阅读说明：本技术 一种铝钪合金靶材的扩散焊接方法 (Diffusion welding method for aluminum-scandium alloy target ) 是由 谢小林 蔡新志 童培云 朱刘 郑双明 于 2021-06-28 设计创作，主要内容包括：本发明揭示了一种铝钪合金靶材的扩散焊接方法,包括以下步骤：准备铝钪合金靶材与背板；对铝钪合金靶材和背板的焊接面进行光洁处理；对铝钪合金靶材和背板进行清洗；将铝钪合金靶材与无氧铜或铝合金放置于金属包套中,进行脱气处理；对金属包套进行抽真空、密封处理；对金属包套进行热等静压处理,即可完成铝钪合金靶材的扩散焊接,所述热等静压的过程中,金属包套升温升压至400～580℃、60～80mpa,保温保压1～2h,随炉冷却至室温。本发明和现有铝材料和其他金属材料的扩散焊接方法的优点有三点：第一：本发明提高了材料的利用率；第二：本发明简便了生产加工过程,提高了生产效率；第三：本发明有利于靶材的回收,特别是价格昂贵的钪元素。(The invention discloses a diffusion welding method of an aluminum-scandium alloy target, which comprises the following steps: preparing an aluminum-scandium alloy target and a back plate; carrying out polishing treatment on the welding surface of the aluminum-scandium alloy target and the back plate; cleaning the aluminum-scandium alloy target and the back plate; placing the aluminum-scandium alloy target material and oxygen-free copper or aluminum alloy in a metal sheath, and performing degassing treatment; vacuumizing and sealing the metal sheath; and performing hot isostatic pressing treatment on the metal sheath to finish the diffusion welding of the aluminum-scandium alloy target, wherein in the hot isostatic pressing process, the temperature and the pressure of the metal sheath are raised to 400-580 ℃ and 60-80 mpa, the temperature and the pressure are kept for 1-2 h, and the metal sheath is cooled to room temperature along with the furnace. The invention has three advantages compared with the prior diffusion welding method of aluminum materials and other metal materials: firstly, the method comprises the following steps: the invention improves the utilization rate of the material; secondly, the method comprises the following steps: the invention simplifies the production and processing process and improves the production efficiency; thirdly, the method comprises the following steps: the invention is beneficial to the recovery of the target material, in particular to the scandium element with high price.)

1. A diffusion welding method of an aluminum-scandium alloy target is characterized by comprising the following steps:

s1: preparing an aluminum-scandium alloy target and a back plate;

s2: carrying out polishing treatment on the welding surface of the aluminum-scandium alloy target and the back plate;

s3: cleaning the aluminum-scandium alloy target and the back plate;

s4: placing the aluminum-scandium alloy target material and the back plate in a metal sheath, and performing degassing treatment;

s5: vacuumizing and sealing the metal sheath;

s6: and performing hot isostatic pressing treatment on the metal sheath to finish the diffusion welding of the aluminum-scandium alloy target, wherein in the hot isostatic pressing process, the temperature and the pressure of the metal sheath are raised to 400-580 ℃ and 60-80 mpa, the temperature and the pressure are kept for 1-2 h, and the metal sheath is cooled to room temperature along with the furnace.

2. The method of claim 1, wherein in the step S1, the content of scandium in the aluminum-scandium alloy target is 8 to 20 at%, and the balance is aluminum.

3. The method according to claim 1, wherein in the step S6, the temperature and the pressure of the metal sheath are raised to 480 ℃ and 68mpa, the temperature and the pressure are maintained for 1-2 h, and the metal sheath is cooled to room temperature along with the furnace.

4. The method of claim 1, wherein the step S2 comprises turning the weld face with a lathe to a roughness of 0.3 μm or less and a flatness of 0.1mm or less.

5. The method of claim 1, wherein the cleaning step S3 is performed by using a dust-free wiping cloth stained with absolute ethanol.

6. The method according to claim 1, wherein in the degassing process of step S4, the metal sheath is heated to 150-200 ℃, kept for 2-4 hours, and cooled to room temperature along with the furnace, thereby completing the degassing treatment.

7. The method according to claim 1, wherein the relative vacuum degree of the metal sheath after vacuum pumping is less than or equal to 10^-2Pa。

8. The method of claim 1 wherein a layer of graphite paper is disposed outside of said metal wrap.

9. The method of claim 1, wherein the material of the backing plate is oxygen-free copper or aluminum alloy.

Technical Field

The invention relates to the technical field of target processing, in particular to a diffusion welding method of an aluminum-scandium alloy target.

Background

The aluminum scandium alloy target material is used as a novel wiring material of an integrated circuit, not only can improve the hardness of the material, but also can improve the stress displacement of the material, and effectively avoids the electron migration related to the outflow and the disconnection of aluminum atoms.

