CN114481052B - Aluminum alloy target and preparation method thereof - Google Patents
Aluminum alloy target and preparation method thereof Download PDFInfo
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- CN114481052B CN114481052B CN202210029390.XA CN202210029390A CN114481052B CN 114481052 B CN114481052 B CN 114481052B CN 202210029390 A CN202210029390 A CN 202210029390A CN 114481052 B CN114481052 B CN 114481052B
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- 229910000838 Al alloy Inorganic materials 0.000 title claims abstract description 55
- 238000002360 preparation method Methods 0.000 title claims abstract description 35
- 238000000034 method Methods 0.000 claims abstract description 43
- 238000005096 rolling process Methods 0.000 claims abstract description 38
- 238000005242 forging Methods 0.000 claims abstract description 35
- 239000013077 target material Substances 0.000 claims abstract description 33
- 238000009694 cold isostatic pressing Methods 0.000 claims abstract description 20
- 238000003466 welding Methods 0.000 claims abstract description 20
- WPPDFTBPZNZZRP-UHFFFAOYSA-N aluminum copper Chemical compound [Al].[Cu] WPPDFTBPZNZZRP-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000010438 heat treatment Methods 0.000 claims abstract description 18
- 238000007493 shaping process Methods 0.000 claims abstract description 11
- 238000012545 processing Methods 0.000 claims abstract description 10
- 238000010894 electron beam technology Methods 0.000 claims abstract description 9
- 238000005240 physical vapour deposition Methods 0.000 claims abstract description 5
- 238000004321 preservation Methods 0.000 claims description 10
- 238000003754 machining Methods 0.000 claims description 5
- 238000001291 vacuum drying Methods 0.000 claims description 3
- 125000004122 cyclic group Chemical group 0.000 claims description 2
- 238000005516 engineering process Methods 0.000 abstract description 6
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 239000012535 impurity Substances 0.000 abstract description 3
- 238000003825 pressing Methods 0.000 abstract description 3
- 230000008595 infiltration Effects 0.000 abstract description 2
- 238000001764 infiltration Methods 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 10
- 229910052782 aluminium Inorganic materials 0.000 description 9
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 9
- 239000013078 crystal Substances 0.000 description 9
- 238000009826 distribution Methods 0.000 description 7
- 229910001094 6061 aluminium alloy Inorganic materials 0.000 description 5
- 229910000881 Cu alloy Inorganic materials 0.000 description 5
- 239000002994 raw material Substances 0.000 description 5
- 238000005336 cracking Methods 0.000 description 4
- 238000001513 hot isostatic pressing Methods 0.000 description 4
- 238000003384 imaging method Methods 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 238000005498 polishing Methods 0.000 description 4
- 238000000137 annealing Methods 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 238000013461 design Methods 0.000 description 3
- 238000007689 inspection Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 238000001953 recrystallisation Methods 0.000 description 3
- 230000035882 stress Effects 0.000 description 3
- 229910000831 Steel Inorganic materials 0.000 description 2
- 229910052738 indium Inorganic materials 0.000 description 2
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 2
- 238000004806 packaging method and process Methods 0.000 description 2
- 238000010079 rubber tapping Methods 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 238000004544 sputter deposition Methods 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- 229910001369 Brass Inorganic materials 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000010951 brass Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000000110 cooling liquid Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 210000001787 dendrite Anatomy 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000004992 fission Effects 0.000 description 1
- 239000011888 foil Substances 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000005022 packaging material Substances 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 238000012805 post-processing Methods 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000005477 sputtering target Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000007514 turning Methods 0.000 description 1
- 238000009461 vacuum packaging Methods 0.000 description 1
- 238000009489 vacuum treatment Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23P—METAL-WORKING NOT OTHERWISE PROVIDED FOR; COMBINED OPERATIONS; UNIVERSAL MACHINE TOOLS
- B23P15/00—Making specific metal objects by operations not covered by a single other subclass or a group in this subclass
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/04—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of aluminium or alloys based thereon
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
- C23C14/3414—Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Pressure Welding/Diffusion-Bonding (AREA)
Abstract
The invention provides an aluminum alloy target and a preparation method thereof, and belongs to the field of target preparation. The invention provides a method for obtaining a target blank by rotary forging, rolling shaping and heat treatment of an aluminum copper cast ingot. And (3) processing the V-shaped tooth grooves on the target blank and the aluminum alloy backboard, and performing cold isostatic pressing treatment and V-shaped tooth combined edge concave electron beam welding after clamping to obtain the aluminum alloy target. The invention uses the mode of combining cold isostatic pressing treatment and electron beam welding to ensure that the combination rate is higher than 98 percent. The V-shaped tooth meshing technology increases the area of a joint surface, greatly improves the joint rate, reduces the labor cost, reduces the traditional binding energy consumption and improves the comfort of personnel. The cold isostatic pressing treatment secondary circulation pressing process greatly ensures the bonding strength of the target material, reduces the infiltration of impurities to a certain extent and ensures the integrity of the target material. The aluminum alloy target material is suitable for application in physical vapor deposition.
