WO2021046929A1

WO2021046929A1 - Large-diameter ni-cr rotating target containing trace elements and preparation method therefor

Info

Publication number: WO2021046929A1
Application number: PCT/CN2019/108215
Authority: WO
Inventors: 吴宇宁; 卿海标; 周其刚
Original assignee: 南京达迈科技实业有限公司
Priority date: 2019-09-12
Filing date: 2019-09-26
Publication date: 2021-03-18
Also published as: CN110484885A

Abstract

A large-diameter Ni-Cr rotating target containing trace elements, comprising the following raw material components in mass percentage: C 0.01-0.05%, B 0.02-0.08%, Zr 0.01-0.06%, Mg 0.05-0.1%, Cr 7-44%, and the balance being Ni and inevitable impurities. Also provided is a preparation method for a large-diameter Ni-Cr rotating target containing trace elements.

Description

Large-diameter Ni-Cr rotating target material containing trace elements and preparation method thereof

Technical field

The invention relates to a magnetron sputtering target material and its preparation, in particular to a large-diameter Ni-Cr rotating target material containing trace elements and a preparation method thereof.

Background technique

With the rapid development of electronics, new energy, construction and other industrial fields, the application requirements for thin film resistors, solar spectrum selective absorption films, and coated glass are also increasing. Therefore, the magnetron sputtering coating technology needs to be more perfect, and the target material is the most critical basic consumable in the magnetron sputtering coating process. How to improve the utilization rate of the target material and the quality of the deposited film? Targets with small and uniform grain size have the advantages of high electrical conductivity, high thermal conductivity, and high strength.

At present, most of the nickel-chromium targets used in China are plane targets, and rotating targets account for only a small part. Blocked by foreign technology, only a few small diameter nickel-chromium rotating targets can be produced in China. Compared with a flat target with a utilization rate of only 20-30%, the utilization rate of a rotating target material can be as high as 70%, or even more than 70%, especially a large-diameter nickel-chromium rotating target material has a higher utilization rate. In addition, large-diameter nickel-chromium rotating targets can be applied to special product coatings, so as to meet more market demands. However, in the traditional pipe-piercing and rolling process of large-diameter nickel-chromium alloy pipes, multiple reaming and mold replacement are required, which is quite costly, and defects such as cracks, inclusions and eccentricity often occur, and the yield is very low. As a result, the production cost of nickel-chromium alloy pipes remains high. In addition, due to the sustainable development concept of environmental protection, the use of heating agents to increase the feeding rate of steel ingots in the alloy smelting process has been banned. In order to improve the yield rate, a simple production process, high yield rate, high precision, and cost are sought. The preparation method of the lower large diameter Ni-Cr rotating target is imperative.

Summary of the invention

Objective of the invention: One of the objectives of the present invention is to provide a large-diameter Ni-Cr rotating target material containing trace elements. The addition of trace elements enables the alloy to be effectively fed during the later stage of solidification, reducing the area of defect formation, and It can inhibit the initiation of cracks, improve the bonding force of the grain boundary, and refine the grains, thereby increasing the yield; the second purpose of the present invention is to improve the preparation method of a large-diameter Ni-Cr rotating target containing trace elements. The obtained rotating target material has high utilization rate, can be applied to special coating industry, and can overcome the problems of nickel-chromium tube cracking, inclusions, defects, eccentricity and processing difficulties during the preparation process.

Technical solution: The large diameter Ni-Cr rotating target containing trace elements of the present invention includes the following components in terms of mass percentage: C 0.01～0.05%, B 0.02～0.08%, Zr 0.01～0.06%, Mg 0.05 ~0.1%, Cr 7~44%, the balance Ni and unavoidable impurities. Among them, the inevitable impurities such as Al, Fe and so on.

Preferably, the content of Fe as an impurity in the rotating target is less than 0.01%. Impurity iron has the greatest impact on the target magnetron sputtering, so the appropriate raw material composition ratio and preparation process are adopted to reduce the impurity iron content in the rotating target.

