CN117161534A - Binding method of aluminum-titanium alloy target and aluminum alloy backboard - Google Patents
Binding method of aluminum-titanium alloy target and aluminum alloy backboard Download PDFInfo
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- CN117161534A CN117161534A CN202311138482.2A CN202311138482A CN117161534A CN 117161534 A CN117161534 A CN 117161534A CN 202311138482 A CN202311138482 A CN 202311138482A CN 117161534 A CN117161534 A CN 117161534A
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- UQZIWOQVLUASCR-UHFFFAOYSA-N alumane;titanium Chemical compound [AlH3].[Ti] UQZIWOQVLUASCR-UHFFFAOYSA-N 0.000 title claims abstract description 135
- 229910001069 Ti alloy Inorganic materials 0.000 title claims abstract description 133
- 229910000838 Al alloy Inorganic materials 0.000 title claims abstract description 90
- 238000000034 method Methods 0.000 title claims abstract description 55
- 238000003466 welding Methods 0.000 claims abstract description 116
- 238000003825 pressing Methods 0.000 claims abstract description 49
- 238000010438 heat treatment Methods 0.000 claims abstract description 21
- 238000001513 hot isostatic pressing Methods 0.000 claims abstract description 21
- 239000013077 target material Substances 0.000 claims abstract description 21
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 46
- 229910052782 aluminium Inorganic materials 0.000 claims description 46
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 28
- 238000004140 cleaning Methods 0.000 claims description 22
- 238000005554 pickling Methods 0.000 claims description 19
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 14
- 229910017604 nitric acid Inorganic materials 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- 239000000463 material Substances 0.000 claims description 13
- 239000000243 solution Substances 0.000 claims description 11
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 238000003754 machining Methods 0.000 claims description 7
- 239000011259 mixed solution Substances 0.000 claims description 7
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 6
- 238000004321 preservation Methods 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 2
- 239000002775 capsule Substances 0.000 claims 1
- 239000010410 layer Substances 0.000 description 104
- 230000000052 comparative effect Effects 0.000 description 9
- 238000009792 diffusion process Methods 0.000 description 8
- 239000007788 liquid Substances 0.000 description 4
- 238000005477 sputtering target Methods 0.000 description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 3
- 239000010949 copper Substances 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 3
- 238000004544 sputter deposition Methods 0.000 description 3
- 238000005219 brazing Methods 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 239000011229 interlayer Substances 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 239000010409 thin film Substances 0.000 description 2
- 230000000712 assembly Effects 0.000 description 1
- 238000000429 assembly Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000010408 film Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000005488 sandblasting Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910000679 solder Inorganic materials 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000011343 solid material Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
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Abstract
The invention relates to a binding method of an aluminum-titanium alloy target and an aluminum alloy backboard, which comprises the following steps: preparing an aluminum-titanium alloy target, an intermediate layer and an aluminum alloy backboard, arranging threads on the welding surfaces of the aluminum-titanium alloy target and the aluminum alloy backboard, pressing the threads on the welding surfaces of the aluminum-titanium alloy target into the intermediate layer, and then performing heat treatment on the aluminum-titanium alloy target and the intermediate layer to obtain an aluminum-titanium alloy target-intermediate layer; applying pressure on the surface of the aluminum-titanium alloy target material-middle layer, and then assembling an aluminum alloy backboard and the aluminum-titanium alloy target material-middle layer to obtain a target material assembly; and placing the target assembly into a sheath for hot isostatic pressing welding. The binding method not only can reduce the influence of welding stress, but also can reduce the risk caused by deformation, and simultaneously ensures the welding bonding strength and the welding bonding rate between the aluminum-titanium alloy target material, the aluminum alloy backboard and the middle layer.
Description
Technical Field
The invention belongs to an assembly method of a target assembly, and particularly relates to a binding method of an aluminum-titanium alloy target and an aluminum alloy backboard.
Background
Sputtering is one of the main techniques for preparing thin film materials, when charged particles bombard the surface of solid materials, surface atoms collide and generate energy and momentum transfer, so that the bombarded material atoms escape from the surface and deposit on a substrate, and the bombarded solid is a raw material for preparing deposited thin films by a sputtering method, and is generally called as sputtering target materials.
Because the sputtering targets have different strength, in the practical application process, the sputtering targets meeting the performance requirement and the backboard with certain strength are bound to form the target assembly. The backing plate can provide support for the sputter target while conducting heat, typically by bonding the sputter target to the backing plate by welding. CN112122726a discloses a brazing method of an aluminum target and an aluminum back plate, wherein a first groove is formed in a welding surface of the aluminum back plate, and a second groove is formed in the first groove; the diameter of the first groove is equal to the diameter of the aluminum target; the aluminum target welding surface is provided with a protrusion matched with the second groove of the aluminum backboard welding surface; the brazing method comprises the following steps: (1) Carrying out sand blasting treatment on the welding surface of the aluminum target until the roughness is 2-3 mu m, and carrying out anodic oxidation treatment on the welding surface of the aluminum backboard; (2) And adding solder into the first groove and the second groove of the aluminum backboard, and then performing braze welding to obtain the aluminum target assembly. According to the welding method, by setting a special welding structure and carrying out specific treatment on the welding surface, good welding of the aluminum target material and the aluminum backboard is realized, the welding combination rate is more than or equal to 97%, the stress distribution of the welding surface is uniform, and the service life of the target material assembly is obviously prolonged.
