CN112620851A - Method for connecting graphite and stainless steel through high-temperature brazing of composite gradient interlayer - Google Patents
Method for connecting graphite and stainless steel through high-temperature brazing of composite gradient interlayer Download PDFInfo
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- CN112620851A CN112620851A CN202011544679.2A CN202011544679A CN112620851A CN 112620851 A CN112620851 A CN 112620851A CN 202011544679 A CN202011544679 A CN 202011544679A CN 112620851 A CN112620851 A CN 112620851A
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- 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
- B23K1/00—Soldering, e.g. brazing, or unsoldering
- B23K1/008—Soldering within a furnace
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- 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
- B23K1/00—Soldering, e.g. brazing, or unsoldering
- B23K1/20—Preliminary treatment of work or areas to be soldered, e.g. in respect of a galvanic coating
-
- 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
- B23K1/00—Soldering, e.g. brazing, or unsoldering
- B23K1/20—Preliminary treatment of work or areas to be soldered, e.g. in respect of a galvanic coating
- B23K1/206—Cleaning
-
- 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
- B23K3/00—Tools, devices, or special appurtenances for soldering, e.g. brazing, or unsoldering, not specially adapted for particular methods
- B23K3/08—Auxiliary devices therefor
Abstract
A high-temperature brazing connection method for graphite and stainless steel selects amorphous TiZrNiCu foil brazing filler metal, Ti foil, amorphous BNi-2 brazing filler metal foil and Ni foil as brazing materials, and after the graphite, the stainless steel, the amorphous TiZrNiCu foil, the Ti foil, the amorphous BNi-2 foil and the Ni foil are cleaned, a graphite/amorphous TiZrNiCu foil/Ti foil/amorphous BNi-2 foil/Ni foil/amorphous BNi-2 foil/stainless steel sandwich structure is formed, the structure is placed in a vacuum furnace, the temperature is increased to 980 and 1080 ℃ at the speed of 5-8 ℃/min, the temperature is kept for 60-120min for brazing connection, and then the graphite/amorphous TiZrNiCu foil/amorphous BNi-2 foil/stainless steel sandwich structure is cooled to room temperature slowly by means of sectional heat preservation. The invention effectively solves the problems of serious mismatching and wettability of the thermal expansion coefficients of graphite and stainless steel, greatly reduces the thermal stress of the joint, avoids cracks from growing in the joint area and realizes good connection of the graphite and the stainless steel.
Description
Technical Field
The invention relates to connection of graphite and stainless steel, in particular to a method for connecting graphite and stainless steel by high-temperature brazing of a composite gradient interlayer, and belongs to the field of material connection.
Background
Graphite is a novel high-strength material, has good chemical stability at normal temperature, extremely high melting point, excellent corrosion resistance, compressive strength and high thermal conductivity, has low relative density, and is widely applied to national defense industry, aerospace, energy and traffic industries. Stainless steel, especially austenitic stainless steel, has good mechanical properties and processing properties, good corrosion resistance and high strength, and is a metal material widely used in industrial departments of petroleum, chemical industry, chemical fertilizers and the like. The graphite and stainless steel connecting piece is expected to have the advantages of the graphite and stainless steel connecting piece, and has wide development prospect in the aspects of national defense and civil industry.
Because the wettability of graphite and stainless steel is poor, and the graphite and the stainless steel have great difference in thermal conductivity and thermal expansion coefficient, the graphite and the stainless steel can generate great thermal stress and cracking phenomena in the welding process. Therefore, the graphite and stainless steel have the outstanding problem of cracking in the welding process, which can seriously cause the direct fracture of the welding joint, and hinder the popularization and the application of the graphite and stainless steel composite structure. At present, the connection method of graphite and stainless steel mainly comprises two methods: firstly, mechanical riveting, namely, connecting graphite and stainless steel together by using a fixing piece such as a rivet; and the second is adhesive bonding which comprises an organic adhesive and an inorganic adhesive. The mechanical riveting has defects in the connection aspect of thick and large parts, and the bonding of the adhesive is also insufficient in the aspects of strength and high-temperature service. Therefore, it is necessary to develop a new connecting process to expand the range of use thereof. Brazing has a low requirement on the surface condition of the base material, can complete connection under the condition of no pressure or small pressure, and has various joint structure forms. Thus, brazing is well suited for the joining of graphite to stainless steel. In addition, because of the poor high temperature oxidation resistance of graphite, vacuum brazing is an excellent method for joining the graphite.
