CN114273814A - Brazing filler metal and preparation method thereof - Google Patents
Brazing filler metal and preparation method thereof Download PDFInfo
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- CN114273814A CN114273814A CN202210038543.7A CN202210038543A CN114273814A CN 114273814 A CN114273814 A CN 114273814A CN 202210038543 A CN202210038543 A CN 202210038543A CN 114273814 A CN114273814 A CN 114273814A
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Abstract
The invention provides a brazing filler metal and a preparation method thereof. The present invention provides a brazing filler metal comprising: 0.1 to 3 parts by mass of α -Fe; 0.5 to 15 parts by mass of mullite; 50 to 60 parts by mass of bismuth; 22 to 49.4 parts by mass of tin. The invention solves the problems of unstable connection between the FCBGA device and the substrate and easy failure of welding points, improves the mechanical property and thermal fatigue resistance of the brazing joint by strengthening the brazing joint, and realizes high-performance interconnection of the FCBGA device.
Description
Technical Field
The invention relates to the technical field of electronic interconnection solder, in particular to solder and a preparation method thereof.
Background
FCBGA device is a flip chip ball grid array package form, and flip chip package is widely promoted in the industry by the advantages of high I/O number, small size of welding spot, low electrolyte constant, high reliability and the like. The weight of the chip is supported and the height of the bumps is controlled by mainly utilizing the surface tension of the melting bumps, and the bare chip is mounted on the substrate with the front side facing downwards, so that the packaging method becomes the best choice for high-density, high-performance, multifunctional and high-I/O pin packaging. At the beginning of the FCBGA development, bumps on the surface of the chip were prepared using Sn-Pb solder. With the gradual increase of environmental awareness of people, the european union has led to the introduction of instructions on scrapped electronic and electrical equipment and instructions on prohibition of use of certain harmful substances in electronic and electrical equipment, so that the electronic and electrical equipment is required to comprehensively meet the environmental protection requirements of no lead, no cadmium and no toxicity, and the use of toxic substances such as lead in electronic devices is also required in various ways in the united states, japan, china and the like, so that the conventional Sn-Pb solder needs to be replaced by an environment-friendly lead-free solder.
At present, the lead-free brazing filler metal which is widely applied is five brazing filler metal systems of Sn-Ag-Cu, Sn-Ag, Sn-Bi, Sn-Zn and Sn-Cu, the reaction process of the brazing filler metal and a substrate mainly comprises a Sn matrix and an interface intermetallic compound, but the interface intermetallic compound is a hard brittle phase, and during service, due to the change of environmental temperature, the part near the intermetallic compound is easy to become a stress concentration area, cracks are easy to be generated, and the failure of welding spots is caused. Moreover, compared with the QFP device and the BGA device, the FCBGA device has a large number of bumps, and the bumps can realize the interconnection between the FCBGA device and the substrate through the welding with the substrate. But the number of the area array bumps is larger and can even reach more than 1000. During service, due to the alternating change of temperature, a welding spot array, particularly a corner welding spot, is very easy to become a stress concentration area, and the initiated crack has early failure, so that the failure of the whole electronic device is caused. Therefore, how to develop a novel environment-friendly lead-free solder and improve the high reliability of the FCBGA device becomes an important research topic in the field.
Disclosure of Invention
The invention solves the problems of unstable connection between the FCBGA device and the substrate and easy failure of welding points, improves the mechanical property and thermal fatigue resistance of the brazing joint by strengthening the brazing joint, and realizes high-performance interconnection of the FCBGA device.
In order to solve the above problems, the present invention provides a brazing filler metal, comprising: 0.1 to 3 parts by mass of α -Fe; 0.5 to 15 parts by mass of mullite; 50 to 60 parts by mass of bismuth; 22 to 49.4 parts by mass of tin.