Although the method realizes good welding of the aluminum target and the aluminum backboard, the welding strength of the aluminum target and the aluminum backboard needs to be improved. Because the working environment of the target assembly in the sputtering process is bad, if the welding combination degree between the target and the backboard in the target assembly is low, the target can deform, crack and even fall off from the backboard under the heated condition.
In addition, the thermal expansion coefficients of the titanium-aluminum alloy and the aluminum alloy are nearly doubled, and the two materials are directly subjected to diffusion welding in an environment of more than 400 ℃, so that the product is greatly deformed due to welding stress, the subsequent processing is extremely difficult, and the cracking and the welding are locally carried out when the welding stress is severe. Therefore, developing a binding method of an aluminum-titanium alloy target and an aluminum alloy backboard, which can solve the problem of easy deformation of the target assembly while ensuring the welding combination rate and the welding combination strength, is a technical problem which needs to be solved by the technicians in the field.
Disclosure of Invention
In order to solve the technical problems, the invention provides a binding method of an aluminum-titanium alloy target and an aluminum alloy backboard, which can reduce the influence of welding stress, further reduce risks caused by deformation, and ensure the welding bonding strength and the welding bonding rate between the aluminum-titanium alloy target and the aluminum alloy backboard and the middle layer.
In order to achieve the technical effects, the invention adopts the following technical scheme:
the invention provides a binding method of an aluminum-titanium alloy target and an aluminum alloy backboard, which comprises the following steps:
(1) Preparing an aluminum-titanium alloy target, an intermediate layer and an aluminum alloy backboard, arranging threads on the welding surfaces of the aluminum-titanium alloy target and the aluminum alloy backboard, pressing the threads on the welding surfaces of the aluminum-titanium alloy target into the intermediate layer, and then performing heat treatment on the aluminum-titanium alloy target and the intermediate layer to obtain an aluminum-titanium alloy target-intermediate layer;
(2) Applying pressure on the surface of the aluminum-titanium alloy target material-middle layer in the step (1), and then assembling an aluminum alloy backboard with the aluminum-titanium alloy target material-middle layer to obtain a target material assembly;
(3) And (3) placing the target assembly in the step (2) in a sheath for hot isostatic pressing welding.
According to the binding method provided by the invention, on the basis of arranging the intermediate layer, threads are arranged on the welding surfaces of the aluminum-titanium alloy target and the aluminum alloy backboard through the thread design with increased contact area, and the method that the target is combined with the intermediate layer and then combined with the backboard is adopted, so that the influence of welding stress is reduced, the risk brought by deformation is further reduced, and meanwhile, the welding combination strength and the welding combination rate between the aluminum-titanium alloy target and the aluminum alloy backboard and the intermediate layer are ensured.
In a preferred embodiment of the present invention, the material of the intermediate layer in the step (1) includes aluminum having a purity of > 99%, for example, 99.1%, 99.2%, 99.3%, 99.4%, 99.5% or 99.9%, but is not limited to the above-mentioned values, and other non-mentioned values within the above-mentioned ranges are equally applicable.
The aluminum material with the purity of more than 99% is adopted as the middle layer, so that the aluminum material has low hardness, is easy to deform and is beneficial to stress release, and meanwhile, the aluminum material is easy to combine with titanium aluminum alloy and aluminum alloy.
Preferably, the thickness of the intermediate layer in the step (1) is 3-7mm, for example, 3.5mm, 4mm, 4.5mm, 5mm, 5.5mm, 6mm or 6.5mm, etc., but the intermediate layer is not limited to the recited values, and other non-recited values within the above-mentioned range are equally applicable.
Preferably, the roughness Ra of the interface between the intermediate layer and the aluminum-titanium alloy target in the step (1) is less than 0.8. Mu.m, for example, 0.7. Mu.m, 0.65. Mu.m, 0.6. Mu.m, 0.55. Mu.m, 0.5. Mu.m, or 0.4. Mu.m, etc., but the present invention is not limited to the above-mentioned values, and other values not mentioned in the above-mentioned numerical ranges are equally applicable.
As a preferable mode of the present invention, the pitch of the threads in the adjacent step (1) is 0.3 to 0.5mm, for example, 0.32mm, 0.35mm, 0.37mm, 0.4mm, 0.42mm, 0.45mm or 0.47mm, etc., but the present invention is not limited to the above-mentioned values, and other values not mentioned in the above-mentioned value ranges are equally applicable.
Preferably, the depth of the thread in step (1) is > 0.2mm, for example, 0.22mm, 0.24mm, 0.25mm, 0.26mm, 0.28mm, 0.3mm or 0.32mm, etc., but not limited to the values recited, and other values not recited in the above ranges are equally applicable.
In the invention, the threads on the welding surface of the aluminum-titanium alloy target and the aluminum alloy backboard are distributed in concentric circles.
