Method for integrally preparing aluminum-scandium alloy target by molding and welding
Technical Field
The invention belongs to the technical field of magnetron sputtering target manufacturing, and particularly relates to a method for integrally preparing an aluminum-scandium alloy target by molding and welding.
Background
The high-purity AlSc alloy target is mainly used for sputtering a high-purity AlScN film, has stronger and better piezoelectric performance compared with the existing piezoelectric films such as AlN, ZnO, lead zirconate titanate (PZT) and the like, and is a core material for manufacturing high-frequency mobile communication (5G) radio frequency filter chips, MEMS micro advanced sensors and the like. Because the melting point difference between Al and Sc is large, the solid solubility of Sc in Al is low, the scandium vapor pressure is high, and as the scandium content in the AlSc alloy is increased, hard and brittle intermediate compounds are gradually formedPhase (Al) 3 Sc、Al 2 Sc、AlSc、AlSc 2 ) The difficulty in preparing a large-size high-quality target blank without cracks is high; and as the solid-liquid solidification interval is increased, the flowability of the AlSc alloy is reduced, and the formed cast ingot has more defects of looseness, holes and the like. At present, a typical preparation technology of an aluminum-scandium alloy target with low scandium content mainly adopts a vacuum induction melting mode to prepare an ingot with a smaller diameter, and then adopts rolling modes such as upsetting, rolling and the like to eliminate casting defects and extend the size of the ingot to obtain a large-size AlSc alloy target blank. And after machining the large-size AlSc alloy target blank, diffusion welding the large-size AlSc alloy target blank with a back plate to form an AlSc alloy target diffusion welding assembly. The method has long process, and the target blank is easy to crack in the rolling process, and the yield is low.
Disclosure of Invention
Aiming at the problems in the prior art, the invention discloses a method for integrally preparing an aluminum-scandium alloy target by molding and welding. The method comprises the steps of putting an AlSc alloy cast ingot with the Sc content of less than or equal to 20 at% and a back plate into an Al alloy jacket for calendering to form a large-size AlSc alloy target blank and a back plate welding assembly, then carrying out heat treatment at the temperature of 300-600 ℃, forming a recrystallization annealing state structure and promoting the diffusion between the AlSc alloy target blank and the back plate, and finally obtaining the AlSc alloy target diffusion welding assembly with the average grain size of less than 100 mu m, the welding strength of more than 70MPa, the welding rate of more than 99% and no cracks. According to the method, the AlSc alloy ingot with large size and few defects can be obtained by rolling the AlSc alloy ingot and the back plate together, the diffusion welding of the AlSc alloy target and the back plate can be realized, and the process flow is shortened. Meanwhile, stress generated in the rolling process can be released in an Al sheath deformation mode through an Al sheath rolling mode, and a large-size AlSc alloy target material without cracking is obtained.
The invention relates to a method for integrally preparing an aluminum-scandium alloy target by molding and welding, which comprises the following steps:
step (1), preparing 1 piece of AlSc alloy ingot with the diameter of 100-150 mm and the Sc content of less than or equal to 20 at% and a backboard respectively;
step (2), performing ultrasonic cleaning on the prepared AlSc alloy ingot and the prepared back plate to remove surface oil stains;
step (3), pickling the AlSc alloy cast ingot and the back plate after oil stain removal to remove surface oxide skin, and exposing a fresh surface;
step (4), placing the AlSc alloy cast ingot and the backboard into an Al alloy sheath for sealing and welding;
step (5), heating and softening the Al alloy sheath obtained in the step (4), wherein the heating temperature is 200-500 ℃, and the heat preservation time is 0.5-1 h;
step (6), carrying out rolling treatment on the Al alloy sheath obtained in the step (5) to form a large-size AlSc alloy target blank and a backboard welding assembly, wherein the rolling treatment method comprises the method of carrying out single or combined upsetting, forging, rolling and the like;
step (7), carrying out heat treatment on the large-size AlSc alloy target blank obtained in the step (6) and the back plate welding assembly, wherein the heat treatment temperature is 300-600 ℃, and the heat treatment time is 2-8 h, so that a recrystallization annealing state structure is formed, and the diffusion between the AlSc alloy target blank and the back plate is promoted;
and (8) after the heat treatment in the step (7) is finished, machining to remove the Al alloy sheath, and finally obtaining the AlSc alloy target diffusion welding assembly with the average grain size of less than 100 microns, the welding strength of more than 70MPa, the welding rate of more than 99% and no cracks.
Compared with the prior art, the technical scheme has the following advantages:
(1) the process flow is short: according to the method, the AlSc alloy ingot with large size and few defects can be obtained by calendering the AlSc alloy ingot and the back plate together, and the diffusion welding of the AlSc alloy target and the back plate can be realized at the same time, so that the process flow is shortened;
(2) no cracking: according to the method, stress generated in the rolling process can be released in an Al sheath deformation mode through an Al sheath rolling mode, and the large-size AlSc alloy target material without cracking is obtained.
(3) The welding rate is high: the AlSc alloy target blank obtained by the method has no crack, and the problem that the welding rate is influenced after the crack is expanded does not exist in the welding process and the later heat treatment process.
