CN114481052A - Aluminum alloy target and preparation method thereof - Google Patents
Aluminum alloy target and preparation method thereof Download PDFInfo
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- CN114481052A CN114481052A CN202210029390.XA CN202210029390A CN114481052A CN 114481052 A CN114481052 A CN 114481052A CN 202210029390 A CN202210029390 A CN 202210029390A CN 114481052 A CN114481052 A CN 114481052A
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- 229910000838 Al alloy Inorganic materials 0.000 title claims abstract description 54
- 238000002360 preparation method Methods 0.000 title claims abstract description 38
- 238000005096 rolling process Methods 0.000 claims abstract description 43
- 238000000034 method Methods 0.000 claims abstract description 42
- 238000005242 forging Methods 0.000 claims abstract description 31
- 238000010438 heat treatment Methods 0.000 claims abstract description 21
- 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 14
- 238000012545 processing Methods 0.000 claims abstract description 13
- 238000007493 shaping process Methods 0.000 claims abstract description 13
- 238000010894 electron beam technology Methods 0.000 claims abstract description 9
- 238000005240 physical vapour deposition Methods 0.000 claims abstract description 6
- 238000003754 machining Methods 0.000 claims description 5
- 238000001291 vacuum drying Methods 0.000 claims description 3
- 239000013077 target material Substances 0.000 abstract description 40
- 238000005516 engineering process Methods 0.000 abstract description 5
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 239000012535 impurity Substances 0.000 abstract description 3
- 230000008595 infiltration Effects 0.000 abstract description 3
- 238000001764 infiltration Methods 0.000 abstract description 3
- 238000003825 pressing Methods 0.000 abstract description 3
- 239000013078 crystal Substances 0.000 description 17
- 230000000052 comparative effect Effects 0.000 description 10
- 238000009826 distribution Methods 0.000 description 8
- 238000004321 preservation Methods 0.000 description 8
- 229910052782 aluminium Inorganic materials 0.000 description 7
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 7
- 239000002994 raw material Substances 0.000 description 6
- 229910001094 6061 aluminium alloy Inorganic materials 0.000 description 5
- 238000001513 hot isostatic pressing Methods 0.000 description 5
- 229910000881 Cu alloy Inorganic materials 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
- 239000000243 solution Substances 0.000 description 4
- 229910000831 Steel Inorganic materials 0.000 description 3
- JRBRVDCKNXZZGH-UHFFFAOYSA-N alumane;copper Chemical compound [AlH3].[Cu] JRBRVDCKNXZZGH-UHFFFAOYSA-N 0.000 description 3
- 238000000137 annealing Methods 0.000 description 3
- 238000005336 cracking 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
- 238000011160 research Methods 0.000 description 3
- 239000010959 steel Substances 0.000 description 3
- 230000007547 defect Effects 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 238000007599 discharging Methods 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
- 238000007789 sealing Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 238000004544 sputter deposition Methods 0.000 description 2
- 230000035882 stress Effects 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
- 239000005030 aluminium foil 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
- 238000005097 cold rolling Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000001816 cooling 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
- 238000002474 experimental method Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000013021 overheating Methods 0.000 description 1
- 239000005022 packaging material Substances 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000006104 solid solution Substances 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
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000007514 turning Methods 0.000 description 1
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- 238000009489 vacuum treatment Methods 0.000 description 1
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Images
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
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 target blank obtained by rotary forging, rolling, shaping and heat treatment of an aluminum-copper cast ingot. And (3) carrying out V-shaped tooth groove processing on the target blank and the aluminum alloy back plate, clamping, carrying out cold isostatic pressing treatment and V-shaped tooth combination edge concave surface electron beam welding to obtain the aluminum alloy target. The invention ensures that the bonding rate is higher than 98% by combining cold isostatic pressing treatment and electron beam welding. The V-shaped tooth meshing technology increases the area of a combined surface, greatly improves the combining rate, simultaneously reduces the labor cost, reduces the traditional binding energy consumption, and improves the comfort of personnel. The cold isostatic pressing treatment secondary cycle 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
At present, the Physical Vapor Deposition (PVD) technology is one of the most critical processes of semiconductor chips, and is used as a main raw material, namely a sputtering metal target, and the PVD technology is most widely applied to high-purity aluminum and aluminum alloy targets. The grain size, structure composition and grain orientation of the target greatly affect the sputtering film-forming process of semiconductors, so that the preparation of the target with the average grain size of less than 150um by a new process method is particularly important. In the existing target material preparation process and method, the grain size is difficult to control through a simple rolling and indium binding process, rolling deformation can form internal stress, the grains are arched by heating, the deformation quantity is insufficient, and the grains cannot be refined due to incomplete grain crushing. Meanwhile, the indium binding process can cause the temperature of the joint surface of the target blank and the back plate to rise, the crystal grains are thick and uneven in distribution, and the requirements of fine and even distribution of the crystal grains cannot be met. It is particularly important how to find a balance point between the process and the target grains.