Compared with the prior art, the technical scheme has the following technical effects: and strengthening the soldered joint. The brazing filler metal of the invention achieves the effect of strengthening the welding spot by the coupling effect of alpha-Fe, mullite, bismuth and tin. In 100 parts by mass of the brazing filler metal, 50-60 parts by mass of bismuth and 22-49.4 parts by mass of tin are used as base materials for forming the brazing filler metal, and the bismuth is mainly used for reducing the melting temperature of the brazing filler metal, so that the brazing filler metal is easy to realize welding. After the brazing filler metal is used for brazing, a brazing welding spot comprises an internal structure and an interface structure, wherein the internal structure consists of a bismuth-rich phase and a tin-rich phase, the bismuth-rich phase forms bismuth-rich crystal grains, and the tin-rich phase forms tin-rich crystal grains. In the process of long-term service of a brazing welding spot and an FCBGA device, due to the influence of environmental factors such as temperature and the like, the interface of bismuth-rich grains and tin-rich grains is easy to become a crack initiation area. In the brazing filler metal, bismuth-rich crystal grains and tin-rich crystal grains are connected by adding alpha-Fe; the added mullite is mainly gathered at the grain boundary of the bismuth-rich grains and the tin-rich grains and has the function of fixing alpha-Fe connection. The coupling effect of the alpha-Fe and the mullite strengthens the connection of the bismuth-rich grains and the tin-rich grains, effectively prevents cracks from being generated at the interface of the bismuth-rich grains and the tin-rich grains, and strengthens the soldered joint. After brazing, an intermetallic compound phase is formed in an interface structure area of the brazing welding spot, the intermetallic compound phase is a hard and brittle phase, and the brazing welding spot fails in an early stage due to the excessively thick intermetallic compound phase. In the brazing welding spot formed by the brazing filler metal, part of alpha-Fe and mullite are enriched in an interface structure area, so that element diffusion is prevented, and the rapid growth of an interface intermetallic compound is inhibited. Therefore, the brazing filler metal can form a brazing joint with excellent mechanical property and thermal fatigue resistance, and high-performance interconnection of FCBGA devices is realized.
In one example of the invention, the mullite is a copper coated mullite.
Compared with the prior art, the technical scheme has the following technical effects: enhancing the fixation of the mullite phase. Compared with mullite, the connection effect of copper with the bismuth-rich phase and the tin-rich phase is better, and the mullite phase gathered at the grain boundary of the bismuth-rich grains and the tin-rich grains has better function of fixing the alpha-Fe connection part by coating the mullite with the copper.
In one example of the invention, the copper-coated mullite is a copper-coated mullite submicron particle.
Compared with the prior art, the technical scheme has the following technical effects: and strengthening the soldered joint. The grain diameter of the copper-coated mullite submicron particles is 100-1000 nanometers, and the grain diameter of the particles is very small, so that the effects of reducing dislocation and crack are achieved. The copper-coated mullite submicron particles are gathered at the interface of the bismuth-rich crystal grains and the tin-rich crystal grains, and the generation of surface cracks of the bismuth-rich crystal grains and the tin-rich crystal grains can be reduced while the alpha-Fe connection is fixed, so that the performance of a soldered joint is greatly enhanced, and the high-performance interconnection of an FCBGA device can be better realized.
In one example of the present invention, α -Fe is α -Fe nanowires.
Compared with the prior art, the technical scheme has the following technical effects: and strengthening the soldered joint. The alpha-Fe nanowire has a certain length, is small in diameter, and has the function of preventing crack generation and diffusion. In the brazing filler metal, the alpha-Fe nanowires can also bind and connect bismuth-rich crystal grains and tin-rich crystal grains, so that cracks at the interface of the bismuth-rich crystal grains and the tin-rich crystal grains are prevented, and the effect of strengthening the internal structure of a brazing joint is achieved. Therefore, the generation and the diffusion of cracks in the soldered joint can be greatly reduced by adding the alpha-Fe nanowires into the solder, so that the soldered joint still maintains excellent connection performance under the action of influence factors such as temperature alternation and the like.
In one example of the invention, the mass part ratio of the alpha-Fe nanowire to the copper-coated mullite submicron particle is 1: 5.
Compared with the prior art, the technical scheme has the following technical effects: the soldered joint is remarkably strengthened. In the process of long-term service of a brazing welding spot and an FCBGA device, due to the influence of environmental factors such as temperature and the like, the interface of bismuth-rich grains and tin-rich grains is easy to become a crack initiation area. The addition of the alpha-Fe nanowires can form a network-like structure in the internal structure of the soldered joint, and the alpha-Fe nanowires can bind and connect the bismuth-rich grains and the tin-rich grains. The added copper-coated mullite submicron particles can be gathered at the crystal boundary of the bismuth-rich crystal grains and the tin-rich crystal grains to pin and fix the alpha-Fe nanowire. The coupling effect of the alpha-Fe nanowire and the copper-coated mullite submicron particles strengthens the connection of the bismuth-rich grains and the tin-rich grains, effectively prevents the generation and the diffusion of cracks at the interface of the bismuth-rich grains and the tin-rich grains, and remarkably strengthens the soldered joint. When the mass part ratio of the alpha-Fe nanowire to the copper-coated mullite submicron particles is 1:5, the modification effect can be exerted to the maximum extent, so that the strengthened soldered joint has excellent mechanical property and thermal fatigue resistance, and the high-performance interconnection of FCBGA devices under various use scenes is met.
