CN108602121B - Solder powder, method for producing the same, and method for producing soldering paste using the same - Google Patents
Solder powder, method for producing the same, and method for producing soldering paste using the same Download PDFInfo
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- CN108602121B CN108602121B CN201680080194.8A CN201680080194A CN108602121B CN 108602121 B CN108602121 B CN 108602121B CN 201680080194 A CN201680080194 A CN 201680080194A CN 108602121 B CN108602121 B CN 108602121B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/17—Metallic particles coated with metal
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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
- B23K35/02—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by mechanical features, e.g. shape
- B23K35/0222—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by mechanical features, e.g. shape for use in soldering, brazing
- B23K35/0244—Powders, particles or spheres; Preforms made therefrom
- B23K35/025—Pastes, creams, slurries
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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
-
- 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
- B23K35/26—Selection of soldering or welding materials proper with the principal constituent melting at less than 400 degrees C
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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
- B23K35/26—Selection of soldering or welding materials proper with the principal constituent melting at less than 400 degrees C
- B23K35/262—Sn 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
- B23K35/22—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
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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
- B23K35/302—Cu 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
Abstract
A metal salt of mixed nickel was added to the copper powder dispersion to obtain a 1 st solution in which the metal salt was dissolved and the copper powder was dispersed. After the pH of the solution was adjusted, 1 st reducing agent was added and mixed to reduce nickel ions, thereby obtaining a dispersion in which precipitated nickel-coated copper powder was dispersed. The liquid was subjected to solid-liquid separation, and the solid content was dried to obtain a metal powder in which a copper core was coated with a diffusion preventing layer made of nickel. To the dispersion of the metal powder, a metal salt of mixed tin was added to obtain a 2 nd solution in which the metal salt was dissolved and the metal powder was dispersed. After the pH of the solution was adjusted, a 2 nd reducing agent was added and mixed to reduce tin ions, thereby obtaining a dispersion in which the precipitated tin-coated metal powder was dispersed. The liquid is subjected to solid-liquid separation, and the solid component is dried, thereby obtaining solder powder in which the metal powder is coated with a tin layer.
Description
Technical Field
The present invention relates to a solder powder for mounting electronic components or the like, in which a core is made of copper and a clad layer includes a tin layer, a method for producing the same, and a method for producing a paste for soldering using the same. In addition, the international application claims that all the contents of patent application 2015-.
Background
Conventionally, solder powder having a central core made of copper and a coating layer made of tin and having an average particle diameter of 5 μm or less has been disclosed (for example, see patent document 1). The solder powder is lead-free and fine in terms of environmental protection, and therefore has excellent printability. Further, since the metal element constituting the central core is copper, not only the clad layer but also the central core are melted at the time of reflow to form a Cu — Sn alloy, the mechanical strength of the solder is improved by the formed Cu — Sn alloy.
However, in the solder powder described in patent document 1 in which the center core is made of copper and the clad layer is made of tin, when the solder powder is stored for a long period of time after the production of the solder powder, since the diffusion coefficient of copper into tin is larger than the diffusion coefficient of tin into copper, there is a possibility that the copper in the center core diffuses into tin in the clad layer, and Cu is formed between the center core and the clad layer3Sn、Cu6Sn5The intermetallic compound layer having a high equi-melting point or the central core has all copper diffused into tin of the clad layer, and the entire clad layer is formed as an intermetallic compound of copper and tin.
In order to solve this problem, a Cu core ball is disclosed which includes a core layer made of a Cu ball and a solder layer made of tin as a main component covering the core layer, and a diffusion preventing layer made of Ni is formed between the Cu ball and the solder layer (for example, see patent document 2). The diffusion preventing layer prevents diffusion of Cu constituting the Cu ball into the solder layer. Patent document 2 discloses a known method for forming a solder layer on a Cu ball, such as an electrolytic plating method such as barrel plating, a method for forming a plating film on a Cu ball by generating a high-speed turbulent flow of a plating solution in a plating tank by a pump connected to the plating tank, a method for forming a plating film on a Cu ball by vibrating the plating solution at a predetermined frequency while agitating the plating solution at a high-speed turbulent flow by providing a vibrating plate in the plating tank, and a method for forming a plating film on a Cu ball by a turbulent flow of the plating solution.
Further, patent document 2 describes that a solder layer contains 40% or more of Sn and 20ppm to 220ppm of Ge, and that a Cu ball having a diameter of 100 μm is coated with an Ni plating layer having a film thickness (one side) of 2 μm, and then an Sn — Ag — Cu — Ge solder plating film having a film thickness (one side) of 18 μm is formed, and that a Cu core ball having a diameter of about 140 μm is shown.
Patent document 1: japanese patent laid-open No. 2008-138266 (claim 1, paragraph [0005] or paragraph [0014 ])
Patent document 2: japanese patent publication No. 5652560 (claim 1, paragraph [0033], paragraph [0035], paragraph [0067], paragraph [0068 ])
However, as described in patent document 2, in the method of coating Cu balls with a diffusion preventing layer made of Ni by nickel plating such as barrel plating, there are problems that the balls adhere to each other and are likely to form aggregated balls, and the thickness of the plating film is likely to vary. Further, when the radius of the Cu ball (copper core) is 1, the diffusion preventing layer made of Ni of the Cu core ball shown in patent document 2 has a thickness ratio of 0.02, and therefore, there is a problem that it is difficult to prevent diffusion of Cu to tin.
Disclosure of Invention
The present invention has as its object 1 the provision of a method for producing a solder powder which, when holding a powder, does not cause copper in the central core to diffuse into tin in the tin layer, does not cause adhesion of the powders to each other, and which has a small variation in the thickness of a diffusion preventing layer made of nickel, and a slurry for soldering using the same. It is another object of the present invention 2 to provide a solder powder which does not cause poor bonding due to insufficient melting of solder even when reflow soldering is performed on a solder powder stored for a long period of time at a temperature at which the solder powder melts before or during storage for a short period of time, a method for producing the same, and a method for producing a soldering paste using the same. It is a further object of the present invention 3 to provide a solder powder which is less likely to be remelted and reduced in bonding strength after reflow and which is particularly suitable for mounting electronic components and the like exposed to a high-temperature environment, a method for producing the same, and a method for producing a paste for soldering using the same.