CN104625389A discloses a welding method of aluminum alloy sputtering target for integrated circuit packaging material, which comprises: processing convex teeth with certain shape and size on the welding surface of the target material, processing a corresponding groove on the back plate, assembling and combining the target material and the back plate, putting the target material and the back plate into a sheath for vacuum sealing welding, then completely filling the groove with materials by adopting a hot isostatic pressing method, and connecting the target material and the back plate. Due to the low welding temperature, the growth of aluminum alloy crystal grains can be avoided, the welding strength between the target and the back plate is high, the overall deformation of the target is small, and the later-stage processing is facilitated. According to the method, convex teeth are required to be machined on the welding surface of the target material, grooves with corresponding sizes are required to be machined on the back plate, and the machining process is complex and is not suitable for large-scale production. CN112475802A discloses an assembling method of an aluminum target and an aluminum alloy backing plate, which comprises the following steps: (1) carrying out solid solution treatment and aging treatment on the aluminum alloy back plate to obtain a hardness-enhanced aluminum alloy back plate; (2) performing thread turning on the welding surface of the hardness-enhanced aluminum alloy backboard obtained in the step (1), and performing acid washing treatment on the aluminum target material and the aluminum alloy backboard to obtain a pretreated aluminum target material and an pretreated aluminum alloy backboard; (3) and assembling the pretreated aluminum target and the aluminum alloy back plate, placing the assembly in a sheath, vacuumizing, and performing hot isostatic pressing welding. The assembling method effectively improves the hardness of the aluminum alloy back plate while not influencing the grain size of the aluminum target material, and can also ensure that the back plate and the aluminum target material have higher welding bonding strength. However, the hot isostatic pressing process is expensive, the target packing capacity is small, the hot isostatic pressing process is not suitable for mass production, and the welding deformation between the backing plate and the target is easily caused by the increase of the temperature, which affects the use.
Therefore, it is a technical problem to be overcome to develop a method for preparing an aluminum alloy target material with controllable grains, firm bonding between the target material and the back plate, and no influence on the grains of the target material when the target material is bonded with the back plate.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides an aluminum alloy target and a preparation method thereof. The invention mainly controls the grain size and the grain orientation through forging, rolling and heat treatment, controls the bonding strength by designing the bonding mode (V-tooth meshing) of the 6061 aluminum alloy back plate and the aluminum copper target blank and adopts the CIP mode to control the grain of the bonding surface not to generate the dendritic crystal growth phenomenon.
In order to achieve the purpose, the invention adopts the technical scheme that: the invention provides a preparation method of an aluminum alloy target, which comprises the following steps:
(1) rotationally forging the aluminum-copper cast ingot;
(2) rolling and shaping the aluminum alloy obtained in the step (1);
(3) carrying out heat treatment on the aluminum alloy obtained in the step (2) to obtain a target blank;
(4) carrying out V-shaped tooth groove processing on the target blank obtained in the step (3) and the aluminum alloy back plate;
(5) clamping the target blank obtained after the V-shaped tooth groove processing in the step (4) with an aluminum alloy back plate, and then carrying out cold isostatic pressing treatment to obtain a target;
(6) and (4) carrying out vacuum drying on the target obtained in the step (5), and then carrying out V-shaped tooth combination edge concave surface electron beam welding to obtain the aluminum alloy target.
In a preferred embodiment of the present invention, in the step (1), the rotary forging is performed in two steps, wherein the pass deformation is 10 to 15%, and the total forging deformation is 60 to 70%.
The inventor finds that the aluminum copper cast ingot is forged by using the forging equipment with the force of 200t, the pass deformation is ensured to be 10-15%, and researches show that the crystal grains can be well crushed when the metal and the alloy are subjected to forging process treatment, the relative deformation of each pass reaches 10-15%, and the total deformation of forging reaches 60-70%. The crystal grains can be crushed to the nanometer level, so that the uniformity of the crystal 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 rolling and shaping is 20 to 40%.
In a preferred embodiment of the present invention, in the step (2), the flatness of the rolled and reshaped aluminum alloy is less than 0.5 mm.