In one example of the present invention, the solidus temperature of the solder is 138.3 ℃ to 200.2 ℃.
Compared with the prior art, the technical scheme has the following technical effects: the brazing filler metal is easy to weld. The tissues with the same components and structures are collectively called phases, and the solid phase is a phase composed of solids. When the alloy cools, it will be at T1The solid crystals begin to form at the temperature, and then continue to cool, and the temperature is T2The temperature becomes completely solid. As the alloy composition changes, the two temperature points also change, the T of different alloy compositions2The line in the phase diagram of the temperature composition is a solidus line, and phases below the solidus line are all solid phases. The solidus temperature can represent the highest temperature at which the solder is completely solidified into a solid phase, and the solidus temperature of the solder is between 138.3 and 200.2 ℃, which shows that the solder can be solidified from the solid phase within the range of between 138.3 and 200.2 ℃ according to different solder formulasAnd (3) converting into a solid-liquid mixed phase or converting from the solid-liquid mixed phase to a solid phase. Therefore, the solidus temperature of the brazing filler metal is low, so that the brazing filler metal is easy to weld.
In one example of the invention, the liquidus temperature of the solder is 140.1 ℃ to 216.1 ℃.
Compared with the prior art, the technical scheme has the following technical effects: the brazing filler metal is easy to weld. The tissues with the same composition and structure are collectively called phases, and the liquid phase is a phase consisting of liquid. When the alloy cools, it will be at T1The solid crystals begin to form at the temperature, and then continue to cool, and the temperature is T2The temperature becomes completely solid. As the alloy composition changes, the two temperature points also change, the T of different alloy compositions1The lines of the temperature composition in the phase diagram are the liquidus line, above which all the liquid phase is present, and below which the solid phase appears. The liquidus temperature can represent the lowest temperature at which the solder becomes liquid completely, and the liquidus temperature of the solder is 140.1 ℃ to 216.1 ℃, which shows that the solder can be converted into a solid-liquid mixed phase from a liquid phase or a solid-liquid mixed phase into a liquid phase from the liquid phase within the range of 140.1 ℃ to 216.1 ℃ according to different solder formulas. The difference between the liquidus temperature and the solidus temperature of the brazing filler metal is small, so that the brazing filler metal can be rapidly solidified after brazing, welding is realized, and the brazing filler metal is beneficial to forming a brazing joint with good mechanical property.
The invention also provides a preparation method of the brazing filler metal, which is used for preparing the brazing filler metal and comprises the following steps:
s10: preparing a primer according to the proportion, and mixing the primer and the flux paste to prepare a first solder paste;
s20: adding the first additive into the first soldering paste to obtain a second soldering paste;
s30: adding the second additive into the second soldering paste to obtain a solder;
the base material comprises tin and bismuth, the first additive comprises mullite, and the second additive comprises alpha-Fe.
Compared with the prior art, the technical scheme has the following technical effects: used for preparing the brazing filler metal. S10, mixing tin, bismuth and flux paste to obtain the first solder paste. The flux paste contains mixed rosin resin, thixotropic agent, stabilizer, active auxiliary agent, active agent, solvent and other agents, and has the functions of removing surface oxide, preventing surface oxidation of welding material and reducing surface tension of material. The melting point of the flux paste should be 10 ℃ to 30 ℃ lower than that of the solder. S20 is the second solder paste obtained by mixing mullite with the first solder paste sufficiently. And S30, fully mixing the alpha-Fe and the second soldering paste to obtain the final product solder. When the material is actually selected, a nano material, a powder material, or the like of α -Fe can be selected. The solder prepared by the preparation method is easy to realize welding, and the welded joint has good mechanical property and higher thermal fatigue resistance, and can realize high-performance interconnection of FCBGA devices.
In one embodiment of the invention, the tin is tin powder and the bismuth is bismuth powder; and/or the mullite is copper-coated mullite submicron particles; and/or, the alpha-Fe is an alpha-Fe nanowire; and/or the second additive also comprises a dispersant.
Compared with the prior art, the technical scheme has the following technical effects: used for preparing the brazing filler metal. Tin powder and bismuth powder are selected as base materials, on one hand, the tin powder and the bismuth powder can be purchased in the market; on the other hand, compared with the bulk material, the tin powder and the bismuth powder are easier to be uniformly and well combined with the flux paste. When tin powder and bismuth powder are selected, spherical powder is superior to elliptical powder, and the smaller the spherical surface is, the lower the oxidation ability is. The particle size of the copper-coated mullite submicron particles is very small, and the copper-coated mullite submicron particles can be well and uniformly mixed with the first soldering paste. Compared with alpha-Fe powder, the alpha-Fe nanowire can be better prepared to obtain brazing filler metal with excellent performance. The dispersant is added into the second additive, so that the alpha-Fe nanowires can be promoted to be uniformly dispersed in the second solder paste.
