CN114951873A - Composite solder containing high-entropy alloy and method for connecting AlN and Cu through brazing - Google Patents
Composite solder containing high-entropy alloy and method for connecting AlN and Cu through brazing Download PDFInfo
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- CN114951873A CN114951873A CN202210664876.0A CN202210664876A CN114951873A CN 114951873 A CN114951873 A CN 114951873A CN 202210664876 A CN202210664876 A CN 202210664876A CN 114951873 A CN114951873 A CN 114951873A
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- entropy alloy
- composite
- filler metal
- aln
- brazing
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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: a 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. Also discloses a method for braze welding AlN and Cu by using the composite solder, which comprises the following steps: assembling components to be brazed with a sandwich structure according to Cu/composite solder/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 5-20 min. The composite solder is used for braze welding of AlN and Cu, can relieve the residual stress of the joint and can obtain a high-strength brazed joint.
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 AlN and Cu by using the composite brazing filler metal.
Background
With the development of science and technology, high-power electronic devices are gradually and widely applied to various fields in industry, and as the power of the electronic devices is improved and heat is inevitably generated, the electronic devices are easy to lose effectiveness after long-term service, and the service life of the electronic devices is shortened. The principle of the method is that the heat generated by a chip in the electronic packaging device is transferred out by utilizing the high thermal conductivity of an AlN lining plate and a Cu-coated plate, but the AlN and the Cu belong to ceramics and metals respectively, and physical parameters and thermal expansion coefficients have large difference, so that the problems of wettability and large residual stress can occur in the brazing connection process, and the brazing joint connection strength is low.
At present, the brazing filler metal for brazing connection of AlN ceramic and pure Cu is mainly AgCuTi system and AgCuInTi system, and active metal element Ti is added into the brazing filler metal to improve the wettability of the liquid brazing filler metal on the surface of the ceramic, so that the connection of the ceramic and the metal is promoted. However, the two solders can only solve the wettability problem of the solder on the AlN side, and cannot further relieve the residual stress in the joint, so that the ceramic may crack even when subjected to a small external load.
Therefore, it is highly desired to develop a novel solder for solder joining of AlN ceramic and Cu which alleviates residual stress of joints and is excellent in high-temperature performance.
Disclosure of Invention
Based on the technical problems, the invention provides a composite solder containing high-entropy alloy, which is characterized in that the high-entropy alloy with specific composition and AgCuTi active solder are matched to be used as a soldering material for soldering connection of AlN ceramic and Cu, so that the residual stress of a joint can be relieved, and a high-strength soldered 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: a 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 has x not less than 0 and not more than 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 solder is less than or equal to 4.5 percent.
Preferably, the composite solder is prepared by taking AgCuTi active solder and high-entropy alloy as raw materials and performing ball milling and powder mixing.
The grade 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 and the like.
The invention also provides a method for connecting AlN and Cu by brazing, which comprises the following steps: assembling components to be brazed with a sandwich structure according to Cu/composite solder/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 5-20 min; the composite solder is the composite solder of any one of the above.
Preferably, the vacuum degree of the vacuum condition is less than or equal to 5 multiplied by 10 -3 Pa, pressure of 0.05-0.1 MPa.
Compared with the prior art, beneficial effect does:
the composite solder containing the high-entropy alloy can solve the problems of large residual stress and low connection strength of the AlN ceramic copper-clad joint, and can effectively relieve the residual stress to obtain a high-strength soldered joint.
Al originally having high temperature stability x CoCrFeNi y Is a high-entropy alloy, and under the brazing temperature of 825-875 ℃ and the brazing condition (the heat preservation time is 5-20min), the high-entropy alloy system is changed, and Al does not exist in the obtained welding line any more x CoCrFeNi y The high-entropy alloy phase reacts with Cu and Ti in an AgCuTi active brazing filler metal matrix in situ to generate particle solid phases with low CTE (copper, Ni) Ti, TiCoNiFeCu and the like, so that the thermal expansion coefficient of a brazing filler metal system is effectively reduced, and the effect of relieving joint stress is achieved.
Based on this, the strengthening mechanism of the invention is: on 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, the in-situ generated particle solid phases with low CTE, such as (Cu, Ni) Ti, TiCoNiFeCu and the like, can play a pinning role on the brazing filler metal matrix when being used as strengthening phases, so that the joint strength is further improved; meanwhile, the low CTE particle solid phase is uniformly dispersed in the brazing seam, which is beneficial to refining the AgCu eutectic phase in the brazing filler metal, the refined AgCu eutectic structure matrix and the improvement of the mechanical property of the brazed joint of AlN ceramic and Cu.
