CN108555474B - Halogen-free environment-friendly lead-free tin paste and preparation method thereof - Google Patents
Halogen-free environment-friendly lead-free tin paste and preparation method thereof Download PDFInfo
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- CN108555474B CN108555474B CN201810286338.6A CN201810286338A CN108555474B CN 108555474 B CN108555474 B CN 108555474B CN 201810286338 A CN201810286338 A CN 201810286338A CN 108555474 B CN108555474 B CN 108555474B
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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
- B23K35/0244—Powders, particles or spheres; Preforms made therefrom
-
- 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
-
- 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
Landscapes
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Electric Connection Of Electric Components To Printed Circuits (AREA)
Abstract
The invention belongs to the field of electronic packaging welding materials, and provides halogen-free environment-friendly lead-free tin paste and a preparation method thereof. The halogen-free environment-friendly lead-free tin paste consists of 80-90% of tin-based alloy powder and 10-20% of soldering paste; the tin-based alloy powder is one of Sn-3.0Ag-0.5Cu and Sn-3.0Ag-0.5Cu-0.01P, n-3.0Ag-0.5Cu-0.05 Pr; the flux paste comprises the following components in percentage by weight: 25-49% of rosin resin, 0.5-6% of diisooctyl fumarate, 0.5-6% of pentaerythritol palmitate, 1-10% of dimethylolbutyric acid, 0.5-2% of ethylene bis-lauric amide, 0.05-12% of surfactant, 1-8% of thixotropic agent, 25-47% of solvent and 0.2-10% of antioxidant. The lead-free tin paste is halogen-free, environment-friendly, high in expansion rate, high in surface insulation resistance, low in hole rate and resistant to thermal collapse, and is particularly suitable for the packaging requirements of high-end precise electronic products.
Description
Technical Field
The invention relates to the field of electronic packaging welding materials, in particular to halogen-free environment-friendly lead-free tin paste and a preparation method thereof.
Background
With the rapid development of the electronic industry, electronic products have more and more complete functions and wider application range, but the use environment is increasingly severe, and particularly, the mechanical reliability problem caused by the gradual reduction of the size of a welding spot in recent years brings new challenges to the use of the electronic products, and people have higher requirements on the service reliability of the electronic products. In the lead-free development process of the last decade, lead-free tin paste has been rapidly developed. Most of the lead-free solder pastes currently used in the market use halogen-containing materials as active agents (such as dibromobutenediol, cyclohexylamine hydrochloride, etc.) to remove the oxide films from the base material to be soldered and the solder powder during the soldering process. For example, chinese patent CN102069323B discloses a medium temperature tin alloy solder paste for through hole coating operation, which uses dibromobutenediol. However, if the halogen active agent is used excessively, if the halogen active agent is not properly matched, the halogen active agent is not decomposed and volatilized to remain in the welding point after the welding, which brings potential adverse effects on the mechanical property and the electrical property of the welding point, such as corrosion to the welding point and a substrate, reduction of surface insulation resistance, short circuit and the like; on the other hand, the halogen active agent volatilizes chemical smog containing halogen during the soldering heating process, and brings serious harm to the health of operators. Therefore, there is a great need for formulation improvement of currently used lead-free solder paste.
Disclosure of Invention
In order to solve the technical problems, the invention aims to provide a halogen-free environment-friendly lead-free tin paste and a preparation method thereof.
The object of the invention is achieved by at least one of the following solutions.
The lead-free solder paste comprises the following components in percentage by weight: 80-90% of tin-based alloy powder and 10-20% of flux paste;
the tin-based alloy powder comprises Sn-3.0Ag-0.5Cu, Sn-0.3Ag-0.7Cu-0.01P,
One of Sn-0.3Ag-0.7Cu-0.05Pr, Sn-1.0Ag-0.5Cu-0.01P, Sn-1 Ag-0.5Cu-0.05 Pr;
the flux paste comprises the following components in percentage by weight: 25-49% of rosin resin, 0.5-6% of diisooctyl fumarate, 0.5-6% of pentaerythritol palmitate, 1-10% of dimethylolbutyric acid, 0.5-2% of ethylene bis-lauric amide, 0.2-12% of surfactant, 1-8% of thixotropic agent, 25-47% of solvent and 0.2-10% of antioxidant.
