CN114453795B - Halogen-free soldering flux for lead-free solder paste - Google Patents
Halogen-free soldering flux for lead-free solder paste Download PDFInfo
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- CN114453795B CN114453795B CN202111509132.3A CN202111509132A CN114453795B CN 114453795 B CN114453795 B CN 114453795B CN 202111509132 A CN202111509132 A CN 202111509132A CN 114453795 B CN114453795 B CN 114453795B
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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
- B23K35/36—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
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- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Electric Connection Of Electric Components To Printed Circuits (AREA)
Abstract
The invention discloses a halogen-free soldering flux for lead-free solder paste, which comprises the following components in percentage by mass: 30-40% of solvent, 30-45% of resin, 5-10% of surfactant, 5-15% of activator, 3-10% of antioxidant and 2-8% of thixotropic agent. The halogen-free soldering flux produced by using petroleum resin has wide viscosity range, high surface insulation resistance and good high temperature resistance, the residual soldering flux on the welded substrate is firmly adhered, and the petroleum resin effectively shields active substances in the residues, so that the electrical property of electronic products is improved, and the lead-free soldering paste can be widely applied to the field of welding of electronic materials.
Description
Technical Field
The invention relates to a soldering flux for the technical field of electronic welding materials, in particular to a halogen-free soldering flux for lead-free soldering paste.
Background
With the development of integration, miniaturization and high performance of electronic information products, surface Mount Technology (SMT) has become a mainstream technology in the electronic assembly industry. The key process in SMT is the use of solder paste, the properties of which in large part determine the quality of the electronic product.
Soldering paste fluxes are usually composed of solvents, resins, surfactants, activators, antioxidants, thixotropic agents, the different components of which exert different effects, and the components are a whole which influences each other. In the soldering flux system, the soldering flux system has the key effects that the soldering flux system is composed of organic acid, organic amine, halogenate salt and surfactant, and plays a role in playing a role in activating at a certain soldering temperature, reacting with lead-free tin alloy powder and metal oxide on the surface of a bonding pad to remove an oxide film, and finally forming a good welding spot to realize mechanical and electrical interconnection between components and circuits. The active substances in the traditional soldering flux are generally active agents such as halogenates of organic amines, for example diethylamine hydrochloride, dibromoethylamine hydrobromide, L-glutamic acid hydrochloride, triethylamine hydrobromide, cetyltrimethylammonium chloride, hydrobromic acid cyclohexylamine salt and the like. The material has very high activity, and the prepared soldering flux has high tin-plating speed and good soldering effect; however, the substances have a large amount of halogen residues after welding, so that great potential safety hazards are brought to the use reliability of products, particularly under the conditions of high temperature and high humidity, the substances are easy to ionize halogen ions under the interaction of a thermal field and an electric field, corrode a circuit board and welding spots, cause short circuits among pins of electronic components, cause failure of the components, reduce surface insulation resistance and lead the reliability of the electronic products to face great examination.
The organic acid serving as an activator component is applied to the preparation of halogen-free soldering flux by virtue of the advantages of low corrosiveness, high reliability and the like, however, the use of the organic acid ensures that the acidic component in residues after soldering is easy to corrode a circuit board in a wet environment, reduces the reliability of electronic products, improves the activity of the halogen-free soldering flux, ensures that better electrical performance is achieved after soldering of the halogen-free soldering flux, and is a key technical problem in developing the halogen-free soldering flux for lead-free solder paste.
Disclosure of Invention
Aiming at the problems in the background technology, the invention provides the halogen-free soldering flux for the lead-free soldering paste, which has wider viscosity range and no halogen, ensures that the lead-free soldering paste has good high temperature resistance and higher surface insulation resistance in the use process, ensures that the active substances in the residual soldering flux are firmly shielded in resin by petroleum resin after the circuit board is welded, effectively improves the electrical performance of the circuit board, and can be widely applied to the field of electronic material welding.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
a halogen-free soldering flux for lead-free solder paste comprises a solvent, a resin, a surfactant, an activator, an antioxidant and a thixotropic agent, and is characterized in that: the mass percentages of the components are as follows: 30-40% of solvent, 30-45% of resin, 5-10% of surfactant, 5-15% of activator, 3-10% of antioxidant and 2-8% of thixotropic agent, wherein the solvent consists of one or two of isodecanol and isophorone; the resin is one or two of C5-C9 copolymerized petroleum resin and C9 hydrogenated petroleum resin; the surfactant is one or two of a hydroxyl acrylic acid copolymer and isomeric dodecanol; the activating agent is one or more than two of butanedioic acid amine salt, 1-ethyl-3-methylimidazole acetate and formic acid amine; the antioxidant is one or two of N, N '-1, 6-hexamethylene-bis- [3, 5-di-tert-butyl-4-hydroxy-phenyl-propionamide ] and 4,4' -thiobis (6-tert-butyl-3-methylphenol); the thixotropic agent is oxidized polyethylene wax.