In one example of the present invention, includes:
s11: preparing a primer according to the proportion, and mixing the primer and the flux paste to prepare a first solder paste;
s21: preparing a first additive material by adopting a vacuum reaction, and adding the first additive material into the first soldering paste to obtain a second soldering paste;
s31: adding the second additive into the second soldering paste, and stirring to obtain a brazing filler metal;
the base material comprises tin powder and bismuth powder, the first additive comprises copper-coated mullite submicron particles, and the second additive comprises alpha-Fe nanowires and a dispersing agent.
Compared with the prior art, the technical scheme has the following technical effects: used for preparing the brazing filler metal with high connection performance. S11, mixing tin, bismuth and flux paste to obtain the first solder paste. S21, preparing copper-coated mullite submicron particles through vacuum reaction, and then fully mixing the copper-coated mullite submicron particles with the first soldering paste to obtain a second soldering paste. And S31, adding the alpha-Fe nanowires mixed with the dispersing agent into the second soldering paste, and fully mixing to obtain the final solder. The method adopts the sequence that copper is firstly put in to coat mullite submicron particles, and then alpha-Fe nanowires are put in: on one hand, the copper-coated mullite submicron particles are firstly gathered at the interface of the bismuth-rich grains and the tin-rich grains, so that the problem that the copper-coated mullite submicron particles are difficult to enter the grain interface after the bismuth-rich grains and the tin-rich grains are bound by the alpha-Fe nanowire is prevented, and the fixing effect of the copper-coated mullite submicron particles is poor; on the other hand, the alpha-Fe nanowires are easy to curl after being stirred for transition, and can not form a network structure well, so that the strengthening effect is poor. The solder prepared by the preparation method is easy to realize welding, and the soldered joint has excellent mechanical property and thermal fatigue resistance and meets the requirement of high-performance interconnection of FCBGA devices in various use scenes.
The invention also provides a preparation method of the copper-coated mullite submicron particle, which comprises the following steps:
s12: carrying out ultrasonic cleaning on the submicron mullite particles in an ethanol solution, and drying the submicron mullite particles in a drying oven for 20 hours at the temperature of 150 ℃;
s22: putting the dried submicron mullite particles into silica sol for mixing, then adding copper nano powder into the silica sol for fully stirring, and drying the mixture for 10 hours in a drying oven at the temperature of 150 ℃;
s32: and putting the mixture of the submicron mullite particles and the copper nano powder into a 950 ℃ vacuum furnace, and heating for 10 hours through vacuum reaction to form the copper-coated mullite submicron particles.
Compared with the prior art, the technical scheme has the following technical effects: is used for preparing the copper-coated mullite submicron particles. The copper-coated mullite submicron particles prepared by the method have the advantages that the copper layer is uniformly distributed, the particle size of the particles is relatively uniform, and the alpha-Fe joint can be well fixed.
Drawings
FIG. 1 shows the results of the first test.
FIG. 2 shows the results of the second test.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in detail below.
The first embodiment is as follows:
the embodiment provides a solder with the following components: 0.1 part by mass of alpha-Fe nanowire, 0.5 part by mass of copper-coated mullite submicron particles, 57 parts by mass of bismuth and 42.4 parts by mass of tin.
Detecting the main performance of the brazing filler metal: the solidus temperature is about 138.3 ℃, the liquidus temperature is about 140.1 ℃ (considering test errors), and the high-performance composite material has excellent performance.
The embodiment also provides a preparation method of the brazing filler metal, which comprises the following steps:
s10: mixing 57 parts by mass of bismuth powder and 42.4 parts by mass of tin powder with a flux paste to prepare a first solder paste;
s20: preparing copper-coated mullite submicron particles through vacuum reaction treatment;
s30: adding 0.5 part by mass of copper-coated mullite submicron particles into the first soldering paste to obtain a second soldering paste;
s40: and adding 0.1 part by mass of alpha-Fe nanowire mixed with the dispersing agent into the second soldering paste, and fully stirring to prepare the brazing filler metal.
Example two:
the embodiment provides a solder with the following components: 0.2 part by mass of alpha-Fe nanowire, 1 part by mass of copper-coated mullite submicron particles, 57 parts by mass of bismuth and 41.8 parts by mass of tin.
Detecting the main performance of the brazing filler metal: the solidus temperature is about 138.7 ℃, the liquidus temperature is about 140.7 ℃ (considering test errors), and the high-performance composite material has excellent performance.