Further, the rosin resin is one or a combination of more of perhydrogenated rosin, rosin pentaerythritol ester and modified chlorine-vinegar copolymer resin (such as the type H15/45M produced by Germany);
further, the surfactant is one or a combination of more of polyoxyethylene glycerol ether, sec-octylphenol polyoxyethylene ether and nonylphenol polyoxyethylene ether;
furthermore, the thixotropic agent is a composition of one or two of modified hydrogenated castor oil and octadecyl stearate amine; the modified hydrogenated castor oil can be ST-modified hydrogenated castor oil (THIXATROL ST).
Furthermore, the solvent is one or a combination of several of ethyl hexanediol, tetrahydrofurfuryl alcohol, propylene glycol phenyl ether, tetraethylene glycol dimethyl ether and triethyl carbitol ether;
further, the antioxidant is one or a combination of more of 2-mercaptobenzimidazole, 1-vinyl imidazole, 2-methyl imidazole and 2, 6-di-tert-butyl-4-methylphenol;
further, the preparation method of the halogen-free environment-friendly lead-free tin paste comprises the following steps:
(1) weighing the components according to the weight percentage for later use;
(2) adding rosin resin, an antioxidant and a solvent into a reaction container, heating to 130-150 ℃, and stirring for 20-40 minutes to uniformly mix;
(3) cooling the mixture obtained in the step (2) to 100-120 ℃, then adding dimethylolbutyric acid, and stirring for 20-40 minutes to uniformly mix the mixture;
(4) continuously cooling the mixture obtained in the step (3) to 70-90 ℃, then sequentially adding diisooctyl fumarate, pentaerythritol palmitate and a surfactant, and stirring for 10-30 minutes to uniformly mix the diisooctyl fumarate, the pentaerythritol palmitate and the surfactant;
(5) continuously cooling the mixture obtained in the step (4) to 50-70 ℃, then sequentially adding ethylene bis-lauric acid amide and a thixotropic agent, emulsifying for 10-30 minutes at an emulsifying speed of 4000-7000 r/min, and fully emulsifying and uniformly mixing;
(6) cooling the mixture prepared in the step (5) to room temperature, grinding for three times by using a three-roll grinder, and standing for 24-48 hours to obtain the flux paste, wherein the granularity of the flux paste is 1-5 mu m;
(7) putting the soldering paste prepared in the step (6) and the tin-based alloy powder into a tin paste stirrer, and then vacuumizing to 10 degrees of vacuum-2Pa, stirring the flux paste and the tin-based alloy powder at a stirring speed of 150-250 r/min for 30-50 minutes to uniformly mix the flux paste and the tin-based alloy powder, thus obtaining the halogen-free environment-friendly lead-free tin paste.
The invention is mainly developed aiming at the problems that the existing lead-free tin paste has a large amount of halogen raw materials, causes harm to human bodies in the welding process and has low reliability of welding spots after welding, diisooctyl fumarate and pentaerythritol palmitate are selected as active agents, the two active agents belong to liquid active agents, have good compatibility with rosin resin, antioxidant and the like, have low activity at room temperature, can decompose fumaric acid, palmitic acid and alcohol substances with strong activity in the reflow welding process, effectively remove oxides in a welded parent metal and lead-free tin powder and assist in wetting; meanwhile, the soldering flux can greatly enhance the soldering activity of the soldering flux paste by matching with a dimethylolbutyric acid activator with higher activity, so as to obtain full and bright welding spots; the ethylene bis-lauric acid amide is used for effectively improving the dispersion degree of each component of the soldering paste in the emulsification process; the thixotropic property of the tin paste can be effectively improved by using ST modified hydrogenated castor oil (THIXATROL ST) and octadecyl stearamide, so that the tin paste is easy to demould in the printing process; the imidazole substance and the methyl phenol used in the soldering process can be preferably used for the reaction between tin in tin powder and oxygen in the atmosphere, so that the oxidation of tin paste is prevented, the soldering porosity is reduced, and the mechanical strength of a soldering point is improved.
