Binding method for titanium-niobium alloy target material and back plate

Abstract

The invention provides a method for binding a titanium-niobium alloy target material and a back plate. The binding method comprises the following steps: sequentially carrying out sand blasting and nickel plating on a welding surface of the titanium-niobium alloy target material; the titanium-niobium alloy target material and the back plate are independently subjected to two-stage heating, and then the titanium-niobium alloy target material and the back plate are infiltrated through welding flux; and a welding flux groove is formed in the welding face of the back plate, a copper wire is placed in the welding flux groove, the titanium-niobium alloy target and the welding face of the back plate are attached and pressed, and welding is completed. According to the binding method, welding binding of the titanium-niobium alloy target material and the back plate is achieved, the welding binding rate of the target material and the back plate reaches 99.2% or above, the welding strength reaches 4.7 MPa or above, it is ensured that the target material and the back plate are firmly bound in the sputtering use process, and unsoldering does not occur.

Description

Technical Field

[0001] The invention belongs to the technical field of sputtering target materials, and relates to a titanium-niobium alloy target material, and in particular to a method for binding the titanium-niobium alloy target material to a back plate. Background Art

[0002] Titanium and niobium are both important rare metals developed in the mid-20th century. Titanium has the characteristics of low density, high strength and good corrosion resistance, while niobium is known for its excellent chemical stability and ability to enhance alloy strength. Both have excellent properties in corrosion resistance, high temperature resistance, superconductivity, biocompatibility and other aspects.

[0003] Titanium-niobium alloy is mainly composed of two elements, titanium (Ti) and niobium (Nb). It has high strength, good corrosion resistance and excellent biocompatibility. It can also maintain stable performance in extreme environments, meeting the high standards of materials required by modern technological development. The ratio of the two elements directly affects the performance and application of the alloy.

[0004] Sputtering is one of the main technologies for preparing thin film materials. When charged particles bombard the surface of solid materials, surface atoms collide and energy and momentum transfer occurs, causing the bombarded material atoms to escape from the surface and deposit on the substrate. The bombarded solid is the raw material for preparing deposited thin films by sputtering, generally referred to as sputtering targets. Due to the different strengths of sputtering targets, in actual applications, it is necessary to bind the sputtering target and the backing plate to form a target assembly for use on the sputtering machine, and ensure that the target does not fall off the backing plate during the sputtering process.

[0005] CN112059349A discloses a method for welding a titanium target and a copper back plate, wherein the welding surfaces of the titanium target and the copper back plate are sandblasted and acid treated in sequence, and then solder is added for brazing; CN113579393A discloses a method for brazing a niobium target and a copper back plate, wherein the welding surfaces of the niobium target are sandblasted and chemically nickel plated in sequence, and then the niobium target and the copper back plate are infiltrated with solder respectively, and the infiltrated target and the back plate are welded. The above two methods are respectively used to bind the titanium target and the niobium target to the back plate. However, the performance of titanium-niobium alloy is very different from that of single-element targets of titanium and niobium. In the prior art, there is no example of a method for binding a titanium-niobium alloy target to a back plate, and the bonding strength and bonding rate of the titanium-niobium alloy target to the back plate need to be improved.

[0006] Based on this, it is necessary to provide a method for binding a titanium-niobium alloy target and a back plate. Summary of the invention

[0007] In view of the shortcomings of the prior art, the purpose of the present invention is to provide a method for binding a titanium-niobium alloy target and a back plate to improve the welding effect of the titanium-niobium alloy target and the back plate.

[0008] To achieve this object, the present invention adopts the following technical solutions:

[0009] The present invention provides a method for binding a titanium-niobium alloy target material and a back plate, and the binding method comprises the following steps:

[0010] (1) sequentially sandblasting and nickel plating the welding surface of the titanium-niobium alloy target;

[0011] (2) heating the titanium-niobium alloy target and the backing plate independently in two stages and then infiltrating them with solder;

[0012] (3) A solder groove is formed on the welding surface of the back plate and a copper wire is placed therein, and the titanium-niobium alloy target is bonded to the welding surface of the back plate and pressure is applied to complete the welding.