The embodiment also provides a preparation method of the brazing filler metal, which comprises the following steps:
s10: mixing 57 parts by mass of bismuth powder and 41.8 parts by mass of tin powder with a flux paste to prepare a first flux paste;
s20: preparing copper-coated mullite submicron particles through vacuum reaction treatment;
s30: adding 1 part by mass of copper-coated mullite submicron particles into the first soldering paste to obtain a second soldering paste;
s40: and adding 0.2 part by mass of alpha-Fe nanowire mixed with the dispersing agent into the second soldering paste, and fully stirring to prepare the brazing filler metal.
Example three:
the embodiment provides a solder with the following components: 0.3 part by mass of alpha-Fe nanowire, 1.5 parts by mass of copper-coated mullite submicron particles, 57 parts by mass of bismuth and 41.2 parts by mass of tin.
Detecting the main performance of the brazing filler metal: the solidus temperature is about 139.2 ℃, the liquidus temperature is about 141.5 ℃ (considering test error), and the high-performance composite material has excellent performance.
The embodiment also provides a preparation method of the brazing filler metal, which comprises the following steps:
s10: mixing 57 parts by mass of bismuth powder and 41.2 parts by mass of tin powder with a flux paste to prepare a first flux paste;
s20: preparing copper-coated mullite submicron particles through vacuum reaction treatment;
s30: adding 1.5 parts by mass of copper-coated mullite submicron particles into the first soldering paste to obtain a second soldering paste;
s40: and adding 0.3 part by mass of alpha-Fe nanowire mixed with the dispersing agent into the second soldering paste, and fully stirring to prepare the brazing filler metal.
Example four:
the embodiment provides a solder with the following components: 0.4 part by mass of alpha-Fe nanowire, 2.0 parts by mass of copper-coated mullite submicron particles, 57 parts by mass of bismuth and 40.6 parts by mass of tin.
Detecting the main performance of the brazing filler metal: the solidus temperature is about 140.2 ℃, the liquidus temperature is about 142 ℃ (considering test errors), and the high-performance composite material has excellent performance.
The embodiment also provides a preparation method of the brazing filler metal, which comprises the following steps:
s10: mixing 57 parts by mass of bismuth powder and 40.6 parts by mass of tin powder with a flux paste to prepare a first flux paste;
s20: preparing copper-coated mullite submicron particles through vacuum reaction treatment;
s30: adding 2.0 parts by mass of copper-coated mullite submicron particles into the first soldering paste to obtain a second soldering paste;
s40: and adding 0.4 part by mass of alpha-Fe nanowire mixed with the dispersing agent into the second soldering paste, and fully stirring to prepare the brazing filler metal.
Example five:
the embodiment provides a solder with the following components: 0.5 part by mass of alpha-Fe nanowire, 2.5 parts by mass of copper-coated mullite submicron particles, 57 parts by mass of bismuth and 40.0 parts by mass of tin.
Detecting the main performance of the brazing filler metal: the solidus temperature is about 141.2 ℃, the liquidus temperature is about 143.5 ℃ (considering test error), and the high-performance aluminum alloy has excellent performance.
The embodiment also provides a preparation method of the brazing filler metal, which comprises the following steps:
s10: mixing 57 parts by mass of bismuth powder and 40.0 parts by mass of tin powder with the flux paste to prepare a first solder paste;
s20: preparing copper-coated mullite submicron particles through vacuum reaction treatment;
s30: adding 2.5 parts by mass of copper-coated mullite submicron particles into the first soldering paste to obtain a second soldering paste;
s40: and adding 0.5 part by mass of alpha-Fe nanowire mixed with the dispersing agent into the second soldering paste, and fully stirring to prepare the brazing filler metal.
Example six:
the embodiment provides a solder with the following components: 0.6 part by mass of alpha-Fe nanowire, 3.0 parts by mass of copper-coated mullite submicron particles, 57 parts by mass of bismuth and 39.4 parts by mass of tin.
Detecting the main performance of the brazing filler metal: the solidus temperature is about 142.3 ℃, the liquidus temperature is about 144.7 ℃ (considering test errors), and the high-performance composite material has excellent performance.
The embodiment also provides a preparation method of the brazing filler metal, which comprises the following steps:
s10: mixing 57 parts by mass of bismuth powder and 39.4 parts by mass of tin powder with a flux paste to prepare a first solder paste;
s20: preparing copper-coated mullite submicron particles through vacuum reaction treatment;
s30: adding 3.0 parts by mass of copper-coated mullite submicron particles into the first soldering paste to obtain a second soldering paste;
s40: and adding 0.6 part by mass of alpha-Fe nanowire mixed with the dispersing agent into the second soldering paste, and fully stirring to prepare the brazing filler metal.
