CN112247397A - Composite brazing filler metal for brazing aluminum nitride ceramic and metal and preparation method thereof - Google Patents
Composite brazing filler metal for brazing aluminum nitride ceramic and metal and preparation method thereof Download PDFInfo
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- CN112247397A CN112247397A CN202011203576.XA CN202011203576A CN112247397A CN 112247397 A CN112247397 A CN 112247397A CN 202011203576 A CN202011203576 A CN 202011203576A CN 112247397 A CN112247397 A CN 112247397A
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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
- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/22—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by the composition or nature of the material
- B23K35/24—Selection of soldering or welding materials proper
- B23K35/30—Selection of soldering or welding materials proper with the principal constituent melting at less than 1550 degrees C
- B23K35/3013—Au as the principal constituent
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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
- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/40—Making wire or rods for soldering or welding
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Abstract
The invention discloses a composite brazing filler metal for brazing aluminum nitride ceramics and metals and a preparation method thereof, wherein the composite brazing filler metal comprises the following components in parts by weight: 85-90 parts of gold powder, 8-15 parts of germanium powder, 0.1-2 parts of nickel sulfide NiS powder, 0-1 part of flaky aluminum nitride powder, 2-3 parts of binder and 7-8 parts of solvent. The composite brazing filler metal can be well adapted to an aluminum nitride ceramic substrate, the residual stress of a joint is reduced, the shearing strength of a joint is improved, the brazing filler metal at the joint is prevented from overflowing, short circuits are reduced, and the brazing quality is more reliable and stable. By adding the flaky aluminum nitride, particularly after the one-dimensional nickel sulfide is loaded on the flaky aluminum nitride, the effects of eliminating the residual stress of the interface and inhibiting the overflow of the brazing filler metal are more prominent, and the brazing quality can be further improved.
Description
Technical Field
The invention relates to the technical field of welding, in particular to a composite brazing filler metal for brazing aluminum nitride ceramics and metals and a preparation method thereof.
Background
Solder means a filler added in or beside the gap thereof in order to achieve bonding of the two materials. The brazing filler metal wets the base metal and forms a solid solution-like structure with the base metal during welding to realize tight combination of welding materials. For the sake of brazing quality, many factors such as melting point, wettability, joint strength, etc. must be considered when selecting the brazing filler metal.
Taking the brazing of an aluminum nitride ceramic substrate and an oxygen-free copper plate to form a copper-clad ceramic substrate as an example, the aluminum nitride substrate has high thermal conductivity (170W/m.K) and thermal expansion coefficient matched with silicon material, and is an ideal ceramic substrate material; the oxygen-free copper has high conductivity and excellent welding performance, and can etch circuit patterns in various shapes like a PCB circuit board. Therefore, the aluminum nitride ceramic oxygen-free copper-coated substrate forms a key device for packaging and connecting the chip and the heat dissipation base of the power module (IGBT) in the power electronic field.
However, when the existing brazing filler metal is used for brazing an aluminum nitride ceramic substrate and a copper plate, the joint has large residual stress, so that the strength of the joint formed by welding is generally low; in addition to the bending strength (350 MPa) and fracture toughness (2.7 MPa. m) of aluminum nitride itself-1/2) Compared with other ceramic materials, the aluminum nitride ceramic substrate is easy to crack in the using process after welding oxygen-free copper due to the existence of residual stress, and the reliability of the whole power module is influenced. Therefore, how to relieve the residual stress in the welded joint of the aluminum nitride ceramic substrate and the copper plate is the key point for manufacturing the high-quality copper-clad ceramic substrate.
Further, with the progress of high integration, the problem of the overflow of the brazing material at the joint is becoming more acute. Avoiding solder at the joint from overflowing and contacting to avoid short circuit is one of the bases for realizing good, stable and reliable thermal cycle of the circuit.
Therefore, it is necessary to develop a composite brazing filler metal that can reduce the residual stress at the joint between the aluminum nitride ceramic substrate and the copper plate and can suppress the overflow of the brazing filler metal at the joint.
Disclosure of Invention
An object of the present invention is to provide a composite brazing material for brazing aluminum nitride ceramics and metals, which can alleviate residual stress in a welded joint between an aluminum nitride ceramic substrate and a copper plate and can suppress the overflow of the brazing material at a joint.
The invention also aims to provide a preparation method of the composite solder for soldering ceramics and metals, which can inhibit the overflow of the solder at the joint and relieve the residual stress in the welded joint of the aluminum nitride ceramic substrate and the copper plate.
