CN114914135A - High-temperature-resistant composite anode matrix and preparation method thereof - Google Patents
High-temperature-resistant composite anode matrix and preparation method thereof Download PDFInfo
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Abstract
The invention provides a high-temperature-resistant composite anode matrix and a preparation method thereof. The preparation method has high production efficiency, and the prepared composite anode matrix has the advantages of high-temperature strength and high dynamic balance precision.
Description
Technical Field
The invention belongs to the technical field of preparation of anode targets for X-ray tubes, and particularly relates to a high-temperature-resistant composite anode matrix and a preparation method thereof.
Background
The anode target is a vital component in the X-ray tube, and the performance of the anode target directly affects the emission intensity and the service life of the X-ray tube. The anode target material is required to have the characteristics of electron bombardment resistance, high X-ray emission dose and rapid heat dissipation under the high-temperature use condition, so that tungsten with high atomic number, high melting point and high density is generally adopted as a target surface material of the anode target material in the prior art, and a small amount of rhenium is added into the tungsten to further improve the electron bombardment resistance of the target surface material, effectively reduce the dose attenuation speed and prolong the service life; and molybdenum alloy with large heat capacity and smaller specific gravity than tungsten is used as the matrix material of the anode target material, so that the output power of the anode target material is improved, the heat loss is accelerated, and the service life of the anode target material is further prolonged.
At present, the preparation of the anode target material for the X-ray tube is based on the literature "general description of the rotary anode target for the foreign X-ray tube" (rare metal and cemented carbide, 1987, Z1), and the following three processes are mainly used: one is a powder metallurgy method, namely, various powders are filled in a metal die layer by layer according to the shape and the requirement of a designed target material, and then the powders are pressed by adopting a certain process and further sintered and molded; although the process is simple, the sintering density is low. And secondly, preparing a tungsten-rhenium-molybdenum alloy sintering blank by adopting a powder metallurgy method, forging for 3-4 times, and then preparing a product by a mechanical processing mode. The third is to adopt vapor deposition of tungsten-rhenium alloy on a molybdenum alloy matrix, and the process is easy to crack when in use at high temperature due to the low density of the tungsten-rhenium layer and the low bonding strength with the molybdenum alloy matrix, so that the service life of the X-ray tube is short, and the process is easy to pollute the environment.
In addition, the invention patent CN1048117C discloses a manufacturing method of a butterfly-shaped molybdenum-based tungsten target, the molybdenum-based tungsten target is prepared by combining a powder metallurgy method and a forging method, and practice proves that the forging process has multiple forging passes, and the local area of the product is easy to generate stress concentration to cause cracks, so that the efficiency is low and the cost is high.
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 laminating WMo powder in a graphite die and then hot-pressing and sintering the laminated WMo powder.
The invention discloses a preparation method of a high-precision dynamic balance rotary anode target material, which comprises the steps of firstly arranging a positioning cone in a pressing die, then respectively filling tungsten powder and molybdenum powder into the pressing die for pressing, and then carrying out a sintering process and a turning process to obtain the rotary anode target material, wherein in the turning process, a central through hole is firstly processed by taking the vertex of a conical surface formed by the positioning cone in a sintered blank as a center, and then turning is carried out by taking the central through hole as a reference. Practice proves that the target disc prepared by the method is easy to crack in the using process due to lower sintered strength.
The invention patent CN107081517A discloses an SPS diffusion welding method of TZM and WRe dissimilar refractory alloy, Ti powder is used as an active intermediate layer, and the TZM alloy and the WRe alloy are subjected to diffusion welding at the recrystallization temperature lower than that of a base material by Spark Plasma Sintering (SPS), so that a connecting piece of the TZM alloy and the WRe alloy is obtained; practice proves that the method has higher requirements on manufacturing conditions, can not be produced in batch, and has higher cost and lower yield. The invention patent CN112958770A discloses a preparation method of a WRe/TZM composite material; firstly, filling TZM alloy powder into a die for prepressing, then filling ball-milled WRe alloy powder for pressing, finally wrapping a layer of carbon felt outside the die, and putting the die into an SPS furnace chamber for spark plasma sintering to prepare a WRe/TZM composite material; practice proves that the method has poor batch stability and is not suitable for batch production.
Disclosure of Invention
Aiming at the defects and defects of the prior art, the invention aims to provide a high-temperature-resistant composite anode matrix and a preparation method thereof. The preparation method has high production efficiency, and the prepared composite anode matrix has the advantages of high-temperature strength and high dynamic balance precision.
