CN113510445A - Preparation method of niobium steel composite component - Google Patents
Preparation method of niobium steel composite component Download PDFInfo
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- CN113510445A CN113510445A CN202110647947.1A CN202110647947A CN113510445A CN 113510445 A CN113510445 A CN 113510445A CN 202110647947 A CN202110647947 A CN 202110647947A CN 113510445 A CN113510445 A CN 113510445A
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- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 title claims abstract description 126
- 239000010955 niobium Substances 0.000 title claims abstract description 112
- 229910052758 niobium Inorganic materials 0.000 title claims abstract description 112
- 229910000831 Steel Inorganic materials 0.000 title claims abstract description 107
- 239000010959 steel Substances 0.000 title claims abstract description 107
- 239000002131 composite material Substances 0.000 title claims abstract description 48
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 238000003466 welding Methods 0.000 claims abstract description 34
- 238000000034 method Methods 0.000 claims abstract description 28
- 238000001513 hot isostatic pressing Methods 0.000 claims abstract description 20
- 238000007789 sealing Methods 0.000 claims abstract description 14
- 230000007704 transition Effects 0.000 claims abstract description 12
- 238000004140 cleaning Methods 0.000 claims abstract description 8
- 238000004519 manufacturing process Methods 0.000 claims abstract description 8
- 229910001220 stainless steel Inorganic materials 0.000 claims description 20
- 239000010935 stainless steel Substances 0.000 claims description 20
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 18
- 229910052751 metal Inorganic materials 0.000 claims description 11
- 239000002184 metal Substances 0.000 claims description 11
- 238000005219 brazing Methods 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 9
- 238000003754 machining Methods 0.000 claims description 9
- 238000010894 electron beam technology Methods 0.000 claims description 7
- 239000010949 copper Substances 0.000 claims description 6
- 239000007789 gas Substances 0.000 claims description 6
- 229910000679 solder Inorganic materials 0.000 claims description 6
- 229910045601 alloy Inorganic materials 0.000 claims description 4
- 239000000956 alloy Substances 0.000 claims description 4
- 238000004381 surface treatment Methods 0.000 claims description 4
- 239000010936 titanium Substances 0.000 claims description 4
- 229910052719 titanium Inorganic materials 0.000 claims description 4
- 239000010963 304 stainless steel Substances 0.000 claims description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 3
- 229910000589 SAE 304 stainless steel Inorganic materials 0.000 claims description 3
- 229910052802 copper Inorganic materials 0.000 claims description 3
- 239000000843 powder Substances 0.000 claims description 3
- 239000002253 acid Substances 0.000 claims description 2
- 239000011248 coating agent Substances 0.000 claims description 2
- 238000000576 coating method Methods 0.000 claims description 2
- 229910052737 gold Inorganic materials 0.000 claims description 2
- 239000011261 inert gas Substances 0.000 claims description 2
- 150000002739 metals Chemical class 0.000 claims description 2
- 229910052750 molybdenum Inorganic materials 0.000 claims description 2
- 229910052759 nickel Inorganic materials 0.000 claims description 2
- 238000005498 polishing Methods 0.000 claims description 2
- 239000002994 raw material Substances 0.000 claims description 2
- 229910052709 silver Inorganic materials 0.000 claims description 2
- 229910052715 tantalum Inorganic materials 0.000 claims description 2
- 229910052721 tungsten Inorganic materials 0.000 claims description 2
- 229910052720 vanadium Inorganic materials 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- 229910052726 zirconium Inorganic materials 0.000 claims description 2
- 239000001307 helium Substances 0.000 description 10
- 229910052734 helium Inorganic materials 0.000 description 10
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 10
- 229910000619 316 stainless steel Inorganic materials 0.000 description 9
- 238000012545 processing Methods 0.000 description 8
- 230000001133 acceleration Effects 0.000 description 4
- 238000011161 development Methods 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 238000009792 diffusion process Methods 0.000 description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- 238000010276 construction Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- -1 304 Inorganic materials 0.000 description 1
- 229910002481 CuNiMn Inorganic materials 0.000 description 1
- 229910000576 Laminated steel Inorganic materials 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 230000005658 nuclear physics Effects 0.000 description 1
- 230000005433 particle physics related processes and functions Effects 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 230000008646 thermal stress Effects 0.000 description 1
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23P—METAL-WORKING NOT OTHERWISE PROVIDED FOR; COMBINED OPERATIONS; UNIVERSAL MACHINE TOOLS
- B23P15/00—Making specific metal objects by operations not covered by a single other subclass or a group in this subclass
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- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Pressure Welding/Diffusion-Bonding (AREA)
- Powder Metallurgy (AREA)
Abstract
The invention discloses a hot isostatic pressing preparation method of a niobium/steel composite part. The method comprises the following steps: A) preparation of niobium and steel parts: preparing niobium and steel parts with different thicknesses according to the requirements of products, and cleaning the surfaces of the niobium and steel parts; B) assembling: assembling the cleaned niobium and steel parts together; C) sealing and welding: sealing and welding under vacuum or atmosphere protection according to the structure of the niobium/steel composite part; D) hot isostatic pressing: and C), carrying out hot isostatic pressing treatment on the niobium/steel composite member subjected to sealing welding in the step C), and thus obtaining the niobium/steel composite member. The niobium/steel composite member has the advantages of controllable interface shape, uniform thickness of the transition layer, better interface shear strength than that of a niobium steel composite plate of a base body, capability of realizing free combination of niobium and steel with different thicknesses, simple production process, low cost and the like.
