CN113714679A - Washing-free residue-free high-wetting SMT soldering paste and preparation method thereof - Google Patents

Washing-free residue-free high-wetting SMT soldering paste and preparation method thereof Download PDF

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Publication number
CN113714679A
CN113714679A CN202111023304.6A CN202111023304A CN113714679A CN 113714679 A CN113714679 A CN 113714679A CN 202111023304 A CN202111023304 A CN 202111023304A CN 113714679 A CN113714679 A CN 113714679A
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Prior art keywords
powder
residue
acid
free
wetting
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CN202111023304.6A
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冷青松
张群
丰昭
李鹏
刘瑞鸿
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Jiangsu Zhengneng Electronic Technology Co ltd
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Jiangsu Zhengneng Electronic Technology Co ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B23MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23KSOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K35/00Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
    • B23K35/22Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by the composition or nature of the material
    • B23K35/24Selection of soldering or welding materials proper
    • B23K35/26Selection of soldering or welding materials proper with the principal constituent melting at less than 400 degrees C
    • B23K35/262Sn as the principal constituent
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B23MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23KSOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K35/00Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
    • B23K35/02Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by mechanical features, e.g. shape
    • B23K35/0222Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by mechanical features, e.g. shape for use in soldering, brazing
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B23MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23KSOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K35/00Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
    • B23K35/22Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by the composition or nature of the material
    • B23K35/36Selection 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
    • B23K35/362Selection of compositions of fluxes

Abstract

The invention provides a no-clean residue-free and high-wetting SMT soldering paste and a preparation method thereof, wherein the SMT soldering paste comprises alloy powder and soldering flux, and the soldering flux comprises the following components: 0.5-3 wt% of rare earth powder, including one or more of cerium powder Ce, yttrium powder Y, niobium powder Nb and rubidium powder Rb; 0.5-5% by weight of an antioxidant; 4-18% by weight of a resin; 1-5% by weight of an active agent; 0.5-0.8% by weight of a thixotropic agent; 0.5-5% by weight of a solvent; 0.01-0.5% by weight of a wetting agent; 0.01-3 wt% of corrosion inhibitor. The invention has the advantages of high wettability, corrosion resistance, expansion rate, good thixotropy, effective reduction of tin bead generation, less surface residue and the like, and meets related detection standards.

Description

Washing-free residue-free high-wetting SMT soldering paste and preparation method thereof
Technical Field
The invention belongs to the technical field of soldering paste, and particularly relates to a washing-free residue-free high-wetting SMT soldering paste and a preparation method thereof.
Background
At present, the development of electronic products towards super-large scale, digitalization and miniaturization makes the Surface Mount Technology (SMT) become the mainstream technology of electronic assembly. Solder paste is used as an important welding material and widely applied to surface assembly processes. The welding method plays a series of roles of fixing electronic components, removing surface oxidation films, forming reliable welding spots and the like in the welding process, and the quality of the welding method is directly related to the quality of surface assembly components.
Among the prior art, the solder paste exists multiple not enough, like during two-sided pieces welding, the dropping of components and parts: the wettability and weldability of the soldering paste are poor; tin beads are generated on the surface of the welded plate: antioxidants are not suitable; improper flux formulation per se and non-volatile solvent or liquid additives or activators; the welded plate surface has more residues: the rosin resin content is too high or the quality is not good; while printing, a ribbon of tin wires, adhesion, blurred images, etc. are spool: the viscosity of the soldering paste is low; poor solder paste overflow; the metal components in the soldering paste are low; the proportion of the components of the soldering flux is higher; incomplete tin soldering on soldering points: the activity of the soldering flux is not enough, the oxidation substances of the SMT welding position cannot be completely removed, and the SMT welding position has a serious oxidation phenomenon; the wettability and the cutting-off property of the soldering flux are poor; when reflow soldering is carried out, the preheating time is too long or the preheating temperature is too high, the active agent fails, and the working temperature range of the active agent is too narrow; the welding spot is not bright: the tin powder in the tin paste has oxidation phenomenon; the soldering flux has an additive causing a delustering effect; the residual of the volatile matters is difficult to exist on the surface of the welding spot; the residual rosin or resin exists on the surface of the welding spot after welding.