Compared with the prior art, the technology of the invention has the following characteristics:
a) the formula system of the flux paste does not contain any halogen elements of fluorine, chlorine, bromine, iodine and astatine, so that the flux paste is environment-friendly and harmless;
b) the printing process has good printing performance, no printing defects of tip pulling, cold collapse and bridging, high wettability in the brazing process and no hot collapse defect;
c) after brazing, the solder joint has low porosity, high surface insulation resistance and no cleaning, and is suitable for the packaging requirement of high-end precise electronic products.
Detailed Description
The practice of the present invention is described in further detail below with reference to specific examples, but the practice and protection of the present invention is not limited thereto.
Example 1
The halogen-free environment-friendly lead-free tin paste of the embodiment 1 of the invention comprises the following components in percentage by weight (such as 100g by total weight):
sn-3.0Ag-0.5Cu 88.5% and flux paste 11.5%;
the flux paste comprises the following components in percentage by weight: 49% of perhydrogenated rosin, 0.5% of diisooctyl fumarate, 6% of pentaerythritol palmitate, 1% of dimethylolbutyric acid, 0.5% of ethylene dilauramide, 12% of polyoxyethylene glycerol ether, 5.8% of ST-modified hydrogenated castor oil (THIXATROL ST), 10% of ethyl hexanediol, 15% of tetraethylene glycol dimethyl ether and 0.2% of 2-mercaptobenzimidazole.
The preparation method comprises the following steps:
(1) weighing the components according to the weight percentage for later use;
(2) adding perhydrogenated rosin, 2-mercaptobenzimidazole, ethylhexanediol and tetraethylene glycol dimethyl ether into a reaction vessel, heating to 130 ℃, and stirring for 20 minutes to uniformly mix the perhydrogenated rosin, the 2-mercaptobenzimidazole, the ethylhexanediol and the tetraethylene glycol dimethyl ether;
(3) cooling the mixture obtained in the step (2) to 100 ℃, adding dimethylolbutyric acid, and stirring for 20 minutes to uniformly mix the dimethylolbutyric acid and the dimethylolbutyric acid;
(4) continuously cooling the mixture obtained in the step (3) to 90 ℃, then sequentially adding diisooctyl fumarate, pentaerythritol palmitate and a surfactant, and stirring for 30 minutes to uniformly mix the diisooctyl fumarate, the pentaerythritol palmitate and the surfactant;
(5) continuously cooling the mixture obtained in the step (4) to 70 ℃, then sequentially adding ethylene bis-lauric acid amide and a thixotropic agent, emulsifying for 30 minutes at an emulsifying speed of 7000r/min, and fully emulsifying and uniformly mixing;
(6) cooling the mixture prepared in the step (5) to room temperature, grinding for three times by using a three-roll grinder, and standing for 24 hours to prepare the soldering paste, wherein the granularity of the soldering paste is 1-5 mu m;
(7) putting the soldering paste prepared in the step (6) and the weighed Sn-3.0Ag-0.5Cu tin-based alloy powder into a tin paste stirrer, and then vacuumizing the stirrer with the vacuum degree of 10-2Pa, stirring the soldering paste and the Sn-3.0Ag-0.5Cu tin-based alloy powder at a stirring speed of 250r/min for 50 minutes to uniformly mix the soldering paste and the Sn-3.0Ag-0.5Cu tin-based alloy powder, thus obtaining the halogen-free environment-friendly lead-free tin paste.