Description
Technical Field
The invention belongs to the technical field of radio frequency superconducting particle accelerators, is mainly used for a liquid helium tank of a radio frequency superconducting resonant cavity, and particularly relates to a method for preparing a niobium steel composite component for the radio frequency superconducting resonant cavity by adopting a hot isostatic pressing diffusion bonding technology.
Background
With the development of nuclear physics, high-energy particle physics, basic material science, and life science, there is an urgent need for high-energy and high-flux particle accelerators in humans. Compared with a normal-temperature resonant acceleration cavity, the resonant acceleration cavity adopting a Radio Frequency Superconducting (Superconducting Radio Frequency) technology has extremely low heat loss, high acceleration gradient and high beam stability, so that the resonant acceleration cavity can have a plurality of advantages in a long-pulse (continuous wave mode) and high-flow-intensity particle accelerator, and is favored by particle accelerator devices in the international leading-edge field.
When the superconducting cavity operates, the superconducting cavity needs to be soaked in liquid helium in a helium tank to ensure that the superconducting cavity has superconducting performance. Titanium with a thermal expansion coefficient close to that of niobium is used for processing most of the existing superconducting cavity helium tanks, but the defects of complicated welding process, difficult forming, high cost and the like limit the development of a new cavity type and increase the construction cost of an accelerator. In order to solve the problem, laboratories at home and abroad are always seeking a titanium substitute material for processing a helium tank of a superconducting cavity. The 316L stainless steel has the characteristics of low cost, simple welding process, easy forming and the like, and is adopted by a superconducting cavity in a large-scale superconducting linear accelerator which is operated internationally or some superconducting cavities in a development stage. However, the welding is challenged by the overlarge difference (1:2.6) between the thermal expansion coefficients of niobium and 316L stainless steel, and meanwhile, the vacuum leakage of the superconducting cavity is greatly risked under the dual actions of thermal stress accumulated in multiple 873K to 2K cold and heat cycles of the stainless steel helium tank and tuning force in a liquid helium environment. Therefore, if the stainless steel helium tank can be used for a long time, a proper welding method needs to be selected for connecting niobium and stainless steel.
At present, the niobium and the stainless steel are usually connected internationally by adopting a vacuum brazing and explosion welding method, when the size in the connection scheme is small (the inner diameter of a niobium pipe is less than 45mm), the niobium and the stainless steel prepared by the vacuum brazing method have high mechanical property, reliable vacuum property and low cost, and when the size is large (the inner diameter of the niobium pipe is more than 45mm), the thickness consistency of a welding seam is poor, so that the mechanical property and the vacuum property of the welding seam are poor, and the welding seam cannot stably work for a long time in a liquid helium environment. The niobium and stainless steel transition piece prepared by the explosive welding method has uneven bonding surface and is of a wavy structure, and the bonding surface of the transition piece has low shear strength due to the wavy structure.
Disclosure of Invention
The invention aims to provide a hot isostatic pressing preparation method of a niobium/steel composite piece. The niobium/steel composite part prepared by the method has the advantages of controllable interface shape, uniform thickness of the transition layer, superior interface shear strength to a matrix, adjustable thickness of niobium and steel layers, low comprehensive use cost and the like.