As shown in fig. 1, a 1 st aspect of the present invention is a method for manufacturing solder powder, including: a step S1 of preparing a 1 st dispersion liquid in which copper powder is dispersed; a step S2 of adding and mixing a metal salt of nickel to the 1 st dispersion of copper powder to prepare a 1 st solution in which the metal salt of nickel is dissolved and the copper powder is dispersed; step S3 of adjusting the pH of the 1 st solution; a step S4 of adding and mixing a 1 st reducing agent to the 1 st solution having the adjusted pH to reduce nickel ions, thereby preparing a 2 nd dispersion in which the precipitated nickel-coated copper powder is dispersed; a step S5 of performing solid-liquid separation on the 2 nd dispersion and drying the solid component of the solid-liquid separation to produce a metal powder in which a copper core is coated with a diffusion-preventing layer made of nickel; a step S6 of preparing a 3 rd dispersion liquid in which the metal powder is dispersed; a step S7 of adding and mixing a metal salt of tin to the 3 rd dispersion of metal powder to prepare a 2 nd solution in which the metal salt of tin is dissolved and the metal powder is dispersed; step S8 of adjusting the pH of the solution No. 2; a step S9 of adding and mixing a 2 nd reducing agent to the pH-adjusted 2 nd solution to reduce tin ions, thereby preparing a 4 th dispersion in which the precipitated tin-coated metal powder is dispersed; and a step S10 of performing solid-liquid separation on the 4 th dispersion and drying the solid component of the solid-liquid separation to produce solder powder in which the metal powder is coated with a tin layer.
As shown in fig. 2, the invention according to claim 2 is a solder powder 10 in which a diffusion preventing layer 12 made of nickel covers a copper core 11, and a metal powder 13 is covered with a tin layer 14. The solder powder has an average particle diameter of 1 to 30 [ mu ] m, a copper content of 2 to 70 mass% relative to 100 mass% of the total solder powder, and a ratio of the thickness of the diffusion preventing layer made of nickel to 0.04 to 0.51 when the radius of the copper core is 1.
The 3 rd aspect of the present invention is a method for producing a soldering paste, which comprises mixing and gelatinizing the solder powder produced by the method according to the 1 st aspect or the solder powder according to the 2 nd aspect with a soldering flux to prepare a soldering paste.
The 4 th aspect of the present invention is a method for mounting an electronic component using the paste for soldering manufactured by the method according to the 3 rd aspect.
In the method for producing a solder powder according to claim 1 of the present invention, the diffusion preventing layer made of nickel is formed on the surface of the copper core by reducing nickel ions in the 1 st solution in which the copper powder is dispersed, and the tin layer is formed on the surface of the metal powder in which the copper core is covered with the diffusion preventing layer made of nickel, thereby producing the solder powder. As a result, unlike the method such as the barrel plating method described in patent document 2, the layer structure of the solder powder has small variations in the respective powders, the powders do not adhere to each other, and variations in the thickness of the diffusion preventing layer made of nickel are also small.
As shown in fig. 2, in the solder powder 10 according to the 2 nd aspect of the present invention, the diffusion preventing layer 12 made of nickel covers the metal powder 13 having the copper core 11 covered therewith, and the thickness of the diffusion preventing layer 12 made of nickel is 0.04 or more and 0.51 or less when the radius of the copper core is 1. That is, in the solder powder 10 of the present invention, since the diffusion preventing layer 12 made of nickel having a predetermined thickness is interposed between the copper core 11 and the tin layer 14, not only can the diffusion of tin from the copper core to the tin layer be prevented, but also the diffusion of copper from the tin layer to the center core can be prevented without greatly changing the soldering characteristics of the conventional solder powder made of a copper core and a tin layer covering the copper core. As a result, the following excellent effects are exhibited: even if the solder powder stored for a long period of time is reflowed at a temperature at which the solder powder melts before or during storage for a short period of time, a poor bonding caused by insufficient melting of the solder does not occur. And, after reflow, formed of Cu3Sn、Cu6Sn5、Ni3Sn、Ni3Sn2、Ni3Sn4、NiSn3、(Ni,Cu)3Sn4、(Ni,Cu)6Sn5And a bonding layer made of an intermetallic compound having a high melting point and copper, and thus re-melting and a reduction in bonding strength are less likely to occur after reflow, and the bonding layer is particularly suitable for mounting electronic components and the like exposed to a high-temperature environment.
The paste for soldering prepared by the method of the 3 rd aspect of the present invention can be obtained using the solder powder of the present invention described above. Therefore, the slurry for welding is melted rapidly at the time of reflow, and has excellent melting properties.
In the method for mounting an electronic component according to claim 4 of the present invention, since the soldering paste of the present invention is used, the electronic component can be mounted easily and with high accuracy by rapid melting of the soldering paste at the time of reflow and excellent melting property. In the bonded body on which the electronic component is mounted, not only the clad layer but also the core-core are melted during reflow to form a Cu — Sn alloy or a Sn — Ni — Cu alloy, and therefore, the formed Cu — Sn alloy or Sn — Ni — Cu alloy is less likely to cause re-melting and a decrease in bonding strength even when the bonded body is exposed to a high-temperature environment after solder bonding.
Drawings
Fig. 1 is a diagram illustrating a manufacturing process of solder powder according to the present embodiment.
Fig. 2 is a cross-sectional view of the solder powder of the present embodiment in which the metal powder in which the copper core is coated with the diffusion preventing layer made of nickel is coated with the tin layer.
Detailed Description
The mode for carrying out the present invention is described below with reference to the drawings.