It is worth to say that the welding surface of aluminum titanium alloy target and aluminum alloy backplate all is provided with the screw thread to and combine the screw thread of specific interval and degree of depth, on the one hand, it is by doing benefit to increase area of contact, on the other hand, can also break the oxide film on aluminum intermediate level surface.
As a preferred technical scheme of the present invention, before the step (1) of pressing the thread on the welding surface of the aluminum-titanium alloy target into the intermediate layer, the method further includes: and cleaning the aluminum-titanium alloy target and the intermediate layer.
Preferably, the cleaning process is ultrasonic cleaning.
Preferably, the cleaning solution for the cleaning treatment comprises isopropyl alcohol and/or ethanol.
The time of the washing treatment is preferably 5 to 10 minutes, and may be, for example, 6 minutes, 7 minutes, 8 minutes, 9 minutes, or the like, but is not limited to the recited values, and other non-recited values within the above-described range are equally applicable.
As a preferable technical scheme of the invention, the step (1) of pressing the screw thread on the welding surface of the aluminum-titanium alloy target into the middle layer specifically comprises the following steps: the threads on the welding surface of the aluminum-titanium alloy target material are completely pressed into the middle layer by using pressure equipment.
The pressing amount of the pressing device is preferably 2-4mm, and may be, for example, 2.2mm, 2.5mm, 2.7mm, 3mm, 3.2mm, 3.5mm, or 3.7mm, etc., but is not limited to the recited values, and other non-recited values within the above-mentioned range are equally applicable.
It is worth to say that if the pressing amount is too small, the welding surface of the aluminum-titanium alloy target material and the middle layer cannot be tightly attached, so that the welding combination rate is low and the combination strength is low; if the pressing amount is too large, the thickness of the intermediate layer is exceeded, which cannot be achieved.
In a preferred embodiment of the present invention, the temperature of the heat treatment in the step (1) is 400 to 500. DegreeC, for example, 410. DegreeC, 420. DegreeC, 430. DegreeC, 440. DegreeC, 450. DegreeC, 460. DegreeC, 470. DegreeC, 480. DegreeC, 490. DegreeC, etc., but the heat treatment is not limited to the values listed, and other values not listed in the above-mentioned value ranges are equally applicable.
Preferably, the heat treatment in step (1) is performed for a period of 2 to 3 hours, for example, 2.1 hours, 2.2 hours, 2.3 hours, 2.4 hours, 2.5 hours, 2.6 hours, 2.7 hours, 2.8 hours or 2.9 hours, etc., but the heat treatment is not limited to the listed values, and other non-listed values within the above-mentioned range are equally applicable.
It is worth to say that, the invention presses the screw thread on the welding surface of the aluminum-titanium alloy target material into the middle layer completely, then carries on the heat treatment, make the diffusion bond between the materials take place; meanwhile, the temperature of the heat treatment is controlled within a specific range, which is beneficial to improving the welding combination rate and the welding combination strength.
As a preferred embodiment of the present invention, the applying of the pressure in the step (2) is performed by using a pressure device.
The pressing amount of the pressing device is preferably 2-4mm, and may be, for example, 2.2mm, 2.5mm, 2.7mm, 3mm, 3.2mm, 3.5mm, or 3.7mm, etc., but is not limited to the recited values, and other non-recited values within the above-mentioned range are equally applicable.
The invention is worth to describe, apply pressure to the surface of the aluminum-titanium alloy target material-intermediate layer, make the aluminum intermediate layer slightly deform, it can reduce the internal residual pressure after high-temperature diffusion effectively. If the pressing amount is too small, the deformation and the internal stress of the aluminum-titanium alloy target material-intermediate layer after heat treatment cannot be eliminated, so that the final deformation amount of the target material is large; if the pressing amount is too large, the thickness of the intermediate layer is exceeded, which cannot be achieved.
Preferably, after said applying pressure in step (2), before said assembling, further comprising: and (3) machining the middle layer, and then carrying out acid washing treatment on the middle layer and the aluminum alloy backboard.
Preferably, after the intermediate layer is machined, the roughness Ra of the joint surface between the intermediate layer and the aluminum alloy back plate is less than 0.8 μm, and may be, for example, 0.7 μm, 0.65 μm, 0.6 μm, 0.55 μm, 0.5 μm, or 0.4 μm, etc., but is not limited to the values recited, and other values not recited in the above-mentioned numerical ranges are equally applicable.
Preferably, the pickling solution of the pickling treatment is a mixed solution of nitric acid, hydrofluoric acid and water.
Preferably, the molar ratio of nitric acid, hydrofluoric acid and water is (1-2): 1:5, and may be, for example, 1.2:1:5, 1.4:1:5, 1.5:1:5, 1.6:1:5, or 1.8:1:5, etc., but is not limited to the recited values, and other non-recited values within the above ranges are equally applicable.
As a preferred technical solution of the present invention, after the target assembly is placed in the sheath in the step (3), before the hot isostatic pressing, the method further includes: and (5) vacuumizing the sheath.