For example, patent publication No. CN101380699B discloses a tin-zinc series lead-free alloy solder paste and a preparation method thereof, which adopts an alloying method, adds alloy elements in Sn-Zn solder alloy, and adopts a special soldering flux, so that the solder paste is not easy to oxidize when applied to the SMT process, and the phenomenon that solder joints cannot be formed or the quality of the solder joints is poor is avoided. But the method can only avoid the problem of oxidation, and cannot meet the requirements of no residue, no cleaning and high humidity of welding, so that the welding scene and the welding quality are limited.
Disclosure of Invention
The invention aims to provide a no-clean residue-free high-wetting SMT soldering paste and a preparation method thereof, which overcome the defects.
The invention provides the following technical scheme:
the application provides a no-clean residue-free and high-wetting SMT soldering paste, which comprises alloy powder and soldering flux, wherein the weight percentage of the alloy powder is 70-85%, and the soldering flux comprises:
0.5-3 wt% of rare earth powder, including one or more of cerium powder Ce, yttrium powder Y, niobium powder Nb and rubidium powder Rb, for improving strength, toughness, high temperature oxidation resistance and corrosion resistance of the solder paste;
the antioxidant with the weight percentage of 0.5-5 percent is used for avoiding the oxidation of tin powder in the soldering paste, avoiding the generation of tin balls on the board surface after welding and enabling welding spots to be bright;
4-18% of resin by weight percent, which is used for improving the initial viscosity, compatibility, adhesion, oxidation resistance, thermal stability and aging resistance of the soldering paste, so that no residue exists on the surface of the soldering paste after soldering;
1-5% of active agent by weight percentage, which is used for volatilizing after welding, so that no residue is left on the welded plate surface;
0.5-0.8% of thixotropic agent by weight percent, which is used for increasing viscosity and thixotropy and avoiding tin wire, adhesion and image blurring during printing;
0.5-5 wt% of solvent for mixing resin and thixotropic agent to obtain carrier and activated pasty thixotropic agent, and volatilizing after welding to make the welded plate surface have no residue;
the wetting agent with the weight percentage of 0.01-0.5 percent is used for being matched with the active agent to completely remove the oxide layer, so that the tin on the welding spot is full, and the wettability and the cutting-off property of the soldering paste are improved;
0.01-3% by weight of corrosion inhibitor for retarding penetrating corrosion after welding.
Preferably, the alloy powder is micron Sn96.5-3.0Ag-Cu0.5 alloy powder, and the particle size of the powder is 10-50 um.
Preferably, the antioxidant is one or a combination of two or more of butylated hydroxyanisole, dibutyl hydroxy toluene, propyl gallate, tert-butyl hydroquinone, and octadecyl beta (3,5 di-tert-butyl-4-hydroxyphenyl) propionate.
Preferably, the resin is one or a combination of two or more of rosin pentaerythritol ester, rosin ester, dihydrorosin, tetrahydrorosin, acrylic acid modified rosin, dimerized rosin and polyisobutylene.
Preferably, the active agent is one or a combination of two or more of itaconic acid, malic acid, citric acid, methylmalonic acid, methylsuccinic acid, dichloroacetic acid, succinic acid, glutaric acid, diethylamine hydrobromide, 2-bromoethylamine hydrobromide, cyclohexylamine hydrochloride.
Preferably, the thixotropic agent is one or a combination of two or more of polyamide wax, hydrogenated castor oil, stearic acid amide, ethylene bis stearic acid amide, and fumed silica.
Preferably, the solvent is one or a combination of two or more of propylene glycol phenyl ether acetate, diethylene glycol butyl ether acetate, ethylene glycol monobutyl ether, ethylene glycol dimethyl ether, ethylene glycol monobutyl ether, propylene glycol, glycerol, tributyl citrate, and triethylene glycol propyl ether.
Preferably, the wetting agent is 2.4.7.9-tetramethyl-5-decyne-4.7-diol.
Preferably, the corrosion inhibitor is one or a combination of two or more of benzotriazole, tolyltriazole, 2-ethyl-4-methylimidazole, 2-ethylimidazole, 2-methylimidazole, phosphonocarboxylic acid and polyaspartic acid.
