CN111299896A - Soldering paste and preparation method thereof - Google Patents
Soldering paste and preparation method thereof Download PDFInfo
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- CN111299896A CN111299896A CN202010165782.XA CN202010165782A CN111299896A CN 111299896 A CN111299896 A CN 111299896A CN 202010165782 A CN202010165782 A CN 202010165782A CN 111299896 A CN111299896 A CN 111299896A
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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
- 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
-
- 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
Abstract
The invention provides a soldering paste and a preparation method thereof, and relates to the technical field of welding materials. The soldering paste comprises 90.2-91.8 parts of lead-free metal alloy powder and 8.2-9.8 parts of flux paste; wherein the flux paste comprises 37-45 parts of a film forming agent, 30-38 parts of a solvent, 10-18 parts of an activating agent, 4-5.5 parts of a thixotropic agent, 1-2.5 parts of a surfactant, 0.4-0.8 part of an antioxidant and 0.3-0.6 part of a corrosion inhibitor; and the activator includes an organic acid and a bromine-containing compound. The solder paste can be applied to soldering of electrode terminals of a fuse. Continuous production can be realized through reflow soldering, the production efficiency is greatly improved, the connection between the copper cap and the copper handle is tight after welding, the soldering tin on the peripheral edge is smooth and full, no sand hole exists, the cavity area is small, and the electric conductivity and the connection strength are greatly improved.
Description
Technical Field
The invention relates to the technical field of welding materials, in particular to a soldering paste and a preparation method thereof.
Background
The tube fuse is composed of a fuse body and a fuse holder, in which electrode terminals of the fuse are required to have good electrical conductivity and coupling strength. The electrode terminal part mainly comprises a copper cap and an L-shaped copper handle. The connection between the copper cap and the L-shaped copper handle is mainly realized by argon arc welding or rivet connection in the past. The argon arc welding has high welding cost, low efficiency and high working strength, only welding materials are arranged around the copper cap, the whole bottom cavity has large area, and the contact area is small. The rivet is lower in connection efficiency, poor connection can damage the copper part body and influence conductivity and strength, and the whole bottom cavity area is larger.
Disclosure of Invention
The invention aims to provide the soldering paste which has strong welding strength, high conductivity of an electrode terminal after welding and high connection strength.
The invention also aims to provide a preparation method of the soldering paste, which adopts a grinding process and an emulsification process to obtain a uniform and fine product.
The technical problem to be solved by the invention is realized by adopting the following technical scheme.
The invention provides a soldering paste which comprises 90.2-91.8 parts by weight of lead-free metal alloy powder and 8.2-9.8 parts by weight of soldering paste;
the flux paste comprises, by weight, 37-45 parts of a film forming agent, 30-38 parts of a solvent, 10-18 parts of an activator, 4-5.5 parts of a thixotropic agent, 1-2.5 parts of a surfactant, 0.4-0.8 part of an antioxidant and 0.3-0.6 part of a corrosion inhibitor; the activator includes an organic acid and a bromine-containing compound.
The invention also provides a preparation method of the soldering paste, which comprises the following steps:
mixing the film forming agent and part of the solvent, heating to 145-150 ℃, cooling to 100-110 ℃ after complete dissolution, then placing in a sealed container, and storing in 8-12 ℃ cooling water for 6-10 hours to obtain a first paste body;
adding the activator and the thixotropic agent into the paste, and grinding until the paste fineness is not more than 15 mu m to obtain a second paste;
emulsifying the second paste, and adding an intermediate in the emulsifying process to obtain the soldering paste, wherein the intermediate is a mixture of a surfactant, an antioxidant, a corrosion inhibitor and the rest of the solvent;
and mixing the soldering paste and the lead-free metal alloy powder, and stirring to obtain the soldering paste.