Description
Technical Field
The invention belongs to the technical field of target preparation, and particularly relates to an aluminum alloy target and a preparation method thereof.
Background
Physical Vapor Deposition (PVD) technology is currently one of the most critical processes for semiconductor chips, and is the most widely used as a main raw material, sputtering metal targets, including high-purity aluminum and aluminum alloy targets. The grain size, the structure composition and the grain orientation of the target material can greatly influence the sputtering film forming process of the semiconductor, so that the preparation of the target material with the average grain size smaller than 150um by a novel process method is particularly important. The existing target preparation process and method have the defects that the size of the crystal grains is difficult to control through a simple rolling and indium binding process, internal stress is formed by rolling deformation, the internal stress is arched due to heating, deformation quantity is insufficient, and the crystal grains cannot be refined due to incomplete breakage of the crystal grains. Meanwhile, the indium binding process can cause the temperature of the joint surface of the target blank and the backboard to be increased, the grains are coarse and unevenly distributed, and the requirement of fine and even distribution of the grains cannot be met. It is particularly important how to find the equilibrium point between the process and the target grains.
CN104625389a discloses a welding method of an aluminum alloy sputtering target material for integrated circuit packaging materials, which comprises the following steps: and processing convex teeth with a certain shape and size on the welding surface of the target, processing corresponding grooves on the back plate, assembling and combining the target and the back plate, placing the target and the back plate into a sheath for vacuum sealing and welding, and then adopting a hot isostatic pressing method to completely fill the grooves with the material to connect the target and the back plate. Because the welding temperature is low, the growth of aluminum alloy grains can be avoided, the welding strength between the target and the backboard is high, the integral deformation of the target is small, and the post-processing is facilitated. The method needs to process convex teeth on the welding surface of the target material, and also needs to process grooves with corresponding sizes on the back plate, so that the method is complex in processing technology and not suitable for large-scale production. CN112475802a discloses a method for assembling an aluminum target and an aluminum alloy back plate, the method comprising the following steps: (1) Carrying out solution treatment and aging treatment on the aluminum alloy backboard to obtain a hardness-enhanced aluminum alloy backboard; (2) Turning threads on the welding surface of the aluminum alloy backboard with enhanced hardness obtained in the step (1), and carrying out acid washing treatment on the aluminum target material and the aluminum alloy backboard to obtain the pretreated aluminum target material and the aluminum alloy backboard; (3) And assembling the pretreated aluminum target and the aluminum alloy backboard, placing the assembled aluminum target and the aluminum alloy backboard in a sheath, and performing hot isostatic pressing welding after vacuumizing. The assembly method effectively improves the hardness of the aluminum alloy backboard while not affecting the grain size of the aluminum target material, and can also ensure that the backboard and the aluminum target material have higher welding bonding strength. However, the hot isostatic pressing process is expensive, the target material containing capacity is small, the method is not suitable for mass production, and the back plate and the target material are easy to deform due to the fact that the temperature is increased, so that the use is affected.