The present invention also provides a method for preparing the large-diameter Ni-Cr rotating target material containing trace elements. The preparation steps mainly include raw material preparation, vacuum melting, hot forging, machining, hot extrusion, pickling treatment, Solution treatment, cold rolling or boring, annealing treatment, machining or binding; the specific process is:

(1) Vacuum smelting: prepare raw materials before smelting, including photoelectric carbon with purity ≥99.9%, boron particles with purity ≥99.5%, metallic zirconium with purity ≥99.5%, metallic magnesium or nickel-magnesium intermediate alloy with purity ≥99.9%, purity ≥99.43% metallic chromium, 99.96% electrolytic nickel; then the raw materials are mixed with electrolytic nickel, metallic chromium, and photoelectric carbon according to the content of the above components, and then vacuum smelted at 1400～1550℃ for 70～90min, and then zirconium is added , Magnesium or nickel-magnesium master alloy and boron are refined for 10-20 minutes, and then cast in a protective atmosphere to obtain an ingot; wherein the vacuum degree is maintained at less than 4Pa during the entire smelting process; the protective atmosphere during casting can be argon;

(2) Hot forging: rough machining of the ingot before hot forging. The lathe can be used to remove the surface oxide scale and some defects, and the riser can be cut to obtain a round truncated cone-shaped bright ingot, which is carefully ground to remove microcracks, etc.; The ingot is hot forged. The ingot is heated to 1100～1300℃, and after holding for 20～50min, forging is carried out, the forging temperature is 1100～1300℃, and the final forging temperature is 950～1050℃; the ingot is repeatedly roughed and then drawn Long, the deformation is greater than 50%; the deformation of the drawing here is greater than 50%, which is compared with the forging rod after the pier is thick.

(3) Machining: remove the oxide scale on the surface of the hot forged cylindrical forgings, and process the two ends of the forgings smoothly to ensure that the end surface is perpendicular to the cylindrical surface, and then process the center through hole according to the requirements, and process one end of the forging rod Taper holes to obtain alloy cylinders.

(4) Hot extrusion: The alloy cylinder obtained in step (3) is heated by induction heating at a heating temperature of 1100-1200°C; then the hole is expanded at a speed of 150-220mm/s; then a secondary induction is used Heat treatment, the heating temperature is 1110-1220 DEG C, and the hot extruder is used for extrusion, and the extrusion speed is 120-150mm/s, to obtain the waste tube of the rotating target. The waste tube can be processed to an outer diameter of 170-200mm, an inner diameter of 130-160mm, and a length of 2500-4500mm; it can also be adjusted according to the actual needs of the final target processed.

(5) Pickling treatment, solution treatment, cold rolling or boring, annealing treatment, machining or binding are carried out on the waste pipe in sequence.

In the above process, the pickling treatment: pickling the waste pipe to remove defects such as surface pits; the pickling treatment can adopt the common pickling process in the prior art;

Solution treatment: The acid-washed waste pipe is solid-solution treated to obtain a single-phase austenite structure at room temperature, so that the material has the best corrosion resistance, high plasticity, good formability, and can refine the waste pipe The grain structure.

Cold rolling or boring: the surface-treated waste tube is rolled or bored with high precision to obtain a bright tube with an inner hole size tolerance of ±0.2mm.

Annealing treatment: the bright tube is annealed, the annealing temperature is 840～870℃, and the heat preservation is 80～90min.

Machining or binding: Finally, the bright tube is processed to the overall rotating target of the required size, or processed to a certain size, and then the binding rotating target of the required size is made by binding.

Preferably, in step (1) of the above preparation process, the electrolytic nickel is baked at 550-650°C for 5-8 hours. Long-term baking can effectively remove most of the hydrogen contained in electrolytic nickel.

