A surface treatment method for observing the grains of copper materials

Abstract

The present invention relates to a surface treatment method for observing the grains of copper materials. The surface treatment method includes first heat preservation, first turning, second heat preservation, and second turning performed on the copper materials in sequence; the temperature of the first heat preservation > the temperature of the second heat preservation; the tool used for the first turning is a cemented carbide tool, and the tool for the second turning is a diamond turning tool. The surface treatment method provided by the present invention realizes the efficient observation of the grains of the copper materials used in the preparation process of the target by introducing a specific heat preservation process and a specific turning process. After being treated by the surface treatment method of the present invention, it is possible to directly visually confirm whether there is an abnormality in the grain distribution of the copper materials, and achieve the high-efficiency screening of the copper materials used before the preparation of the target.

Description

Technical Field

[0001] The present invention relates to the field of target materials, and particularly to a surface treatment method for observing the crystal grains of copper materials. Background Art

[0002] At present, as a commonly used material for sputtering coating, the performance of target materials has attracted particular attention. Among them, the crystal grains in the target material have a particularly significant impact on the performance, such as being too large, too small, or abnormally distributed. Currently, the regulation of target material crystal grains is mainly controlled during the preparation process.

[0003] For example, CN113458307A discloses a processing method for an aluminum-copper target material, including the following steps: (1) heating the original ingot to a suitable temperature and holding it; (2) upsetting the heated original ingot along the height direction; (3) forging and stretching the upset ingot along the radial direction; (4) repeating steps (2) and (3) at least 2 times, and performing an intermediate annealing treatment on the ingot after each repetition; (5) forging by die forging to obtain a finished blank; (6) performing a final annealing treatment on the finished blank to obtain the aluminum-copper target material; wherein, in step (3), after each forging, the corresponding angle is rotated for circumferential forging so that the cross-section after forging is close to a circle. Using this method to process the aluminum-copper target material can not only improve the non-uniformity of the structure but also ensure the uniformity of the target material structure, effectively refining the crystal grains. At the same time, without excessive removal of side materials, the material utilization rate is improved and the cost is reduced.

[0004] CN111286702A discloses a rotating silver-copper target material and its preparation method. The method includes the following steps: (1) preparing silver-copper powder with a particle size D10≥20μm and D90≤70μm; (2) using a stainless steel tube or a titanium tube as the target base tube, and successively performing surface sandblasting treatment and primer treatment on the target base tube; (3) cold spraying: installing the primer-treated target base tube on a transmission device, making the target base tube rotate around its central axis, and the spray gun move relatively back and forth along the horizontal direction of the target base tube. After starting the cooling device, the silver-copper powder is cold-sprayed onto the surface of the target base tube through the spray gun to deposit and form a coating to obtain the target material. This preparation process is simple and easy to operate, suitable for large-scale industrial production. The obtained rotating silver-copper target material has high purity, unrestricted dimensions, a thickness that can reach 3-12mm, a length that can reach 4000mm, low oxygen content, and small crystal grain size.

[0005] However, when it comes to copper rotating targets, it is necessary to observe the surface grain condition of the raw copper tubes before preparation to ensure that there are no abnormal grains in the tubes used during the preparation process. However, on that day, the process of confirming the surface grains of the copper tubes was to machine the surface with a lathe and then pickle and corrode the copper surface with acid to make the grains appear obvious. However, this process is still complex, and nitric acid is used in the pickling process of the copper surface. If the nitric acid volatilizes and is inhaled by people, it will cause great harm to the human body. Summary of the Invention

[0006] In view of the problems existing in the prior art, the purpose of the present invention is to provide a surface treatment method for observing the grains of copper materials, so as to solve the problems of low efficiency, poor accuracy, and complex treatment process existing in the current observation of the surface grains of copper materials.

[0007] To achieve this purpose, the present invention adopts the following technical solutions:

[0008] The present invention provides a surface treatment method for observing the grains of copper materials. The surface treatment method includes first heat preservation, first turning, second heat preservation, and second turning performed on the copper materials in sequence;

[0009] The temperature of the first heat preservation > the temperature of the second heat preservation;

[0010] The tool used for the first turning is a cemented carbide tool, and the tool for the second turning is a diamond turning tool.

