CN109604804A - A kind of connector and the connection method of copper and niobium - Google Patents

A kind of connector and the connection method of copper and niobium Download PDF

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Publication number
CN109604804A
CN109604804A CN201811549784.8A CN201811549784A CN109604804A CN 109604804 A CN109604804 A CN 109604804A CN 201811549784 A CN201811549784 A CN 201811549784A CN 109604804 A CN109604804 A CN 109604804A
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China
Prior art keywords
niobium
copper
silver
connection
layer
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Pending
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CN201811549784.8A
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Chinese (zh)
Inventor
胡胜鹏
付伟
李绵绵
宋晓国
卞红
冯吉才
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Harbin Institute of Technology Weihai
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Harbin Institute of Technology Weihai
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Priority to CN201811549784.8A priority Critical patent/CN109604804A/en
Publication of CN109604804A publication Critical patent/CN109604804A/en
Pending legal-status Critical Current

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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B23MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23KSOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K20/00Non-electric welding by applying impact or other pressure, with or without the application of heat, e.g. cladding or plating
    • B23K20/02Non-electric welding by applying impact or other pressure, with or without the application of heat, e.g. cladding or plating by means of a press ; Diffusion bonding
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B23MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23KSOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K20/00Non-electric welding by applying impact or other pressure, with or without the application of heat, e.g. cladding or plating
    • B23K20/02Non-electric welding by applying impact or other pressure, with or without the application of heat, e.g. cladding or plating by means of a press ; Diffusion bonding
    • B23K20/023Thermo-compression bonding
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B23MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23KSOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K20/00Non-electric welding by applying impact or other pressure, with or without the application of heat, e.g. cladding or plating
    • B23K20/16Non-electric welding by applying impact or other pressure, with or without the application of heat, e.g. cladding or plating with interposition of special material to facilitate connection of the parts, e.g. material for absorbing or producing gas
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B23MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23KSOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K20/00Non-electric welding by applying impact or other pressure, with or without the application of heat, e.g. cladding or plating
    • B23K20/24Preliminary treatment

Abstract

The present invention relates to the manufacture technology fields of copper niobium superconductor cavity, connector and the connection method of specifically a kind of copper and niobium, it is characterized in that the connector by copper sheet, silver-colored middle layer and niobium board group at, the upper and lower ends of the silver-colored middle layer are connected with copper sheet and niobium plate respectively, the connection method includes the following steps: (one), polishing to joint face to niobium plate and copper sheet, fresh metal surface is obtained, and is cleaned by ultrasonic with acetone or alcohol;(2), eutectic reaction can be occurred with copper by choosing, and the metallic silver of solid solution is capable of forming with niobium, as middle layer;(3), niobium plate, silver-colored middle layer and copper sheet are fitted together, it is put into heating furnace, pressurization, it vacuumizes, then heating is attached, it is taken out after cooling and obtains niobium silver-bearing copper connector, have many advantages, such as that method simply, using silver is used as middle layer connection copper and niobium, realizes connection at a lower temperature, guarantees connector with good intensity and deformability.