Preferably, in the step (1), zirconium, magnesium, and boron are added in the vacuum melting process by enclosing the zirconium, magnesium, and boron by nickel foil; and the trace alloy elements metal zirconium and metal magnesium are added in the vacuum melting process in the above manner. , Boron particles can avoid boiling and sputtering of molten steel caused by direct addition.

Preferably, the deformation of the pier thickness in the step (2) is 45-60%. In the forging process, the roughness and lengthening are repeated, and the deformation of the roughness is 45-60%, which can fully crush the coarse grain structure, thereby increasing the extrusion yield.

Preferably, the diameter of the central through hole in the step (3) is 20-40 mm, and the taper of the tapered hole is 20°-40°. The central through hole and tapered hole here facilitate the reaming head to correspond to the alloy, and prevent eccentricity caused by reaming.

Preferably, in the step (4), the temperature of the secondary induction heating is 10-20°C higher than the temperature of the previous induction heating. The hole is expanded after induction heating, and then extruded after the second induction heating, and the temperature of the second induction heating is slightly higher than 10-20℃, which can prevent defects or scraps caused by the temperature drop during the extrusion preparation process.

Preferably, in the step (5) solution treatment, the waste pipe is heated to 1000-1100° C. for heat preservation, and then water quenched. A solution treatment at a lower temperature and rapid cooling are adopted to obtain a waste tube with fine grains and improve the plasticity and corrosion resistance of the material.

Preferably, the annealing treatment in the step (5) is specifically: the annealing temperature is 840-870° C., and the heat preservation is 80-90 min.

Principle of the invention: The present invention optimizes the composition by adding a small amount of alloying elements C, B, Zr, and Mg during the vacuum melting process, so that the alloy can be effectively fed in the later stage of solidification, reducing the formation area of defects, and reducing oxygen, sulfur, hydrogen, Nitrogen and other content, and can inhibit the initiation of cracks, improve the grain boundary bonding force of the target material, refine the crystal grains, thereby increasing the yield. Among them, the addition of B element, B segregates on the grain boundary or vacancy type defects, improves the grain boundary bonding force, forms fine M ₃ B ₂ type borides, reduces the formation of TCP phase formed by the combination of impurity elements, and inhibits cracks. It can effectively feed the alloy in the later stage of solidification and reduce the generation of microscopic shrinkage; adding Zr element, Zr can absorb a large amount of oxygen, hydrogen and other gases when heating, especially during high-temperature smelting, it can violently absorb nitrogen, and at the same time , Zr can promote the dispersion of Cr and refine the crystal grains; adding C and Mg elements can further deoxidize, desulfurize, purify the molten metal, and will volatilize at high temperatures without affecting the purity of the molten metal, thereby reducing the purity of the nickel-chromium alloy. The content of interstitial gases such as hydrogen, oxygen, nitrogen, etc., while removing harmful sulfur impurities and refining crystal grains, thereby improving the quality of the alloy and optimizing the alloy composition.

The two key technical links of the present invention are the design of the ratio of the raw materials of the Ni-Cr rotating target and the control of the process conditions, which are complementary to each other. Through suitable component ratio and optimized preparation method, Ni-Cr rotating target is successfully prepared, which can be used to manufacture integral rotating target or bind rotating target to meet more usage requirements.

Beneficial effect: Compared with the prior art,

(1) On the basis of Ni-Cr, the present invention adds a small amount of alloying elements C, B, Zr, and Mg to optimize the composition, so that the alloy can be effectively fed in the later stage of solidification, reducing the area of defect formation, and reducing oxygen, sulfur, The content of hydrogen, nitrogen, etc., and can inhibit the initiation of cracks, improve the bonding force of the grain boundary of the target material, and refine the grains, thereby increasing the yield;