The invention provides a preparation method of a high-temperature-resistant composite anode matrix, which adopts the following technical scheme:
a preparation method of a high-temperature-resistant composite anode matrix comprises the following steps:
firstly, designing and processing a base component of the composite anode substrate according to the shape requirement of the composite anode substrate, wherein the base component comprises a tungsten alloy target surface blank and a molybdenum alloy substrate blank which are sequentially stacked from top to bottom;
welding the outer ring edge connecting part of the tungsten alloy target surface blank and the molybdenum alloy matrix blank to obtain a forming assembly;
step three, firstly heating the molding assembly, then loading the molding assembly subjected to heating treatment into a mold for real-time heating pressing treatment (isothermal pressing treatment), and obtaining a pressed composite anode substrate;
step four, carrying out machining treatment on the pressed composite anode matrix according to the shape requirement to obtain the machined composite anode matrix;
and step five, cleaning the machined composite anode substrate, and then performing high-temperature exhaust treatment to obtain a composite anode substrate finished product.
Firstly, designing and processing a tungsten alloy target surface blank and a molybdenum alloy substrate blank according to the shape requirement of a composite anode substrate, and then carrying out welding, isothermal pressing, machining and high-temperature exhaust treatment to obtain a composite anode substrate finished product; because the tungsten alloy target surface blank and the molybdenum alloy matrix blank belong to morphotropic alloy pieces and are obtained by further vacuum heat treatment, compared with the traditional powder metallurgy, the method has the advantages of high density and high strength, and the finally obtained composite anode matrix finished product has the advantages of high-temperature strength, high dynamic balance precision and the like. Further, in the invention, the connection of the contact surface between the tungsten alloy target surface blank and the molybdenum alloy matrix blank is realized through isothermal pressing treatment, namely under certain temperature and certain pressure, and a diffusion layer is formed on the interface through the mutual diffusion of bonding layer atoms for a period of time, so that a firm and stable connection interface is finally generated between the tungsten alloy target surface blank and the molybdenum alloy matrix blank. In addition, because the charging amount of each furnace is large and the isothermal pressing treatment time is short, the production efficiency of the isothermal pressing process is about 2-10 sheets/h, and the production efficiency is greatly improved compared with that of a high-temperature vacuum hot-pressing welding process (1 sheet/furnace, 1 furnace every day).
In the above manufacturing method, as a preferred embodiment, in the step one, the tungsten alloy target surface blank is subjected to plastic working and/or plastic working by using a tungsten alloy as a raw materialMachining and vacuum heat treatment; 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 less than or equal to 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, ZrC; preferably, the temperature of the vacuum heat treatment is 1500- -4 Pa。
The tungsten alloy target surface blank is prepared by adopting tungsten alloy as a raw material through plastic processing and/or machining and vacuum heat treatment, wherein the density and the strength of the tungsten alloy target surface blank can be further improved through plastic processing (such as stamping or spinning into an umbrella shape), the vacuum heat treatment can remove surface pollution, oxidation and residual gas in the tungsten alloy target surface blank, and the phenomenon that the strength of a connecting part is low or diffusion connection fails in subsequent isothermal pressing treatment is avoided. The rhenium element is added into the tungsten alloy, so that the plasticity of tungsten can be effectively improved, the shock resistance of a tungsten alloy target surface blank is improved, and the cost is high and the performance is wasted due to the overhigh rhenium content. The shape, thickness and the like of the tungsten alloy target surface blank in the invention depend on the design requirements of the composite anode substrate finished product, in the existing composite anode substrate finished product, the tungsten alloy target surface blank is generally umbrella-shaped, and the thickness is 1-1.5mm, so the thickness of the tungsten alloy target surface blank is controlled to be about 3mm in order to keep the processing allowance, and the method for preparing the composite anode substrate by adopting isothermal pressing diffusion connection is also suitable for processing the tungsten alloy target surface blank with thicker or thinner thickness.