Therefore, developing an aluminum alloy target preparation method with controllable crystal grains, firm combination of the target and the backboard, and no influence on the crystal grains of the target due to the combination of the target and the backboard becomes a technical problem to be overcome.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide an aluminum alloy target and a preparation method thereof. The invention mainly controls the grain size and grain orientation through forging, rolling and heat treatment, designs the combination mode (V tooth meshing) of the 6061 aluminum alloy backboard and the aluminum copper target blank, and controls the combination strength and the phenomenon that dendrite growth does not occur on the grain at the combination surface by adopting a CIP mode.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows: the invention provides a preparation method of an aluminum alloy target, which comprises the following steps:
(1) Rotary forging aluminum copper cast ingots;
(2) Rolling and shaping the aluminum alloy obtained in the step (1);
(3) Performing heat treatment on the aluminum alloy obtained in the step (2) to obtain a target blank;
(4) Processing the target blank obtained in the step (3) and the aluminum alloy backboard into a V-shaped tooth slot;
(5) The target blank obtained after the V-shaped tooth slot in the step (4) is clamped with an aluminum alloy backboard, and then the target is obtained through cold isostatic pressing treatment;
(6) And (3) carrying out vacuum drying on the target material obtained in the step (5), and then carrying out V-shaped tooth combined edge concave electron beam welding to obtain the aluminum alloy target material.
In a preferred embodiment of the present invention, in the step (1), the rotary forging is performed in two steps, and the pass deformation is 10 to 15% and the total forging deformation is 60 to 70%.
The inventor finds that the forging equipment is used for forging aluminum copper cast ingots by 200t force to ensure the pass deformation amount to be 10-15%, and researches show that the metal and alloy are subjected to forging process treatment, the relative deformation amount of each pass is 10-15%, and the total forging deformation amount is 60-70%, so that grains can be well crushed. The grains can be crushed to the nanometer level, so that the uniformity of the grains is ensured, and the crystal texture is ensured.
In a preferred embodiment of the present invention, in the step (2), the total deformation amount of the roll forming is 20 to 40%.
In the step (2), the flatness of the aluminum alloy after the rolling shaping is less than 0.5mm.
In the step (2), the thickness of the rolled steel sheet is reduced by 0.5 to 1mm per pass in the rolling and shaping.
In a more preferred embodiment of the present invention, in the step (2), the thickness of the rolled steel sheet is reduced by 0.2 to 0.5mm per pass.
The inventor finds that rolling shaping is carried out at a temperature lower than the recrystallization temperature of aluminum-copper alloy, a 25KW double-roller mill is adopted, the rolling speed is 30-40m/min, the forged blank is horizontally placed on a rolling mill tray, continuous rolling is carried out, each pass is reduced by 0.2-0.5 mm, the thickness is reduced to 10-15mm, a vernier caliper is used for measuring the size and the thickness after each pass, the total rolling deformation is ensured to be 20-40%, and finally the flatness and roundness shaping are finished by carrying out 60-degree rotary rolling for multiple times for two times, so that the flatness is ensured to be below 0.5. The above-mentioned steps can cause the crystal grains to undergo fission to form a large number of sub-crystals, and as the deformation amount increases, the crystal grains are elongated in the rolling direction to form a certain orientation zone, and the cold rolled S texture, the Copper texture and the Brass texture are gradually increased to become main textures.
In the step (3), the annealing temperature is 250-300 ℃ and the holding time is 2-3 h.
The inventor finds that the annealing time is 2-3 hours at 250-300 ℃. The average grain size is 60-190 um, and the grain size and distribution are uniform. The internal stress concentration of the aluminum copper target caused by large plastic deformation such as forging, rolling and the like is eliminated through heat treatment, so that the internal defects are reduced, the plastic toughness is properly reduced, and the hardness is improved; and meanwhile, the annealing recrystallization treatment can effectively control the grain size, so that the grain dispersion is uniform, and the grain size requirement of the high-purity aluminum copper target is met.
In the step (4), the distance between adjacent V-shaped teeth processed by the target blank and the aluminum alloy backboard is 2.8mm, the tooth height is 1.1mm, the included angle between teeth is 120-150 degrees, and the depth of the V-shaped tooth groove is 0.9mm.
In the step (4), the distance between adjacent V-shaped teeth processed by the target blank and the V-shaped teeth of the aluminum alloy backboard is 2.8mm, the tooth height is 1.1mm, the included angle between teeth is 150 degrees, and the depth of the V-shaped teeth is 0.9mm.
The inventor finds that in the traditional tooth meshing method, teeth are distributed and dispersed, every two adjacent teeth are combined by a section of plane, and the included angle between the teeth is 120 degrees, so that the machining difficulty is reduced, the tooth meshing fault tolerance is improved, and the bonding strength between a target blank and a back plate is weakened. The key point of the invention is that the center of the target blank is taken as a base point, and 150V-shaped teeth are designed at the rest positions, so that the fault tolerance is improved, the contact area of the target blank and the backboard is increased, and the bonding strength is further improved.