(2) Electrolytic nickel can effectively remove the hydrogen contained in electrolytic nickel through long-term high-temperature baking; through repeated thickening and elongation forging process, reaming after induction heating and extrusion, finishing rolling or finishing after secondary induction heating Processes such as boring can improve the concentricity and yield rate of the rotating target;

(3) The present invention makes the crystal grains of the rotating target material uniform through the addition of trace elements, solution treatment and annealing treatment, and the crystal grain size can be adjusted below 80 μm;

(4) The utilization rate can reach 70%-80% by making the whole rotating target or binding rotating target, which can not only meet more market demands and special needs, but also increase the utilization rate of materials and reduce costs;

(5) The Ni-Cr rotating target containing trace elements of the present invention has simple production process, high yield, high precision, low cost, large pipe diameter, and broad application prospects.

Description of the drawings

Figure 1 is a 100-fold metallographic photograph of the large-diameter Ni-Cr rotating target prepared in Example 1;

2 is a 100-fold metallographic photograph of the large-diameter Ni-Cr rotating target prepared in Example 2;

3 is a 100-fold metallographic photograph of the large-diameter Ni-Cr rotating target prepared in Example 3;

4 is a 100 times metallographic photograph of the large-diameter Ni-Cr rotating target prepared in Example 4;

FIG. 5 is a 100-fold metallographic photograph of the large-diameter Ni-Cr rotating target prepared in Example 5. FIG.

detailed description

The present invention will be described in detail below in conjunction with embodiments.

The reagents and materials used to prepare the large-diameter Ni-Cr rotating target in the following examples are all commercially available.

Example 1:

The composition and content of the large-diameter Ni-Cr rotating target in this embodiment are as follows in terms of mass percentage: C 0.04%, B 0.06%, Zr 0.03%, Mg 0.09%, Cr 44% and the balance Ni and Inevitable impurities.

The preparation method of the large diameter Ni-Cr rotating target includes the following steps:

(1) Vacuum melting: prepare raw materials of photoelectric carbon, boron particles, metal zirconium, metal magnesium, metal chromium, and electrolytic nickel. The raw materials are: photoelectric carbon with a purity of 99.9%, 99.83% boron particles, and 99.9% metal zirconium. 99.9% metallic magnesium, 99.95% metallic chromium, 99.96% electrolytic nickel;

The surface oil stains and oxides of electrolytic nickel and metallic chromium are cleaned and dried and weighed. Then, the electrolytic nickel is kept at 600°C for 6 hours and bake; then the raw materials are prepared according to the content of the above components. First, the electrolytic nickel, metallic chromium, Put the photoelectric carbon into a vacuum melting crucible and smelt with electricity. The melting temperature is 1500℃, and the melting time is 80min. Then add the metal zirconium, metal magnesium and boron particles wrapped in nickel foil successively, and then refining for 15min. The whole melting process is vacuum The degree is less than 4Pa; after smelting, the casting is carried out. Before casting, argon gas 4Mpa is passed in a vacuum state, and the casting is carried out under the condition of protective atmosphere. After 40 minutes of casting, the mold is demolded to obtain the ingot.

(2) The first machining: Use a lathe to remove the oxide scale and some defects on the surface of the ingot, cut off the riser, and obtain a round cone-shaped bright ingot, and carefully grind to remove microcracks, etc.;

(3) Hot forging: heat the machined ingot to 1100°C, hold for 30 minutes, and then perform forging. The forging temperature is 1100°C and the final forging temperature is 950°C; the ingot is repeatedly thickened and thickened. The deformation is 50%, and then it is drawn, and the deformation is 60%. The deformation of the drawing is compared with the forging rod after the pier is thick. Finally forged to

Forging rod

(4) The second machining: remove the surface oxide scale of the cylindrical forging rod, and process both ends of the forging rod to be flat to ensure that the end surface is perpendicular to the cylindrical surface. After processing, it will be a cylinder with a diameter of 299±1mm and a length greater than 500mm. Processed a central through hole with a diameter of 30mm, and processed a tapered hole with a 20° taper at one end to obtain an alloy cylinder;

