CN115464293A - Welding method for spliced niobium target - Google Patents
Welding method for spliced niobium target Download PDFInfo
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- CN115464293A CN115464293A CN202211213390.1A CN202211213390A CN115464293A CN 115464293 A CN115464293 A CN 115464293A CN 202211213390 A CN202211213390 A CN 202211213390A CN 115464293 A CN115464293 A CN 115464293A
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- niobium target
- target
- niobium
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- 229910052758 niobium Inorganic materials 0.000 title claims abstract description 284
- 239000010955 niobium Substances 0.000 title claims abstract description 284
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 title claims abstract description 284
- 238000003466 welding Methods 0.000 title claims abstract description 137
- 238000000034 method Methods 0.000 title claims abstract description 55
- 238000001764 infiltration Methods 0.000 claims abstract description 23
- 230000008595 infiltration Effects 0.000 claims abstract description 23
- 238000002791 soaking Methods 0.000 claims abstract description 22
- 238000007781 pre-processing Methods 0.000 claims abstract description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 34
- 229910000679 solder Inorganic materials 0.000 claims description 33
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 29
- 229910052738 indium Inorganic materials 0.000 claims description 29
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 claims description 29
- 239000002184 metal Substances 0.000 claims description 22
- 229910052751 metal Inorganic materials 0.000 claims description 22
- 229910052802 copper Inorganic materials 0.000 claims description 21
- 239000010949 copper Substances 0.000 claims description 21
- 238000010438 heat treatment Methods 0.000 claims description 21
- 238000005488 sandblasting Methods 0.000 claims description 20
- 238000003825 pressing Methods 0.000 claims description 19
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 18
- 238000000576 coating method Methods 0.000 claims description 18
- 229910052759 nickel Inorganic materials 0.000 claims description 17
- 238000007747 plating Methods 0.000 claims description 17
- 239000011248 coating agent Substances 0.000 claims description 16
- 239000007788 liquid Substances 0.000 claims description 13
- -1 polytetrafluoroethylene Polymers 0.000 claims description 13
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 13
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 13
- 229910000881 Cu alloy Inorganic materials 0.000 claims description 10
- 229910000831 Steel Inorganic materials 0.000 claims description 10
- 239000002390 adhesive tape Substances 0.000 claims description 10
- 239000010959 steel Substances 0.000 claims description 10
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 9
- 239000007864 aqueous solution Substances 0.000 claims description 9
- 229910003437 indium oxide Inorganic materials 0.000 claims description 9
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 claims description 9
- 229910017604 nitric acid Inorganic materials 0.000 claims description 9
- 125000006850 spacer group Chemical group 0.000 claims description 6
- 238000009736 wetting Methods 0.000 claims description 5
- 238000005476 soldering Methods 0.000 claims description 4
- 238000005422 blasting Methods 0.000 claims description 3
- 239000000243 solution Substances 0.000 claims description 3
- 238000004544 sputter deposition Methods 0.000 abstract description 18
- 230000000052 comparative effect Effects 0.000 description 19
- 239000013077 target material Substances 0.000 description 16
- 238000005192 partition Methods 0.000 description 6
- 230000000694 effects Effects 0.000 description 4
- 230000001681 protective effect Effects 0.000 description 4
- 230000004907 flux Effects 0.000 description 3
- 238000005520 cutting process Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 230000035939 shock Effects 0.000 description 2
- 230000008093 supporting effect Effects 0.000 description 2
- 230000002411 adverse Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000005219 brazing Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000002093 peripheral effect Effects 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 238000012797 qualification Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000005477 sputtering target Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K31/00—Processes relevant to this subclass, specially adapted for particular articles or purposes, but not covered by only one of the preceding main groups
- B23K31/02—Processes relevant to this subclass, specially adapted for particular articles or purposes, but not covered by only one of the preceding main groups relating to soldering or welding
-
- 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
-
- 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
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/31—Coating with metals
- C23C18/32—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Physical Vapour Deposition (AREA)
Abstract
The invention relates to a welding method of a spliced niobium target, which comprises the following steps: (1) Preprocessing the welding surface of the back plate to obtain a preprocessed back plate; (2) Sequentially carrying out pre-soaking treatment and fine soaking treatment on the pretreated back plate obtained in the step (1), and then attaching spacing bars to a welding surface to obtain a spacing back plate; (3) Splicing the first niobium target, the second niobium target and the third niobium target on the spacing back plate obtained in the step (2) in sequence to enable the width of the spliced gap to be equal to that of the spacing bar; and then carrying out pressurization treatment to obtain the spliced niobium target. The welding combination rate of the back plate and the niobium target is improved by carrying out pretreatment and infiltration treatment on the back plate and the niobium target; the spacing strips are attached to the welding surface of the back plate, so that the width of a gap formed by splicing the niobium target can be adjusted and controlled, and the use requirement of sputtering is met.
Description
Technical Field
The invention relates to the technical field of sputtering targets, in particular to a welding method of a spliced niobium target.