Based on the solder paste, the application also provides a preparation method of the solder paste, which comprises the following steps:
s1, adding resin into a solvent, heating to 80 ℃, and stirring at 400rpm until the resin is completely dissolved uniformly to obtain a carrier;
s2, adding the thixotropic agent into the solvent, heating to 80 ℃, stirring at 1000rpm until the thixotropic agent is fully mixed to obtain an activated thixotropic agent; if the solvent is a mixture of two solvents, the resin and the thixotropic agent are respectively added into one solvent, and the solvent dosage is related to the amount of the resin and the thixotropic agent; if the solvent is one or more than two solvents, the resin and the thixotropic agent are added after the solvents are fully mixed.
S3, sequentially adding the carrier, the wetting agent, the antioxidant, the corrosion inhibitor, the activator and the activated thixotropic agent into a stainless steel reaction kettle of an emulsifying machine, and fully stirring to obtain the soldering flux;
s4, packaging the alloy powder and the rare earth powder in a vacuum quartz tube, filling high-purity nitrogen serving as protective gas into the vacuum quartz tube, placing the vacuum quartz tube in a reaction furnace, heating and smelting the vacuum quartz tube, and obtaining a solder powder melt after the alloy powder and the rare earth powder are completely melted; then placing the molten solder powder in an inert gas protection box to cool to room temperature, and then placing the cooled molten solder powder into a die to perform hot-pressing sintering to obtain solder alloy powder;
and S5, adding the soldering flux and the solder alloy powder into a double-planet stirrer for the solder paste, stirring for 1 hour to obtain the solder paste, and refrigerating and storing the solder paste in a refrigerator at 6 ℃.
The invention has the beneficial effects that:
1. the addition of rare earth elements of cerium powder Ce, yttrium powder Y, niobium powder Nb and rubidium powder Rb can improve the strength, toughness, high-temperature oxidation resistance and corrosion resistance of the solder paste;
2. one or more of antioxidant butyl hydroxy anisole, dibutyl hydroxy toluene, propyl gallate, tert-butyl hydroquinone and beta (3,5 di-tert-butyl-4-hydroxyphenyl) octadecyl propionate are adopted, so that no tin bead is generated on the surface of the soldered plate after soldering, and no oxidation phenomenon of tin powder in the solder paste occurs, so that the soldered spot is bright;
3. one or more of rosin pentaerythritol ester, glycerin rosin ester, dihydrorosin, tetrahydrorosin, acrylic acid modified rosin, dimerized rosin and polyisobutylene are adopted, no residue exists on the welded plate surface, and initial viscosity, compatibility, adhesion, oxidation resistance, thermal stability and aging resistance are improved;
4. the used solvent and the used activating agent can be volatilized after welding, and no residue is left;
5. one or more of thixotropic agent polyamide wax, hydrogenated castor oil, stearic acid amide, ethylene bis-stearic acid amide and fumed silica are used, so that the viscosity and thixotropy are increased, and tin wires, adhesion, image blurring and the like are avoided during printing;
6. the solder paste is characterized in that one or more of a wetting agent 2.4.7.9-tetramethyl-5-decyne-4.7-diol and an active agent itaconic acid, malic acid, citric acid, methyl malonic acid, methyl succinic acid, dichloroacetic acid, succinic acid, glutaric acid, diethylamine hydrobromide, 2-bromoethylamine hydrobromide, cyclohexylamine hydrobromide and cyclohexylamine hydrochloride are adopted, so that an oxide layer is completely removed, a solder joint is full, and the wettability and the cutting performance of the solder paste are good.
Detailed Description
Example 1
The embodiment provides a non-cleaning residue-free high-wettability SMT soldering paste, which comprises the following specific components in percentage by mass:
70 percent of micron-sized alloy powder Sn96.5-3.0Ag-Cu0.5 by weight percent, and 10-50um of particle size;
0.5% of rare earth element yttrium powder Y;
the antioxidant comprises 5% of dibutyl hydroxy toluene;
the resin comprises 9 percent of glycerin rosin ester and 9 percent of dihydrorosin;
the activator comprises 2% of itaconic acid, 1% of methylsuccinic acid, 1% of dichloroacetic acid and 1% of 2-bromoethylamine hydrobromide;
the thixotropic agent comprises 0.6% polyamide wax;
the solvent comprises 0.25% glycol and 0.25% glycol dimethyl ether;
the wetting agent comprises 0.1% 2.4.7.9-tetramethyl-5-decyne-4.7-diol;
the corrosion inhibitor comprises 0.1 percent of methylbenzotriazole and 0.2 percent of 2-ethylimidazole.