In a preferred embodiment of the present invention, in the step (2), the thickness reduction in each pass of the rolling and shaping is 0.5 to 1 mm.
In a more preferred embodiment of the present invention, in the step (2), the thickness reduction per pass in the rolling and shaping is 0.2 to 0.5 mm.
The inventor finds that rolling shaping is carried out at the temperature lower than the recrystallization temperature of the aluminum-copper alloy, a 25KW double-roller rolling mill is adopted, the rolling speed is 30-40m/min, a forged blank is horizontally placed on a rolling mill tray for continuous rolling, the thickness of the forged blank is reduced by 0.2-0.5 mm in each pass and is rolled to be 10-15mm thick, a vernier caliper is used for measuring the size and the thickness after each pass of rolling, the total deformation amount of rolling is ensured to be 20-40%, and finally, 60-degree rotary rolling is carried out for two times to finish flatness and roundness shaping for multiple times, and the flatness is ensured to be below 0.5. The above process can make the crystal grains split to form a large amount of subgrains, and the crystal grains are elongated in the rolling direction along with the increase of the deformation amount to form a certain orientation band, so that the cold rolling S texture, the Copper texture and the Brass texture are gradually increased to become main textures.
In a preferred embodiment of the invention, in the step (3), the annealing temperature is 250-300 ℃, and the heat preservation time is 2-3 h.
The inventor finds that the annealing time is 2-3 h at 250-300 ℃ through research. The average grain size is 60-190 um, and the grain size and distribution are uniform. 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, internal defects are reduced, the plastic toughness is properly reduced, and the hardness is improved; meanwhile, the annealing recrystallization treatment can effectively control the grain size, so that the grains are dispersed and homogenized, and the grain size requirement of the high-purity aluminum copper target material is met.
In a preferred embodiment of the present invention, in the step (4), the distance between adjacent V-shaped teeth of the target blank and the aluminum alloy backing plate subjected to V-shaped tooth processing is 2.8mm, the tooth height is 1.1mm, the included angle between the teeth is 120 to 150 °, and the depth of the V-shaped tooth groove is 0.9 mm.
In a more preferred embodiment of the present invention, in step (4), the distance between adjacent V-shaped teeth processed by the target blank and the V-shaped teeth of the aluminum alloy backing plate is 2.8mm, the tooth height is 1.1mm, the included angle between the teeth is 150 °, and the depth of the V-shaped tooth groove is 0.9 mm.
The inventor finds that in the traditional tooth meshing method, the teeth are distributed and dispersed, every two adjacent teeth are combined by a section of plane, the included angle between the teeth is 120 degrees, the machining difficulty can be reduced, the tooth meshing fault tolerance rate is improved, and meanwhile, 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 the other positions are all designed with 150-degree V-shaped teeth, thereby not only improving the fault tolerance rate, but also increasing the contact area of the target blank and the back plate, and further improving the bonding strength.
As a more preferred embodiment of the present invention, in the step (4), the target blank and the aluminum alloy backing plate are in a circular range with a diameter from the center of the circle to the edge of 25mm and in an annular range with a diameter from the edge to the center of the circle of 10mm, and are still in plane contact without processing V-shaped teeth.
The inventor finds that after the heat treatment is finished, after the target blank is cooled at room temperature, the CNC numerical control lathe is used for programming to process a V-shaped tooth groove of the target blank and process a V-shaped tooth of a back plate 6061 aluminum alloy, because the hardness and the strength of the 6061 aluminum alloy are higher than those of the aluminum-copper alloy, the designed V-shaped tooth of the back plate can better pierce the aluminum-copper target blank, and the combination is tighter. Through the design of V type tooth, increase area of contact between target blank and the backplate, the tooth meshing mode can improve bonding strength. Meanwhile, the central part (D25mm) of the target blank is still in plane contact with the edge recess (D10mm), so that the V-shaped teeth can be well positioned, the combination is accurate, the staggered teeth do not exist, and the cold isostatic pressing treatment is ready for the next step.
In a preferred embodiment of the present invention, in the step (5), the cold isostatic pressing process is performed under the following conditions: and carrying out circulating pressure maintaining at 360-400 MPa.
In a more preferred embodiment of the present invention, in the step (5), the pressure is maintained at 360MPa, 380MPa and 400MPa for 2min, and the cycle is repeated twice.