[0011] The surface treatment method provided by the present invention realizes the efficient observation of the grains of the copper materials used in the preparation process of the target by introducing a specific heat preservation process and a specific turning process. After being treated by the surface treatment method of the present invention, it is possible to directly visually confirm whether there are abnormalities in the grain distribution of the copper materials, and achieve the high-efficiency screening of the copper materials used before the preparation of the target.

[0012] In the present invention, the copper materials can be copper plates, copper tubes, copper billets, etc., and their purity is high-purity copper materials and ultra-high-purity copper materials.

[0013] In the present invention, the high purity means the purity ≥ 99.99%.

[0014] In the present invention, the ultra-high purity means the purity is above 99.9999%.

[0015] The surface treatment process provided by the present invention is a specific treatment process proposed for high-purity copper or ultra-high-purity copper materials and is not applicable to other metal materials such as aluminum materials, stainless steel, copper alloys, etc. This is because of the existence of a specific heating process. Different heating processes will affect the crystal structure of the material, and further lead to changes in the material properties. The solution proposed by the present invention realizes the efficient treatment of the surface of high-purity copper or ultra-high-purity copper materials by specifically selecting the temperature range while avoiding changes in the grain morphology. It is possible to observe whether there are grain defects (such as locally oversized grains) in the copper material, avoiding the defect in the prior art that after turning, nitric acid treatment is still required.

[0016] In the present invention, for the turning tool used, a tool commonly used in the art can be selected according to the properties of the copper material.

[0017] As a preferred technical solution of the present invention, the temperature of the first heat preservation is 450-570 °C. For example, it can be 450 °C, 455 °C, 460 °C, 465 °C, 470 °C, 475 °C, 480 °C, 485 °C, 490 °C, 500 °C, 505 °C, 510 °C, 515 °C, 520 °C, 525 °C, 530 °C, 535 °C, 540 °C, 545 °C, 550 °C, 555 °C, 560 °C, 565 °C or 570 °C, etc., but is not limited to the listed values. Other unlisted values within this range are equally applicable.

[0018] As a preferred technical solution of the present invention, the time of the first heat preservation is 20-30 min. For example, it can be 20 min, 21 min, 22 min, 23 min, 24 min, 25 min, 26 min, 27 min, 28 min, 29 min or 30 min, etc., but is not limited to the listed values. Other unlisted values within this range are equally applicable.

[0019] As a preferred technical solution of the present invention, the spindle speed in the first turning is 180-200 r / min. For example, it can be 180 r / min, 182 r / min, 184 r / min, 186 r / min, 188 r / min, 190 r / min, 192 r / min, 194 r / min, 196 r / min, 198 r / min or 200 r / min, etc., but is not limited to the listed values. Other unlisted values within this range are equally applicable.

[0020] As a preferred technical solution of the present invention, the feed rate in the first turning is 0.3 - 0.33 mm / r. For example, it can be 0.3 mm / r, 0.302 mm / r, 0.304 mm / r, 0.306 mm / r, 0.308 mm / r, 0.31 mm / r, 0.312 mm / r, 0.314 mm / r, 0.316 mm / r, 0.318 mm / r, 0.32 mm / r, 0.322 mm / r, 0.324 mm / r, 0.326 mm / r, 0.328 mm / r or 0.33 mm / r, etc., but not limited to the listed values. Other unlisted values within this range are equally applicable.

[0021] As a preferred technical solution of the present invention, the temperature of the second heat preservation is 300 - 400 °C. For example, it can be 300 °C, 305 °C, 310 °C, 315 °C, 320 °C, 325 °C, 330 °C, 335 °C, 340 °C, 345 °C, 350 °C, 355 °C, 360 °C, 365 °C, 370 °C, 380 °C, 385 °C, 390 °C, 395 °C or 400 °C, etc., but not limited to the listed values. Other unlisted values within this range are equally applicable.

[0022] Preferably, the time of the second heat preservation is 60 - 90 min. For example, it can be 60 min, 62 min, 64 min, 66 min, 68 min, 70 min, 72 min, 74 min, 76 min, 78 min, 80 min, 82 min, 84 min, 86 min, 88 min or 90 min, etc., but not limited to the listed values. Other unlisted values within this range are equally applicable.