The solder paste and the preparation method thereof have the beneficial effects that:
1) the activator in the flux paste simultaneously adopts organic acid and the activator containing the compound bromine, the activator containing the compound bromine can decompose halogen at a certain temperature during welding, the flux paste has good flux activity, long action time and strong welding force, and the welded fuse electrode terminal has few bubbles inside, reduces the cavity area, and greatly improves the conductivity and the connection strength.
2) The solder paste adopts the compound thixotropic agent, the printing resistance of the solder paste can be improved by adopting the fatty acid amide thixotropic agent, the collapse resistance of the solder paste can be improved by compounding a small amount of fumed silica thixotropic agent, the peripheral tin overflow of the electrode terminal of the fuse during welding can be avoided, and the smoothness and fullness of soldering tin at the edge of the electrode terminal after welding are ensured.
3) The grinding process and the emulsifying process are adopted in the preparation process, so that the uniform and fine soldering paste can be prepared, the printing performance of the soldering paste can be improved, and the storage time can be prolonged.
4) The melting range of the soldering paste prepared from the soldering paste and the lead-free metal alloy powder is 217-227 ℃, the soldering paste can be soldered by using common SMT reflow soldering equipment, continuous production can be realized by reflow soldering, and the production efficiency is greatly improved.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained according to the drawings without inventive efforts.
Fig. 1 is a flow chart of a method of preparing a solder paste according to an embodiment of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
The solder paste and the method of manufacturing the same according to the embodiments of the present invention will be described in detail below.
The solder paste provided by the embodiment of the invention comprises 90.2-91.8 parts by weight of lead-free metal alloy powder and 8.2-9.8 parts by weight of soldering paste.
In one embodiment, the lead-free metal alloy powder is a SnAgCu metal alloy powder. Preferably, the grain size of the SnAgCu metal alloy powder is 45-75 μm, and the grain size is larger than that of the conventional SMT (surface mount technology), so that the generation of voids during welding is reduced, and the welding strength is increased. The weight ratio of Sn, Ag and Cu is 98.8-99.2: 0.2-0.4: 0.6 to 0.8. More preferably, the weight ratio of Sn, Ag and Cu is 99.0:0.3: 0.7. The lead-free SnAgCu is selected, the raw material source is wide, the silver content is low, and the cost can be effectively reduced. And the alloy powder does not contain zinc, so that the oxidation of the solder can be effectively avoided, and various defects in welding, such as large cavities, more tin balls and the like, can be reduced.
In this embodiment, the flux paste comprises, by weight, 37 to 45 parts of a film forming agent, 30 to 38 parts of a solvent, 10 to 18 parts of an activator, 4 to 5.5 parts of a thixotropic agent, 1 to 2.5 parts of a surfactant, 0.4 to 0.8 part of an antioxidant, and 0.3 to 0.6 part of a corrosion inhibitor. The soldering flux paste under the proportion can enable the welded electrode terminal of the fuse to be welded tightly, and has the advantages of smooth and flat surface and high connection strength.
In one embodiment, the film forming agent is selected from one or more of hydrogenated rosin resin, acryl rosin, polymerized rosin, phenolic resin, polyurethane, pentaerythritol rosin ester, polyethylene glycol 1500 and polyethylene glycol 2000. By adopting the film forming agent, the protective film can be formed to coat the welding spot at the welding temperature in the welding process, so that the corrosion resistance is improved, and the film forming agent is favorable for improving the storage stability of the soldering paste.
In one embodiment, the solvent is selected from one or more of dibutyl succinate, triethylene glycol propyl ether, diethylene glycol butyl ether, tetraethylene glycol dimethyl ether, ethylene glycol phenyl ether, diethylene glycol hexyl ether, and dibutyl maleate.
