Copper-manganese alloy ingot, preparation method and application thereof

Abstract

The application provides a copper-manganese alloy ingot and a preparation method and application thereof. The preparation method comprises the following steps: (I) providing a copper charging box, and sealing manganese raw materials in the copper charging box in a vacuum mode; (II) mixing copper raw materials with the copper charging box containing the manganese raw materials in step (I), and then performing a smelting treatment to obtain a copper-manganese alloy melt; and (III) performing a casting treatment on the copper-manganese alloy melt to obtain the copper-manganese alloy ingot. In the application, the manganese raw materials are sealed in the copper charging box in a built-in mode, the corrosion of a crucible is reduced, alloy pollution is avoided, and the quality of the copper-manganese alloy ingot is improved.

Description

Technical Field

[0001] This invention belongs to the field of sputtering target preparation technology, and relates to a copper-manganese alloy ingot, its preparation method and application. Background Technology

[0002] Ultra-high purity 6N (99.9999%) copper-manganese alloy (CuMn alloy) is commonly used as wiring material for integrated circuit chips. With the development of integrated circuit chips, the demand for copper-manganese alloy targets is increasing. In the mass production of copper-manganese alloy target ingots, due to the special requirements of the production process, only high-purity graphite crucibles can be used to manufacture copper-manganese alloy ingots.

[0003] Currently, the common process for manufacturing graphite crucibles is to place high-purity copper electrolytic sheets into the crucible and manganese sheets into the feeding chamber. After the electrolytic copper melts, the manganese sheets are poured from the feeding chamber into the molten copper to melt. After both are fully melted, the mixture is poured to obtain a copper-manganese alloy ingot.

[0004] Existing copper-manganese ingots are mainly made by melting 6N electrolytic copper sheets and 5N manganese sheets. Since oxygen is released during the melting of electrolytic copper sheets, it can easily lead to the oxidation of manganese sheets. At the same time, manganese sheets are highly volatile after melting, resulting in unstable alloy composition. Therefore, it is necessary to use a feeding hopper to separately pack the manganese sheets. After the copper is melted, the manganese sheets in the feeding hopper are added to the copper liquid.

[0005] However, during the addition of manganese flakes, due to equipment design and other factors, splashing can occur, causing the manganese flakes to directly sputter near the crucible or even escape from it. This corrodes the crucible, significantly reducing its lifespan. It also increases the carbon content in the copper-manganese ingot, reducing the quality of the sputtering target. Furthermore, the byproducts of the chemical reaction between the manganese flakes and the graphite crucible also affect the quality of the copper-manganese ingot product. In addition, high-purity graphite crucibles are expensive, and each crucible replacement delays production by at least 15 days, extending production time, severely impacting production, and significantly increasing production costs. Summary of the Invention

[0006] To address the shortcomings of existing technologies, the present invention aims to provide a copper-manganese alloy ingot, its preparation method, and its application. By using a copper container to house and seal the manganese raw material, the oxygen released during copper melting is prevented from oxidizing the manganese raw material, reducing the volatilization of manganese during melting and solving the problems of alloy contamination and crucible corrosion caused by splashing when adding manganese raw material.

[0007] To achieve this objective, the present invention adopts the following technical solution:

[0008] In a first aspect, the present invention provides a method for preparing a copper-manganese alloy ingot, the method comprising:

[0009] (I) Provide a copper material box, and place the manganese raw material in the copper material box and vacuum seal it;

[0010] (II) The copper raw material is mixed with the copper box containing the manganese raw material in step (I) and then smelted to obtain copper-manganese alloy melt;

[0011] (III) The copper-manganese alloy melt is cast to obtain the copper-manganese alloy ingot.

[0012] This invention places manganese raw material in a copper container and seals it, then mixes and melts it with copper raw material. As the copper raw material melts, the manganese raw material is immersed in the copper molten metal and melts naturally. There is no need to use a feeding hopper, which avoids splashing that could cause corrosion or product contamination when manganese raw material is added directly. At the same time, it prevents the oxygen released during copper melting from oxidizing the manganese raw material, reduces the volatilization of manganese during melting, improves the stability of the alloy composition, and can obtain a copper-manganese alloy of higher quality.