In order to achieve the first object, the invention provides the following technical scheme: a composite brazing filler metal for brazing aluminum nitride ceramics and metals comprises the following components in parts by weight: 85-90 parts of gold powder, 8-15 parts of germanium powder, 0.1-2 parts of nickel sulfide NiS powder, 0-1 part of flaky aluminum nitride powder, 2-3 parts of binder and 7-8 parts of solvent.
The gold powder and the germanium powder are combined to form a main body of the brazing filler metal, and the main body and the germanium powder form gold-based eutectic at 356 ℃, so that the aluminum nitride ceramic substrate is well wetted; on the basis, the brazing temperature is 30-50 ℃ higher than the eutectic temperature, the added nickel sulfide NiS is subjected to phase change in the brazing process and is converted into alpha-NiS, and in the process of gradually cooling after brazing, the alpha-NiS is converted into beta-NiS to undergo volume expansion, so that the volume contraction generated in the process of cooling of the gold germanium is partially offset, the thermal expansion coefficient of the brazing filler metal is adapted to the thermal expansion coefficient of the aluminum nitride ceramic substrate, the residual stress in the welded joint of the aluminum nitride ceramic substrate and the copper plate is relieved, and meanwhile, the overflow of the brazing filler metal at the joint is inhibited.
Preferably, the flaky aluminum nitride powder is 0.01 to 1 part by weight. The selected flaky aluminum nitride powder can enhance the wettability of the brazing filler metal to the ceramic substrate, the hard two-dimensional structure of the flaky aluminum nitride powder can be matched with and amplify the volume change of nickel sulfide NiS with a one-dimensional structure, and the volume shrinkage generated when the temperature of the gold germanium is reduced is effectively offset, so that the residual stress in the welding joint of the aluminum nitride ceramic substrate and the copper plate is better relieved, and the overflow of the brazing filler metal at the joint part is inhibited. In order to improve the wettability of the ceramic substrate, it is further preferable that the composite solder comprises the following components in parts by weight: 88 parts of gold powder, 12 parts of germanium powder, 0.1-1 part of nickel sulfide powder, 0.01-0.5 part of flaky aluminum nitride powder, 2-3 parts of binder and 7-8 parts of solvent.
Further preferably, the nickel sulfide powder is supported on the flaky aluminum nitride. Through the load of nickel sulfide on the surface of the flaky aluminum nitride, in the processes of temperature rise and subsequent cooling and cooling in the brazing process, the local single-point volume change of the one-dimensional material of NiS is further amplified through the flaky aluminum nitride of the hard two-dimensional material, so that the residual stress in a welded joint of an aluminum nitride ceramic substrate and a copper plate is relieved better, and the overflow of brazing filler metal at the joint part is inhibited.
Preferably, the flaky aluminum nitride powder has a flake diameter of 3 to 10 μm and a ratio of diameter to thickness of not less than 25; the granularity of the nickel sulfide powder is 300-500 nm; the granularity of the gold powder is 1.5-3.2 mu m, and the granularity of the germanium powder is 300-500 nm. By adopting the particle size matching, the ceramic substrate can be well wetted, and the volume change of the brazing filler metal in the brazing process can be controlled.
Preferably, the binder is polyvinyl acetal; the solvent is terpineol. In addition, the binder and solvent may be other conventional solder binders and solvents.
The brazing temperature of the composite brazing filler metal is 380-400 ℃.
In order to achieve the second purpose of the invention, the invention adopts the following technical scheme: the preparation method of the composite brazing filler metal for brazing the aluminum nitride ceramic and the metal comprises the following steps: weighing gold powder, germanium powder, nickel sulfide powder, flaky aluminum nitride powder, a binder and a solvent according to a ratio; grinding and mixing gold powder and germanium powder by using a grinder, and then drying in vacuum to obtain mixed metal powder; dissolving a binder in a solvent to form a dispersion medium of the composite solder; and finally, adding nickel sulfide powder, flaky aluminum nitride and mixed metal powder into a dispersion medium, and uniformly stirring to obtain the composite solder with uniform components.
Preferably, nickel sulfide powder is supported on the flaky aluminum nitride to form nickel sulfide supported on the aluminum nitride, and then the nickel sulfide supported on the aluminum nitride is added to the dispersion medium. More preferably, the method for loading the nickel sulfide powder on the flaky aluminum nitride comprises the following steps: adding flaky aluminum nitride and nickel sulfide into a polyethylene glycol aqueous solution with the mass percentage concentration of 2-5%, stirring and mixing uniformly, then filtering, and drying in vacuum to obtain the nickel sulfide loaded on the aluminum nitride. Preferably, the weight ratio of the total weight of the flaky alumina and the nickel sulfide to the aqueous polyethylene glycol solution is 1:10 to 1: 50.