Background
Sputtering is a relatively common process technology in the field of semiconductor manufacturing. In the sputtering technique, a target material is a sputtering material as a core, and the influence on the film formation quality after sputtering is large. The target material is usually welded with the back plate to form a target material assembly which is used in actual sputtering coating, and because the working environment of the target material assembly is severe, higher requirements are put forward on the welding combination degree of the target material and the back plate.
CN 207793415U discloses a spliced target, which comprises a back plate and a target assembly arranged on the back plate; the target assembly comprises a plurality of target units; the target units are spliced to form the target assembly; the height of the peripheral edge of the target assembly is higher than the middle height of the target assembly. The spliced target can meet the requirement of sputtering on the size of the target, and resource waste is avoided.
CN 111690903A discloses a target material secondary utilization method, comprising: providing a target assembly, wherein the target assembly comprises a back plate and a target to be recovered, the target to be recovered is connected with the back plate, a bombarded area is arranged on the target to be recovered, and the thickness of the bombarded area is smaller than that of other areas; processing a target material assembly to separate the back plate from the target material to be recovered; performing linear cutting on the target to be recovered according to the bombarded area, and cutting the target into a plurality of target blocks; splicing the target blocks into a new target, wherein the new target is provided with a continuous area with the thickness meeting the sputtering requirement; the new target is welded to the backing plate for secondary use.
The content disclosed above can improve the utilization rate of the target material, but for the splicing of large-size target materials, the splicing seam cannot be effectively regulated and controlled, and the quality of the coating film can be further influenced.
CN 106607667A discloses a method for manufacturing a target assembly, which includes: providing a target, a back plate and a protection plate, wherein the surface of the target for welding is a first welding surface, the surface opposite to the first welding surface is a sputtering surface, and the surface of the back plate for welding is a second welding surface; adhering the protective plate to the sputtering surface of the target material; welding the first welding surface of the target and the second welding surface of the back plate; in the welding process, the protective plate reduces thermal shock caused by mismatching of thermal expansion coefficients of the target and the back plate; and removing the protective plate after welding. Wherein the protective plate is adhered to the sputtering surface of the target material before the target material and the back plate are heated. The method can prevent the target material from being broken due to thermal shock, and can properly regulate and control the width of the splicing seam, but the welding combination rate of the back plate and the target material needs to be further improved.
Aiming at the defects of the prior art, a target welding method which is high in welding bonding rate and adjustable and controllable in splicing seam is needed.
Disclosure of Invention
The invention aims to provide a welding method of a spliced niobium target, which improves the welding combination rate of the niobium target and a back plate by carrying out pretreatment and infiltration treatment on the niobium target and the back plate; meanwhile, the splicing seam of the niobium target is adjustable and controllable by attaching the spacing strips, and the obtained spliced niobium target has high yield and can meet the requirement of sputtering use.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention provides a welding method of a spliced niobium target, which comprises the following steps:
(1) Preprocessing the welding surface of the back plate to obtain a preprocessed back plate;
(2) Sequentially carrying out pre-soaking treatment and fine soaking treatment on the pretreated back plate obtained in the step (1), and then attaching spacing bars to a welding surface to obtain a spacing back plate;
(3) Splicing the first niobium target, the second niobium target and the third niobium target on the spacing back plate obtained in the step (2) in sequence to enable the width of the spliced gap to be equal to that of the spacing bar; then, carrying out pressurization treatment to obtain the spliced niobium target;
the first niobium target, the second niobium target and the third niobium target in the step (3) are obtained by respectively and independently carrying out welding surface sand blasting and nickel plating treatment, and fine infiltration and coating treatment under heating;
the step (2) and the step (3) are carried out under heating.
According to the invention, the welding surfaces of the back plate and the niobium target have higher roughness by respectively carrying out pretreatment, sand blasting and nickel plating treatment on the back plate and the niobium target, so that the welding bonding rate can be effectively improved; the pre-infiltration treatment and the fine infiltration treatment are carried out on the pre-treated back plate, so that the infiltration effect with the treated back plate can be ensured; the niobium target is subjected to fine infiltration and then coating treatment, so that the infiltration degree can be further improved; the width of a splicing seam between the first niobium target, the second niobium target and the third niobium target is adjustable and controllable by attaching the spacing strip to the welding surface of the back plate; the niobium targets are pressurized, so that the welding bonding strength of the back plate and the niobium targets can be obviously improved, and the use requirement of sputtering is met.
Preferably, the backsheet of step (1) comprises an oxygen-free copper backsheet or a copper alloy backsheet.
Preferably, the pretreatment of step (1) comprises sand blasting and/or sanding.
The sand blasting treatment can form a sand layer on the welding surface of the back plate, so that the roughness is increased; the sanding may directly increase the roughness of the back sheet surface.
Preferably, the end point of the pretreatment of step (1) is such that the roughness of the bonding surface is between 5 and 10 μm, and may be, for example, 5 μm, 6 μm, 7 μm, 8 μm, 9 μm or 10 μm, but is not limited to the values recited, and other values not recited in the range of values are equally applicable.
Preferably, the solder used in the pre-wetting treatment and the fine wetting treatment in the step (2) comprises indium solder.
Preferably, the pre-soaking treatment in the step (2) is performed under the action of a steel brush.