(5) Hot extrusion: The alloy cylinder is heated by induction heating at a heating temperature of 1130°C, and then a reaming head is used for reaming at a reaming speed of 200mm/s, and then after a second induction heating, the heating temperature is 1140 ℃, and then use a 6500-ton hot extruder to extrude, the extrusion speed is 130mm/s; through hot extrusion, a waste pipe with an outer diameter of 170-200mm, an inner diameter of 130-160mm, and a length of 2500-4500mm is obtained;

(6) Pickling treatment: pickling the waste pipe to remove defects such as surface pits;

(7)Solution treatment: heat the waste pipe to 1000°C for 1 hour, then water quench;

(8) Cold rolling or boring: high-precision rolling or boring of the surface-treated waste tube to obtain a bright tube with an inner hole size tolerance of ±0.2mm;

(9) Annealing treatment: under the annealing temperature condition of 850℃, heat preservation for 85min for annealing treatment;

(10) Machining or binding: the bright tube is processed to the overall rotating target of the required size, or processed to a certain size, and then the binding rotating target of the required size is made by binding.

The metallographic analysis of the large-diameter Ni-Cr rotating target prepared in this example is carried out. The metallographic picture under 100 times is shown in Figure 1. It can be seen that the crystal grains are fine and uniform, and the average grain size is 45-58 μm. .

Example 2:

The composition and content of the large-diameter Ni-Cr rotating target in this embodiment are as follows in mass percentage: C 0.05%, B 0.08%, Zr 0.01%, Mg 0.1%, Cr 40%, and the balance Ni and Inevitable impurities.

The preparation method of the large-diameter Ni-Cr rotating target of this embodiment is basically the same as that of embodiment 1, except that:

In step (1), the purity of the raw materials is 99.9% of photovoltaic carbon, 99.83% of boron particles, 99.9% of metallic zirconium, 99.9% of metallic magnesium, 99.43% of metallic chromium, and 99.96% of electrolytic nickel; Bake at 550℃, heat preservation for 5 hours; smelting temperature is 1400℃, smelting time is 70min, refining time is 10min;

In step (3), the ingot is heated to 1250°C and kept for 20 minutes; the opening forging temperature is 1250°C, and the final forging temperature is 1050°C; the deformation of the pier thickness is 45%;

In step (4), a central through hole with a diameter of 20mm is machined, and one end is machined into a tapered hole with a 30° taper;

In step (5), the induction heating temperature is 1160°C, and the hole expanding speed is 150mm/s; the second induction heating temperature is 1180°C, and the extrusion speed is 120mm/s;

In step (7), the solution treatment is heated to 1100°C;

In step (9), the annealing temperature is 840° C., and the temperature is kept for 80 minutes.

The metallographic analysis of the large-diameter Ni-Cr rotating target prepared in this example is carried out. The metallographic picture at 100 times is shown in Figure 2. It can be seen that the crystal grains are fine and relatively uniform, and the average grain size is 55～76μm.

Example 3:

The composition and content of the large-diameter Ni-Cr rotating target in this embodiment are as follows in terms of mass percentage: C 0.02%, B 0.04%, Zr 0.04%, Mg 0.06%, Cr 10% and the balance Ni and Inevitable impurities.

In step (1), the purity of the raw materials is 99.9% of photovoltaic carbon, 99.83% of boron particles, 99.9% of metallic zirconium, 99.9% of metallic magnesium, 99.43% of metallic chromium, and 99.96% of electrolytic nickel; Bake at 580℃, heat preservation for 8 hours; smelting temperature is 1550℃, smelting time is 90min, refining time is 20min;

In step (3), the ingot is heated to 1300°C for 40 minutes; the opening forging temperature is 1300°C, and the final forging temperature is 1020°C; the deformation of the pier thickness is 60%;

In step (4), a central through hole with a diameter of 30mm is machined, and a tapered hole with a 40° taper is machined at one end;

In step (5), the induction heating temperature is 1100°C, and the hole expanding speed is 160mm/s; the second induction heating temperature is 1110°C, and the extrusion speed is 150mm/s;

In step (7), the solution treatment is heated to 1100°C;

In step (9), the annealing temperature is 870°C and the temperature is kept for 90 minutes.