[0023] As a preferred technical solution of the present invention, the spindle speed in the second turning is 290 - 310 r / min. For example, it can be 290 r / min, 292 r / min, 294 r / min, 296 r / min, 298 r / min, 300 r / min, 302 r / min, 304 r / min, 306 r / min, 308 r / min or 310 r / min, etc., but not limited to the listed values. Other unlisted values within this range are equally applicable.

[0024] As a preferred technical solution of the present invention, the cutting amount in the second turning is 0.3 - 0.32 mm. For example, it can be 0.3 mm, 0.305 mm, 0.31 mm, 0.315 mm or 0.32 mm, etc., but not limited to the listed values. Other unlisted values within this range are equally applicable.

[0025] As a preferred technical solution of the present invention, the feed rate in the second turning is 0.07 - 0.08 mm / r. For example, it can be 0.07 mm / r, 0.071 mm / r, 0.072 mm / r, 0.073 mm / r, 0.074 mm / r, 0.075 mm / r, 0.076 mm / r, 0.077 mm / r, 0.078 mm / r, 0.079 mm / r or 0.08 mm / r, etc., but not limited to the listed values. Other unlisted values within this range are equally applicable.

[0026] As a preferred technical solution of the present invention, the surface treatment method includes the first heat preservation, the first turning, the second heat preservation and the second turning performed on the copper material in sequence;

[0027] The temperature of the first heat preservation > the temperature of the second heat preservation; the temperature of the first heat preservation is 450 - 570 °C; the time of the first heat preservation is 20 - 30 min; the temperature of the second heat preservation is 300 - 400 °C; the time of the second heat preservation is 60 - 90 min;

[0028] The tool used for the first turning is a cemented carbide tool, and the tool for the second turning is a diamond turning tool; the spindle speed in the first turning is 180 - 200 r / min; the feed rate in the first turning is 0.3 - 0.33 mm / r; the spindle speed in the second turning is 290 - 310 r / min; the cutting amount in the second turning is 0.3 - 0.32 mm; the feed rate in the second turning is 0.07 - 0.08 mm / r.

[0029] Compared with the prior art solutions, the present invention has the following beneficial effects:

[0030] The solution provided by the present invention, by using a specific heat preservation process and turning process in combination for pure copper materials, can achieve efficient observation of the surface grains of copper materials without affecting the crystal morphology, and can directly observe and confirm whether there are problems with abnormal grains, avoiding the problem that the prior art needs to use nitric acid for treatment after turning to achieve observation. Description of the Drawings

[0031] Figure 1 is a photograph of the copper material obtained in Example 1 of the present invention;

[0032] Figure 2 is a photograph of the copper material obtained in Example 2 of the present invention;

[0033] Figure 3 is a photograph of the copper material obtained in Example 3 of the present invention;

[0034] Figure 4 is a photograph of the copper material obtained in Example 4 of the present invention;

[0035] Figure 5 It is a photograph of the copper material obtained in Example 5 of the present invention;

[0036] Figure 6 It is a photograph of the copper material obtained in Example 6 of the present invention;

[0037] Figure 7 It is a photograph of the copper material obtained in Example 7 of the present invention;

[0038] Figure 8 It is a photograph of the copper material obtained in Example 8 of the present invention;

[0039] Figure 9 It is a photograph of the copper material obtained in Example 9 of the present invention;

[0040] Figure 10 It is a photograph of the copper material obtained in Example 10 of the present invention;

[0041] Figure 11 It is a photograph of the copper material obtained in Example 11 of the present invention;

[0042] Figure 12 It is a photograph of the copper material obtained in Example 12 of the present invention;

[0043] Figure 13 It is a photograph of the copper material obtained in Example 13 of the present invention;

[0044] Figure 14 It is a photograph of the copper material obtained by secondary processing of the copper material obtained in Example 9 of the present invention using the processing process of Example 1 of the present application.