In the step (4), the target blank and the aluminum alloy backboard are in plane contact without processing the V-shaped teeth in a circular range with the diameter of 25mm from the center to the edge and in an annular range with the diameter of 10mm from the edge to the center.
The inventor finds that after the heat treatment is finished, the target blank is cooled at room temperature, then the CNC numerical control lathe programming is used for processing the V-shaped tooth grooves of the target blank and the V-shaped teeth of the back plate 6061 aluminum alloy, and the V-shaped teeth of the back plate are processed, so that the back plate design V-shaped teeth can better pierce the aluminum copper target blank due to the fact that the hardness of the 6061 aluminum alloy is higher than that of the aluminum copper alloy, and the combination is tighter. Through V type tooth design, increase the area of contact between target base and the backplate, the tooth meshing mode can improve bonding strength. Meanwhile, the center part (D25 mm) of the target blank is still contacted with the edge concave (D10 mm) in a plane, the V-shaped teeth can be well positioned, the combination is accurate, the teeth are not staggered, and the preparation is made for the next step of cold isostatic pressing treatment.
As a preferred embodiment of the present invention, in the step (5), the conditions of the cold isostatic pressing are: and (3) carrying out cyclic pressure maintaining under 360-400 MPa.
In the step (5), the pressure is maintained for 2min at 360MPa, 380MPa and 400MPa respectively, and the cycle is carried out twice.
The inventors have found that the interdental bonding gap is reduced by Cold Isostatic Pressing (CIP), and the target blank is tightly bonded to the backing plate without voids. Meanwhile, CIP treatment is carried out at room temperature, unlike the traditional Hot Isostatic Pressing (HIP) and friction stir welding process treatment, the contact surface temperature can be greatly increased, grains are rapidly recrystallized, the grains grow so that equiaxed grains appear, and the CIP process adopts low-temperature high-pressure treatment and cannot influence the grain size of a bonding surface.
The aluminum alloy target prepared by the preparation method of any aluminum alloy target is applied to physical vapor deposition.
Compared with the prior art, the invention has the following beneficial effects:
(1) According to the invention, through calculating the forging rolling deformation of the raw materials, the raw material cost is effectively saved, and the loss is reduced. The traditional target blank and the back plate are single in combination mode, the combination strength and the combination rate cannot be well ensured, and the technology can ensure that the combination rate is higher than 98% by combining CIP and electron beam welding.
(2) According to the invention, by designing a novel V-shaped tooth meshing technology, the area of a joint surface is increased, the joint rate is greatly improved, the labor cost is reduced, the traditional binding energy consumption is reduced, and the comfort of personnel is improved.
(3) The method carries out CIP (in-situ plasma) high-pressure vacuum treatment along with 400MPa of the furnace, maintains pressure for a fixed time in different pressure steps, ensures the stability of pressure, simultaneously carries out secondary cycle pressing of the process, greatly ensures the bonding strength of the target, reduces the infiltration of impurities to a certain extent, and ensures the integrity of the target.
Drawings
FIG. 1 is a schematic diagram of the process flow of the present invention.
Detailed Description
For a better description of the objects, technical solutions and advantages of the present invention, the present invention will be further described with reference to the following specific examples. The experimental methods described in the examples are all conventional methods unless otherwise specified; the reagents and materials are commercially available unless otherwise specified.
Example 1
As an embodiment of the preparation method of the aluminum alloy target material, the specific implementation steps comprise:
(1) Forging, namely taking a raw material 5N high-purity aluminum copper cast ingot D200 x 123mm. After the raw materials are detected to be qualified, sawing is carried out by using a sawing machine to form two D200 x 60mm aluminum copper cast ingots, the thickness loss of sawing is about 3mm, and during the sawing process, cooling liquid is used for continuously pouring, so that the cutter is prevented from being damaged by friction overheat. Forging the male die by using a 200t forging machine, wherein the first step of forging: the maximum force is changed from 60mm thickness to 24mm thickness by multidirectional rotary forging at room temperature, the rotation angle is 135 degrees, and the pass deformation is required to be more than 15 percent. And step two, forging: the method adopts a mode of forging while rotating, the rotation angle is 10-30 degrees as much as possible, the forging is carried out until the thickness is 18-20mm, and the rolling repair shaping is carried out with the allowance. The forging is divided into two steps, the size and thickness of the cast ingot are measured by using a high-precision vernier caliper once every forging, the thickness is required to be 18-20mm after the forging is finished, the minimum diameter is more than 365mm, and the total deformation is 70%. No obvious burrs and pits are formed on the surface.