According to the formula, 9% of resin of glycerol rosin ester and 9% of dihydrorosin are added into 0.25% of solvent of ethylene glycol, heated to 80 ℃, and stirred at 400rpm until the resin is completely dissolved uniformly to obtain the carrier. Adding the thixotropic agent polyamide wax into a solvent ethylene glycol dimethyl ether, heating to 80 ℃, stirring at 1000rpm until the materials are fully mixed to obtain the activated thixotropic agent. Sequentially adding a carrier, 2.4.7.9-tetramethyl-5-decyne-4.7-diol, an antioxidant of dibutyl hydroxy toluene, an activator of 2% itaconic acid, 1% methyl succinic acid, 1% dichloroacetic acid, 1% 2-bromoethylamine hydrobromide, a corrosion inhibitor of 0.1% methyl benzotriazole, 0.2% 2-ethylimidazole and an activated thixotropic agent into a stainless steel reaction kettle of an emulsifying machine, and fully stirring to obtain the soldering flux.
Sn96.5-3.0Ag-Cu0.5 alloy powder with the particle size of 10-50um and rare earth powder yttrium powder Y are packaged in a vacuum quartz tube, high-purity nitrogen is filled into the vacuum quartz tube as protective gas, the vacuum quartz tube is placed in a reaction furnace and is heated and smelted, and after the solder powder is completely melted, a solder powder melt is obtained; and then placing the molten solder powder in an inert gas protection box to cool to room temperature, and then placing the cooled molten solder powder into a die to perform hot-pressing sintering to obtain solder alloy powder.
Adding soldering flux and solder alloy powder into a double-planetary mixer for soldering paste, stirring for 1 hour to obtain the soldering paste, and refrigerating and storing in a refrigerator at 6 ℃.
Example 2
The embodiment provides a non-cleaning residue-free high-wettability SMT soldering paste which is prepared from the following components in percentage by mass:
the weight percentage of the micron-sized Sn96.5-3.0Ag-Cu0.5 alloy powder is 75 percent;
1% of rare earth element cerium powder Ce;
the antioxidant comprises 1% of butylated hydroxyanisole;
the resin comprises 8.2 percent of rosin pentaerythritol ester and 8.2 percent of tetrahydrorosin;
the active agent comprises 1% of citric acid, 1% of methylmalonic acid, 1% of succinic acid and 1% of diethylamine hydrobromide;
the thixotropic agent comprises 0.5% hydrogenated castor oil;
the solvent comprises 1% propylene glycol phenyl ether acetate and 1% ethylene glycol monobutyl ether;
the wetting agent comprises 0.02% 2.4.7.9-tetramethyl-5-decyne-4.7-diol;
the corrosion inhibitor comprises 0.02 percent of benzotriazole, 0.02 percent of methyl benzotriazole, 0.02 percent of 2-ethylimidazole and 0.02 percent of phosphonic carboxylic acid;
adding the rosin pentaerythritol ester and the tetrahydrorosin into propylene glycol phenyl ether acetate according to the formula, heating to 80 ℃, and stirring at 400rpm until the rosin is completely and uniformly dissolved to obtain the carrier. Adding hydrogenated castor oil into ethylene glycol monobutyl ether, heating to 80 ℃, stirring at 1000rpm until the materials are fully mixed to obtain the activated thixotropic agent. Sequentially adding a carrier, 2.4.7.9-tetramethyl-5-decyne-4.7-diol, butyl hydroxy anisole, benzotriazole, methyl benzotriazole, 2-ethylimidazole, phosphonocarboxylic acid, citric acid, methylmalonic acid, succinic acid, diethylamine hydrobromide and the activated thixotropic agent into a stainless steel reaction kettle of an emulsifying machine, and fully stirring to obtain the soldering flux.
Packaging Sn96.5-3.0Ag-Cu0.5 alloy powder and rare earth powder cerium powder Ce in a vacuum quartz tube, filling high-purity nitrogen as protective gas into the vacuum quartz tube, placing the vacuum quartz tube in a reaction furnace, heating and smelting the vacuum quartz tube, and obtaining molten solder powder after the solder powder is completely melted; and then placing the molten solder powder in an inert gas protection box to cool to room temperature, and then placing the cooled molten solder powder into a die to perform hot-pressing sintering to obtain solder alloy powder.