[0045] The present invention will be further described in detail below. However, the following examples are merely simple examples of the present invention and do not represent or limit the scope of the protection of the present invention. The scope of protection of the present invention shall be subject to the claims. Detailed implementation manners

[0046] To better illustrate the present invention and facilitate understanding of the technical solution of the present invention, typical but non-limiting embodiments of the present invention are as follows:

[0047] Example 1

[0048] This embodiment provides a surface treatment method for observing the grains of copper materials. The surface treatment method includes first heat preservation, first turning, second heat preservation, and second turning performed on the copper material in sequence;

[0049] The temperature of the first heat preservation > the temperature of the second heat preservation;

[0050] The temperature of the first heat preservation is 470 °C; the time of the first heat preservation is 22 min;

[0051] The temperature of the second heat preservation is 400 °C; the time of the second heat preservation is 84 min;

[0052] The tool used for the first turning is a cemented carbide tool, the spindle speed in the first turning is 186 r / min; the feed rate in the first turning is 0.31 mm / r;

[0053] The tool for the second turning is a diamond turning tool; the spindle speed in the second turning is 290 r / min; the cutting amount in the second turning is 0.3 mm; the feed rate in the second turning is 0.08 mm / r.

[0054] In this embodiment, the copper material targeted is copper pipe with a purity of 99.99%.

[0055] For the observation of the copper material obtained after processing, see Table 1 in detail, and the photo of the obtained copper material is as Figure 1 shown.

[0056] Example 2

[0057] The present invention provides a surface treatment method for observing the grains of copper material, and the surface treatment method includes first heat preservation, first turning, second heat preservation and second turning sequentially performed on the copper material;

[0058] The temperature of the first heat preservation > the temperature of the second heat preservation;

[0059] The temperature of the first heat preservation is 500 °C; the time of the first heat preservation is 28 min;

[0060] The temperature of the second heat preservation is 300 °C; the time of the second heat preservation is 60 min;

[0061] The tool used for the first turning is a cemented carbide tool, the spindle speed in the first turning is 200 r / min; the feed rate in the first turning is 0.33 mm / r;

[0062] The tool for the second turning is a diamond turning tool; the spindle speed in the second turning is 310 r / min; the cutting amount in the second turning is 0.32 mm; the feed rate in the second turning is 0.07 mm / r.

[0063] In this embodiment, the copper material targeted is copper pipe with a purity of 99.99%.

[0064] For the observation of the copper material obtained after processing, see Table 1 in detail, and the photo of the obtained copper material is as Figure 2 shown.

[0065] Example 3

[0066] The present invention provides a surface treatment method for observing the grains of copper materials. The surface treatment method includes first heat preservation, first turning, second heat preservation, and second turning performed on the copper materials in sequence;

[0067] The temperature of the first heat preservation > the temperature of the second heat preservation;

[0068] The temperature of the first heat preservation is 570 °C; the time of the first heat preservation is 20 min;

[0069] The temperature of the second heat preservation is 320 °C; the time of the second heat preservation is 90 min;

[0070] The tool used for the first turning is a cemented carbide tool. The spindle speed in the first turning is 180 r / min; the feed rate in the first turning is 0.32 mm / r;

[0071] The tool for the second turning is a diamond turning tool; the spindle speed in the second turning is 300 r / min; the cutting amount in the second turning is 0.31 mm; the feed rate in the second turning is 0.074 mm / r.

[0072] In this embodiment, the copper material targeted is a copper tube with a purity of 99.9999%.

[0073] For the observation situation of the processed copper materials, see Table 1 in detail. The photos of the obtained copper materials are as Figure 3 shown.

[0074] Example 4

[0075] The present invention provides a surface treatment method for observing the grains of copper materials. The surface treatment method includes first heat preservation, first turning, second heat preservation, and second turning performed on the copper materials in sequence;

[0076] The temperature of the first heat preservation > the temperature of the second heat preservation;

[0077] The temperature of the first heat preservation is 450 °C; the time of the first heat preservation is 30 min;

[0078] The temperature of the second heat preservation is 380 °C; the time of the second heat preservation is 72 min;

[0079] The tool used for the first turning is a cemented carbide tool. The spindle speed in the first turning is 193 r / min; the feed rate in the first turning is 0.31 mm / r;

[0080] The tool for the second turning is a diamond turning tool; the spindle speed in the second turning is 302 r / min; the cutting amount in the second turning is 0.3 mm; the feed rate in the second turning is 0.076 mm / r.