[0013] As a preferred embodiment of the present invention, in step (I), the purity of the copper box is ≥99.9999 wt%.

[0014] Preferably, the purity of the manganese raw material is ≥99.999 wt%.

[0015] Preferably, the manganese raw material is electrolytic manganese flakes.

[0016] As a preferred embodiment of the present invention, in step (I), the vacuum degree of the vacuum seal is ≤6.7×10⁻⁶. - 1 Pa.

[0017] Preferably, the vacuum sealing method includes: opening a through hole in the middle of the copper material box, inserting the manganese raw material into the copper material box through the through hole, then placing it in a vacuum chamber to evacuate the vacuum, and sealing the through hole.

[0018] The present invention does not specifically limit the sealing method, and any method known to those skilled in the art can be used. For example, electron beam welding of through holes can be used for sealing.

[0019] This invention, by using a vacuum-sealed copper material box, not only avoids the oxidation of manganese raw materials but also reduces the volatilization of manganese during melting, preventing the formation of manganese carbide that contaminates alloy products and thus improving alloy quality.

[0020] It should be noted that the present invention does not specifically limit the protective gas used in the vacuum sealing process, and it can be any protective atmosphere for vacuuming that is well known to those skilled in the art, such as nitrogen or argon.

[0021] As a preferred technical solution of the present invention, in step (I), the mass ratio of the copper box to the manganese raw material is (15-30):1, for example, it can be 15:1, 16:1, 18:1, 20:1, 22:1, 24:1, 25:1, 28:1 or 30:1, but it is not limited to the listed values. Other unlisted values ​​within this range are also applicable.

[0022] As a preferred embodiment of the present invention, in step (II), the copper raw material is electrolytic copper sheet.

[0023] Preferably, the purity of the electrolytic copper sheet is ≥99.9999 wt%.

[0024] Preferably, the manganese content in the copper-manganese alloy melt is 0.2 to 1 wt%, for example, it can be 0.2 wt%, 0.3 wt%, 0.4 wt%, 0.5 wt%, 0.6 wt%, 0.7 wt%, 0.8 wt%, 0.9 wt%, or 1 wt%, but it is not limited to the listed values. Other unlisted values ​​within this range are also applicable.

[0025] It should be noted that the copper box and the copper raw material in this invention are of the same quality, both using high-purity copper material with a purity of ≥99.9999wt%.

[0026] As a preferred technical solution of the present invention, in step (II), the smelting process includes: putting the copper raw material and copper box into a graphite crucible, heating and holding the temperature for smelting, so that the manganese raw material and copper raw material melt to obtain an alloy melt, and then shaking the graphite crucible to make the alloy melt evenly distributed.

[0027] This invention avoids direct contact or adhesion of manganese raw materials to the graphite crucible by placing them inside a sealed copper container, thus preventing corrosion of the crucible. This extends the crucible's service life, reduces the frequency of crucible replacement, and significantly lowers production costs.

[0028] Preferably, the temperature for heat preservation and melting is 1300-1400℃, for example, it can be 1300℃, 1310℃, 1320℃, 1325℃, 1330℃, 1340℃, 1350℃, 1355℃, 1360℃, 1370℃, 1380℃, 1390℃ or 1400℃, but it is not limited to the listed values, and other unlisted values ​​within this range are also applicable.

[0029] Preferably, the heat preservation and melting time is 60 to 240 minutes, for example, it can be 60 minutes, 70 minutes, 80 minutes, 90 minutes, 100 minutes, 110 minutes, 120 minutes, 150 minutes, 180 minutes, 200 minutes, 220 minutes or 240 minutes, but it is not limited to the listed values. Other unlisted values ​​within this range are also applicable.