CN 110527956A discloses a method for preparing an aluminum-scandium alloy sputtering target material containing 5 at% -50 at% of scandium and the balance of aluminum, the method uses a vacuum magnetic suspension smelting furnace to completely alloy raw material aluminum and raw material scandium, then adopts a rapid casting process to cast and prepare the aluminum-scandium alloy target material, and the aluminum-scandium alloy target material is forged or rolled to the required specification, and the method can be used for preparing the aluminum-scandium alloy target material.

CN 110093588A discloses a method for preparing a fine-grain aluminum scandium alloy target, which comprises mixing nano-scale aluminum powder, nano-scale scandium powder and a special mixed solution, performing wet ball milling to obtain aluminum scandium alloy target slurry, performing slip casting on the aluminum scandium alloy target slurry, and sequentially performing degreasing and sintering on an obtained aluminum scandium alloy blank to obtain a fine-grain scandium alloy target.

However, in the magnetron sputtering process, the aluminum scandium alloy target material needs to be welded with the oxygen-free copper (or other materials such as aluminum alloy) back plate, and the bonding area between the target material and the chassis is required to be larger than 98% to ensure that the welded target material meets the requirements of good heat conduction and electric conduction performance and no falling. The welding method mainly comprises brazing and diffusion welding, wherein the brazing generally adopts In, Sn and alloy materials with low melting points for welding, the process is simple, but the melting point of the welding flux is low, the requirement of high-power sputtering coating cannot be met, and the diffusion welding has the advantages of high welding rate, high welding strength and the like, and is particularly suitable for high-power and high-efficiency sputtering coating target materials. Generally, in order to improve the welding strength, a material with higher hardness is selected from a target material and a back plate, threads are machined on the welding surface of the target material and the back plate, and the threads are embedded into the material with the lower hardness during welding, so that the contact area of welding is increased, and the welding strength and the welding bonding rate are improved.

For example, CN 110369897 a discloses a method for welding a target and a backing plate, which provides a method for welding a target and a backing plate according to the present invention, the method includes selecting a material with higher hardness from the target and the backing plate, machining threads on a welding surface of the material, combining the target and the backing plate, placing the combined material in a metal sheath for degassing treatment, then sealing the metal sheath, and welding the target and the backing plate by using a hot isostatic pressing manner to form a target assembly. The method avoids the brazing mode, reduces the cost required by the brazing flux, but needs to process the target and the back plate at the same time, has higher processing cost and higher difficulty, and increases the raw material cost because scandium is expensive.

Aiming at the defects of the prior art, the invention provides a diffusion welding method of an aluminum-scandium alloy target.

Disclosure of Invention

The invention aims to overcome the defects of the prior art and provide a diffusion welding method of an aluminum-scandium alloy target.

In order to achieve the purpose, the invention adopts the following technical scheme.

The invention provides a diffusion welding method of an aluminum-scandium alloy target, which comprises the following steps:

s1: preparing an aluminum-scandium alloy target and a back plate;

s2: carrying out polishing treatment on the welding surface of the aluminum-scandium alloy target and the back plate;

s3: cleaning the aluminum-scandium alloy target and the back plate;

s4: placing the aluminum-scandium alloy target material and the back plate in a metal sheath, and performing degassing treatment;

s5: vacuumizing and sealing the metal sheath;

s6: and performing hot isostatic pressing treatment on the metal sheath to finish the diffusion welding of the aluminum-scandium alloy target, wherein in the hot isostatic pressing process, the temperature and the pressure of the metal sheath are raised to 400-580 ℃ and 60-80 mpa, the temperature and the pressure are kept for 1-2 h, and the metal sheath is cooled to room temperature along with the furnace.

As a further improvement of the present invention, in the step S1, the content of scandium element in the aluminum-scandium alloy target material is 8 to 20 at%, and the balance is aluminum element.

As a further improvement of the invention, in the step S6, the temperature and the pressure of the metal sheath are raised to 480 ℃ and 68mpa, the temperature and the pressure are kept for 1-2 h, and the metal sheath is cooled to room temperature along with the furnace.

As a further improvement of the invention, in the step S2, during the finishing treatment, a lathe is used for turning the welding surface, so that the roughness of the welding surface is less than or equal to 0.3 μm, and the flatness is less than or equal to 0.1 mm.

As a further improvement of the invention, the cleaning in step S3 is performed by using a dust-free wiping cloth stained with absolute ethyl alcohol.

As a further improvement of the invention, in the degassing process of the step S4, the temperature of the metal sheath is raised to 150-200 ℃, the temperature is kept for 2-4 hours, and the metal sheath is cooled to room temperature along with the furnace, so that the degassing treatment is completed.

