WO2021046928A1

WO2021046928A1 - Large pipe-diameter ni-v rotary target material containing trace elements and preparation method therefor

Info

Publication number: WO2021046928A1
Application number: PCT/CN2019/108213
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: CN110468382B; CN110468382A

Abstract

Disclosed are a large pipe-diameter Ni-V rotary target material containing trace elements and a preparation method therefor. The rotary target material comprises the following components in mass percentages: 0.01-0.05% of C, 0.01-0.08% of B, 0.001-0.006% of Ti, 0.01-0.05% of Mg, 6-8% of V, and the balance being Ni and inevitable impurities. The preparation steps successively use vacuum melting, hot forging, machining, hot squeezing, an acid pickling treatment, a solution treatment, cold rolling or boring, an annealing treatment, and machining or binding. On the basis of Ni-V, the present invention optimizes the ingredients by adding trace elements C, B, Ti and Mg, and decreases the content of oxygen, sulfur, etc., and the present invention can inhibit the creation of cracks, improves the grain boundary binding force and strength of the target material, and refines the crystal grains, thereby improving the yield; furthermore, the invention reduces the rejection rate by optimizing the hot processing parameters.

Description

Large-diameter Ni-V 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-V rotating target material containing trace elements and a preparation method thereof.

Background technique

With the development of science and technology, the development of coating technology is becoming more and more perfect. Magnetron sputtering coating technology, which occupies an important position in the coating field, is also being further improved. Target materials are the most critical basic consumables in the magnetron sputtering coating process. Only the most suitable target materials with high utilization rate, high quality and high quality can fully meet the demand and drive the development of science and technology.

At present, the magnetron sputtering coating technology of nickel-vanadium targets has a relatively large market in the domestic solar field, but most of the nickel-vanadium targets are flat targets, and rotating targets only account for a small part. The main reason is that the current domestic technology can only mass-produce some small-diameter nickel-vanadium rotating targets with a diameter of less than 100mm. Large-diameter nickel-vanadium rotating targets with a diameter of more than 100mm are produced in the traditional pipe-piercing and rolling process. It requires multiple reaming and mold replacement, and the cost is quite high, and defects such as cracks, inclusions and eccentricity often occur, the scrap rate is extremely high, and the cost is too high. Compared with the plane target with a utilization rate of only 30%, the utilization rate of the rotating target can be as high as 70%, especially the utilization rate of the large-diameter nickel-vanadium rotating target can be as high as 80% and above, and the utilization rate of the large-diameter nickel-vanadium rotating target can be as high as 80% and above. The nickel-vanadium rotating target can also be bound by brazing material to meet more market demands. Therefore, it is imperative to find a method for preparing a large-diameter nickel-vanadium rotating target with suitable composition, simple production process, high yield, high precision, and low cost.

Summary of the invention

Objective of the invention: One of the objectives of the present invention is to provide a large-diameter Ni-V rotating target containing trace elements, which uses the addition of trace elements C, B, Ti, and Mg to improve the performance of the rotating target; The second purpose is to provide a method for preparing a large-diameter Ni-V rotating target containing trace elements, which can overcome the problems of nickel-vanadium tube cracking, inclusions, defects, eccentricity, and processing difficulties. Vanadium rotating target.

Technical solution: The large-diameter Ni-V rotating target containing trace elements of the present invention includes the following raw material components in terms of mass percentage: C 0.01-0.05%, B 0.01-0.08%, Ti 0.001-0.006%, Mg 0.01～0.05%, V 6～8%, the balance Ni and unavoidable impurities. Among them, the inevitable impurities such as Al, Fe and so on.

The present invention also provides a method for preparing the large-diameter Ni-V 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, graphite with purity ≥ 99.9, boron particles with purity ≥ 99.9, metallic titanium with purity ≥ 99.9, metallic magnesium with purity ≥ 99.9, metallic vanadium with purity ≥ 99.9, electrolytic nickel with purity ≥ 99.96; Then, the raw materials are mixed with electrolytic nickel, metallic vanadium, and graphite according to the content of the above-mentioned components, and then smelted in a vacuum at 1400-1550°C for 70-90 minutes, and then titanium, magnesium, and boron are added for refining for 10-20 minutes, and then under a protective atmosphere The ingot is obtained by casting; wherein the vacuum degree is kept at less than 4 Pa during the whole 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 1090～1120℃, and after holding for 20～50min, forging is carried out, the forging temperature is 1090～1120℃, and the final forging temperature is 990～1050℃; 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 990 to 1130°C; then the hole is expanded at a speed of 150 to 220 mm/s; and then a secondary induction is used Heat treatment, the heating temperature is 1000～1150℃, and the hot extruder is used for extrusion, and the extrusion speed is 120～150mm/s;

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

Pickling treatment: the waste pipe is pickled 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-mentioned preparation process, the electrolytic nickel is baked at 580-620° C. for 5-8 hours. Long-term baking can effectively remove most of the hydrogen contained in electrolytic nickel.