[0013] The method provided by the present invention is used for welding and binding a titanium-niobium alloy target material and a back plate, thereby solving the problem that welding of the titanium-niobium alloy target material and the back plate is prone to defects and low welding strength, and improving the welding bonding rate and welding strength of the target material and the back plate.

[0014] Preferably, the composition of the titanium-niobium alloy target includes: 85-95wt% titanium and 5-15wt% niobium.

[0015] In the titanium-niobium alloy target, the titanium content is 85-95wt%, for example, 85wt%, 88wt%, 90wt%, 92wt% or 95wt%, but is not limited to the listed values, and other values ​​not listed within the numerical range are also applicable.

[0016] In the titanium-niobium alloy target, the niobium content is 5-15wt%, for example, 5wt%, 8wt%, 10wt%, 12wt% or 15wt%, but is not limited to the listed values, and other values ​​not listed within the numerical range are also applicable.

[0017] Preferably, the pressure of the sandblasting in step (1) is 3-5 kg, for example, 3 kg, 3.5 kg, 4 kg, 4.5 kg or 5 kg, but is not limited to the listed values, and other values ​​not listed within the numerical range are also applicable.

[0018] Preferably, the blasting material in step (1) comprises glass beads.

[0019] Preferably, the particle size of the sandblasting material in step (1) is 100-200 mesh, for example, it can be 100 mesh, 125 mesh, 150 mesh, 175 mesh or 200 mesh, but is not limited to the listed values, and other values ​​not listed within the numerical range are also applicable.

[0020] Preferably, the nickel plating in step (1) is chemical nickel plating.

[0021] The chemical nickel plating method comprises: washing the target welding surface after sandblasting with a high-pressure water gun for 2-4 minutes, then removing the oxide scale and impurities on the surface by pickling, then performing surface activation to remove the hydroxide produced by pickling, and finally performing chemical nickel plating for 40 minutes.

[0022] Preferably, the nickel layer thickness of the nickel plating in step (1) is 20-60 μm, for example, 20 μm, 30 μm, 40 μm, 50 μm or 60 μm, but is not limited to the listed values, and other values ​​not listed within the numerical range are also applicable.

[0023] Preferably, the two-stage heating process of step (2) is: heating to a first heating temperature at a first heating rate, keeping the temperature, and then heating to a second heating temperature at a second heating rate.

[0024] Preferably, the first heating rate is 2-3°C / min, for example, 2°C / min, 2.3°C / min, 2.5°C / min, 2.8°C / min or 3°C / min, but is not limited to the listed values, and other unlisted values ​​within the numerical range are also applicable.

[0025] Preferably, the first heating temperature is 140-160°C, for example, 140°C, 145°C, 150°C, 155°C or 160°C, but is not limited to the listed values, and other unlisted values ​​within the numerical range are also applicable.

[0026] Preferably, the insulation time is 20-30 min, for example, 20 min, 23 min, 25 min, 28 min or 30 min, but is not limited to the listed values, and other unlisted values ​​within the numerical range are also applicable.

[0027] Preferably, the second heating rate is 1-2°C / min, for example, 1°C / min, 1.3°C / min, 1.5°C / min, 1.8°C / min or 2°C / min, but is not limited to the listed values, and other unlisted values ​​within the numerical range are also applicable.

[0028] Preferably, the second heating temperature is 210-220°C, for example, 210°C, 213°C, 215°C, 218°C or 220°C, but is not limited to the listed values, and other unlisted values ​​within the numerical range are also applicable.

[0029] Preferably, the infiltration in step (2) is carried out by ultrasonic infiltration.