Compared with the prior art, the invention has the beneficial effects that: the composite brazing filler metal can better adapt to an aluminum nitride ceramic substrate, reduce the residual stress of a brazed joint, improve the shearing strength of a joint, inhibit the brazing filler metal at the joint from overflowing, reduce short circuit and enable the brazing quality to be more reliable and stable. By adding the flaky aluminum nitride, particularly loading the one-dimensional nickel sulfide on the flaky aluminum nitride, the residual stress of the interface is further effectively eliminated, the overflow of the brazing filler metal is inhibited, and the brazing quality is improved.
Detailed Description
The following further describes embodiments of the present invention with reference to examples. The following embodiments are only used to more clearly illustrate the technical solutions of the present invention, and the protection scope of the present invention is not limited thereby.
Example 1
The composite brazing filler metal for brazing aluminum nitride ceramics and metals comprises the following components in parts by weight: 88 parts of gold powder, 12 parts of germanium powder, 0.5 part of nickel sulfide NiS powder, 2.5 parts of polyvinyl acetal and 7.5 parts of terpineol. Wherein the granularity of the NiS powder is 300-500 nm; the granularity of the gold powder is 1.5-3.2 mu m, and the granularity of the germanium powder is 300-500 nm. The brazing temperature of the composite brazing filler metal is 380-400 ℃, wherein the gold powder and the germanium powder form eutectic at 356 ℃ to form good wetting on the aluminum nitride ceramic substrate; in the process of brazing, nickel sulfide NiS is subjected to phase change and is converted into alpha-NiS, and in the process of gradually cooling after brazing, the alpha-NiS is converted into beta-NiS to undergo volume expansion, so that the volume shrinkage generated when the gold-germanium metal component in the brazing filler metal is cooled is partially offset, the residual stress in the welded joint of the aluminum nitride ceramic substrate and the copper plate is reduced to a certain extent, and meanwhile, the overflow of the brazing filler metal at the joint part is also inhibited.
The preparation method of the composite solder comprises the following steps: weighing gold powder, germanium powder, nickel sulfide powder, polyvinyl acetal and terpineol according to the proportion; grinding and mixing gold powder and germanium powder by using a grinder, and then drying in vacuum to obtain mixed metal powder; dissolving polyvinyl acetal in terpineol to form a dispersion medium of the composite solder; and finally, adding nickel sulfide powder and mixed metal powder into a dispersion medium, and uniformly stirring to obtain the composite solder with uniform components.
Example 2
Different from the embodiment 1, in the embodiment 2, the composition and the parts by weight of the composite solder are as follows: 88 parts of gold powder, 12 parts of germanium powder, 0.5 part of nickel sulfide powder, 0.5 part of flaky aluminum nitride powder, 2.5 parts of polyvinyl acetal and 7.5 parts of terpineol. Wherein the sheet diameter of the sheet aluminum nitride is 3-10 μm, and the ratio of the diameter to the thickness is not less than 25.
The preparation method of the composite solder comprises the following steps: weighing gold powder, germanium powder, nickel sulfide powder, flaky aluminum nitride powder, polyvinyl acetal and terpineol according to the proportion; grinding and mixing gold powder and germanium powder by using a grinder, and then drying in vacuum to obtain mixed metal powder; dissolving polyvinyl acetal in terpineol to form a dispersion medium of the composite solder; and finally, adding nickel sulfide powder, flaky aluminum nitride and mixed metal powder into a dispersion medium, and uniformly stirring to obtain the composite solder with uniform components.
Example 3
Unlike example 2, in example 3, nickel sulfide powder was first supported on the surface of the flaky aluminum nitride and then added to the dispersion medium in the preparation of the composite filler metal. Specifically, gold powder, germanium powder, nickel sulfide powder, flaky aluminum nitride powder, polyvinyl acetal and terpineol are weighed according to a ratio; then grinding and mixing the gold powder and the germanium powder by using a grinder, and then drying in vacuum to obtain mixed metal powder; adding nickel sulfide powder and flaky aluminum nitride into 3% polyethylene glycol aqueous solution by mass percent, selecting the weight ratio of the total weight of the flaky aluminum oxide and the nickel sulfide to the polyethylene glycol aqueous solution to be 1:20, stirring and mixing uniformly, filtering, and drying in vacuum to obtain nickel sulfide loaded on aluminum nitride; and then adding nickel sulfide loaded on aluminum nitride into polyvinyl acetal to be dissolved in a dispersion medium formed by terpineol, adding dried mixed metal powder, and uniformly stirring to obtain the composite solder with uniform components.
