CN114951873B - Composite brazing filler metal containing high-entropy alloy and method for brazing and connecting AlN and Cu by composite brazing filler metal - Google Patents
Composite brazing filler metal containing high-entropy alloy and method for brazing and connecting AlN and Cu by composite brazing filler metal Download PDFInfo
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- CN114951873B CN114951873B CN202210664876.0A CN202210664876A CN114951873B CN 114951873 B CN114951873 B CN 114951873B CN 202210664876 A CN202210664876 A CN 202210664876A CN 114951873 B CN114951873 B CN 114951873B
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Classifications
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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
-
- 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
Abstract
The invention discloses a composite solder containing high-entropy alloy, which comprises the following components: high entropy alloy and AgCuTi active solder matrix; the high-entropy alloy accounts for 0.5-2% of the total mass of the composite solder; the high-entropy alloy is Al x CoCrFeNi y Is a high-entropy alloy, x and y are molar ratio, x is more than or equal to 0 and less than or equal to 2; y is more than 0 and less than or equal to 5. The method for brazing and connecting AlN and Cu by using the composite brazing filler metal comprises the following steps: assembling the components to be brazed into a sandwich structure according to Cu/composite brazing filler metal/AlN ceramic; carrying out braze welding connection on the components to be brazed under a vacuum condition; the brazing temperature is 825-875 ℃, and the heat preservation time is 5-20min. The composite solder is used for brazing and connecting AlN and Cu, so that the residual stress of the joint can be relieved, and a high-strength brazing joint is obtained.
Description
Technical Field
The invention belongs to the technical field of brazing, and particularly relates to a composite brazing filler metal containing high-entropy alloy and a method for brazing and connecting AlN and Cu by using the composite brazing filler metal.
Background
Along with the development of science and technology, high-power electronic devices are gradually and widely applied to various fields in industry, and due to the fact that the power of the electronic devices is improved and heat is inevitably generated, the electronic devices are easy to fail after long-term service, and the service life of the electronic devices is reduced. The brazing connection of AlN ceramic and pure Cu is a common method for solving the problem of package failure of the high-power electronic device at present, and the principle is that the heat generated by a chip in the electronic package device is transferred out by utilizing the high heat conductivity of an AlN lining plate and a Cu-coated plate, but the AlN and the Cu respectively belong to ceramic and metal, and the physical parameters and the thermal expansion coefficients are greatly different, so that the problems of wettability and larger residual stress can occur in the brazing connection process, and the connection strength of a brazing joint is lower.
At present, the brazing filler metal for brazing connection of AlN ceramics and pure Cu is mainly AgCuTi system and AgCuInTi system, and the wettability of liquid brazing filler metal on the surface of the ceramics is improved by adding active metal element Ti into the brazing filler metal, so that the connection of the ceramics and metal is promoted. However, the two solders can only solve the wettability problem of the solders on the AlN side, and cannot further relieve the residual stress in the joint, so that crack initiation and even cracking phenomenon can occur when the ceramic bears smaller external load.
Therefore, there is a need to develop a novel brazing filler metal for braze-joining AlN ceramics and Cu for relieving the residual stress of joints and excellent in high-temperature performance.
Disclosure of Invention
Based on the technical problems, the invention provides the composite brazing filler metal containing the high-entropy alloy, which is prepared by matching the high-entropy alloy with the AgCuTi active brazing filler metal with specific composition as a brazing material for brazing connection of AlN ceramic and Cu, so that the residual stress of the joint can be relieved, and the high-strength brazing joint can be obtained.
The specific scheme of the invention is as follows:
the invention provides a composite solder containing high-entropy alloy, which comprises the following components: high entropy alloy and AgCuTi active solder matrix; the high-entropy alloy accounts for 0.5-2% of the total mass of the composite solder;
the high-entropy alloy is Al x CoCrFeNi y Is a high-entropy alloy, x and y are molar ratio, x is more than or equal to 0 and less than or equal to 2; y is more than 0 and less than or equal to 5.
Preferably, the high entropy alloy is Al x The CoCrFeNi series high entropy alloy is that x is more than or equal to 0 and less than or equal to 2.
Preferably, the high entropy alloy is selected from Al 0.5 CoCrFeNi、AlCoCrFeNi、Al 2 Any one of CoCrFeNi.
Preferably, the high entropy alloy is AlCoCrFeNi y Is a high-entropy alloy, and y is more than or equal to 0.1 and less than or equal to 3.
Preferably, the high entropy alloy is selected from AlCoCrFeNi 0.5 、AlCoCrFeNi 2.1 、AlCoCrFeNi 3 Any one of them.
