CN114453795A - Halogen-free soldering flux for lead-free soldering paste - Google Patents
Halogen-free soldering flux for lead-free soldering paste Download PDFInfo
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- CN114453795A CN114453795A CN202111509132.3A CN202111509132A CN114453795A CN 114453795 A CN114453795 A CN 114453795A CN 202111509132 A CN202111509132 A CN 202111509132A CN 114453795 A CN114453795 A CN 114453795A
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- free
- lead
- halogen
- resin
- solder paste
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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
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 lead-free soldering paste has the advantages that the halogen-free soldering flux produced by using the petroleum resin has wide viscosity range, high surface insulation resistance and good high temperature resistance, the residual soldering flux on the substrate is firmly adhered after welding, the petroleum resin effectively shields active substances in the residual, the electrical performance of electronic products is improved, and the lead-free soldering paste can be widely applied to the field of electronic material welding.
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 electronic information products toward integration, miniaturization and high performance, Surface Mount Technology (SMT) has become the mainstream technology in the electronic assembly industry. The key process in the SMT process is the use of solder paste, and the performance of the solder paste determines the quality of electronic products in a large range.
Soldering flux for solder paste usually consists of solvent, resin, surfactant, activator, antioxidant and thixotropic agent, and its different components play different roles and are an integral body which can be mutually influenced. In a soldering flux system, the soldering flux is composed of organic acid, organic amine, halide and surfactant, and plays a role in playing activity 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 soldering spot to realize mechanical and electrical interconnection between components and circuits. The active substance in the conventional soldering flux is generally an active agent such as halide of organic amine, for example, diethylamine hydrochloride, di-bromoethylamine hydrobromide, L-glutamic acid hydrochloride, triethylamine hydrobromide, hexadecyltrimethylammonium chloride, cyclohexylamine hydrobromide, etc. The substances have very high activity, and the prepared soldering flux has high tin coating speed and good soldering effect; however, the substances have a large amount of halogen residues after welding, which brings great potential safety hazards to the use reliability of products, and 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 circuit between pins of electronic components, cause component failure, reduce surface insulation resistance, and make the reliability of electronic products face huge tests.
The organic acid used as the activating agent component is applied to the preparation of the halogen-free soldering flux by virtue of the advantages of low corrosivity, high reliability and the like, but the use of the organic acid enables the acidic component in the residues after welding to easily corrode a circuit board in a humid environment, reduces the reliability of electronic products, improves the activity of the halogen-free soldering flux, enables the halogen-free soldering flux to achieve better electrical performance after welding, and is a key technical problem for the development of the halogen-free soldering flux for the lead-free tin paste.
Disclosure of Invention
The invention provides a halogen-free soldering flux for lead-free solder paste, which has a wider viscosity range and is halogen-free, ensures that the lead-free solder paste has good high temperature resistance and higher surface insulation resistance in the use process, and effectively improves the electrical performance of a circuit board after the circuit board is welded, and can be widely applied to the field of electronic material welding.
In order to achieve the purpose, the invention adopts the following technical scheme:
a halogen-free soldering flux for lead-free solder paste comprises a solvent, resin, a surfactant, an activator, an antioxidant and a thixotropic agent, and is characterized in that: the mass percentages of the components are respectively 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 is one or two of isodecyl alcohol and isophorone; the resin is composed of one or two of C5-C9 copolymerized petroleum resin and C9 hydrogenated petroleum resin; the surfactant is composed of one or two of a hydroxy acrylic acid copolymer and isomeric dodecanol; the activating agent is one or more than two of ammonium succinate salt, 1-ethyl-3-methylimidazole acetate and ammonium formate; the antioxidant is one or two of N, N '-1, 6-hexamethylene-bis- [3, 5-di-tert-butyl-4-hydroxy hydrocinnamamide ] and 4,4' -thiobis (6-tert-butyl-3-methylphenol); the thixotropic agent is oxidized polyethylene wax.
Further, the oxidized polyethylene wax is 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, the resin and the surfactant are completely dissolved to obtain a mixture 1;
2. cooling the mixture 1 to 90-100 ℃, adding a certain amount of activating agent and antioxidant, and stirring until the activating agent and the antioxidant are completely dissolved to obtain a mixture 2;
3. and 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 solder 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, a solvent is composed of one or two of isodecyl alcohol and isophorone for the first time; the resin is composed of 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 activator is composed of one or more than two of ammonium succinate salt, 1-ethyl-3-methylimidazole acetate and ammonium formate 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 hydrocinnamamide ] and 4,4' -thiobis (6-tert-butyl-3-methylphenol) for the first time; the thixotropic agent adopts oxidized polyethylene wax for the first time. By the composition requirement and the proportioning requirement of the invention, the produced soldering flux has stable performances and can be used for preparing soldering paste.