Example seven:
the embodiment provides a solder with the following components: 0.7 part by mass of alpha-Fe nanowire, 3.5 parts by mass of copper-coated mullite submicron particles, 57 parts by mass of bismuth and 38.8 parts by mass of tin.
Detecting the main performance of the brazing filler metal: the solidus temperature is about 144.1 ℃, the liquidus temperature is about 147.1 ℃ (considering the test error), and the high-performance composite material has excellent performance.
The embodiment also provides a preparation method of the brazing filler metal, which comprises the following steps:
s10: mixing 57 parts by mass of bismuth powder and 38.8 parts by mass of tin powder with a flux paste to prepare a first solder paste;
s20: preparing copper-coated mullite submicron particles through vacuum reaction treatment;
s30: adding 3.5 parts by mass of copper-coated mullite submicron particles into the first soldering paste to obtain a second soldering paste;
s40: and adding 0.7 mass part of alpha-Fe nanowire mixed with the dispersing agent into the second soldering paste, and fully stirring to prepare the brazing filler metal.
Example eight:
the embodiment provides a solder with the following components: 0.8 part by mass of alpha-Fe nanowire, 4.0 parts by mass of copper-coated mullite submicron particles, 57 parts by mass of bismuth and 38.2 parts by mass of tin.
Detecting the main performance of the brazing filler metal: the solidus temperature is about 145.6 ℃, the liquidus temperature is about 148.9 ℃ (test error is considered), and the high-performance high-temperature-resistant alloy has excellent performance.
The embodiment also provides a preparation method of the brazing filler metal, which comprises the following steps:
s10: mixing 57 parts by mass of bismuth powder and 38.2 parts by mass of tin powder with a flux paste to prepare a first solder paste;
s20: preparing copper-coated mullite submicron particles through vacuum reaction treatment;
s30: adding 4.0 parts by mass of copper-coated mullite submicron particles into the first soldering paste to obtain a second soldering paste;
s40: and adding 0.8 part by mass of alpha-Fe nanowire mixed with the dispersing agent into the second soldering paste, and fully stirring to prepare the brazing filler metal.
Example nine:
the embodiment provides a solder with the following components: 0.9 mass part of alpha-Fe nanowire, 4.5 mass parts of copper-coated mullite submicron particles, 57 mass parts of bismuth and 37.6 mass parts of tin.
Detecting the main performance of the brazing filler metal: the solidus temperature is about 147.5 ℃, the liquidus temperature is about 150.2 ℃ (considering the test error), and the high-performance composite material has excellent performance.
The embodiment also provides a preparation method of the brazing filler metal, which comprises the following steps:
s10: mixing 57 parts by mass of bismuth powder and 37.6 parts by mass of tin powder with a flux paste to prepare a first solder paste;
s20: preparing copper-coated mullite submicron particles through vacuum reaction treatment;
s30: adding 4.5 parts by mass of copper-coated mullite submicron particles into the first soldering paste to obtain a second soldering paste;
s40: and adding 0.9 mass part of alpha-Fe nanowire mixed with the dispersing agent into the second soldering paste, and fully stirring to prepare the brazing filler metal.
Example ten:
the embodiment provides a solder with the following components: 1.0 mass part of alpha-Fe nanowire, 5.0 mass parts of copper-coated mullite submicron particles, 57 mass parts of bismuth and 37 mass parts of tin.
Detecting the main performance of the brazing filler metal: the solidus temperature is about 148.7 ℃, the liquidus temperature is about 152.1 ℃ (considering test errors), and the high-performance composite material has excellent performance.
The embodiment also provides a preparation method of the brazing filler metal, which comprises the following steps:
s10: mixing 57 parts by mass of bismuth powder and 37 parts by mass of tin powder with a flux paste to prepare a first solder paste;
s20: preparing copper-coated mullite submicron particles through vacuum reaction treatment;
s30: adding 5 parts by mass of copper-coated mullite submicron particles into the first soldering paste to obtain a second soldering paste;
s40: and adding 1 part by mass of alpha-Fe nanowire mixed with the dispersing agent into the second soldering paste, and fully stirring to prepare the brazing filler metal.
Example eleven:
the embodiment provides a solder with the following components: 1.1 parts of alpha-Fe nanowire, 5.5 parts of copper-coated mullite submicron particles, 57 parts of bismuth and 36.4 parts of tin.
Detecting the main performance of the brazing filler metal: the solidus temperature is about 150.2 ℃, the liquidus temperature is about 154.1 ℃ (considering test errors), and the high-performance composite material has excellent performance.