(2) Rolling, namely rolling and shaping at a temperature lower than the recrystallization temperature of the aluminum-copper alloy, adopting a 25KW double-roller mill, wherein the rolling speed is 33m/min, horizontally placing a D365 x 18 forging blank on a rolling mill tray, continuously rolling, reducing the thickness of each pass by 0.5mm, rolling to a thickness of 14-16mm, measuring the size and the thickness by using a vernier caliper after each pass of rolling, ensuring the total rolling deformation to be 20%, and finally carrying out 60-degree rotary rolling for multiple times for finishing flatness and roundness shaping in two passes, thereby ensuring the flatness to be below 0.5. After rolling, the surface is smooth, and no cracking occurs.
(3) And (3) heat treatment, namely, carrying out heat treatment at the temperature of 250 ℃ on the rolled and formed target blank, preserving heat for 2 hours, and obtaining clear microscopic grain morphology after electrolytic polishing treatment and HF corrosive liquid, wherein the result shows that the average grain size is 60um after heat treatment at the temperature of 250 ℃ and heat preservation is carried out for 2 hours, and the grain size and distribution are uniform.
(4) The V-shaped teeth are machined, the target blank is cooled at room temperature after heat treatment, CNC numerical control lathe programming is used for machining V-shaped tooth grooves of the target blank, and the V-shaped teeth of the back plate 6061 aluminum alloy are machined, so that the strength of the V-shaped teeth is higher than that of the aluminum copper alloy due to the fact that the hardness of the 6061 aluminum alloy is higher than that of the aluminum copper alloy, and the back plate can be used for well penetrating the aluminum copper target blank due to the fact that the V-shaped teeth are designed in the back plate, and the combination is tighter. The adjacent V-shaped teeth are 2.8mm apart, the tooth height is 1.1mm, the included angle between the teeth is 150 degrees, the tooth groove depth of the V-shaped teeth is 0.9mm, meanwhile, the center part (D25 mm) of the target blank and the edge concave part (D10 mm) are still contacted in a plane, the V-shaped teeth can be well positioned, and the combination is accurate, and no staggered teeth exist.
(5) After CIP high-pressure maintaining treatment and machining, after aluminum copper target blank and 6061 backboard are manually clamped, the flatness is required to be smaller than 0.05mm, the inter-tooth bonding gap is 0.2mm, in order to prevent vacuum pumping, a sealing bag is clamped at the gap, and aluminum foil with the diameter of 345mm, the thickness of 0.1mm and the width of 5mm is used for protecting the target gap. And then carrying out vacuumizing and packaging treatment by using a double-layer vacuum packaging bag, and standing for 1h to ensure that packaging is free from air leakage. And then the target material is horizontally placed on a metal storage rack, bound by a binding belt, placed in a cold isostatic pressing device furnace, and pressurized with 400MPa at room temperature along with the furnace, and respectively pressurized for 2min at 360MPa, 380MPa and 400MPa to ensure pressure stability. After the circulation is carried out twice, the pressure is automatically reduced and the furnace is discharged.
(6) And E, electron beam welding, namely performing vacuum drying treatment on the target material at 40 ℃ after the CIP treatment of the last step, performing V-shaped tooth bonding edge concave surface (D10 mm) electron beam welding treatment, vacuumizing a welding furnace to below 1.0 x 10 < -6 > MPa, performing electron beam automatic welding under high pressure 69.45KV and beam current 19.80mA after the electron beam gun is precisely positioned, and ensuring the tight bonding between the target blank and the backboard, wherein the welding depth is 15 mm.
