CN113020735A - Preparation method of silicon nitride ceramic/stainless steel braze welding joint with corrosion resistance and stress relief - Google Patents
Preparation method of silicon nitride ceramic/stainless steel braze welding joint with corrosion resistance and stress relief Download PDFInfo
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- CN113020735A CN113020735A CN202110303142.5A CN202110303142A CN113020735A CN 113020735 A CN113020735 A CN 113020735A CN 202110303142 A CN202110303142 A CN 202110303142A CN 113020735 A CN113020735 A CN 113020735A
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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
- B23K1/0008—Soldering, e.g. brazing, or unsoldering specially adapted for particular articles or work
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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
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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
- B23K2103/00—Materials to be soldered, welded or cut
- B23K2103/02—Iron or ferrous alloys
- B23K2103/04—Steel or steel alloys
- B23K2103/05—Stainless steel
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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
- B23K2103/00—Materials to be soldered, welded or cut
- B23K2103/50—Inorganic material, e.g. metals, not provided for in B23K2103/02 – B23K2103/26
- B23K2103/52—Ceramics
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Abstract
A preparation method of a silicon nitride ceramic/stainless steel braze welding joint with corrosion resistance and stress relief relates to a preparation method of a silicon nitride ceramic/stainless steel braze welding joint. The invention aims to solve the technical problems that the silicon nitride ceramic cracks due to bearing of larger residual stress and the brazing filler metal is not corrosion-resistant because the self expansion coefficients of the brazing filler metal and the metal base metal are too large when the existing active metal of the silicon nitride ceramic and the metal is brazed. The invention is based on the brazing filler metal AgCuTi and AgCu, develops a composite brazing filler metal layer suitable for connecting silicon nitride ceramics and 316L stainless steel, the AgCuTi brazing filler metal and the Ag foil, the AgCu brazing filler metal and the Ag foil are mutually dissolved, Ag-based solid solution is formed on two sides of Mo, the residual stress of a joint can be reduced, the integral corrosion resistance of the joint is improved, no large holes are formed in the whole welding seam area after corrosion, and the integral joint presents better corrosion resistance.
Description
Technical Field
The invention relates to a preparation method of a silicon nitride ceramic/stainless steel braze welding joint.
Background
Silicon nitride ceramics (Si)3N4) Is a high-temperature ceramic with high strength, high hardness, wear resistance, oxidation resistance and self-lubrication, becomes a candidate material which is hopeful to be widely applied in the high-tech field, and Si3N4Has excellent corrosion resistance, such as acid resistance, corrosion of molten salt and the like, and can be used in a harsher corrosion environment. But due to Si3N4While ceramic is inherently brittle and limits its development, metallic materials have excellent room temperature strength and ductility, and if two materials can be combined to make a complex part that meets the requirements, Si will be incorporated into the composite material3N4The application of the ceramic is a major breakthrough, and scholars at home and abroad make extensive research and discussion on the application. 316L stainless steel (022Cr17Ni12Mo2) belongs to a derivative steel grade of 18-8 type austenitic stainless steel, 2-3% of Mo element is added, the excellent corrosion resistance is widely applied in the chemical industry, and the Mo content of 316L ensures that the steel grade has excellent pitting corrosion resistance, can be safely applied to Cl-containing steel-The plasma ion environment is a material frequently selected in the marine environment. Since 316L stainless steel has good workability, if Si is realized3N4The ceramic and the 316L stainless steel are connected, so that the advantages of the ceramic and the 316L stainless steel are fully exerted, a reliable composite component is manufactured, and the application of the ceramic and the 316L stainless steel can be greatly expanded, particularly the application under the marine environment condition. Thus Si3N4the/316L composite component is expected to replace a pure 316L stainless steel component, so that the service life of the component is prolonged, and the production cost is reduced.
The connection of silicon nitride ceramics and metals comprises methods such as active metal brazing, transient liquid phase connection, diffusion welding, oxide glass connection, oxygen-nitrogen glass connection and the like. The current research results show that the method of active metal brazing is most commonly used, and the solders Ag69Cu28Ti3 (wt.%) and Ag28Cu (wt.%) are used as two common commercial solders, although the connection effect is good, the silicon nitride ceramics are cracked due to the large residual stress borne by the solders and the too large expansion coefficient of the metal base metal, and the solders are not corrosion-resistant. Therefore, it is necessary to develop a composite solder layer suitable for ceramic and metal bonding.