Preferably, the fine infiltration treatment in the step (2) is performed under the action of ultrasonic waves.
The invention can effectively promote the solder to fully infiltrate the back plate by pre-infiltrating treatment and then fine infiltrating treatment, and prevent the solder from losing and overflowing during one-step infiltrating treatment, thereby reducing the infiltrating effect.
Preferably, the ultrasonic wave has a frequency of 20-25KHz, such as 20KHz, 21KHz, 22KHz, 23KHz, 24KHz or 25KHz, but not limited to the enumerated values, and other unrecited values in the numerical range are also applicable.
Preferably, the spacer bars of step (2) comprise polytetrafluoroethylene bars.
According to the invention, the spacer bars are attached to the welding surface of the back plate, so that the widths of splicing gaps among the first niobium target, the second niobium target and the third niobium target can be adjusted and controlled without introducing a partition plate to isolate the niobium targets of each part and subsequently drawing out the partition plate, the operation is simple, and the splicing gap is accurately adjusted and controlled.
Preferably, the medium for attaching in step (2) comprises heat-resistant adhesive tape.
When the heat-resistant adhesive tape is used, the spacer bars are required to be ensured not to deform or bend.
Preferably, the method further comprises the steps of removing an oxide layer and placing a metal wire after the step (2) of attaching the spacer and before the step (3) of splicing.
Preferably, the step of removing the oxide layer and placing the metal wire comprises: and removing an oxide layer on the welding surface of the back plate attached with the spacing bar, and then respectively placing metal wires at the splicing positions of the first niobium target, the second niobium target and the third niobium target.
The oxide layer is removed, so that the bonding degree during welding can be improved; the metal wire is placed at the splicing part, so that the polymerization degree of the welding flux can be improved, the uniformity and compactness of a welding flux layer are guaranteed, meanwhile, the metal wire can play a supporting role, the overflow rate of the welding flux is reduced when the niobium target is spliced with the back plate, and the welding combination rate is improved.
Preferably, the oxide layer comprises indium oxide.
Preferably, 5 to 6 wires, for example, 5 or 6 wires, are placed at equal distances at the joint of the first niobium target.
Preferably, 2 to 3 metal wires are respectively and equidistantly arranged at the splicing part of the second niobium target and the third niobium target, and the number of the metal wires can be 2 or 3.
Preferably, the wire has a diameter of 0.3 to 0.5mm, for example 0.3mm, 0.35mm, 0.4mm, 0.45mm or 0.5mm, but is not limited to the values recited, and other values not recited within the range of values are equally applicable.
Preferably, the metal wire comprises a copper wire.
Preferably, the length of the first niobium target in step (3) is greater than the length of the second niobium target and the third niobium target.
Preferably, the first niobium target is spliced at the center of the back plate, and the second niobium target and the third niobium target are spliced at two ends of the back plate.
And compacting the two ends of the first niobium target, the second niobium target and the third niobium target after splicing so as to ensure the accuracy that the width of a spliced gap is equal to that of the spacing bar.
Preferably, the size is adjusted by using calipers after splicing and before pressurization in the step (3).
Preferably, the step of pressurizing treatment of step (3) includes: placing 20-40kg of pressing blocks in the center of the first niobium target, and placing 5-15kg of pressing blocks at two ends; and 20-40kg of pressing blocks are placed in the centers of the second niobium target and the third niobium target.
Compared with the application of the same weight, the pressurization treatment of the invention can further improve the welding bonding strength of the niobium target and the back plate by applying different weights to different niobium targets, thereby meeting the use requirement of sputtering.
The first niobium target may have a centrally located 20-40kg compact, such as 20kg, 25kg, 30kg, 35kg or 40kg, but is not limited to the values recited, and other values not recited in the range of values are equally applicable.
5-15kg compacts, for example, 5kg, 8kg, 10kg, 12kg or 15kg, are placed on both ends of the first niobium target, but the invention is not limited to the recited values, and other values not recited in the range of values are also applicable.
The second niobium target and the third niobium target are centered on 20-40kg compacts, such as 20kg, 25kg, 30kg, 35kg or 40kg, but not limited to the recited values, and other values not recited in the range of values are also applicable.
The grit blasting is terminated at a roughness of 4 to 10 μm, for example 4, 5, 6, 8 or 10 μm, but is not limited to the values recited and other values not recited within the range of values are equally applicable.
Preferably, the time for the nickel plating treatment of the welding surface is 20-40min, for example, 20min, 25min, 30min, 35min or 40min, but is not limited to the values listed, and other values not listed in the numerical range are also applicable.
Preferably, the solution for nickel plating treatment of the welding surface comprises a mixed aqueous solution of hydrofluoric acid and nitric acid.
The nickel plating treatment can increase the wettability of brazing, thereby improving the welding qualification rate of the niobium target and the back plate.
Preferably, the coating liquid used for the coating process comprises liquid indium solder.
The niobium target is subjected to fine infiltration treatment and then is coated with the liquid indium solder, so that the infiltration effect of the niobium target can be further improved, and the subsequent welding combination rate with the back plate is ensured.