In the case of brazed joints of dissimilar materials, particularly ceramic to metal materials, the thermal expansion coefficients are severely mismatched and thus generate significant thermal stresses. In order to improve the quality of the joint, the ceramic surface is usually modified; or adding a material with a thermal expansion coefficient between the parent metals into the brazing filler metal to form thermal expansion coefficient gradient transition; or a plastic intermediate layer is added, and the thermal stress is relieved through the plastic deformation of the plastic intermediate layer; or a hard intermediate layer having an expansion coefficient between the base materials is added, or both the hard intermediate layer and the plastic intermediate layer are bonded. And because the melting point of the stainless steel is much lower than that of the graphite, and the use temperature of the stainless steel is between 196 ℃ below zero and 800 ℃, the graphite and the stainless steel are welded by using high-melting-point brazing filler metal (the melting point of the stainless steel is about 1300 ℃ to 1400 ℃). Amorphous solder is a new type of solder that has been developed in recent years. The term "amorphous" is used in relation to the crystalline state, and is characterized by the retention of the structure and anisotropy of the disordered arrangement of the atoms of the liquid metal, but by the metallic bonding of the atoms to one another. The amorphous solder has uniform chemical components and high purity, and the components of the solder are not separated, so that the strength of a soldered joint can be obviously improved. Compared with the paste solder, the solder does not contain adhesive, the heating rate is not limited, the brazing seam does not contain non-metal slag inclusion, and the soldered joint has high quality. Generally, under the same brazing gap and brazing specification, the diffusion depth and the distribution uniformity of elements in the brazing joint area of the amorphous brazing filler metal are larger than those of the crystalline brazing filler metal. Therefore, the joint strength of amorphous solder is much higher than that of crystalline solder.
Aiming at the problems of graphite and stainless steel in the welding process, the invention provides a method for connecting graphite and stainless steel by high-temperature brazing of an amorphous brazing alloy/hard intermediate layer/amorphous brazing alloy/plastic intermediate layer/amorphous brazing alloy composite gradient intermediate layer formed by an amorphous nickel-based brazing alloy, a hard intermediate layer and a plastic intermediate layer by utilizing the characteristics that the excellent performance of a brazing joint of the amorphous brazing alloy and the hard intermediate layer and the plastic intermediate layer can effectively relieve the residual stress.
Disclosure of Invention
The invention provides a method for connecting graphite and stainless steel by high-temperature brazing of a composite gradient interlayer, aiming at the problems of great thermal expansion coefficient mismatching and wettability during welding of the graphite and the stainless steel. The amorphous TiZrNiCu foil, the hard Ti foil, the amorphous BNi-2 foil and the plastic Ni foil form a composite gradient interlayer structure, and a series of complex physical and chemical reactions occur with a welded parent metal, so that the thermal stress of a joint is effectively relieved, the welded joint with good high-temperature mechanical properties is obtained, and the good connection between the parent metals is realized. The method is characterized by comprising the following steps:
(1) pretreatment: respectively putting stainless steel, Ti sheets, amorphous TiZrNiCu foils, amorphous BNi-2 foils and Ni foils which are polished by graphite and sand paper into an alcohol solution for ultrasonic cleaning for 10-40min, then cleaning with deionized water, and drying for later use.