Disclosure of Invention
The invention provides a preparation method of a silicon nitride ceramic/stainless steel brazing joint with corrosion resistance and stress relief, aiming at solving the technical problems that the silicon nitride ceramic cracks due to bearing larger residual stress and the brazing filler metal is not corrosion resistant because of overlarge self expansion coefficients of the brazing filler metal and a metal base metal during the existing active metal brazing of the silicon nitride ceramic and the metal.
The preparation method of the silicon nitride ceramic/stainless steel braze welding joint with corrosion resistance and stress relief comprises the following steps:
firstly, base material Si3N4Sequentially polishing the surfaces to be welded of the ceramics to be smooth by using 300# metallographic abrasive paper, 600# metallographic abrasive paper and 1000# metallographic abrasive paper, ultrasonically oscillating in acetone for 3-5 min, and then putting into an oven for drying;
secondly, polishing the 316L stainless steel base material by using 600# SiC abrasive paper and 1000# SiC abrasive paper in sequence to remove a surface oxide layer, then polishing by using 800# metallographic abrasive paper and 1000# metallographic abrasive paper in sequence until the stainless steel base material is bright, then ultrasonically oscillating and cleaning in acetone for 3-5 min, and finally putting the material into an oven for drying;
respectively repeating the operation in the second step on the X metal foil, the Ag foil, the brazing filler metal AgCuTi and the brazing filler metal AgCu; x in the X metal foil is Mo, W, Cr or Nb;
thirdly, drying the materials in the first step and the second step according to the base material of 316L stainless steel/AgCu/Ag/X/Ag/AgCuTi/base material of Si3N4Assembling the ceramic structure, bonding every two layers by using organic glue during assembling, and naturally placing until the organic glue is solidified;
fourthly, putting the joint prepared in the third step into a graphite grinding tool, and putting the base material Si3N4Ceramic on top, in the base material Si3N4Placing a graphite block on the upper surface of the ceramic for physical pressurization;
fifthly, placing the graphite mold in the fourth step into a vacuum brazing furnace, vacuumizing until the vacuum degree is kept at 6 multiplied by 10-6Pa above, heating to 300-350 ℃ within 45-50 min, keeping stable for 20-25 min, heating to the brazing temperature at 7.5-8 ℃/min, keeping the temperature for 10-15 min, reducing to 280-300 ℃ at 5-6 ℃/min, and cooling with the furnace to complete the connection;
the brazing temperature is 900-950 ℃.
The invention is based on the solders AgCuTi and AgCu, develops a composite solder layer suitable for connecting silicon nitride ceramics and 316L stainless steel, the AgCuTi solders and Ag foils, the AgCu solders and the Ag foils are mutually dissolved, Ag-based solid solutions are formed on two sides of Mo, the residual stress of the joint can be reduced, and the integral corrosion resistance of the joint can be improved.
The X metal foil is a Mo foil as an example, and the thickness of the Mo foil is adjusted according to the sizes of different weldments. The residual stress on the ceramic side is reduced due to the increase of the thickness of the Mo foil (the relation between the residual stress on the ceramic side and the thickness of the middle layer made of other metals is subjected to finite element simulation, and the thickness is selected).
Drawings
FIG. 1 is a schematic view of the assembly of the joint prepared in step three of experiment one, 1 being Si3N4Ceramic, 2 is brazing filler metal AgCuTi, 3 is Ag foil, 4 is Mo foil, 5 is brazing filler metal AgCu, and 6 is 316L stainless steel;
FIG. 2 is an SEM image of a joint prepared in step five of experiment one;
FIG. 3 is an SEM image of a joint prepared in step five of test one after corrosion;
FIG. 4 is a brazing of Si with conventional AgCuTi as the brazing filler metal3N4And a residual stress simulation cloud chart of the 316L stainless steel joint;
fig. 5 is a simulated cloud of residual stresses for the joint prepared in step five of test one.
