A high-temperature-resistant composite anode substrate and a preparation method thereof

Abstract

The application provides a high-temperature-resistant composite anode base and a preparation method thereof. The preparation method comprises the following steps: firstly, designing and processing a basic component of the composite anode base according to the shape requirement of the composite anode base; and then, welding, isothermal pressing, mechanical processing and high-temperature exhaust treatment are sequentially performed to obtain the finished product of the composite anode base. The preparation method has high production efficiency, and the composite anode base prepared by the method has the advantages of high high-temperature strength and high dynamic balance precision. In addition, the preparation process is relatively simple, and the requirement for equipment is relatively low.

Description

TECHNICAL FIELD

[0001] The present application belongs to the technical field of anode target material for X-ray tube, and particularly relates to a high-temperature-resistant composite anode base and a preparation method thereof. BACKGROUND

[0002] The anode target material is a crucial component in the X-ray tube, and its performance will directly affect the emission intensity and service life of the X-ray tube. The anode target material is required to have the characteristics of resistance to electron bombardment, high X-ray emission dose and rapid heat dissipation under high-temperature use conditions. Therefore, in the prior art, tungsten with high atomic number, high melting point and high density is usually used as the target surface material of the anode target material, a small amount of rhenium is added to the tungsten to improve the resistance to electron bombardment of the target surface material, effectively reduce the dose decay rate and improve the service life; and molybdenum alloy with large heat capacity and smaller specific gravity than tungsten is used as the base material of the anode target material to improve the output power of the anode target material and accelerate heat dissipation, thereby further improving the service life of the anode target material.

[0003] At present, according to the literature “Overview of Rotating Anode Targets for X-ray Tubes Abroad” (Rare Metal and Hard Alloy, Z1, 1987), the preparation of the anode target material for the X-ray tube mainly has the following three processes: one is a powder metallurgy method, that is, various powders are layered and filled in a metal mold according to the shape and requirements of the designed target material, and then pressed and sintered to form a product; this method is simple in process, but the sintering density is low. The second is to use the powder metallurgy method to prepare tungsten-rhenium-molybdenum alloy sintered blanks, and then to obtain the product through mechanical processing after 3-4 times of forging; this process has many forging passes, and stress concentration is easily generated in the local area of the product, leading to cracks, low efficiency and high cost. The third is to use gas phase deposition of tungsten-molybdenum alloy on the molybdenum alloy base; this process often has low density of the tungsten-rhenium layer and low bonding strength with the molybdenum alloy base, so that cracks are easily generated at high temperature, resulting in short service life of the X-ray tube, and this process also easily pollutes the environment.

[0004] In addition, the invention patent CN1048117C discloses a manufacturing method of a butterfly-shaped molybdenum-based tungsten target, which is prepared by combining the powder metallurgy method and the forging method; it is proved in practice that this process has many forging passes, and stress concentration is easily generated in the local area of the product, leading to cracks, so that the efficiency is low and the cost is high.

[0005] The invention patent CN101290852B discloses a preparation method of a WMo graphite composite target material for a high-power X-ray tube, which is prepared by hot-pressing and sintering after layering and stacking the WMo powder in a graphite mold; however, experiments prove that the target disc prepared by this method has high gas impurity content, and the tungsten-molybdenum layer interface has a situation of interlocking of tungsten-molybdenum materials.

[0006] Invention patent CN109702191B discloses a kind of preparation method of high-precision dynamic balance rotating anode target material, first positioning cone is set in pressing mould, then respectively fill tungsten powder and molybdenum powder into pressing mould respectively for pressing after sintering process, turning processing procedure obtains rotating anode target material, wherein, first with the vertex of the taper surface formed by positioning cone in sintered blank as center to process center through hole in turning processing procedure, then with center through hole as reference to turning processing.It is proved that the target disc prepared by the method is prone to crack during use due to the low strength of sintered state.

[0007] Invention patent CN107081517A discloses a kind of SPS diffusion welding method of TZM and WRe dissimilar refractory alloy, uses Ti powder as active intermediate layer, and carries out diffusion welding on TZM alloy and WRe alloy below the recrystallization temperature of base material by using spark plasma sintering technology (SPS), so as to obtain the connecting piece of TZM alloy and WRe alloy;It is proved that this method has high manufacturing condition requirement, cannot be mass-produced, has high cost and low yield.Invention patent CN112958770A discloses a kind of preparation method of WRe / TZM composite material;first, pre-press TZM alloy powder in mould, then press WRe alloy powder after ball milling, finally wrap a layer of carbon felt outside the mould, put into SPS furnace cavity and carry out spark plasma sintering to prepare WRe / TZM composite material;It is proved that the method has poor batch stability and is not suitable for mass production. SUMMARY

[0008] In view of the deficiencies and defects of the prior art, the present application aims to provide a high-temperature-resistant composite anode base and a preparation method thereof.The preparation method of the present application first designs and processes a basic assembly of the composite anode base according to the shape requirements of the composite anode base, and then obtains the finished product of the composite anode base through welding, isothermal pressing, machining, and high-temperature exhaust treatment.The preparation method of the present application has high production efficiency, and the composite anode base prepared thereby has high high-temperature strength and high dynamic balance precision.In addition, the preparation process of the present application is relatively simple and requires relatively low equipment.

