CN113070604A - Double-layer solder sheet and preparation process thereof - Google Patents
Double-layer solder sheet and preparation process thereof Download PDFInfo
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- CN113070604A CN113070604A CN202110374896.XA CN202110374896A CN113070604A CN 113070604 A CN113070604 A CN 113070604A CN 202110374896 A CN202110374896 A CN 202110374896A CN 113070604 A CN113070604 A CN 113070604A
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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
-
- 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
- B23K35/0233—Sheets, foils
-
- 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
- B23K35/36—Selection of non-metallic compositions, e.g. coatings, fluxes; Selection of soldering or welding materials, conjoint with selection of non-metallic compositions, both selections being of interest
- B23K35/3612—Selection of non-metallic compositions, e.g. coatings, fluxes; Selection of soldering or welding materials, conjoint with selection of non-metallic compositions, both selections being of interest with organic compounds as principal constituents
- B23K35/3613—Polymers, e.g. resins
-
- 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
- B23K35/36—Selection of non-metallic compositions, e.g. coatings, fluxes; Selection of soldering or welding materials, conjoint with selection of non-metallic compositions, both selections being of interest
- B23K35/362—Selection of compositions of fluxes
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- Engineering & Computer Science (AREA)
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- Electric Connection Of Electric Components To Printed Circuits (AREA)
Abstract
The invention relates to the technical field of solder sheet preparation, in particular to a double-layer solder sheet and a preparation process thereof; the structure is a sandwich structure consisting of two layers of solder sheets and soldering flux positioned in the middle of the two layers of solder sheets; the solder sheet is made of SnAgCu alloy, and the specific alloy content of the solder sheet is Sn: 95-96%, Ag: 2.5-3.5% and the balance of copper; the soldering flux consists of the following raw materials: rosin modified phenolic epoxy resin, hydrogenated rosin resin, methyl hexahydrophthalic anhydride, 2-ethyl-4-methylimidazole, a diluent, an activator, a surfactant, a corrosion inhibitor, a thixotropic agent, a film-forming assistant and the balance of an addition assistant; when the flux is used in welding operation, the quantity of the used scaling powder is easy to control accurately, and the phenomenon of poor welding quality caused by welding 'cavities' and excessive welding residues can be effectively reduced; moreover, the oxidation rate of the metal raw materials can be effectively reduced, and the welding quality and quality are ensured.
Description
Technical Field
The invention relates to the technical field of solder sheet preparation, in particular to a double-layer solder sheet and a preparation process thereof.
Background
With the development of electronic packaging technology, people have higher and higher requirements on the performance of small-sized, high-power and high-frequency power devices. Soldering is a welding method in which a low-melting-point metal solder is melted by heating and then penetrates into and fills a gap at a joint of metal parts. The solder is named because the solder is usually tin-based alloy. Soldering irons are commonly used as heating tools, which are widely used in the electronics industry.
Solder sheets are increasingly used in the field of soldering as a raw material commonly used in the field of soldering. However, in military industry, the solder sheet used in China is of a single-layer structure. Although the soldering flux can play a certain role in soldering, the soldering flux needs to be coated on the surface of the substrate during soldering operation, the quantity of the soldering flux is difficult to accurately control, and the phenomenon of void and more soldering residues can be caused due to excessive use of the soldering flux; the soldering flux consumption is less, and the soldering flux effect is not realized; this seriously affects the quality and quality of the weld. In addition, the metal substances in the solder sheet used in the soldering process are easily oxidized, thereby affecting the quality of soldering.
Based on this, the invention provides a double-layer solder sheet and a preparation process thereof, so as to solve the above problems.
Disclosure of Invention
The invention aims to provide a double-layer welding flux sheet and a preparation process thereof, wherein the quantity of the used scaling powder is easy to control accurately in the welding operation, so that the phenomenon of poor welding quality caused by welding 'holes' and excessive welding residues can be effectively reduced; moreover, the oxidation rate of the metal raw materials can be effectively reduced, and the welding quality and quality are ensured.