As a further improvement of the invention, the relative vacuum degree of the metal sheath after vacuum pumping is less than or equal to 10^-2Pa。

As a further improvement of the invention, a layer of graphite paper is arranged outside the metal sheath.

As a further improvement of the invention, the material of the back plate is oxygen-free copper or aluminum alloy.

The invention has three advantages compared with the prior diffusion welding method of aluminum materials and other metal materials: firstly, the method comprises the following steps: the invention improves the utilization rate of the material; secondly, the method comprises the following steps: the invention simplifies the production and processing process and improves the production efficiency; thirdly, the method comprises the following steps: the invention is beneficial to the recovery of the target material, and particularly, the scandium element is expensive.

Detailed Description

The technical solutions will be described clearly and completely in the following with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.

The invention provides a diffusion welding method of an aluminum-scandium alloy target, which comprises the following steps:

s1: preparing an aluminum-scandium alloy target and a back plate;

s2: carrying out polishing treatment on the welding surface of the aluminum-scandium alloy target and the back plate;

s3: cleaning the aluminum-scandium alloy target and the back plate;

s4: placing the aluminum-scandium alloy target material and the back plate in a metal sheath, and performing degassing treatment;

s5: vacuumizing and sealing the metal sheath;

s6: and performing hot isostatic pressing treatment on the metal sheath to finish the diffusion welding of the aluminum-scandium alloy target, wherein in the hot isostatic pressing process, the temperature and the pressure of the metal sheath are raised to 400-580 ℃ and 60-80 mpa, the temperature and the pressure are kept for 1-2 h, and the metal sheath is cooled to room temperature along with the furnace.

In the process of the diffusion welding method for the aluminum-scandium alloy target, the aluminum-scandium alloy target and the oxygen-free copper or aluminum alloy are placed in the metal sheath, the metal sheath is heated and pressurized to 400-580 ℃ and 60-80 mpa, the target for completing diffusion welding in a high-temperature and high-pressure environment is high in welding rate and stable in performance, the prepared target can resist impact of high temperature and high pressure, and the target can continuously keep welding stability without falling off in the subsequent sputtering process; in the research process, the inventor finds that the temperature and the pressure of the metal sheath are increased to 400-580 ℃ and 60-80 mpa, the heat preservation and the pressure maintenance are carried out for 1-2 hours, and the obtained target material has the highest welding rate which is over 99 percent.

Preferably, in the step S1, the content of scandium in the aluminum-scandium alloy target is 8 to 20 at%, and the balance is aluminum.

Preferably, in the step S6, the temperature and pressure of the metal sheath are increased to 480 ℃ and 68mpa, the temperature and pressure are maintained for 1-2 hours, and the metal sheath is cooled to room temperature along with the furnace.

Preferably, in the finishing treatment of step S2, the welding surface is turned by a lathe, so that the roughness of the welding surface is less than or equal to 0.3 μm and the flatness is less than or equal to 0.1 mm.

Preferably, the cleaning in step S3 is performed by using a dust-free wiping cloth stained with anhydrous ethanol.

Preferably, in the degassing process in the step S4, the temperature of the metal sheath is raised to 150-200 ℃, the temperature is maintained for 2-4 hours, and the metal sheath is cooled to room temperature along with the furnace, so that the degassing treatment is completed.

Preferably, the relative vacuum degree of the metal sheath after vacuum pumping is less than or equal to 10^-2Pa。

Preferably, a layer of graphite paper is arranged outside the metal sheath.

Preferably, the material of the back plate is oxygen-free copper or aluminum alloy.

For further understanding of the present invention, the method and effects of the present invention will be described in further detail with reference to specific examples. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.

Example 1.

S1: preparing an aluminum-scandium alloy target material and a back plate, wherein the content of scandium is 8-20 at%, and the balance is aluminum;

s2: carrying out polishing treatment on the welding surface of the aluminum-scandium alloy target and the back plate to ensure that the roughness of the welding surface is less than or equal to 0.3 mu m and the flatness is less than or equal to 0.1 mm;

s3: cleaning the aluminum-scandium alloy target and the back plate;

s4: placing the aluminum-scandium alloy target and the back plate in a metal sheath, and performing degassing treatment, wherein in the degassing process, the temperature of the metal sheath is raised to 150-200 ℃, the temperature is kept for 2-4 h, and the metal sheath is cooled to room temperature along with a furnace, so that the degassing treatment is completed;

s5: vacuumizing the metal sheath until the relative vacuum degree is less than or equal to 10^-2Pa, and then sealing;

s6: and performing hot isostatic pressing treatment on the metal sheath, wherein in the hot isostatic pressing process, the temperature of the metal sheath is raised and increased to 480 ℃ and 68mpa, the temperature and pressure are kept for 1-2 h, the metal sheath is cooled to room temperature along with a furnace, diffusion welding of the aluminum-scandium alloy target material can be completed after the hot isostatic pressing is finished, and the binding welding rate is 99.8% measured by using c-scan.