[ method for producing solder powder ]
Copper powder is used to form the central core. First, as shown in steps S1 and S2 of fig. 1, a 1 st dispersion liquid in which copper powder is dispersed is prepared by adding and mixing copper powder and a dispersant into a solvent, and a 1 st solution in which copper powder is dispersed and a nickel-containing compound is dissolved is prepared by adding and mixing a nickel-containing compound to the first dispersion liquid. The copper powder preferably has an average particle diameter of 0.1 to 27 μm. If the average particle diameter of the copper powder is less than the lower limit, the average particle diameter of the solder powder is likely to be less than 1 μm, the specific surface area increases, and the melting property of the solder is lowered by the influence of the surface oxide layer of the powder. If the average particle size of the copper powder exceeds the upper limit, the average particle size of the solder powder easily exceeds 30 μm. When the average particle size of the solder powder exceeds 30 μm, a problem occurs in that coplanarity of bumps is reduced when forming the bumps, and coating unevenness occurs when coating the pattern surface with the solder, so that the pattern cannot be uniformly coatedThe average particle size of the powder is a volume accumulation Median diameter (Median diameter, D diameter) measured by a particle size distribution measuring device of laser diffraction/scattering type (HORIBA, ltttt transmission = L "&ttt/t &ttttd.) manufactured by a particle size distribution measuring device of laser diffraction/scattering type L a-950), in this specification, the average particle size of the powder is obtained by a physical method such as atomization method in addition to a chemical method based on reduction reaction50)。
The proportions of the copper powder and the nickel compound in the solution 1 are adjusted so that the content ratio of each metal element is in the range described later after the production of the solder powder. Examples of the nickel compound include nickel (II) chloride, nickel (II) sulfate, and nickel (II) nitrate. Examples of the solvent include water, alcohols, ethers, ketones, and esters. Examples of the dispersant include cellulose, vinyl, and polyol, and gelatin, casein, and the like can be used in addition to these.
The pH of the prepared solution 1 was adjusted as shown in step S3 in fig. 1. The pH is preferably adjusted to a range of 0.1 to 2.0 in consideration of re-dissolution of the solder powder to be produced, and the like. Alternatively, the nickel compound may be dissolved in a solvent by adding the nickel compound, and then a dispersant may be added after the nickel is complexed by adding a complexing agent. By adding the complexing agent, nickel ions are not precipitated even when the pH is on the alkali side, and a wide-range synthesis can be performed. Examples of the complexing agent include succinic acid, tartaric acid, glycolic acid, lactic acid, phthalic acid, malic acid, citric acid, oxalic acid, ethylenediaminetetraacetic acid, iminodiacetic acid, nitrilotriacetic acid, and salts thereof.
Next, an aqueous solution in which a reducing agent was dissolved was prepared, and the pH of the aqueous solution was adjusted to the same level as that of the 1 st solution. Examples of the reducing agent include phosphoric acid compounds such as sodium phosphinate, boron hydrides such as sodium tetrahydroborate and dimethylamine borane, nitrogen compounds such as hydrazine, and metal ions such as trivalent titanium ions and divalent chromium ions.
Next, as shown in step S4 of fig. 1, a reducing agent aqueous solution is added to and mixed with the 1 st solution containing nickel ions, whereby nickel ions in the 1 st solution are reduced, thereby preparing a 2 nd dispersion in which precipitated nickel-coated copper powder is dispersed. Examples of the method for mixing the 1 st solution and the aqueous solution of the reducing agent include a method in which the aqueous solution of the reducing agent is added dropwise to the solution in the vessel at a predetermined addition rate and stirred with a stirrer or the like; or a method of using a reaction tube having a predetermined diameter, injecting a double liquid into the reaction tube at a predetermined flow rate, and mixing the two liquids.
Next, as shown in step S5 in fig. 1, the 2 nd dispersion is subjected to solid-liquid separation by decantation or the like, and the recovered solid component is washed with water, an aqueous hydrochloric acid solution adjusted to a pH of 0.5 to 2, an aqueous nitric acid solution, an aqueous sulfuric acid solution, methanol, ethanol, acetone, or the like. After the washing, solid-liquid separation was performed again to recover the solid content. Preferably, the steps from washing to solid-liquid separation are repeated 2 to 5 times. The recovered solid content was vacuum-dried to prepare a metal powder with a Cu core and a Ni layer, the metal powder being composed of a central core (copper core) made of copper and a nickel layer (diffusion preventing layer made of nickel) covering the central core.
Next, as shown in steps S6 and S7 of fig. 1, a 3 rd dispersion in which the metal powder having the Cu nuclei and the Ni layer is dispersed is prepared by adding and mixing the metal powder and the dispersant to the solvent, and a 2 nd solution in which the metal powder having the Cu nuclei and the Ni layer is dispersed and the tin compound is dissolved is prepared by adding and mixing the tin compound to the third dispersion. Examples of the tin compound include tin (II) chloride, tin (II) sulfate, tin (II) acetate, and tin (II) oxalate. The addition ratio of the tin-containing compound is adjusted so that the content ratio of each metal element after the production of the solder powder falls within the range described later. The dispersion medium and the solvent used are the same as those described above.
As shown in step S8 of fig. 1, the pH of the prepared solution 2 was adjusted. The pH is preferably adjusted to a range of 0.1 to 2.0 in consideration of re-dissolution of the solder powder to be produced, and the like. Alternatively, the tin compound may be dissolved by adding the tin compound to a solvent, and then the tin may be complexed by adding a complexing agent, and then a dispersant may be added. By adding the complexing agent, tin ions are not precipitated even when the pH is on the alkali side, and a wide-range synthesis can be performed. As the complexing agent, the same complexing agent as described above is used.
Next, as shown in step S9 of fig. 1, an aqueous reducing agent solution in which the same reducing agent as the above-mentioned reducing agent is dissolved is added and mixed to the above-mentioned tin ion-containing second solution in the same manner as the above-mentioned method, and the tin ions in the second solution are reduced to prepare a precipitated tin-coated metal powder having a Cu core and a Ni layer and dispersed therein as a 4 th dispersion.