In order to achieve the purpose, the invention provides the following technical scheme:
a double-layer solder sheet is a sandwich structure consisting of two layers of solder sheets and soldering flux positioned in the middle of the two layers of solder sheets;
the solder sheet is made of SnAgCu alloy, and the specific alloy content of the solder sheet is Sn: 95-96%, Ag: 2.5-3.5% and the balance of copper;
the soldering flux comprises the following raw materials in percentage by weight: 40-50% of rosin modified phenolic epoxy resin, 8-12% of hydrogenated rosin resin, 3-10% of methyl hexahydrophthalic anhydride, 1.8-5% of 2-ethyl-4-methylimidazole, 4-12% of diluent, 1.5-3.2% of activating agent, 0.3-0.8% of surfactant, 0.1-0.5% of corrosion inhibitor, 2-5% of thixotropic agent, 0.5-2.5% of film forming additive and the balance of additive.
Furthermore, the diluent is any one of dodecyl glycidyl ether and polyethylene glycol diglycidyl ether.
Furthermore, the activating agent is prepared from an amine organic substance and an organic acid according to a mass ratio of 5-9: 1 mixing and blending; the amine organic matter is any one of diethanolamine and triethanolamine; the organic acid is selected from any one of succinic acid, itaconic acid and sorbic acid.
Furthermore, the surfactant is any one of octylphenol polyoxyethylene ether, isooctylphenol polyoxyethylene ether and nonionic fluorocarbon surfactant.
Furthermore, the corrosion inhibitor is any one of benzotriazole and hydrazine hydrate.
Further, the thixotropic agent is selected from any one of kaolin, polyamide wax or hydrogenated castor oil.
Furthermore, the film forming auxiliary agent is any one of glycerol, polyethylene glycol 1000 and polyethylene glycol 2000.
Furthermore, the preparation method of the addition auxiliary agent comprises the following steps: adding porous metal powder and polyacrylic acid into isopropanol, uniformly mixing by ultrasonic waves, and heating the obtained mixed component; mixing and stirring the porous metal powder under the protection of inert gas after the porous metal powder is melted; then transferring the obtained mixed material to an emulsifying machine for emulsification and dispersion treatment, and finally cooling to obtain alloy micro powder; ball-milling the obtained alloy micro powder to 1.2-1.8 μm, and immersing the alloy micro powder in polyether dimethyl silicone oil; and after filtering, drying the obtained alloy micro powder at the temperature of 40-55 ℃ to obtain the finished product of the addition agent.
Still further, the method for preparing the porous metal powder comprises the steps of:
i, 95.5: 2.5: 2.0, accurately weighing proper amounts of tin powder, zinc powder and indium powder with the particle size of 100-200 nm respectively; mixing the three metal powders, and then transferring the mixture into a planetary ball mill for ball milling for 8-12 h; adding stearic acid with the mass being 60-70% of the volume of a grinding tank of the ball mill as a process control agent in the ball milling process;
II, mixing the mixed powder subjected to ball milling with sodium chloride according to the volume ratio of 40-75%, and then putting the mixed powder into a ball milling tank; after vacuum mixing, tabletting the obtained mixed powder, and storing the obtained blank for later use;
III, placing the obtained blank in a muffle furnace, and sintering at high temperature for 8-15 h under the condition of inert gas; after sintering, soaking the sintered material in deionized water at the temperature of 50-65 ℃ for heat preservation for 10-15 h; after filtering, sequentially cleaning and drying the obtained solid materials; and obtaining the finished product of the porous metal powder.
A preparation process of a double-layer solder sheet comprises the following steps:
s1, accurately weighing appropriate amount of metal raw materials and soldering flux for manufacturing the solder sheet according to the formula; then, the melt obtained after the metal raw materials are mixed and melted is poured into a crystallizer from a storage container in a controlled way, and the melt is cast into a strip by a belt type continuous casting machine or a block casting machine; wherein, when casting the material, a continuous casting strip with the thickness of 3-8 mm is pulled out in a controlled manner, the average cooling speed along the thickness of the strip in the casting process is 30-150 ℃/s, and the continuous casting speed is 1.8-2.4 mm/min; storing the obtained cast strip for later use;
s2, transferring the obtained cast strip into a special strip mill, and rolling the cast strip at the temperature of 200-230 ℃ through a hot rolling process; cleaning the obtained solder sheet with ethanol for degreasing, cleaning with deionized water, and drying in a drying device; storing for later use;
s3, uniformly coating a layer of flux with the thickness of 10-15 μm on one end face of the solder sheet according to a certain proportion; coating the soldering flux between the two layers of solder sheets by a coating machine; observing the state of the soldering flux by using an X-ray fluoroscopy instrument; and then sequentially rolling and shearing the double-layer solder sheet crude product obtained after the cladding treatment, and packaging the double-layer solder sheet crude product after the final required size is reached to obtain the double-layer solder sheet finished product.