[0030] Preferably, the frequency of the ultrasonic wave is 15-20 kHz, for example, 15 kHz, 16 kHz, 17 kHz, 18 kHz, 19 kHz or 20 kHz, but is not limited to the listed values, and other values ​​not listed within the numerical range are also applicable.

[0031] Preferably, the wetting time of the titanium-niobium alloy target is 10-15 min, for example, 10 min, 11 min, 12 min, 13 min, 14 min or 15 min, but is not limited to the listed values, and other values ​​not listed within the numerical range are also applicable.

[0032] Preferably, the wetting time of the backplane is 15-25 min, for example, 15 min, 18 min, 20 min, 23 min or 25 min, but is not limited to the listed values, and other unlisted values ​​within the numerical range are also applicable.

[0033] Preferably, the diameter of the copper wire in step (3) is 0.3-0.5 mm, for example, 0.3 mm, 0.35 mm, 0.4 mm, 0.45 mm or 0.5 mm, but is not limited to the listed values, and other values ​​not listed within the numerical range are also applicable.

[0034] Preferably, the depth of the solder groove in step (3) is 1-3 mm, for example, 1 mm, 1.5 mm, 2 mm, 2.5 mm or 3 mm, but is not limited to the listed values, and other values ​​not listed within the numerical range are also applicable.

[0035] Preferably, the material of the back panel in step (3) includes A5083.

[0036] Preferably, the pressure in step (3) is applied by placing a 20-25 kg pressure block, for example, 20 kg, 21 kg, 22 kg, 23 kg, 24 kg or 25 kg, but is not limited to the listed values, and other values ​​not listed within the numerical range are also applicable.

[0037] As a preferred technical solution of the binding method provided by the present invention, the binding method comprises the following steps:

[0038] (1) cleaning the welding surface of the titanium-niobium alloy target, and sandblasting the target with glass beads having a particle size of 100-200 meshes at a pressure of 3-5 kg; then placing the titanium-niobium alloy target in a nickel plating tank for chemical nickel plating, wherein the thickness of the nickel layer after nickel plating is 20-60 μm;

[0039] (2) heating the titanium-niobium alloy target and the back plate on a heating platform, first heating the temperature to 140-160°C at a heating rate of 2-3°C / min, keeping the temperature for 20-30 minutes, and then heating the temperature to 210-220°C at a heating rate of 1-2°C / min, placing molten solder on the welding surface of the titanium-niobium alloy target and the welding surface of the back plate and performing ultrasonic infiltration, the ultrasonic frequency is 15-20kHz, the titanium-niobium alloy target infiltration time is 10-15 minutes, and the back plate infiltration time is 15-25 minutes;

[0040] (3) A solder groove is formed on the welding surface of the back plate and a 0.3-0.5 mm copper wire is placed therein. Then, the titanium-niobium alloy target and the welding surface of the back plate are bonded together, and a 20-25 kg pressure block is placed thereon for pressure. After cooling, the welding is completed.

[0041] Compared with the prior art, the present invention has the following beneficial effects:

[0042] The binding method provided by the present invention realizes the welding binding of the titanium-niobium alloy target material and the back plate, the welding bonding rate of the target material and the back plate reaches 99.2%, and the welding strength reaches 4.7MPa, ensuring that the target material is firmly bound to the back plate during sputtering without desoldering. DETAILED DESCRIPTION

[0043] The technical solution of the present invention is further illustrated below through specific implementation methods.

[0044] In order to clearly illustrate the technical solution of the present invention, in a specific implementation manner, the composition of the titanium-niobium alloy target used is: 85-95wt% titanium, 5-15wt% niobium, and the back plate material used is aluminum alloy.