Finally, as shown in step S10 of fig. 1, the 4 th dispersion liquid is washed by the same method as the above-described method, and solid-liquid separation is performed to recover the solid component. Preferably, the steps from washing to solid-liquid separation are repeated 2 to 5 times. The recovered solid content was vacuum-dried to prepare solder powder in which the metal powder having a Cu core and a Ni layer was coated with a tin layer.
[ solder powder ]
As shown in fig. 2, in the solder powder 10 produced by the above method, the metal powder 13 in which the copper core 11 of the central core is covered with the diffusion preventing layer 12 made of nickel is covered with the tin layer 14. Since the solder powder has a structure in which the central core made of copper is covered with the coating layer of the tin layer having a low melting point, the melting property at the time of reflow is excellent. Further, since copper and tin are contained in one metal particle constituting the powder, melting unevenness and composition variation at the time of reflow are less likely to occur, and high bonding strength can be obtained. Further, since the solder powder has the diffusion preventing layer made of nickel between the core and the clad layer, it is possible to prevent diffusion of copper into tin and diffusion of tin into copper. Moreover, since Cu is formed after reflow3Sn、Cu6Sn5、Ni3Sn、Ni3Sn2、Ni3Sn4、NiSn3、(Ni,Cu)3Sn4、(Ni,Cu)6Sn5The intermetallic compound and copper having high melting points are not easily remelted and the bonding strength is not easily lowered after reflow, and the bonding layer is particularly suitable for mounting and exposing to a high-temperature environmentElectronic components of (1), and the like.
When the radius of the copper core is 1, the thickness of the diffusion preventing layer 12 made of nickel is 0.04 or more and 0.51 or less. Preferably 0.05 or more and 0.20 or less. If the thickness of the diffusion preventing layer 12 is less than 0.04, diffusion of copper or tin cannot be prevented, and if the thickness of the diffusion preventing layer 12 exceeds 0.51, the fusibility of the solder powder is reduced.
Thus, the solder powder 10 produced by the above method has an average particle diameter of 1 μm or more and 30 μm or less. The reason why the average particle diameter of the solder powder is limited to 1 μm or more and 30 μm or less is as described above.
In the solder powder 10 produced by the above method, the content of copper is 2 mass% or more and 70 mass% or less with respect to 100 mass% of the total amount of the powder. Since conventional solder powder is used as a substitute for Sn — Pb eutectic solder (composition ratio Sn: Pb 63:37 mass%), copper is contained at a ratio of 0.5 to 1.5 mass% for the reason that the melting points are close and the eutectic composition is required. On the other hand, the solder powder produced by the above method contains more than 2 mass% of copper, and thus, after reflow, a Sn-Cu alloy having a high solidification start temperature of about 880 to 600 ℃ or a Sn-Ni-Cu alloy having a high solidification start temperature of about 800 to 400 ℃ is formed. In addition, even if the content ratio of copper is small, after reflow, a Sn — Cu alloy or a Sn — Ni — Cu alloy having a higher solidification start temperature than tin is formed, but by containing more copper, the solidification start temperature is further increased because the ratio of intermetallic compounds having a high melting point in the alloying process is further increased. Thus, the solder bump formed by reflow of the solder paste containing the solder powder has greatly improved heat resistance, and re-melting and a decrease in bonding strength can be prevented. Therefore, it can be suitably used particularly as a high-temperature solder for mounting electronic components and the like exposed to a high-temperature environment. If the content of copper is less than 2 mass%, the solidification start temperature is low, and therefore sufficient heat resistance cannot be obtained in the solder bump formed after reflow, and re-melting occurs when used in a high-temperature environment, and the solder cannot be used as a high-temperature solder. On the other hand, if the content of copper exceeds 70 mass%, the solidification start temperature becomes too high, and the solder is not sufficiently melted, so that a defect in bonding failure may occur. The content of copper in 100 mass% of the total amount of the powder is preferably 10 to 60 mass%.
The content of nickel in the solder powder is 1 mass% or more and less than 15 mass%, preferably 2 to 10 mass%, relative to 100 mass% of the total amount of the solder powder. The thickness of the diffusion preventing layer made of nickel is determined based on the content ratio. If the content of nickel is less than 1 mass%, it is difficult to prevent diffusion of copper or tin, and if the content of nickel exceeds 15 mass%, the problem arises that the fusibility of the solder powder is reduced.
The total amount of the solder powder is 100 mass%, and the content of tin in the solder powder, that is, the remaining portion of the powder excluding the copper and nickel, is 29 mass% or more and less than 97 mass%, preferably 40 to 90 mass%. This is because if the content of tin is less than 29 mass%, the low melting point required for the solder powder is not exhibited at the time of reflow. When the content of tin is 97 mass% or more, the content of copper decreases as a result, and the heat resistance of the solder bump formed after reflow decreases. That is, when the mounted solder is exposed to a high-temperature environment, the mounted solder is remelted or a liquid phase is generated in a part of the solder, which may reduce the bonding strength between the solder and the substrate or the like.
[ slurry for welding and method for producing the same ]
The solder powder produced by the above method can be suitably used as a material for obtaining a paste for soldering by mixing with a flux for soldering and pasting. The soldering paste is prepared by mixing and pasting solder powder and soldering flux at a predetermined ratio. The flux for soldering used for preparing the paste for soldering is not particularly limited, and a flux prepared by mixing components such as a solvent, rosin, a thixotropic agent, and an activator can be used.
Examples of a solvent suitable for preparing the above-mentioned flux for soldering include organic solvents having a boiling point of 180 ℃ or higher, such as diethylene glycol monohexyl ether, diethylene glycol monobutyl ether acetate, tetraethylene glycol, 2-ethyl-1, 3-hexanediol, and α -terpineol.