Compared with the prior art, the invention has the beneficial effects that:
according to the invention, tin powder, zinc powder, indium powder, stearic acid and sodium chloride are used as raw materials for preparing the porous metal powder, and the prepared porous metal powder has a rich pore structure, so that the porous metal powder has a larger specific surface area. Meanwhile, the alloy has the characteristic of low melting point. And then, placing the polyacrylic acid and the porous metal powder into isopropanol for melting, emulsifying, dispersing and ball-milling treatment. Finally, the alloy micro powder is immersed in the polyether dimethyl silicone oil, and then the obtained alloy micro powder is dried, so that the polyether dimethyl silicone oil is fully coated on the surface and the pores of the porous metal powder, and the heat conduction efficiency of the porous metal powder is effectively improved. But also greatly improves the hydrophobic property of the organic phase and makes the organic phase mixed more uniformly.
The obtained additive is used as a raw material of the soldering flux, so that the soldering flux positioned in the middle of the double-layer solder sheet can be uniformly heated and quickly and uniformly melted in the welding process, and the melted soldering flux is cooperatively matched with the hydrogenated rosin resin, the activator, the surfactant, the corrosion inhibitor, the thixotropic agent and the film-forming additive, so that the oxidation rate of metal raw materials can be effectively reduced. Moreover, the design of the sandwich structure can accurately control the flux, reduce the phenomenon of poor welding quality caused by welding holes and excessive welding residues, and ensure the welding quality. The circuit board connector is used for circuit board connection and has a good effect.
In addition, under the synergistic effect of methyl hexahydrophthalic anhydride and 2-ethyl-4-methylimidazole, the rosin modified novolac epoxy resin can effectively improve the bonding performance of the rosin modified novolac epoxy resin, effectively bonds two solder sheets and ensures the stability of the structure of the double-layer solder sheet. But also the welding quality and quality are not affected.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
A double-layer solder sheet is a sandwich structure consisting of two layers of solder sheets and soldering flux positioned in the middle of the two layers of solder sheets;
wherein, the solder sheet is made of SnAgCu alloy, and the specific alloy content is Sn: 95%, Ag: 2.5 percent, and the balance of copper;
the soldering flux comprises the following raw materials in percentage by weight: 40% of rosin modified phenolic epoxy resin, 8% of hydrogenated rosin resin, 3% of methyl hexahydrophthalic anhydride, 1.8% of 2-ethyl-4-methylimidazole, 4% of diluent, 1.5% of activating agent, 0.3% of surfactant, 0.1% of corrosion inhibitor, 2% of thixotropic agent, 0.5% of film-forming assistant and the balance of additive.
The diluent is dodecyl glycidyl ether.
The activating agent is prepared from amine organic matters and organic acids according to the mass ratio of 5: 1 mixing and blending; and the amine organic substance is diethanolamine; the organic acid is succinic acid.
The surfactant is octyl phenol polyethenoxy ether.
The corrosion inhibitor is benzotriazole.
The thixotropic agent is kaolin.
The film-forming assistant is glycerol.
The preparation method of the additive comprises the following steps: adding porous metal powder and polyacrylic acid into isopropanol, uniformly mixing by ultrasonic waves, and heating the obtained mixed component; mixing and stirring the porous metal powder under the protection of inert gas after the porous metal powder is melted; then transferring the obtained mixed material to an emulsifying machine for emulsification and dispersion treatment, and finally cooling to obtain alloy micro powder; ball-milling the obtained alloy micro powder to 1.2 mu m, and then immersing the alloy micro powder in polyether dimethyl silicone oil; and after filtering, drying the obtained alloy micro powder at the temperature of 40 ℃ to obtain the finished product of the addition agent.