Preferably, the temperature of the hot isostatic press welding in the step (3) is 200 to 300 ℃, and may be, for example, 210 ℃, 220 ℃, 230 ℃, 240 ℃, 250 ℃, 260 ℃, 270 ℃, 280 ℃, 290 ℃, or the like, but is not limited to the values listed, and other values not listed in the above-mentioned value ranges are equally applicable.
It is worth noting that the welding combination rate and the welding combination strength are improved by controlling the temperature of the hot isostatic pressing welding.
Preferably, the pressure of the hot isostatic welding in the step (3) is 80-120MPa, and may be, for example, 85MPa, 90MPa, 95MPa, 100MPa, 105MPa, 110MPa or 115MPa, etc., but not limited to the values listed, and other values not listed in the above-mentioned value ranges are equally applicable.
Preferably, the time of the hot isostatic pressing welding in the step (3) is 3-5h, for example, 3.2h, 3.5h, 3.7h, 4h, 4.2h, 4.5h, 4.7h or 4.9h, etc., but not limited to the listed values, and other non-listed values in the above-mentioned value ranges are equally applicable.
In the invention, after the hot isostatic pressing welding is finished, the required target assembly is obtained after the sheath is removed.
In a preferred embodiment of the present invention, the welding strength between the aluminum-titanium alloy target and the intermediate layer is not less than 130MPa, and may be, for example, 132MPa, 135MPa, 137MPa, 139MPa, 140MPa, 145MPa, or the like, but is not limited to the values listed, and other values not listed in the above-mentioned numerical ranges are equally applicable.
Preferably, the welding strength between the aluminum alloy back plate and the intermediate layer is not less than 100MPa, for example, 102MPa, 105MPa, 107MPa, 109MPa, 110MPa, 115MPa, or the like, but the present invention is not limited to the above-mentioned values, and other values not shown in the above-mentioned value ranges are equally applicable.
As a preferred technical solution of the present invention, the binding method includes:
(1) Preparing an aluminum-titanium alloy target, an intermediate layer with the thickness of 3-7mm and an aluminum alloy backboard, wherein the roughness Ra of the joint surface of the intermediate layer and the aluminum-titanium alloy target is less than 0.8 mu m, arranging threads on the joint surface of the aluminum-titanium alloy target and the aluminum alloy backboard, then cleaning the aluminum-titanium alloy target and the intermediate layer for 5-10min, completely pressing the threads on the joint surface of the aluminum-titanium alloy target into the intermediate layer by using pressure equipment, and then carrying out heat treatment and heat preservation on the aluminum-titanium alloy target and the intermediate layer for 2-3h at 400-500 ℃ to obtain an aluminum-titanium alloy target-intermediate layer;
the distance between adjacent threads is 0.3-0.5mm, and the depth of the threads is more than 0.2mm;
the pressing amount of the pressure equipment is 2-4mm;
(2) Applying pressure to the surface of the aluminum-titanium alloy target material-middle layer in the step (1) by using pressure equipment, then machining the middle layer, wherein the roughness Ra of the joint surface of the middle layer and the aluminum alloy backboard is less than 0.8 mu m, then carrying out pickling treatment on the middle layer and the aluminum alloy backboard, and then assembling the aluminum alloy backboard and the aluminum-titanium alloy target material-middle layer to obtain a target material assembly;
the pressing amount of the pressure equipment is 2-4mm;
the pickling solution for the pickling treatment is a mixed solution of nitric acid, hydrofluoric acid and water; the molar ratio of nitric acid to hydrofluoric acid to water is (1-2) 1:5;
(3) Placing the target assembly in the step (2) in a sheath, vacuumizing the sheath, and performing hot isostatic pressing welding for 3-5h at 200-300 ℃ and 80-120MPa;
the welding bonding strength of the aluminum-titanium alloy target and the middle layer is more than or equal to 130MPa;
the welding bonding strength of the aluminum alloy backboard and the middle layer is more than or equal to 100MPa.
The numerical ranges recited herein include not only the recited point values, but also any point values between the recited numerical ranges that are not recited, and are limited to, and for the sake of brevity, the invention is not intended to be exhaustive of the specific point values that the recited range includes.
Compared with the prior art, the invention has the following beneficial effects:
according to the binding method provided by the invention, on the basis of arranging the intermediate layer, threads are arranged on the welding surfaces of the aluminum-titanium alloy target and the aluminum alloy backboard through the design of the threads with increased contact area, and the method that the target is combined with the intermediate layer and then combined with the backboard is adopted, so that the influence of welding stress is reduced, the risk brought by deformation is further reduced, the welding combination strength of the aluminum-titanium alloy target and the aluminum intermediate layer is ensured to be more than or equal to 130MPa, the welding combination strength of the aluminum alloy backboard and the aluminum intermediate layer is ensured to be more than or equal to 100MPa, the welding combination rate of the two welding surfaces is more than or equal to 99.9%, the integral deformation is less than or equal to 0.5mm, and the use requirement of the semiconductor sputtering target is met.
Detailed Description
To facilitate understanding of the present invention, examples are set forth below. It will be apparent to those skilled in the art that the examples are merely to aid in understanding the invention and are not to be construed as a specific limitation thereof.