[0045] Example 1

[0046] This embodiment provides a method for binding a titanium-niobium alloy target and a back plate, and the binding method comprises the following steps:

[0047] (1) Wipe the welding surface of the titanium-niobium target with alcohol to remove surface dirt, and use tape to protect and mask the rest of the surface except the welding surface to prevent damage during sandblasting. Then, sandblast the welding surface using glass beads with a particle size of 150 mesh and a sandblasting pressure of 4 kg;

[0048] (2) ultrasonically cleaning the titanium-niobium target to remove surface stains, and then chemically nickel-plating the welding surface. The titanium-niobium target is placed in a nickel plating tank for chemical nickel plating. The nickel layer thickness is 40 μm, and then blown dry with an air gun;

[0049] (3) The titanium-niobium target and the back plate are placed separately on a heating platform, and the temperature is raised to 150°C at a heating rate of 2.5°C / min, and then kept at this temperature for 25 minutes to allow the titanium-niobium target and the back plate to be fully and evenly heated, and then the temperature is raised to 215°C at a heating rate of 1.5°C / min, and molten solder is placed on the welding surface of the titanium-niobium target and the welding surface of the back plate and ultrasonically infiltrated. The ultrasonic frequency is 18 kHz, the infiltration time of the titanium-niobium target is 12 minutes, and the infiltration time of the back plate is 20 minutes, so that the back plate and the target are fully infiltrated;

[0050] (4) Place a 0.4 mm copper wire in the solder groove of the backplane, the depth of the solder groove is 2 mm, then fit the target material and the welding surface of the backplane together, and then place a 22 kg pressure block on it, and complete the welding after cooling.

[0051] Example 2

[0052] This embodiment provides a method for binding a titanium-niobium alloy target and a back plate, and the binding method comprises the following steps:

[0053] (1) Wipe the welding surface of the titanium-niobium target with alcohol to remove surface dirt, and use tape to protect and mask the rest of the surface except the welding surface to prevent damage during sandblasting. Then, sandblast the welding surface using glass beads with a particle size of 100 mesh and a sandblasting pressure of 3 kg;

[0054] (2) ultrasonically cleaning the titanium-niobium target to remove surface stains, and then chemically nickel-plating the welding surface. The titanium-niobium target is placed in a nickel plating tank for chemical nickel plating. The nickel layer thickness is 20 μm, and then blown dry with an air gun;

[0055] (3) The titanium-niobium target and the back plate are placed separately on a heating platform, and the temperature is raised to 140°C at a heating rate of 2°C / min, and then kept warm for 30 minutes to allow the titanium-niobium target and the back plate to be fully and evenly heated, and then the temperature is raised to 220°C at a heating rate of 2°C / min, and molten solder is placed on the welding surface of the titanium-niobium target and the welding surface of the back plate and ultrasonically infiltrated. The ultrasonic frequency is 15kHz, the infiltration time of the titanium-niobium target is 15 minutes, and the infiltration time of the back plate is 25 minutes, so that the back plate and the target are fully infiltrated;

[0056] (4) Place a 0.3 mm copper wire in the solder groove of the backplane. The depth of the solder groove is 2 mm. Then fit the target material and the welding surface of the backplane together. Then place a 20 kg pressure block on it. After cooling, the welding is completed.

[0057] Example 3

[0058] This embodiment provides a method for binding a titanium-niobium alloy target and a back plate, and the binding method comprises the following steps:

[0059] (1) Wipe the welding surface of the titanium-niobium target with alcohol to remove surface dirt, and use tape to protect and mask the rest of the surface except the welding surface to prevent damage during sandblasting. Then, sandblast the welding surface using glass beads with a particle size of 200 mesh and a sandblasting pressure of 5 kg;

[0060] (2) ultrasonically cleaning the titanium-niobium target to remove surface stains, and then chemically nickel-plating the welding surface. The titanium-niobium target is placed in a nickel plating tank for chemical nickel plating, with a nickel layer thickness of 60 μm, and then blown dry with an air gun;