[0009] The first aspect of the present application provides a preparation method of a high-temperature-resistant composite anode base, which adopts the following technical solution:

[0010] A preparation method of a high-temperature-resistant composite anode base, comprising the following steps:

[0011] Step one, first, design and process a basic assembly of the composite anode base according to the shape requirements of the composite anode base, the basic assembly includes tungsten alloy target surface blank, molybdenum alloy base blank stacked in order from top to bottom;

[0012] Step two, the tungsten alloy target surface blank and the outer edge of the molybdenum alloy base blank are welded to obtain a shaped assembly;

[0013] Step three, the shaped assembly is first heated, and then the heated shaped assembly is loaded into a mold for real-time heating and pressing treatment (isothermal pressing treatment) to obtain a pressed composite anode base;

[0014] Step four, the pressed composite anode base is machined according to the shape requirement to obtain a machined composite anode base;

[0015] Step five, the machined composite anode base is first cleaned and then subjected to high-temperature exhaust treatment to obtain a composite anode base product.

[0016] In the present application, first, the tungsten alloy target surface blank and the molybdenum alloy base blank are designed and processed according to the shape requirement of the composite anode base, and then the composite anode base product is obtained through welding, isothermal pressing, machining and high-temperature exhaust treatment. Since the tungsten alloy target surface blank and the molybdenum alloy base blank are deformed alloy pieces and are further vacuum heat treated, they have the advantages of high density and high strength compared to traditional powder metallurgy, so that the final composite anode base product has the advantages of high high-temperature strength and high dynamic balance precision. Further, in the present application, the contact surface between the tungsten alloy target surface blank and the molybdenum alloy base blank is connected through isothermal pressing treatment under certain temperature and pressure. After a period of mutual diffusion of atoms in the bonding layer, a diffusion layer is formed on the interface, and finally a stable and reliable connection interface between the tungsten alloy target surface blank and the molybdenum alloy base blank is achieved. In addition, in the present application, the amount of each furnace is large and the isothermal pressing treatment time is short, and the production efficiency of the isothermal pressing process is about 2-10 pieces / h, which is greatly improved compared to the high-temperature vacuum hot pressing welding process (1 piece / furnace, 1 furnace per day).

[0017] In the above preparation method, as a preferred embodiment, in step one, the tungsten alloy target surface blank is prepared by plastic processing and / or machining, vacuum heat treatment using tungsten alloy as raw material; preferably, in the tungsten alloy, the mass fraction of rhenium is 0-10% (such as 0.5%, 1%, 2%, 3%, 5%, 7%, 9%), and the balance is tungsten; preferably, in the tungsten alloy, the mass fraction of rhenium is 0-10% (such as 0.5%, 1%, 2%, 3%, 5%, 7%, 9%), the mass fraction of carbide is ≤1% (such as 0.05%, 0.1%, 0.2%, 0.3%, 0.5%, 0.7%, 0.9%), and the balance is tungsten, wherein the carbide is one or more of HfC, TaC, and ZrC; preferably, the temperature of the vacuum heat treatment is 1500-1700°C (such as 1550°C, 1600°C, 1650°C), the holding time is 60-120 min (such as 80 min, 100 min, 110 min), and the vacuum degree is ≤5×10 -4 Pa.

[0018] The tungsten alloy target surface blank in the present application is prepared by plastic processing and / or machining, vacuum heat treatment using tungsten alloy as raw material, wherein the plastic processing (such as stamping or spinning into an umbrella shape) can further improve the density and strength of the tungsten alloy target surface blank, and the vacuum heat treatment can remove the surface pollution, oxidation and internal residual gas of the tungsten alloy target surface blank, avoiding low joint strength or diffusion connection failure in the subsequent isothermal pressing process. The tungsten alloy in the present application is obtained by powder metallurgy / vacuum melting combined with deformation processing technology. Adding rhenium element in the tungsten alloy can effectively improve the plasticity of tungsten and improve the impact resistance of the tungsten alloy target surface blank, but too high content of rhenium will cause high cost and performance waste. The shape and thickness of the tungsten alloy target surface blank in the present application depend on the design requirements of the composite anode substrate product. In the existing composite anode substrate product, the shape of the tungsten alloy target surface blank is generally umbrella-shaped, and the thickness is 1-1.5 mm. Therefore, in order to leave a processing allowance, the thickness of the tungsten alloy target surface blank is controlled at about 3 mm. The method for preparing the composite anode substrate by isothermal pressing diffusion connection in the present application is also applicable to processing tungsten alloy target surface blanks with greater thickness or thinner thickness.