In the above preparation method, as a preferred embodiment, in the step one, the molybdenum alloy base blank is prepared by using a molybdenum alloy as a raw material and performing plastic processing and/or machining and vacuum heat treatment;preferably, the molybdenum alloy is one of Mo-Ti-Zr alloy (TZM), Mo-Hf-C alloy (MHC) and Mo-La alloy (MoLa); preferably, in the Mo-Ti-Zr alloy, in mass fraction, Ti: 0.40-0.55% (e.g., 0.45%, 0.50%, 0.52%), Zr: 0.06-0.12% (e.g., 0.07%, 0.09%, 0.11%), C: 0.01-0.04% (e.g., 0.02%, 0.025%, 0.03%), with the balance being Mo; preferably, in the Mo-Hf-C alloy, the mass fraction of Hf: 0.8-1.2% (e.g., 0.9%, 1.0%, 1.1%), C: 0.05-0.12% (e.g., 0.08%, 0.1%, 0.11%), and the balance Mo; preferably, La is present in the Mo-La alloy in a mass fraction 2 O 3 : 0.3-0.8% (e.g., 0.4%, 0.5%, 0.7%), with the balance being Mo; preferably, the temperature of the vacuum heat treatment is 1500- -4 Pa。
The molybdenum alloy matrix blank is prepared by adopting molybdenum alloy as a raw material through plastic processing and/or machining and vacuum heat treatment, wherein the density and the strength of the molybdenum alloy matrix blank can be further improved through plastic processing (such as upsetting and forming into a blank cone shape), the surface pollution, oxidation and residual gas in the molybdenum alloy matrix blank can be removed through the vacuum heat treatment, and the phenomenon that the strength of a connecting part is low or diffusion connection fails in subsequent isothermal pressing treatment is avoided. In addition, the shape, the thickness and the like of the molybdenum alloy matrix blank in the invention depend on the design requirements of the composite anode matrix finished product, the thickness of the molybdenum alloy matrix blank in the existing composite anode matrix finished product is generally within 15mm, and the method for preparing the composite anode matrix by adopting isothermal pressing diffusion connection is also suitable for processing the molybdenum alloy matrix blank with thicker or thinner thickness.
In the above manufacturing method, as a preferred embodiment, in the first step, the surface roughness Ra of the contact surface of the tungsten alloy target surface blank and the molybdenum alloy base blank is less than or equal to 0.8.
Among the above-mentioned preparation methods, one preferable isIn the second step, in the formed assembly obtained by the welding treatment, the welding treatment is carried out by adopting an electron beam or laser; more preferably, the weld leak rate is less than or equal to 1 multiplied by 10 -10 Pa·m 3 /s。
In the invention, the leakage rate of the welding seam is limited to be less than or equal to 1 multiplied by 10 -10 Pa·m 3 And/s, air can be prevented from entering between the contact surfaces of the tungsten alloy target surface blank and the molybdenum alloy base body blank, so that effective connection cannot be formed in the subsequent isothermal pressing treatment.
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 temperature of the heat treatment is 1500-.
According to the invention, the forming assembly is heated in the hydrogen heating protection device, so that the forming assembly is favorable for realizing better diffusion connection between the tungsten alloy target surface blank and the molybdenum alloy matrix blank in the subsequent real-time heating pressing treatment process; the hydrogen is introduced into the hydrogen heating protection device to prevent the molding assembly from being oxidized during heating. If the temperature of the heating treatment is lower than 1500 ℃, the formed assembly is easy to crack in the subsequent real-time heating pressing treatment process, and effective diffusion connection cannot be realized; if the temperature of the heat treatment is higher than 1700 ℃, it is difficult to realize with the current hydrogen heating apparatus. In addition, on the premise of achieving the same diffusion bonding effect, energy is wasted due to too high heating temperature.
In the above production method, as a preferred embodiment, in step three, the real-time heating and pressing treatment is performed in a hydraulic press equipped with a real-time heating die; preferably, the preheating temperature of the mold when the molding assembly is assembled is 1200-1300 ℃ (such as 1220 ℃, 1240 ℃, 1260 ℃, 1280 ℃), the pressing pressure is 200-400MPa (such as 220MPa, 250MPa, 300MPa, 350MPa), and the heat preservation and pressure maintaining time is 5-20min (such as 8min, 12min, 16min, 18 min).
The hydraulic press with the real-time heating die can be the existing equipment, and can also be realized by adding a die system on the basis of the hydraulic press, when the preheating temperature of the die is lower than 1200 ℃, the temperature of the forming assembly placed in the die is reduced too fast due to too low temperature of the die, so that the atoms of the bonding layer can not realize effective diffusion, or the composite anode substrate is easy to generate cracks due to too fast temperature reduction of the forming assembly; if the temperature of the die is higher than 1300 ℃, the temperature is too high, which easily causes the short service life of the die, and the die material can be hot-work die steel such as H13, 3Cr2W8V, and the like.
In the above preparation method, as a preferred embodiment, in the step five, the temperature of the high-temperature exhaust treatment is 1500- -4 Pa。
The high-temperature exhaust treatment is carried out in a vacuum heating furnace, and the vacuum degree in the furnace is kept to be less than or equal to 5 multiplied by 10 -4 Pa, the main purpose of the high-temperature exhaust treatment is to remove residual gas in the composite anode matrix, thereby avoiding the composite anode matrix from losing efficacy due to overlarge exhaust amount when the composite anode matrix is used in a high-temperature and high-vacuum environment.