Preferably, in the step (1), titanium, magnesium, and boron are added in the vacuum melting process by using nickel foil to enclose the titanium, magnesium, and boron; during the vacuum melting process, the micro-alloying elements metal titanium and metal magnesium are added in the above-mentioned 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 greater than 50%. In the forging process, the pier roughening and drawing length are repeated, the pier rough deformation is more than 50%, and the coarse grain structure is fully broken, 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. Enlarging the hole after induction heating, and then extruding after the second induction heating; and the temperature of the second induction heating is slightly higher by 10-20°C, which can prevent defects or scrapping in the extrusion process caused by the temperature drop during the extrusion preparation process .

Preferably, in the step (5) solution treatment, the waste pipe is heated to 950-1000° 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, annealing treatment: annealing the bright tube, 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 trace elements C, B, Ti, Mg in the high vacuum smelting process, reduces the content of oxygen, sulfur, etc., and can inhibit the initiation of cracks, and improve the grain boundary bonding force of the target material. Strength, and refine the grains, thereby increasing the yield. Among them, adding 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, and reduces the formation of μ phase in the TCP phase formed by the combination of impurity elements , Inhibit the generation of cracks; due to the relatively high viscosity of nickel and vanadium during the smelting process, it is difficult to feed during the solidification process. The addition of element B can improve the feeding of the alloy in the later stage of solidification and reduce the generation of microscopic shrinkage; adding Ti Since the impurity element Al and Ni in the alloy form a Ni ₃ Al intermetallic compound, the addition of Ti can replace _{the Al atom in Ni 3} Al to form a Ni ₃ (Al, Ti) type strengthening phase, thereby further improving the alloy’s Strength; adding C and Mg elements, mainly for deoxidation, desulfurization, and purification of molten metal, and will volatilize at high temperatures, and does not affect the purity of molten metal. Thereby reducing the content of interstitial gases such as hydrogen, oxygen and nitrogen in the nickel-vanadium alloy, while removing harmful sulfur impurities and refining crystal grains. Thereby improving the quality of the alloy and optimizing the alloy composition.

Among them, the large-diameter Ni-V rotating target containing trace elements in the present invention is very critical in hot forging and hot extrusion temperature during the hot working process. Based on the hot working principle of the nickel-based alloy, the nickel-based alloy (Ni93V7 ) Carry out experiments and theoretical simulations, and use the thermal processing map to not only get the evolution law of the deformed structure of the material, but also to distinguish the safe area (stable area) and unsafe area (instability area) of the material deformation, so as to achieve the control structure The purpose of evolving, avoiding unsafe areas (instability areas) and optimizing thermal processing parameters. The research method of thermal processing map of dynamic material model has now become the most effective method to study the workability of metal materials and control the deformed structure.

A thermal simulation single-pass compression experiment was performed on a nickel-based alloy (Ni93V7). During the experiment, three sets of rates were set, namely 0.001s ^-1 , 0.1s ^-1 , and 1s ^-1 , and each set of rates set four temperatures: 1000 ℃, 1050℃, 1100℃, 1150℃. Then, based on the flow stress curve results obtained, combined with the processing drawing technology, the thermal deformation behavior of the new material is systematically explored. And through the dynamic material model theory and DMM-based rheological instability determination, the thermal processing diagram of the nickel-based alloy is drawn. Based on the flow stress curve of the nickel-vanadium alloy, the power dissipation of the alloy based on the dynamic material model is established Figure. Because there is no instability phenomenon, the generation of the thermal processing map does not need to superimpose the power dissipation map and the rheological instability map. The power dissipation map is the final thermal processing map.

Based on the analysis of the thermal processing diagram, the specific conclusions are as follows:

(1) Experiments with nickel-vanadium alloy in three sets of strain rates, 0.001s ^-1 , 0.1s ^-1 , 1s ^-1 , and four temperatures for each set of rates: 1000 ℃, 1050 ℃, 1100 ℃, 1150 ℃ Under the conditions, there is no unstable state, and there is no unstable area and rheological instability diagram.