In this embodiment, the activator includes an organic acid and a bromine-containing compound. The activator containing bromine in chemical state can decompose halogen at certain temperature during welding, and has good welding-aid activity, long action time and strong welding force. Preferably, the organic acid is selected from one or more of 4-n-butylbenzoic acid, aminobenzoic acid, bipropionic acid, p-hydroxyphenylacetic acid, a polyacid, a dimer acid and maleic acid, and the bromine-containing compound is selected from one or more of 2, 3-dibromobutenediol, tris (2, 3-dibromopropyl) isocyanate and 2, 3-dibromosuccinic acid. More preferably, the activator is comprised of two organic acids and a bromine-containing chemical. The weight ratio of the organic acid to the bromine-containing compound is 11-15: 1-2. The activator obtained under the conditions can ensure that few bubbles are in the electrode terminal of the fuse after welding, reduce the area of a cavity and greatly improve the conductivity and the connection strength.
In one embodiment, the thixotropic agent is selected from at least two of a polyamide wax, a fatty acid amide, and fumed silica. The fatty acid amide may be ethylene bis-lauric acid amide, ethylene bis-stearic acid amide, or the like. Preferably, the thixotropic agent is selected from a mixture of a polyamide wax and fumed silica, or a mixture of a fatty acid amide and fumed silica. The thixotropic agent obtained by compounding the polyamide wax or the fatty acid amide with the fumed silica can improve the printing resistance of the solder paste, improve the collapse resistance of the solder paste, avoid tin overflow around the electrode terminal of the fuse during welding and ensure that the edge of the electrode terminal is smooth and full in soldering tin after welding.
In one embodiment, the surfactant is selected from one or more of tetra (2-hydroxypropyl) ethylenediamine, aromatic amine, trimethylamine, aniline, and diethylpropylamine.
In one embodiment, the antioxidant is selected from one or more of antioxidant 1010, antioxidant DLTP, antioxidant BHT, antioxidant TBHQ.
In one embodiment, the corrosion inhibitor is selected from one or more of triallyl isocyanurate, 2-phenylimidazole and 2-ethylimidazole.
The embodiment of the invention also provides a preparation method of the soldering paste, which comprises the following steps:
s1, mixing the film forming agent and part of the solvent, heating to 145-150 ℃, cooling to 100-110 ℃ after complete dissolution, then placing in a sealed container, and storing in 8-12 ℃ cooling water for 6-10 hours to obtain a first paste.
And S2, adding an activator and a thixotropic agent into the first paste, and grinding until the paste fineness is not more than 15 mu m to obtain a second paste. In the step, the activating agent and the thixotropic agent are added and ground together with the first paste, so that the paste is prevented from forming micelles. In a preferred embodiment, the grinding step is: coarse grinding twice and fine grinding once, and repeating the grinding process until the paste fineness is less than 15 μm.
And S3, emulsifying the second paste, and adding an intermediate in the emulsifying process to obtain the soldering paste, wherein the intermediate is a mixture of a surfactant, an antioxidant, a corrosion inhibitor and the residual solvent.
In one embodiment, the step of emulsifying the second paste comprises:
(1) and (3) placing the second paste into emulsification equipment, and stirring at the temperature of 40-45 ℃ at the speed of 25-35 r/min for 5-15 min. Firstly, low-speed anchor stirring is carried out, so that the paste is preliminarily mixed.
(2) The temperature is maintained at 40-45 ℃ and the stirring speed is 35-45 r/min (anchor stirring), 1400-1600 r/min (distributed shearing 1) and 1700-1900 r/min (distributed shearing 2) for 55-65 min. In the step, the paste adhered to the stirring device is cleaned before stirring, so that the emulsification uniformity is ensured. And simultaneously operating an anchor type stirring piece, a distributed type shearing piece 1 and a distributed type shearing piece 2 on the emulsifying equipment, and completing preliminary emulsification of the paste body through the processes of low-speed anchor type stirring, medium-speed distributed type stirring and high-speed distributed type stirring.
(3) Heating to 50-55 ℃, and stirring at 35-45 r/min (anchor stirring), 1400-1600 r/min (distributed shearing 1), 1700-1900 r/min (distributed shearing 2) for 55-65 min. Similarly, in the step, the paste adhered to the stirring device is cleaned before stirring, so that the emulsification uniformity is ensured. And (3) after the temperature is raised, repeating the stirring process in the step (2) to further promote the mixing and emulsification of the components.