The preparation method of the porous metal powder comprises the following steps:
i, 95.5: 2.5: 2.0, accurately weighing proper amounts of tin powder, zinc powder and indium powder with the particle size of 100nm respectively; mixing the three kinds of metal powder, and then transferring the mixture into a planetary ball mill for ball milling for 8 hours; adding stearic acid with the mass being 60 percent of the volume of a grinding tank of the ball mill as a process control agent in the ball milling process;
II, mixing the mixed powder subjected to ball milling with sodium chloride according to the volume ratio of 40%, and then putting the mixed powder into a ball milling tank; after vacuum mixing, tabletting the obtained mixed powder, and storing the obtained blank for later use;
III, placing the obtained blank in a muffle furnace, and sintering at high temperature for 8 hours under the condition of inert gas; after sintering, soaking the sintered ceramic into deionized water at 50 ℃ for heat preservation for 10 hours; after filtering, sequentially cleaning and drying the obtained solid materials; and obtaining the finished product of the porous metal powder.
A preparation process of a double-layer solder sheet comprises the following steps:
s1, accurately weighing appropriate amount of metal raw materials and soldering flux for manufacturing the solder sheet according to the formula; then, the melt obtained after the metal raw materials are mixed and melted is poured into a crystallizer from a storage container in a controlled way, and the melt is cast into a strip by a belt type continuous casting machine or a block casting machine; wherein, when casting, a continuous casting strip with the thickness of 3mm is drawn out in a controlled manner, and the average cooling speed along the thickness of the strip in the casting process is 30 ℃/s, and the continuous casting speed is 1.8 mm/min; storing the obtained cast strip for later use;
s2, transferring the obtained cast strip into a special strip mill, and rolling the cast strip at the temperature of 200 ℃ through a hot rolling process; cleaning the obtained solder sheet with ethanol for degreasing, cleaning with deionized water, and drying in a drying device; storing for later use;
s3, uniformly coating a layer of soldering flux with the thickness of 10 μm on one end face of the solder sheet according to a certain proportion; coating the soldering flux between the two layers of solder sheets by a coating machine; observing the state of the soldering flux by using an X-ray fluoroscopy instrument; and then sequentially rolling and shearing the double-layer solder sheet crude product obtained after the cladding treatment, and packaging the double-layer solder sheet crude product after the final required size is reached to obtain the double-layer solder sheet finished product.
Example 2
A double-layer solder sheet is a sandwich structure consisting of two layers of solder sheets and soldering flux positioned in the middle of the two layers of solder sheets;
wherein, the solder sheet is made of SnAgCu alloy, and the specific alloy content is Sn: 95.5%, Ag: 2.8 percent, and the balance of copper;
the soldering flux comprises the following raw materials in percentage by weight: 45% of rosin modified phenolic epoxy resin, 9% of hydrogenated rosin resin, 5% of methyl hexahydrophthalic anhydride, 2.5% of 2-ethyl-4-methylimidazole, 7% of diluent, 2.5% of activator, 0.5% of surfactant, 0.2% of corrosion inhibitor, 3% of thixotropic agent, 1.0% of film-forming assistant and the balance of additive.
The diluent is polyethylene glycol diglycidyl ether.
The activator is prepared from amine organic matters and organic acid according to the mass ratio of 7: 1 mixing and blending; and the amine organic matter is triethanolamine; the organic acid is itaconic acid.
The surfactant is isooctyl phenol polyoxyethylene ether.
The corrosion inhibitor is hydrazine hydrate.
The thixotropic agent is selected from polyamide wax.
The film-forming assistant is polyethylene glycol 1000.
The preparation method of the additive comprises the following steps: adding porous metal powder and polyacrylic acid into isopropanol, uniformly mixing by ultrasonic waves, and heating the obtained mixed component; mixing and stirring the porous metal powder under the protection of inert gas after the porous metal powder is melted; then transferring the obtained mixed material to an emulsifying machine for emulsification and dispersion treatment, and finally cooling to obtain alloy micro powder; ball-milling the obtained alloy micro powder to 1.4 mu m, and then immersing the alloy micro powder in polyether dimethyl silicone oil; and after filtering, drying the obtained alloy micro powder at the temperature of 45 ℃ to obtain the finished product of the addition agent.
The preparation method of the porous metal powder comprises the following steps:
i, 95.5: 2.5: 2.0, accurately weighing appropriate amounts of tin powder, zinc powder and indium powder with the particle size of 150nm respectively; mixing the three kinds of metal powder, and then transferring the mixture into a planetary ball mill for ball milling for 9 hours; adding stearic acid with the mass being 65 percent of the volume of a grinding tank of the ball mill as a process control agent in the ball milling process;
II, mixing the mixed powder subjected to ball milling with sodium chloride according to the volume ratio of 50%, and then putting the mixed powder into a ball milling tank; after vacuum mixing, tabletting the obtained mixed powder, and storing the obtained blank for later use;
III, placing the obtained blank in a muffle furnace, and sintering at high temperature for 10 hours under the condition of inert gas; after sintering, soaking the sintered ceramic into deionized water at 55 ℃ for heat preservation for 12 hours; after filtering, sequentially cleaning and drying the obtained solid materials; and obtaining the finished product of the porous metal powder.