[0030] As a preferred embodiment of the present invention, the heating method is as follows: heating to 300-400℃ at a rate of 0.2-0.4℃ / s and holding for 10-15 minutes to complete the first stage of heating; heating to 650-800℃ at a rate of 0.6-0.8℃ / s and holding for 10-15 minutes to complete the second stage of heating; heating to 1000-1200℃ at a rate of 0.6-0.8℃ / s and holding for 5-10 minutes to complete the third stage of heating; and then heating to the required temperature for holding and melting at a rate of 0.3-0.5℃ / s.

[0031] Preferably, the frequency of the shaking is 4 to 6 times / min, for example, it can be 4 times / min, 5 times / min or 6 times / min.

[0032] As a preferred embodiment of the present invention, the casting process includes: sequentially subjecting the copper-manganese alloy melt to a static treatment, melt pouring, cooling treatment, and demolding treatment to obtain the copper-manganese alloy ingot.

[0033] It should be noted that the present invention does not impose specific limitations on the methods, processing times and process parameters of static treatment, molten metal pouring, cooling treatment and demolding treatment. Any static treatment, molten metal pouring, cooling treatment and demolding treatment methods known to those skilled in the art can be used, and the processing time and process parameters can be adjusted according to the actual situation.

[0034] To help those skilled in the art better understand the overall technical solution and working process of the present invention, the present invention provides, by way of example, specific steps of a method for preparing copper-manganese alloy ingots:

[0035] (1) Provide a copper material box with a purity ≥99.9999wt%, make a through hole in the middle of the copper material box, insert manganese raw material with a purity ≥99.999wt% into the copper material box through the through hole, and place it in a vacuum chamber and evacuate it to a vacuum degree ≤6.7×10. -1 Pa, then the through hole is sealed;

[0036] (2) Put copper raw material with a purity ≥99.9999wt% and copper material box containing manganese raw material in step (1) into graphite crucible. Heat to 300-400℃ at a rate of 0.2-0.4℃ / s and hold for 10-15min to complete the first stage of heating. Heat to 650-800℃ at a rate of 0.6-0.8℃ / s and hold for 10-15min to complete the second stage of heating. Heat to 1000-1200℃ at a rate of 0.6-0.8℃ / s and hold for 5-10min to complete the third stage of heating. Heat to 1300-1400℃ at a rate of 0.3-0.5℃ / s and hold for 60-240min to melt manganese raw material and copper raw material to obtain alloy melt.

[0037] (3) Shake the graphite crucible at a frequency of 4 to 6 times / min to make the alloy melt evenly distributed and obtain copper-manganese alloy melt.

[0038] (4) The copper-manganese alloy melt is subjected to static treatment, melt pouring, cooling treatment and demolding treatment in sequence to obtain the copper-manganese alloy ingot.

[0039] In a second aspect, the present invention provides a copper-manganese alloy ingot, wherein the copper-manganese alloy ingot is prepared by the method for preparing copper-manganese alloy ingots described in the first aspect.

[0040] Thirdly, the present invention provides an application of the copper-manganese alloy ingot described in the second aspect, wherein the copper-manganese alloy ingot is used to prepare copper-manganese alloy targets.

[0041] The numerical range described in this invention includes not only the point values ​​listed above, but also any point values ​​within the numerical ranges not listed above. Due to space limitations and for the sake of brevity, this invention will not exhaustively list all the specific point values ​​included in the range.

[0042] Compared with the prior art, the beneficial effects of the present invention are as follows:

[0043] This invention provides a copper-manganese alloy ingot, its preparation method, and its application. Manganese raw material is placed in a sealed copper container and then mixed and smelted with copper raw material. As the copper raw material melts, the manganese raw material is immersed in the molten copper and melts naturally. This eliminates the need for a feeding hopper, avoiding splashing that could cause crucible corrosion or product contamination when manganese raw material is added directly. Simultaneously, it prevents the oxygen released during copper melting from oxidizing the manganese raw material, reducing manganese volatilization during melting, improving the stability of the alloy composition, and resulting in a copper-manganese alloy of superior quality. Detailed Implementation

[0044] The technical solution of the present invention will be further illustrated below through specific embodiments.