Adding soldering flux and solder alloy powder into a double-planetary mixer for soldering paste, stirring for 1 hour to obtain the soldering paste, and refrigerating and storing in a refrigerator at 6 ℃.
Example 3
The embodiment provides a non-cleaning residue-free high-wettability SMT soldering paste which is prepared from the following components in percentage by mass:
77.5 percent micron-sized Sn96.5-3.0Ag-Cu0.5 alloy powder;
the rare earth elements comprise 0.3 percent of yttrium powder Y and 0.2 percent of rubidium powder Rb;
the antioxidant comprises 3% of tert-butyl hydroquinone;
the resin comprises 2.5 percent of tetrahydrorosin, 2.5 percent of acrylic acid modified rosin, 3 percent of dimerized rosin and 2.75 percent of polyisobutylene;
the active agent comprises 0.25% of itaconic acid, 0.25% of citric acid, 0.25% of cyclohexylamine hydrobromide and 0.25% of glutaric acid;
the thixotropic agent comprises 0.25% ethylene bis stearamide and 0.25% fumed silica;
the solvent comprises 2.5% of glycerol and 2.5% of tributyl citrate;
the wetting agent comprises 0.25% 2.4.7.9-tetramethyl-5-decyne-4.7-diol;
the corrosion inhibitor comprises 0.5 percent of methylbenzotriazole, 0.5 percent of 2-ethylimidazole and 0.5 percent of polyaspartic acid.
Adding resin 2.5% of tetrahydrorosin, 2.5% of acrylic acid modified rosin, 3% of dimerized rosin and 2.75% of polyisobutylene into solvent glycerol according to the formula, heating to 80 ℃, and stirring at 400rpm until the resins are completely dissolved uniformly to obtain the carrier. Adding 0.25 percent of ethylene bis stearamide as a thixotropic agent and 0.25 percent of fumed silica into a solvent tributyl citrate, heating to 80 ℃, and stirring at 1000rpm until the materials are fully mixed to obtain the activated thixotropic agent. Sequentially adding a carrier, 2.4.7.9-tetramethyl-5-decyne-4.7-diol, an antioxidant tert-butylhydroquinone, 0.25% of itaconic acid, 0.25% of citric acid, 0.25% of cyclohexylamine hydrobromide, 0.25% of glutaric acid, a corrosion inhibitor, 0.5% of methyl benzotriazole, 0.5% of 2-ethylimidazole, 0.5% of polyaspartic acid and an activated thixotropic agent into a stainless steel reaction kettle of an emulsifying machine, and fully stirring to obtain the soldering flux.
Packaging Sn96.5-3.0Ag-Cu0.5 alloy powder, 0.3% yttrium powder Y of rare earth powder and 0.2% rubidium powder Rb in a vacuum quartz tube, filling high-purity nitrogen as protective gas into the vacuum quartz tube, placing the vacuum quartz tube in a reaction furnace, heating and smelting the reaction furnace, and obtaining solder powder melt after the solder powder is completely melted; and then placing the molten solder powder in an inert gas protection box to cool to room temperature, and then placing the cooled molten solder powder into a die to perform hot-pressing sintering to obtain solder alloy powder.
Adding soldering flux and solder alloy powder into a double-planetary mixer for soldering paste, stirring for 1 hour to obtain the soldering paste, and refrigerating and storing in a refrigerator at 6 ℃.
Example 4
The embodiment provides a non-cleaning residue-free high-wettability SMT soldering paste which is prepared from the following components in percentage by mass:
80% micron-sized Sn96.5-3.0Ag-Cu0.5 alloy powder;
the rare earth elements comprise 3 percent of niobium powder Nb;
the antioxidant comprises 0.5% propyl gallate;
the resin comprises 4 percent of glycerin rosin ester and 3.3 percent of dimerized rosin;
the active agent comprises 0.5% of itaconic acid, 0.5% of malic acid, 0.5% of citric acid and 0.5% of methylmalonic acid;
the thixotropic agent comprises 0.7% ethylene bis stearamide;
the solvent comprises 1.5 percent of ethylene glycol monobutyl ether and 1.5 percent of propylene glycol;
the wetting agent comprises 0.5% 2.4.7.9-tetramethyl-5-decyne-4.7-diol;
the corrosion inhibitor comprises 1 percent of benzotriazole, 1 percent of 2-ethyl-4-methylimidazole and 1 percent of polyaspartic acid.