A preparation process of a double-layer solder sheet comprises the following steps:
s1, accurately weighing appropriate amount of metal raw materials and soldering flux for manufacturing the solder sheet according to the formula; then, the melt obtained after the metal raw materials are mixed and melted is poured into a crystallizer from a storage container in a controlled way, and the melt is cast into a strip by a belt type continuous casting machine or a block casting machine; wherein, when casting, a continuous casting strip with the thickness of 5mm is drawn out in a controlled manner, and the average cooling speed along the thickness of the strip in the casting process is 80 ℃/s, and the continuous casting speed is 2.0 mm/min; storing the obtained cast strip for later use;
s2, transferring the obtained cast strip into a special strip mill, and rolling the cast strip at the temperature of 210 ℃ through a hot rolling process; cleaning the obtained solder sheet with ethanol for degreasing, cleaning with deionized water, and drying in a drying device; storing for later use;
s3, uniformly coating a layer of soldering flux with the thickness of 12 μm on one end face of the solder sheet according to a certain proportion; coating the soldering flux between the two layers of solder sheets by a coating machine; observing the state of the soldering flux by using an X-ray fluoroscopy instrument; and then sequentially rolling and shearing the double-layer solder sheet crude product obtained after the cladding treatment, and packaging the double-layer solder sheet crude product after the final required size is reached to obtain the double-layer solder sheet finished product.
Example 3
A double-layer solder sheet is a sandwich structure consisting of two layers of solder sheets and soldering flux positioned in the middle of the two layers of solder sheets;
wherein, the solder sheet is made of SnAgCu alloy, and the specific alloy content is Sn: 95.8%, Ag: 3.2 percent, and the balance of copper;
the soldering flux comprises the following raw materials in percentage by weight: 48 percent of rosin modified phenolic epoxy resin, 10 percent of hydrogenated rosin resin, 8 percent of methyl hexahydrophthalic anhydride, 4.2 percent of 2-ethyl-4-methylimidazole, 10 percent of diluent, 3.0 percent of activator, 0.6 percent of surfactant, 0.4 percent of corrosion inhibitor, 4 percent of thixotropic agent, 2.0 percent of film-forming assistant and the balance of additive.
The diluent is any one of dodecyl glycidyl ether and polyethylene glycol diglycidyl ether.
The activator is prepared from amine organic matters and organic acid according to the mass ratio of 7: 1 mixing and blending; and the amine organic substance is diethanolamine; the organic acid is sorbic acid.
The surfactant is nonionic fluorocarbon surfactant.
The corrosion inhibitor is benzotriazole.
The thixotropic agent is hydrogenated castor oil.
The film-forming assistant is polyethylene glycol 2000.
The preparation method of the additive comprises the following steps: adding porous metal powder and polyacrylic acid into isopropanol, uniformly mixing by ultrasonic waves, and heating the obtained mixed component; mixing and stirring the porous metal powder under the protection of inert gas after the porous metal powder is melted; then transferring the obtained mixed material to an emulsifying machine for emulsification and dispersion treatment, and finally cooling to obtain alloy micro powder; ball-milling the obtained alloy micro powder to 1.6 mu m, and then immersing the alloy micro powder in polyether dimethyl silicone oil; and after filtering, drying the obtained alloy micro powder at the temperature of 50 ℃ to obtain the finished product of the addition agent.
The preparation method of the porous metal powder comprises the following steps:
i, 95.5: 2.5: 2.0, accurately weighing appropriate amounts of tin powder, zinc powder and indium powder with the particle size of 180nm respectively; mixing the three kinds of metal powder, and then transferring the mixture into a planetary ball mill for ball milling for 10 hours; adding stearic acid with the mass being 65 percent of the volume of a grinding tank of the ball mill as a process control agent in the ball milling process;
II, mixing the mixed powder subjected to ball milling with sodium chloride according to the volume ratio of 60%, and then putting the mixed powder into a ball milling tank; after vacuum mixing, tabletting the obtained mixed powder, and storing the obtained blank for later use;
III, placing the obtained blank in a muffle furnace, and sintering at high temperature for 12 hours under the condition of inert gas; after sintering, soaking the sintered ceramic in deionized water at 60 ℃ for heat preservation for 13 hours; after filtering, sequentially cleaning and drying the obtained solid materials; and obtaining the finished product of the porous metal powder.