(4) Cooling to 25-35 ℃, and stirring at 35-45 r/min (anchor stirring), 1400-1600 r/min (distributed shearing 1), 1700-1900 r/min (distributed shearing 2) for 55-65 min. And the temperature is reduced and the stirring is carried out after the temperature is raised and the stirring, so that the formation of a micelle after the temperature is reduced is avoided, and the storage stability of the product can be further improved.
(5) Stirring at 25-35 deg.C at 35-45 r/min (anchor stirring), 1700-1900 r/min (distributed shearing 1), 1900-2100 r/min (distributed shearing 2) for 55-65 min, and dripping the intermediate during stirring. In the later stage of emulsification, surfactant, antioxidant, corrosion inhibitor and residual solvent are added at a lower temperature to avoid damaging material components by temperature. The components are controlled to be dripped in the stirring process, and the speed of distributed stirring is increased, so that the components are mixed with the original components to the maximum extent.
(6) The temperature is maintained at 25-35 ℃, and the stirring is carried out for 25-35 min at the speed of 35-45 r/min (anchor stirring), 1700-1900 r/min (distributed shearing 1) and 1900-2100 r/min (distributed shearing 2). After all the materials are added, the stirring process of low speed, medium speed and high speed is continued, and the emulsifying effect is further improved.
(7) And maintaining the temperature at 25-35 ℃, vacuumizing to 0.07-0.09 MPa, and stirring at the speed of 35-45 r/min for 25-35 min to obtain the flux paste. And finally, carrying out low-speed anchor stirring after vacuumizing to finish the emulsification process of the flux paste.
And finally completing the emulsification of the soldering paste by sequentially carrying out the seven steps. By controlling the parameters of stirring speed, temperature, time and the like of each step, the uniform and fine soldering paste is finally prepared, the printing performance of the soldering paste can be improved, and the storage time is prolonged by more than one time.
And S4, mixing the flux paste and the lead-free metal alloy powder, and stirring to obtain the solder paste.
In one embodiment, the step of stirring the flux paste and the lead-free metal alloy powder comprises:
stirring at the speed of 15-25 r/min for 5-15 min at the temperature of 20-30 ℃; then, the temperature is maintained at 20-30 ℃, and the mixture is stirred for 15-25 min at the speed of 25-35 r/min; and finally, maintaining the temperature at 20-30 ℃, vacuumizing to 0.07-0.09 MPa, and stirring at the speed of 25-35 r/min for 15-25 min. In the step, the paste adhered to the stirring device is cleaned before each stirring stage, so that the emulsification uniformity is ensured.
The embodiment of the invention also provides the solder paste for reflow soldering of the electrode terminal of the fuse, and the reflow soldering steps and conditions are as follows:
| step (ii) of | Process for producing a metal oxide | Temperature of | Retention time s | Rate of temperature rise/s |
| 1 | Preheating zone | Room temperature to 150 deg.c | 120 | 1～2 |
| 2 | Thermal insulation area | 150～180 | 60～120 | 1～3 |
| 3 | Reflux zone | 217～245～217 | 30～90 | 1～3 |
| 4 | Cooling zone | At room temperature | / | -3～-4 |
The melting range of the solder paste prepared by the embodiment of the invention is 217-227 ℃, the solder paste can be welded by common SMT reflow soldering equipment, continuous production can be realized by reflow soldering, and the production efficiency is greatly improved.
The features and properties of the present invention are described in further detail below with reference to examples.