Example 4
Different from the embodiment 3, in the embodiment 4, the composition and the parts by weight of the composite solder are as follows: 85 parts of gold powder, 15 parts of germanium powder, 2 parts of nickel sulfide NiS powder, 1 part of flaky aluminum nitride powder, 2 parts of polyvinyl acetal and 8 parts of terpineol. The preparation method of the composite solder is similar to that of the embodiment 3. In the preparation process of the composite solder, 2 parts by weight of nickel sulfide powder and 1 part by weight of flaky aluminum nitride in the composite solder are added into 2 mass percent of polyethylene glycol aqueous solution, the weight ratio of the total weight of the flaky aluminum oxide and the nickel sulfide to the polyethylene glycol aqueous solution is selected to be 1:50, after the mixture is stirred and mixed uniformly, the mixture is filtered and dried in vacuum to obtain the nickel sulfide loaded on the aluminum nitride, and the rest steps are the same as those in the embodiment 3.
Example 5
Different from the embodiment 3, in the embodiment 5, the composition and the parts by weight of the composite solder are as follows: 90 parts of gold powder, 8 parts of germanium powder, 0.1 part of nickel sulfide NiS powder, 0.01 part of flaky aluminum nitride powder, 3 parts of polyvinyl acetal and 7 parts of terpineol. The preparation method of the composite solder is similar to that of the embodiment 3. In the preparation process of the composite solder, 0.1 part by weight of nickel sulfide powder and 0.01 part by weight of flaky aluminum nitride in the composite solder are added into a polyethylene glycol aqueous solution with the mass percentage concentration of 5%, the weight ratio of the total weight of the flaky aluminum oxide and the nickel sulfide to the polyethylene glycol aqueous solution is selected to be 1:10, after the mixture is uniformly stirred and mixed, the mixture is filtered and dried in vacuum to obtain the nickel sulfide loaded on the aluminum nitride, and the rest steps are the same as those in the embodiment 3.
Example 6
Different from the embodiment 3, in the embodiment 6, the composition and the parts by weight of the composite solder are as follows: 90 parts of gold powder, 8 parts of germanium powder, 1 part of nickel sulfide NiS powder, 0.5 part of flaky aluminum nitride powder, 3 parts of polyvinyl acetal and 7 parts of terpineol. The preparation method of the composite solder is similar to that of the embodiment 3. In the preparation process of the composite solder, 1 weight part of nickel sulfide powder and 0.5 weight part of flaky aluminum nitride in the composite solder are added into a polyethylene glycol aqueous solution with the mass percentage concentration of 3%, the weight ratio of the total weight of the flaky aluminum oxide and the nickel sulfide to the polyethylene glycol aqueous solution is selected to be 1:30, after the mixture is uniformly stirred and mixed, the mixture is filtered and dried in vacuum, the nickel sulfide loaded on the aluminum nitride is obtained, and the other steps are the same as those in the embodiment 3.
Comparative example 1
This comparative example is a corresponding solder without the addition of nickel sulphide. Specifically, the brazing filler metal in the comparative example comprises the following components in parts by weight: 88 parts of gold powder, 12 parts of germanium powder, 2.5 parts of polyvinyl acetal and 7.5 parts of terpineol. The brazing filler metal is prepared by the following steps: weighing gold powder, germanium powder, polyvinyl acetal and terpineol according to a ratio; grinding and mixing gold powder and germanium powder by using a grinder, and then drying in vacuum to obtain mixed metal powder; dissolving polyvinyl acetal in terpineol to form a dispersion medium of the composite solder; and finally, adding mixed metal powder into the dispersion medium, and uniformly stirring to obtain the brazing filler metal with uniform components.
The composite solder obtained in the above examples and the corresponding solder in comparative example 1 were subjected to a performance test. The method specifically comprises the following steps: respectively scrubbing an aluminum nitride substrate and an oxygen-free copper plate by using acetone, carrying out tape casting on the brazing filler metal in a suspension form on the aluminum nitride substrate to obtain a composite brazing filler metal film with the thickness of 150 mu m, and then carrying out vacuum drying for 5h at the temperature of 50 ℃. Then fixing the ceramic layer, the brazing material layer and the metal layer together according to the pattern, putting the ceramic layer, the brazing material layer and the metal layer into a vacuum brazing furnace, and controlling the vacuum degree of the brazing furnace to be 10-2-10-3Pa, keeping at 250 ℃ for 1h, then heating to 400 ℃ for sintering for 5min, then cooling to 150 ℃ for 20min, and finally naturally cooling to room temperature along with the furnace. The obtained soldered joint was subjected to a shear test, and the shear strength of the joint was converted from the maximum load output at the time of shearing, and the test results are shown in table 1.