Example 1
The embodiment provides a binding method of an aluminum-titanium alloy target and an aluminum alloy backboard, which comprises the following steps:
(1) Preparing an aluminum-titanium alloy target, an aluminum intermediate layer with the thickness of 5mm and the purity of 99.5 percent and an aluminum alloy backboard, wherein the roughness Ra of the joint surface of the intermediate layer and the aluminum-titanium alloy target is 0.7 mu m, threads are arranged on the welding surfaces of the aluminum-titanium alloy target and the aluminum alloy backboard, then the aluminum-titanium alloy target and the intermediate layer are subjected to 8min of cleaning treatment, then the threads on the welding surfaces of the aluminum-titanium alloy target are completely pressed into the intermediate layer by using pressure equipment, and then the aluminum-titanium alloy target and the aluminum intermediate layer are subjected to heat treatment at the temperature of 450 ℃ and are subjected to heat preservation for 2.5h, so that an aluminum-titanium alloy target-intermediate layer is obtained;
the distance between adjacent threads is 0.4mm, and the depth of the threads is 0.3mm;
the cleaning treatment is ultrasonic cleaning, and the cleaning liquid is isopropanol;
the pressing amount of the pressure equipment is 3mm;
(2) Applying pressure to the surface of the aluminum-titanium alloy target material-middle layer in the step (1) by using pressure equipment, then machining the middle layer, wherein the roughness Ra of the joint surface of the middle layer and the aluminum alloy backboard is 0.7 mu m, then carrying out pickling treatment on the middle layer and the aluminum alloy backboard, and then assembling the aluminum alloy backboard and the aluminum-titanium alloy target material-middle layer to obtain a target material assembly;
the pressing amount of the pressure equipment is 3mm;
the pickling solution for the pickling treatment is a mixed solution of nitric acid, hydrofluoric acid and water; the molar ratio of nitric acid to hydrofluoric acid to water is 1.5:1:5;
(3) Placing the target assembly in the step (2) in a sheath, vacuumizing the sheath, performing hot isostatic pressing welding for 4 hours at the temperature of 250 ℃ and the pressure of 100MPa, and removing the sheath.
Example 2
The embodiment provides a binding method of an aluminum-titanium alloy target and an aluminum alloy backboard, which comprises the following steps:
(1) Preparing an aluminum-titanium alloy target, an aluminum intermediate layer with the thickness of 3.5mm and the purity of 99.5%, and an aluminum alloy backboard, wherein the roughness Ra of the joint surface of the intermediate layer and the aluminum-titanium alloy target is 0.75 mu m, threads are arranged on the welding surfaces of the aluminum-titanium alloy target and the aluminum alloy backboard, then the aluminum-titanium alloy target and the intermediate layer are subjected to cleaning treatment for 10min, then the threads on the welding surfaces of the aluminum-titanium alloy target are completely pressed into the intermediate layer by using pressure equipment, and then the aluminum-titanium alloy target and the aluminum intermediate layer are subjected to heat treatment at 400 ℃ and heat preservation for 3h, so that an aluminum-titanium alloy target-intermediate layer is obtained;
the distance between adjacent threads is 0.32mm, and the depth of the threads is 0.25mm;
the cleaning treatment is ultrasonic cleaning, and the cleaning liquid is ethanol;
the pressing amount of the pressure equipment is 2mm;
(2) Applying pressure to the surface of the aluminum-titanium alloy target material-middle layer in the step (1) by using pressure equipment, then machining the middle layer, wherein the roughness Ra of the joint surface of the middle layer and the aluminum alloy backboard is 0.75 mu m, then carrying out pickling treatment on the middle layer and the aluminum alloy backboard, and then assembling the aluminum alloy backboard and the aluminum-titanium alloy target material-middle layer to obtain a target material assembly;
the pressing amount of the pressure equipment is 2.5mm;
the pickling solution for the pickling treatment is a mixed solution of nitric acid, hydrofluoric acid and water; the molar ratio of nitric acid to hydrofluoric acid to water is 1:1:5;
(3) Placing the target assembly in the step (2) in a sheath, vacuumizing the sheath, performing hot isostatic pressing welding for 5 hours at 200 ℃ and 85MPa, and removing the sheath.