[0019] In the preparation method, as a preferred embodiment, in step one, the molybdenum alloy base blank is prepared by plastic processing and / or machining, vacuum heat treatment using molybdenum alloy as raw material; preferably, the molybdenum alloy is one of Mo-Ti-Zr alloy (TZM), Mo-Hf-C alloy (MHC), Mo-La alloy (MoLa); preferably, in the Mo-Ti-Zr alloy, Ti is 0.40-0.55% (such as 0.45%, 0.50%, 0.52%) by mass fraction, Zr is 0.06-0.12% (such as 0.07%, 0.09%, 0.11%) by mass fraction, C is 0.01-0.04% (such as 0.02%, 0.025%, 0.03%) by mass fraction, and the balance is Mo; preferably, in the Mo-Hf-C alloy, Hf is 0.8-1.2% (such as 0.9%, 1.0%, 1.1%) by mass fraction, C is 0.05-0.12% (such as 0.08%, 0.1%, 0.11%) by mass fraction, and the balance is Mo; preferably, in the Mo-La alloy, La2O3 is 0.3-0.8% (such as 0.4%, 0.5%, 0.7%) by mass fraction, and the balance is Mo; preferably, the temperature of the vacuum heat treatment is 1500-1700°C (such as 1550°C, 1600°C, 1650°C), the holding time is 60-120 min (such as 80 min, 100 min, 110 min), and the vacuum degree is ≤5×10-3Pa. -4 Pa.

[0020] The molybdenum alloy base blank in the application is prepared by plastic processing and / or machining, vacuum heat treatment using molybdenum alloy as raw material, wherein the plastic processing (such as upsetting forming into a blank cone shape) can further improve the density and strength of the molybdenum alloy base blank, and the vacuum heat treatment can remove the surface pollution, oxidation and internal residual gas of the molybdenum alloy base blank, so as to avoid low joint strength or diffusion connection failure in the subsequent isothermal pressing process. The molybdenum alloy in the application is obtained by powder metallurgy / vacuum melting combined with deformation processing technology. In addition, the shape and thickness of the molybdenum alloy base blank in the application depend on the design requirements of the composite anode base finished product. In the existing composite anode base finished product, the thickness of the molybdenum alloy base blank is generally within 15 mm. The method for preparing the composite anode base by isothermal pressing diffusion connection in the application is also applicable to processing molybdenum alloy base blanks with greater or smaller thickness.

[0021] In the preparation method, as a preferred embodiment, in step one, the surface roughness Ra of the contact surface of the tungsten alloy target surface blank and the molybdenum alloy base blank is ≤0.8.

[0022] In the above preparation method, as a preferred embodiment, in step two, the welding treatment is performed by electron beam or laser in the forming assembly; more preferably, the weld leakage rate is ≤1×10 -10 Pa·m 3 / s.

[0023] In the present application, by limiting the weld leakage rate to ≤1×10 -10 Pa·m 3 / s, it can be ensured that air does not enter between the tungsten alloy target surface blank and the molybdenum alloy base blank, so as to avoid that effective connection cannot be formed in the subsequent isothermal pressing treatment.

[0024] In the above preparation method, as a preferred embodiment, in step three, the heating treatment is performed in a hydrogen heating protection device, and hydrogen is introduced during the heating treatment; preferably, the heating treatment temperature is 1500-1700℃ (such as 1550℃, 1600℃, 1620℃, 1680℃), and the holding time is 10-30min (such as 12min, 15min, 20min, 25min).

[0025] In the present application, first, the forming assembly is subjected to heating treatment in a hydrogen heating protection device, which is beneficial to better diffusion connection between the tungsten alloy target surface blank and the molybdenum alloy base blank in the subsequent real-time heating pressing treatment; wherein the main purpose of introducing hydrogen in the hydrogen heating protection device is to avoid oxidation of the forming assembly during heating. In the present application, if the heating treatment temperature is lower than 1500℃, the forming assembly is prone to cracking during the subsequent real-time heating pressing treatment, and effective diffusion connection cannot be achieved; if the heating treatment temperature is higher than 1700℃, it is difficult to achieve for the current hydrogen heating device. In addition, under the premise of achieving the same diffusion connection effect, too high heating temperature also causes waste of energy.