Example 1
The solder paste provided by the embodiment is prepared according to the following steps:
1) the flux paste comprises the following components in parts by weight: 30 parts of hydrogenated rosin resin, 8 parts of polymerized rosin, 5 parts of pentaerythritol rosin ester, 20 parts of dibutyl succinate, 16 parts of ethylene glycol phenyl ether, 6 parts of 4-n-butyl benzoic acid, 6 parts of polyacid, 1.2 parts of 2, 3-dibromosuccinic acid, 4 parts of polyamide wax, 0.8 part of fumed silica, 2 parts of tetra (2-hydroxypropyl) ethylenediamine, 10100.5 parts of antioxidant and 0.5 part of triallyl isocyanurate.
2) Hydrogenated rosin resin, polymerized rosin and pentaerythritol rosin ester are added into a partial solvent, heated to 150 ℃ for dissolution, naturally cooled to 105 ℃, covered in initial cooling water (10 +/-2 ℃) and ground after eight hours.
3) Adding an activating agent and a thixotropic agent into the mixture obtained in the step 2) and grinding the mixture until the paste fineness is less than 15 mu m.
4) And (3) emulsifying the paste in the step 3) according to the parameters in the table 1 to obtain the flux paste. Wherein the intermediate is a mixed solution of a surfactant, an antioxidant, a corrosion inhibitor and the residual solvent.
TABLE 1
5) Mixing 90.5 percent of metal alloy powder Sn99.0Ag0.3Cu0.7 percent by weight and 9.5 percent of flux paste by weight, and stirring according to the parameters in the table 2 to obtain the soldering paste.
TABLE 2
Example 2
The solder paste provided by the embodiment is prepared according to the following steps:
1) the flux paste comprises the following components in parts by weight: 28 parts of acrylic rosin, 6 parts of polymerized rosin, 15007 parts of polyethylene glycol, 18 parts of triethylene glycol propyl ether, 18 parts of dibutyl maleate, 5 parts of p-hydroxyphenylacetic acid, 8 parts of maleic acid, 1.8 parts of 2, 3-dibromobutylene glycol, 4.5 parts of ethylene dilauramide, 0.6 part of fumed silica, 2.2 parts of aniline, 0.6 part of antioxidant BHT and 0.3 part of 2-phenylimidazole.
2) Adding acrylic rosin, polymerized rosin and polyethylene glycol 1500 into an organic solvent, heating to 150 ℃ for dissolving, naturally cooling to 105 ℃, covering in initial cooling water (10 +/-2 ℃), and grinding after eight hours.
3) Adding an activating agent and a thixotropic agent into the mixture obtained in the step 2) and grinding the mixture until the paste fineness is less than 15 mu m.
4) The paste of 3) above was emulsified according to the parameters of table 1 in example 1 to obtain a flux paste. Wherein the intermediate is a mixed solution of a surfactant, an antioxidant, a corrosion inhibitor and the residual solvent.
5) The metal alloy powder of 91.0 percent by weight and the flux paste of 9.0 percent by weight are mixed, and the mixture is stirred according to the parameters in the table 2 in the example 1 to obtain the soldering paste.
Example 3
The solder paste provided by the embodiment is prepared according to the following steps:
the flux paste comprises the following components in parts by weight: 21 parts of acrylic rosin, 9 parts of polymerized rosin, 8 parts of pentaerythritol rosin ester, 15 parts of diethylene glycol hexyl ether, 20 parts of tetraethylene glycol dimethyl ether, 7 parts of bi-dipropionic acid, 8 parts of aminobenzoic acid, 1.1 parts of 2, 3-dibromobutylene glycol, 4.0 parts of ethylene bis stearamide, 1.0 part of fumed silica, 1.9 parts of trimethylamine, 0.5 part of antioxidant DLTP and 0.5 part of 2-ethylimidazole.
2) Adding acrylic rosin, polymerized rosin and pentaerythritol rosin ester into a partial solvent, heating to 150 ℃ for dissolving, naturally cooling to 105 ℃, sealing in initial cooling water (10 +/-2 ℃), and grinding after eight hours.
3) Adding an activating agent and a thixotropic agent into the mixture obtained in the step 2) and grinding the mixture until the paste fineness is less than 15 mu m.