[0081] In this embodiment, the copper material targeted is a copper tube with a purity of 99.99%.

[0082] For the observation of the copper material obtained after processing, see Table 1 in detail. The photo of the obtained copper material is as Figure 4 shown.

[0083] Example 5

[0084] The present invention provides a surface treatment method for observing the grains of copper material. The surface treatment method includes first heat preservation, first turning, second heat preservation, and second turning sequentially performed on the copper material;

[0085] The temperature of the first heat preservation > the temperature of the second heat preservation;

[0086] The temperature of the first heat preservation is 500 °C; the time of the first heat preservation is 25 min;

[0087] The temperature of the second heat preservation is 385 °C; the time of the second heat preservation is 77 min;

[0088] The tool used for the first turning is a cemented carbide tool. The spindle speed in the first turning is 183 r / min; the feed rate in the first turning is 0.32 mm / r;

[0089] The tool for the second turning is a diamond turning tool; the spindle speed in the second turning is 302 r / min; the cutting amount in the second turning is 0.3 mm; the feed rate in the second turning is 0.075 mm / r.

[0090] In this embodiment, the copper material targeted is a copper tube with a purity of 99.999%.

[0091] For the observation of the copper material obtained after processing, see Table 1 in detail. The photo of the obtained copper material is as Figure 5 shown.

[0092] Example 6

[0093] The present invention provides a surface treatment method for observing the grains of copper material. The surface treatment method includes first heat preservation, first turning, second heat preservation, and second turning sequentially performed on the copper material;

[0094] The temperature of the first heat preservation > the temperature of the second heat preservation;

[0095] The temperature of the first heat preservation is 467 °C; the time of the first heat preservation is 24 min;

[0096] The temperature of the second heat preservation is 334 °C; the time of the second heat preservation is 75 min;

[0097] The tool used for the first turning is a cemented carbide tool, the spindle speed in the first turning is 184 r / min; the feed rate in the first turning is 0.33 mm / r;

[0098] The tool for the second turning is a diamond turning tool; the spindle speed in the second turning is 300 r / min; the cutting amount in the second turning is 0.32 mm; the feed rate in the second turning is 0.08 mm / r.

[0099] In this embodiment, the copper material targeted is copper pipe, and the purity is 99.99%.

[0100] For the observation of the copper material obtained after processing, see Table 1 in detail, and the photo of the obtained copper material is as Figure 6 shown.

[0101] Example 7

[0102] The difference from Example 1 is only that the first heat preservation is not carried out. For the observation of the copper material obtained after processing, see Table 1 in detail, and the photo of the obtained copper material is as Figure 7 shown.

[0103] Example 8

[0104] The difference from Example 1 is only that the second heat preservation is not carried out. For the observation of the copper material obtained after processing, see Table 1 in detail, and the photo of the obtained copper material is as Figure 8 shown.

[0105] Example 9

[0106] The difference from Example 1 is only that the temperatures of the first heat preservation and the second heat preservation are swapped, that is, the temperature of the first heat preservation < the temperature of the second heat preservation. For the observation of the copper material obtained after processing, see Table 1 in detail, and the photo of the obtained copper material is as Figure 9 shown. The obtained copper material is processed twice by the scheme of Example 1, and the photo of the obtained copper material is as Figure 14 shown, and it can be seen that the grain distribution on the surface can be clearly observed.

[0107] Example 10

[0108] The difference from Example 1 is only that the time of the first heat preservation is 70 min. For the observation of the copper material obtained after processing, see Table 1 in detail, and the photo of the obtained copper material is as Figure 10 shown.

[0109] Example 11

[0110] The difference from Example 1 is only that the tool used for the first turning is replaced with a diamond turning tool. The observation of the copper material obtained after processing is shown in detail in Table 1, and the photo of the obtained copper material is as shown in Figure 11 shown.

[0111] Example 12

[0112] The difference from Example 1 is only that the tool used for the second turning is replaced with a cemented carbide tool. The observation of the copper material obtained after processing is shown in detail in Table 1, and the photo of the obtained copper material is as shown in Figure 12 shown.