The preparation method of the niobium/steel composite part comprises 4 main steps of niobium and steel part preparation, assembly, seal welding and hot isostatic pressing diffusion welding, and comprises the following specific steps:
A) preparation of niobium and steel parts: preparing niobium and steel parts with corresponding sizes according to the requirements of products, and carrying out surface treatment on the niobium and steel parts;
B) assembling niobium and steel parts: assembling the cleaned niobium part and the steel part together;
C) sealing and welding niobium and steel parts: sealing and welding under vacuum or atmosphere protection according to the structure of the niobium/steel composite part;
D) hot isostatic pressing: and C), carrying out hot isostatic pressing treatment on the niobium/steel composite member subjected to sealing welding in the step C), and thus obtaining the niobium/steel composite member.
In step a) of the above method, the niobium or steel member may be in the form of powder, block, plate or tube. For example, niobium plates and steel plates can be adopted, wherein the thickness of the niobium plates and the steel plates can be adjusted, and the adjustable range of the niobium plates is 4-10 mm; the adjustable range of the steel plate is 10-50 mm.
The steel member may be a non-magnetic or weakly magnetic stainless steel, such as 304, 316L, 316 LN.
In the step A), the surface treatment comprises machining, mechanical polishing, acid washing and cleaning solution treatment such as alcohol, acetone and the like, so that the obtained smooth finish of the niobium and steel surface is 1.6-3.2 microns.
In step B), the assembling is to assemble the steel member and the niobium member to form a fit; such as a mosaic of tubes, holes, or a plate-plate stack.
In the step B), a metal transition layer (with the thickness of 0.05-1mm) can be added between the niobium and the steel part during the assembly; the raw material of the metal transition layer is at least one metal or an alloy formed by at least two metals: cu, Ni, Co, Ti, Ta, Zr, V, Ag, Au, W, Mo; the metal transition layer can be introduced by coating the surface of niobium or steel parts or directly adding an intermediate layer.
In the step C), the sealing method is selected from any one of the following methods: electron beam welding, vacuum brazing and sheathing.
The electron beam welding is to combine the niobium piece and the steel piece together and weld the edge joint between the combined pieces through the electron beam.
The vacuum brazing is to combine a steel piece and a niobium piece together, and perform vacuum brazing for 15-30 minutes (specifically, 15 minutes and 30 minutes) at 800-1050 ℃ (specifically, 800 ℃ and 1000 ℃); the adopted solder is Cu-based, Mn-based, Ag-based, Au-based or Ni-based solder.
The sheathing method is that niobium and steel are combined together and put into a sheathing, and the sheathing is vacuumized and sealed and welded at the room temperature to 1000 ℃ (specifically 200 ℃ and 700 ℃); the sheath is made of steel or copper or alloy thereof;
the atmosphere is provided by inert gas and/or reducing gas, specifically selected from Ar gas and H2Gas, N2Gas, CO, NH3One or more mixed gases;
in the step D), the hot isostatic pressing treatment is performed at a treatment temperature of 500 to 1300 ℃ (specifically, 500 ℃, 700 ℃, 900 ℃, 1070 ℃, 1000 ℃, 1300 ℃), at a treatment pressure of 5 to 200MPa (specifically, 5MPa, 60MPa, 100MPa, 140MPa, 200MPa), and for a treatment time of 2 to 3 hours.
Aiming at the problems in the prior art, the invention realizes the preparation of the niobium-316L composite board by hot isostatic pressing diffusion welding, so that the niobium and stainless steel have reliable vacuum performance and mechanical performance when connected, the welding cost of the niobium and stainless steel can be reduced, the connection scheme of the niobium and stainless steel can be simplified, the stainless steel helium tank can be engineered, the development of a new cavity type is promoted, and the construction cost of an accelerator is reduced.
The niobium/steel composite member has the advantages of controllable interface shape, uniform thickness of the transition layer, better interface shear strength than that of a niobium steel composite plate of a base body, capability of realizing free combination of niobium and steel with different thicknesses, simple production process, low cost and the like.
Drawings
FIG. 1 shows the interfacial morphology of the niobium steel composite part prepared in example 1.
FIG. 2 shows the microstructure of the interface of the niobium steel composite part prepared in example 5.
Detailed Description
The present invention will be further illustrated with reference to the following specific examples, but the present invention is not limited to the following examples. The method is a conventional method unless otherwise specified. The starting materials are commercially available from the open literature unless otherwise specified.
The method for measuring the interfacial strength of the niobium/steel composite member in the following examples was performed according to the regulations in the test method for mechanical and processing properties of the composite steel sheet (GB/T6369-2008).