Further, the oxidized polyethylene wax is selected from Crayvallac60P manufactured by ARKEMA, france.
A halogen-free soldering flux for lead-free solder paste is prepared by the following method:
1. accurately weighing a certain amount of solvent, resin and surfactant, adding into a reaction vessel, heating to 120-150 ℃, and stirring until the solvent, resin and surfactant are completely dissolved to obtain a mixture 1;
2. cooling the mixture 1 to 90-100 ℃, then adding a certain amount of activating agent and antioxidant, and stirring until the mixture is completely dissolved to obtain a mixture 2;
3. and (3) cooling the mixture 2 to 50-70 ℃, adding a certain amount of thixotropic agent, stirring until the thixotropic agent is completely dissolved, and cooling to room temperature to obtain the halogen-free soldering flux for the lead-free soldering paste.
Compared with the prior art, the invention has the beneficial technical effects that:
1. in the aspect of raw material components of the soldering paste, the solvent is composed of one or two of isodecyl alcohol and isophorone for the first time; the resin adopts one or two of C5-C9 copolymerized petroleum resin and C9 hydrogenated petroleum resin for the first time; the surfactant is composed of one or two of a hydroxy acrylic acid copolymer and isomeric dodecanol for the first time; the activating agent is composed of one or more than two of butanedioic acid amine salt, 1-ethyl-3-methylimidazole acetate and formic acid amine for the first time; the antioxidant is composed of one or two of N, N '-1, 6-hexamethylene-bis- [3, 5-di-tert-butyl-4-hydroxy-phenyl-propionamide ] and 4,4' -thiobis (6-tert-butyl-3-methylphenol) for the first time; the thixotropic agent adopts oxidized polyethylene wax for the first time. The soldering flux produced by the invention has stable performances and can be prepared into solder paste by the composition requirement and the proportioning requirement.
2. The resin of the invention adopts petroleum resin, ensures that the solder paste has better adhesive force, can obtain solder paste with wider viscosity range by adjusting the proportion of the solvent and the resin, and meets the requirement of reflow soldering with small gaps.
3. According to the invention, after the welding of the solder paste of petroleum resin is finished, the adhesive force of resin residues to the bonding pad is enhanced, the hardness of the residues is high, the water resistance is enhanced, the active substances in the soldering flux are effectively shielded, and the corrosion of the active agents in the residues to electronic components and bonding pads is prevented. After the welding is finished, the welding is placed in an environment with the temperature of 80 ℃ and the humidity of 80% for 168 hours, and the residue is firm and does not change color. The surface insulation resistance is greater than 1X1014 ohms.
4. The solder paste prepared by the invention has good stability and strong high temperature resistance, and the viscosity of the solder paste is increased to 10-20PAS after the solder paste is placed in a 50-DEG C incubator for 120 hours.
Detailed Description
The soldering paste prepared by using the lead-free tin powder and the halogen-free soldering flux for the lead-free soldering paste according to the technical scheme of the invention is prepared by using 85-90wt.% of lead-free tin powder and 10-15wt.% of soldering flux, preferably 88.8wt.% of soldering powder and 11.2wt.% of soldering flux, wherein the composition of the soldering powder is 95.3-99.3wt.% of tin, 0.3-4.0wt.% of silver and 0.3-0.7wt.% of copper, and the lead-free soldering paste prepared by using the halogen-free soldering flux according to the technical scheme of the invention is used for a comparison test with the lead-free soldering paste sold on the market, and the invention is further described in detail by combining specific examples and comparative examples. Specific examples are as follows:
example 1
The halogen-free soldering flux for the lead-free soldering paste comprises the following components in percentage by mass: 20% of isodecyl alcohol, 15% of isophorone, 10% of C5-C9 copolymerized petroleum resin, 30% of C9 hydrogenated petroleum resin, 5% of hydroxyacrylic acid copolymer, 5% of succinic acid amine salt, 2% of 1-ethyl-3-methylimidazole acetate, 3% of N, N '-1, 6-hexamethylene-bis- [3, 5-di-tert-butyl-4-hydroxyphenylpropionamide ], 2% of 4,4' -thiobis (6-tert-butyl-3-methylphenol) and 8% of oxidized polyethylene wax.