Examples of the thixotropic agent include hardened castor oil, fatty acid amide, natural oils and fats, synthetic oils and fats, N' -ethylenebis-12-hydroxystearamide, 12-hydroxystearic acid, 1,2,3, 4-dibenzylidene-D-sorbitol, and derivatives thereof.
The active agent is preferably an amine hydrohalide, and specific examples thereof include hydrochloride and hydrobromide salts of amines such as triethanolamine, diphenylguanidine, ethanolamine, butylamine, aminopropanol, polyoxyethylene oleylamine, polyoxyethylene lauryl amine, polyoxyethylene stearamide, diethylamine, triethylamine, methoxypropylamine, dimethylaminopropylamine, dibutylaminopropylamine, ethylhexylamine, ethoxypropylamine, ethylhexyloxypropylamine, dipropylamine, isopropylamine, diisopropylamine, piperidine, 2, 6-dimethylpiperidine, aniline, methylamine, ethylamine, butylamine, 3-amino-1-propene, isopropylamine, dimethylhexylamine, and cyclohexylamine.
The flux for soldering can be obtained by mixing the above components at a predetermined ratio. The solvent is preferably 30 to 60 mass% based on 100 mass% of the total amount of the flux, the thixotropic agent is preferably 1 to 10 mass% based on 100 mass% of the total amount of the flux, and the active agent is preferably 0.1 to 10 mass% based on 100 mass% of the total amount of the flux. If the ratio of the solvent is less than the lower limit, the viscosity of the flux is too high, and the viscosity of the paste for soldering using the flux is increased accordingly, which may cause problems such as frequent decrease in filling property of the solder and decrease in printability such as uneven application. On the other hand, if the ratio of the solvent exceeds the upper limit value, the viscosity of the flux is too low, and therefore the viscosity of the soldering paste using the flux is also lowered, and a problem may occur in which the solder powder and the flux component are precipitated and separated. If the ratio of the thixotropic agent is less than the lower limit value, the viscosity of the soldering paste is too low, and thus the solder powder and the flux component may be precipitated and separated. On the other hand, if the ratio of the thixotropic agent exceeds the upper limit, the viscosity of the paste for soldering becomes too high, and thus a problem of a decrease in printability such as solder filling property or coating unevenness may occur. If the ratio of the activator is less than the lower limit, the solder powder may not be melted, and a sufficient bonding strength may not be obtained, while if the ratio of the activator exceeds the upper limit, the activator may easily react with the solder powder during storage, and thus the storage stability of the soldering paste may be lowered. In addition, a viscosity stabilizer may be added to the soldering flux. Examples of the viscosity stabilizer include polyphenols, phosphoric acid-based compounds, sulfur-based compounds, tocopherols, tocopherol derivatives, ascorbic acid derivatives, and the like which are soluble in a solvent. If the viscosity stabilizer is too large, problems such as a reduction in the melting property of the solder powder may occur, and therefore, it is preferable to be 10 mass% or less.
The amount of the flux for soldering to be mixed in the preparation of the paste for soldering is preferably such that the proportion of the flux in 100 mass% of the paste after the preparation is 5 to 30 mass%. This is because if the mixing amount of the flux for soldering is less than the lower limit value, the flux is insufficient and the paste is difficult to be made, while if the mixing amount of the flux for soldering exceeds the upper limit value, the content ratio of the flux in the paste becomes too large, the content ratio of the metal decreases, and it becomes difficult to obtain a solder bump of a desired size when the solder is melted.
Since the solder powder of the present invention is used as a material in the paste for soldering, the paste is melted rapidly at the time of reflow and has excellent melting property, and on the other hand, the melted solder powder forms an intermetallic compound having a high melting point after reflow and has increased heat resistance, so that re-melting due to heat is less likely to occur. Therefore, the paste for soldering of the present invention can be suitably used particularly for mounting electronic components and the like exposed to a high-temperature environment.
[ mounting method of electronic component Using soldering paste and bonded body ]
When an electronic component such as a silicon chip or an L ED chip is mounted on a substrate such as a heat dissipating substrate, FR4(Flame Retardant Type 4) substrate, Kovar (Kovar) substrate, or the like using the paste for soldering prepared by the above method, the paste for soldering is transferred to a predetermined position on the substrate by a pin transfer method, or the paste for soldering is printed at a predetermined position by a printing method.
Examples
Next, examples of the present invention will be described in detail together with comparative examples.
< example 1 >
First, 4.35 × 10 was added to 50m L water-3mol of nickel (II) sulfate, 9.66 × 10-4mol of sodium phosphinate, 3.29 × 10-4After the pH of the solution was adjusted to 5.0 with sulfuric acid, 0.2g of polyvinyl alcohol 500 (polyvinyl alcohol having an average molecular weight of 500) as a dispersant was added, and further, 3.40g of a dispersion in which 0.2g of polyvinyl alcohol 500 (polyvinyl alcohol having an average molecular weight of 500) as a dispersant was dispersed and copper powder having an average particle size of 0.18 μm was dispersed was added to the solution, followed by stirring at 500rpm for 10 minutes at 50m L to obtain a dispersion in which nickel-coated copper powder in which nickel was precipitated on the surface of copper powder was dispersed, and cleaning was repeated four times or less, wherein the dispersion was left to stand for 60 minutes to precipitate the resultant powder, the supernatant was discarded, 100m L water was added thereto, and the resultant was stirred at 300rpm for 10 minutes, and finally, the dispersion was dried by a vacuum dryer to obtain a powder (coating layer) in which copper was the core and the diffusion barrier layer (nickel-preventing layer) was the diffusion layer 1.