Preferably, the heating temperature is 210 to 250 ℃, for example 210 ℃, 220 ℃, 230 ℃, 240 ℃ or 250 ℃, but not limited to the recited values, and other values not recited within the numerical ranges are equally applicable.
Preferably, the heating is furnace cooled.
As a preferable aspect of the welding method of the present invention, the welding method includes the steps of:
(1) Pretreating the welding surface of the back plate until the roughness is 5-10 mu m to obtain a pretreated back plate;
(2) Sequentially carrying out steel brush pre-soaking treatment and 20-25KHz ultrasonic fine soaking treatment on the pretreated backboard obtained in the step (1) by adopting indium solder, and then attaching a spacing bar on a welding surface by adopting a heat-resistant adhesive tape; removing indium oxide on the welding surface, and then respectively placing metal wires at the splicing positions of the first niobium target, the second niobium target and the third niobium target to obtain a spacing back plate;
5-6 metal wires are arranged at the splicing position of the first niobium target at equal intervals; 2-3 metal wires are respectively arranged at the splicing positions of the second niobium target and the third niobium target at equal intervals; the diameter of the metal wire is 0.3-0.5mm;
(3) Splicing the first niobium target, the second niobium target and the third niobium target on the spacing back plate obtained in the step (2) in sequence to enable the width of the spliced gap to be equal to the width of the spacing bar; then, carrying out pressurization treatment to obtain the spliced niobium target;
the first niobium target, the second niobium target and the third niobium target are respectively and independently subjected to welding surface sand blasting until the roughness is 4-10 mu m, and nickel plating treatment is carried out on a mixed aqueous solution of hydrofluoric acid and nitric acid for 20-40min; then carrying out ultrasonic fine infiltration and liquid indium solder coating treatment under the heating of 210-250 ℃ to obtain the indium solder; the length of the first niobium target is greater than the length of the second niobium target and the third niobium target; the step of pressurizing treatment comprises: placing 20-40kg of pressing blocks in the center of the first niobium target, and placing 5-15kg of pressing blocks at two ends; placing 20-40kg of a compact in the center of the second niobium target and the third niobium target;
the step (2) and the step (3) are carried out under the heating of 210-250 ℃.
Compared with the prior art, the invention has the following beneficial effects:
according to the welding method of the spliced niobium target, provided by the invention, the welding combination rate of the back plate and the niobium target can reach 99.8% by carrying out pretreatment and infiltration treatment on the back plate and the niobium target; the width of a splicing gap between each part of niobium targets is adjustable and controllable by attaching the spacing strips to the welding surface of the back plate; the niobium targets of all parts are pressurized in different weights, so that the welding bonding strength of the back plate and the niobium targets is improved, and the bonding strength can reach 8.3MPa, thereby meeting the use requirement of sputtering.
Drawings
Fig. 1 is a schematic structural diagram of a spliced niobium target provided in example 1 of the present invention;
FIG. 2 is a schematic view of the pressurization treatment provided in example 1 of the present invention;
wherein: 1, a copper alloy backing plate; 2, tetrafluoroethylene strips; 3, a first niobium target; 4, a second niobium target; 5, a third niobium target.
Detailed Description
The technical solution of the present invention is further explained by the following embodiments. It should be understood by those skilled in the art that the examples are only for the understanding of the present invention and should not be construed as the specific limitation of the present invention.
Example 1
The embodiment provides a welding method for splicing a niobium target, which comprises the following steps:
(1) Carrying out sand blasting on the welding surface of the copper alloy backboard 1 until the roughness is 8 mu m to obtain a pretreated backboard;
(2) Sequentially carrying out steel brush pre-soaking treatment and 22KHz ultrasonic fine-soaking treatment on the pretreated back plate obtained in the step (1) by adopting indium solder, and then attaching polytetrafluoroethylene strips 2 to a welding surface by adopting a heat-resistant adhesive tape; removing indium oxide on the welding surface, and then respectively placing copper wires at the splicing positions of the first niobium target 3, the second niobium target 4 and the third niobium target 5 to obtain a spacing back plate;
5 copper wires are placed at the splicing position of the first niobium target 3 at equal intervals; 2 copper wires are respectively arranged at the splicing positions of the second niobium target 4 and the third niobium target 5 at equal intervals; the diameter of the copper wire is 0.4mm;
(3) Sequentially splicing a first niobium target 3, a second niobium target 4 and a third niobium target 5 on the spacing back plate obtained in the step (2) to enable the width of the spliced gap to be equal to that of the polytetrafluoroethylene strip 2; then, carrying out pressurization treatment, as shown in fig. 2, to obtain the spliced niobium target, wherein the structural schematic diagram is shown in fig. 1;
the first niobium target 3, the second niobium target 4 and the third niobium target 5 are respectively and independently subjected to welding surface sand blasting until the roughness is 6 mu m, and nickel plating treatment is carried out on a mixed aqueous solution of hydrofluoric acid and nitric acid for 30min; then heating at 230 ℃ and carrying out ultrasonic fine infiltration and liquid indium solder coating treatment to obtain the indium solder; the length of the first niobium target 3 is greater than the length of the second niobium target 4 and the third niobium target 5; the step of pressure treatment comprises: 30kg of compacts were placed in the center of the first niobium target 3, and 10kg of compacts were placed at both ends; placing 30kg of a pressing block in the centers of the second niobium target 4 and the third niobium target 5;
the step (2) and the step (3) are carried out under the heating of 230 ℃.