Drawings
FIG. 1 is an SEM photograph of a brazed joint obtained in example 1;
FIG. 2 is a partially enlarged SEM photograph of a brazed joint obtained in example 1;
FIG. 3 is an SEM photograph of a brazed joint obtained in example 2;
fig. 4 is an SEM image of the brazed joint obtained in example 3.
Detailed Description
Hereinafter, the technical solution of the present invention will be described in detail by specific examples, but these examples should be explicitly proposed for illustration, but should not be construed as limiting the scope of the present invention.
The composite solder containing the high-entropy alloy is obtained by ball-milling and mixing powder, and specifically comprises the following steps: mixing 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, performing ball milling treatment for 1h at the rotating speed of 200r/min, ensuring that the powders are uniformly mixed, then drying, and collecting to obtain the composite brazing filler metal powder. Particle size of powder<74 μm. Wherein, the AgCuTi active solder adopts (AgCu)98Ti2 actually, and the AgCu is Ag72Cu 28.
The obtained AlN ceramic and Cu brazed joint was tested for shear strength using a universal testing machine.
Example 1
A composite brazing filler metal containing 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 braze welding connection of AlN and Cu by using the composite brazing filler metal containing the high-entropy alloy comprises the following specific steps:
(1) base material pretreatment: polishing the surfaces of AlN ceramics and Cu to be brazed step by using abrasive paper until no trace exists, then placing the AlN ceramics and Cu in an acetone solution for ultrasonic cleaning, then taking out the AlN ceramics and Cu out, placing the AlN ceramics and Cu in an alcohol solution for ultrasonic cleaning, and finally drying to obtain a parent material after surface treatment; wherein, Cu is pure copper, and the content of Cu is 99.95-99.99%;
(2) the assembly to be brazed: assembling a component to be brazed with a sandwich structure according to Cu/composite brazing filler metal containing high-entropy alloy/AlN ceramic;
(3) vacuum brazing: under vacuum (degree of vacuum of 2X 10) -3 Pa, the pressure is 0.05MPa), the temperature is raised to 300 ℃ from the room temperature at the heating rate of 10 ℃/min, and the temperature is kept for 10 min; then the temperature is raised to the brazing temperature of 850 ℃ at the speed of 10 ℃/min, and the temperature is kept for 10 min; and finally, cooling to 300 ℃ at the speed of 6 ℃/min, and naturally cooling to room temperature along with the furnace to obtain the brazing joint. The test shows that the shear strength of the soldered joint is 210.6 MPa. The obtained soldered joint was examined by scanning electron microscopy, and its low-magnification and high-magnification SEM images and partial enlarged views are shown in fig. 1 and 2.
It can be seen that the welding seam interface prepared by the method has no phenomena of holes, cracks and the like, and has a uniform tissue structure. And combining EDS and XRD detection to determine that the joint comprises AgCu eutectic phases (Ag (s, s), Cu (s, s)), CuTi, (Cu, Ni) Ti, TiCoNiFeCu and TiN phases.
Example 2
A composite brazing filler metal containing 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 braze welding of AlN and Cu by using the composite brazing filler metal containing the high-entropy alloy is the same as that of the embodiment 1, and a brazed joint is obtained. The test shows that the shear strength of the soldered joint is 207.4 MPa. Scanning electron microscope detection is carried out on the obtained soldered joint, and a low-power and high-power SEM image is shown in figure 3.
Example 3
A composite brazing filler metal containing 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 braze welding of AlN and Cu by using the composite brazing filler metal containing the high-entropy alloy is the same as that of the embodiment 1, and a brazed joint is obtained. The test shows that the shear strength of the soldered joint is 179.8 MPa. Scanning electron microscope detection is carried out on the obtained soldered joint, and a low-power and high-power SEM image is shown in FIG. 4.
Example 4
A composite brazing filler metal containing high-entropy alloy comprises the following components in percentage by mass: 0.5 percent of AlCoCrFeNi high-entropy alloy and the balance of AgCuTi active solder matrix.