Next, 0.37g of the above powder was dispersed in 50m L of water to prepare a dispersion, and 2.56 × 10-2After the mixed solution was adjusted to pH0.5 with sulfuric acid, 0.5g of polyvinyl alcohol 500 (polyvinyl alcohol having an average molecular weight of 500) as a dispersant was added thereto, and further, the mixed solution was stirred at a rotation speed of 300rpm for 10 minutes, then, 1.58 mol/L of a divalent chromium ion aqueous solution 50m L having a pH adjusted to 0.5 was added thereto at an addition speed of 50m L/min, and the mixed solution was stirred at a rotation speed of 500rpm for 10 minutes to reduce tin ions, thereby obtaining a dispersion in which a nickel-coated copper powder having tin as an outermost layer deposited on the surface of the nickel-coated copper powder was dispersed, and cleaning was repeated four times by leaving the dispersion to stand for 60 minutes to precipitate the resultant powder, discarding the supernatant, adding 100m L water thereto, stirring at a rotation speed of 300rpm for 10 minutes, and finally, the dispersion was dried by a vacuum dryer, thereby obtaining a dispersion having an average particle diameter of 1.1 μm, and having copper as a diffusion preventing layer (core) and a core layer (core layer) of copper as a second diffusion preventing layer (core layer) (1.2).
< examples 2 to 28, comparative examples 1 to 55 >
Solder powder was obtained in the same manner as in example 1, except that in examples 2 to 28 and comparative examples 1 to 55, the particle size of the copper powder and the amount of addition of the copper powder, the amounts of addition of nickel (II) sulfate and tin (II) sulfate, and the ratio of other components were also adjusted so as to control the solder powder to have a predetermined copper central nucleus radius, thicknesses of the nickel diffusion preventing layer and the tin outermost layer, and a predetermined particle size.
< comparative example 56 >
First, 4.35 × 10 was added to 50m L water-3mol of nickel (II) sulfate, 9.66 × 10-4mol of sodium phosphinate, 3.29 × 10-4mol of sodium citrate was stirred for 5 minutes at a rotation speed of 300rpm using a stirrer to prepare a solution. The pH of the solution was adjusted to 5.0 with sulfuric acid, and 0.2g of polyvinyl alcohol 500 (average molecular weight: Mw) was added as a dispersant500 parts of polyvinyl alcohol), and further stirred at a rotation speed of 300rpm for 10 minutes, then, a dispersion in which 0.2g of polyvinyl alcohol 500 (polyvinyl alcohol having an average molecular weight of 500) as a dispersant was dissolved in 50m L of water and 3.40g of copper powder having an average particle diameter of 0.18 μm was dispersed was added to the solution, and stirred at a rotation speed of 500rpm for 10 minutes, to obtain a dispersion in which nickel-coated copper powder in which nickel was precipitated on the surface of the copper powder was dispersed, the operation of leaving the supernatant after the dispersion was allowed to stand for 60 minutes to precipitate the resultant powder, adding 100m L of water thereto, and stirring at a rotation speed of 300rpm for 10 minutes, and finally, the dispersion was dried by a vacuum dryer to obtain a powder in which copper was used as a central core and nickel was used as the 1 st coating layer (diffusion prevention layer).
Then, the powder having copper as a center core and nickel as a diffusion preventing layer was tin-plated using a small barrel apparatus manufactured by YAMAMOTO-MS co., L TD, and a solution in which 5.0g of the powder was dispersed in a plating solution 150m L of sodium stannate 100 g/L, sodium hydroxide 10 g/L and sodium acetate 15 g/L was used as a composition of a plating solution used, and tin was used as an anode, a bath temperature was 50 ℃, a barrel rotation speed was 19rpm, and a voltage was 0.8v as a plating treatment condition, and a plating film thickness was adjusted by a treatment time, and in this comparative example, a dispersion liquid in which a nickel-coated copper powder having an outermost layer of tin, in which tin was deposited on the surface of the nickel-coated copper powder, was dispersed was obtained by leaving the dispersion liquid to stand for 60 minutes, a supernatant was added thereto, and a water-based dispersion liquid was stirred for 100m and dried by a vacuum drier (L minutes) to obtain a final dispersion liquid in which the core-coated copper powder has an average particle size of 300 μm and the core was dried by a vacuum drier (363 μm).
< comparative examples 57 to 65 >
In comparative examples 57 to 65, solder powder was obtained in the same manner as in comparative example 56, except that the particle size of the copper powder used, the amount of addition of the copper powder, the amounts of addition of nickel (II) sulfate and tin (II) sulfate, and the ratios of other components and processing conditions were also adjusted to control the solder powder to have a predetermined copper central nucleus radius, thicknesses of the nickel diffusion preventing layer and the tin outermost layer, and a predetermined particle size.
< comparative test and evaluation >
The solder powders obtained in examples 1 to 28 and comparative examples 1 to 65 were measured for the content of copper [ mass% ], the average particle diameter [ μm ], the average radius of the central core composed of copper [ μm ], the average thickness of the diffusion preventing layer composed of nickel [ μm ], and the average thickness of the clad layer composed of tin [ μm ] by the following methods. The results are shown in tables 1 to 5 below. Then, a paste for soldering was prepared using each of these solder powders, and the bonding strength was evaluated by changing the maximum holding temperature at the time of reflow. The results are shown in tables 6 to 10 below. The average radius of the solder powder was defined as the sum of the average radius of the center core made of copper, the average thickness of the diffusion preventing layer made of nickel, and the average thickness of the coating layer made of tin.
[ Table 1]
[ Table 2]
[ Table 3]
[ Table 4]
[ Table 5]
(1) Analysis of copper content ratio in solder powder: the content ratio of copper in the solder powder was analyzed by inductively coupled plasma emission spectrometry (ICP emission spectrometer ICPS-7510, manufactured by Shimadzu Corporation).
(2) Average particle diameter of solder powder the particle diameter distribution was measured by a particle size distribution measuring device (horiba, laser diffraction/scattering particle size distribution measuring device L a-950) using a laser diffraction scattering method, and the volume cumulative Median diameter (Median diameter, D50) was defined as the average particle diameter of the solder powder.