[0026] In the above preparation method, as a preferred embodiment, in step three, the real-time heating pressing treatment is performed in a hydraulic machine with a real-time heating die; preferably, the preheating temperature of the die when the forming assembly is loaded is 1200-1300℃ (such as 1220℃, 1240℃, 1260℃, 1280℃), the pressing pressure is 200-400MPa (such as 220MPa, 250MPa, 300MPa, 350MPa), and the holding time is 5-20min (such as 8min, 12min, 16min, 18min).

[0027] The hydraulic machine with real-time heating mold in the application can be an existing device, or a mold system can be added to the hydraulic machine to achieve the purpose, when the preheating temperature of the mold is lower than 1200 DEG C, the temperature of the molding assembly placed in the mold drops too fast, so that the atoms in the bonding layer cannot realize effective diffusion, or the temperature of the molding assembly drops too fast, which easily causes cracks in the composite anode matrix; if the temperature of the mold is higher than 1300 DEG C, the temperature is too high, which easily causes short service life of the mold, and the mold material can be H13, 3Cr2W8V and other hot work die steel.

[0028] In the above preparation method, as a preferred embodiment, in step five, the temperature of the high-temperature exhaust treatment is 1500-1700 DEG C (such as 1550 DEG C, 1600 DEG C, 1620 DEG C, 1680 DEG C), the holding time is 60-120 min (such as 70 min, 90 min, 100 min, 110 min), and the exhaust vacuum degree is ≤5*10 -4 Pa.

[0029] The high-temperature exhaust treatment in the application is carried out in a vacuum heating furnace, and the vacuum degree in the furnace is kept ≤5*10 -4 Pa, and the main purpose of the high-temperature exhaust treatment is to remove the residual gas in the composite anode matrix, so as to avoid failure of the composite anode matrix due to excessive gas emission when used in a high-temperature and high-vacuum environment.

[0030] The second aspect of the application provides a high-temperature-resistant composite anode matrix, which is prepared by the above preparation method.

[0031] In the above high-temperature-resistant composite anode matrix, as a preferred embodiment, the unbalance of the composite anode matrix before weight removal is ≤1 g·cm.

[0032] Compared with the prior art, the application has the following positive effects:

[0033] (1) The tungsten alloy target surface blank and the molybdenum alloy matrix blank are designed and processed according to the shape requirements of the composite anode matrix, and the tungsten alloy target surface blank and the molybdenum alloy matrix blank are respectively made of deformed tungsten alloy and molybdenum alloy as raw materials and are prepared by vacuum heat treatment, so they have the advantages of high density and high strength, and compared with the composite anode matrix prepared by the traditional powder metallurgy method, the problems of poor dynamic balance precision caused by uneven powder laying and poor strength caused by small forging deformation are avoided, and the composite anode matrix has the advantages of high strength and high dynamic balance precision.

[0034] (2) The preparation method of the present invention introduces the isothermal pressing process, which greatly improves the production efficiency, enables mass production, and has a high yield compared with the high temperature vacuum hot pressing welding process and SPS diffusion welding process. The production efficiency of the isothermal pressing process of the present invention is about 2-10 pieces / h, which is much higher than that of the high temperature vacuum hot pressing welding process (because the heating and cooling time of this process is long, the holding time is also long, and only one piece can be produced per furnace, the production efficiency of this process is 1 piece / furnace, 1 furnace / day). Under the premise of ensuring the welding quality of the bonding surface between the tungsten alloy target blank and the molybdenum alloy substrate blank, the production cost of the present invention is greatly reduced.

[0035] (3) The isothermal pressing process of the present invention can ensure the bonding strength between the tungsten alloy target blank and the molybdenum alloy substrate blank. No cracks appeared on the bonding surface of the two blanks during use, and no delamination occurred on the bonding surface of the two blanks. Through non-destructive ultrasonic testing, the interface bonding rate of the tungsten alloy target blank and the molybdenum alloy substrate blank is ≥98%; the unbalance of the composite anode substrate before weight removal is ≤1g·cm; and the service life of the finished composite anode substrate is ≥2 years. Attached Figure Description

[0036] Figure 1 This is a schematic cross-sectional view of the molded component obtained using the preparation method of the present invention.

[0037] Explanation of reference numerals in the attached drawings: 1. Tungsten alloy target blank; 2. Molybdenum alloy substrate blank; 3. Welding point. Detailed Implementation

[0038] The technical solutions in the embodiments of the present invention will be clearly and completely described below to enable those skilled in the art to practice and reproduce them. All other embodiments obtained by those skilled in the art based on the embodiments of the present invention are within the scope of protection of the present invention.

[0039] Unless otherwise specified, the test methods in the following embodiments are conventional methods and can be performed according to the techniques or conditions described in the literature in this field or according to the product instructions. The raw materials described in the following embodiments are all available from publicly available commercial sources.

[0040] The high-temperature resistant composite anode matrix prepared by the method of this invention can be used as an anode target material for X-ray tubes.