Description

A kind of connector and the connection method of copper and niobium
Technical field
It is specifically a kind of to be connected using silver as middle layer the present invention relates to the manufacture technology field of copper niobium superconductor cavity Copper and niobium, realization connect at a lower temperature, guarantee that connector has the connection of copper and niobium of good intensity and deformability Part and connection method.
Background technique
It is well known that metal niobium has excellent low-temperature superconducting performance, it is the critical component material in Superconducting cavity LINAC, so And the cost of niobium is high, and thermal coefficient is lower, only 53.7 W/ (mK), in order to guarantee its good working order, needs To be combined with the copper (386 W/ (mK)) with high thermal conductivity coefficient, copper niobium chamber more and more attention has been paid to.
Currently, existing document " development and preliminary experiment of the low β superconductor cavity of copper niobium sputtering type, Hao Jiankui, Zhao's a one-legged monster in fable, Zhang Bao Clear, Xie great Lin, Wang Lifang are all-victorious literary, Shen Zilin, Tang Yuxing, Zhang Yunchi, Yang Xi, Hu Yanle, Zhao Kun high-energy physics and core object 2001,25 (6) of reason: 582-587 " discloses a kind of method for sputtering one layer of niobium film on copper chamber surface, and this method is difficult to obtain Niobium film fine and close and in homogeneous thickness, on the other hand guarantee is very difficult with good adhesion between the two, because copper/ Niobium system is in the positive enthalpy of formation, and there are larger differences between density, fusing point and crystal structure, in equilbrium phase diagram, either liquid Or solid phase, mutual solubility is limited, and existing method is it is difficult to ensure that the bonding strength and copper niobium chamber of copper and niobium have well in a word Performance.
Summary of the invention
Present invention aim to address above-mentioned the deficiencies in the prior art, provide it is a kind of using silver as middle layer connection copper and Niobium, realization connect at a lower temperature, guarantee connector have the copper of good intensity and deformability and the connector of niobium and Connection method.
The technical solution adopted by the present invention to solve the technical problems is:
A kind of connector of copper and niobium, it is characterised in that the connector is by copper sheet, silver-colored middle layer and niobium board group in the silver The upper and lower ends of interbed are connected with copper sheet and niobium plate respectively, the silver-colored middle layer with a thickness of 6 ~ 120 μm.
Further, niobium plate described above with a thickness of 0.5mm ~ 5mm, the copper sheet with a thickness of 8mm ~ 20mm.
A kind of connection method of copper and niobium, it is characterised in that the connection method includes the following steps:
(1), polishing to joint face to niobium plate and copper sheet, obtains fresh metal surface, and with acetone or alcohol ultrasound Cleaning;
(2), eutectic reaction can be occurred with copper by choosing, and the metallic silver of solid solution is capable of forming with niobium, as middle layer;
(3), niobium plate, silver-colored middle layer and copper sheet are fitted together, are put into heating furnace, pressurizeed, vacuumize, then heat into Row connection takes out after cooling and obtains niobium silver-bearing copper connector.
Further, the roughness of the fresh metal surface finally obtained in step described above (one) is less than 5 μm.
Further, the mode that silver-colored middle layer is introduced in step described above (two) is silver powder, silver foil piece, silvering.
Further, the axial compressive force applied in step described above (three) to niobium plate and copper sheet sub-assembly is 2 ~ 25 MPa。
Further, vacuum degree is 6 × 10 in furnace chamber in connection procedure in step described above (three)-3 ~ 8 × 10-4 Pa。
Further, heating process is to be heated to first with the rate of 5 ~ 30 oC/min in step described above (three) 700 ~ 750 oC keep the temperature 20 ~ 60 min, are then heated to 800 ~ 950 oC with the rate of 5 ~ 20 oC/min, keep the temperature 30 ~ 90 min are finally down to room temperature with the rate of 5 ~ 10 oC/min.
Further, heating process is to be heated to 750 first with the rate of 15 oC/min in step described above (three) OC keeps the temperature 50 min, is then heated to 850 oC with the rate of 10 oC/min, 70 min is kept the temperature, finally with the speed of 5 oC/min Rate is down to room temperature.
The beneficial effects of the present invention are as follows: silver-colored and copper be total on the one hand is utilized as middle layer connection copper and niobium using silver Crystalline substance reaction, can realize connection at a lower temperature, meanwhile, silver-bearing copper eutectic structure can be obtained after cooling;On the other hand, silver and niobium Solid solution structure can be formed, then brittle intermetallic compound phase is not present in entire jointing, it is ensured that connector With good intensity and deformability, there is method simply, using silver as middle layer to connect copper and niobium, realization lower At a temperature of connection, guarantee connector have many advantages, such as good intensity and deformability.