The embodiment also provides a preparation method of the brazing filler metal, which comprises the following steps:
s10: mixing 57 parts by mass of bismuth powder and 36.4 parts by mass of tin powder with a flux paste to prepare a first solder paste;
s20: preparing copper-coated mullite submicron particles through vacuum reaction treatment;
s30: adding 5.5 parts by mass of copper-coated mullite submicron particles into the first soldering paste to obtain a second soldering paste;
s40: and adding 1.1 parts by mass of alpha-Fe nanowires mixed with the dispersant into the second solder paste, and fully stirring to prepare the brazing filler metal.
Example twelve:
the embodiment provides a solder with the following components: 1.2 parts of alpha-Fe nanowire, 6 parts of copper-coated mullite submicron particles, 57 parts of bismuth and 35.8 parts of tin.
Detecting the main performance of the brazing filler metal: the solidus temperature is about 152.3 ℃, the liquidus temperature is about 157.7 ℃ (considering test error), and the high-performance composite material has excellent performance.
The embodiment also provides a preparation method of the brazing filler metal, which comprises the following steps:
s10: mixing 57 parts by mass of bismuth powder and 35.8 parts by mass of tin powder with a flux paste to prepare a first solder paste;
s20: preparing copper-coated mullite submicron particles through vacuum reaction treatment;
s30: adding 6 parts by mass of copper-coated mullite submicron particles into the first soldering paste to obtain a second soldering paste;
s40: and adding 1.2 parts by mass of alpha-Fe nanowires mixed with the dispersant into the second solder paste, and fully stirring to prepare the brazing filler metal.
Example thirteen:
the embodiment provides a solder with the following components: 1.3 parts of alpha-Fe nanowire, 6.5 parts of copper-coated mullite submicron particles, 57 parts of bismuth and 35.2 parts of tin.
Detecting the main performance of the brazing filler metal: the solidus temperature is about 155.4 ℃, the liquidus temperature is about 159.6 ℃ (test error is considered), and the high-performance aluminum alloy has excellent performance.
The embodiment also provides a preparation method of the brazing filler metal, which comprises the following steps:
s10: mixing 57 parts by mass of bismuth powder and 35.2 parts by mass of tin powder with a flux paste to prepare a first flux paste;
s20: preparing copper-coated mullite submicron particles through vacuum reaction treatment;
s30: adding 6.5 parts by mass of copper-coated mullite submicron particles into the first soldering paste to obtain a second soldering paste;
s40: and adding 1.3 parts by mass of alpha-Fe nanowires mixed with the dispersant into the second solder paste, and fully stirring to prepare the brazing filler metal.
Example fourteen:
the embodiment provides a solder with the following components: 1.4 parts of alpha-Fe nanowire, 7 parts of copper-coated mullite submicron particles, 57 parts of bismuth and 34.6 parts of tin.
Detecting the main performance of the brazing filler metal: the solidus temperature is about 152.3 ℃, the liquidus temperature is about 157.7 ℃ (considering test error), and the high-performance composite material has excellent performance.
The embodiment also provides a preparation method of the brazing filler metal, which comprises the following steps:
s10: mixing 57 parts by mass of bismuth powder and 34.6 parts by mass of tin powder with a flux paste to prepare a first solder paste;
s20: preparing copper-coated mullite submicron particles through vacuum reaction treatment;
s30: adding 7 parts by mass of copper-coated mullite submicron particles into the first soldering paste to obtain a second soldering paste;
s40: and adding 1.4 parts by mass of alpha-Fe nanowires mixed with the dispersant into the second solder paste, and fully stirring to prepare the brazing filler metal.
Example fifteen:
the embodiment provides a solder with the following components: 3 parts of alpha-Fe nanowire, 15 parts of copper-coated mullite submicron particles, 50 parts of bismuth and 32 parts of tin.
Detecting the main performance of the brazing filler metal: the solidus temperature is about 190 ℃, the liquidus temperature is about 204.2 ℃ (considering test errors), and the high-performance composite material has excellent performance.
The embodiment also provides a preparation method of the brazing filler metal, which comprises the following steps:
s10: mixing 50 parts by mass of bismuth powder and 32 parts by mass of tin powder with a flux paste to prepare a first flux paste;
s20: preparing copper-coated mullite submicron particles through vacuum reaction treatment;
s30: adding 15 parts by mass of copper-coated mullite submicron particles into the first soldering paste to obtain a second soldering paste;
s40: and adding 3 parts by mass of alpha-Fe nanowires mixed with the dispersing agent into the second soldering paste, and fully stirring to prepare the brazing filler metal.