The inventor researches and discovers that the Cold Isostatic Pressing (CIP) reduces the bonding gap between the teeth and tightly bonds the target blank and the back plate without pores. Meanwhile, the CIP treatment is carried out at room temperature, which is different from the traditional Hot Isostatic Pressing (HIP) and friction stir welding process treatment, the temperature of a contact surface is greatly increased, crystal grains are rapidly recrystallized, equiaxial crystals appear due to the growth of the crystal grains, and the CIP process adopts low-temperature high-pressure treatment, so that the size of the crystal grains on a joint surface cannot be influenced.
The aluminum alloy target material prepared by the preparation method of any one of the aluminum alloy target materials provided by the invention 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 deformation amount of the forging and rolling of the raw materials, the cost of the raw materials is effectively saved, and the loss is reduced. The traditional target blank and back plate are combined in a single mode, the combination strength and the combination rate cannot be well guaranteed, and the combination rate can be guaranteed to be higher than 98% by the aid of the combination of 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, meanwhile, the labor cost is reduced, the traditional binding energy consumption is reduced, and the personnel comfort is improved.
(3) According to the invention, CIP is carried out along with the furnace 400MPa high-pressure vacuum treatment, different pressure steps are carried out for fixed time pressure maintaining, the stability of the pressure is ensured, and meanwhile, the process secondary cycle pressing is carried out, so that the bonding strength of the target material is greatly ensured, the impurity infiltration is reduced to a certain extent, and the target material integrity is ensured.
Drawings
FIG. 1 is a schematic view of the process of the present invention.
Detailed Description
To better illustrate the objects, technical solutions and advantages of the present invention, the present invention will be further described with reference to specific examples. In the examples, unless otherwise specified, the experimental methods are all conventional methods; unless otherwise indicated, all reagents and materials are commercially available.
Example 1
As an embodiment of the preparation method of the aluminum alloy target material, the specific implementation steps comprise:
(1) forging, and taking a 5N high-purity aluminum copper ingot D200 x 123 mm. After the raw materials are detected to be qualified, a sawing machine is used for sawing the raw materials into two D200 x 60mm aluminum-copper cast ingots, the thickness loss of the raw materials is about 3mm, cooling liquid is continuously sprayed and poured during the sawing process, and the cutter is prevented from being damaged by friction and overheating. The open-air ann yang uses 200t forging machine to forge, and first step is forged: and performing multidirectional rotary forging on the steel plate with the maximum force of 60mm to 24mm at room temperature, wherein the steel plate is rotated by 135 degrees, and the pass deformation is required to be more than 15 percent. And a second step of forging: the method is characterized in that the forging is carried out while rotating, the round shape is realized as far as possible, the rotating angle is 10-30 degrees, the forging is carried out until the thickness is 18-20mm, and the rolling, repairing and shaping are carried out while the allowance is left. The forging is divided into two steps, wherein the size and the thickness of the cast ingot are measured by using a high-precision vernier caliper once per 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%. The surface has no obvious burr and pit.
(2) Rolling, performing rolling shaping at the temperature lower than the recrystallization temperature of the aluminum-copper alloy, adopting a 25KW double-roller mill, rolling at the speed of 33m/min, flatly placing a D365 x 18 forged blank on a rolling mill tray, performing continuous rolling, reducing the thickness of each pass by 0.5mm, rolling to the thickness of 14-16mm, measuring the size and the thickness of each pass by using a vernier caliper after rolling, ensuring that the total deformation amount of the rolling is 20%, and finally performing 60-degree rotary rolling for two passes for multiple times to finish flatness and roundness shaping, and ensuring that the flatness is below 0.5. After rolling, the surface is flat and no crack appears.
(3) And (3) performing heat treatment, namely performing heat treatment on the rolled and formed target blank at the heat treatment temperature of 250 ℃, preserving heat for 2 hours, and obtaining a clear microscopic crystal grain appearance by adopting electrolytic polishing treatment and HF corrosive liquid, wherein the result shows that the average crystal grain size is 60 mu m and the crystal grain size and distribution are uniform after the heat treatment temperature is 250 ℃ and the heat preservation is performed for 2 hours.
(4) V type tooth processing, heat treatment accomplish the back target blank, after the room temperature cooling, use CNC numerical control lathe programming to carry out target base V type tooth groove processing to and backplate 6061 aluminum alloy's V type tooth processing, this is because 6061 aluminum alloy hardness, intensity is higher than the aluminium-copper alloy, and backplate design V type tooth can be better impale aluminium-copper target base, combines inseparabler. The distance between adjacent V-shaped teeth is 2.8mm, the tooth height is 1.1mm, the included angle between the teeth is 150 degrees, the depth of the V-shaped tooth groove is 0.9mm, meanwhile, the center part (D25mm) of the target blank is still in plane contact with the edge recess (D10mm), the V-shaped teeth can be well positioned, combined accurately, and no wrong teeth exist.