The invention provides a high-temperature-resistant composite anode matrix in a second aspect, and the composite anode matrix is prepared by the preparation method.
In the high-temperature resistant composite anode matrix, the unbalance amount of the composite anode matrix before weight removal is less than or equal to 1g cm as a preferable implementation.
Compared with the prior art, the invention has the following positive effects:
(1) according to the invention, firstly, a tungsten alloy target surface blank and a molybdenum alloy base blank are designed and processed according to the shape requirement of the composite anode base, and the tungsten alloy target surface blank and the molybdenum alloy base blank are respectively prepared by adopting a morphotropic tungsten alloy and a molybdenum alloy as raw materials through vacuum heat treatment, so that the tungsten alloy target surface blank and the molybdenum alloy base blank have the advantages of high density and high strength.
(2) Compared with the high-temperature vacuum hot-pressing welding process, SPS diffusion welding process and other processes, the isothermal pressing treatment process has the advantages that the production efficiency is greatly improved, the batch production can be realized, the yield is high, the production efficiency of the isothermal pressing treatment process is about 2-10 sheets/h and is far higher than that of the high-temperature vacuum hot-pressing welding process (because the process has longer temperature rise and fall time and long heat preservation time, each furnace can only produce a single sheet, the production efficiency of the process is 1 sheet/furnace and every day/furnace), and the production cost is greatly reduced on the premise of ensuring the welding quality of the joint surface of the tungsten alloy target surface blank and the molybdenum alloy matrix blank.
(3) The isothermal pressing process can ensure the bonding strength between the tungsten alloy target surface blank and the molybdenum alloy matrix blank, the bonding surface of the two blanks has no crack in the using process, the bonding surface of the two blanks has no layering condition, and the interface bonding rate of the tungsten alloy target surface blank and the molybdenum alloy matrix blank is more than or equal to 98% through nondestructive ultrasonic detection; the unbalance amount of the composite anode substrate before de-weighting is less than or equal to 1g cm; the service life of the obtained composite anode substrate finished product is more than or equal to 2 years.
Drawings
Fig. 1 is a schematic sectional structure view of a molded component obtained by the production method of the present invention.
Description of reference numerals: 1. a tungsten alloy target surface blank; 2. a molybdenum alloy base blank; 3. and (7) welding points.
Detailed Description
The technical solutions in the embodiments of the present invention will be described below clearly and completely to enable those skilled in the art to practice and reproduce. All other embodiments that can be derived by one of ordinary skill in the art from the embodiments given herein are intended to be within the scope of the present invention.
The test methods in the following examples are conventional methods unless otherwise specified, and may be carried out according to the techniques or conditions described in the literature in the art or according to the product specifications. The starting materials described in the following examples are all commercially available from the public.
The high-temperature-resistant composite anode substrate prepared by the method can be used as an anode target material of an X-ray tube.
Embodiment 1 a method for preparing a high temperature resistant composite anode substrate, comprising the steps of:
(1) firstly, according to the shape requirements shown in fig. 1, designing and processing to obtain a base assembly of the composite anode substrate (the overall shape is a circular truncated cone, the diameter of the upper surface is recorded as D, the diameter of the lower surface is recorded as D, and the angle between the upper surface and the adjacent side surface, namely the angle of the track layer is recorded as alpha), wherein the base assembly comprises a tungsten alloy target surface blank (the thickness of the tungsten alloy target surface blank is recorded as h1) and a molybdenum alloy substrate blank (the thickness of the molybdenum alloy substrate blank is recorded as h2) which are sequentially stacked from top to bottom; wherein, the tungsten alloy target surface blank adopts W5Re alloy (Re: 5% by mass and the balance W) as raw material, and is formed by plate punching and machining or machining, and then the vacuum degree is less than or equal to 5 multiplied by 10 -4 Is prepared by vacuum heat treatment at 1600 ℃ for 60min under the condition of Pa, and the thickness h1 is 3 mm; the molybdenum alloy matrix blank adopts TZM molybdenum alloy as a raw material and is formed by upsetting, machining or machining, and then the blank is not more than 5 multiplied by 10 in vacuum degree -4 Is prepared by vacuum heat treatment at 1600 ℃ for 60min under the condition of Pa, and the thickness h2 is 9 mm; the diameter D of the upper surface of the base component is 45mm, the diameter D of the lower surface of the base component is 93mm, the angle alpha of the track layer is 13 degrees, and the surface roughness Ra of the contact surface of the tungsten alloy target surface blank and the molybdenum alloy matrix blank is less than or equal to 0.8.