4) The paste of 3) above was emulsified according to the parameters of table 1 in example 1 to obtain a flux paste. Wherein the intermediate is a mixed solution of a surfactant, an antioxidant, a corrosion inhibitor and the residual solvent.
5) Mixing the metal alloy powder of 90.8 wt% and the flux paste of 9.2 wt%, and stirring according to the parameters in table 2 in example 1 to obtain the solder paste.
Comparative example 1
The comparative example provides a solder paste, which is prepared according to the following steps:
1) the flux paste comprises the following components in parts by weight: 30 parts of hydrogenated rosin resin, 8 parts of polymerized rosin, 5 parts of pentaerythritol rosin ester, 20 parts of dibutyl succinate, 16 parts of ethylene glycol phenyl ether, 6 parts of 4-n-butyl benzoic acid, 6 parts of polyacid, 1.2 parts of 2, 3-dibromosuccinic acid, 4 parts of polyamide wax, 0.8 part of fumed silica, 2 parts of tetra (2-hydroxypropyl) ethylenediamine, 10100.5 parts of antioxidant and 0.5 part of triallyl isocyanurate.
2) Hydrogenated rosin resin, polymerized rosin and pentaerythritol rosin ester are added into a partial solvent, heated to 150 ℃ for dissolution, naturally cooled to 105 ℃, covered in initial cooling water (10 +/-2 ℃) and ground after eight hours. Adding an activating agent, a thixotropic agent, a surfactant, an antioxidant and a corrosion inhibitor into the mixture obtained in the step 2), uniformly stirring, and grinding until the paste fineness is less than 15 mu m to obtain the soldering paste.
3) Adding an activating agent, a thixotropic agent, a surfactant, an antioxidant and a corrosion inhibitor into the paste obtained in the step 2), uniformly stirring, and grinding until the paste fineness is less than 15 mu m to obtain the soldering paste.
4) The metal alloy powder and the flux paste are mixed according to the weight percentage of 90.5 percent and 9.5 percent, and the mixture is stirred according to the parameters in the table 2 in the embodiment 1 to obtain the soldering paste.
Comparative example 2
The comparative example provides a solder paste, which is prepared according to the following steps:
1) the flux paste comprises the following components in parts by weight: 28 parts of acrylic rosin, 6 parts of polymerized rosin, 15007 parts of polyethylene glycol, 18 parts of triethylene glycol propyl ether, 18 parts of dibutyl maleate, 5 parts of p-hydroxyphenylacetic acid, 8 parts of maleic acid, 1.8 parts of 2, 3-dibromobutylene glycol, 4.5 parts of ethylene dilauramide, 0.6 part of fumed silica, 2.2 parts of aniline, 0.6 part of antioxidant BHT and 0.3 part of 2-phenylimidazole.
2) Adding acrylic rosin, polymerized rosin and polyethylene glycol 1500 into an organic solvent, heating to 150 ℃ for dissolving, naturally cooling to 105 ℃, covering in initial cooling water (10 +/-2 ℃), and grinding after eight hours.
3) Adding an activating agent, a thixotropic agent, a surfactant, an antioxidant and a corrosion inhibitor into the paste obtained in the step 2), uniformly stirring, and grinding until the paste fineness is less than 15 mu m to obtain the soldering paste.
4) The metal alloy powder and the flux paste are mixed according to the weight percentage of 91.0 percent and 9.0 percent, and the mixture is stirred according to the parameters in the table 2 in the example 1 to obtain the soldering paste.
Comparative example 3
The comparative example provides a solder paste, which is prepared according to the following steps:
1) the flux paste comprises the following components in parts by weight: 21 parts of acrylic rosin, 9 parts of polymerized rosin, 8 parts of pentaerythritol rosin ester, 15 parts of diethylene glycol hexyl ether, 20 parts of tetraethylene glycol dimethyl ether, 7 parts of bi-dipropionic acid, 8 parts of aminobenzoic acid, 1.1 parts of 2, 3-dibromobutylene glycol, 4.0 parts of ethylene bis stearamide, 1.0 part of fumed silica, 1.9 parts of trimethylamine, 0.5 part of antioxidant DLTP and 0.5 part of 2-ethylimidazole.