(5) CIP high pressure pressurize is handled, and after the machine tooling was accomplished, the aluminium copper target blank carried out artifical block with 6061 backplate after, required the plane degree to be less than 0.05mm, and the intertooth space combines the gap 0.2mm, for preventing to take out the vacuum makes the sealing bag card in gap department, adopts diameter 345mm, thickness 0.1mm, width 5mm opening aluminium foil to carry out target gap department protection. And then, carrying out vacuumizing and packaging treatment by using a double-layer vacuum packaging bag, and standing for 1h to ensure that the packaging is free from air leakage. And then, flatly placing the target material on a metal storage rack, binding the target material by using a binding belt, placing the target material in a cold isostatic pressing equipment furnace, increasing the pressure of 400MPa along with the furnace at room temperature, and respectively maintaining the pressure at the pressure of 360MPa, 380MPa and 400MPa for 2min to ensure the pressure stability. After the circulation is carried out for two times, the pressure is automatically reduced and the furnace is discharged.
(6) And (3) electron beam welding, wherein after the CIP treatment in the previous step, the target is subjected to vacuum drying treatment at 40 ℃, the concave surface (D10mm) of the V-shaped tooth bonding edge is subjected to electron beam welding treatment, a welding furnace is vacuumized to below 1.0X 10-6MPa, an electron beam gun is accurately positioned, and then the electron beam is automatically welded under high pressure of 69.45KV and beam current of 19.80mA, wherein the welding depth is 15mm, so that the target blank and a back plate are tightly bonded.
Example 2
As an example of the preparation method of the aluminum alloy target material, except forging, forging is carried out by a 100t forging machine, and the first step of forging is as follows: and performing multidirectional rotary forging on the steel plate from the thickness of 60mm to the thickness of 30mm at the maximum force at room temperature, wherein the pass deformation is required to be 10%. And a second step of forging: forging to a thickness of 24-26mm, a minimum diameter of more than 350mm and a total deformation of 60%; the rolling was carried out in the same manner as in example 1 except that the total rolling strain was 40%. The average grain size after the heat treatment of the embodiment is 90um, and the grain size and the distribution are uniform due to different forging and rolling processes.
Example 3
As an embodiment of the preparation method of the aluminum alloy target material, the preparation method is different from the embodiment 1 in that the heat treatment condition is 250 ℃ and the heat preservation time is 3h, and other preparation processes and conditions are the same. And obtaining clear microscopic grain morphology by adopting electrolytic polishing treatment and HF corrosive liquid. The result shows that the average grain size is 150um and the grain size and distribution are uniform after the heat treatment temperature is 250 ℃ and the heat preservation is carried out for 3 hours.
Example 4
As an embodiment of the preparation method of the aluminum alloy target material, the preparation method is different from the embodiment 1 in that the heat treatment condition is 300 ℃ and the heat preservation time is 2h, and other preparation processes and conditions are the same. And obtaining clear microscopic grain morphology by adopting electrolytic polishing treatment and HF corrosive liquid. The result shows that the average grain size is 190um and the grain size and distribution are uniform after the heat treatment temperature is 300 ℃ and the heat preservation is carried out for 2 hours.
Example 5
As an embodiment of the preparation method of the aluminum alloy target material, the preparation method is different from the embodiment 1 in that the heat treatment condition is 300 ℃ and the heat preservation time is 3h, and other preparation processes and conditions are the same. And obtaining clear microscopic grain morphology by adopting electrolytic polishing treatment and HF corrosive liquid. The result shows that the average grain size is 200um and the grain size and distribution are uniform after the heat treatment temperature is 300 ℃ and the heat preservation is carried out for 3 hours.
Example 6
As an embodiment of the preparation method of the aluminum alloy target material, the preparation processes and conditions are the same except that the rolling condition is that the reduction of 1.0mm per pass is different from that of the embodiment 1. After rolling, cracking occurred on the surface.
Example 7
As an embodiment of the preparation method of the aluminum alloy target material, the preparation processes and conditions are the same except that the rolling condition is that the reduction of 0.2mm per pass is different from that of the embodiment 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, the preparation method is the same except that the tooth-forming process is different from that of example 2 in that the included angle between teeth is 120 degrees. The binding rate was 95% as measured by 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 CIP removing process conditions are as follows: keeping the pressure at 400MPa for 12min respectively to ensure the pressure to be stable, automatically reducing the pressure and discharging, which is different from the embodiment 1 and is the same as other preparation methods.