(3) Measurement of the radius of the central core made of copper, the thickness of the diffusion preventing layer made of nickel, and the thickness of the coating layer made of tin: the solder powder was embedded in a thermosetting epoxy resin, the cross section of the solder powder was dry-polished, and then observed with an Electron Microscope (SEM), and the radius of the center core made of copper, the thickness of the diffusion preventing layer made of nickel, and the thickness of the coating layer made of tin were measured for 30 solder particles, respectively, and the average values of the respective values were obtained. Then, the ratio of the average value of the thicknesses (diffusion preventing layer thickness/radius of the central core) was calculated from the average value of the thicknesses of the diffusion preventing layers made of nickel and the radius of the central core made of copper obtained by the above measurement.
(4) The solder powder was judged for its cohesiveness by measuring the particle size distribution using a particle size distribution measuring device of laser diffraction/scattering type (manufactured by horiba, laser diffraction/scattering particle size distribution measuring device L A-950), and determining that there was "agglomeration" in the case where two or more particle size curves having a distribution peak on the particle size side larger than the desired particle size in addition to the distribution peak of the particle size were present in the obtained particle size distribution curve, and that there was "no" in the case where no such peak was observed.
(5) Bonding strength: flux was prepared by mixing 50 mass% of diethylene glycol monohexyl ether as a solvent, 46 mass% of polymerized rosin (softening point 95 ℃ C.) as a rosin, 1.0 mass% of cyclohexylamine hydrobromide as an active agent, and 3.0 mass% of hardened castor oil as a thixotropic agent. Next, the flux and the solder powder obtained in examples 1 to 28 and comparative examples 1 to 65 were mixed in a ratio of 88 mass% of the flux and 12 mass% of the solder powder, respectively, to prepare a paste for soldering.
The paste prepared above was transferred to a predetermined position of a kovar (Fe — Ni — Co alloy) substrate having a thickness of 0.5mm by a pin transfer method using a pin having a tip diameter of 100 μm, nickel plating was performed on the kovar substrate, and Au flash plating was performed thereon, then, a L ED chip having a thickness of 0.9mm × 0.9.9 mm was mounted on the paste subjected to transfer, and furthermore, the L ED chip and the kovar substrate were bonded by reflow soldering in a nitrogen atmosphere at a predetermined maximum holding temperature for 0.17 hours by an infrared heating furnace while the L ED chip and the substrate were pressed at a pressure of 1.0MPa using a pressing jig, and three bonding samples were obtained for each example or each comparative example by setting the maximum holding temperature at reflow to different temperatures of 250 ℃.
In the table, "excellent" indicates that the relative shear strength is 90 or more, "good" indicates that the relative shear strength is less than 90 to 80, "ok" indicates that the relative shear strength is less than 80 to 70, and "not" indicates that the relative shear strength is less than 70, in the case where the relative shear strength is 100 when the chip package is stored at 300 ℃ for 0 day and 30 days, the lead-free solder test method described in JIS Z3198-7, the "method for measuring the shear strength of solder bonding in a chip package" in section 7.
[ Table 6]
[ Table 7]
[ Table 8]
[ Table 9]
[ Table 10]
The following results were obtained by comparing examples 1 to 28 and comparative examples 1 to 65 in tables 6 to 10.
In the comparative example in which the average particle size of the solder powder was 0.5 μm, the solder powder was not melted before the solder powder was held in the tube due to the influence of the oxide film on the powder surface because the particle size was too small. In the comparative example in which the thickness of the diffusion preventing layer made of nickel is 0.03 when the radius of the copper core is 1, the diffusion of copper or tin cannot be prevented because the thickness of the diffusion preventing layer is too thin, and the bonding strength may not be sufficient. In the comparative example in which the copper content is about 75 mass%, the solidification start temperature is too high because the copper content is too high, and the solder may not be melted at the time of reflow. In the comparative example in which the copper content is about 1.5 mass%, the copper content is too small, the solidification start temperature is lowered, and sufficient heat resistance cannot be obtained, so that the bonding strength may not be obtained.
In the comparative example in which the average particle size of the solder powder is about 40 μm, the particle size is too large, and a bonding layer having large pores (voids) is formed after reflow, and a dense bonding layer cannot be obtained, and therefore, the bonding strength may not be sufficient. In the comparative example in which the ratio of the thickness of the diffusion preventing layer to the radius of the central core is less than 0.04, the diffusion preventing effect is small, and therefore copper diffuses into the clad layer made of tin, which may lower the melting property of the solder powder and make the bonding strength impossible. In contrast, in the comparative example in which the ratio of the thickness of the diffusion preventing layer to the radius of the central core exceeds 0.51, the ratio of nickel is too high, and the melting property of the solder powder is lowered, so that the bonding strength may not be sufficient. In the comparative example in which the coating layer made of tin was formed by barrel plating, since a large amount of strongly aggregated powder was generated, a significantly different value was obtained with respect to the value of the average particle diameter of the solder powder obtained by the laser diffraction scattering method and the average particle diameter of the solder powder obtained by measurement through SEM observation, and a good printed film was not obtained, and the bonding strength was not measured for any of the samples.
On the other hand, in examples 1 to 28 in which the average particle diameter of the solder powder is in the range of 1 μm to 30 μm, the content of copper is in the range of 2 mass% to 70 mass% with respect to 100 mass% of the total amount of the solder powder, and the radius of the copper core is 1, and the thickness of the diffusion preventing layer made of nickel is in the range of 0.04 to 0.51, a good printed film can be obtained with almost no aggregated powder, and the bonding strength is satisfactory, good or excellent at all reflow temperatures of 250 ℃, 300 ℃, and 350 ℃ before and after the solder powder is stored for 30 days.
Industrial applicability
The present invention can be suitably used for producing solder powder which may be stored for a long period of time. Moreover, the present invention can be suitably used for mounting electronic components, and is particularly suitable for mounting electronic components exposed to a high-temperature environment.