(2) The outer ring edge joint of the tungsten alloy target surface blank and the molybdenum alloy matrix blank is formed by electron beam welding to obtain a formed component, and the requirement of ensuring that the leakage rate of a welding seam is less than or equal to 1 multiplied by 10 -10 Pa·m 3 /s。
(3) Heating the formed assembly in a hydrogen protection heating furnace at 1600 ℃ for 10 min; then taking out and putting into a hydraulic press with a real-time heating mould to carry out real-time heating and pressing treatment; wherein the preheating temperature of the die is 1300 ℃, the pressing pressure is 300MPa, and the heat preservation and pressure maintaining time is 5min when the die is installed in a molding assembly.
(4) Machining the pressed composite anode substrate according to the shape requirement to obtain a machined composite anode substrate with the lower surface diameter D of 90 mm;
(5) cleaning the machined composite anode substrate, and then performing high-temperature exhaust treatment to obtain a composite anode substrate finished product; the temperature of high-temperature exhaust treatment is 1650 ℃, the heat preservation time is 90min, and the exhaust vacuum degree is less than or equal to 3 multiplied by 10 -4 Pa。
Testing the unbalance amount of the composite anode substrate before de-weighting by adopting a Scheck HM10BK dynamic balancing machine, wherein the unbalance amount result is 0.2g cm, and the interface bonding rate of the tungsten alloy target surface blank and the molybdenum alloy substrate blank is more than or equal to 98% through nondestructive ultrasonic testing; the service life of the obtained composite anode substrate finished product is more than or equal to 2 years.
Embodiment 2 a method for preparing a high temperature resistant composite anode substrate, comprising the steps of:
(1) firstly, according to the shape requirements shown in fig. 1, designing and processing to obtain a base assembly of the composite anode substrate (the overall shape is a circular truncated cone, the diameter of the upper surface is recorded as D, the diameter of the lower surface is recorded as D, and the angle between the upper surface and the adjacent side surface, namely the angle of the track layer is recorded as alpha), wherein the base assembly comprises a tungsten alloy target surface blank (the thickness of the tungsten alloy target surface blank is recorded as h1) and a molybdenum alloy substrate blank (the thickness of the molybdenum alloy substrate blank is recorded as h2) which are sequentially stacked from top to bottom; wherein, the tungsten alloy target surface blank adopts W10Re alloy (Re: 10% by mass and the balance W) as raw material, is formed by plate punching and machining, and then is processed to vacuum degree less than or equal to 5 multiplied by 10 -4 Is prepared by vacuum heat treatment at 1550 ℃ for 120min under the condition of Pa, and the thickness h1 is 3 mm; the molybdenum alloy matrix blank is made of MHC molybdenum alloy as a raw material and subjected to upsetting, machining and forming or machining and forming, and then the vacuum degree is less than or equal to 5 multiplied by 10 -4 Is prepared by vacuum heat treatment at 1550 ℃ for 120min under the condition of Pa, and the thickness h2 is 10 mm; the diameter D of the upper surface of the base component is 106mm, the diameter D of the lower surface of the base component is 143mm, the angle alpha of the track layer is 8 degrees, and the surface roughness Ra of the contact surface of the tungsten alloy target surface blank and the molybdenum alloy matrix blank is less than or equal to 0.8.
(2) Mixing tungsten alloy target surface blank with molybdenum alloy baseThe outer ring edge joint of the body blank is formed by laser welding to obtain a formed component, and the requirement of ensuring that the leakage rate of a welding seam is less than or equal to 1 multiplied by 10 -10 Pa·m 3 /s。
(3) Heating the molding assembly in a hydrogen protection heating furnace at 1650 ℃ for 20 min; then taking out and putting into a hydraulic press with a real-time heating mould to carry out real-time heating and pressing treatment; wherein, the preheating temperature of the die is 1250 ℃, the pressing pressure is 400MPa, and the heat preservation and pressure maintaining time is 20min when the die is arranged in the forming assembly.
(4) Machining the pressed composite anode substrate according to the shape requirement to obtain a machined composite anode substrate with the lower surface diameter D of 140 mm;
(5) cleaning the machined composite anode substrate, and then performing high-temperature exhaust treatment to obtain a composite anode substrate finished product; the temperature of high-temperature exhaust treatment is 1600 ℃, the heat preservation time is 120min, and the exhaust vacuum degree is less than or equal to 5 multiplied by 10 -4 Pa。
Testing the unbalance amount of the composite anode substrate before weight removal by adopting a Scheck HM10BK dynamic balancing machine, wherein the unbalance amount result is 0.35g cm, and the interface bonding rate of the tungsten alloy target surface blank and the molybdenum alloy substrate blank is more than or equal to 98% through nondestructive ultrasonic testing; the service life of the obtained composite anode substrate finished product is more than or equal to 2 years.