Detailed Description
The first embodiment is as follows: the embodiment is a preparation method of a silicon nitride ceramic/stainless steel braze welding joint with corrosion resistance and stress relief, which comprises the following specific processes:
firstly, base material Si3N4Sequentially polishing the surfaces to be welded of the ceramics to be smooth by using 300# metallographic abrasive paper, 600# metallographic abrasive paper and 1000# metallographic abrasive paper, ultrasonically oscillating in acetone for 3-5 min, and then putting into an oven for drying;
secondly, polishing the 316L stainless steel base material by using 600# SiC abrasive paper and 1000# SiC abrasive paper in sequence to remove a surface oxide layer, then polishing by using 800# metallographic abrasive paper and 1000# metallographic abrasive paper in sequence until the stainless steel base material is bright, then ultrasonically oscillating and cleaning in acetone for 3-5 min, and finally putting the material into an oven for drying;
respectively repeating the operation in the second step on the X metal foil, the Ag foil, the brazing filler metal AgCuTi and the brazing filler metal AgCu; x in the X metal foil is Mo, W, Cr or Nb;
thirdly, drying the materials in the first step and the second step according to the base material of 316L stainless steel/AgCu/Ag/X/Ag/AgCuTi/base material of Si3N4Assembling the ceramic structure, bonding every two layers by using organic glue during assembling, and naturally placing until the organic glue is solidified;
fourthly, putting the joint prepared in the third step into a graphite grinding tool, and putting the base material Si3N4Ceramic on top, in the base material Si3N4Placing a graphite block on the upper surface of the ceramic for physical pressurization;
fifthly, placing the graphite mold in the fourth step into a vacuum brazing furnace, vacuumizing until the vacuum degree is kept at 6 multiplied by 10-6Pa above, heating to 300-350 ℃ within 45-50 min, keeping stable for 20-25 min, heating to the brazing temperature at 7.5-8 ℃/min, keeping the temperature for 10-15 min, reducing to 280-300 ℃ at 5-6 ℃/min, and cooling with the furnace to complete the connection;
the brazing temperature is 900-950 ℃.
The second embodiment is as follows: the first difference between the present embodiment and the specific embodiment is: the ultrasonic oscillation in the step one is carried out in an ultrasonic oscillator. The rest is the same as the first embodiment.
The third concrete implementation mode: the present embodiment differs from the first or second embodiment in that: the frequency of the ultrasonic oscillation in the step one is 40 KHz. The others are the same as in the first or second embodiment.
The fourth concrete implementation mode: the difference between this embodiment mode and one of the first to third embodiment modes is: the drying in the step one is drying for 2 hours at 80 ℃. The rest is the same as one of the first to third embodiments.
The fifth concrete implementation mode: the fourth difference between this embodiment and the specific embodiment is that: and the ultrasonic oscillation in the step two is carried out in an ultrasonic oscillator. The rest is the same as the fourth embodiment.
The sixth specific implementation mode: the fourth difference between this embodiment and the specific embodiment is that: and the frequency of the ultrasonic oscillation in the step two is 40 KHz. The rest is the same as the fourth embodiment.
The seventh embodiment: the fourth difference between this embodiment and the specific embodiment is that: and the drying in the second step is drying for 2 hours at the temperature of 80 ℃. The rest is the same as the fourth embodiment.
The specific implementation mode is eight: the fourth difference between this embodiment and the specific embodiment is that: the brazing filler metal AgCuTi in the second step is Ag69Cu28Ti3 (wt.%). The rest is the same as the fourth embodiment.
The specific implementation method nine: the fourth difference between this embodiment and the specific embodiment is that: the brazing filler metal AgCu in the second step is Ag28Cu (wt.%). The rest is the same as the fourth embodiment.
The detailed implementation mode is ten: the fourth difference between this embodiment and the specific embodiment is that: the organic glue in the third step is glue 502. The rest is the same as the fourth embodiment.
The concrete implementation mode eleven: the fourth difference between this embodiment and the specific embodiment is that: in the fifth step, the graphite mould in the fourth step is placed in a vacuum brazing furnace, and the graphite mould is vacuumized until the vacuum degree is kept at 6 multiplied by 10-6And Pa above, heating to 300 ℃ within 45min, keeping the temperature for 20min, heating to the brazing temperature at 7.5 ℃/min, keeping the temperature for 10min, reducing to 300 ℃ at 5 ℃/min, and cooling along with the furnace to complete the connection. The rest is the same as the fourth embodiment.
The specific implementation mode twelve: the fourth difference between this embodiment and the specific embodiment is that: and when the brazing temperature in the step five is 950 ℃, the thicknesses of the brazing filler metal AgCuTi and the brazing filler metal AgCu in the step two are both 100 micrometers, the thickness of the Ag foil is 2031.11 micrometers, and the thickness of the X metal foil is 100 micrometers-500 micrometers. The rest is the same as the fourth embodiment.
The specific implementation mode is thirteen: the fourth difference between this embodiment and the specific embodiment is that: and when the brazing temperature in the step five is 900 ℃, the thicknesses of the brazing filler metal AgCuTi and the brazing filler metal AgCu in the step two are both 100 micrometers, the thickness of the Ag foil is 305.47 micrometers, and the thickness of the X metal foil is 100 micrometers-500 micrometers. The rest is the same as the fourth embodiment.