Example 3
The embodiment provides a binding method of an aluminum-titanium alloy target and an aluminum alloy backboard, which comprises the following steps:
(1) Preparing an aluminum-titanium alloy target, an aluminum intermediate layer with the thickness of 7mm and the purity of 99.7%, and an aluminum alloy backboard, wherein the roughness Ra of the joint surface of the intermediate layer and the aluminum-titanium alloy target is 0.65 mu m, threads are arranged on the welding surfaces of the aluminum-titanium alloy target and the aluminum alloy backboard, then the aluminum-titanium alloy target and the intermediate layer are subjected to cleaning treatment for 5min, then the threads on the welding surface of the aluminum-titanium alloy target are completely pressed into the intermediate layer by using pressure equipment, and then the aluminum-titanium alloy target and the aluminum intermediate layer are subjected to heat treatment at 500 ℃ and are subjected to heat preservation for 2h, so that an aluminum-titanium alloy target-intermediate layer is obtained;
the distance between adjacent threads is 0.45mm, and the depth of the threads is 0.35mm;
the cleaning treatment is ultrasonic cleaning, and the cleaning liquid is ethanol;
the pressing amount of the pressure equipment is 4mm;
(2) Applying pressure to the surface of the aluminum-titanium alloy target material-middle layer in the step (1) by using pressure equipment, then machining the middle layer, wherein the roughness Ra of the joint surface of the middle layer and the aluminum alloy backboard is 0.7 mu m, then carrying out pickling treatment on the middle layer and the aluminum alloy backboard, and then assembling the aluminum alloy backboard and the aluminum-titanium alloy target material-middle layer to obtain a target material assembly;
the pressing amount of the pressure equipment is 4mm;
the pickling solution for the pickling treatment is a mixed solution of nitric acid, hydrofluoric acid and water; the molar ratio of nitric acid to hydrofluoric acid to water is 2:1:5;
(3) Placing the target assembly in the step (2) in a sheath, vacuumizing the sheath, performing hot isostatic pressing welding for 2 hours at 300 ℃ and 120MPa, and removing the sheath.
Example 4
The present example provided a binding method of an aluminum-titanium alloy target and an aluminum alloy back plate, except that the "aluminum intermediate layer with a thickness of 5mm and a purity of 99.5% was replaced with" copper intermediate layer with a thickness of 5mm and a purity of 99.5% ", all the other conditions were the same as in example 1.
Example 5
The embodiment provides a binding method of an aluminum-titanium alloy target and an aluminum alloy backboard, and the binding method is the same as that of the embodiment 1 except that the depth of the thread in the step (1) is 0.1 mm.
Example 6
The embodiment provides a binding method of an aluminum-titanium alloy target and an aluminum alloy backboard, and the binding method is the same as that of embodiment 1 except that the distance between adjacent threads in the step (1) is 0.7 mm.
Example 7
The embodiment provides a binding method of an aluminum-titanium alloy target and an aluminum alloy backboard, and the binding method is the same as that of embodiment 1 except that the pressing amount of the pressing device in the step (1) is 1 mm.
Example 8
The embodiment provides a binding method of an aluminum-titanium alloy target and an aluminum alloy backboard, and the binding method is the same as that of embodiment 1 except that the pressing amount of the pressing device in the step (1) is 6 mm.
Example 9
The present embodiment provides a method for binding an aluminum-titanium alloy target and an aluminum alloy backing plate, and the conditions are the same as those in embodiment 1 except that the temperature of the heat treatment in step (1) is 350 ℃.
Example 10
The present embodiment provides a method for binding an aluminum-titanium alloy target and an aluminum alloy backing plate, which is the same as that of embodiment 1 except that the heat treatment temperature in step (1) is 550 ℃.
Example 11
The present embodiment provides a method for binding an aluminum-titanium alloy target and an aluminum alloy backing plate, and the conditions are the same as those of embodiment 1 except that the temperature of the hot isostatic pressing welding in the step (3) is 150 ℃.
Example 12
The present embodiment provides a method for binding an aluminum-titanium alloy target and an aluminum alloy backing plate, and the conditions are the same as those of embodiment 1 except that the temperature of the hot isostatic pressing welding in the step (3) is 350 ℃.
Comparative example 1
The present comparative example provides a binding method of an aluminum-titanium alloy target and an aluminum alloy back plate, and the conditions are the same as those of example 1 except that no screw thread is provided on the welding surface of the aluminum-titanium alloy target and the aluminum alloy back plate in step (1).
Comparative example 2
The present comparative example provides a binding method of an aluminum-titanium alloy target and an aluminum alloy back plate, and the conditions are the same as those of example 1 except that no pressure device is used to apply pressure to the surface of the aluminum-titanium alloy target-intermediate layer in step (2).
Comparative example 3
The comparative example provides a binding method of an aluminum-titanium alloy target and an aluminum alloy backboard, which comprises the following steps:
(1) Preparing an aluminum-titanium alloy target, an aluminum intermediate layer with the thickness of 5mm and the purity of 99.5 percent and an aluminum alloy backboard, arranging threads on the welding surfaces of the aluminum-titanium alloy target and the aluminum alloy backboard, cleaning the aluminum-titanium alloy target, the intermediate layer and the aluminum alloy backboard for 8 minutes, and then assembling the aluminum-titanium alloy target, the aluminum intermediate layer and the aluminum alloy backboard to obtain a target assembly;
the roughness Ra of the bonding surface of the intermediate layer and the aluminum-titanium alloy target is 0.7 mu m; the roughness Ra of the joint surface of the middle layer and the aluminum alloy backboard is 0.7 mu m;
the distance between adjacent threads is 0.4mm, and the depth of the threads is 0.3mm;
the cleaning treatment is ultrasonic cleaning, and the cleaning liquid is isopropanol;
(2) Placing the target assembly in the step (1) in a sheath, vacuumizing the sheath, performing hot isostatic pressing welding for 4 hours at the temperature of 250 ℃ and the pressure of 100MPa, and removing the sheath.