[0045] In one specific embodiment, the present invention provides a method for preparing copper-manganese alloy ingots, which specifically includes the following steps:

[0046] (1) Provide a copper material box with a purity ≥ 99.9999 wt%, make a through hole in the middle of the copper material box, insert manganese raw material with a purity ≥ 99.999 wt% into the copper material box through the through hole, and evacuate to a vacuum degree ≤ 6.7 × 10⁻⁶. -1 Pa, then the through hole is sealed, wherein the mass ratio of copper box to manganese raw material is (15-30):1;

[0047] (2) Put copper raw material with a purity ≥ 99.9999 wt% and copper material box containing manganese raw material in step (1) into graphite crucible. Heat to 300-400℃ at a rate of 0.2-0.4℃ / s and hold for 10-15 min to complete the first stage of heating. Heat to 650-800℃ at a rate of 0.6-0.8℃ / s and hold for 10-15 min to complete the second stage of heating. Heat to 1000-1200℃ at a rate of 0.6-0.8℃ / s and hold for 5-10 min to complete the third stage of heating. Then heat to 1300-1400℃ at a rate of 0.3-0.5℃ / s and hold for 60-240 min to melt manganese raw material and copper raw material to obtain alloy melt.

[0048] (3) Shake the graphite crucible at a frequency of 4 to 6 times / min to make the alloy melt evenly distributed, and obtain a copper-manganese alloy melt with a manganese content of 0.2 to 1 wt%.

[0049] (4) The copper-manganese alloy melt is subjected to static treatment, melt pouring, cooling treatment and demolding treatment in sequence to obtain the copper-manganese alloy ingot.

[0050] In another specific embodiment, the present invention provides a copper-manganese alloy ingot, prepared using the method described in one specific embodiment. The copper-manganese alloy ingot of the present invention has stable composition and excellent quality, and can be used in the preparation of copper-manganese alloy targets.

[0051] Example 1

[0052] This embodiment provides a method for preparing copper-manganese alloy ingots, specifically including the following steps:

[0053] (1) Provide a copper material box with a purity ≥ 99.9999 wt%. Make a through hole in the middle of the copper material box, insert an electrolytic manganese sheet with a purity ≥ 99.999 wt% into the copper material box through the through hole, and evacuate to a vacuum degree ≤ 6.7 × 10⁻⁶. -1 Pa, then the through hole is sealed, wherein the mass ratio of copper box to manganese sheet is 15:1;

[0054] (2) Put copper sheets with a purity ≥ 99.9999 wt% and copper boxes containing manganese sheets from step (1) into a graphite crucible. Heat the material to 360°C at a rate of 0.3°C / s and hold for 10 minutes to complete the first stage of heating. Heat the material to 800°C at a rate of 0.6°C / s and hold for 15 minutes to complete the second stage of heating. Heat the material to 1100°C at a rate of 0.8°C / s and hold for 8 minutes to complete the third stage of heating. Then heat the material to 1400°C at a rate of 0.4°C / s and hold for 60 minutes to melt the manganese and copper raw materials to obtain an alloy melt.

[0055] (3) Shake the graphite crucible at a frequency of 6 times / min to make the alloy melt evenly distributed, and obtain copper-manganese alloy melt with a manganese content of 0.5wt%.

[0056] (4) The copper-manganese alloy melt is subjected to static treatment, melt pouring, cooling treatment and demolding treatment in sequence to obtain copper-manganese alloy ingot.

[0057] Example 2

[0058] This embodiment provides a method for preparing copper-manganese alloy ingots, specifically including the following steps:

[0059] (1) Provide a copper material box with a purity ≥ 99.9999 wt%. Make a through hole in the middle of the copper material box, insert an electrolytic manganese sheet with a purity ≥ 99.999 wt% into the copper material box through the through hole, and evacuate to a vacuum degree ≤ 6.7 × 10⁻⁶. -1 Pa, then the through hole is sealed, wherein the mass ratio of copper box to manganese raw material is 18:1;

[0060] (2) Put copper sheets with a purity ≥ 99.9999 wt% and copper boxes containing manganese sheets from step (1) into a graphite crucible. Heat the material to 300°C at a rate of 0.2°C / s and hold for 12 minutes to complete the first stage of heating. Heat the material to 750°C at a rate of 0.8°C / s and hold for 10 minutes to complete the second stage of heating. Heat the material to 1000°C at a rate of 0.6°C / s and hold for 10 minutes to complete the third stage of heating. Then heat the material to 1300°C at a rate of 0.5°C / s and hold for 90 minutes to melt the manganese and copper raw materials to obtain an alloy melt.