[0041] Example 1: A method for preparing a high-temperature resistant composite anode substrate, comprising the following steps:

[0042] (1) First, according to Figure 1The shape requirement is shown, and a base assembly of the composite anode substrate (the overall shape is a truncated cone, the diameter of the upper surface is d, the diameter of the lower surface is D, and the angle between the upper surface and the adjacent side surface is the track layer angle α) is designed and processed, which comprises a tungsten alloy target surface blank (the thickness is h1) and a molybdenum alloy substrate blank (the thickness is h2) stacked in sequence from top to bottom; wherein the tungsten alloy target surface blank is made of W5Re alloy (Re: 5% by mass, the balance being W) as raw material by plate stamping + machining forming or machining forming, and then vacuum heat treatment at 1600°C for 60 min under the condition of vacuum degree ≤5×10 -4 Pa, and the thickness h1 is 3 mm; the molybdenum alloy substrate blank is made of TZM molybdenum alloy as raw material by upsetting + machining forming or machining forming, and then vacuum heat treatment at 1600°C for 60 min under the condition of vacuum degree ≤5×10 -4 Pa, and the thickness h2 is 9 mm; the diameter d of the upper surface of the base assembly is 45 mm, the diameter D of the lower surface is 93 mm, and the track layer angle α is 13°, and the surface roughness Ra of the contact surface of the tungsten alloy target surface blank and the molybdenum alloy substrate blank is ≤0.8.

[0043] (2) The outer edge joint of the tungsten alloy target surface blank and the molybdenum alloy substrate blank is formed by electron beam welding to obtain a shaped assembly, which requires that the weld leakage rate is ≤1×10 -10 Pa·m 3 / s.

[0044] (3) The shaped assembly is first heated in a hydrogen gas protection heating furnace, the heating temperature is 1600°C, and the holding time is 10 min; then it is taken out and put into a hydraulic machine with a real-time heating die for real-time heating and pressing treatment; wherein the preheating temperature of the die when the shaped assembly is loaded is 1300°C, the pressing pressure is 300 MPa, and the holding and pressing time is 5 min.

[0045] (4) The composite anode substrate after pressing is mechanically processed according to the shape requirement to obtain a machined composite anode substrate with a lower surface diameter D of 90 mm;

[0046] (5) The machined composite anode substrate is first cleaned and then subjected to high-temperature exhaust treatment to obtain a composite anode substrate product; the temperature of the high-temperature exhaust treatment is 1650°C, the holding time is 90 min, and the exhaust vacuum degree is ≤3×10 -4 Pa.

[0047] The unbalance of the composite anode substrate before weight removal was tested using a Schenker HM10BK dynamic balancing machine. The unbalance result was 0.2 g·cm. Through non-destructive ultrasonic testing, the interface bonding rate between the tungsten alloy target blank and the molybdenum alloy substrate blank was ≥98%. The service life of the resulting composite anode substrate product was ≥2 years.

[0048] Example 2: A method for preparing a high-temperature resistant composite anode substrate, comprising the following steps:

[0049] (1) First, according to Figure 1 The shape requirements are shown. A basic component for the composite anode substrate is designed and fabricated (the overall shape is a frustum, with the diameter of the upper surface denoted as d, the diameter of the lower surface as D, and the angle between the upper surface and its adjacent side surface, i.e., the orbital layer angle, denoted as α). This basic component includes tungsten alloy target blanks (thickness denoted as h1) and molybdenum alloy substrate blanks (thickness denoted as h2) stacked sequentially from top to bottom. The tungsten alloy target blanks are made from W10Re alloy (by mass fraction, Re: 10%, balance W) formed by sheet metal stamping and machining, and then subjected to a vacuum degree ≤ 5 × 10⁻⁶. -4 The molybdenum alloy substrate blank is prepared by vacuum heat treatment at 1550℃ for 120 min under conditions of Pa, with a thickness h1 of 3 mm. The molybdenum alloy substrate blank is made of MHC molybdenum alloy as raw material and is formed by upsetting and machining or machining, and then subjected to vacuum heat treatment at a vacuum degree ≤5×10. -4 The tungsten alloy target blank was prepared by vacuum heat treatment at 1550℃ for 120 min under the condition of Pa, and its thickness h2 is 10 mm. The upper surface diameter d of the base component is 106 mm, the lower surface diameter D is 143 mm, the orbital layer angle α is 8°, and the surface roughness Ra of the contact surface between the tungsten alloy target blank and the molybdenum alloy substrate blank is ≤0.8.

[0050] (2) The outer edge of the tungsten alloy target blank and the molybdenum alloy substrate blank is laser welded to form a molded component, requiring a weld leakage rate ≤1×10⁻⁶. -10 Pa·m 3 / s.