Example 2.

S1: preparing an aluminum-scandium alloy target material and a back plate, wherein the content of scandium is 8-20 at%, and the balance is aluminum;

s2: carrying out polishing treatment on the welding surface of the aluminum-scandium alloy target and the back plate to ensure that the roughness of the welding surface is less than or equal to 0.3 mu m and the flatness is less than or equal to 0.1 mm;

s3: cleaning the aluminum-scandium alloy target and the back plate;

s4: placing the aluminum-scandium alloy target and the back plate in a metal sheath, and performing degassing treatment, wherein in the degassing process, the metal sheath is heated to 150-200 ℃, is subjected to heat preservation for 2-4 h, and is cooled to room temperature along with a furnace, so that the degassing treatment can be completed;

s5: vacuumizing the metal sheath until the relative vacuum degree is less than or equal to 10^-2Pa, and then sealing;

s6: and performing hot isostatic pressing treatment on the metal sheath, wherein in the hot isostatic pressing process, the temperature of the metal sheath is raised to 405 ℃ and 62mpa, the temperature and pressure are kept for 1-2 h, the metal sheath is cooled to room temperature along with a furnace, diffusion welding of the aluminum-scandium alloy target material can be completed after the hot isostatic pressing is finished, and the binding welding rate is 99.5% measured by using c-scan.

Example 3.

S1: preparing an aluminum-scandium alloy target material and a back plate, wherein the content of scandium is 8-20 at%, and the balance is aluminum;

s2: carrying out polishing treatment on the welding surface of the aluminum-scandium alloy target and the back plate to ensure that the roughness of the welding surface is less than or equal to 0.3 mu m and the flatness is less than or equal to 0.1 mm;

s3: cleaning the aluminum-scandium alloy target and the back plate;

s4: placing the aluminum-scandium alloy target and the back plate in a metal sheath, and performing degassing treatment, wherein in the degassing process, the metal sheath is heated to 150-200 ℃, is subjected to heat preservation for 2-4 h, and is cooled to room temperature along with a furnace, so that the degassing treatment can be completed;

s5: vacuumizing the metal sheath until the relative vacuum degree is less than or equal to 10^-2Pa, and then sealing;

s6: and performing hot isostatic pressing treatment on the metal sheath, wherein in the hot isostatic pressing process, the temperature of the metal sheath is raised to 530 ℃ and the pressure of the metal sheath is raised to 75mpa, the temperature and the pressure are kept for 1-2 h, the metal sheath is cooled to room temperature along with a furnace, diffusion welding of the aluminum-scandium alloy target material can be completed after the hot isostatic pressing is finished, and the binding welding rate is 99.4% measured by using c-scan.

Comparative example 1.

The difference between the comparative example and the example 1 is that the hot isostatic pressing treatment is directly carried out on the aluminum-scandium alloy target and the back plate without adopting a metal sheath to complete the diffusion welding of the aluminum-scandium alloy target, and the bonding rate is measured by c-scan to be 50%.

Comparative example 2.

The difference between the comparative example and the example 1 is that the temperature is increased to 700 ℃ during the hot isostatic pressing treatment, the diffusion welding of the aluminum-scandium alloy target is completed, and the bonding rate is 96.7% measured by c-scan.

Comparative example 3.

The difference between the comparative example and the example 1 is that the temperature is increased to 400 ℃ in the hot isostatic pressing process, the diffusion welding of the aluminum-scandium alloy target is completed, and the bonding rate is 93.5% measured by c-scan.

Comparative example 4.

The difference between the comparative example and the example 1 is that the pressure is increased to 50mpa during the hot isostatic pressing treatment, the diffusion welding of the aluminum-scandium alloy target material is completed, and the bonding rate is 98.2% measured by c-scan.

Comparative example 5.

The difference between the comparative example and the example 1 is that the pressure is increased to 90mpa during the hot isostatic pressing treatment, the diffusion welding of the aluminum-scandium alloy target material is completed, and the bonding rate is 98.7% measured by c-scan.

The invention has three advantages compared with the prior diffusion welding method of aluminum materials and other metal materials: firstly, the method comprises the following steps: the invention improves the utilization rate of the material; secondly, the method comprises the following steps: the invention simplifies the production and processing process and improves the production efficiency; thirdly, the method comprises the following steps: the invention is beneficial to the recovery of the target material, and particularly, the scandium element is expensive.

Although the preferred embodiments of the present invention have been disclosed for illustrative purposes, those skilled in the art will appreciate that various modifications, additions and substitutions are possible, without departing from the scope and spirit of the invention as disclosed in the accompanying claims.