(2) Based on the power dissipation diagram with a strain of 0.2, the value of power dissipation η continues to increase, so there is only one peak area in the nickel-vanadium alloy, and the peak power dissipation area is basically stable at high temperature and high strain rate.

(3) According to the hot working diagram, the best hot working parameters of nickel-vanadium alloy are in the interval of ^{1090～1120℃, 1s -1.}

The two key technical links of the present invention are the ratio design of the Ni-V rotating target material and the control of the process conditions, which are complementary to each other. Especially for hot forging and hot extrusion process parameters, Ni-V rotating targets have been successfully prepared through suitable component ratios and optimized preparation methods. The entire rotating target can be made or bound with the rotating target to meet more requirements. More usage needs.

Beneficial effect: Compared with the prior art,

(1) On the basis of Ni-V, the present invention adds a small amount of alloying elements C, B, Ti, Mg to optimize the composition, reduces the content of oxygen, sulfur, etc., and can inhibit the initiation of cracks, and improve the grain boundary bonding of the target material Strength, strength, and grain refinement can improve the feeding of the alloy in the later stage of solidification, reduce the generation of microscopic shrinkage, and increase the yield.

(2) Electrolytic nickel can effectively remove part of the hydrogen contained in electrolytic nickel through long-term high-temperature baking; through repeated thickening and elongation forging process, hole expansion after induction heating, and extrusion and finish rolling after secondary induction heating Or boring and other technological processes can improve the concentricity and yield rate of the rotating target;

(3) The present invention does not need to add rare earth elements, and successfully prepares a large diameter Ni-V rotating target with low cost and excellent performance through the optimization of the composition and the control of the process conditions;

(4) Through the combination of experiment and theoretical simulation, the present invention draws the hot processing diagram of the nickel-based alloy, obtains the hot forging and hot extrusion optimization parameters of the rotating target, and greatly improves the finished product of the large-diameter Ni-V rotating target rate;

(5) The preparation method of the present invention can overcome the problems of nickel-vanadium tube cracking, inclusions, defects, eccentricity, and processing difficulties, etc., a large-diameter nickel-vanadium rotating target material;

(6) The present invention can achieve 70%-80% utilization rate by manufacturing an integral rotating target or a bound rotating target, which can not only meet more market demands and special demands, but also increase the utilization rate of materials and reduce costs.

Description of the drawings

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

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

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

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

5 is a 100-fold metallographic photograph of the large-diameter Ni-V rotating target prepared in Example 5;

Fig. 6 is a 100-fold metallographic photograph of the large-diameter Ni-V rotating target prepared in Example 6;

Figure 7 is a low-magnification photo of the comparative example during the preparation of Ni-V rotating target;

Figure 8 is a 100-fold metallographic picture of the target of the comparative example.

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-V rotating target in the following examples are all commercially available.

Example 1:

In this embodiment, the composition and content of the large-diameter Ni-V rotating target containing trace elements are as follows: C 0.02%, B 0.03%, Ti 0.005%, Mg 0.01%, V 6% and The balance Ni and unavoidable impurities.

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

(1) Vacuum melting: prepare raw material graphite, boron particles, metallic titanium, metallic magnesium, metallic vanadium, electrolytic nickel, among which the purity of raw materials is 99.9% graphite, 99.9% boron particles, 99.9% metallic titanium, 99.9% Metal magnesium, 99.9% metallic vanadium, 99.96% electrolytic nickel;

The surface oil stains and oxides of electrolytic nickel and metal vanadium are cleaned and dried and weighed. Then, the electrolytic nickel is baked at 600°C for 6 hours; then the raw materials are prepared according to the content of the above components. First, the electrolytic nickel, metal vanadium, Graphite is put into a vacuum melting crucible and smelted with electricity. The melting temperature is 1500℃, and the melting time is 80 minutes. Then, the metal titanium, metal magnesium and boron particles wrapped in nickel foil are added successively, and then refined for 15 minutes. The vacuum degree during the entire melting process Less than 4Pa; casting is performed after smelting, and argon gas 4Mpa is passed in a vacuum state before casting, and the casting is performed under protective atmosphere conditions, and the ingot is demolded after 40 minutes of casting.