Embodiment 3 a method for preparing a high temperature resistant composite anode substrate, comprising the steps of:
(1) firstly, according to the shape requirements shown in fig. 1, designing and processing to obtain a base assembly of the composite anode substrate (the overall shape is a circular truncated cone, the diameter of the upper surface is recorded as D, the diameter of the lower surface is recorded as D, and the angle between the upper surface and the adjacent side surface, namely the angle of the track layer is recorded as alpha), wherein the base assembly comprises a tungsten alloy target surface blank (the thickness of the tungsten alloy target surface blank is recorded as h1) and a molybdenum alloy substrate blank (the thickness of the molybdenum alloy substrate blank is recorded as h2) which are sequentially stacked from top to bottom; wherein, the tungsten alloy target surface blank adopts W10Re alloy (Re: 10% by mass and the balance W) as raw material, is formed by plate punching and machining, and then is processed to vacuum degree less than or equal to 5 multiplied by 10 -4 Is prepared by vacuum heat treatment at 1600 deg.C for 90min under Pa, and has high thicknessDegree h1 is 3 mm; the molybdenum alloy matrix blank adopts MoLa molybdenum alloy (La according to mass fraction) 2 O 3 0.5 percent, the balance being Mo) as raw materials, and carrying out upsetting, machining and forming or machining and forming on the raw materials, wherein the vacuum degree is less than or equal to 5 multiplied by 10 -4 Is prepared by vacuum heat treatment at 1600 ℃ for 90min under the condition of Pa, and the thickness h2 is 12 mm; the diameter D of the upper surface of the base component is 143mm, the diameter D of the lower surface of the base component is 193mm, the angle alpha of the track layer is 7 degrees, and the surface roughness Ra of the contact surface of the tungsten alloy target surface blank and the molybdenum alloy matrix blank is less than or equal to 0.8.
(2) The outer ring edge joint of the tungsten alloy target surface blank and the molybdenum alloy matrix blank is formed by electron beam welding to obtain a formed component, and the requirement of ensuring that the leakage rate of a welding seam is less than or equal to 1 multiplied by 10 -10 Pa·m 3 /s。
(3) Heating the formed assembly in a hydrogen protection heating furnace at 1700 ℃ for 30 min; then taking out and putting into a hydraulic press with a real-time heating mould to carry out real-time heating and pressing treatment; wherein, the preheating temperature of the die is 1300 ℃, the pressing pressure is 400MPa, and the heat preservation and pressure maintaining time is 20min when the die is arranged in a forming assembly.
(4) Machining the pressed composite anode substrate according to the shape requirement to obtain a machined composite anode substrate with the lower surface diameter D of 190 mm;
(5) cleaning the machined composite anode substrate, and then performing high-temperature exhaust treatment to obtain a composite anode substrate finished product; the high-temperature exhaust treatment temperature is 1700 ℃, the heat preservation time is 60min, and the exhaust vacuum degree is less than or equal to 5 multiplied by 10 -4 Pa。
Testing the unbalance amount of the composite anode substrate before weight removal by adopting a Scheck HM10BK dynamic balancing machine, wherein the unbalance amount result is 0.65g cm, and the interface bonding rate of the tungsten alloy target surface blank and the molybdenum alloy substrate blank is more than or equal to 98% through nondestructive ultrasonic detection; the service life of the obtained composite anode substrate finished product is more than or equal to 2 years.
Embodiment 4 a method for preparing a high temperature resistant composite anode substrate, comprising the steps of:
(1) firstly, according to the shape requirement shown in figure 1, designing and processing to obtainA base assembly of the composite anode substrate (the overall shape is a circular truncated cone, the diameter of the upper surface is recorded as D, the diameter of the lower surface is recorded as D, and the angle between the upper surface and the adjacent side surface, namely the angle of the track layer is recorded as alpha), wherein the base assembly comprises a tungsten alloy target surface blank (the thickness of the tungsten alloy target surface blank is recorded as h1) and a molybdenum alloy substrate blank (the thickness of the molybdenum alloy substrate blank is recorded as h2) which are stacked in sequence from top to bottom; wherein, the tungsten alloy target surface blank adopts W10Re-0.37HfC alloy (according to the mass fraction, Re is 10 percent, HfC is 0.37 percent, and the balance is W) as raw material, is formed by plate punching and machining, and then is processed and formed at the vacuum degree of less than or equal to 5 multiplied by 10 -4 Is prepared by vacuum heat treatment at 1600 ℃ for 90min under the condition of Pa, and the thickness h1 is 3 mm; the molybdenum alloy matrix blank adopts MoLa molybdenum alloy (La according to mass fraction) 2 O 3 0.8 percent, the balance being Mo) as raw materials, and carrying out upsetting, machining and forming or machining and forming on the raw materials, wherein the vacuum degree is less than or equal to 5 multiplied by 10 -4 Is prepared by heat treatment under the condition of Pa and the temperature of 1600 ℃ for 90min in vacuum, and the thickness h2 is 12 mm; the diameter D of the upper surface of the base component is 143mm, the diameter D of the lower surface of the base component is 193mm, the angle alpha of the track layer is 7 degrees, and the surface roughness Ra of the contact surface of the tungsten alloy target surface blank and the molybdenum alloy matrix blank is less than or equal to 0.8.