[0061] (3) The titanium-niobium target and the back plate are placed separately on a heating platform, and the temperature is raised to 160°C at a heating rate of 3°C / min, and then kept at this temperature for 20 minutes to allow the titanium-niobium target and the back plate to be fully and evenly heated, and then the temperature is raised to 210°C at a heating rate of 1°C / min, and molten solder is placed on the welding surface of the titanium-niobium target and the welding surface of the back plate and ultrasonically infiltrated. The ultrasonic frequency is 20 kHz, the infiltration time of the titanium-niobium target is 10 minutes, and the infiltration time of the back plate is 15 minutes, so that the back plate and the target are fully infiltrated;

[0062] (4) Place a 0.5 mm copper wire in the solder groove of the backplane, the depth of the solder groove is 2 mm, then fit the target material and the welding surface of the backplane together, and then place a 25 kg pressure block on it, and complete the welding after cooling.

[0063] Example 4

[0064] This embodiment provides a method for binding a titanium-niobium alloy target to a back plate. Compared with Embodiment 1, the second heating temperature in step (3) is controlled to be 200° C., and the rest is the same as Embodiment 1.

[0065] Example 5

[0066] This embodiment provides a method for binding a titanium-niobium alloy target to a back plate. Compared with Embodiment 1, the second heating temperature in step (3) is controlled to be 230° C., and the rest is the same as Embodiment 1.

[0067] Example 6

[0068] This embodiment provides a method for binding a titanium-niobium alloy target to a backing plate. Compared with Embodiment 1, the second heating rate in step (3) is controlled to be 3° C. / min, and the rest is the same as Embodiment 1.

[0069] Example 7

[0070] This embodiment provides a method for binding a titanium-niobium alloy target to a back plate. Compared with Embodiment 1, the first heating temperature in step (3) is controlled to be 120° C., and the rest is the same as Embodiment 1.

[0071] Example 8

[0072] This embodiment provides a method for binding a titanium-niobium alloy target to a back plate. Compared with Embodiment 1, the first heating temperature in step (3) is controlled to be 180° C., and the rest is the same as Embodiment 1.

[0073] Comparative Example 1

[0074] This comparative example provides a method for binding a titanium-niobium alloy target and a backing plate. Compared with Example 1, one-stage heating is adopted in the control step (3), that is, the titanium-niobium target and the backing plate are directly heated to 215° C., and the rest is the same as Example 1.

[0075] Comparative Example 2

[0076] This comparative example provides a method for binding a titanium-niobium alloy target to a back plate. Compared with Example 1, the control step (1) is not sandblasted, and the rest is the same as Example 1.

[0077] Comparative Example 3

[0078] This comparative example provides a method for binding a titanium-niobium alloy target to a back plate. Compared with Example 1, nickel plating is not performed in step (2), and the rest is the same as Example 1.

[0079] Comparative Example 4

[0080] This comparative example provides a method for binding a titanium-niobium alloy target to a back plate. Compared with Example 1, infiltration is not performed in the control step (3), and the rest is the same as Example 1.

[0081] The target material and back plate assembly bound by the method provided in the embodiment and the comparative example were tested for their welding bonding rate, welding bonding strength and defect conditions, and the results are listed in Table 1.

[0082] The testing method for welding bonding rate is: ultrasonic C-SCAN scanning.

[0083] The test method for welding bond strength is: tensile test.

[0084] The testing method for defects is: ultrasonic C-SCAN scanning.

[0085] Table 1

[0086]

[0087]

[0088] The “overall defect rate” in the table is the ratio of defect area to welding area.

[0089] As can be seen from Table 1, the binding method provided by the present invention has a good welding bonding rate of more than 99.2%, and has a high welding strength of more than 4.7 MPa, and has few defects. Compared with Example 1, in Examples 4-8, after adjusting the process parameters, the welding performance is slightly reduced. In Comparative Examples 1-4, the lack of any step in the process leads to a significant decrease in the bonding effect. Each step of the binding method of the present invention is crucial and indispensable.