(2) Assembling: amorphous TiZrNiCu foil, Ti foil, amorphous BNi-2 foil, Ni foil and amorphous BNi-2 foil are sequentially arranged between the to-be-welded surfaces of the graphite and the stainless steel to form a sandwich structure, namely graphite/amorphous TiZrNiCu foil/Ti foil/amorphous BNi-2 foil/Ni foil/amorphous BNi-2 foil/stainless steel, and the to-be-welded structure is fixed and then placed in a vacuum furnace.
(3) Brazing: the vacuum degree is better than 2 x 10 in the brazing process-3Pa, raising the temperature to 980-1080 ℃ at the speed of 5-8 ℃/min, and preserving the temperature for 60-120 min.
(4) And (3) cooling: cooling to 750-; then cooling to 650-750 ℃ at the speed of 2-4 ℃/min, and preserving heat for 30-60 min; cooling to 650 ℃ at the speed of 2-3 ℃/min, and preserving heat for 40-80 min; and finally, cooling to room temperature along with the furnace.
In the above steps, the thickness of the amorphous TiZrNiCu foil is 30-100 microns, the thickness of the Ti foil is 100-500 microns, the thickness of the amorphous BNi-2 brazing filler metal foil is 30-100 microns, and the thickness of the Ni foil is 50-300 microns.
The invention uses amorphous TiZrNiCu foil/Ti sheet/amorphous BNi-2 foil/Ni foil/amorphous BNi-2 foil as a composite gradient interlayer for high-temperature brazing to connect graphite and stainless steel, and has the advantages that:
(1) the diffusion depth and the distribution uniformity of elements in the brazing joint area of the amorphous brazing filler metal are both larger than those of the crystalline brazing filler metal, and particularly, the diffusion distance of element atoms (B, Si) for controlling the formation of a brittle compound phase in the brazing filler metal is far longer than that of the common crystalline brazing filler metal, so that the concentration reduction of elements formed by the brittle phase in a brazing seam and the homogenization of the joint area structure are facilitated.
(2) The active element Ti in the amorphous TiZrNiCu brazing filler metal foil can react with the element C in the graphite to generate metal carbide of Ti, so that the brazing filler metal is promoted to wet the to-be-welded surface of the graphite, and the bonding strength of a welding joint can be effectively improved.
(3) In this brazing structure, the graphite has a thermal expansion coefficient of 5.85X 10-6The coefficient of thermal expansion of TiC, the main product on the graphite surface, is 7.74X 10-6The thermal expansion coefficient of the Ti metal layer is 9.41-10.03 multiplied by 10-6The Ni metal layer has a thermal expansion coefficient of 13.0 × 10 at/° C-6The coefficient of thermal expansion of 304 stainless steel is 16-19.7 x 10 DEG C-6Per DEG C (20-900 ℃), a thermal expansion coefficient gradient transition layer is perfectly formed, and the residual stress and deformation between graphite and stainless steel can be effectively relieved, so that the cracking tendency of the joint is greatly reduced.
(4) In addition, the plastic metal Ni foil serving as the middle layer can relieve partial residual stress and deformation through plastic deformation, and the cracking tendency of the joint is further reduced.
(5) Through the stepped sectional slow cooling process, the residual stress and deformation are effectively controlled, the formation of cracks is avoided, and the soldered joint with good mechanical property can be obtained.
Detailed Description
The present invention provides a method for joining graphite and stainless steel by high temperature brazing of a composite gradient interlayer, and the present invention is further explained by the following specific examples.
Example 1
The isostatic graphite and 304 stainless steel are brazed by using 30 micron thick amorphous TiZrNiCu foil, 100 micron thick Ti foil, 300 micron thick Ni foil, and 30 micron thick amorphous BNi-2 foil as composite gradient interlayers:
(1) pretreatment: and putting stainless steel, a graphite Ti sheet, an amorphous TiZrNiCu foil, an amorphous BNi-2 foil and a Ni foil which are respectively polished by 400#, 600# and 800# sandpaper into an alcohol solution for ultrasonic cleaning for 40min, then cleaning by deionized water, and drying for later use.