A preparation process of a double-layer solder sheet comprises the following steps:
s1, accurately weighing appropriate amount of metal raw materials and soldering flux for manufacturing the solder sheet according to the formula; then, the melt obtained after the metal raw materials are mixed and melted is poured into a crystallizer from a storage container in a controlled way, and the melt is cast into a strip by a belt type continuous casting machine or a block casting machine; wherein, when casting, a continuous casting strip with the thickness of 6mm is drawn out in a controlled manner, the average cooling speed along the thickness of the strip in the casting process is 120 ℃/s, and the continuous casting speed is 2.2 mm/min; storing the obtained cast strip for later use;
s2, transferring the obtained cast strip into a special strip mill, and rolling the cast strip at 220 ℃ through a hot rolling process; cleaning the obtained solder sheet with ethanol for degreasing, cleaning with deionized water, and drying in a drying device; storing for later use;
s3, uniformly coating a layer of flux with the thickness of 14 μm on one end face of the solder sheet according to a certain proportion; coating the soldering flux between the two layers of solder sheets by a coating machine; observing the state of the soldering flux by using an X-ray fluoroscopy instrument; and then sequentially rolling and shearing the double-layer solder sheet crude product obtained after the cladding treatment, and packaging the double-layer solder sheet crude product after the final required size is reached to obtain the double-layer solder sheet finished product.
Example 4
A double-layer solder sheet is a sandwich structure consisting of two layers of solder sheets and soldering flux positioned in the middle of the two layers of solder sheets;
wherein, the solder sheet is made of SnAgCu alloy, and the specific alloy content is Sn: 96%, Ag: 3.5 percent, and the balance of copper;
the soldering flux comprises the following raw materials in percentage by weight: 50% of rosin modified phenolic epoxy resin, 12% of hydrogenated rosin resin, 10% of methyl hexahydrophthalic anhydride, 5% of 2-ethyl-4-methylimidazole, 12% of diluent, 3.2% of activating agent, 0.8% of surfactant, 0.5% of corrosion inhibitor, 5% of thixotropic agent, 2.5% of film-forming assistant and the balance of additive.
The diluent is dodecyl glycidyl ether.
The activator is prepared from amine organic matters and organic acid according to the mass ratio of 9: 1 mixing and blending; and the amine organic matter is triethanolamine; the organic acid is succinic acid.
The surfactant is octyl phenol polyethenoxy ether.
The corrosion inhibitor is hydrazine hydrate.
The thixotropic agent is kaolin.
The film-forming assistant is glycerol.
The preparation method of the additive comprises the following steps: adding porous metal powder and polyacrylic acid into isopropanol, uniformly mixing by ultrasonic waves, and heating the obtained mixed component; mixing and stirring the porous metal powder under the protection of inert gas after the porous metal powder is melted; then transferring the obtained mixed material to an emulsifying machine for emulsification and dispersion treatment, and finally cooling to obtain alloy micro powder; ball-milling the obtained alloy micro powder to 1.8 mu m, and then immersing the alloy micro powder in polyether dimethyl silicone oil; and after filtering, drying the obtained alloy micro powder at the temperature of 40-55 ℃ to obtain the finished product of the addition agent.
The preparation method of the porous metal powder comprises the following steps:
i, 95.5: 2.5: 2.0, accurately weighing appropriate amounts of tin powder, zinc powder and indium powder with the particle size of 200nm respectively; mixing the three kinds of metal powder, and then transferring the mixture into a planetary ball mill for ball milling for 12 hours; stearic acid with the mass being 70 percent of the volume of a grinding tank of the ball mill as a process control agent is added in the ball milling process;
II, mixing the mixed powder subjected to ball milling with sodium chloride according to the volume ratio of 75%, and then putting the mixed powder into a ball milling tank; after vacuum mixing, tabletting the obtained mixed powder, and storing the obtained blank for later use;
III, placing the obtained blank in a muffle furnace, and sintering at high temperature for 15 hours under the condition of inert gas; after sintering, soaking the sintered ceramic in deionized water at 65 ℃ for heat preservation for 15 h; after filtering, sequentially cleaning and drying the obtained solid materials; and obtaining the finished product of the porous metal powder.