Example 2
The halogen-free soldering flux for the lead-free soldering paste comprises the following components in percentage by mass: 10% of isodecyl alcohol, 20% of isophorone, 30% of C5-C9 copolymerized petroleum resin, 15% of C9 hydrogenated petroleum resin, 6% of isomeric dodecanol, 1% of 1-ethyl-3-methylimidazole acetate, 6% of amine formate, 4% of N, N '-1, 6-hexamethylene-bis- [3, 5-di-tert-butyl-4-hydroxyphenylpropionamide ], 2% of 4,4' -thiobis (6-tert-butyl-3-methylphenol) and 6% of oxidized polyethylene wax
Example 3
The halogen-free soldering flux for the lead-free soldering paste comprises the following components in percentage by mass: 25% of isodecyl alcohol, 10% of isophorone, 30% of C5-C9 copolymerized petroleum resin, 10% of C9 hydrogenated petroleum resin, 2% of hydroxyacrylic acid copolymer, 5% of isomeric dodecanol, 7% of succinic acid amine salt, 4% of formic acid amine, 2% of N, N '-1, 6-hexamethylene-bis- [3, 5-di-tert-butyl-4-hydroxy-phenyl-propionamide ], 1% of 4,4' -thiobis (6-tert-butyl-3-methylphenol) and 4% of oxidized polyethylene wax.
Example 4
The halogen-free soldering flux for the lead-free soldering paste comprises the following components in percentage by mass: 10% of isodecyl alcohol, 25% of isophorone, 30% of C5-C9 copolymerized petroleum resin, 5% of C9 hydrogenated petroleum resin, 5% of hydroxyacrylic acid copolymer, 3% of isomeric dodecanol, 2% of succinic acid amine salt, 2% of 1-ethyl-3-methylimidazole acetate, 9% of formic acid amine, 1% of N, N '-1, 6-hexamethylene-bis- [3, 5-di-tert-butyl-4-hydroxy-phenyl-propionamide ], 3% of 4,4' -thiobis (6-tert-butyl-3-methylphenol) and 5% of oxidized polyethylene wax.
The results of the performance comparison test of the performance of the halogen-free soldering flux for preparing the lead-free soldering paste and the performance of the commercial lead-free soldering paste are shown in table 1.
Table 1 results of comparison of the indexes related to the examples and comparative examples
As can be seen from the experimental data of the above examples 1-4 and comparative examples 1-2, the lead-free halogen-free solder paste prepared according to the present invention has no halogen, good stability, and a viscosity increase of 10-20PAS after being placed in a 50 ℃ incubator for 120 hours, and a post-soldering surface insulation resistance of 1X10 14 Ohmic, the post-weld residue was firmly transparent. The residue remained firm after being left for 168 hours in an environment with a temperature of 80 ℃ and a humidity of 80%Is solid and transparent and does not turn white. The electronic performance of the circuit board after welding is ensured, and the method can be widely applied to the field of electronic material welding.
Claims (3)
1. A halogen-free soldering flux for lead-free solder paste comprises a solvent, a resin, a surfactant, an activator, an antioxidant and a thixotropic agent, and is characterized in that: the mass percentages of the components are as follows: 30-40% of solvent, 30-45% of resin, 5-10% of surfactant, 5-15% of activator, 3-10% of antioxidant and 2-8% of thixotropic agent, wherein the solvent consists of one or two of isodecanol and isophorone; the resin is one or two of C5-C9 copolymerized petroleum resin and C9 hydrogenated petroleum resin; the surfactant is one or two of a hydroxyl acrylic acid copolymer and isomeric dodecanol; the activating agent is one or more than two of butanedioic acid amine salt, 1-ethyl-3-methylimidazole acetate and formic acid amine; the antioxidant is one or two of N, N '-1, 6-hexamethylene-bis- [3, 5-di-tert-butyl-4-hydroxy-phenyl-propionamide ] and 4,4' -thiobis (6-tert-butyl-3-methylphenol); the thixotropic agent is oxidized polyethylene wax.
2. A halogen-free soldering flux for lead-free solder paste as claimed in claim 1, wherein: the oxidized polyethylene wax is Crayvallac60P manufactured by ARKEMA of France.
3. A halogen-free soldering flux for lead-free solder paste as claimed in claim 1, wherein: the preparation method comprises the following steps:
(1) Accurately weighing a certain amount of solvent, resin and surfactant, adding into a reaction vessel, heating to 120-150 ℃, and stirring until the solvent, resin and surfactant are completely dissolved to obtain a mixture 1;
(2) Cooling the mixture 1 to 90-100 ℃, then adding a certain amount of activating agent and antioxidant, and stirring until the mixture is completely dissolved to obtain a mixture 2;
(3) And (3) cooling the mixture 2 to 50-70 ℃, adding a certain amount of thixotropic agent, stirring until the thixotropic agent is completely dissolved, and cooling to room temperature to obtain the halogen-free soldering flux for the lead-free soldering paste.
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| CN202111509132.3A CN114453795B (en) | 2021-12-10 | 2021-12-10 | Halogen-free soldering flux for lead-free solder paste |
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| CN202111509132.3A CN114453795B (en) | 2021-12-10 | 2021-12-10 | Halogen-free soldering flux for lead-free solder paste |
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