wire obtained in step (1) to 950° C. until it is completely softened;

[0023] (3) Tableting: The completely softened wire is placed in a tabletting mold and pressed into a sheet of wire with a width of 6.0 mm and a thickness of about 1.0 mm;

[0024] (4) Bending and surface treatment: The sheet-like wire obtained in step (3) is bent into After forming, the surface is treated by a spectrum sample making machine to make the surface particle size of the wire material 0.124 mm, thus obtaining a wire material that can be used for direct reading spectrum detection.

[0025] The wire material obtained in Example 1 and used for direct reading spectrum detection was detected by using a direct reading spectrometer, and the detection results are shown in Table 1.

[0026] Table 1 Element detection results of the wire material obtained in Example 1 that can be used for direct reading spectroscopy detection

[0027]

[0028] It can be seen from Table 1 that the test results obtained in this embodiment are relatively close to the manual (wet method) chemical analysis data, and the results are accurate. The sample preparation method of the present invention has no effect on the test results.

[0029] Example 2

[0030] This embodiment provides a method for preparing a sample of a silk material that can be used for direct reading spectroscopy detection, comprising the following steps:

[0031] (1) Sampling: Take 120 mm of ERNiCrMo-3 nickel-based high-temperature alloy wire with a diameter of 6 mm and grind the wire edge until there is no flying skin on the edge of the wire;

[0032] (2) high temperature treatment: heating the wire obtained in step (1) to 1000° C. until it is completely softened;

[0033] (3) Tableting: The completely softened wire is placed in a tabletting mold and pressed into a sheet of wire with a width of 7.0 mm and a thickness of about 1.0 mm;

[0034] (4) Bending and surface treatment: The sheet-like wire obtained in step (3) is bent into After forming, the surface is treated by a spectrum sample making machine so that the surface particle size is 0.25 mm, and the wire material that can be used for direct reading spectrum detection is obtained.

[0035] The wire material obtained in Example 2 and used for direct reading spectrum detection was detected by using a direct reading spectrometer, and the detection results are shown in Table 2.

[0036] Table 2 Element detection results of the wire material obtained in Example 2 that can be used for direct reading spectroscopy detection

[0037]

[0038] It can be seen from Table 2 that the test results obtained in this embodiment are relatively close to the manual chemical analysis data, and the results are accurate. The sample preparation method of the present invention has no effect on the test results.

[0039] Example 3

[0040] This embodiment provides a method for preparing a sample of a silk material that can be used for direct reading spectroscopy detection, comprising the following steps:

[0041] (1) Sampling: Take 100 mm of GH625 nickel-based high-temperature alloy wire with a diameter of 10 mm and grind the wire edge until there is no flying skin on the edge of the wire;

[0042] (2) high temperature treatment: heating the wire obtained in step (1) to 1200° C. until it is completely softened;

[0043] (3) Tableting: The completely softened wire is placed in a tabletting mold and pressed into a sheet of wire with a width of 8.0 mm and a thickness of about 2.0 mm;

[0044] (4) Bending and surface treatment: The sheet-like wire obtained in step (3) is bent into After forming, the surface is treated by a spectrum sample making machine so that the surface particle size is 0.25 mm, and the wire material that can be used for direct reading spectrum detection is obtained.

[0045] The wire material obtained in Example 3 and used for direct reading spectrum detection was tested by using a direct reading spectrometer, and the test results are shown in Table 3:

[0046] Table 3 Element detection results of the wire material obtained in Example 3 that can be used for direct reading spectrum detection

[0047] element C Si Mn P S Cr Mo Al Cu Ti Co Nb B Direct reading spectral data 0.026 0.042 0.046 0.0017 0.0013 22.13 9.11 0.15 0.024 0.23 0.075 3.67 0.0031 Wet Chemistry Data 0.024 0.041 0.051 0.0019 0.0011 21.91 9.01 0.15 0.026 0.25 0.066 3.78 0.0040

[0048] It can be seen from Table 3 that the test results obtained in this embodiment are relatively close to the manual chemical analysis data, and the results are accurate. The sample preparation method of the present invention has no effect on the test results.

[0049] Example 4

[0050] This embodiment provides a method for preparing a sample of a silk material that can be used for direct reading spectroscopy detection, comprising the following steps:

[0051] (1) Sampling: Take 100 mm of GH2132 iron-based high-temperature alloy wire with a diameter of 8 mm and grind the wire edge until there is no flying skin on the edge of the wire;

[0052] (2) high temperature treatment: heating the wire obtained in step (1) to 900° C. until it is completely softened;

[0053] (3) Tableting: The completely softened wire is placed in a tabletting mold and pressed into a sheet of wire with a width of 9.0 mm and a thickness of about 2.0 mm;

[0054] (4) Bending and surface treatment: The sheet-like wire obtained in step (3) is bent into After forming, the surface is treated by a spectrum sample making machine to make the surface particle size of the wire material 0.148 mm, thus obtaining a wire material that can be used for direct reading spectrum detection.