The invention was verified with the following tests:
test one: the test is a preparation method of a silicon nitride ceramic/stainless steel braze welding joint with corrosion resistance and stress relief, and the specific process is as follows:
firstly, base material Si3N4Sequentially polishing the to-be-welded surfaces of the ceramics to be smooth by using 300# metallographic abrasive paper, 600# metallographic abrasive paper and 1000# metallographic abrasive paper, ultrasonically oscillating for 3min in acetone, and then putting into an oven for drying; the ultrasonic oscillation in the step one is carried out in an ultrasonic oscillator; the frequency of the ultrasonic oscillation in the step one is 40 KHz; the drying in the step one is drying for 2 hours at 80 ℃;
secondly, polishing the 316L stainless steel base material by using 600# SiC abrasive paper and 1000# SiC abrasive paper in sequence to remove a surface oxide layer, then polishing by using 800# metallographic abrasive paper and 1000# metallographic abrasive paper in sequence until the stainless steel base material is bright, then ultrasonically oscillating and cleaning in acetone for 3min, and finally putting the material into an oven for drying; the ultrasonic oscillation in the step two is carried out in an ultrasonic oscillator; the frequency of the ultrasonic oscillation in the step two is 40 KHz; the drying in the step two is drying for 2 hours at the temperature of 80 ℃; the brazing filler metal AgCuTi in the second step is Ag69Cu28Ti3 (wt%); the brazing filler metal AgCu in the second step is Ag28Cu (wt%); the thickness of the brazing filler metal AgCuTi and the brazing filler metal AgCu in the second step are both 100 mu m, the thickness of the Ag foil is 305.47 mu m, and the thickness of the Mo foil is 500 mu m;
respectively repeating the operation in the second step on the Mo foil, the Ag foil, the brazing filler metal AgCuTi and the brazing filler metal AgCu;
thirdly, drying the materials in the first step and the second step according to the base material of 316L stainless steel/AgCu/Ag/Mo/Ag/AgCuTi/base material of Si3N4Assembling the ceramic structure, wherein in order to stably assemble the brazing filler metal layer during assembling, 502 glue is used for bonding every two layers, and the ceramic structure is naturally placed until 502 glue is solidified;
fourthly, putting the joint prepared in the third step into a graphite grinding tool, and putting the base material Si3N4Ceramic on top, in the base material Si3N4The graphite blocks are placed on the upper surface of the ceramic for physical pressurization, so that the situation that the base metal is separated from the original position due to melting of the metal brazing filler metal in the temperature rising process, and the welding effect is greatly reduced is avoided;
fifthly, placing the graphite mold in the fourth step into a vacuum brazing furnace, vacuumizing until the vacuum degree is kept at 6 multiplied by 10-6Pa above, heating to 300 ℃ within 45min, keeping the temperature for 20min so as to volatilize the organic glue in the joint completely, heating to the brazing temperature at 7.5 ℃/min, keeping the temperature for 10min, reducing to 300 ℃ at 5 ℃/min, and cooling along with the furnace to finish connection;
the brazing temperature is 900 ℃.
The joint prepared in the fifth step of the first test was evaluated for shear strength, and the room temperature strength of the joint was 80.31 MPa.
Fig. 2 is an SEM image of the joint prepared in step five of experiment one, and it can be observed that the AgCuTi filler metal and the Ag foil, the AgCu filler metal and the Ag foil are mutually soluble, and an Ag-based solid solution is formed on both sides of Mo.
In order to observe the appearance of the corroded joint, the joint prepared in the fifth step of the first test is corroded: accelerated corrosion of joint is carried out by adopting potentiodynamic polarization method, the used instrument is an electrochemical workstation, wherein a platinum electrode is used as a counter electrode, the joint is a working electrode, a saturated calomel electrode is a standard electrode, 3.5 wt.% of NaCl aqueous solution is electrolytic solution, and the cross section area of the tested joint is 4 multiplied by 8mm2The test voltage range is-0.3V, and the scanning rate is 5 mV/s. SEM shape after etchingAs shown in fig. 3, no large holes are formed in the entire weld zone, and the entire joint exhibits good corrosion resistance.
FIG. 4 is a brazing of Si with conventional AgCuTi as the brazing filler metal3N4And a residual stress simulation cloud chart of the 316L stainless steel joint;
fig. 5 is a simulated cloud of residual stresses for the joint prepared in step five of test one. It can be seen that the AgCu/Ag/Mo/Ag/AgCuTi composite solder of test one is adopted to weld Si3N4And the maximum residual stress (165.4MPa) of the 316L stainless steel joint is significantly less than the maximum residual stress (303.4MPa) of the joint using conventional AgCuTi as the brazing filler metal.