[0061] (3) Shake the graphite crucible at a frequency of 5 times / min to make the alloy melt evenly distributed, and obtain copper-manganese alloy melt with a manganese content of 0.5wt%.

[0062] (4) The copper-manganese alloy melt is subjected to static treatment, melt pouring, cooling treatment and demolding treatment in sequence to obtain copper-manganese alloy ingot.

[0063] Example 3

[0064] This embodiment provides a method for preparing copper-manganese alloy ingots, specifically including the following steps:

[0065] (1) Provide a copper material box with a purity ≥ 99.9999 wt%. Make a through hole in the middle of the copper material box, insert an electrolytic manganese sheet with a purity ≥ 99.999 wt% into the copper material box through the through hole, and evacuate to a vacuum degree ≤ 6.7 × 10⁻⁶. -1 Pa, then the through hole is sealed, wherein the mass ratio of copper box to manganese raw material is 21:1;

[0066] (2) Put copper sheets with a purity ≥ 99.9999 wt% and copper boxes containing manganese sheets from step (1) into a graphite crucible. Heat the material to 400°C at a rate of 0.4°C / s and hold for 10 min to complete the first stage of heating. Heat the material to 600°C at a rate of 0.6°C / s and hold for 10 min to complete the second stage of heating. Heat the material to 1200°C at a rate of 0.8°C / s and hold for 5 min to complete the third stage of heating. Then heat the material to 1350°C at a rate of 0.5°C / s and hold for 120 min to melt the manganese and copper raw materials to obtain an alloy melt.

[0067] (3) Shake the graphite crucible at a frequency of 4 times / min to make the alloy melt evenly distributed, and obtain copper-manganese alloy melt with a manganese content of 0.5wt%.

[0068] (4) The copper-manganese alloy melt is subjected to static treatment, melt pouring, cooling treatment and demolding treatment in sequence to obtain copper-manganese alloy ingot.

[0069] Example 4

[0070] This embodiment provides a method for preparing copper-manganese alloy ingots, specifically including the following steps:

[0071] (1) Provide a copper material box with a purity ≥ 99.9999 wt%. Make a through hole in the middle of the copper material box, insert an electrolytic manganese sheet with a purity ≥ 99.999 wt% into the copper material box through the through hole, and evacuate to a vacuum degree ≤ 6.7 × 10⁻⁶. -1 Pa, then the through hole is sealed, wherein the mass ratio of copper box to manganese raw material is 24:1;

[0072] (2) Put copper sheets with a purity ≥ 99.9999 wt% and copper boxes containing manganese sheets from step (1) into a graphite crucible. Heat the material to 350°C at a rate of 0.3°C / s and hold for 10 min to complete the first stage of heating. Heat the material to 700°C at a rate of 0.7°C / s and hold for 12 min to complete the second stage of heating. Heat the material to 1150°C at a rate of 0.6°C / s and hold for 8 min to complete the third stage of heating. Then heat the material to 1400°C at a rate of 0.5°C / s and hold for 180 min to melt the manganese and copper raw materials to obtain an alloy melt.

[0073] (3) Shake the graphite crucible at a frequency of 6 times / min to make the alloy melt evenly distributed, and obtain copper-manganese alloy melt with a manganese content of 0.5wt%.

[0074] (4) The copper-manganese alloy melt is subjected to static treatment, melt pouring, cooling treatment and demolding treatment in sequence to obtain copper-manganese alloy ingot.