Preferably, the high-entropy alloy accounts for 0.5% -1% of the total mass of the composite solder.
Preferably, the mass fraction of Ti in the AgCuTi active filler metal is less than or equal to 4.5%.
Preferably, the composite brazing filler metal is prepared by taking AgCuTi active brazing filler metal and high-entropy alloy as raw materials and performing ball milling and powder mixing.
The brand of the AgCuTi active solder is not particularly limited, and includes, but is not limited to: agCu-2Ti, agCu-3Ti, agCu-1.8Ti, agCu-1.5Ti, agCu-4.5Ti, etc.
The invention also provides a method for brazing and connecting AlN and Cu, which comprises the following steps: assembling the components to be brazed into a sandwich structure according to Cu/composite brazing filler metal/AlN ceramic; carrying out braze welding connection on the components to be brazed under a vacuum condition; the brazing temperature is 825-875 ℃, and the heat preservation time is 5-20min; the composite solder is any one of the above composite solders.
Preferably, the vacuumVacuum degree of condition is less than or equal to 5 multiplied by 10 -3 Pa, and the pressure is 0.05-0.1MPa.
Compared with the prior art, the beneficial effects are as follows:
the composite brazing filler metal containing the high-entropy alloy can solve the problems of high residual stress and low connection strength of an AlN ceramic copper-clad joint, and can effectively relieve the residual stress to obtain a high-strength brazing joint.
Al originally having high temperature stability x CoCrFeNi y Is high-entropy alloy, and under the brazing material system and brazing condition (brazing temperature 825-875 ℃ and heat preservation time 5-20 min), the high-entropy alloy system is changed, and Al is not existed in the obtained welding line x CoCrFeNi y The high-entropy alloy phase is reacted with Cu and Ti in the AgCuTi active solder matrix in situ to generate (Cu, ni) Ti, tiCoNiFeCu and other low-CTE particle solid phases, so that the thermal expansion coefficient of the solder system is effectively reduced, and the effect of relieving joint stress is achieved.
Based on this, the strengthening mechanism of the invention is: on the one hand, ti and AlN in the AgCuTi active brazing filler metal react to generate a TiN reaction layer with the thickness of about 1 mu m, so that the base metal is reliably connected; on the other hand, when in-situ generated (Cu, ni) Ti, tiCoNiFeCu and other low CTE particle solid phases are used as strengthening phases, the pinning effect on the solder matrix can be achieved, and the joint strength is further improved; meanwhile, the low CTE granular solid phase is uniformly dispersed in the brazing seam, so that the AgCu eutectic phase in the brazing filler metal is thinned, and the thinned AgCu eutectic structure matrix is also beneficial to improving the mechanical properties of the AlN ceramic and Cu braze welding joint.
Drawings
FIG. 1 is an SEM image of a braze joint obtained in example 1;
FIG. 2 is an enlarged view of a portion of an SEM of a soldered joint obtained in example 1;
FIG. 3 is an SEM image of a braze joint obtained in example 2;
fig. 4 is an SEM image of the soldered joint obtained in example 3.
Detailed Description
The technical scheme of the present invention will be described in detail by means of specific examples, which should be explicitly set forth for illustration, but should not be construed as limiting the scope of the present invention.
The composite brazing filler metal containing the high-entropy alloy is prepared by ball milling and powder mixing, and specifically comprises the following components: agCuTi active solder powder and Al x CoCrFeNi y Weighing high-entropy alloy powder according to a proportion; placing the two raw materials and the acetone solution together in a planetary ball mill for ball milling treatment for 1h at a rotating speed of 200r/min, ensuring uniform mixing among the powders, drying, and collecting the composite solder powder. Particle size of the powder<74 μm. Wherein, the AgCuTi active solder actually adopts (AgCu) 98Ti2, and the AgCu is Ag72Cu28.
The shear strength of the obtained braze joint of AlN ceramic and Cu was tested by a universal tester.
Example 1
The composite brazing filler metal containing the high-entropy alloy comprises the following components in percentage by mass: 0.5% AlCoCrFeNi 2.1 High entropy alloy and the balance of AgCuTi active solder matrix.