[0090] The specific embodiments described above further illustrate the objectives, technical solutions and beneficial effects of the present invention in detail. It should be understood that the above description is only a specific embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present invention should be included in the protection scope of the present invention.

Claims

1. A method for binding a titanium-niobium alloy target material to a backing plate, characterized in that: The binding method comprises the following steps: (1) sequentially sandblasting and nickel plating the welding surface of the titanium-niobium alloy target; (2) heating the titanium-niobium alloy target and the backing plate independently in two stages, and then infiltrating the titanium-niobium alloy target and the backing plate with solder; (3) A solder groove is formed on the welding surface of the back plate and a copper wire is placed therein, and the titanium-niobium alloy target is bonded to the welding surface of the back plate and pressure is applied to complete the welding.

2. The binding method according to claim 1, characterized in that: The composition of the titanium-niobium alloy target material includes: 85-95wt% titanium and 5-15wt% niobium.

3. The binding method according to claim 1 or 2, characterized in that: The pressure of the sandblasting in step (1) is 3-5 kg; Preferably, the blasting material of the sandblasting in step (1) comprises glass beads; Preferably, the particle size of the sandblasting material in step (1) is 100-200 mesh.

4. The binding method according to any one of claims 1 to 3, characterized in that: The nickel plating in step (1) is chemical nickel plating; Preferably, the nickel layer thickness of the nickel plating in step (1) is 20-60 μm.

5. The binding method according to any one of claims 1 to 4, characterized in that: The two-stage heating process of step (2) is: heating to the first heating temperature at a first heating rate, keeping the temperature, and then heating to the second heating temperature at a second heating rate.

6. The binding method according to claim 5, characterized in that: The first heating rate is 2-3°C / min; Preferably, the first heating temperature is 140-160°C; Preferably, the insulation time is 20-30 minutes; Preferably, the second heating rate is 1-2°C / min; Preferably, the second heating temperature is 210-220°C.

7. The binding method according to any one of claims 1 to 6, characterized in that: The infiltration in step (2) is carried out by ultrasonic infiltration; Preferably, the frequency of the ultrasonic wave is 15-20kHz; Preferably, the wetting time of the titanium-niobium alloy target is 10-15 min; Preferably, the infiltration time of the backplane is 15-25 minutes.

8. The binding method according to any one of claims 1 to 7, characterized in that: The diameter of the copper wire in step (3) is 0.3-0.5 mm; Preferably, the depth of the solder groove in step (3) is 1-3 mm; Preferably, the material of the back plate in step (3) includes aluminum alloy A5083.

9. The binding method according to any one of claims 1 to 8, characterized in that: The pressure in step (3) is applied by placing a 20-25 kg pressing block.

10. The binding method according to any one of claims 1 to 9, characterized in that: The binding method comprises the following steps: (1) cleaning the welding surface of the titanium-niobium alloy target, and sandblasting the target with glass beads having a particle size of 100-200 meshes at a pressure of 3-5 kg; then placing the titanium-niobium alloy target in a nickel plating tank for chemical nickel plating, wherein the thickness of the nickel layer after nickel plating is 20-60 μm; (2) heating the titanium-niobium alloy target and the back plate on a heating platform, first heating the temperature to 140-160°C at a heating rate of 2-3°C / min, keeping the temperature for 20-30 minutes, and then heating the temperature to 210-220°C at a heating rate of 1-2°C / min, placing molten solder on the welding surface of the titanium-niobium alloy target and the welding surface of the back plate and performing ultrasonic infiltration, the ultrasonic frequency is 15-20kHz, the titanium-niobium alloy target infiltration time is 10-15 minutes, and the back plate infiltration time is 15-25 minutes; (3) A solder groove is formed on the welding surface of the back plate and a 0.3-0.5 mm copper wire is placed therein. Then, the titanium-niobium alloy target and the welding surface of the back plate are bonded together, and a 20-25 kg pressure block is placed thereon for pressure. After cooling, the welding is completed.

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