2) Adding acrylic rosin, polymerized rosin and pentaerythritol rosin ester into an organic solvent, heating to 150 ℃ for dissolving, naturally cooling to 105 ℃, sealing in initial cooling water (10 +/-2 ℃), and grinding after eight hours.
3) Adding an activating agent, a thixotropic agent, a surfactant, an antioxidant and a corrosion inhibitor into the paste obtained in the step 2), uniformly stirring, and grinding until the paste fineness is less than 15 mu m to obtain the soldering paste.
4) Mixing the metal alloy powder with 90.8 wt% and the flux paste with 9.2 wt%, and stirring according to the parameters in the table 2 in the examples to obtain the soldering paste.
Test example 1
The solder pastes obtained in examples 1 to 3 were soldered to the electrode terminals of the fuse in accordance with the parameters of the reflow soldering, 5 sets of examples were prepared, and the test results are shown in table 3 below:
TABLE 3
Therefore, when the soldering paste obtained by the embodiment of the invention is used for reflow soldering of the electrode terminal of the fuse, the inside of the electrode terminal of the fuse is almost free of bubbles after soldering, the soldering force is strong, and the electric conductivity is good.
Test example 2
The solder pastes obtained in examples 1 to 3 and comparative example were tested for printing performance and storage performance, and the test results are shown in Table 4.
TABLE 4
Therefore, the emulsification step plays a key role in the storage performance and the printing performance of the solder paste, the storage time of the solder paste is increased from 3 months to more than 6 months through multi-program emulsification treatment, the continuous printing life is prolonged from 3-4 hours to more than 8 hours, the adhesion is not easy to occur, and the service performance is extremely excellent.
The embodiments described above are some, but not all embodiments of the invention. The detailed description of the embodiments of the present invention is not intended to limit the scope of the invention as claimed, but is merely representative of selected embodiments of the invention. 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.
Claims (10)
1. A solder paste is characterized in that,
the lead-free solder paste comprises 90.2-91.8 parts by weight of lead-free metal alloy powder and 8.2-9.8 parts by weight of solder paste;
the flux paste comprises, by weight, 37-45 parts of a film forming agent, 30-38 parts of a solvent, 10-18 parts of an activator, 4-5.5 parts of a thixotropic agent, 1-2.5 parts of a surfactant, 0.4-0.8 part of an antioxidant and 0.3-0.6 part of a corrosion inhibitor; the activator includes an organic acid and a bromine-containing compound.
2. The solder paste as claimed in claim 1, wherein the lead-free metal alloy powder is a SnAgCu metal alloy powder having a particle size of 45 to 75 μm, and a weight ratio of Sn, Ag, and Cu is 98.8 to 99.2: 0.2-0.4: 0.6 to 0.8.
3. Solder paste according to claim 1, characterized in that the organic acid is selected from one or more of 4-n-butylbenzoic acid, aminobenzoic acid, bisdipropionic acid, p-hydroxyphenylacetic acid, a polyacid, a dimer acid and maleic acid, and the bromine-containing compound is selected from one or more of 2, 3-dibromobutenediol, tris (2, 3-dibromopropyl) isocyanate and 2, 3-dibromosuccinic acid.
4. Solder paste according to claim 1, characterized in that the thixotropic agent is selected from at least two of the group consisting of polyamide waxes, fatty acid amides and fumed silica.
5. Solder paste according to claim 1, characterized in that the corrosion inhibitor is selected from one or more of triallyl isocyanurate, 2-phenylimidazole and 2-ethylimidazole.
6. Solder paste according to claim 1, characterized in that the film former is selected from one or more of hydrogenated rosin resin, acryl rosin, polymerized rosin, phenolic resin, polyurethane, pentaerythritol rosin ester, polyethylene glycol 1500 and polyethylene glycol 2000.