[0113] Example 13

[0114] The difference from Example 1 is only that the spindle speed of the second turning is adjusted to be the same as that of the first turning. The observation of the copper material obtained after processing is shown in detail in Table 1, and the photo of the obtained copper material is as shown in Figure 13 shown.

[0115] In the above embodiments, the cemented carbide tool used is the cemented carbide tool of the SD-SN1500-CCGT120408 model of Suder. The diamond tool used is the CCGW120404 diamond blade.

[0116] Table 1

[0117]

[0118]

[0119] From the results of the above embodiments, it can be seen that the solution provided by the present invention, without affecting the roughness, that is, obviously the purpose of this application is not the introduction of a specific heat preservation process, nor to improve the final roughness after turning, but for a specific selection to observe the grain situation on the surface of the steel, realizes the observation of whether the grains on the surface of the copper material are abnormal, and realizes the high-efficiency screening of the copper material used before the preparation of the target.

[0120] It is declared that the present invention uses the above embodiments to illustrate the detailed structural features of the present invention, but the present invention is not limited to the above detailed structural features, that is, it does not mean that the present invention must rely on the above detailed structural features to be implemented. Those skilled in the art should understand that any improvement to the present invention, the equivalent replacement of the components selected by the present invention, the addition of auxiliary components, and the selection of specific methods, etc., all fall within the protection scope and disclosure scope of the present invention.

[0121] The preferred embodiments of the present invention have been described in detail above. However, the present invention is not limited to the specific details in the above embodiments. Within the scope of the technical concept of the present invention, various simple modifications can be made to the technical solutions of the present invention, and these simple modifications all fall within the protection scope of the present invention.

[0122] In addition, it should be noted that, among the various specific technical features described in the above specific embodiments, they can be combined in any appropriate manner without conflict. To avoid unnecessary repetition, the present invention will not separately describe various possible combination methods.

[0123] Furthermore, any combination can be made between various different embodiments of the present invention, as long as it does not violate the idea of the present invention, and it should also be regarded as the content disclosed by the present invention.

Claims

1. A surface treatment method for observing the grains of copper materials, characterized in that, The surface treatment method includes first heat preservation, first turning, second heat preservation, and second turning performed on the copper material in sequence; The temperature of the first heat preservation > the temperature of the second heat preservation. The temperature of the first heat preservation is 450 - 570 °C, and the temperature of the second heat preservation is 300 - 400 °C; The tool used for the first turning is a cemented carbide tool, and the tool for the second turning is a diamond turning tool.

2. The surface treatment method according to claim 1, characterized in that, The time of the first heat preservation is 20 - 30 min.

3. The surface treatment method according to claim 1, characterized in that, The spindle speed in the first turning is 180 - 200 r / min.

4. The surface treatment method according to claim 1, characterized in that, The feed rate in the first turning is 0.3 - 0.33 mm / r.

5. The surface treatment method according to claim 1, characterized in that, The time of the second heat preservation is 60 - 90 min.

6. The surface treatment method according to claim 1, characterized in that, The spindle speed in the second turning is 290 - 310 r / min.

7. The surface treatment method according to claim 1, characterized in that, The cutting amount in the second turning is 0.3 - 0.32 mm.

8. The surface treatment method according to claim 1, characterized in that, The feed rate in the second turning is 0.07 - 0.08 mm / r.

9. The surface treatment method according to claim 1, wherein The surface treatment method includes first heat preservation, first turning, second heat preservation, and second turning performed on the copper material in sequence; The temperature of the first heat preservation > the temperature of the second heat preservation; the temperature of the first heat preservation is 450 - 570 °C; the time of the first heat preservation is 20 - 30 min; the temperature of the second heat preservation is 300 - 400 °C; the time of the second heat preservation is 60 - 90 min; The tool used for the first turning is a cemented carbide tool, and the tool for the second turning is a diamond turning tool; the spindle speed in the first turning is 180 - 200 r / min; the feed rate in the first turning is 0.3 - 0.33 mm / r; the spindle speed in the second turning is 290 - 310 r / min; the cutting amount in the second turning is 0.3 - 0.32 mm; the feed rate in the second turning is 0.07 - 0.08 mm / r.

Images