Detailed description of the invention
Fig. 1 is structural schematic diagram of the invention.
Specific embodiment
The following further describes the present invention with reference to the drawings:
As shown in the picture, the connector of a kind of copper and niobium, it is characterised in that the connector is by copper sheet, silver-colored middle layer and niobium board group At, the upper and lower ends of the silver-colored middle layer are connected with copper sheet and niobium plate respectively, the niobium plate with a thickness of 0.5mm ~ 5mm, the copper sheet with a thickness of 8mm ~ 20mm, the silver-colored middle layer with a thickness of 6 ~ 120 μm, under connection method includes State step: (one), polishing to joint face to niobium plate and copper sheet obtains fresh metal surface, the fresh metal of acquisition The roughness on surface is cleaned by ultrasonic less than 5 μm, and with acetone or alcohol;(2), eutectic reaction can be occurred with copper by choosing, with Niobium is capable of forming the metallic silver of solid solution, and as middle layer, the mode for introducing silver-colored middle layer is silver powder, silver foil piece, silvering Or other modes;(3), niobium plate, silver-colored middle layer and copper sheet are fitted together, is put into heating furnace, pressurizes, to niobium plate and copper The axial compressive force that board group component applies is 2 ~ 25 MPa, is vacuumized, and vacuum degree is 6 × 10 in furnace chamber in connection procedure-3 ~ 8 × 10-4Pa, then heating is attached, and is heated to 700 ~ 750 oC first with the rate of 5 ~ 30 oC/min, is kept the temperature Then 20 ~ 60 min are heated to 800 ~ 950 oC with the rate of 5 ~ 20 oC/min, keep the temperature 30 ~ 90 min, finally It is down to room temperature with the rate of 5 ~ 10 oC/min, is taken out after cooling and obtains niobium silver-bearing copper connector, bending resistance survey is carried out to connector Examination, niobium plate are used as outside, and Bend diameter is 24 mm, and bending angle reaches 60o, and Extrude Face and joint face be not cracked.
Embodiment 1:
Take the copper sheet with a thickness of 8mm and the niobium plate with a thickness of 1mm as connecting material, use with a thickness of 100 μm silver foil piece as Middle layer.It is successively polished to connection surface with 1000#, 1200#, 1500# SiC sand paper copper sheet and niobium plate, until surface Roughness is 3 μm.It is put into acetone and is cleaned by ultrasonic 10min, take out and air-dry.According to copper sheet/silver foil piece/niobium plate sequence, from upper Under fit together.Workpiece to be connected is put into heating furnace, 10MPa axial compressive force is applied to workpiece by upper push-down head.It closes Closed furnace door, is evacuated to 5 × 10-3Pa.Then 750 oC are heated to the rate of 20 oC/min, keep the temperature 30 min, then 850 oC are heated to the rate of 10 oC/min, 60 min is kept the temperature, room temperature is finally down to the rate of 5 oC/min, obtains niobium Silver-bearing copper connector, Extrude Face and joint face be not cracked when connector bending angle reaches 60o.
Embodiment 2:
It takes the copper sheet with a thickness of 8mm and the niobium plate with a thickness of 2mm as connecting material, successively uses 1000#, 1200#, 1500# SiC sand paper is polished to connection surface copper sheet and niobium plate, until surface roughness is 3 μm.It is put into acetone and is cleaned by ultrasonic 10min takes out and air-dries.80 μ m-thicks are spread between copper sheet and niobium plate, the Argent grain that average grain diameter is 20 μm.It will work be connected Part is put into heating furnace, applies 25MPa axial compressive force to workpiece by upper push-down head.Fire door is closed, is evacuated to 5 × 10-3 Pa.Then 750 oC are heated to the rate of 20 oC/min, keep the temperature 40 min, is then heated to the rate of 10 oC/min 850 oC keep the temperature 60 min, are finally down to room temperature with the rate of 10 oC/min, obtain niobium silver-bearing copper connector, connector bending angle Extrude Face and joint face be not cracked when degree reaches 60o.
Embodiment 3:
It takes the copper sheet with a thickness of 8mm and the niobium plate with a thickness of 1mm as connecting material, successively uses 1000#, 1200#, 1500# SiC sand paper is polished to connection surface copper sheet and niobium plate, until surface roughness is 2 μm.It is put into acetone and is cleaned by ultrasonic 10min takes out and air-dries.Using magnetron sputtering technique, 20 μm and 20 μm are deposited respectively to connection surface in copper and niobium plate Silver layer.According to copper sheet (silvered face)/(silvered face) niobium plate sequence, fit together from top to bottom.Workpiece to be connected is put into and is added In hot stove, 20MPa axial compressive force is applied to workpiece by upper push-down head.Fire door is closed, 3 × 10-3 Pa is evacuated to.Then 750 oC are heated to the rate of 15 oC/min, 50 min is kept the temperature, 850 oC is then heated to the rate of 10 oC/min, are protected 70 min of temperature, are finally down to room temperature with the rate of 5 oC/min, obtain niobium silver-bearing copper connector, connector bending angle reaches 60o When Extrude Face and joint face it is not cracked.