Example 2
The halogen-free environment-friendly lead-free tin paste of embodiment 2 of the invention comprises the following components in percentage by weight:
sn-0.3Ag-0.7Cu-0.01P 90% and flux paste 10%;
the flux paste comprises the following components in percentage by weight: 10% of rosin pentaerythritol ester, 15% of H15/45M modified vinyl chloride-acetate copolymer resin, 6% of diisooctyl fumarate, 0.5% of pentaerythritol palmitate, 10% of dimethylolbutyric acid, 2% of ethylene bis-laurate amide, 0.1% of sec-octylphenol polyoxyethylene ether, 0.1% of nonylphenol polyoxyethylene ether, 4% of ST-modified hydrogenated castor oil (THIXATROL ST), 4% of octadecyl stearate amine, 38.3% of triethylcarbitol ether, 5% of 1-vinylimidazole and 5% of 2-methylimidazole.
The preparation method can refer to example 1.
Example 3
The halogen-free environment-friendly lead-free tin paste of embodiment 3 of the invention comprises the following components in percentage by weight:
80 percent of Sn-0.3Ag-0.7Cu-0.05Pr and 20 percent of flux paste;
the flux paste comprises the following components in percentage by weight: 32% of rosin pentaerythritol ester, 6% of diisooctyl fumarate, 4% of pentaerythritol palmitate, 3% of dimethylolbutyric acid, 1% of ethylene dilauramide, 1% of polyoxyethylene glycerol ether, 2% of sec-octylphenol polyoxyethylene ether, 2% of nonylphenol polyoxyethylene ether, 1% of octadecyl stearate amine, 15% of ethyl hexanediol, 15% of tetrahydrofurfuryl alcohol, 17% of propylene glycol phenyl ether and 1% of 2, 6-di-tert-butyl-4-methylphenol.
The preparation method can refer to example 1.
Example 4
The halogen-free environment-friendly lead-free tin paste of embodiment 4 of the invention comprises the following components in percentage by weight:
sn-1.0Ag-0.5Cu-0.01P 88% and flux paste 12%;
the flux paste comprises the following components in percentage by weight: 20% of perhydrogenated rosin, 10% of rosin pentaerythritol ester, 10% of H15/45M modified vinyl chloride-acetate copolymer resin, 3% of diisooctyl fumarate, 4% of pentaerythritol palmitate, 5% of dimethylolbutyric acid, 1% of ethylene bis-lauric acid amide, 3% of polyoxyethylene glycerol ether, 6% of octadecyl stearate amine, 14% of tetrahydrofurfuryl alcohol, 20% of propylene glycol phenyl ether and 4% of 2, 6-di-tert-butyl-4-methylphenol.
The preparation method can refer to example 1.
Example 5
The halogen-free environment-friendly lead-free tin paste of embodiment 5 of the invention comprises the following components in percentage by weight:
sn-1.0Ag-0.5Cu-0.01P 88.5% and flux paste 11.5%;
the flux paste comprises the following components in percentage by weight: 30% of perhydrogenated rosin, 15% of H15/45M modified vinyl chloride-acetate copolymer resin, 2% of diisooctyl fumarate, 1% of pentaerythritol palmitate, 8% of dimethylolbutyric acid, 1.5% of ethylene dilauramide, 2% of sec-octylphenol polyoxyethylene ether, 7% of ST modified hydrogenated castor oil (THIXATROL ST), 20% of tetraethylene glycol dimethyl ether, 8.5% of triethylcarbitol ether and 5% of 2, 6-di-tert-butyl-4-methylphenol.
The preparation method can refer to example 1.
The properties of examples 1 to 5 of the above invention were evaluated according to GB/T9491-2002 and IPC-TM-650, and the results are shown in Table 1.
Table 1 evaluation results of examples 1 to 5
The evaluation results in table 1 show that the halogen-free environmentally friendly lead-free solder paste of the present invention has the advantages of high spreading rate, high surface insulation resistance, low void ratio, cold and thermal collapse resistance, etc., and can meet the packaging requirements of high-end precision electronic products.