[0075] Example 5

[0076] This embodiment provides a method for preparing copper-manganese alloy ingots, specifically including the following steps:

[0077] (1) Provide a copper material box with a purity ≥ 99.9999 wt%. Make a through hole in the middle of the copper material box, insert an electrolytic manganese sheet with a purity ≥ 99.999 wt% into the copper material box through the through hole, and evacuate to a vacuum degree ≤ 6.7 × 10⁻⁶. -1 Pa, then the through hole is sealed, wherein the mass ratio of copper box to manganese raw material is 30:1;

[0078] (2) Put copper sheets with a purity ≥ 99.9999 wt% and copper boxes containing manganese sheets from step (1) into a graphite crucible. Heat the material to 400°C at a rate of 0.4°C / s and hold for 10 min to complete the first stage of heating. Heat the material to 680°C at a rate of 0.8°C / s and hold for 15 min to complete the second stage of heating. Heat the material to 1150°C at a rate of 0.6°C / s and hold for 10 min to complete the third stage of heating. Then heat the material to 1300°C at a rate of 0.4°C / s and hold for 240 min to melt the manganese and copper raw materials to obtain an alloy melt.

[0079] (3) Shake the graphite crucible at a frequency of 5 times / min to make the alloy melt evenly distributed, and obtain copper-manganese alloy melt with a manganese content of 0.5%.

[0080] (4) The copper-manganese alloy melt is subjected to static treatment, melt pouring, cooling treatment and demolding treatment in sequence to obtain copper-manganese alloy ingot.

[0081] Comparative Example 1

[0082] This comparative example provides a method for preparing copper-manganese alloy ingots, specifically including the following steps:

[0083] (1) Place the electrolytic copper sheet in the graphite crucible and the electrolytic manganese sheet in the feeding bin;

[0084] (2) The graphite crucible is heated to 1400℃ so that the copper sheet begins to melt. Then the manganese sheet in the feeding bin is added to the copper melt for smelting so that the manganese melts and forms a copper-manganese alloy melt.

[0085] (3) The copper-manganese alloy melt is subjected to static treatment, melt pouring, cooling treatment and demolding treatment in sequence to obtain copper-manganese alloy ingot.

[0086] Comparative Example 2

[0087] This comparative example provides a method for preparing copper-manganese alloy ingots. The difference from Example 1 is that the copper box with the manganese sheet implanted was not vacuum sealed in step (1). The other operation methods and process parameters are the same as in Example 1.

[0088] The present invention tested the manganese content, metal impurity content and carbon particulate matter (≥1.3μm) of the copper-manganese alloy ingots obtained in the above embodiments and comparative examples, and observed the corrosion of the graphite crucible after the melting was completed. The results are shown in Table 1.

[0089] In this invention, inductively coupled plasma optical emission spectrometry (ICP-OES) is used to detect the manganese content; PP-TOFMS glow discharge mass spectrometry is used to test the purity of copper-manganese ingots; and an insoluble particulate detector (LPC) is used to detect the carbon content.

[0090] Table 1

[0091] Example 1 0.5 Non-corrosive 99.99995 0.59 Example 2 0.5 Non-corrosive 99.99994 0.61 Example 3 0.5 Non-corrosive 99.99992 0.58 Example 4 0.5 Non-corrosive 99.99992 0.61 Example 5 0.5 Non-corrosive 99.99993 0.60 Comparative Example 1 0.43 Minor corrosion 99.99966 0.90 Comparative Example 2 0.45 Minor corrosion 99.99973 0.76

[0092] As shown in Table 1, the copper-manganese ingots obtained in Examples 1 to 5 have high purity, low amount of carbon particles, and high product quality. Furthermore, there is no corrosion in the graphite crucible, which meets the quality requirements for copper-manganese ingots.

[0093] Compared to Example 1, the copper-manganese ingot of Comparative Example 1 showed reduced purity, increased carbon content, fluctuating manganese content, and slight corrosion of the graphite crucible. This was mainly due to the oxygen released during copper melting in Comparative Example 1, which oxidized the manganese flakes, generating manganese oxides. This increased the number of oxide particles in the molten copper, reducing the purity of the copper-manganese ingot. Furthermore, the splashing of manganese flakes during the addition of manganese flakes from the feeding bin in Comparative Example 1 caused direct contact between the manganese and the graphite crucible, resulting in crucible corrosion.