Example 2
As an example of the method for producing an aluminum alloy target of the present invention, except forging, forging was performed by a 100t forging machine, the first step of forging: the maximum force is changed from 60mm thickness to 30mm thickness by multi-directional rotary forging at room temperature, and the pass deformation is required to be 10%. And step two, forging: forging to a thickness of 24-26mm, wherein the minimum diameter is more than 350mm, and the total deformation is 60%; the total rolling deformation was 40% and the same as in example 1, except that the other production methods were the same. The average grain size after the heat treatment in this embodiment is 90um due to different forging and rolling processes, and the grain size and distribution are uniform.
Example 3
As an example of the preparation method of the aluminum alloy target material, the heat removal treatment condition is 250 ℃, the heat preservation time is 3h, and other preparation processes and conditions are the same except that the heat preservation time is different from that of the example 1. And (3) obtaining clear microscopic grain morphology after electrolytic polishing treatment and HF corrosive liquid. The result shows that the heat treatment temperature is 250 ℃, the average grain size is 150um after the heat treatment is carried out for 3 hours, and the grain size and the distribution are uniform.
Example 4
As an example of the preparation method of the aluminum alloy target material, the heat removal treatment condition is 300 ℃, the heat preservation time is 2h, and other preparation processes and conditions are the same except that the heat preservation time is different from that of the example 1. And (3) obtaining clear microscopic grain morphology after electrolytic polishing treatment and HF corrosive liquid. The result shows that the heat treatment temperature is 300 ℃, and after the heat preservation is carried out for 2 hours, the average grain size is 190um, and the grain size and the distribution are uniform.
Example 5
As an example of the preparation method of the aluminum alloy target material, the heat removal treatment condition is 300 ℃, the heat preservation time is 3h, and other preparation processes and conditions are the same except that the heat preservation time is different from that of the example 1. And (3) obtaining clear microscopic grain morphology after electrolytic polishing treatment and HF corrosive liquid. The result shows that the heat treatment temperature is 300 ℃, and after the heat preservation is carried out for 3 hours, the average grain size is 200um, and the grain size and the distribution are uniform.
Example 6
As an example of the preparation method of the aluminum alloy target material, the preparation process and conditions are the same except that the rolling condition is 1.0mm drop per pass, which is different from example 1. After rolling, cracking occurs on the surface.
Example 7
As an example of the method for preparing an aluminum alloy target material of the present invention, the preparation process and conditions were the same except that the rolling condition was decreased by 0.2mm per pass, which was different from example 1. After rolling, the surface is smooth and flat, the material loss is low, and no cracking occurs.
Example 8
As an example of the preparation method of the aluminum alloy target material, other preparation methods are the same except that the included angle between teeth in the tooth processing process is 120 degrees different from that in example 2. The binding rate was 95% by inspection using an ultrasonic C-scan imaging flaw detector.
Comparative example 1
As a comparative example of the preparation method of the aluminum alloy target material, the conditions except CIP process are as follows: pressure is maintained for 12min at 400MPa respectively, pressure stability is guaranteed, automatic depressurization and tapping are carried out, and other preparation methods are the same as those of the embodiment 1.
Comparative example 2
As a comparative example of the preparation method of the aluminum alloy target material, the conditions except CIP process are as follows: pressure is maintained for 12min at 400MPa respectively, pressure stability is guaranteed, automatic depressurization and tapping are carried out, and other preparation methods are the same as those of the embodiment 1. The binding rate was detected to be 91% by using an ultrasonic C-scan imaging flaw detector.
Comparative example 3
As a comparative example of the preparation method of the aluminum alloy target material of the invention, other preparation methods were the same except that the conditions for manually clamping the aluminum copper target blank and the 6061 back plate and then not CIP process were different from those of example 1. The binding rate was 90% by inspection using an ultrasonic C-scan imaging flaw detector.
Comparative example 4
As a comparative example of the preparation method of the aluminum alloy target material of the present invention, the preparation method was the same except that V-shaped tooth processing was not performed unlike example 1. The binding rate was 86% by inspection using an ultrasonic C-scan imaging flaw detector.
From a comparison of examples 1-2, it was found that both the pass deformation of the forging process and the total deformation of the rolling process affect the average grain size of the material. Comparison of example 1 with examples 3-5 shows that the average grain size of the target increases progressively with increasing temperature and heat treatment time. Comparison of example 1 with examples 6-7 shows that an excessive thickness drop per pass in the rolling conditions results in cracking of the surface after rolling. Comparison of example 1 and example 8 shows that the adjacent V-shaped teeth have a tooth space of 2.8mm, a tooth height of 1.1mm, and V-shaped teeth with an included angle between the teeth of 0.9mm deep in the tooth space, and the included angle between the teeth of 150 degrees is better than the bonding degree between the 120-degree target and the back plate.