Example 1: preparation of niobium/steel composite components
Processing a niobium plate with the size of 400mm x 5mm and a 316L stainless steel plate with the size of 400mm x 18mm to the surface smoothness of 3.2 microns, cleaning the surfaces of the niobium plate and the steel plate by using alcohol and acetone, then overlapping the niobium plate and the steel plate together, placing CuNiMn solder on the edge of the bonding surface of the niobium/steel plate, placing the assembled welding part into a vacuum brazing furnace, preserving the temperature for 30 minutes at the temperature of 1000 ℃, then carrying out hot isostatic pressing treatment on the brazed niobium/steel plate for 2 hours at the temperature of 500 ℃ and 200MPa, and machining to obtain the niobium/steel composite part. The niobium/steel composite member prepared by the process has the interface shear strength of 180MPa, and the interface microstructure is shown in figure 1. As can be seen from fig. 1, the interface is a flat structure.
Example 2: preparation of niobium/steel composite components
Processing a niobium plate with the size of 500mm x 300mm x 4mm and a 304 stainless steel plate with the size of 500mm x 300mm x 20mm to the surface smoothness of 3.2 microns, cleaning the surfaces of the niobium plate and the steel plate by using alcohol and acetone, then overlapping the niobium part and the steel part together, placing Ag-28Cu solder on the edge of the bonding surface of the niobium/steel part, placing the assembled welding part into a vacuum brazing furnace, preserving the heat at the temperature of 800 ℃ for 20 minutes, then carrying out hot isostatic pressing treatment on the brazed niobium/steel part at the temperature of 700 ℃ and the pressure of 90MPa for 2 hours, and machining to obtain the niobium/steel composite part. The interfacial shear strength of the niobium/steel composite member prepared by the process is 205 MPa.
Example 3: preparation of niobium/steel composite components
A niobium sheet having a size of 350mm x 300mm x 5mm and a 316L stainless steel sheet having a size of 350mm x 300mm x 20mm were processed to a surface finish of 1.6 μm, and the surfaces thereof were cleaned with alcohol and acetone, and then a niobium piece and a steel piece were laminated, wherein the surface of the niobium piece in contact with the steel piece was plated with a Ta-Zr layer having a thickness of 5 to 20 μm, and the edges of the laminated steel piece and niobium piece were welded by electron beam. And welding the niobium/steel composite piece which is packaged by the electron beam, carrying out hot isostatic pressing treatment for 3h at 1300 ℃ and 5MPa, and machining to obtain the niobium steel composite component. The interface shear strength of the niobium steel composite member prepared by the process is 245 Mpa.
Example 4: preparation of niobium/steel composite components
Niobium plates of 600mm x 300mm x 8mm size and 316 stainless steel plates of 600mm x 300mm x 25mm size were machined to a surface finish of 1.6 microns and 0.05mm ni layers were electroless plated on the surface of the niobium part to be clad with the steel. Then, the surfaces thereof were cleaned with alcohol and acetone, and the niobium member and the steel member plated with 0.05mm ni layer were laminated together. At Ar + H2Keeping the temperature at 600 ℃ for 90 minutes under the protection of CO mixed atmosphere(ii) a Welding two ends of the niobium and steel parts together by adopting electron beam welding, carrying out hot isostatic pressing treatment on the welded niobium/steel part for 2 hours at 1070 ℃ and 30MPa, and machining to obtain the niobium/steel composite component. The interfacial shear strength of the niobium/steel composite member prepared by the process parameters is 285 Mpa.
Example 5: preparation of niobium/steel composite components
Processing a niobium plate with the size of 200mm x 6mm and a 316L stainless steel plate with the size of 200mm x 17mm to the surface smoothness of 3.2 microns, cleaning the surfaces of the niobium plate and the steel plate by using alcohol and acetone, then overlapping the niobium part and the steel part together, adding a 0.05mm Cu sheet between the niobium part and the steel part, putting the niobium part and the steel part into a sheath made of 20# steel, vacuumizing for 8h at 300 ℃, sealing, welding the niobium/steel part sheath, performing hot isostatic pressing treatment for 4h at 1000 ℃ and 120MPa, removing the sheath, and machining to obtain the niobium/steel composite member. The interface shear strength of the niobium/steel composite member prepared by the process is 198Mpa, and the interface microstructure is shown in figure 2. As can be seen from FIG. 2, the interface is a flat structure and the thickness of the copper layer is uniform.