Comparative example 2
As a comparative example of the preparation method of the aluminum alloy target material, the CIP removing process conditions are as follows: keeping the pressure at 400MPa for 12min respectively to ensure the pressure to be stable, automatically reducing the pressure and discharging, which is different from the embodiment 1 and is the same as other preparation methods. The binding rate was 91% as measured 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, the preparation method is the same except that after the machining is finished, the aluminum copper target blank is manually clamped with the 6061 back plate, and the CIP process is not carried out, which is different from that in the embodiment 1. The binding rate was 90% as measured by using an ultrasonic C-scan imaging detector.
Comparative example 4
As a comparative example of the preparation method of the aluminum alloy target material of the invention, the preparation method is the same except that the V-shaped teeth are not processed, which is different from that of the example 1. The binding rate was 86% as measured by using an ultrasonic C-scan imaging detector.
From the comparison of examples 1-2, it was found that both the amount of pass deformation during forging and the amount of total deformation during rolling affect the average grain size of the material. Example 1 in comparison with examples 3-5 shows that the average grain size of the target material increases gradually with increasing temperature and heat treatment time. Comparison of example 1 with examples 6-7 shows that excessive thickness reduction per pass in the rolling conditions leads to cracking of the surface after rolling. The comparison between the embodiment 1 and the embodiment 8 shows that the V-shaped teeth with the adjacent V-shaped teeth spacing of 2.8mm, the tooth height of 1.1mm and the V-shaped tooth groove depth of 0.9mm have better bonding degree between the teeth and the target of 150 degrees than the target of 120 degrees and the back plate.
The comparison between the example 1 and the comparative examples 1 to 3 shows that the fixation time pressure maintaining is carried out by adopting different pressure steps, so that the pressure stability can be ensured, the process secondary cycle pressing is carried out, the target material bonding strength is greatly ensured, the impurity infiltration is reduced to a certain extent, the target material integrity is ensured, and the bonding degree can be obviously improved. The result of the comparative example 4 shows that the V-shaped tooth meshing technology increases the area of the joint surface, greatly improves the joint rate, 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 used for illustrating the technical solutions of the present invention and not for limiting the protection scope of the present invention, and although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (10)
1. The preparation method of the aluminum alloy target is characterized by comprising the following steps of:
(1) rotationally forging the aluminum-copper cast ingot;
(2) rolling and shaping the aluminum alloy obtained in the step (1);
(3) carrying out heat treatment on the aluminum alloy obtained in the step (2) to obtain a target blank;
(4) carrying out V-shaped tooth groove processing on the target blank obtained in the step (3) and the aluminum alloy back plate;
(5) clamping the target blank obtained after the V-shaped tooth groove processing in the step (4) with an aluminum alloy back plate, and then carrying out cold isostatic pressing treatment to obtain a target;
(6) and (4) carrying out vacuum drying on the target obtained in the step (5), and then carrying out V-shaped tooth combination edge concave surface electron beam welding to obtain the aluminum alloy target.
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 rolling and shaping is 20-40%.
4. The method of claim 1, wherein in step (2), the flatness of the roll-formed aluminum alloy is less than 0.5 mm.
5. The method according to claim 1, wherein in the step (2), the thickness reduction in each pass in the rolling and shaping is 0.5-1 mm.
6. The method according to claim 1, wherein in the step (3), the temperature of the heat treatment is 250-300 ℃, and the holding time is 2-3 h.
7. The method according to claim 1, wherein in the step (4), the target blank and the aluminum alloy back plate are subjected to V-shaped tooth machining, the distance between adjacent V-shaped teeth is 2.8mm, the tooth height is 1.1mm, the included angle between the teeth is 120-150 degrees, and the depth of the V-shaped tooth groove is 0.9 mm.
8. The method according to claim 1, wherein in the step (4), the target blank and the aluminum alloy backing plate are in plane contact without machining V-shaped teeth in a circular range with a diameter from the center to the edge of 25mm and in an annular range with a diameter from the edge to the center of 10 mm.
9. The method according to claim 1, wherein in the step (5), the cold isostatic pressing conditions are as follows: and carrying out circulating pressure maintaining at 360-400 MPa.
10. Use of an aluminum alloy target prepared by the method according to any one of claims 1 to 9 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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