(2) The outer ring edge joint of the tungsten alloy target surface blank and the molybdenum alloy matrix blank is formed by electron beam welding to obtain a formed component, and the requirement of ensuring that the leakage rate of a welding seam is less than or equal to 1 multiplied by 10 -10 Pa·m 3 /s。
(3) Heating the molding assembly in a hydrogen protection heating furnace at 1650 ℃ for 30 min; then taking out and putting into a hydraulic press with a real-time heating mould to carry out real-time heating and pressing treatment; wherein, the preheating temperature of the die is 1300 ℃, the pressing pressure is 400MPa, and the heat preservation and pressure maintaining time is 20min when the die is arranged in a forming assembly.
(4) Machining the pressed composite anode substrate according to the shape requirement to obtain a machined composite anode substrate with the lower surface diameter D of 190 mm;
(5) cleaning the machined composite anode substrate, and then performing high-temperature exhaust treatment to obtain a composite anode substrate finished product; the temperature of high-temperature exhaust treatment is 1700 ℃, and heat preservation is carried outThe time is 60min, the exhaust vacuum degree is less than or equal to 5 multiplied by 10 -4 Pa。
Testing the unbalance amount of the composite anode substrate before weight removal by adopting a Scheck HM10BK dynamic balancing machine, wherein the unbalance amount result is 0.55g cm, and the interface bonding rate of the tungsten alloy target surface blank and the molybdenum alloy substrate blank is more than or equal to 98% through nondestructive ultrasonic detection; the service life of the obtained composite anode substrate finished product is more than or equal to 2 years.
Comparative example 1
Comparative example 1 is the same as example 2 except that step (3) is different from example 2, specifically: (3) heating the molding assembly in a hydrogen protection heating furnace at 1650 ℃ for 30 min; then taking out and putting into a hydraulic press with a real-time heating mould to carry out real-time heating and pressing treatment; wherein, the preheating temperature of the die is 1100 ℃, the pressing pressure is 400MPa, and the heat preservation and pressure maintaining time is 20min when the die is arranged in the forming assembly. The molded components were cracked after discharge and failed to achieve effective connection.
Comparative example 2
Comparative example 2 the same as example 2 except that the step (3) is different from example 2, specifically: (3) heating the molding assembly in a hydrogen protection heating furnace at 1650 ℃ for 30 min; then taking out and putting into a hydraulic press with a real-time heating mould to carry out real-time heating and pressing treatment; wherein, the preheating temperature of the die is 1400 ℃, the pressing pressure is 400MPa, and the heat preservation and pressure maintaining time is 20min when the die is arranged in the forming assembly. After the die is taken out of the furnace, the deformation of the inner cavity of the die due to overhigh heating temperature is found, and the continuous normal use is influenced.
Comparative example 3
Comparative example 3 the same as example 2 except that the step (1) is different from example 2, specifically: (1) firstly, according to the shape requirements shown in fig. 1, designing and processing to obtain a base assembly of the composite anode substrate (the overall shape is a circular truncated cone, the diameter of the upper surface is recorded as D, the diameter of the lower surface is recorded as D, and the angle between the upper surface and the adjacent side surface, namely the angle of the track layer is recorded as alpha), wherein the base assembly comprises a tungsten alloy target surface blank (the thickness of the tungsten alloy target surface blank is recorded as h1) and a molybdenum alloy substrate blank (the thickness of the molybdenum alloy substrate blank is recorded as h2) which are sequentially stacked from top to bottom; wherein, the tungsten alloy target surface blank is prepared by taking W10Re alloy (Re is 10 percent and the balance is W) as raw material through plate punching and machining, and the thickness h1 is 3 mm; the molybdenum alloy matrix blank is formed by upsetting, machining or machining MHC (major histocompatibility complex) molybdenum alloy serving as a raw material, and has the thickness h2 of 10 mm; the diameter D of the upper surface of the base component is 106mm, the diameter D of the lower surface of the base component is 143mm, the angle alpha of the track layer is 8 degrees, and the surface roughness Ra of the contact surface of the tungsten alloy target surface blank and the molybdenum alloy matrix blank is less than or equal to 0.8.