(2) Assembling: amorphous TiZrNiCu foil, Ti foil, amorphous BNi-2 foil, Ni foil and amorphous BNi-2 foil are sequentially arranged between the to-be-welded surfaces of the graphite and the stainless steel to form a sandwich structure, namely graphite/amorphous TiZrNiCu foil/Ti foil/amorphous BNi-2 foil/Ni foil/amorphous BNi-2 foil/stainless steel, and the to-be-welded structure is fixed and then placed in a vacuum furnace.
(3) Brazing: the vacuum degree is better than 2 x 10 in the brazing process-3Pa, raising the temperature to 1080 ℃ at the speed of 8 ℃/min, and preserving the temperature for 60 min.
(4) And (3) cooling: cooling to 850 deg.C at a speed of 5 deg.C/min, and maintaining for 20 min; then cooling to 750 ℃ at the speed of 2 ℃/min, and preserving heat for 30 min; cooling to 500 deg.C at a speed of 2 deg.C/min, and maintaining for 80 min; and finally, cooling to room temperature along with the furnace.
And performing performance test on the obtained connecting piece, wherein the average shear strength of the obtained graphite and 304 stainless steel joint at room temperature is 30.5 MPa.
Example 2
The isostatic graphite and 304 stainless steel are brazed by using 100 micron thick amorphous TiZrNiCu foil, 500 micron thick Ti foil, 100 micron thick Ni foil, 100 micron thick amorphous BNi-2 foil as composite gradient interlayer:
(1) pretreatment: and putting stainless steel, graphite Ti sheets, amorphous TiZrNiCu foils, amorphous BNi-2 foils and Ni foils which are respectively polished by 600#, 800#, and 1000# sandpaper into an alcohol solution for ultrasonic cleaning for 20min, then cleaning with deionized water, and drying for later use.
(2) Assembling: amorphous TiZrNiCu foil, Ti foil, amorphous BNi-2 foil, Ni foil and amorphous BNi-2 foil are sequentially arranged between the to-be-welded surfaces of the graphite and the stainless steel to form a sandwich structure, namely graphite/amorphous TiZrNiCu foil/Ti foil/amorphous BNi-2 foil/Ni foil/amorphous BNi-2 foil/stainless steel, and the to-be-welded structure is fixed and then placed in a vacuum furnace.
(3) Brazing: the vacuum degree is better than 2 x 10 in the brazing process-3Pa, raising the temperature to 980 ℃ at the speed of 5 ℃/min, and preserving the temperature for 120 min.
(4) And (3) cooling: cooling to 850 deg.C at a speed of 5 deg.C/min, and maintaining for 20 min; then cooling to 750 ℃ at the speed of 2 ℃/min, and preserving heat for 30 min; cooling to 500 deg.C at a speed of 2 deg.C/min, and maintaining for 80 min; and finally, cooling to room temperature along with the furnace.
And performing performance test on the obtained connecting piece, wherein the average shear strength of the obtained graphite and 304 stainless steel joint at room temperature is 34.2 MPa.
Example 3
The isostatic graphite and 316L stainless steel were brazed using a 50 micron thick amorphous TiZrNiCu foil, a 300 micron thick Ti foil, a 200 micron thick Ni foil, and a 50 micron thick amorphous BNi-2 foil as a composite gradient interlayer:
(1) pretreatment: and putting stainless steel, a graphite Ti sheet, an amorphous TiZrNiCu foil, an amorphous BNi-2 foil and a Ni foil which are respectively polished by 600#, 800# and 1500# sandpaper into an alcohol solution for ultrasonic cleaning for 30min, then cleaning by deionized water, and drying for later use.
(2) Assembling: amorphous TiZrNiCu foil, Ti foil, amorphous BNi-2 foil, Ni foil and amorphous BNi-2 foil are sequentially arranged between the to-be-welded surfaces of the graphite and the stainless steel to form a sandwich structure, namely graphite/amorphous TiZrNiCu foil/Ti foil/amorphous BNi-2 foil/Ni foil/amorphous BNi-2 foil/stainless steel, and the to-be-welded structure is fixed and then placed in a vacuum furnace.