The invention is further illustrated by the following figures and detailed description of the drawings, which are not meant to limit the scope of the invention.
Drawings
FIG. 1 is a schematic structural view of an AlSc alloy ingot and a back plate before being rolled integrally.
FIG. 2 is a schematic structural view of an AlSc alloy ingot and a back plate after being rolled integrally.
FIG. 3 is a flow chart of the procedures of examples and comparative examples.
Detailed Description
For better explanation of the present invention and for better understanding, the present invention will be described in detail below with reference to specific embodiments and comparative examples.
Examples 1 to 9
1. Preparing materials: preparing 1 piece of AlSc alloy ingot with the diameter of 150mm and the Sc content of 8-20 at% and 1 piece of Al alloy back plate respectively;
2. ultrasonic cleaning: carrying out ultrasonic cleaning on the prepared AlSc alloy cast ingot and the Al alloy back plate to remove surface oil stains;
3. acid washing: pickling the AlSc alloy cast ingot and the Al alloy back plate after oil stain removal to remove surface oxide skin, and exposing a fresh surface;
4. sealing and welding: placing the pickled AlSc alloy cast ingot and the Al alloy back plate into an Al alloy sheath for sealing and welding;
5. heating and softening: heating and softening the obtained Al alloy sheath at 500 ℃ for 1 h;
6. rolling: carrying out calendering treatment on the obtained Al alloy sheath to form a large-size AlSc alloy target blank and a back plate welding assembly;
7. and (3) heat treatment: carrying out heat treatment on the obtained large-size AlSc alloy target blank and the back plate welding assembly, wherein the heat treatment temperature is 300-600 ℃, and the heat treatment time is 2-8 h, so that a recrystallization annealing state structure is formed, and the diffusion between the AlSc alloy target blank and the back plate is promoted;
8. machining: and after the heat treatment is finished, removing the Al alloy sheath by machining, and finally obtaining the AlSc alloy target diffusion welding assembly with the average grain size of less than 100 mu m, the welding strength of more than 70MPa, the welding rate of more than 99 percent and no cracks.
Comparative example
1. Preparing an AlSc alloy ingot: preparing 1 piece of AlSc alloy cast ingot with the diameter of 150mm and the Sc content of 8-20 at%;
2. heating and softening: heating and softening the AlSc alloy cast ingot, wherein the heating temperature is 500 ℃, and the heat preservation time is 1 h;
3. rolling: carrying out calendering treatment on the heated AlSc alloy cast ingot to form a large-size AlSc alloy target blank;
4. and (3) heat treatment: carrying out heat treatment on the rolled AlSc alloy cast ingot, wherein the heat treatment temperature is 600 ℃, and the heat treatment time is 8 hours, so that a recrystallization annealing state structure is formed, and the internal stress generated in the rolling process is eliminated;
5. machining: machining the rolled AlSc alloy ingot to obtain an AlSc alloy target blank with a regular shape;
6. preparing a back plate: preparing 1 large-size Al alloy backboard;
7. ultrasonic cleaning: carrying out ultrasonic cleaning on the large-size AlSc alloy target blank and the Al alloy back plate to remove surface oil stains;
8. acid washing: pickling the AlSc alloy target blank and the Al alloy back plate after oil stain removal to remove surface oxide skin, and exposing a fresh surface;
9. degassing and sealing welding: placing the acid-washed AlSc alloy target blank and the Al alloy back plate into an Al alloy sheath for degassing and sealing welding;
10. diffusion welding: placing the Al alloy sheath subjected to degassing sealing welding into a hot isostatic pressing furnace for diffusion welding, wherein the welding temperature is 600 ℃, the welding pressure is 100MPa, and the welding time is 8 hours;
11. machining: and removing the Al alloy sheath by machining, and finally obtaining the AlSc alloy target diffusion welding assembly with internal defect rate of 0.7%, average grain size of 96 mu m, welding strength of 105MPa, welding rate of 95.3% and cracks.
The main preparation process and performance of the AlSc alloy target materials in examples 1-9 and comparative example 1 are shown in table 1.
TABLE 1 examples and comparative examples AlSc alloy target material forming welding process main preparation process and required number of processes, welding rate and cracking condition
As can be seen from the results shown in table 1, the present technical solution has the following advantages:
(1) the process flow is short: according to the method, the AlSc alloy ingot with large size and few defects can be obtained by rolling the AlSc alloy ingot and the back plate together, the diffusion welding of the AlSc alloy target and the back plate can be realized at the same time, the process flow is shortened, and as shown in FIG. 3, the number of required processes of examples 1-4 is 8, and the number of required processes of the examples is 11;
(2) no cracking: according to the method, stress generated in the rolling process can be released in an Al sheath deformation mode through an Al sheath rolling mode, and a large-size AlSc alloy target material without cracking is obtained as in examples 1-4; the AlSc alloy target of the comparative example was believed to crack;
(3) the welding rate is high: the AlSc alloy target blank obtained by the method has no crack, and the problem that the welding rate is influenced after the crack is expanded does not exist in the welding process and the later heat treatment process, such as examples 1-9, wherein the welding rate is 99.8-99.9%; and the welding rate of the comparative example is 95.3 percent.