[0051] (3) The molding component is first heated in a hydrogen-protected heating furnace at a temperature of 1650°C and a holding time of 20 min; then it is taken out and placed in a hydraulic press equipped with a real-time heating mold for real-time heating and pressing; wherein, when the molding component is loaded, the preheating temperature of the mold is 1250°C, the pressing pressure is 400 MPa, and the holding time is 20 min.

[0052] (4) The pressed composite anode substrate is machined according to the shape requirements to obtain a machined composite anode substrate with a lower surface diameter D of 140 mm.

[0053] (5) The machined composite anode substrate is first cleaned and then subjected to high-temperature exhaust treatment to obtain the finished composite anode substrate; the high-temperature exhaust treatment temperature is 1600℃, the holding time is 120min, and the exhaust vacuum degree is ≤5×10 -4 Pa.

[0054] The unbalance of the composite anode substrate before weight removal was tested using a Schenker HM10BK dynamic balancing machine. The unbalance result was 0.35 g·cm. Through non-destructive ultrasonic testing, the interface bonding rate between the tungsten alloy target blank and the molybdenum alloy substrate blank was ≥98%. The service life of the resulting composite anode substrate product was ≥2 years.

[0055] Example 3: A method for preparing a high-temperature resistant composite anode substrate, comprising the following steps:

[0056] (1) First, according to Figure 1 The shape requirements are shown. A basic component for the composite anode substrate is designed and fabricated (the overall shape is a frustum, with the diameter of the upper surface denoted as d, the diameter of the lower surface as D, and the angle between the upper surface and its adjacent side surface, i.e., the orbital layer angle, denoted as α). This basic component includes tungsten alloy target blanks (thickness denoted as h1) and molybdenum alloy substrate blanks (thickness denoted as h2) stacked sequentially from top to bottom. The tungsten alloy target blanks are made from W10Re alloy (by mass fraction, Re: 10%, balance W) formed by sheet metal stamping and machining, and then subjected to a vacuum degree ≤ 5 × 10⁻⁶. -4 The molybdenum alloy substrate blank was prepared by vacuum heat treatment at 1600℃ for 90 min under conditions of Pa, with a thickness h1 of 3 mm. The molybdenum alloy substrate blank was prepared by upsetting and machining or machining by mass fraction of MoLa molybdenum alloy (La2O3: 0.5%, balance Mo) and then heat-treated under vacuum of ≤5×10⁻⁶ Pa. -4 The tungsten alloy target blank was prepared by vacuum heat treatment at 1600℃ for 90 min under the condition of Pa, and its thickness h2 is 12 mm. The upper surface diameter d of the base component is 143 mm, the lower surface diameter D is 193 mm, the orbital layer angle α is 7°, and the surface roughness Ra of the contact surface between the tungsten alloy target blank and the molybdenum alloy substrate blank is ≤0.8.

[0057] (2) The outer edge of the tungsten alloy target blank and the molybdenum alloy substrate blank is connected by electron beam welding to form a molded component, requiring a weld leakage rate of ≤1×10⁻⁶. -10 Pa·m 3 / s.

[0058] (3) The molding component is first heated in a hydrogen-protected heating furnace at a temperature of 1700°C and a holding time of 30 min; then it is taken out and placed in a hydraulic press equipped with a real-time heating mold for real-time heating and pressing; wherein, when the molding component is loaded, the preheating temperature of the mold is 1300°C, the pressing pressure is 400 MPa, and the holding time is 20 min.

[0059] (4) The pressed composite anode substrate is machined according to the shape requirements to obtain a machined composite anode substrate with a lower surface diameter D of 190 mm.

[0060] (5) The machined composite anode substrate is first cleaned and then subjected to high-temperature exhaust treatment to obtain the finished composite anode substrate; the high-temperature exhaust treatment temperature is 1700℃, the holding time is 60min, and the exhaust vacuum degree is ≤5×10 -4 Pa.

[0061] The unbalance of the composite anode substrate before weight removal was tested using a Schenker HM10BK dynamic balancing machine. The unbalance result was 0.65 g·cm. Through non-destructive ultrasonic testing, the interface bonding rate between the tungsten alloy target blank and the molybdenum alloy substrate blank was ≥98%. The service life of the resulting composite anode substrate product was ≥2 years.