Example sixteen:
the embodiment provides a solder with the following components: 3 parts of alpha-Fe nanowire, 15 parts of copper-coated mullite submicron particles, 60 parts of bismuth and 22 parts of tin.
Detecting the main performance of the brazing filler metal: the solidus temperature is about 200.2 ℃, the liquidus temperature is about 216.1 ℃ (considering test errors), and the high-performance composite material has excellent performance.
The embodiment also provides a preparation method of the brazing filler metal, which comprises the following steps:
s10: mixing 60 parts by mass of bismuth powder and 22 parts by mass of tin powder with a flux paste to prepare a first flux paste;
s20: preparing copper-coated mullite submicron particles through vacuum reaction treatment;
s30: adding 15 parts by mass of copper-coated mullite submicron particles into the first soldering paste to obtain a second soldering paste;
s40: and adding 3 parts by mass of alpha-Fe nanowires mixed with the dispersing agent into the second soldering paste, and fully stirring to prepare the brazing filler metal.
Example seventeen:
test one: under the condition that the content of copper-coated mullite submicron particles and bismuth is fixed, the content of alpha-Fe nanowires in the brazing filler metal is changed, the shear strength of a brazing joint formed by the brazing filler metals with different components is detected, and the detection result is shown in figure 1. Table 1 shows the solder compositions of the 9 experimental groups.
TABLE 1
As can be seen from fig. 1, the coupling of the α -Fe nanowire, the copper-coated mullite submicron particle, bismuth, and tin can significantly improve the shear strength of the soldered joint.
And (2) test II: the shearing performance of the soldered joints with two different components of Sn-58Bi and Sn-58Bi-10(2SiO 2.3 Al2O3) -2.0 alpha-Fe during service under different numbers of thermal cycles is detected. Wherein Sn-58Bi represents that the joint contains 58 parts by mass of bismuth and 42 parts by mass of tin; sn-58Bi-10(2SiO 2.3 Al2O3) -2.0 alpha-Fe means that the joint contains 58 parts by mass of bismuth, 10 parts by mass of mullite, 2 parts by mass of alpha-Fe nanowire and 30 parts by mass of tin. The detection result is shown in fig. 2, and it can be seen from fig. 2 that the thermal fatigue resistance of the brazed joint strengthened by the α -Fe nanowire and the mullite is significantly improved.
Although the present invention is disclosed above, the present invention is not limited thereto. Various changes and modifications may be effected therein by one skilled in the art without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (10)
1. A brazing filler metal, comprising:
0.1 to 3 parts by mass of α -Fe;
0.5 to 15 parts by mass of mullite;
50 to 60 parts by mass of bismuth;
22 to 49.4 parts by mass of tin.
2. Brazing filler metal according to claim 1, wherein the mullite is copper coated mullite.
3. The braze of claim 2 wherein the copper coated mullite is a copper coated mullite submicron particle.
4. The brazing filler metal of claim 3, wherein the α -Fe is α -Fe nanowires.
5. The brazing filler metal according to claim 4, wherein the mass part ratio of the alpha-Fe nanowires to the copper-coated mullite submicron particles is 1: 5.
6. A brazing filler metal according to claim 1, wherein the brazing filler metal has a solidus temperature of 138.3 ℃ to 200.2 ℃.
7. Solder according to claim 1, characterized in that the liquidus temperature of the solder is between 140.1 ℃ and 216.1 ℃.
8. A method for producing a filler metal, characterized by comprising, for producing the filler metal of claims 1 to 7:
s10: preparing a primer according to the proportion, and mixing the primer and the flux paste to prepare a first solder paste;
s20: adding a first additive into the first soldering paste to obtain a second soldering paste;
s30: adding a second additive into the second soldering paste to obtain the solder;
the base material comprises tin and bismuth, the first addition material comprises mullite, and the second addition material comprises alpha-Fe.
9. The method according to claim 8,
the tin is tin powder, and the bismuth is bismuth powder; and/or
The mullite is copper-coated mullite submicron particles; and/or
The alpha-Fe is an alpha-Fe nanowire; and/or
The second additive also comprises a dispersant.
10. The method of claim 8, comprising:
s11: preparing the primer according to the proportion, and mixing the primer and the soldering paste to prepare the first soldering paste;
s21: preparing the first additive material by adopting a vacuum reaction, and adding the first additive material into the first soldering paste to obtain the second soldering paste;
s31: adding the second additive into the second soldering paste, and stirring to obtain the brazing filler metal;
the base material comprises tin powder and bismuth powder, the first additive comprises copper-coated mullite submicron particles, and the second additive comprises alpha-Fe nanowires and a dispersing agent.
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