Example 2
The embodiment provides a welding method for splicing a niobium target, which comprises the following steps:
(1) Carrying out sand blasting on the welding surface of the copper alloy backboard 1 until the roughness is 9 mu m to obtain a pretreated backboard;
(2) Sequentially carrying out steel brush pre-soaking treatment and 21KHz ultrasonic fine soaking treatment on the pretreated backboard obtained in the step (1) by adopting indium solder, and then attaching polytetrafluoroethylene strips 2 to a welding surface by adopting a heat-resistant adhesive tape; removing indium oxide on the welding surface, and then respectively placing copper wires at the splicing positions of the first niobium target 3, the second niobium target 4 and the third niobium target 5 to obtain a spacing back plate;
5 copper wires are placed at the splicing position of the first niobium target 3 at equal intervals; 2 copper wires are respectively arranged at the splicing positions of the second niobium target 4 and the third niobium target 5 at equal intervals; the diameter of the copper wire is 0.45mm;
(3) Sequentially splicing a first niobium target 3, a second niobium target 4 and a third niobium target 5 on the spacing back plate obtained in the step (2) to enable the width of the spliced gap to be equal to that of the polytetrafluoroethylene strip 2; then, carrying out pressurization treatment to obtain the spliced niobium target;
the first niobium target 3, the second niobium target 4 and the third niobium target 5 are respectively and independently subjected to welding surface sand blasting until the roughness is 5 mu m, and nickel plating treatment is carried out on a mixed aqueous solution of hydrofluoric acid and nitric acid for 35min; then heating at 220 ℃ to perform ultrasonic fine infiltration and liquid indium solder coating treatment to obtain the indium solder; the length of the first niobium target 3 is greater than the length of the second niobium target 4 and the third niobium target 5; the step of pressure treatment comprises: placing a 35kg pressing block at the center of the first niobium target 3, and placing 12kg pressing blocks at the two ends; placing 35kg of compacts at the centers of the second niobium target 4 and the third niobium target 5;
the step (2) and the step (3) are carried out under the heating of 220 ℃.
Example 3
The embodiment provides a welding method for a spliced niobium target, which comprises the following steps:
(1) Carrying out sand blasting on the welding surface of the copper alloy backboard 1 until the roughness is 6 microns to obtain a pretreated backboard;
(2) Sequentially carrying out steel brush pre-soaking treatment and 24KHz ultrasonic fine soaking treatment on the pretreated backboard obtained in the step (1) by adopting indium solder, and then attaching polytetrafluoroethylene strips 2 to a welding surface by adopting a heat-resistant adhesive tape; removing indium oxide on the welding surface, and then respectively placing copper wires at the splicing positions of the first niobium target 3, the second niobium target 4 and the third niobium target 5 to obtain a spacing back plate;
5 copper wires are placed at the splicing position of the first niobium target 3 at equal intervals; 2 copper wires are respectively arranged at the splicing positions of the second niobium target 4 and the third niobium target 5 at equal intervals; the diameter of the copper wire is 0.35mm;
(3) Sequentially splicing a first niobium target 3, a second niobium target 4 and a third niobium target 5 on the spacing back plate obtained in the step (2) to enable the width of the spliced gap to be equal to that of the polytetrafluoroethylene strip 2; then, carrying out pressurization treatment to obtain the spliced niobium target;
the first niobium target 3, the second niobium target 4 and the third niobium target 5 are respectively and independently subjected to welding surface sand blasting until the roughness is 8 mu m, and nickel plating treatment is carried out on a mixed aqueous solution of hydrofluoric acid and nitric acid for 25min; then heating at 240 ℃ and carrying out ultrasonic fine infiltration and liquid indium solder coating treatment to obtain the indium solder; the length of the first niobium target 3 is greater than the length of the second niobium target 4 and the third niobium target 5; the step of pressure treatment comprises: placing 25kg of pressing blocks in the center of the first niobium target 3, and placing 8kg of pressing blocks at two ends; placing 25kg of compacts at the centers of the second niobium target 4 and the third niobium target 5;
the step (2) and the step (3) are carried out under the heating of 240 ℃.