(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 to obtain a round truncated 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 1000°C; the ingot is repeatedly thickened and thickened. The amount of deformation is 60%, and then the drawing is carried out, and the drawing deformation is 60%; the drawing deformation here is compared with the forging rod after the pier is thick; the final forging is

Forging rod

(4) Second machining: remove the oxide scale on the surface of the cylindrical forging rod, and process both ends of the forging rod to be flat, ensuring that the end face is perpendicular to the cylindrical surface, and after machining, it will be a cylinder with a diameter of 300 ± 3 mm and a length greater than 500 mm. 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 1000°C, and then the hole is expanded by a reaming head at a reaming speed of 200mm/s, and then subjected to secondary induction heating at a heating temperature of 1020. ℃, and then use a 6500-ton hot extruder for extrusion at a speed of 120mm/s to obtain a waste pipe with an outer diameter of 170-200mm, an inner diameter of 130-160mm, and a length of 2500-4500mm;

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

(7)Solution treatment: heat the waste pipe to 950℃ for heat preservation, heat preservation for 1 hour, and 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 condition of annealing temperature of 850℃, annealing holding time is 80min 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-V 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 there are fine precipitates dispersed at the grain boundary, thus Play a strengthening effect, the grain distribution is uniform, and the average grain size is 47-63μm.

Example 2:

In this embodiment, the composition and content of the large-diameter Ni-V rotating target are as follows: C 0.03%, B 0.01%, Ti 0.003%, Mg 0.03%, V 7% and the balance Ni and Inevitable impurities.

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

In step (1), the electrolytic nickel is baked at 580°C for 5 hours; the melting temperature is 1450°C, the melting time is 70 minutes, and the refining time is 10 minutes;

In step (3), the ingot is heated to 1090°C and held for 20 minutes before forging. The forging temperature is 1090°C and the final forging temperature is 1000°C; the deformation of the pier thickness is 55%, and the deformation after drawing is 55%;

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 1100°C, and the hole expanding speed is 180mm/s; the second induction heating temperature is 1110°C, and the extrusion speed is 130mm/s;

In step (7), the solution treatment is heated to 980°C;

In step (9), the annealing temperature is 840° C., and the annealing holding time is 85 min.

The metallographic analysis of the large-diameter Ni-V rotating target prepared in this example is carried out. The metallographic picture under 100 times is shown in Figure 2. It can be seen that there are fine precipitates dispersed in the grain boundary, thus Play a strengthening effect, the grain distribution is relatively uniform, and the average grain size is 47～80μm

Example 3:

The composition and content of the large-diameter Ni-V rotating target in this embodiment are as follows in terms of mass percentage: C 0.05%, B 0.08%, Ti 0.001%, Mg 0.05%, V 8%, and the balance Ni and Inevitable impurities.

In step (1), the electrolytic nickel is baked at 610°C for 8 hours; the melting temperature is 1400°C, the melting time is 90 minutes, and the refining time is 20 minutes;

In step (3), the ingot is heated to 1110°C and kept for 40 minutes before forging. The forging temperature is 1110°C and the final forging temperature is 990°C; the deformation of the upset thickness is 65%;

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 990°C, and the hole expanding speed is 150mm/s; the second induction heating temperature is 1000°C, and the extrusion speed is 140mm/s;

In step (7), the solution treatment is heated to 970°C;

In step (9), the annealing temperature is 860°C, and the annealing holding time is 90 min.

The metallographic analysis of the large-diameter Ni-V 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 a small amount of fine precipitates are distributed at the grain boundaries, thus Play a strengthening effect, the grain distribution is relatively uniform, and the average grain size is 45-73μm.

Example 4:

The composition and content of the large-diameter Ni-V rotating target in this embodiment are as follows in terms of mass percentage: C 0.03%, B 0.05%, Ti 0.002%, Mg 0.04%, V 6% and the balance Ni and Inevitable impurities.

In step (1), the electrolytic nickel is baked at 620°C for 7 hours; the smelting temperature is 1550°C, and the smelting time is 70min;

In step (3), the ingot is heated to 1120°C and held for 50 minutes before forging. The forging temperature is 1120°C and the final forging temperature is 1050°C; the deformation of the upset 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 1050°C, and the hole expanding speed is 200mm/s; the second induction heating temperature is 1060°C, and the extrusion speed is 150mm/s;

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

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

The metallographic analysis of the large-diameter Ni-V rotating target prepared in this example is carried out. The metallographic picture at 100 times is shown in Figure 4. It can be seen that there are fine precipitates dispersed at the grain boundary, thus Play a strengthening effect, the grain distribution is relatively uniform, and the average grain size is 47-80μm.