The target assemblies obtained in the above examples and comparative examples were subjected to the tests of the welding bonding rate, the welding bonding strength and the deformation amount, and the test results are shown in table 1.
TABLE 1
From table 1, the following points can be found:
(1) The binding method provided by the embodiments 1-3 of the invention can effectively reduce the stress of the welding position, further reduce the deformation of the target assembly after high-temperature welding, and simultaneously improve the welding bonding rate and the welding bonding strength, wherein the welding bonding strength of the aluminum-titanium alloy target and the aluminum intermediate layer is more than or equal to 130MPa, the welding bonding strength of the aluminum alloy backboard and the aluminum intermediate layer is more than or equal to 100MPa, the welding bonding rate of the two welding surfaces is up to 100%, and the overall deformation is less than 0.5mm;
(2) As can be seen from the comparison of the example 1 and the example 4, when copper is selected as the interlayer material, the copper material is unfavorable for stress release, so that the welding combination rate and the welding combination strength between the aluminum titanium alloy target material and the aluminum alloy backboard and the aluminum interlayer are reduced;
(3) As can be seen from the comparison of the comprehensive examples 1 and examples 5-6 and the comparative example 1, when the depth of the screw thread is too low or the interval between the adjacent screw threads is too large, the contact area between each of the aluminum-titanium alloy target material and the aluminum alloy backboard and the aluminum intermediate layer is reduced, the diffusion rate between the aluminum-titanium alloy target material and the aluminum alloy backboard is reduced, and the welding combination rate and the welding combination strength between each of the aluminum-titanium alloy target material and the aluminum alloy backboard and the aluminum intermediate layer are reduced;
(4) As can be seen from comparison of the example 1 and the examples 7-8, when the pressing amount of the pressing device in the step (1) is too small, the welding surfaces cannot be tightly attached to each other, so that the welding bonding rate and bonding strength between the aluminum-titanium alloy target and the aluminum intermediate layer are low; when the pressing amount of the pressing equipment in the step (1) is too large, the thickness of the middle layer is exceeded;
(5) As can be seen from the comparison of the example 1 and the examples 9 to 10, when the heat treatment temperature in the step (1) is too low, the bonding strength between the aluminum-titanium alloy target and the aluminum intermediate layer is low because the aluminum-titanium alloy target and the aluminum intermediate layer cannot form diffusion bonding; when the heat treatment temperature in the step (1) is too high, the diffusion layer between the aluminum-titanium alloy target and the aluminum intermediate layer has brittle precipitated phase, so that the bonding strength between the aluminum-titanium alloy target and the aluminum intermediate layer is low;
(6) As can be seen from comparing the examples 1 and 11-12, when the hot isostatic pressing welding temperature in the step (3) is too low, the bonding strength between the aluminum alloy back plate and the aluminum intermediate layer is low because diffusion bonding cannot be formed between the aluminum alloy back plate and the aluminum intermediate layer; when the hot isostatic pressing welding temperature in the step (3) is too high, the deformation of the target is large due to the difference of the thermal expansion coefficients of the materials;
(7) As can be seen from comparison of the comprehensive examples 1 and 2, if no pressure is applied to the bonded aluminum-titanium alloy target-intermediate layer, residual stress of high-temperature diffusion bonding cannot be effectively released, so that deformation after welding is difficult to eliminate, and the overall deformation amount becomes large;
(8) As can be seen from comparison of the comprehensive examples 1 and the comparative examples 3, when only one-step hot isostatic pressing welding is performed after the assembly of the target assembly, deformation after welding is difficult to eliminate due to the difference of thermal expansion coefficients between materials, so that the overall deformation of the target is large, and great difficulty is brought to subsequent processing.
The applicant declares that the above is only a specific embodiment of the present invention, but the scope of the present invention is not limited thereto, and it should be apparent to those skilled in the art that any changes or substitutions that are easily conceivable within the technical scope of the present invention disclosed by the present invention fall within the scope of the present invention and the disclosure.
Claims (10)
1. The binding method of the aluminum-titanium alloy target and the aluminum alloy backboard is characterized by comprising the following steps of:
(1) Preparing an aluminum-titanium alloy target, an intermediate layer and an aluminum alloy backboard, arranging threads on the welding surfaces of the aluminum-titanium alloy target and the aluminum alloy backboard, pressing the threads on the welding surfaces of the aluminum-titanium alloy target into the intermediate layer, and then performing heat treatment on the aluminum-titanium alloy target and the intermediate layer to obtain an aluminum-titanium alloy target-intermediate layer;
(2) Applying pressure on the surface of the aluminum-titanium alloy target material-middle layer in the step (1), and then assembling an aluminum alloy backboard with the aluminum-titanium alloy target material-middle layer to obtain a target material assembly;
(3) And (3) placing the target assembly in the step (2) in a sheath for hot isostatic pressing welding.