The method for connecting AlN and Cu by adopting the composite brazing filler metal containing the high-entropy alloy comprises the following specific steps:
(1) Pretreatment of base materials: step-by-step grinding the surfaces of AlN ceramic and Cu to be brazed by adopting sand paper, polishing until no mark exists, then placing the surfaces in an acetone solution for ultrasonic cleaning, taking out the surfaces, placing the surfaces in an alcohol solution for ultrasonic cleaning, and finally drying the surfaces to obtain a base material after surface treatment; wherein Cu is pure copper, and the content of Cu is 99.95-99.99%;
(2) And (3) a component to be brazed: assembling the composite brazing filler metal/AlN ceramic containing the Cu/high-entropy alloy into a to-be-brazed assembly with a sandwich structure;
(3) Vacuum brazing: under vacuum (vacuum degree at 2×10) -3 Pa, the pressure is 0.05 MPa), heating to 300 ℃ from room temperature at a heating rate of 10 ℃/min, and preserving heat for 10min; heating to the brazing temperature of 850 ℃ at the speed of 10 ℃/min, and preserving heat for 10min; and finally cooling to 300 ℃ at the speed of 6 ℃/min, and naturally cooling to room temperature along with a furnace to obtain the soldered joint. The test shows that the shear strength of the soldered joint is 210.6MPa. For the obtained drill rodThe welding head is subjected to scanning electron microscope detection, and low-power and high-power SEM images and partial enlarged images thereof are shown in figures 1 and 2.
It can be seen that the weld joint interface prepared by the method has no phenomena of holes, cracks and the like, and has uniform tissue structure. In combination with EDS and XRD detection, agCu eutectic phases (Ag (s, s), cu (s, s)), cuTi, (Cu, ni) Ti, tiCoNiFeCu, and TiN phases were determined to be included in the joint.
Example 2
The composite brazing filler metal containing the high-entropy alloy comprises the following components in percentage by mass: 1% AlCoCrFeNi 2.1 High entropy alloy and the balance of AgCuTi active solder matrix.
The method for brazing and connecting AlN and Cu by using the composite brazing filler metal containing the high-entropy alloy is the same as that in the embodiment 1, and a braze joint is obtained. The test shows that the shear strength of the soldered joint is 207.4MPa. Scanning electron microscopy was performed on the resulting soldered joint, and a low-power and high-power SEM image thereof was shown in fig. 3.
Example 3
The composite brazing filler metal containing the high-entropy alloy comprises the following components in percentage by mass: 2% AlCoCrFeNi 2.1 High entropy alloy and the balance of AgCuTi active solder matrix.
The method for brazing and connecting AlN and Cu by using the composite brazing filler metal containing the high-entropy alloy is the same as that in the embodiment 1, and a braze joint is obtained. The test shows that the shear strength of the soldered joint is 179.8MPa. Scanning electron microscopy was performed on the resulting soldered joint, and a low-power and high-power SEM image thereof was shown in fig. 4.
Example 4
The composite brazing filler metal containing the high-entropy alloy comprises the following components in percentage by mass: 0.5% AlCoCrFeNi high entropy alloy and the balance of AgCuTi active solder matrix.
The method for connecting AlN and Cu by adopting the composite brazing filler metal containing the high-entropy alloy comprises the following specific steps:
(1) Pretreatment of base materials: step-by-step grinding the surfaces of AlN ceramic and Cu to be brazed by adopting sand paper, polishing until no mark exists, then placing the surfaces in an acetone solution for ultrasonic cleaning, taking out the surfaces, placing the surfaces in an alcohol solution for ultrasonic cleaning, and finally drying the surfaces to obtain a base material after surface treatment; wherein Cu is pure copper, and the content of Cu is 99.95-99.99%;
(2) And (3) a component to be brazed: assembling the composite brazing filler metal/AlN ceramic containing the Cu/high-entropy alloy into a to-be-brazed assembly with a sandwich structure;
(3) Vacuum brazing: under vacuum (vacuum degree at 2×10) -3 Pa, the pressure is 0.05 MPa), heating to 300 ℃ from room temperature at a heating rate of 10 ℃/min, and preserving heat for 10min; heating to a brazing temperature of 875 ℃ at a speed of 10 ℃/min, and preserving heat for 8min; and finally cooling to 300 ℃ at the speed of 6 ℃/min, and naturally cooling to room temperature along with a furnace to obtain the soldered joint.
Example 5
The composite brazing filler metal containing the high-entropy alloy comprises the following components in percentage by mass: 0.5% Al 0.5 CoCrFeNi high entropy alloy and the balance of AgCuTi active solder matrix.
Example 6
The composite brazing filler metal containing the high-entropy alloy comprises the following components in percentage by mass: 0.5% Al 2 CoCrFeNi high entropy alloy and the balance of AgCuTi active solder matrix.
Comparative example 1
A method for braze-joining AlN ceramic and Cu using AgCuTi active braze, the method and control parameters being the same as in example 1, except that the composite braze powder containing the high-entropy alloy in example 1 was replaced with pure AgCuTi active braze powder. Wherein, the AgCuTi active solder actually adopts (AgCu) 98Ti2, and the AgCu is Ag72Cu28.