And (2) test II: this test differs from the test one in that: the brazing temperature in the fifth step is 950 ℃, and the thickness of the Ag foil in the second step is 2031.11 μm. The rest is the same as test one.
And evaluating the performance of the joint prepared in the fifth step of the second test on the shear strength to obtain the joint with the room-temperature strength of 63.36 MPa.
Claims (13)
1. A method for preparing a silicon nitride ceramic/stainless steel braze welding joint with corrosion resistance and stress relief is characterized in that the method for preparing the silicon nitride ceramic/stainless steel braze welding joint with corrosion resistance and stress relief comprises the following steps:
firstly, base material Si3N4Sequentially polishing the surfaces to be welded of the ceramics to be smooth by using 300# metallographic abrasive paper, 600# metallographic abrasive paper and 1000# metallographic abrasive paper, ultrasonically oscillating in acetone for 3-5 min, and then putting into an oven for drying;
secondly, polishing the 316L stainless steel base material by using 600# SiC abrasive paper and 1000# SiC abrasive paper in sequence to remove a surface oxide layer, then polishing by using 800# metallographic abrasive paper and 1000# metallographic abrasive paper in sequence until the stainless steel base material is bright, then ultrasonically oscillating and cleaning in acetone for 3-5 min, and finally putting the material into an oven for drying;
respectively repeating the operation in the second step on the X metal foil, the Ag foil, the brazing filler metal AgCuTi and the brazing filler metal AgCu; x in the X metal foil is Mo, W, Cr or Nb;
thirdly, drying the dried product in the first step and the second stepThe material is prepared from base material 316L stainless steel/AgCu/Ag/X/Ag/AgCuTi/base material Si3N4Assembling the ceramic structure, bonding every two layers by using organic glue during assembling, and naturally placing until the organic glue is solidified;
fourthly, putting the joint prepared in the third step into a graphite grinding tool, and putting the base material Si3N4Ceramic on top, in the base material Si3N4Placing a graphite block on the upper surface of the ceramic for physical pressurization;
fifthly, placing the graphite mold in the fourth step into a vacuum brazing furnace, vacuumizing until the vacuum degree is kept at 6 multiplied by 10-6Pa above, heating to 300-350 ℃ within 45-50 min, keeping stable for 20-25 min, heating to the brazing temperature at 7.5-8 ℃/min, keeping the temperature for 10-15 min, reducing to 280-300 ℃ at 5-6 ℃/min, and cooling with the furnace to complete the connection;
the brazing temperature is 900-950 ℃.
2. The method according to claim 1, wherein the ultrasonic vibration is performed in an ultrasonic vibrator.
3. The method according to claim 1, wherein the ultrasonic vibration frequency in the first step is 40 KHz.
4. The method of claim 1, wherein the drying step in step one is carried out at 80 ℃ for 2 h.
5. The method according to claim 1, wherein the ultrasonic vibration is performed in an ultrasonic vibrator.
6. The method according to claim 1, wherein the ultrasonic vibration frequency in step two is 40 KHz.
7. The method of claim 1, wherein the step of drying is performed at 80 ℃ for 2h in step two.
8. The method of claim 1, wherein the brazing filler metal AgCuTi in step two is Ag69Cu28Ti 3.
9. The method of claim 1, wherein the brazing filler metal AgCu of step two is Ag28 Cu.
10. The method of claim 1 wherein the organic glue in step three is glue 502.
11. The method of claim 1, wherein the graphite mold of the fourth step is placed in a vacuum brazing furnace, and vacuum is applied until the vacuum degree is maintained at 6 x 10-6And Pa above, heating to 300 ℃ within 45min, keeping the temperature for 20min, heating to the brazing temperature at 7.5 ℃/min, keeping the temperature for 10min, reducing to 300 ℃ at 5 ℃/min, and cooling along with the furnace to complete the connection.
12. The method of claim 1, wherein the thickness of the brazing filler metal AgCuTi and the brazing filler metal AgCu in the second step are 100 μm, the thickness of Ag foil is 2031.11 μm, and the thickness of X metal foil is 100 μm to 500 μm, when the brazing temperature in the fifth step is 950 ℃.
13. The method of claim 1, wherein the thickness of the brazing filler metal AgCuTi and the brazing filler metal AgCu in the second step are 100 μm, the thickness of Ag foil is 305.47 μm, and the thickness of X metal foil is 100 μm to 500 μm, when the brazing temperature in the fifth step is 900 ℃.
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CN115991609A (en) * | 2023-01-09 | 2023-04-21 | 南京理工大学 | Ceramic-metal discharge plasma connection method |
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