The resin is prepared by mixing the following components in parts by weight: 4% of glycerin rosin ester and 3.3% of dimerized rosin, wherein the solvent is added: and (3) heating ethylene glycol monobutyl ether to 80 ℃, and stirring at 400rpm until the ethylene glycol monobutyl ether is completely dissolved uniformly to obtain the carrier. Mixing a thixotropic agent: adding ethylene bis stearamide into propylene glycol serving as a solvent, heating to 80 ℃, and stirring at 1000rpm until the ethylene bis stearamide is fully mixed to obtain the activated thixotropic agent. Sequentially adding a carrier, 2.4.7.9-tetramethyl-5-decyne-4.7-diol, an antioxidant propyl gallate, an active agent itaconic acid, malic acid, citric acid, methyl malonic acid, a corrosion inhibitor benzotriazole, 2-ethyl-4-methylimidazole, polyaspartic acid and an activated thixotropic agent into a stainless steel reaction kettle of an emulsifying machine, and fully stirring to obtain the soldering flux.
Packaging Sn96.5-3.0Ag-Cu0.5 alloy powder and rare earth powder niobium powder Nb in a vacuum quartz tube, filling high-purity nitrogen as protective gas into the vacuum quartz tube, placing the vacuum quartz tube in a reaction furnace, heating and smelting the vacuum quartz tube, and obtaining a solder powder solution after the solder powder is completely melted; and then placing the molten solder powder in an inert gas protection box to cool to room temperature, and then placing the cooled molten solder powder into a die to perform hot-pressing sintering to obtain solder alloy powder.
Adding soldering flux and solder alloy powder into a double-planetary mixer for soldering paste, stirring for 1 hour to obtain the soldering paste, and refrigerating and storing in a refrigerator at 6 ℃.
Example 5
The embodiment provides a non-cleaning residue-free high-wettability SMT soldering paste which is prepared from the following components in percentage by mass:
85% micron-sized Sn96.5-3.0Ag-Cu0.5 alloy powder;
the rare earth elements comprise 2% of rubidium powder Rb;
the antioxidant comprises 2% octadecyl beta (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate;
the resin comprises 2% of acrylic acid modified rosin and 2% of polyisobutylene;
the active agent comprises 1% of malic acid, 1% of glutaric acid and 1% of cyclohexylamine hydrochloride;
the thixotropic agent comprises 0.9% stearic acid amide;
the solvent comprises 1.5 percent of diethylene glycol butyl ether acetate and 1.5 percent of triethylene glycol propyl ether;
the wetting agent comprises 0.05% 2.4.7.9-tetramethyl-5-decyne-4.7-diol;
the corrosion inhibitor comprises 0.01 percent of 2-ethyl-4-methylimidazole, 0.02 percent of 2-methylimidazole and 0.02 percent of polyaspartic acid.
According to the formula, the acrylic acid modified rosin and polyisobutylene are added into diethylene glycol butyl ether acetate, heated to 80 ℃, stirred at 400rpm until the acrylic acid modified rosin and the polyisobutylene are completely and uniformly dissolved to obtain the carrier. Adding stearic acid amide into triethylene glycol propyl ether, heating to 80 ℃, stirring at 1000rpm until the stearic acid amide and the triethylene glycol propyl ether are fully mixed to obtain the activated thixotropic agent. Sequentially adding a carrier, 2.4.7.9-tetramethyl-5-decyne-4.7-diol, beta (3, 5-di-tert-butyl-4-hydroxyphenyl) octadecyl propionate, malic acid, glutaric acid, cyclohexylamine hydrochloride, 2-ethyl-4-methylimidazole, 2-methylimidazole, polyaspartic acid and an activated thixotropic agent into a stainless steel reaction kettle of an emulsifying machine, and fully stirring to obtain the soldering flux.
Encapsulating (D50:10-50um) Sn96.5-3.0Ag-Cu0.5 alloy powder and rare earth powder Rb into a vacuum quartz tube, filling high-purity nitrogen as protective gas into the vacuum quartz tube, placing the vacuum quartz tube into a reaction furnace, heating and smelting the vacuum quartz tube, and obtaining solder powder melt after the solder powder is completely melted; and then placing the molten solder powder in an inert gas protection box to cool to room temperature, and then placing the cooled molten solder powder into a die to perform hot-pressing sintering to obtain solder alloy powder.