[0094] The purity of the copper-manganese ingot in Comparative Example 2 was lower than that in Example 1, with a slight increase in carbon content, and a certain degree of corrosion of the graphite crucible. This was mainly because the copper box in Comparative Example 2 was not vacuum-sealed, allowing oxygen generated during copper melting to enter the copper box, causing the manganese flakes to oxidize and generate carbon particles, thus reducing the product purity. Furthermore, some manganese flakes melted first after being heated and overflowed from the copper box, directly contacting the graphite crucible and adhering to it, causing corrosion.

[0095] The applicant declares that the above description is only a specific embodiment of the present invention, but the protection scope of the present invention is not limited thereto. Those skilled in the art should understand that any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope disclosed in the present invention fall within the protection and disclosure scope of the present invention.

Claims

1. A method for preparing a copper-manganese alloy ingot, characterized in that, The preparation method includes: (I) Provide a copper material box, and place the manganese raw material in the copper material box and vacuum seal it; (II) The copper raw material and the copper container containing the manganese raw material from step (I) are placed into a graphite crucible. After heating, the mixture is kept at that temperature for melting, so that the manganese and copper raw materials melt to obtain an alloy melt. The graphite crucible is then shaken to ensure that the alloy melt is evenly distributed, resulting in a copper-manganese alloy melt. The manganese content in the copper-manganese alloy melt is 0.2~1wt%. (III) The copper-manganese alloy melt is cast to obtain the copper-manganese alloy ingot.

2. The preparation method according to claim 1, characterized in that, In step (I), the purity of the copper box is ≥99.9999wt%.

3. The preparation method according to claim 1, characterized in that, The purity of the manganese raw material is ≥99.999 wt%.

4. The preparation method according to claim 1, characterized in that, The manganese raw material is electrolytic manganese flakes.

5. The preparation method according to claim 1, characterized in that, In step (I), the vacuum degree of the vacuum seal is ≤6.7×10⁻⁶. -1 Pa.

6. The preparation method according to claim 1, characterized in that, The vacuum sealing method includes: making a through hole in the middle of the copper material box, inserting the manganese raw material into the copper material box through the through hole, then placing it in a vacuum chamber to evacuate the vacuum, and sealing the through hole.

7. The preparation method according to claim 1, characterized in that, In step (I), the mass ratio of the copper box to the manganese raw material is (15~30):

1.

8. The preparation method according to claim 1, characterized in that, In step (II), the copper raw material is electrolytic copper sheet.

9. The preparation method according to claim 8, characterized in that, The purity of the electrolytic copper sheet is ≥99.9999 wt%.

10. The preparation method according to claim 1, characterized in that, The temperature for heat preservation and melting is 1300~1400℃.

11. The preparation method according to claim 1, characterized in that, The heat preservation and melting time is 60~240 minutes.

12. The preparation method according to claim 1, characterized in that, The heating method is as follows: The first stage of heating is completed by raising the temperature to 300-400℃ at a rate of 0.2-0.4℃ / s and holding it for 10-15 minutes; the second stage of heating is completed by raising the temperature to 650-800℃ at a rate of 0.6-0.8℃ / s and holding it for 10-15 minutes; the third stage of heating is completed by raising the temperature to 1000-1200℃ at a rate of 0.6-0.8℃ / s and holding it for 5-10 minutes; and then the temperature is raised to the required melting temperature at a rate of 0.3-0.5℃ / s.

13. The preparation method according to claim 1, characterized in that, The frequency of the shaking is 4 to 6 times per minute.

14. The preparation method according to claim 1, characterized in that, The casting process includes: sequentially subjecting the copper-manganese alloy melt to a static treatment, molten melt pouring, cooling treatment, and demolding treatment to obtain the copper-manganese alloy ingot.