Claims (5)
1. The halogen-free environment-friendly lead-free tin paste is characterized by comprising the following components in percentage by weight: 80-90% of tin-based alloy powder and 10-20% of flux paste;
the tin-based alloy powder is one of Sn-3.0Ag-0.5Cu, Sn-0.3Ag-0.7Cu-0.01P, Sn-0.3Ag-0.7Cu-0.05Pr, Sn-1.0Ag-0.5Cu-0.01P, Sn-1 Ag-0.5Cu-0.05 Pr;
the flux paste comprises the following components in percentage by weight: 25-49% of rosin resin, 0.5-6% of diisooctyl fumarate, 0.5-6% of pentaerythritol palmitate, 1-10% of dimethylolbutyric acid, 0.5-2% of ethylene bis-lauric amide, 0.2-12% of surfactant, 1-8% of thixotropic agent, 25-47% of solvent and 0.2-10% of antioxidant; the antioxidant is one or a combination of more of 2-mercaptobenzimidazole, 1-vinyl imidazole, 2-methylimidazole and 2, 6-di-tert-butyl-4-methylphenol; the surfactant is one or a combination of more of polyoxyethylene glycerol ether, sec-octyl phenol polyoxyethylene ether and nonyl phenol polyoxyethylene ether; the thixotropic agent is one or a combination of modified hydrogenated castor oil and octadecyl stearate amine.
2. The halogen-free environmentally friendly lead-free solder paste as claimed in claim 1, wherein the rosin resin is one or more of perhydrogenated rosin, pentaerythritol rosin and modified vinyl chloride-acetate copolymer resin.
3. The halogen-free environmentally friendly lead-free tin paste of claim 1, wherein the solvent is one or more selected from the group consisting of ethyl hexanediol, tetrahydrofurfuryl alcohol, propylene glycol phenyl ether, tetraethylene glycol dimethyl ether and triethylcarbitol ether.
4. The method for preparing the halogen-free environmentally friendly lead-free tin paste of any one of claims 1 to 3, characterized by comprising the following steps:
(1) weighing the components according to the weight percentage for later use;
(2) adding rosin resin, an antioxidant and a solvent into a reaction container, heating to 130-150 ℃, and stirring to uniformly mix; stirring for 20-40 minutes;
(3) cooling the mixture finally obtained in the step (2) to 100-120 ℃, then adding dimethylolbutyric acid, and stirring to uniformly mix the dimethylolbutyric acid;
(4) continuously cooling the mixture finally obtained in the step (3) to 70-90 ℃, then sequentially adding diisooctyl fumarate, pentaerythritol palmitate and a surfactant, and stirring to uniformly mix the diisooctyl fumarate, the pentaerythritol palmitate and the surfactant; stirring for 10-30 minutes;
(5) continuously cooling the mixture finally obtained in the step (4) to 50-70 ℃, then sequentially adding ethylene bis-lauric acid amide and a thixotropic agent, fully emulsifying by using an emulsifying machine, and uniformly mixing;
(6) cooling the mixture prepared in the step (5) to room temperature, grinding for three times by using a three-roll grinder, and standing for 24-48 hours to obtain the flux paste, wherein the granularity of the flux paste is 1-5 mu m;
(7) placing the soldering paste prepared in the step (6) and the tin-based alloy powder into a tin paste stirrer, and thenThen vacuum is drawn, the vacuum degree is 10-2Pa, stirring the flux paste and the tin-based alloy powder at a stirring speed of 150-250 r/min for 30-50 minutes to uniformly mix the flux paste and the tin-based alloy powder, thus obtaining the halogen-free environment-friendly lead-free tin paste.
5. The method of claim 4, wherein the emulsifying time in step (5) is 10-30 minutes, and the rotation speed of the emulsifying machine is 4000-7000 r/min.
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| CN109604859B (en) * | 2018-11-30 | 2021-07-23 | 湖南人文科技学院 | Preparation method of solder paste for ceramic packaging, ceramic and packaging method thereof |
| CN111136402A (en) * | 2019-12-20 | 2020-05-12 | 深圳市朝日电子材料有限公司 | Enhanced composite soldering paste and preparation method thereof |
| CN113210931A (en) * | 2021-05-13 | 2021-08-06 | 北京达博长城锡焊料有限公司 | Soldering flux for solder paste, preparation method thereof and halogen-free and lead-free solder paste |
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