2. The binding method of claim 1, wherein the material of the intermediate layer of step (1) comprises aluminum having a purity of > 99%;
preferably, the thickness of the intermediate layer in the step (1) is 3-7mm;
preferably, the roughness Ra of the bonding surface of the intermediate layer and the aluminum-titanium alloy target material in the step (1) is less than 0.8 mu m.
3. A binding method according to claim 1 or 2, wherein the pitch of the threads of adjacent step (1) is 0.3-0.5mm;
preferably, the depth of the thread of step (1) is > 0.2mm.
4. A binding method according to any one of claims 1 to 3, further comprising, prior to said pressing the threads on the welding face of the target of the aluminium-titanium alloy into the intermediate layer in step (1): cleaning the aluminum-titanium alloy target and the intermediate layer;
preferably, the cleaning treatment is ultrasonic cleaning;
preferably, the cleaning solution for the cleaning treatment comprises isopropanol and/or ethanol;
preferably, the time of the washing treatment is 5-10min.
5. The binding method according to any one of claims 1 to 4, wherein the pressing the threads on the welding surface of the aluminum-titanium alloy target into the intermediate layer in the step (1) specifically comprises: completely pressing the screw thread on the welding surface of the aluminum-titanium alloy target into the middle layer by using pressure equipment;
preferably, the pressing amount of the pressing device is 2-4mm.
6. The binding method according to any one of claims 1 to 5, wherein the temperature of the heat treatment of step (1) is 400 to 500 ℃;
preferably, the heat treatment in step (1) is carried out for a period of 2-3 hours.
7. The binding method according to any one of claims 1 to 6, wherein the applying of the pressure in step (2) is performed using a pressure device;
preferably, the pressing amount of the pressure device is 2-4mm;
preferably, after said applying pressure in step (2), before said assembling, further comprising: machining the middle layer, and then carrying out acid washing treatment on the middle layer and the aluminum alloy backboard;
preferably, after the intermediate layer is machined, the roughness Ra of the joint surface of the intermediate layer and the aluminum alloy backboard is less than 0.8 mu m;
preferably, the pickling solution of the pickling treatment is a mixed solution of nitric acid, hydrofluoric acid and water;
preferably, the molar ratio of nitric acid, hydrofluoric acid and water is (1-2): 1:5.
8. The bonding method according to any one of claims 1-7, further comprising, after the target assembly of step (3) is placed in the capsule, prior to the hot isostatic welding: vacuumizing the sheath;
preferably, the temperature of the hot isostatic pressing welding in the step (3) is 200-300 ℃;
preferably, the pressure of the hot isostatic pressing welding in the step (3) is 80-120MPa;
preferably, the hot isostatic pressing welding in step (3) takes 3-5 hours.
9. The binding method according to any one of claims 1 to 8, wherein the welding bonding strength of the aluminum-titanium alloy target and the intermediate layer is not less than 130MPa;
preferably, the welding bonding strength of the aluminum alloy backboard and the middle layer is more than or equal to 100MPa.
10. The binding method according to any one of claims 1 to 9, wherein the binding method comprises:
(1) Preparing an aluminum-titanium alloy target, an intermediate layer with the thickness of 3-7mm and an aluminum alloy backboard, wherein the roughness Ra of the joint surface of the intermediate layer and the aluminum-titanium alloy target is less than 0.8 mu m, arranging threads on the joint surface of the aluminum-titanium alloy target and the aluminum alloy backboard, then cleaning the aluminum-titanium alloy target and the intermediate layer for 5-10min, completely pressing the threads on the joint surface of the aluminum-titanium alloy target into the intermediate layer by using pressure equipment, and then carrying out heat treatment and heat preservation on the aluminum-titanium alloy target and the intermediate layer for 2-3h at 400-500 ℃ to obtain an aluminum-titanium alloy target-intermediate layer;
the distance between adjacent threads is 0.3-0.5mm, and the depth of the threads is more than 0.2mm;
the pressing amount of the pressure equipment is 2-4mm;
(2) Applying pressure to the surface of the aluminum-titanium alloy target material-middle layer in the step (1) by using pressure equipment, then machining the middle layer, wherein the roughness Ra of the joint surface of the middle layer and the aluminum alloy backboard is less than 0.8 mu m, then carrying out pickling treatment on the middle layer and the aluminum alloy backboard, and then assembling the aluminum alloy backboard and the aluminum-titanium alloy target material-middle layer to obtain a target material assembly;
the pressing amount of the pressure equipment is 2-4mm;
the pickling solution for the pickling treatment is a mixed solution of nitric acid, hydrofluoric acid and water; the molar ratio of nitric acid to hydrofluoric acid to water is (1-2) 1:5;
(3) Placing the target assembly in the step (2) in a sheath, vacuumizing the sheath, and performing hot isostatic pressing welding for 3-5h at 200-300 ℃ and 80-120MPa;
the welding bonding strength of the aluminum-titanium alloy target and the middle layer is more than or equal to 130MPa;
the welding bonding strength of the aluminum alloy backboard and the middle layer is more than or equal to 100MPa.
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| CN202311138482.2A CN117161534A (en) | 2023-09-05 | 2023-09-05 | Binding method of aluminum-titanium alloy target and aluminum alloy backboard |
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