Example 4
The embodiment provides a welding method for a spliced niobium target, which comprises the following steps:
(1) Carrying out sand blasting treatment on the welding surface of the copper alloy backboard 1 until the roughness is 10 mu m to obtain a pretreated backboard;
(2) Sequentially carrying out steel brush pre-soaking treatment and 20KHz ultrasonic fine-soaking treatment on the pretreated back plate obtained in the step (1) by adopting indium solder, and then attaching polytetrafluoroethylene strips 2 to a welding surface by adopting a heat-resistant adhesive tape; removing indium oxide on the welding surface, and then respectively placing copper wires at the splicing positions of the first niobium target 3, the second niobium target 4 and the third niobium target 5 to obtain a spacing back plate;
5 copper wires are placed at the splicing position of the first niobium target 3 at equal intervals; 2 copper wires are respectively arranged at the splicing positions of the second niobium target 4 and the third niobium target 5 at equal intervals; the diameter of the copper wire is 0.5mm;
(3) Sequentially splicing a first niobium target 3, a second niobium target 4 and a third niobium target 5 on the spacing back plate obtained in the step (2) to enable the width of the spliced gap to be equal to that of the polytetrafluoroethylene strip 2; then, carrying out pressurization treatment to obtain the spliced niobium target;
the first niobium target 3, the second niobium target 4 and the third niobium target 5 are respectively and independently subjected to welding surface sand blasting until the roughness is 4 mu m, and nickel plating treatment is carried out on a mixed aqueous solution of hydrofluoric acid and nitric acid for 40min; then carrying out ultrasonic fine infiltration and liquid indium solder coating treatment under the heating of 210 ℃ to obtain the indium solder; the length of the first niobium target 3 is greater than the length of the second niobium target 4 and the third niobium target 5; the step of pressurizing treatment comprises: placing 40kg of pressing blocks at the center of the first niobium target 3, and placing 15kg of pressing blocks at the two ends; placing 40kg of compacts at the centers of the second niobium target 4 and the third niobium target 5;
the step (2) and the step (3) are carried out under the heating of 210 ℃.
Example 5
The embodiment provides a welding method for splicing a niobium target, which comprises the following steps:
(1) Carrying out sand blasting on the welding surface of the copper alloy backboard 1 until the roughness is 5 mu m to obtain a pretreated backboard;
(2) Sequentially carrying out steel brush pre-soaking treatment and 25KHz ultrasonic fine soaking treatment on the pretreated backboard obtained in the step (1) by adopting indium solder, and then attaching polytetrafluoroethylene strips 2 to a welding surface by adopting a heat-resistant adhesive tape; removing indium oxide on the welding surface, and then respectively placing copper wires at the splicing positions of the first niobium target 3, the second niobium target 4 and the third niobium target 5 to obtain a spacing back plate;
5 copper wires are placed at the splicing position of the first niobium target 3 at equal intervals; 2 copper wires are respectively arranged at the splicing positions of the second niobium target 4 and the third niobium target 5 at equal intervals; the diameter of the copper wire is 0.3mm;
(3) Sequentially splicing a first niobium target 3, a second niobium target 4 and a third niobium target 5 on the spacing back plate obtained in the step (2) to enable the width of the spliced gap to be equal to that of the polytetrafluoroethylene strip 2; then, carrying out pressurization treatment to obtain the spliced niobium target;
the first niobium target 3, the second niobium target 4 and the third niobium target 5 are respectively and independently subjected to welding surface sand blasting until the roughness is 10 mu m, and nickel plating treatment is carried out on a mixed aqueous solution of hydrofluoric acid and nitric acid for 20min; then heating at 250 ℃ to perform ultrasonic fine infiltration and liquid indium solder coating treatment to obtain the indium solder; the length of the first niobium target 3 is greater than the length of the second niobium target 4 and the third niobium target 5; the step of pressure treatment comprises: placing 20kg of compacts at the center of the first niobium target 3 and 5kg of compacts at both ends; placing a 20kg pressing block in the centers of the second niobium target 4 and the third niobium target 5;
the step (2) and the step (3) are carried out under the heating of 250 ℃.
Example 6
This example provides a welding method of a spliced niobium target, which is different from example 1 in that it is the same as example 1 except that the sandblasting treatment described in step (1) is performed to a roughness of 3 μm.
Example 7
This example provides a welding method of a spliced niobium target, which is different from example 1 in that it is the same as example 1 except that the sandblasting treatment of step (1) is performed to a roughness of 12 μm.
Example 8
The embodiment provides a welding method for splicing niobium targets, which is different from the welding method in embodiment 1 in that 3 copper wires are equidistantly placed at the splicing position of the first niobium target 3 in the step (2); the splicing positions of the second niobium target 4 and the third niobium target 5 are respectively provided with 1 copper wire at equal intervals, and the rest is the same as that in the embodiment 1.
Example 9
The embodiment provides a welding method for splicing niobium targets, which is different from the welding method in embodiment 1 in that 8 copper wires are equidistantly placed at the splicing position of the first niobium target 3 in the step (2); the splicing positions of the second niobium target 4 and the third niobium target 5 are respectively provided with 5 copper wires at equal intervals, and the rest is the same as that in the embodiment 1.
Example 10
This example provides a welding method of a spliced niobium target, which differs from example 1 in that, except for the first niobium target 3 of step (3), 18kg of compacts are placed at the center and 3kg of compacts are placed at both ends; the same procedure as in example 1 was repeated except that 18kg of compacts were placed at the centers of the second niobium target 4 and the third niobium target 5.
Example 11
This example provides a welding method of a spliced niobium target, which is different from example 1 in that, except that 42kg of compacts are placed at the center and 18kg of compacts are placed at both ends of the first niobium target 3 in step (3); the same procedure as in example 1 was repeated except that 42kg of compacts were placed at the centers of the second niobium target 4 and the third niobium target 5.