TABLE 1
| Compare comparative example 1 | Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Example 6 |
| Increase in shear Strength (%) | 11% | 18% | 24% | 34% | 17% | 31% |
As a result, it was found that the shear strength of the joints formed by the composite solders of examples 1 to 6 was improved to a different extent than that of the joint formed by comparative example 1 without the addition of the nickel sulfide solder. Particularly, after nickel sulfide loaded on the flaky silicon nitride is added, the shear strength of the connecting joint is improved more obviously. Meanwhile, it was observed from the shape observation of the joints formed by brazing that the solder overflow at the edges of the joints of examples 1 to 6 was significantly less than that of comparative example 1.
Although the preferred embodiments of the present patent have been described in detail, the present patent is not limited to the above embodiments, and various changes can be made without departing from the spirit of the present patent within the knowledge of those skilled in the art.
Claims (10)
1. The composite brazing filler metal for brazing aluminum nitride ceramics and metals is characterized by comprising the following components in parts by weight: 85-90 parts of gold powder, 8-15 parts of germanium powder, 0.1-2 parts of nickel sulfide NiS powder, 0-1 part of flaky aluminum nitride powder, 2-3 parts of binder and 7-8 parts of solvent.
2. The composite filler metal for brazing aluminum nitride ceramics and metals according to claim 1, wherein the flaky aluminum nitride powder is 0.01 to 1 part by weight.
3. The composite solder for brazing aluminum nitride ceramics and metals according to claim 2, wherein the composite solder comprises the following components in parts by weight: 88 parts of gold powder, 12 parts of germanium powder, 0.1-1 part of nickel sulfide powder, 0.01-0.5 part of flaky aluminum nitride powder, 2-3 parts of binder and 7-8 parts of solvent.
4. The composite filler metal for brazing aluminum nitride ceramics and metals according to any one of claims 1 to 3, wherein the nickel sulfide powder is supported on the flaky aluminum nitride.
5. The composite filler metal for brazing aluminum nitride ceramic and metal as claimed in any one of claims 1 to 3, wherein the flaky aluminum nitride powder has a flake diameter of 3 to 10 μm and a ratio of diameter to thickness of not less than 25; the granularity of the nickel sulfide powder is 300-500 nm; the granularity of the gold powder is 1.5-3.2 mu m; the granularity of the germanium powder is 300-500 nm.
6. The composite filler metal for brazing aluminum nitride ceramic and metal as claimed in claim 1, wherein the binder is polyvinyl acetal; the solvent is terpineol.
7. The composite filler metal for brazing aluminum nitride ceramic and metal as claimed in claim 1, wherein the brazing temperature of the composite filler metal is 380-400 ℃.
8. The method for preparing the composite filler metal for brazing aluminum nitride ceramics and metals according to any one of claims 1 to 7, characterized by comprising the steps of: weighing gold powder, germanium powder, nickel sulfide powder, flaky aluminum nitride powder, a binder and a solvent according to a ratio; grinding and mixing gold powder and germanium powder by using a grinder, and then drying in vacuum to obtain mixed metal powder; dissolving a binder in a solvent to form a dispersion medium of the composite solder; and finally, adding nickel sulfide powder, flaky aluminum nitride and mixed metal powder into a dispersion medium, and uniformly stirring to obtain the composite solder with uniform components.
9. The method for producing a composite filler metal for brazing aluminum nitride ceramics and metals according to claim 8, wherein the nickel sulfide powder is supported on the aluminum nitride flakes to form nickel sulfide supported on the aluminum nitride, and then added to the dispersion medium.
10. The method for preparing the composite filler metal for brazing aluminum nitride ceramic and metal according to claim 9, wherein the method for loading the nickel sulfide powder on the flaky aluminum nitride comprises the following steps: adding flaky aluminum nitride and nickel sulfide into a polyethylene glycol aqueous solution with the mass percentage concentration of 2-5%, stirring and mixing uniformly, then filtering, and drying in vacuum to obtain the nickel sulfide loaded on the aluminum nitride.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114669816A (en) * | 2022-04-22 | 2022-06-28 | 湖南省新化县鑫星电子陶瓷有限责任公司 | Alumina ceramic-metal brazing method |
| CN115890058A (en) * | 2022-11-21 | 2023-04-04 | 湖南圣瓷科技有限公司 | Au-based composite brazing filler metal of aluminum nitride ceramic and preparation and brazing methods thereof |
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