A preparation process of a double-layer solder sheet comprises the following steps:
s1, accurately weighing appropriate amount of metal raw materials and soldering flux for manufacturing the solder sheet according to the formula; then, the melt obtained after the metal raw materials are mixed and melted is poured into a crystallizer from a storage container in a controlled way, and the melt is cast into a strip by a belt type continuous casting machine or a block casting machine; wherein, when casting, a continuous casting strip with the thickness of 8mm is drawn out in a controlled manner, and the average cooling speed along the thickness of the strip in the casting process is 150 ℃/s, and the continuous casting speed is 2.4 mm/min; storing the obtained cast strip for later use;
s2, transferring the obtained cast strip into a special strip mill, and rolling the cast strip at 230 ℃ through a hot rolling process; cleaning the obtained solder sheet with ethanol for degreasing, cleaning with deionized water, and drying in a drying device; storing for later use;
s3, uniformly coating a layer of soldering flux with the thickness of 15 μm on one end face of the solder sheet according to a certain proportion; coating the soldering flux between the two layers of solder sheets by a coating machine; observing the state of the soldering flux by using an X-ray fluoroscopy instrument; and then sequentially rolling and shearing the double-layer solder sheet crude product obtained after the cladding treatment, and packaging the double-layer solder sheet crude product after the final required size is reached to obtain the double-layer solder sheet finished product.
Comparative example: a solder sheet of a commercially available single-layer structure, and the composition of the solder sheet is the same as that of the solder sheet used in comparative examples 1 to 4;
performance testing
The two-layer solder sheets prepared by examples 1 to 4 of the present invention were referred to as experimental examples 1 to 4, respectively; then, the double-layer solder sheets prepared in examples 1 to 4 and the single-layer solder sheet provided in the comparative example were tested for their soldering performance, and the data obtained for each group were recorded in the following table:
note: 1. thixotropic coefficient: the determination is carried out according to the test method of GB/T9491-2002;
2. and (3) testing tin beads: the measurement is carried out according to the decimal line in the appendix of JIS.Z.3284;
3. testing the bonding strength of the soldering flux: testing according to the standard of GB 50367-2006;
4. and (3) testing the void ratio: performing void ratio test by reflow soldering and X-ray probing method, wherein the void ratio is (S)1-S2)/S1In the formula S1For the solderable area of the chip, S2The actual bonding area of the chip;
5. and (3) testing the wetting property: testing according to the standard IPCTM-6502.4.45 solder paste-wetting test;
as can be seen from the relevant data in the table, the quantity of the used scaling powder is easy to control accurately when the double-layer welding flux sheet prepared by the invention is used in the welding operation, thus not only effectively reducing the phenomenon of poor welding quality caused by welding 'holes' and excessive welding residues; moreover, the oxidation rate of the metal raw materials can be effectively reduced, and the welding quality and quality are ensured. Therefore, the double-layer solder sheet prepared by the invention has wider market prospect and is more suitable for popularization.
In the description herein, references to the description of "one embodiment," "an example," "a specific example" or the like are intended to mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The preferred embodiments of the invention disclosed above are intended to be illustrative only. The preferred embodiments are not intended to be exhaustive or to limit the invention to the precise embodiments disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best utilize the invention. The invention is limited only by the claims and their full scope and equivalents.
Claims (10)
1. A dual-layer solder sheet characterized by: the structure is a sandwich structure consisting of two layers of solder sheets and soldering flux positioned in the middle of the two layers of solder sheets;
the solder sheet is made of SnAgCu alloy, and the specific alloy content of the solder sheet is Sn: 95-96%, Ag: 2.5-3.5% and the balance of copper;
the soldering flux comprises the following raw materials in percentage by weight: 40-50% of rosin modified phenolic epoxy resin, 8-12% of hydrogenated rosin resin, 3-10% of methyl hexahydrophthalic anhydride, 1.8-5% of 2-ethyl-4-methylimidazole, 4-12% of diluent, 1.5-3.2% of activating agent, 0.3-0.8% of surfactant, 0.1-0.5% of corrosion inhibitor, 2-5% of thixotropic agent, 0.5-2.5% of film forming additive and the balance of additive.