[0062] Example 4: A method for preparing a high-temperature resistant composite anode substrate, comprising the following steps:

[0063] (1) First, according to Figure 1 As shown in the shape requirements, the basic component of the composite anode substrate was designed and processed (the overall shape is a frustum, the diameter of its upper surface is denoted as d, the diameter of its lower surface is denoted as D, and the angle between the upper surface and its adjacent side surface, i.e., the orbital layer angle, is denoted as α). The basic component includes tungsten alloy target blanks (thickness denoted as h1) and molybdenum alloy substrate blanks (thickness denoted as h2) stacked from top to bottom. The tungsten alloy target blanks are made of W10Re-0.37HfC alloy (by mass fraction, Re: 10%, HfC: 0.37%, balance W) as raw material, formed by sheet metal stamping and machining, and then subjected to a vacuum degree ≤5×10 -4 The molybdenum alloy substrate blank was prepared by vacuum heat treatment at 1600℃ for 90 min under conditions of Pa, with a thickness h1 of 3 mm. The molybdenum alloy substrate blank was prepared by upsetting and machining or machining by mass fraction of MoLa molybdenum alloy (La2O3: 0.8%, balance Mo) and then subjected to vacuum heat treatment at ≤5×10⁻⁶ Pa. -4The tungsten alloy target surface blank and the molybdenum alloy base blank are connected at the outer edge by electron beam welding to obtain a shaped assembly, and the welding seam leakage rate is required to be less than or equal to 1*10-6Pa·m / s.

[0064] (2) The tungsten alloy target surface blank and the molybdenum alloy base blank are connected at the outer edge by electron beam welding to obtain a shaped assembly, and the welding seam leakage rate is required to be less than or equal to 1*10-6Pa·m / s. -10 Pa·m 3 / s.

[0065] (3) The shaped assembly is first heated in a hydrogen-protected heating furnace, the heating temperature is 1650℃, and the holding time is 30min; then it is taken out and placed in a hydraulic machine with a real-time heating mold for real-time heating and pressing treatment; wherein the preheating temperature of the mold when the shaped assembly is loaded is 1300℃, the pressing pressure is 400MPa, and the holding and pressing time is 20min.

[0066] (4) The composite anode base after pressing is mechanically processed according to the shape requirements to obtain a machined composite anode base with a lower surface diameter D of 190mm;

[0067] (5) The machined composite anode base is first cleaned and then subjected to high-temperature exhaust treatment to obtain a composite anode base product; the high-temperature exhaust treatment temperature is 1700℃, the holding time is 60min, and the exhaust vacuum degree is less than or equal to 5*10-4Pa. -4 Pa.

[0068] The unbalance of the composite anode base before deburring is tested by Schenck HM10BK dynamic balancing machine, the unbalance result is 0.55g·cm, and the interface bonding rate of the tungsten alloy target surface blank and the molybdenum alloy base blank is greater than or equal to 98%; the service life of the composite anode base product is greater than or equal to 2 years.

[0069] Comparative Example 1

[0070] In Comparative Example 1, except that step (3) is different from Example 2, the rest are the same as Example 2, specifically: (3) The shaped assembly is first heated in a hydrogen-protected heating furnace, the heating temperature is 1650℃, and the holding time is 30min; then it is taken out and placed in a hydraulic machine with a real-time heating mold for real-time heating and pressing treatment; wherein the preheating temperature of the mold when the shaped assembly is loaded is 1100℃, the pressing pressure is 400MPa, and the holding and pressing time is 20min. The shaped assembly is found to be cracked after being taken out of the furnace, and effective connection is not achieved.

[0071] Comparative Example 2

[0072] In Comparative Example 2, except for step (3), which differs from Example 2, everything else is the same as in Example 2. Specifically, (3) the molding component is first heated in a hydrogen-protected heating furnace at a temperature of 1650°C for 30 minutes; then it is taken out and placed in a hydraulic press equipped with a real-time heating mold for real-time heating and pressing; wherein, the preheating temperature of the mold when the molding component is loaded is 1400°C, the pressing pressure is 400 MPa, and the holding and pressing time is 20 minutes. After exiting the furnace, it was found that the inner cavity of the mold was deformed due to excessive heating, which affected its continued normal use.

[0073] Comparative Example 3

[0074] In Comparative Example 3, except for step (1), which is different from Example 2, everything else is the same as Example 2, specifically: (1) First, according to Figure 1 As shown in the shape requirements, the basic component of the composite anode substrate is designed and processed (the overall shape is a frustum, the diameter of its upper surface is denoted as d, the diameter of its lower surface is denoted as D, and the angle between its upper surface and its adjacent side surface, i.e., the orbital layer angle, is denoted as α). The basic component includes tungsten alloy target blanks (thickness denoted as h1) and molybdenum alloy substrate blanks (thickness denoted as h2) stacked from top to bottom. The tungsten alloy target blank is made of W10Re alloy (by mass fraction, Re: 10%, with the balance being W) through sheet metal stamping and machining, and its thickness h1 is 3mm. The molybdenum alloy substrate blank is made of MHC molybdenum alloy through upsetting and machining or machining, and its thickness h2 is 10mm. The upper surface diameter d of the basic component is 106mm, the lower surface diameter D is 143mm, the orbital layer angle α is 8°, and the surface roughness Ra of the contact surface between the tungsten alloy target blank and the molybdenum alloy substrate blank is ≤0.8.