Embodiment 4:
It takes with a thickness of the copper sheet of 10mm and the niobium plate of thickness 3mm as connecting material, successively uses 1000#, 1200#, 1500# SiC Sand paper is polished to connection surface copper sheet and niobium plate, until surface roughness is 4 μm.It is put into acetone and is cleaned by ultrasonic 10min takes out and air-dries.Using magnetron sputtering technique, in the silver for depositing 8 μm and 3 μm respectively to connection surface of copper and niobium plate Layer.According to copper sheet (silvered face)/(silvered face) niobium plate sequence, fit together from top to bottom.Workpiece to be connected is put into heating In furnace, 20MPa axial compressive force is applied to workpiece by upper push-down head.Fire door is closed, 3 × 10-3 Pa is evacuated to.Then with The rate of 15 oC/min is heated to 750 oC, keeps the temperature 50 min, is then heated to 850 oC with the rate of 10 oC/min, keeps the temperature 70 min are finally down to room temperature with the rate of 5 oC/min, niobium silver-bearing copper connector are obtained, when connector bending angle reaches 60o Extrude Face and joint face be not cracked.
Embodiment 5:
It takes the copper sheet with a thickness of 20mm and the niobium plate with a thickness of 0.5mm as connecting material, successively uses 1000#, 1200#, 1500# SiC sand paper is polished to connection surface copper sheet and niobium plate, until surface roughness is 1 μm.It is put into acetone and is cleaned by ultrasonic 10min takes out and air-dries.50 μ m-thicks are spread between copper sheet and niobium plate, the Argent grain that average grain diameter is 20 μm.It will work be connected Part is put into heating furnace, applies 20MPa axial compressive force to workpiece by upper push-down head.Fire door is closed, 3 × 10-3 is evacuated to Pa.Then 750 oC are heated to the rate of 15 oC/min, keep the temperature 50 min, is then heated to the rate of 10 oC/min 850 oC keep the temperature 70 min, are finally down to room temperature with the rate of 5 oC/min, obtain niobium silver-bearing copper connector, connector bending angle Extrude Face and joint face be not cracked when degree reaches 60o.
Embodiment 6:
It takes the copper sheet with a thickness of 8mm and the niobium plate with a thickness of 5mm as connecting material, uses the silver foil piece with a thickness of 6 μm in Interbed.It is successively polished to connection surface with 1000#, 1200#, 1500# SiC sand paper copper sheet and niobium plate, until surface is thick Rugosity is 3 μm.It is put into acetone and is cleaned by ultrasonic 10min, take out and air-dry.According to copper sheet/silver foil piece/niobium plate sequence, from top to bottom It fits together.Workpiece to be connected is put into heating furnace, 10MPa axial compressive force is applied to workpiece by upper push-down head.It closes Fire door is evacuated to 5 × 10-3Pa.Then 750 oC are heated to the rate of 20 oC/min, keep the temperature 30 min, then with The rate of 10 oC/min is heated to 850 oC, keeps the temperature 60 min, is finally down to room temperature with the rate of 5 oC/min, obtains niobium silver Copper connector, Extrude Face and joint face be not cracked when connector bending angle reaches 60o.
Embodiment 7:
Take the copper sheet with a thickness of 15mm and the niobium plate with a thickness of 3mm as connecting material, with the silver foil piece work with a thickness of 120 μm For middle layer.It is successively polished to connection surface with 1000#, 1200#, 1500# SiC sand paper copper sheet and niobium plate, until table Surface roughness is 3 μm.It is put into acetone and is cleaned by ultrasonic 10min, take out and air-dry.Sequentially according to copper sheet/silver foil piece/niobium plate, from upper It is fitted together under and.Workpiece to be connected is put into heating furnace, 10MPa axial compressive force is applied to workpiece by upper push-down head. Fire door is closed, is evacuated to 5 × 10-3Pa.Then 750 oC are heated to the rate of 20 oC/min, keep the temperature 30 min, so 850 oC are heated to the rate of 10 oC/min afterwards, 60 min is kept the temperature, room temperature is finally down to the rate of 5 oC/min, is obtained Niobium silver-bearing copper connector, Extrude Face and joint face be not cracked when connector bending angle reaches 60o.
Embodiment 8:
Take the copper sheet with a thickness of 8mm and the niobium plate with a thickness of 3mm as connecting material, use with a thickness of 15 μm silver foil piece as Middle layer.It is successively polished to connection surface with 1000#, 1200#, 1500# SiC sand paper copper sheet and niobium plate, until surface Roughness is 3 μm.It is put into acetone and is cleaned by ultrasonic 10min, take out and air-dry.According to copper sheet/silver foil piece/niobium plate sequence, from upper Under fit together.Workpiece to be connected is put into heating furnace, 10MPa axial compressive force is applied to workpiece by upper push-down head.It closes Closed furnace door, is evacuated to 5 × 10-3Pa.Then 750 oC are heated to the rate of 20 oC/min, keep the temperature 30 min, then 850 oC are heated to the rate of 10 oC/min, 60 min is kept the temperature, room temperature is finally down to the rate of 5 oC/min, obtains niobium Silver-bearing copper connector, Extrude Face and joint face be not cracked when connector bending angle reaches 60o.