And testing the shear strength of the obtained soldered joint, wherein the shear strength of the soldered joint is 135.4MPa.
Combining the data and tissue morphology analysis to infer: (1) When the addition amount of the high-entropy alloy is 0.5% -1%, the added particles can be decomposed with Cu and Ti in the AgCuTi active brazing filler metal to generate (Cu, ni) Ti, tiCoNiFeCu and other strengthening phases, so that the shearing strength is improved; (2) When the addition of the high-entropy alloy reaches 2%, a large amount of strengthening phases are generated in the reaction, but at the same time, ti in the brazing filler metal is consumed in a large amount, and at the same time, the brittle strengthening phase brazing filler metal deteriorates the plasticity of the brazing filler metal layer, and the addition of the large-size high-entropy alloy particles increases the brazing seam width, which in turn causes a decrease in the shear strength relative to the addition amount of 0.5%.
The foregoing is only a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art, who is within the scope of the present invention, should make equivalent substitutions or modifications according to the technical scheme of the present invention and the inventive concept thereof, and should be covered by the scope of the present invention.
Claims (8)
1. A method of brazing AlN to Cu, comprising the steps of: assembling the components to be brazed into a sandwich structure according to Cu/composite brazing filler metal/AlN ceramic; carrying out braze welding connection on the components to be brazed under a vacuum condition; the brazing temperature is 825-875 ℃, and the heat preservation time is 5-20min;
the composite solder comprises: high entropy alloy and AgCuTi active solder matrix; the high-entropy alloy accounts for 0.5-1% of the total mass of the composite solder; the high-entropy alloy is Al x CoCrFeNi y Is a high-entropy alloy, x and y are molar ratio, x is more than or equal to 0 and less than or equal to 2; y is more than 0 and less than or equal to 5; the high-entropy alloy system is changed, and Al is no longer present in the welding line x CoCrFeNi y The high-entropy alloy phase is reacted with Cu and Ti in the AgCuTi active brazing filler metal matrix in situ to generate (Cu, ni) Ti and TiCoNiFeCu granular solid phase with low thermal expansion coefficient.
2. The method of brazing AlN to Cu according to claim 1, wherein the high-entropy alloy is Al x The CoCrFeNi series high entropy alloy is that x is more than or equal to 0 and less than or equal to 2.
3. The method of brazing AlN to Cu according to claim 1 or 2, wherein the high-entropy alloy is selected from Al 0.5 CoCrFeNi、AlCoCrFeNi、Al 2 Any one of CoCrFeNi.
4. The method of brazing AlN to Cu according to claim 1, wherein the high-entropy alloy is AlCoCrFeNi y Is a high-entropy alloy, and y is more than or equal to 0.1 and less than or equal to 3.
5. The method of brazing AlN to Cu according to claim 1 or 4, wherein the high entropy alloy is selected from AlCoCrFeNi 0.5 、AlCoCrFeNi 2.1 、AlCoCrFeNi 3 Any one of them.
6. The method for brazing AlN and Cu according to claim 1 or 2, wherein the mass fraction of Ti in the AgCuTi active filler metal is not more than 4.5%.
7. The method for brazing and connecting AlN and Cu according to claim 1 or 2, wherein the composite brazing filler metal is obtained by taking AgCuTi active brazing filler metal and high-entropy alloy as raw materials and performing ball milling and powder mixing.
8. The method for brazing AlN and Cu according to claim 1, wherein the vacuum degree of the vacuum condition is 5X 10 or less -3 Pa, and the pressure is 0.05-0.1MPa.
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| CN202210664876.0A CN114951873B (en) | 2022-06-14 | 2022-06-14 | Composite brazing filler metal containing high-entropy alloy and method for brazing and connecting AlN and Cu by composite brazing filler metal |
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Address after: 310000 No. 372, Jinpeng street, Sandun Industrial Park, Xihu District, Hangzhou City, Zhejiang Province Applicant after: Zhejiang Yatong New Materials Co.,Ltd. Applicant after: JIANG University OF TECHNOLOGY Address before: 310000 No. 372, Jinpeng street, Sandun Industrial Park, Xihu District, Hangzhou City, Zhejiang Province Applicant before: ZHEJIANG ASIA GENERAL SOLDERING & BRAZING MATERIAL Co.,Ltd. Applicant before: JIANG University OF TECHNOLOGY |
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| GR01 | Patent grant | ||
| GR01 | Patent grant |