[0075] The unbalance of the composite anode substrate before weight removal was tested using a Schenker HM10BK dynamic balancing machine, and the unbalance result was 0.5 g·cm. Non-destructive ultrasonic testing showed that the interfacial bonding rate between the tungsten alloy target blank and the molybdenum alloy substrate blank was approximately 85%. Because no vacuum heat treatment was performed, the surface contaminants at the welding interface were not thoroughly cleaned, and excessive adsorbed gases were present, thus affecting the interfacial bonding rate.

[0076] The above description is merely a preferred embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention shall be within the scope of protection of the pending claims of the present invention.

Claims

1. A method of producing a high temperature resistant composite anode substrate, characterized by, It comprises the following steps: Step one, first according to the shape requirements of the composite anode base, design and processing to get the basic components of the composite anode base, the basic components include from top to bottom in turn stacked tungsten alloy target surface blank, molybdenum alloy base blank; Step two, the tungsten alloy target surface blank and the outer edge of the molybdenum alloy base blank are connected and welded to obtain a shaped component; Step three, the shaped component is first subjected to heating treatment, and then the shaped component after heating treatment is loaded into a mold for real-time heating and pressing treatment to obtain a pressed composite anode base; Step four, the composite anode base after pressing is machined according to the shape requirements to obtain a machined composite anode base; Step five, the machined composite anode base is first cleaned and then subjected to high temperature exhaust treatment to obtain a composite anode base finished product; In step one, the tungsten alloy target surface blank is made of tungsten alloy as raw material by plastic processing and / or machining, vacuum heat treatment; the temperature of the vacuum heat treatment is 1500-1700℃, the holding time is 60-120min, the vacuum degree is ≤5×10 - 4 Pa; In step one, the molybdenum alloy base blank is made of molybdenum alloy as raw material through plastic processing and / or machining, vacuum heat treatment; the temperature of the vacuum heat treatment is 1500-1700℃, the holding time is 60-120min, and the vacuum degree is ≤5×10 - 4 Pa; In step three, the heating treatment is carried out in a hydrogen heating protection device, and hydrogen is introduced during the heating treatment; the temperature of the heating treatment is 1500-1700℃, and the holding time is 10-30min; In step three, the real-time heating and pressing treatment is carried out in a hydraulic machine with a real-time heating mold; when the shaped component is loaded, the preheating temperature of the mold is 1200-1300℃, the pressing pressure is 200-400MPa, and the holding and pressure maintaining time is 5-20min; In step five, the temperature of the high-temperature exhaust treatment is 1500-1700℃, the holding time is 60-120min, and the exhaust vacuum degree is ≤5×10 -4 Pa.

2. The production method according to claim 1, characterized by, The mass fraction of rhenium in the tungsten alloy is 0-10%, and the balance is tungsten.

3. The preparation method according to claim 1, characterized in that, The mass fraction of rhenium in the tungsten alloy is 0-10%, the mass fraction of carbide is ≤1%, and the balance is tungsten, wherein the carbide is one or more of HfC, TaC and ZrC.

4. The preparation method according to claim 1, characterized in that, The molybdenum alloy is one of Mo-Ti-Zr alloy, Mo-Hf-C alloy and Mo-La alloy.

5. The preparation method according to claim 4, characterized in that, In the Mo-Ti-Zr alloy, the mass fraction of Ti is 0.40-0.55%, the mass fraction of Zr is 0.06-0.12%, the mass fraction of C is 0.01-0.04%, and the balance is Mo.

6. The preparation method according to claim 4, characterized in that, In the Mo-Hf-C alloy, the mass fraction of Hf is 0.8-1.2%, the mass fraction of C is 0.05-0.12%, and the balance is Mo.

7. The preparation method according to claim 4, characterized in that, In the Mo-La alloy, the mass fraction of La2O3 is 0.3-0.8%, and the balance is Mo.

8. The method of claim 1, wherein, In step one, the surface roughness Ra of the contact surface of the tungsten alloy target surface blank and the molybdenum alloy base blank is ≤0.

8.

9. The method of claim 1, wherein, In step two, the welding treatment to obtain the shaped component is carried out by electron beam or laser welding.

10. The method of claim 9, wherein, The weld leakage rate of the welding process is ≤ 1 x 10 - 10 Pa·m 3 / s.

11. A high temperature resistant composite anode substrate, characterized in that, The composite anode base is prepared by the method of any one of claims 1-10.

12. The refractory composite anode matrix according to claim 11, characterized in that The unbalance of the composite anode base before weight removal is ≤1 g·cm.

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