(3) Brazing: the vacuum degree is better than 2 x 10 in the brazing process-3Pa, raising the temperature to 1020 ℃ at the speed of 6 ℃/min, and keeping the temperature for 90 min.
(4) And (3) cooling: cooling to 800 deg.C at a rate of 4 deg.C/min, and maintaining for 30 min; then cooling to 700 ℃ at the speed of 3 ℃/min, and preserving heat for 40 min; cooling to 560 deg.C at a speed of 2 deg.C/min, and maintaining for 60 min; and finally, cooling to room temperature along with the furnace.
And performing performance test on the obtained connecting piece, wherein the average shear strength of the obtained graphite and the 316L stainless steel joint at room temperature is 38.6 MPa.
Example 4
The amorphous TiZrNiCu foil with the thickness of 70 microns, the Ti foil with the thickness of 200 microns, the Ni foil with the thickness of 300 microns and the amorphous BNi-2 foil with the thickness of 70 microns are used as composite gradient interlayers to braze and connect the isostatic pressure graphite and 316L stainless steel:
(1) pretreatment: and putting stainless steel, a graphite Ti sheet, an amorphous TiZrNiCu foil, an amorphous BNi-2 foil and a Ni foil which are respectively polished by 600#, 800# and 1500# sandpaper into an alcohol solution for ultrasonic cleaning for 30min, then cleaning by deionized water, and drying for later use.
(2) Assembling: amorphous TiZrNiCu foil, Ti foil, amorphous BNi-2 foil, Ni foil and amorphous BNi-2 foil are sequentially arranged between the to-be-welded surfaces of the graphite and the stainless steel to form a sandwich structure, namely graphite/amorphous TiZrNiCu foil/Ti foil/amorphous BNi-2 foil/Ni foil/amorphous BNi-2 foil/stainless steel, and the to-be-welded structure is fixed and then placed in a vacuum furnace.
(3) Brazing: the vacuum degree is better than 2 x 10 in the brazing process-3Pa, raising the temperature to 1050 ℃ at the speed of 7 ℃/min, and keeping the temperature for 100 min.
(4) And (3) cooling: cooling to 750 deg.C at a speed of 5 deg.C/min, and maintaining for 20 min; then cooling to 660 ℃ at the speed of 2 ℃/min, and preserving heat for 30 min; cooling to 520 deg.C at a speed of 2 deg.C/min, and maintaining for 70 min; and finally, cooling to room temperature along with the furnace.
And performing performance test on the obtained connecting piece, wherein the average shear strength of the obtained graphite and the 316L stainless steel joint at room temperature is 31.6 MPa.
Example 5
The 100 micron thick amorphous TiZrNiCu foil, the 100 micron thick Ti foil, the 100 micron thick Ni foil and the 100 micron thick amorphous BNi-2 foil are used as composite gradient interlayers to braze and connect the isostatic pressure graphite and the 316L stainless steel:
(1) pretreatment: and putting stainless steel, a graphite Ti sheet, an amorphous TiZrNiCu foil, an amorphous BNi-2 foil and a Ni foil which are respectively polished by 400#, 800# and 1500# sandpaper into an alcohol solution for ultrasonic cleaning for 20min, then cleaning by deionized water, and drying for later use.
(2) Assembling: amorphous TiZrNiCu foil, Ti foil, amorphous BNi-2 foil, Ni foil and amorphous BNi-2 foil are sequentially arranged between the to-be-welded surfaces of the graphite and the stainless steel to form a sandwich structure, namely graphite/amorphous TiZrNiCu foil/Ti foil/amorphous BNi-2 foil/Ni foil/amorphous BNi-2 foil/stainless steel, and the to-be-welded structure is fixed and then placed in a vacuum furnace.
(3) Brazing: the vacuum degree is better than 2 x 10 in the brazing process-3Pa, raising the temperature to 1070 ℃ at the speed of 7 ℃/min, and keeping the temperature for 100 min.