Claims (9)

1. the connector of a kind of copper and niobium, it is characterised in that the connector is by copper sheet, silver-colored middle layer and niobium board group at the silver The upper and lower ends of middle layer are connected with copper sheet and niobium plate respectively, the silver-colored middle layer with a thickness of 6 ~ 120 μm.
2. the connector of a kind of copper and niobium according to claim 1, it is characterised in that the niobium plate with a thickness of 0.5mm ~ 5mm, the copper sheet with a thickness of 8mm ~ 20mm.
3. the connection method of a kind of copper and niobium, it is characterised in that the connection method includes the following steps:
(1), polishing to joint face to niobium plate and copper sheet, obtains fresh metal surface, and with acetone or alcohol ultrasound Cleaning;
(2), eutectic reaction can be occurred with copper by choosing, and the metallic silver of solid solution is capable of forming with niobium, as middle layer;
(3), niobium plate, silver-colored middle layer and copper sheet are fitted together, are put into heating furnace, pressurizeed, vacuumize, then heat into Row connection takes out after cooling and obtains niobium silver-bearing copper connector.
4. the connection method of a kind of copper and niobium according to claim 3, it is characterised in that final in the step (one) The roughness of the fresh metal surface of acquisition is less than 5 μm.
5. the connection method of a kind of copper and niobium according to claim 3, it is characterised in that introduced in the step (two) The mode of silver-colored middle layer is silver powder, silver foil piece, silvering.
6. the connection method of a kind of copper and niobium according to claim 3, it is characterised in that niobium in the step (three) The axial compressive force that plate and copper sheet sub-assembly apply is 2 ~ 25 MPa.
7. the connection method of a kind of copper and niobium according to claim 3, it is characterised in that connection in the step (three) Vacuum degree is 6 × 10 in furnace chamber in the process-3 ~ 8 × 10-4 Pa。
8. the connection method of a kind of copper and niobium according to claim 3, it is characterised in that heating in the step (three) Process is, is heated to 700 ~ 750 oC first with the rate of 5 ~ 30 oC/min, keeps the temperature 20 ~ 60 min, then with 5 ~ The rate of 20 oC/min is heated to 800 ~ 950 oC, keeps the temperature 30 ~ 90 min, is finally dropped with the rate of 5 ~ 10 oC/min To room temperature.
9. the connection method of a kind of copper and niobium according to claim 8, it is characterised in that heating in the step (three) Process is to be heated to 750 oC first with the rate of 15 oC/min, keeps the temperature 50 min, is then heated with the rate of 10 oC/min To 850 oC, 70 min are kept the temperature, room temperature is finally down to the rate of 5 oC/min.
CN201811549784.8A 2018-12-18 2018-12-18 A kind of connector and the connection method of copper and niobium Pending CN109604804A (en)

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Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1473705A (en) * 2002-08-09 2004-02-11 韩国科学技术研究院 Anti-corrosion composite plate and its producing method
CN1663786A (en) * 2004-03-06 2005-09-07 韩国科学技术研究院 Corrosion-resistant clad plate with high bonding strength and fabricating method thereof
CN101254572A (en) * 2008-01-17 2008-09-03 武汉理工大学 Method diffusion welding titanium alloy and copper alloy using niobium central layer
CN101546684A (en) * 2009-04-30 2009-09-30 福州大学 Anti-oxidation composite membrane electrode
CN102218594A (en) * 2011-06-24 2011-10-19 武汉理工大学 Low-temperature diffusion welding method for molybdenum alloy and copper alloy
CN102699558A (en) * 2012-06-29 2012-10-03 哈尔滨工业大学 Flexible composite middle layer brazing alloy and method of utilizing brazing ceramic and metal
CN106956078A (en) * 2017-03-15 2017-07-18 江苏科技大学 A kind of method for improving steel niobium laser weld joint intensity

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1473705A (en) * 2002-08-09 2004-02-11 韩国科学技术研究院 Anti-corrosion composite plate and its producing method
CN1663786A (en) * 2004-03-06 2005-09-07 韩国科学技术研究院 Corrosion-resistant clad plate with high bonding strength and fabricating method thereof
CN101254572A (en) * 2008-01-17 2008-09-03 武汉理工大学 Method diffusion welding titanium alloy and copper alloy using niobium central layer
CN101546684A (en) * 2009-04-30 2009-09-30 福州大学 Anti-oxidation composite membrane electrode
CN102218594A (en) * 2011-06-24 2011-10-19 武汉理工大学 Low-temperature diffusion welding method for molybdenum alloy and copper alloy
CN102699558A (en) * 2012-06-29 2012-10-03 哈尔滨工业大学 Flexible composite middle layer brazing alloy and method of utilizing brazing ceramic and metal
CN106956078A (en) * 2017-03-15 2017-07-18 江苏科技大学 A kind of method for improving steel niobium laser weld joint intensity

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