7. Solder paste according to claim 1, characterized in that the solvent is selected from one or more of dibutyl succinate, triethylene glycol propyl ether, diethylene glycol butyl ether, tetraethylene glycol dimethyl ether, ethylene glycol phenyl ether, diethylene glycol hexyl ether and dibutyl maleate.
8. A method for preparing a solder paste as defined in any one of claims 1 to 7, characterized by comprising the steps of:
mixing the film forming agent and part of the solvent, heating to 145-150 ℃, cooling to 100-110 ℃ after complete dissolution, then placing in a sealed container, and storing in 8-12 ℃ cooling water for 6-10 hours to obtain a first paste body;
adding the activator and the thixotropic agent into the first paste, and grinding until the paste fineness is not more than 15 mu m to obtain a second paste;
emulsifying the second paste, and adding an intermediate in the emulsifying process to obtain the soldering paste, wherein the intermediate is a mixture of a surfactant, an antioxidant, a corrosion inhibitor and the rest of the solvent;
and mixing the soldering paste and the lead-free metal alloy powder, and stirring to obtain the soldering paste.
9. The method for preparing solder paste as claimed in claim 8, wherein the step of emulsifying the second paste comprises:
(1) putting the second paste body into emulsification equipment, and stirring at the temperature of 40-45 ℃ at the speed of 25-35 r/min in an anchor type manner for 5-15 min;
(2) keeping the temperature at 40-45 ℃, and simultaneously operating anchor type stirring at the speed of 35-45 r/min, distributed shearing at the speed of 1400-1600 r/min and distributed shearing at the speed of 1700-1900 r/min, and stirring for 55-65 min;
(3) heating to 50-55 ℃, and simultaneously carrying out anchor type stirring at the speed of 35-45 r/min, distributed shearing at the speed of 1400-1600 r/min and distributed shearing at the speed of 1700-1900 r/min, and stirring for 55-65 min;
(4) cooling to 25-35 ℃, and stirring for 55-65 min by 35-45 r/min and anchor stirring at the running speed of 35-45 r/min, distributed shearing at the speed of 1400-1600 r/min and distributed shearing at the speed of 1700-1900 r/min;
(5) stirring for 55-65 min at the temperature of 25-35 ℃ by using 35-45 r/min and simultaneously operating anchor stirring at the speed of 35-45 r/min, distributed shearing at the speed of 1700-1900 r/min and distributed shearing at the speed of 1900-2100 r/min, and dropwise adding the intermediate in the stirring process;
(6) keeping the temperature at 25-35 ℃, and simultaneously operating anchor type stirring at the speed of 35-45 r/min, distributed shearing at the speed of 1700-1900 r/min and distributed shearing at the speed of 1900-2100 r/min, and stirring for 25-35 min;
(7) and maintaining the temperature at 25-35 ℃, vacuumizing to 0.07-0.09 MPa, and performing anchor stirring at the speed of 35-45 r/min for 25-35 min to obtain the soldering paste.
10. The method for preparing solder paste as claimed in claim 8, wherein the step of stirring the flux paste and the lead-free metal alloy powder comprises:
(1) stirring at the speed of 15-25 r/min for 5-15 min at the temperature of 20-30 ℃;
(2) keeping the temperature at 20-30 ℃, and stirring for 15-25 min at the speed of 25-35 r/min;
(3) maintaining the temperature at 20-30 ℃, vacuumizing to 0.07-0.09 MPa, and stirring at the speed of 25-35 r/min for 15-25 min.
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Denomination of invention: Solder paste and its preparation method Effective date of registration: 20221208 Granted publication date: 20210720 Pledgee: Fujian Zhangzhou Rural Commercial Bank Co.,Ltd. Pledgor: Zhangzhou Jialian Chemical Co.,Ltd. Registration number: Y2022350000178 |