Comparative example 1
This comparative example provides a welding method of a spliced niobium target, which differs from example 1 in that the blasting step described in step (1) is not performed, and the rest is the same as example 1.
Comparative example 2
This comparative example provides a welding method for spliced niobium targets, which differs from example 1 in that step (2) is a steel brush-free pre-wetting treatment step, and the rest is the same as example 1.
Comparative example 3
The comparative example provides a welding method of a spliced niobium target, and the welding method is different from the welding method of the example 1 in that the polytetrafluoroethylene strip 2 attached to the welding surface in the step (2) is adjusted to be used for welding a heat-resistant partition plate, the heat-resistant partition plate is removed after the pressurization treatment in the step (3), and the rest is the same as that of the example 1.
Comparative example 4
This comparative example provides a welding method of a spliced niobium target, which is different from example 1 in that no compacts are placed at both ends of the first niobium target 3 in step (3), and the rest is the same as example 1.
Comparative example 5
This comparative example provides a welding method of a spliced niobium target, which is different from example 1 in that the first niobium target 3, the second niobium target 4, and the third niobium target 5 in step (3) are not subjected to nickel plating treatment, and the rest is the same as example 1.
Comparative example 6
This comparative example provides a method of welding spliced niobium targets, which differs from example 1 in that the first niobium target 3, the second niobium target 4, and the third niobium target 5 of step (3) are free of liquid indium solder coating treatment, and the rest is the same as example 1.
Welding the copper alloy back plate and the niobium target according to the welding methods provided by the embodiments 1 to 11 and the comparative examples 1 to 6 to obtain a spliced niobium target, and detecting the welding bonding rate by using an ultrasonic C scanning imager, wherein the obtained results are shown in Table 1;
the copper alloy backing plate and the niobium target were welded according to the welding methods provided in examples 1 to 11 and comparative examples 1 to 6 to obtain a spliced niobium target, and a weld bonding strength test was performed using a tensile tester, and the results are shown in table 1.
TABLE 1
As can be seen from table 1, as can be seen from comparison between example 1 and examples 2 to 5, the welding bonding rate of the back plate and the niobium target of the spliced target material obtained by the welding method provided by the invention is high, and the bonding strength can meet the use requirement of sputtering;
as can be seen from comparison of example 1 with examples 6 and 7, when the back sheet is pretreated, the roughness of the welding surface is too small or too large, which reduces the bonding degree with the niobium target, and the bonding strength is also reduced, and thus the back sheet cannot be used in the sputtering technique; compared with the examples 8 and 9, the comparison of the example 1 and the examples 9 shows that the number of the copper wires placed on the welding surface has certain influence on the welding bonding rate, the number is small, the indium solder cannot be effectively polymerized, the supporting effect is reduced, the number is too large, and the adverse influence is brought to the bonding strength of the back plate and the niobium target; as is clear from comparison between example 1 and examples 10 and 11, when the weight of the niobium target subjected to the pressure treatment is small, the bonding rate between the back plate and the niobium target is low, and when the weight is large, the indium solder is squeezed excessively to cause a loss, thereby reducing the bonding rate and bonding strength of soldering;
as can be seen from comparison between example 1 and comparative example 1, the back sheet without pretreatment significantly reduces the welding bonding rate and bonding strength; as can be seen from comparison between example 1 and comparative example 2, the infiltration effect of the back sheet is reduced without the pre-immersion treatment, so that the bonding rate and strength are reduced during welding; compared with the comparative example 3, the embodiment 1 has the advantages that the heat-resistant partition plate is adopted to regulate and control the width of the splicing gap, the subsequent removal of the heat-resistant partition plate is complex, the gap width is easily influenced, and the welding bonding rate of the spliced niobium target is influenced; as can be seen from comparison between example 1 and comparative example 4, when no pressure is applied to both ends of the first niobium target, the welding degree of the niobium target and the respective portions of the backing plate is not uniform, resulting in a decrease in welding strength; as can be seen from the comparison between example 1 and comparative examples 5 and 6, the niobium target has reduced welding rate and bonding strength with the backing plate without nickel plating and coating.
In summary, according to the welding method for splicing the niobium target provided by the invention, the welding combination rate of the back plate and the niobium target can reach 99.8% by performing pretreatment and infiltration treatment on the back plate and the niobium target; the width of a splicing gap between each part of niobium targets is adjustable and controllable by attaching the spacing strips to the welding surface of the back plate; the niobium targets of all parts are pressurized in different weights, so that the welding bonding strength of the back plate and the niobium targets is improved, and the bonding strength can reach 8.3MPa, thereby meeting the use requirement of sputtering.
The above description is only for the specific embodiment of the present invention, but the protection scope of the present invention is not limited thereto, and it should be understood by those skilled in the art that any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are within the protection scope and the disclosure of the present invention.