Claims (4)
1. A method of manufacturing solder powder, comprising:
preparing a 1 st dispersion of copper powder;
adding and mixing a metal salt of nickel to the 1 st dispersion of copper powder to prepare a 1 st solution in which the metal salt of nickel is dissolved and the copper powder is dispersed;
adjusting the pH of the 1 st solution;
a step of adding and mixing a 1 st reducing agent to the 1 st solution having the adjusted pH to reduce nickel ions, thereby preparing a 2 nd dispersion in which the precipitated nickel-coated copper powder is dispersed;
a step of subjecting the 2 nd dispersion to solid-liquid separation, and drying the solid component of the solid-liquid separation to produce a metal powder in which a copper core is coated with a diffusion-preventing layer made of nickel;
preparing a 3 rd dispersion of the metal powder;
adding and mixing a metal salt of tin to the 3 rd dispersion of the metal powder to prepare a 2 nd solution in which the metal salt of tin is dissolved and the metal powder is dispersed;
adjusting the pH of the 2 nd solution;
a step of adding and mixing a 2 nd reducing agent to the 2 nd solution having the adjusted pH to reduce tin ions, thereby preparing a 4 th dispersion in which the precipitated tin is dispersed while coating the metal powder; and
a step of subjecting the 4 th dispersion to solid-liquid separation and drying the solid component of the solid-liquid separation to produce solder powder in which the metal powder is coated with a tin layer,
the drying of the solid content obtained by solid-liquid separation of the 2 nd dispersion was performed as follows: washing the solid component with water or a hydrochloric acid aqueous solution, a nitric acid aqueous solution, a sulfuric acid aqueous solution, or methanol, ethanol, or acetone having a pH adjusted to 0.5 to 2, washing, performing solid-liquid separation again to recover the solid component, repeating the steps from the washing to the solid-liquid separation 2 to 5 times, and vacuum-drying the recovered solid component.
2. A solder powder in which a metal powder in which a copper core is covered with a diffusion preventing layer made of nickel is covered with a tin layer,
the average particle diameter of the solder powder is 1-30 μm,
the content ratio of copper is 2-70 mass% relative to 100 mass% of the total amount of the solder powder,
the diffusion preventing layer made of nickel has a thickness ratio of 0.04 to 0.51, where the radius of the copper core is 1.
3. A method for producing a soldering paste, comprising mixing and gelatinizing a solder powder produced by the method according to claim 1 or the solder powder according to claim 2 with a soldering flux.
4. A method of mounting an electronic component using the soldering paste manufactured by the method according to claim 3.
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| JP2015244270A JP6587099B2 (en) | 2015-12-15 | 2015-12-15 | Solder powder, method for producing the same, and method for preparing solder paste using the powder |
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| PCT/JP2016/086694 WO2017104562A1 (en) | 2015-12-15 | 2016-12-09 | Solder powder, method for manufacturing same, and method for preparing solder paste using this powder |
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| KR102489331B1 (en) * | 2019-12-31 | 2023-01-17 | 덕산하이메탈(주) | Solder ball and the manufacturing method thereof |
| KR102314236B1 (en) * | 2020-09-22 | 2021-10-19 | 엘티메탈 주식회사 | Bonding paste with high temperature stability and manufacturing method thereof |
| CN112475313B (en) * | 2020-11-11 | 2023-04-28 | 昆明理工大学 | Method for preparing nanoscale solder additive through chemical reaction |
| CN113751922A (en) * | 2021-10-11 | 2021-12-07 | 中国科学院电工研究所 | Lead-free solder and preparation method and application thereof |
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| JP2002120086A (en) * | 2000-10-12 | 2002-04-23 | Sanyo Electric Co Ltd | Lead-free solder and its production method |
| JP4144694B2 (en) | 2002-11-01 | 2008-09-03 | 三井金属鉱業株式会社 | Tin-coated copper powder, method for producing the tin-coated copper powder, and conductive paste using the tin-coated copper powder |
| JP4791685B2 (en) * | 2003-05-22 | 2011-10-12 | シャープ株式会社 | Conductive ball, electrode structure, method of forming electrode of electronic component, electronic component and electronic device |
| JP4494108B2 (en) * | 2004-07-22 | 2010-06-30 | 三井金属鉱業株式会社 | Nickel-coated copper powder manufacturing method, nickel-coated copper powder and conductive paste |
| JP2007075856A (en) * | 2005-09-14 | 2007-03-29 | Nippon Steel Materials Co Ltd | Cu CORE BALL |
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| EP2017031B1 (en) * | 2006-04-26 | 2017-09-13 | Senju Metal Industry Co., Ltd | Solder paste |
| JP2008138266A (en) | 2006-12-04 | 2008-06-19 | Mitsubishi Materials Corp | Solder powder, and solder paste using the same |
| WO2008132933A1 (en) * | 2007-04-13 | 2008-11-06 | Sekisui Chemical Co., Ltd. | Electroconductive fine particles, anisotropic electroconductive material, and electroconductive connection structure |
| JP5736799B2 (en) * | 2011-01-26 | 2015-06-17 | 三菱マテリアル株式会社 | Solder powder and manufacturing method thereof |
| JP5754582B2 (en) * | 2011-02-28 | 2015-07-29 | 三菱マテリアル株式会社 | Precoat solder paste |
| CN102528025A (en) * | 2012-01-31 | 2012-07-04 | 南昌航空大学 | Method for preparing core-shell type copper-based alloy powder capable of resisting high-temperature oxidization |
| JP5367924B1 (en) * | 2012-03-23 | 2013-12-11 | 株式会社Ｎｅｏｍａｘマテリアル | Solder-coated ball and method for manufacturing the same |
| CN103857483B (en) * | 2012-04-23 | 2018-09-25 | Lg化学株式会社 | The core-shell particles for preparing the method for core-shell particles and being prepared by this method |
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| JP5652560B1 (en) * | 2014-02-04 | 2015-01-14 | 千住金属工業株式会社 | Cu core ball, solder paste, foam solder and solder joint |
| CN103894603B (en) * | 2014-04-11 | 2016-04-27 | 上海理凯材料科技有限公司 | The method of zinc-plated copper powder is prepared in electronation |
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