The method for braze welding connection of AlN and Cu by using the composite brazing filler metal containing the high-entropy alloy comprises the following specific steps:
(1) base metal pretreatment: polishing the surfaces of AlN ceramics and Cu to be brazed step by using abrasive paper until no trace exists, then placing the AlN ceramics and Cu in an acetone solution for ultrasonic cleaning, then taking out the AlN ceramics and Cu out, placing the AlN ceramics and Cu in an alcohol solution for ultrasonic cleaning, and finally drying to obtain a parent material after surface treatment; wherein, Cu is pure copper, and the content of Cu is 99.95-99.99%;
(2) the assembly to be brazed: assembling a component to be brazed with a sandwich structure according to Cu/composite brazing filler metal containing high-entropy alloy/AlN ceramic;
(3) vacuum brazing: under vacuum (degree of vacuum of 2X 10) -3 Pa, the pressure is 0.05MPa), the temperature is raised to 300 ℃ from the room temperature at the heating rate of 10 ℃/min, and the temperature is kept for 10 min; then heating to the brazing temperature of 875 ℃ at the speed of 10 ℃/min, and preserving the heat for 8 min; and finally, cooling to 300 ℃ at the speed of 6 ℃/min, and naturally cooling to room temperature along with the furnace to obtain the brazing joint.
Example 5
A composite brazing filler metal containing high-entropy alloy comprises the following components in percentage by mass: 0.5% of Al 0.5 CoCrFeNi high-entropy alloy and the balance of AgCuTi active solder matrix.
Example 6
A composite brazing filler metal containing high-entropy alloy comprises the following components in percentage by mass: 0.5% of Al 2 CoCrFeNi high-entropy alloy and the balance of AgCuTi active solder matrix.
Comparative example 1
A method for brazing AlN ceramic and Cu by using AgCuTi active brazing filler metal is the same as that in example 1, except that pure AgCuTi active brazing filler metal powder is used instead of the composite brazing filler metal powder containing the high-entropy alloy in example 1. Wherein, the AgCuTi active solder adopts (AgCu)98Ti2 actually, and the AgCu is Ag72Cu 28.
The shear strength of the obtained soldered joint was tested, and the shear strength of the soldered joint was 135.4 MPa.
And (3) combining the data and tissue morphology analysis to deduce: (1) when the addition amount of the high-entropy alloy is 0.5-1%, the added particles can generate decomposition reaction with Cu and Ti in the AgCuTi active solder to generate reinforced phases such as (Cu, Ni) Ti and TiCoNiFeCu, so that the shear strength is improved; (2) when the addition of the high-entropy alloy reaches 2%, although a large amount of strengthening phases are generated by reaction, Ti in the brazing filler metal is consumed in a large amount, meanwhile, the plasticity of a brazing filler metal layer is deteriorated by the brittle strengthening phase brazing filler metal, the width of a brazing seam is increased by adding large-size high-entropy alloy particles, and the shearing strength is reduced relative to the addition amount of 0.5%.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (10)
1. A composite brazing filler metal containing high-entropy alloy is characterized by comprising: a 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.
2. A composite brazing filler metal containing high entropy alloy according to claim 1, wherein the high entropy alloy is Al x The CoCrFeNi series high-entropy alloy has x not less than 0 and not more than 2.
3. A composite filler metal containing high entropy alloy according to claim 1 or 2, characterized in that the high entropy alloy is selected from Al 0.5 CoCrFeNi、AlCoCrFeNi、Al 2 Any one of CoCrFeNi.
4. A composite brazing filler metal containing high entropy alloy 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. A composite brazing filler metal containing high entropy alloy 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. A composite filler metal containing high entropy alloy according to any one of claims 1 to 5, wherein the high entropy alloy accounts for 0.5% -1% of the total mass of the composite filler metal.
7. A composite filler metal containing high-entropy alloy according to any one of claims 1 to 6, wherein the mass fraction of Ti in the AgCuTi active filler metal is not more than 4.5%.
8. A composite brazing filler metal containing high-entropy alloy according to any one of claims 1 to 7, wherein the composite brazing filler metal is obtained by using AgCuTi active brazing filler metal and the high-entropy alloy as raw materials and performing ball milling and powder mixing.
9. A method for braze welding AlN and Cu is characterized by comprising the following steps: assembling components to be brazed with a sandwich structure according to Cu/composite solder/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 5-20 min; a composite filler metal according to any one of claims 1 to 8.
10. The method of brazing AlN to Cu according to claim 9, wherein the vacuum condition is a degree of vacuum of 5 x 10 or less -3 Pa, pressure of 0.05-0.1 MPa.
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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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| CN113182632A (en) * | 2021-05-07 | 2021-07-30 | 浙江工业大学 | Method for connecting C/C composite material by adopting high-entropy alloy brazing |
| KR102303704B1 (en) * | 2020-04-03 | 2021-09-16 | 서울시립대학교 산학협력단 | Lead free solder compositions and manufacturing method of the same |
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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 |