(4) And (3) cooling: cooling to 790 deg.C at a rate of 5 deg.C/min, and maintaining for 25 min; then cooling to 680 ℃ at the speed of 4 ℃/min, and preserving heat for 50 min; cooling to 540 deg.C at a speed of 2 deg.C/min, and maintaining for 50 min; and finally, cooling to room temperature along with the furnace.
And performing performance test on the obtained connecting piece, wherein the average shear strength of the obtained graphite and the 316L stainless steel joint at room temperature is 33.3 MPa.
The above-described embodiments are merely exemplary and not intended to limit the present invention in any way, and any simple modifications, equivalent variations and modifications made to the above-described embodiments in accordance with the technical spirit of the present invention are within the scope of the present invention.
Claims (2)
1. A method for connecting graphite and stainless steel by high-temperature brazing of a composite gradient interlayer is characterized by comprising the following specific steps:
(1) pretreatment: respectively putting stainless steel, Ti sheets, amorphous TiZrNiCu foils, amorphous BNi-2 foils and Ni foils which are polished by graphite and sand paper into an alcohol solution for ultrasonic cleaning for 10-40min, then cleaning with deionized water, and drying for later use.
(2) Assembling: amorphous TiZrNiCu foil, Ti foil, amorphous BNi-2 foil, Ni foil and amorphous BNi-2 foil are sequentially arranged between the to-be-welded surfaces of the graphite and the stainless steel to form a sandwich structure, namely graphite/amorphous TiZrNiCu foil/Ti foil/amorphous BNi-2 foil/Ni foil/amorphous BNi-2 foil/stainless steel, and the to-be-welded structure is fixed and then placed in a vacuum furnace.
(3) Brazing: the vacuum degree is better than 2 x 10 in the brazing process-3Pa, raising the temperature to 980-1080 ℃ at the speed of 5-8 ℃/min, and preserving the temperature for 60-120 min.
(4) And (3) cooling: cooling to 750-; then cooling to 650-750 ℃ at the speed of 2-4 ℃/min, and preserving heat for 30-60 min; cooling to 650 ℃ at the speed of 2-3 ℃/min, and preserving heat for 40-80 min; and finally, cooling to room temperature along with the furnace.
2. The method for connecting graphite and stainless steel by high-temperature brazing of the composite gradient interlayer according to claim 1, wherein the method comprises the following steps: in the step (1), the thickness of the amorphous TiZrNiCu foil is 30-100 microns, the thickness of the Ti foil is 100-500 microns, the thickness of the amorphous BNi-2 foil is 30-100 microns, and the thickness of the Ni foil is 50-300 microns.
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| CN114247947A (en) * | 2022-01-12 | 2022-03-29 | 湘潭大学 | Vacuum brazing connection method of C/C radiating fins and Ti tube |
| CN114833410A (en) * | 2022-07-05 | 2022-08-02 | 中机智能装备创新研究院(宁波)有限公司 | Method for reducing residual stress of heterogeneous brazed joint |
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| 中国特钢企业协会不锈钢分会: "焊接与表面加工编", 《不锈钢实用手册》 * |
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| CN114178640A (en) * | 2021-09-24 | 2022-03-15 | 中国航发北京航空材料研究院 | Thermal shock-resistant graphite and metal brazing method |
| CN114247947A (en) * | 2022-01-12 | 2022-03-29 | 湘潭大学 | Vacuum brazing connection method of C/C radiating fins and Ti tube |
| CN114833410A (en) * | 2022-07-05 | 2022-08-02 | 中机智能装备创新研究院(宁波)有限公司 | Method for reducing residual stress of heterogeneous brazed joint |
| CN114833410B (en) * | 2022-07-05 | 2022-10-14 | 中机智能装备创新研究院(宁波)有限公司 | Method for reducing residual stress of heterogeneous brazed joint |
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| CN112620851B (en) | 2022-12-13 |
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