Example 6: preparation of niobium/steel composite components
Processing a niobium plate with the size of 200mm x 6mm and a 304 stainless steel plate with the size of 200mm x 17mm to the surface smoothness of 1.6 microns, cleaning the surfaces of the niobium plate and the steel plate by using alcohol and acetone, then overlapping the niobium part and the steel part together, putting the niobium part and the steel part into a sheath made of 20# steel, vacuumizing for 8 hours at 300 ℃, sealing and welding the niobium/steel part sheath, performing hot isostatic pressing treatment for 4 hours at 1000 ℃ and 150MPa, removing the sheath, and machining to obtain the niobium/steel composite member. The interfacial shear strength of the niobium/steel composite member prepared by the process is 263 Mpa.
Example 7: preparation of niobium/steel composite components
Processing a niobium plate with the size of 200mm x 6mm to the surface smoothness of 1.6 microns, plating a W-Mo-Fe layer with the thickness of 8 microns on the niobium surface, cleaning the surface of the niobium plate by using alcohol and acetone, filling the niobium plate into a sheath made of 20# steel, filling 316L stainless steel powder into the sheath, vacuumizing at room temperature for 2 hours, sealing and welding, performing hot isostatic pressing treatment at the temperature of 1030 ℃ and the pressure of 80MPa for 4 hours, removing the sheath, and machining to obtain the niobium/steel composite member. The niobium/steel composite member prepared by the process parameters has the interface shear strength of 216 MPa.
Claims (9)
1. A method of making a niobium/steel composite part, comprising the steps of:
A) preparation of niobium and steel parts: preparing niobium and steel parts with corresponding sizes according to the requirements of products, and carrying out surface treatment on the niobium and steel parts;
B) assembling: assembling the cleaned niobium part and the steel part together;
C) sealing and welding: sealing and welding under vacuum or atmosphere protection according to the structure of the niobium/steel composite part;
D) hot isostatic pressing: and C), carrying out hot isostatic pressing treatment on the niobium/steel composite member subjected to sealing welding in the step C).
2. The method of claim 1, wherein: in the step A), the niobium and steel parts are in the form of powder, blocks, plates or pipes.
3. The production method according to claim 1 or 2, characterized in that: the steel part is non-magnetic or weak magnetic stainless steel, including 304 stainless steel, 316L stainless steel and 316LN stainless steel.
4. The production method according to claim 1 or 2, characterized in that: in the step 1), the surface treatment comprises machining, mechanical polishing, acid washing and alcohol and acetone cleaning solution treatment, so that the obtained smooth finish of the niobium and steel surfaces is 1.6-3.2 microns.
5. The production method according to any one of claims 1 to 4, characterized in that: in the step B), a metal transition layer is added between the niobium and the steel part during the assembly, and the thickness of the metal transition layer is 0.05-1 mm; the raw material of the metal transition layer is at least one metal or an alloy formed by at least two metals: cu, Ni, Co, Ti, Ta, Zr, V, Ag, Au, W, Mo; the metal transition layer is introduced by coating the surface of niobium or steel parts or directly adding an intermediate layer.
6. The production method according to any one of claims 1 to 5, characterized in that: in the step C), the sealing welding method is selected from any one of the following methods: electron beam welding, vacuum brazing and sheathing;
the atmosphere is provided by inert gas and/or reducing gas, specifically selected from Ar gas and H2Gas, N2Gas, CO, NH3One or more mixed gases.
7. The method of claim 6, wherein:
the vacuum brazing is to combine a steel piece and a niobium piece together and perform vacuum brazing for 15-30 minutes at 800-1050 ℃; the adopted solder is Cu-based, Mn-based, Ag-based, Au-based or Ni-based solder;
the sheath method is that niobium and steel are combined together and put into a sheath, and the sheath is vacuumized at room temperature to 1000 ℃ and sealed and welded; the sheath is made of steel or copper or an alloy thereof.
8. The production method according to any one of claims 1 to 7, characterized in that: in the step D), the hot isostatic pressing treatment is carried out at the treatment temperature of 500-1300 ℃, the treatment pressure of 5-200 MPa and the treatment time of 2-3 hours.
9. A niobium/steel composite part produced by the method of any one of claims 1 to 8.
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Cited By (1)
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| CN115007988A (en) * | 2022-07-20 | 2022-09-06 | 钢研昊普科技有限公司 | Copper alloy-steel composite cylindrical part and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115007988A (en) * | 2022-07-20 | 2022-09-06 | 钢研昊普科技有限公司 | Copper alloy-steel composite cylindrical part and preparation method thereof |
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Application publication date: 20211019 |