2. A dual-layer solder sheet according to claim 1, wherein: the diluent is any one of dodecyl glycidyl ether and polyethylene glycol diglycidyl ether.
3. A dual-layer solder sheet according to claim 1, wherein: the activating agent is prepared from an amine organic substance and an organic acid according to a mass ratio of 5-9: 1 mixing and blending; the amine organic matter is any one of diethanolamine and triethanolamine; the organic acid is selected from any one of succinic acid, itaconic acid and sorbic acid.
4. A dual-layer solder sheet according to claim 1, wherein: the surfactant is any one of octylphenol polyoxyethylene ether, isooctylphenol polyoxyethylene ether and nonionic fluorocarbon surfactant.
5. A dual-layer solder sheet according to claim 1, wherein: the corrosion inhibitor is any one of benzotriazole and hydrazine hydrate.
6. A dual-layer solder sheet according to claim 1, wherein: the thixotropic agent is any one of kaolin, polyamide wax or hydrogenated castor oil.
7. A dual-layer solder sheet according to claim 1, wherein: the film-forming assistant is any one of glycerol, polyethylene glycol 1000 and polyethylene glycol 2000.
8. The double-layer solder sheet according to claim 1, wherein the additive is prepared by a method comprising: adding porous metal powder and polyacrylic acid into isopropanol, uniformly mixing by ultrasonic waves, and heating the obtained mixed component; mixing and stirring the porous metal powder under the protection of inert gas after the porous metal powder is melted; then transferring the obtained mixed material to an emulsifying machine for emulsification and dispersion treatment, and finally cooling to obtain alloy micro powder; ball-milling the obtained alloy micro powder to 1.2-1.8 μm, and immersing the alloy micro powder in polyether dimethyl silicone oil; and after filtering, drying the obtained alloy micro powder at the temperature of 40-55 ℃ to obtain the finished product of the addition agent.
9. The double-layer solder sheet according to claim 8, wherein the porous metal powder is prepared by a method comprising the steps of:
i, 95.5: 2.5: 2.0, accurately weighing proper amounts of tin powder, zinc powder and indium powder with the particle size of 100-200 nm respectively; mixing the three metal powders, and then transferring the mixture into a planetary ball mill for ball milling for 8-12 h; adding stearic acid with the mass being 60-70% of the volume of a grinding tank of the ball mill as a process control agent in the ball milling process;
II, mixing the mixed powder subjected to ball milling with sodium chloride according to the volume ratio of 40-75%, and then putting the mixed powder into a ball milling tank; after vacuum mixing, tabletting the obtained mixed powder, and storing the obtained blank for later use;
III, placing the obtained blank in a muffle furnace, and sintering at high temperature for 8-15 h under the condition of inert gas; after sintering, soaking the sintered material in deionized water at the temperature of 50-65 ℃ for heat preservation for 10-15 h; after filtering, sequentially cleaning and drying the obtained solid materials; and obtaining the finished product of the porous metal powder.
10. The process for preparing a double-layer solder sheet according to any one of claims 1 to 9, comprising the steps of:
s1, accurately weighing appropriate amount of metal raw materials and soldering flux for manufacturing the solder sheet according to the formula; then, the melt obtained after the metal raw materials are mixed and melted is poured into a crystallizer from a storage container in a controlled way, and the melt is cast into a strip by a belt type continuous casting machine or a block casting machine; wherein, when casting the material, a continuous casting strip with the thickness of 3-8 mm is pulled out in a controlled manner, the average cooling speed along the thickness of the strip in the casting process is 30-150 ℃/s, and the continuous casting speed is 1.8-2.4 mm/min; storing the obtained cast strip for later use;
s2, transferring the obtained cast strip into a special strip mill, and rolling the cast strip at the temperature of 200-230 ℃ through a hot rolling process; cleaning the obtained solder sheet with ethanol for degreasing, cleaning with deionized water, and drying in a drying device; storing for later use;
s3, uniformly coating a layer of flux with the thickness of 10-15 μm on one end face of the solder sheet according to a certain proportion; coating the soldering flux between the two layers of solder sheets by a coating machine; observing the state of the soldering flux by using an X-ray fluoroscopy instrument; and then sequentially rolling and shearing the double-layer solder sheet crude product obtained after the cladding treatment, and packaging the double-layer solder sheet crude product after the final required size is reached to obtain the double-layer solder sheet finished product.
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