Adding soldering flux and solder alloy powder into a double-planetary mixer for soldering paste, stirring for 1 hour to obtain the soldering paste, and refrigerating and storing in a refrigerator at 6 ℃.
The properties of the solder pastes prepared in examples 1 to 5 are shown in the following table. As can be seen from the test data of the solder pastes of the following table examples 1-5, compared with the existing solder paste, the solder paste has the advantages of high wettability, corrosion resistance, expansion rate, good thixotropy, effective reduction of generation of solder balls, less surface residue and the like, and meets the relevant detection standards. The soldering paste can be widely used for manufacturing printed PCB (printed circuit board) and components of electronic equipment such as communication equipment, computers, household appliances and the like.
Figure BDA0003240797420000101
Although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art will understand that various changes, modifications and substitutions can be made without departing from the spirit and scope of the invention as defined by the appended claims. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (10)

1. A no-clean residue-free and high-wetting SMT soldering paste comprises alloy powder and soldering flux, wherein the weight percentage of the alloy powder is 70-85%, and the SMT soldering paste is characterized in that: the soldering flux comprises:
0.5-3 wt% of rare earth powder, including one or more of cerium powder Ce, yttrium powder Y, niobium powder Nb and rubidium powder Rb, for improving strength, toughness, high temperature oxidation resistance and corrosion resistance of the solder paste;
the antioxidant with the weight percentage of 0.5-5 percent is used for avoiding the oxidation of tin powder in the soldering paste, avoiding the generation of tin balls on the board surface after welding and enabling welding spots to be bright;
4-18% of resin by weight percent, which is used for improving the initial viscosity, compatibility, adhesion, oxidation resistance, thermal stability and aging resistance of the soldering paste, so that no residue exists on the surface of the soldering paste after soldering;
1-5% of active agent by weight percentage, which is used for volatilizing after welding, so that no residue is left on the welded plate surface;
0.5-0.8% of thixotropic agent by weight percent, which is used for increasing viscosity and thixotropy and avoiding tin wire, adhesion and image blurring during printing;
0.5-5 wt% of solvent for mixing resin and thixotropic agent to obtain carrier and activated pasty thixotropic agent, and volatilizing after welding to make the welded plate surface have no residue;
the wetting agent with the weight percentage of 0.01-0.5 percent is used for being matched with the active agent to completely remove the oxide layer, so that the tin on the welding spot is full, and the wettability and the cutting-off property of the soldering paste are improved;
0.01-3% by weight of corrosion inhibitor for retarding penetrating corrosion after welding.
2. A leave-in, residue-free and highly wetting SMT solder paste according to claim 1, characterized in that: the alloy powder is micron Sn96.5-3.0Ag-Cu0.5 alloy powder with grain size of 10-50 um.
3. A leave-in, residue-free and highly wetting SMT solder paste according to claim 1, characterized in that: the antioxidant is one or a combination of two or more of butylated hydroxyanisole, dibutyl hydroxy toluene, propyl gallate, tert-butyl hydroquinone and beta (3,5 di-tert-butyl-4-hydroxyphenyl) octadecyl propionate.
4. A leave-in, residue-free and highly wetting SMT solder paste according to claim 1, characterized in that: the resin is one or the combination of two or more of rosin pentaerythritol ester, glycerin rosin ester, dihydro rosin, tetrahydro rosin, acrylic acid modified rosin, dimerized rosin and polyisobutylene.
5. A leave-in, residue-free and highly wetting SMT solder paste according to claim 1, characterized in that: the activator is one or the combination of two or more of itaconic acid, malic acid, citric acid, methyl malonic acid, methyl succinic acid, dichloroacetic acid, succinic acid, glutaric acid, diethylamine hydrobromide, 2-bromoethylamine hydrobromide, cyclohexylamine hydrobromide and cyclohexylamine hydrochloride.
6. A leave-in, residue-free and highly wetting SMT solder paste according to claim 1, characterized in that: the thixotropic agent is one or the combination of two or more of polyamide wax, hydrogenated castor oil, stearic acid amide, ethylene bisstearic acid amide and fumed silica.