The metallographic analysis of the large-diameter Ni-Cr rotating target prepared in this example is carried out. The metallographic picture at 100 times is shown in Figure 3. It can be seen that the crystal grains are fine and relatively uniform, and the average grain size is 50～69μm.

Example 4:

The composition and content of the large-diameter Ni-Cr rotating target in this embodiment are as follows in terms of mass percentage: C 0.01%, B 0.02%, Zr 0.06%, Mg 0.05%, Cr 7%, and the balance Ni and Inevitable impurities.

In step (1), the purity of the raw materials is 99.96% of photovoltaic carbon, 99.83% of boron particles, 99.9% of metallic zirconium, 99.9% of metallic magnesium, 99.43% of metallic chromium, and 99.96% of electrolytic nickel; Bake at 650℃, keep warm for 7 hours;

In step (3), the ingot is heated to 1200°C for 50 minutes; the opening forging temperature is 1200°C, and the final forging temperature is 1030°C; the deformation of the pier thickness is 55%;

In step (4), a central through hole with a diameter of 40mm is machined, and a tapered hole with a 40° taper is machined at one end;

In step (5), the induction heating temperature is 1180°C, and the hole expanding speed is 220mm/s; the second induction heating temperature is 1200°C, and the extrusion speed is 140mm/s;

In step (7), the solution treatment is heated to 1000°C;

In step (9), the annealing temperature is 860° C., and the temperature is kept for 85 minutes.

The metallographic analysis of the large-diameter Ni-Cr rotating target prepared in this example is carried out. The metallographic picture at 100 times is shown in Figure 4, and it can be seen that the crystal grains are fine and uniform, and the average grain size is 40-53.5 μm.

Example 5:

The composition and content of the large-diameter Ni-Cr rotating target in this embodiment are as follows in mass percentage: C 0.03%, B 0.05%, Zr 0.05%, Mg 0.08%, Cr 20%, and the balance Ni and Inevitable impurities.

In step (1), the purity of the raw materials is 99.9% of photovoltaic carbon, 99.83% of boron particles, 99.9% of metallic zirconium, 99.9% of metallic magnesium, 99.43% of metallic chromium, and 99.96% of electrolytic nickel; Bake at 620℃, keep heat for 6 hours;

In step (3), the deformation of the pier thickness is 48%;

In step (4), a central through hole with a diameter of 20mm is machined, and a tapered hole with a 40° taper is machined at one end;

In step (5), the induction heating temperature is 1200°C, and the second induction heating temperature is 1220°C;

In step (7), the solution treatment is heated to 1100°C;

The metallographic analysis of the large-diameter Ni-Cr rotating target prepared in this example is carried out. The metallographic picture under 100 times is shown in Figure 5. It can be seen that the crystal grains are fine and uniform, and the average grain size is 47-60 μm. .

Then, the Ni-Cr rotating targets containing trace elements prepared in Examples 1 to 5 were subjected to ICP chemical composition detection and purity testing, and the results are shown in Table 1 and Table 2 respectively. It can be seen from Table 1 that the actual detection content of chromium is slightly higher than the theoretical content (combined purity and input ratio). Trace elements such as zirconium, boron, magnesium, and carbon are all burnt, especially the content of magnesium is very small, so it is not Influencing the purity of the target material, on the contrary, it purifies some impurities and improves the purity; among them, impurity iron has the greatest influence on the magnetron sputtering of the target material, and the iron content of the rotating target material of the present invention is less than 0.01%.