The unbalance of the composite anode substrate before weight removal is tested by adopting a Scheck HM10BK dynamic balancing machine, the unbalance result is 0.5 g-cm, and the interface bonding rate of the tungsten alloy target surface blank and the molybdenum alloy substrate blank is about 85% through nondestructive ultrasonic testing. Because the vacuum heat treatment is not carried out, the cleaning of pollutants on the surface of the welding interface is not clean and the surface adsorption gas is too much, thereby further influencing the interface bonding rate.
The above description is only exemplary of the invention and should not be taken as limiting the invention, as any modification, equivalent replacement, or improvement made within the spirit and principle of the invention is intended to be covered by the appended claims.
Claims (10)
1. The preparation method of the high-temperature-resistant composite anode matrix is characterized by comprising the following steps of:
firstly, designing and processing a base component of the composite anode substrate according to the shape requirement of the composite anode substrate, wherein the base component comprises a tungsten alloy target surface blank and a molybdenum alloy substrate blank which are sequentially stacked from top to bottom;
welding the outer ring edge connecting part of the tungsten alloy target surface blank and the molybdenum alloy matrix blank to obtain a forming assembly;
step three, firstly heating the molding assembly, then loading the molding assembly subjected to heating treatment into a mold for real-time heating and pressing treatment to obtain a pressed composite anode matrix;
machining the pressed composite anode substrate according to the shape requirement to obtain a machined composite anode substrate;
and step five, cleaning the machined composite anode substrate, and then performing high-temperature exhaust treatment to obtain a composite anode substrate finished product.
2. The preparation method according to claim 1, wherein in the step one, the tungsten alloy target surface blank is prepared by plastic processing and/or machining and vacuum heat treatment by taking tungsten alloy as a raw material; preferably, in the tungsten alloy, the mass fraction of rhenium is 0-10%, and the balance is tungsten; preferably, in the tungsten alloy, the mass fraction of rhenium is 0-10%, the mass fraction of carbide is less than or equal to 1%, 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- -4 Pa。
3. The preparation method according to claim 1 or 2, wherein in the first step, the molybdenum alloy base blank is prepared by plastic processing and/or machining and vacuum heat treatment by taking a molybdenum alloy as a raw material; preferably, the molybdenum alloy is one of Mo-Ti-Zr alloy, Mo-Hf-C alloy and Mo-La alloy; preferably, in the Mo-Ti-Zr alloy, in mass fraction, Ti: 0.40-0.55%, Zr: 0.06-0.12%, C: 0.01-0.04% and the balance of Mo; preferably, in the Mo-Hf-C alloy, the mass fraction of Hf: 0.8-1.2%, C: 0.05-0.12 percent of Mo, and the balance of Mo; preferably, La is present in the Mo-La alloy in a mass fraction 2 O 3 : 0.3-0.8%, and the balance of Mo; preferably, the temperature of the vacuum heat treatment is 1500- -4 Pa。
4. The production method according to any one of claims 1 to 3, 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 less than or equal to 0.8.
5. The production method according to any one of claims 1 to 4, wherein in step two, in the welding process to obtain a molded component, a welding process is performed using an electron beam or a laser; more preferably, the weld leak rate is less than or equal to 1 multiplied by 10 -10 Pa·m 3 /s。
6. The preparation method according to any one of claims 1 to 5, wherein in step three, the heating treatment is carried out in a hydrogen heating protection device, and hydrogen is introduced during the heating treatment; preferably, the temperature of the heating treatment is 1500-.
7. The production method according to any one of claims 1 to 6, wherein in step three, the real-time heating and pressing treatment is performed in a hydraulic press equipped with a real-time heating mold; preferably, the preheating temperature of the mold when the molding assembly is installed is 1200-1300 ℃, the pressing pressure is 200-400MPa, and the heat preservation and pressure maintaining time is 5-20 min.
8. The method as claimed in any one of claims 1 to 7, wherein in step five, the temperature of the high-temperature exhaust treatment is 1500- -4 Pa。
9. A high temperature resistant composite anode substrate, wherein the composite anode substrate is prepared by the preparation method of any one of claims 1 to 8.
10. The high temperature resistant composite anode matrix according to claim 9, wherein the unbalance amount of the composite anode matrix before de-weighting is less than or equal to 1 g-cm.
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