7. A leave-in, residue-free and highly wetting SMT solder paste according to claim 1, characterized in that: the solvent is one or the combination of two or more of propylene glycol phenyl ether acetate, diethylene glycol butyl ether acetate, ethylene glycol monobutyl ether, ethylene glycol dimethyl ether, ethylene glycol monobutyl ether, propylene glycol, glycerol, tributyl citrate and triethylene glycol propyl ether.
8. A leave-in residue-free highly wetted SMT solder paste and method of making same according to claim 1, wherein: the wetting agent is 2.4.7.9-tetramethyl-5-decyne-4.7-diol.
9. A leave-in residue-free highly wetted SMT solder paste and method of making same according to claim 1, wherein: the corrosion inhibitor is one or the combination of two or more of benzotriazole, tolyltriazole, 2-ethyl-4-methylimidazole, 2-ethylimidazole, 2-methylimidazole, phosphono carboxylic acid and polyaspartic acid.
10. A method for preparing a leave-in residue-free and highly wetting SMT solder paste according to any of claims 1-9, characterized in that: the method comprises the following steps:
s1, adding resin into a solvent, heating to 80 ℃, and stirring at 400rpm until the resin is completely dissolved uniformly to obtain a carrier;
s2, adding the thixotropic agent into the solvent, heating to 80 ℃, stirring at 1000rpm until the thixotropic agent is fully mixed to obtain an activated thixotropic agent;
s3, sequentially adding the carrier, the wetting agent, the antioxidant, the corrosion inhibitor, the activator and the activated thixotropic agent into a stainless steel reaction kettle of an emulsifying machine, and fully stirring to obtain the soldering flux;
s4, packaging the alloy powder and the rare earth powder in a vacuum quartz tube, filling high-purity nitrogen serving as protective gas into the vacuum quartz tube, placing the vacuum quartz tube in a reaction furnace, heating and smelting the vacuum quartz tube, and obtaining a solder powder melt after the alloy powder and the rare earth powder are completely melted; then placing the molten solder powder in an inert gas protection box to cool to room temperature, and then placing the cooled molten solder powder into a die to perform hot-pressing sintering to obtain solder alloy powder;
and S5, adding the soldering flux and the solder alloy powder into a double-planet stirrer for the solder paste, stirring for 1 hour to obtain the solder paste, and refrigerating and storing the solder paste in a refrigerator at 6 ℃.
CN202111023304.6A 2021-09-01 2021-09-01 Washing-free residue-free high-wetting SMT soldering paste and preparation method thereof Pending CN113714679A (en)

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Citations (7)

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US5150832A (en) * 1991-06-28 1992-09-29 At&T Bell Laboratories Solder paste
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CN102950395A (en) * 2012-10-16 2013-03-06 高新锡业(惠州)有限公司 Environment-friendly soldering tin paste
CN104400257A (en) * 2014-10-29 2015-03-11 重庆理工大学 Scaling powder for no-clean lead-free low-silver welding paste
CN104476016A (en) * 2014-11-05 2015-04-01 苏州赛普特电子科技有限公司 Lead-free and halogen-free soldering paste for semiconductors
CN111360446A (en) * 2020-04-28 2020-07-03 深圳市邦大科技有限公司 Halogen-free lead-free soldering paste and preparation method thereof
WO2021115287A1 (en) * 2019-12-09 2021-06-17 青岛歌尔微电子研究院有限公司 Solder flux and preparation method thereof, tin paste and preparation method thereof

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5150832A (en) * 1991-06-28 1992-09-29 At&T Bell Laboratories Solder paste
CN101642855A (en) * 2009-08-19 2010-02-10 浙江一远电子材料研究院 Rear-earth-containing halogen free Sn-Ag-C series tinol
CN102950395A (en) * 2012-10-16 2013-03-06 高新锡业(惠州)有限公司 Environment-friendly soldering tin paste
CN104400257A (en) * 2014-10-29 2015-03-11 重庆理工大学 Scaling powder for no-clean lead-free low-silver welding paste
CN104476016A (en) * 2014-11-05 2015-04-01 苏州赛普特电子科技有限公司 Lead-free and halogen-free soldering paste for semiconductors
WO2021115287A1 (en) * 2019-12-09 2021-06-17 青岛歌尔微电子研究院有限公司 Solder flux and preparation method thereof, tin paste and preparation method thereof
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