It can be seen from Table 2 that the rotating target of the present invention can maintain the purity above 99.9% through the addition of trace elements and vacuum smelting, and can also prepare a high-purity nickel-chromium rotating target of greater than 99.95%, which satisfies most of the rotating sputtering materials. The purity requirements of the shooting target.

Table 1 Test results of chemical composition of Ni-Cr rotating target containing trace elements

Table 2. Purity test results of Ni-Cr rotating target containing trace elements

Claims

A large-diameter Ni-Cr rotating target containing trace elements, which is characterized by including the following raw material components in terms of mass percentage: C 0.01～0.05%, B 0.02～0.08%, Zr 0.01～0.06%, Mg 0.05 ~0.1%, Cr 7~44%, the balance Ni and unavoidable impurities.
The large-diameter Ni-Cr rotating target containing trace elements according to claim 1, wherein the content of Fe as an impurity in the rotating target is less than 0.01%.
A method for preparing the large-diameter Ni-Cr rotary target containing trace elements according to claim 1 or 2, characterized in that it comprises the following steps:

(1) Vacuum smelting: mix electrolytic nickel, metallic chromium, and photoelectric carbon according to the content of each raw material component, and then vacuum smelt at 1400 to 1550 ℃ for 70 to 90 minutes, then add zirconium, magnesium, and boron to refine for 10 to 20 minutes. Cast in a protective atmosphere to obtain ingots;

(2) Hot forging: heat the ingot to 1100～1300℃ after machining treatment, hold for 20～50min, then carry out forging, the forging temperature is 1100～1300℃, and the final forging temperature is 950～1050℃; The ingot is elongated after repeated thickening, and the deformation is greater than 50%;

(3) Machining: the forging rod obtained in step (2) is subjected to external surface machining treatment, a central through hole is machined according to requirements, and one end of the forging rod is machined with a tapered hole to obtain an alloy cylinder;

(4) Hot extrusion: The alloy cylinder obtained in step (3) is heated by induction heating at a heating temperature of 1100-1200°C; then the hole is expanded at a speed of 150-220mm/s; then a secondary induction is used Heat treatment, the heating temperature is 1110～1220℃, and the hot extruder is used for extrusion, and the extrusion speed is 120～150mm/s to obtain a waste tube;

(5) Pickling treatment, solution treatment, cold rolling or boring, annealing treatment, machining or binding are carried out on the waste pipe in sequence.
The method for preparing a large-diameter Ni-Cr rotating target containing trace elements according to claim 3, wherein the electrolytic nickel in the step (1) is baked at 550-650°C for 5-8 hours .
The method for preparing a large-diameter Ni-Cr rotary target containing trace elements according to claim 3, characterized in that: in the step (1), the addition of zirconium, magnesium, and boron during the vacuum melting process is covered by nickel foil Zirconium, magnesium, boron are added.
The method for preparing a large-diameter Ni-Cr rotating target containing trace elements according to claim 3, wherein the deformation of the pier thickness in the step (2) is 45-60%.
The method for preparing a large-diameter Ni-Cr rotating target containing trace elements according to claim 3, wherein the diameter of the central through hole in the step (3) is 20-40 mm, and the diameter of the tapered hole The taper is 20°～40°.
The method for preparing a large-diameter Ni-Cr rotating target containing trace elements according to claim 3, characterized in that: in the step (4), the temperature of the secondary induction heating is higher than the temperature of the previous induction heating 10～20℃.
The method for preparing a large-diameter Ni-Cr rotating target containing trace elements according to claim 3, wherein the step (5) solution treatment heats the waste pipe to 1000-1100°C for heat preservation, and then water Quenched.
The method for preparing a large-diameter Ni-Cr rotating target containing trace elements according to claim 3, characterized in that: the annealing treatment in the step (5) is specifically: annealing temperature is 840 to 870°C, heat preservation is 80°C. ~90min.