Comparison of example 1 and comparative examples 1-3 shows that the pressure maintaining for a fixed time is performed by adopting different pressure steps, so that the stability of the pressure can be ensured, and meanwhile, the process is performed for the secondary cycle pressing, so that the bonding strength of the target material is greatly ensured, the penetration of impurities is reduced to a certain extent, the integrity of the target material is ensured, and the bonding degree can be remarkably improved. The result of comparative example 4 shows that the V-shaped tooth meshing technology increases the area of the joint surface, greatly improves the joint rate, simultaneously reduces the labor cost, reduces the traditional binding energy consumption and improves the comfort of personnel.
Finally, it should be noted that the above embodiments are only for illustrating the technical solution of the present invention and not for limiting the scope of the present invention, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that the technical solution of the present invention may be modified or substituted equally without departing from the spirit and scope of the technical solution of the present invention.
Claims (8)
1. The preparation method of the aluminum alloy target is characterized by comprising the following steps of:
(1) Rotary forging aluminum copper cast ingots;
(2) Rolling and shaping the aluminum alloy obtained in the step (1);
(3) Performing heat treatment on the aluminum alloy obtained in the step (2) to obtain a target blank;
(4) Processing the target blank obtained in the step (3) and the aluminum alloy backboard into a V-shaped tooth slot;
(5) The target blank obtained after the V-shaped tooth slot in the step (4) is clamped with an aluminum alloy backboard, and then the target is obtained through cold isostatic pressing treatment;
(6) Vacuum drying the target material obtained in the step (5), and then carrying out V-shaped tooth combined edge concave electron beam welding to obtain an aluminum alloy target material;
in the step (3), the temperature of the heat treatment is 250-300 ℃ and the heat preservation time is 2-3 hours;
in the step (5), the conditions of the cold isostatic pressing treatment are as follows: and (5) carrying out cyclic pressure maintaining under 360-400 MPa.
2. The method according to claim 1, wherein in the step (1), the rotary forging is performed in two steps, the pass deformation is 10-15%, and the total forging deformation is 60-70%.
3. The method according to claim 1, wherein in the step (2), the total deformation amount of the roll forming is 20 to 40%.
4. The method of claim 1, wherein in step (2), the roll-formed aluminum alloy has a flatness of less than 0.5mm.
5. The method according to claim 1, wherein in the step (2), the reduction thickness per pass in the rolling and shaping is 0.5 to 1mm.
6. The method according to claim 1, wherein in the step (4), the distance between adjacent V-shaped teeth of the target blank and the aluminum alloy backboard for V-shaped tooth machining is 2.8mm, the tooth height is 1.1mm, the included angle between teeth is 120-150 degrees, and the depth of the V-shaped tooth groove is 0.9mm.
7. The method of claim 1, wherein in step (4), the target blank and the aluminum alloy backing plate are in planar contact without machining V-shaped teeth within a circular range of 25mm in diameter from the center to the edge and a circular range of 10mm in diameter from the edge to the center.
8. The use of an aluminum alloy target material prepared by the method according to any one of claims 1-7 in physical vapor deposition.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104625389A (en) * | 2014-12-22 | 2015-05-20 | 有研亿金新材料有限公司 | Welding method of aluminum alloy sputtering target material for integrated circuit package material |
| CN213417000U (en) * | 2020-09-04 | 2021-06-11 | 深圳市鑫意晟科技有限公司 | Target assembly with composite structure |
| CN113695732A (en) * | 2021-09-10 | 2021-11-26 | 宁波江丰电子材料股份有限公司 | Welding method of aluminum target material assembly |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104625389A (en) * | 2014-12-22 | 2015-05-20 | 有研亿金新材料有限公司 | Welding method of aluminum alloy sputtering target material for integrated circuit package material |
| CN213417000U (en) * | 2020-09-04 | 2021-06-11 | 深圳市鑫意晟科技有限公司 | Target assembly with composite structure |
| CN113695732A (en) * | 2021-09-10 | 2021-11-26 | 宁波江丰电子材料股份有限公司 | Welding method of aluminum target material assembly |
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