[0055] The wire material obtained in Example 4 and used for direct reading spectrum detection was tested using a direct reading spectrometer, and the test results are shown in Table 4:

[0056] Table 4 Element detection results of the wire material obtained in Example 4 that can be used for direct reading spectrum detection

[0057] element C Si Mn P S Cr Ni Mo Al Cu Ti V W Direct reading spectral data 0.041 0.48 1.52 0.018 0.001 13.93 25.82 1.17 0.23 0.12 1.95 0.20 0.16 Wet Chemistry Data 0.042 0.47 1.48 0.016 0.001 13.97 24.89 1.2 0.37 0.12 1.95 0.21 0.15

[0058] It can be seen from Table 4 that the test results obtained in this embodiment are relatively close to the manual chemical analysis data, and the results are accurate. The sample preparation method of the present invention has no effect on the test results.

[0059] Example 5

[0060] This embodiment provides a method for preparing a sample of a silk material that can be used for direct reading spectroscopy detection, comprising the following steps:

[0061] (1) Sampling: Take 100 mm of CN-15 iron-based high-temperature alloy wire with a diameter of 6 mm and grind the wire edge until there is no flying skin on the edge of the wire;

[0062] (2) high temperature treatment: heating the wire obtained in step (1) to 800° C. until it is completely softened;

[0063] (3) Tableting: The completely softened wire is placed in a tabletting mold and pressed into a sheet of wire with a width of 8.0 mm and a thickness of about 2.0 mm;

[0064] (4) Bending and surface treatment: The sheet-like wire obtained in step (3) is bent into After forming, the surface is treated by a spectrum sample making machine to make the surface particle size of the wire material 0.124 mm, thus obtaining a wire material that can be used for direct reading spectrum detection.

[0065] The wire material obtained in Example 5 and used for direct reading spectrum detection was detected by using a direct reading spectrometer, and the detection results are shown in Table 5.

[0066] Table 5 Element detection results of the wire material obtained in Example 5 that can be used for direct reading spectroscopy detection

[0067] element C Si Mn P S Cr Ni Mo Al Cu Ti V B Direct reading spectral data 0.058 0.48 1.77 0.007 0.0040 16.20 18.18 2.39 0.029 0.0075 0.32 0.19 0.0043 Wet Chemistry Data 0.059 0.51 1.76 0.005 0.0037 16.32 15.22 2.40 0.020 0.0067 0.34 0.20 0.0047

[0068] It can be seen from Table 5 that the test results obtained in this embodiment are relatively close to the manual chemical analysis data, and the results are accurate. The sample preparation method of the present invention has no effect on the test results.

[0069] Finally, it should be noted that the above embodiments of the present invention are only examples for illustrating the present invention, and are not intended to limit the implementation methods of the present invention. For those skilled in the art, other different forms of changes and modifications can be made based on the above description. It is impossible to list all implementation methods here. Any obvious changes or modifications derived from the technical solution of the present invention are still within the scope of protection of the present invention.

Claims

1. A method for preparing a sample of a silk material that can be used for direct reading spectroscopy detection, characterized in that: After the wire is edge-grinded until there is no flying skin on the edge of the wire, it is heated until the wire is completely softened, and then the softened wire is pressed into a sheet to obtain a sheet-like wire; finally, the surface of the sheet-like wire is polished to be smooth, thus obtaining a wire that can be used for direct-reading spectroscopy detection.

2. The method for preparing a sample of a silk material that can be used for direct reading spectrum detection according to claim 1, characterized in that: The diameter of the wire material is 4 to 10 mm.

3. The method for preparing a sample of a silk material that can be used for direct reading spectrum detection according to claim 1, characterized in that: The length of the wire is 100-120 mm.

4. The method for preparing a sample of a silk material that can be used for direct reading spectrum detection according to claim 3, characterized in that: The sheet-like wire material is first bent into a type.

5. The method for preparing a sample of a silk material that can be used for direct reading spectrum detection according to claim 4, characterized in that: The sheet-like wire material is ground into After type, The length of the two vertical parts of the type is 30 to 40 mm.

6. The method for preparing a sample of a silk material that can be used for direct reading spectrum detection according to claim 1, characterized in that: The heating temperature is 800-1200°C.

7. The method for preparing a sample of a silk material that can be used for direct reading spectrum detection according to claim 1, characterized in that: The sheet-like wire material has a width of 4 to 12 mm and a thickness of not less than 1.0 mm.

8. The method for preparing a sample of a silk material that can be used for direct reading spectrum detection according to claim 7, characterized in that: The sheet-like wire material has a width of 6 mm and a thickness of 1 mm.

9. The method for preparing a sample of a silk material that can be used for direct reading spectrum detection according to claim 1, characterized in that: After the surface is polished and smooth, the surface particle size of the wire is 0.124-0.25 mm.

10. The method for preparing a sample of a silk material that can be used for direct reading spectrum detection according to claim 1, characterized in that: The wire material is a nickel-based high-temperature alloy wire material or an iron-based high-temperature alloy wire material.

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