Example 5:

In this embodiment, the composition and content of the large-diameter Ni-V rotating target are as follows in terms of mass percentage: C 0.04%, B 0.06%, Ti 0.006%, Mg 0.02%, V 7%, and the balance Ni and Inevitable impurities.

In step (1), the electrolytic nickel is baked at 590°C for 6 hours;

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 1130°C, and the reaming speed is 220mm/s; the second induction heating temperature is 1150°C, and the extrusion speed is 130mm/s;

In step (7), the solution treatment is heated to 960°C;

The metallographic analysis of the large-diameter Ni-V rotating target prepared in this example is carried out. The metallographic picture at 100 times is shown in Figure 5. It can be seen that there are fine precipitates dispersed in the grain boundary, thus Play a strengthening effect, the grain distribution is relatively uniform, and the average grain size is 40-54μm.

Example 6:

In this embodiment, the composition and content of the large-diameter Ni-V rotating target are as follows in terms of mass percentage: C 0.01%, B 0.02%, Ti 0.002%, Mg 0.01%, V 8%, and the balance Ni and Inevitable impurities.

In step (1), the electrolytic nickel is baked at 590°C for 6 hours;

In step (5), the induction heating temperature is 1120°C, and the reaming speed is 160mm/s; the second induction heating temperature is 1140°C, and the extrusion speed is 125mm/s;

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

The metallographic analysis of the large-diameter Ni-V rotating target prepared in this example is carried out. The metallographic picture at 100 times is shown in Figure 6. It can be seen that a small amount of fine precipitates are distributed at the grain boundaries, thus Play a strengthening effect, the grain distribution is relatively uniform, and the average grain size is 45-69μm.

Comparative ratio:

This comparative example is basically the same as Example 1, except that:

In step (3), the ingot is heated to 1150°C, and after holding for 50 minutes, forging is performed, the opening forging temperature is 1150°C, and the final forging temperature is 1000°C;

In step (5), the induction heating temperature is 1140°C; the second induction heating temperature is 1160°C.

As shown in Figure 7, the Ni-V target material of this comparative example was severely cracked after hot extrusion, and obvious cracks can be seen; from Figure 8, it can be seen that the grains are relatively coarse. The grain size is between 80-100μm, the inclusions at the grain boundary are coarse, and the grain boundary is damaged; therefore, the appropriate hot forging temperature and hot extrusion temperature are very important.

Claims

A large-diameter Ni-V rotating target material containing trace elements, which is characterized by including the following components in terms of mass percentage: C 0.01～0.05%, B 0.01～0.08%, Ti 0.001～0.006%, Mg 0.01～ 0.05%, V 6-8% and the balance Ni and unavoidable impurities.
A method for preparing the large-diameter Ni-V rotary target containing trace elements according to claim 1, characterized in that it comprises the following steps:

(1) Vacuum smelting: mix electrolytic nickel, metallic vanadium, and graphite according to the content of each component, then vacuum smelt at 1400～1550℃ for 70～90min, then add titanium, magnesium, boron for refining for 10～20min, and then protect Casting in an atmosphere to obtain an ingot;

(2) Hot forging: heat the ingot to 1090～1120℃ after machining, keep it for 20～50min, then carry out forging, the forging temperature is 1090～1120℃, and the final forging temperature is 990～1050℃; 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 990 to 1130°C; then the hole is expanded at a speed of 150 to 220 mm/s; and then a secondary induction is used Heat treatment, the heating temperature is 1000-1150℃, 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-V rotating target containing trace elements according to claim 2, wherein the electrolytic nickel in the step (1) is baked at 580-620°C for 5-8 hours .
The method for preparing a large-diameter Ni-V rotating target containing trace elements according to claim 2, wherein the addition of titanium, magnesium, and boron in the vacuum melting process in the step (1) is wrapped by nickel foil Titanium, magnesium, boron are added.
The method for preparing a large-diameter Ni-V rotating target containing trace elements according to claim 2, wherein the deformation of the thickness of the pier in the step (2) is greater than 50%.
The method for preparing a large-diameter Ni-V rotating target containing trace elements according to claim 2, 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-V rotating target containing trace elements according to claim 2, 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-V rotating target containing trace elements according to claim 2, characterized in that: in step (5) solution treatment, the waste pipe is heated to 950-1000°C for heat preservation, and then water Quenched.
The method for preparing a large-diameter Ni-V rotating target containing trace elements according to claim 2, characterized in that: the annealing treatment in step (5) is specifically: annealing temperature is 840 to 870°C, heat preservation is 80°C. ~90min.