Claims (10)
1. A welding method for splicing a niobium target is characterized by comprising the following steps:
(1) Preprocessing the welding surface of the back plate to obtain a preprocessed back plate;
(2) Sequentially carrying out pre-soaking treatment and fine soaking treatment on the pretreated back plate obtained in the step (1), and then attaching spacing bars to a welding surface to obtain a spacing back plate;
(3) Splicing the first niobium target, the second niobium target and the third niobium target on the spacing back plate obtained in the step (2) in sequence to enable the width of the spliced gap to be equal to that of the spacing bar; then, carrying out pressurization treatment to obtain the spliced niobium target;
the first niobium target, the second niobium target and the third niobium target in the step (3) are obtained by respectively and independently performing welding surface sand blasting and nickel plating treatment, and fine infiltration and coating treatment under heating;
the step (2) and the step (3) are carried out under heating.
2. The soldering method according to claim 1, wherein the back plate of step (1) comprises an oxygen-free copper back plate or a copper alloy back plate;
preferably, the pretreatment of step (1) comprises sand blasting and/or sanding;
preferably, the end point of the pretreatment in the step (1) is to make the roughness of the welding surface 5-10 μm.
3. The soldering method according to claim 1 or 2, wherein the solder used in the pre-wetting and the fine-wetting in step (2) comprises indium solder;
preferably, the pre-soaking treatment in the step (2) is carried out under the action of a steel brush;
preferably, the fine infiltration treatment in the step (2) is carried out under the action of ultrasonic waves;
preferably, the frequency of the ultrasonic wave is 20-25KHz.
4. The welding method of any of claims 1-3, wherein step (2) the spacer bars comprise polytetrafluoroethylene bars;
preferably, the medium for attaching in step (2) comprises heat-resistant adhesive tape.
5. The welding method according to any one of claims 1 to 4, wherein the step (2) of removing the oxide layer and placing the metal wires is further included after the step (2) of attaching the spacer and before the step (3) of splicing;
preferably, the step of removing the oxide layer and placing the metal wire comprises: and removing an oxide layer on the welding surface of the back plate attached with the spacing bar, and then respectively placing metal wires at the splicing positions of the first niobium target, the second niobium target and the third niobium target.
6. The soldering method according to claim 5, wherein the oxide layer comprises indium oxide;
preferably, 5-6 metal wires are placed at the splicing position of the first niobium target at equal intervals;
preferably, 2-3 metal wires are respectively arranged at the splicing positions of the second niobium target and the third niobium target at equal intervals;
preferably, the diameter of the wire is 0.3-0.5mm;
preferably, the metal wire comprises a copper wire.
7. The welding method of any of claims 1-6, wherein the length of the first niobium target of step (3) is greater than the length of the second niobium target and the third niobium target;
preferably, the step of pressurizing treatment of step (3) includes: placing 20-40kg of pressing blocks at the center of the first niobium target, and placing 5-15kg of pressing blocks at two ends of the first niobium target; and 20-40kg of pressing blocks are placed in the centers of the second niobium target and the third niobium target.
8. The welding method according to any one of claims 1 to 7, wherein the end point of the blasting of the welding face is such that the roughness of the welding face is 4 to 10 μm;
preferably, the time for the nickel plating treatment of the welding surface is 20-40min;
preferably, the solution for nickel plating treatment of the welding surface comprises a mixed aqueous solution of hydrofluoric acid and nitric acid;
preferably, the coating liquid used for the coating process comprises liquid indium solder.
9. Welding method according to any one of claims 1-8, characterised in that the temperature of the heating is 210-250 ℃.
10. Welding method according to any one of claims 1-9, characterized in that it comprises the steps of:
(1) Pretreating the welding surface of the back plate until the roughness is 5-10 mu m to obtain a pretreated back plate;
(2) Sequentially carrying out steel brush pre-soaking treatment and 20-25KHz ultrasonic fine soaking treatment on the pretreated backboard obtained in the step (1) by adopting indium solder, and then attaching a spacing bar on a welding surface by adopting a heat-resistant adhesive tape; removing indium oxide on the welding surface, and then respectively placing metal wires at the splicing positions of the first niobium target, the second niobium target and the third niobium target to obtain a spacing back plate;
5-6 metal wires are placed at the splicing position of the first niobium target at equal intervals; 2-3 metal wires are respectively arranged at the splicing position of the second niobium target and the third niobium target at equal intervals; the diameter of the metal wire is 0.3-0.5mm;
(3) Splicing the first niobium target, the second niobium target and the third niobium target on the spacing back plate obtained in the step (2) in sequence to enable the width of the spliced gap to be equal to the width of the spacing bar; then, carrying out pressurization treatment to obtain the spliced niobium target;
the first niobium target, the second niobium target and the third niobium target are respectively and independently subjected to welding surface sand blasting until the roughness is 4-10 mu m, and nickel plating treatment is carried out on a mixed aqueous solution of hydrofluoric acid and nitric acid for 20-40min; then carrying out ultrasonic fine infiltration and liquid indium solder coating treatment under the heating of 210-250 ℃ to obtain the indium solder; the length of the first niobium target is greater than the length of the second niobium target and the third niobium target; the step of pressure treatment comprises: placing 20-40kg of pressing blocks at the center of the first niobium target, and placing 5-15kg of pressing blocks at two ends of the first niobium target; placing 20-40kg of pressing blocks in the centers of the second niobium target and the third niobium target;
the step (2) and the step (3) are carried out under the heating of 210-250 ℃.
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