2. The resin of the invention adopts petroleum resin, which ensures that the solder paste has better adhesive force, and the solder paste with wider viscosity range can be obtained by adjusting the proportion of the solvent and the resin, thereby meeting the requirements of reflow soldering with fine and small gaps.
3. The invention selects the petroleum resin solder paste to weld and then enhances the adhesive force of the resin residue to the bonding pad, the residue has high hardness and enhanced water resistance, effectively shields the active substances in the soldering flux, and prevents the active substances in the residue from corroding electronic components and the bonding pad. After the welding is finished, the welding material is placed in an environment with the temperature of 80 ℃ and the humidity of 80% for 168 hours, and residues are firm and do 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 rises to 10-20PAS after the solder paste is placed in a thermostat at 50 ℃ for 120 hours.
Detailed Description
The solder paste prepared by using the lead-free solder powder and the halogen-free soldering flux for the lead-free solder paste according to the technical scheme of the invention is composed of 85-90 wt.% of the lead-free solder powder and 10-15 wt.% of the soldering flux, preferably 88.8 wt.% of the solder powder and 11.2 wt.% of the soldering flux, wherein the components of the solder powder are 95.3-99.3 wt.% of tin, 0.3-4.0 wt.% of silver and 0.3-0.7 wt.% of copper. The specific embodiment is as follows:
example 1
A halogen-free soldering flux for lead-free solder 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-methylimidazolium acetate, 3% of N, N '-1, 6-hexamethylene-bis- [3, 5-di-tert-butyl-4-hydroxy-phenylacrylamide ], 2% of 4,4' -thiobis (6-tert-butyl-3-methylphenol) and 8% of oxidized polyethylene wax.
Example 2
A halogen-free soldering flux for lead-free solder 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 isododecyl alcohol, 1-ethyl-3-methylimidazole acetate, 1%, 6% of amine formate, 4% of N, N '-1, 6-hexamethylene-bis- [3, 5-di-tert-butyl-4-hydroxy-phenylacrylamide ], 2% of 4,4' -thiobis (6-tert-butyl-3-methylphenol) and 6% of oxidized polyethylene wax
Example 3
A halogen-free soldering flux for lead-free solder 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 isododecyl alcohol, 7% of succinic acid amine salt, 4% of ammonium formate, 2% of N, N '-1, 6-hexamethylene-bis- [3, 5-di-tert-butyl-4-hydroxy-phenylacrylamide ], 1% of 4,4' -thiobis (6-tert-butyl-3-methylphenol) and 4% of oxidized polyethylene wax.
Example 4
A halogen-free soldering flux for lead-free solder 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 isododecyl alcohol, 2% of butanedioic acid amine salt, 2% of 1-ethyl-3-methylimidazolium acetate, 9% of ammonium formate, 1% of N, N '-1, 6-hexamethylene-bis- [3, 5-di-tert-butyl-4-hydroxybenzamide ], 3% of 4,4' -thiobis (6-tert-butyl-3-methylphenol) and 5% of oxidized polyethylene wax.
The performance comparison test results of the solder paste prepared by the halogen-free soldering flux for the lead-free solder paste and the commercially available lead-free solder paste are shown in table 1.
Table 1 comparative results of indexes related to 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 and good stability, the viscosity of the solder paste increases by 10-20PAS after being placed in a 50 ℃ thermostat for 120 hours, and the insulation resistance of the soldered surface is 1x1014Ohmic, the postweld residue was firm and transparent. The residue remained firm, transparent and non-whitish after 168 hours of standing in an environment at 80 ℃ and 80% humidity. The electronic performance of the circuit board after welding is ensured, and the welding 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, resin, a surfactant, an activator, an antioxidant and a thixotropic agent, and is characterized in that: the mass percentages of the components are respectively 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 is one or two of isodecyl alcohol and isophorone; the resin is composed of one or two of C5-C9 copolymerized petroleum resin and C9 hydrogenated petroleum resin; the surfactant is composed of one or two of a hydroxy acrylic acid copolymer and isomeric dodecanol; the activating agent is one or more than two of ammonium succinate salt, 1-ethyl-3-methylimidazole acetate and ammonium formate; the antioxidant is one or two of N, N '-1, 6-hexamethylene-bis- [3, 5-di-tert-butyl-4-hydroxy hydrocinnamamide ] and 4,4' -thiobis (6-tert-butyl-3-methylphenol); the thixotropic agent is oxidized polyethylene wax.
2. The halogen-free flux for lead-free solder paste according to claim 1, wherein: the oxidized polyethylene wax is Crayvallac60P produced by ARKEMA France.
3. The halogen-free flux for lead-free solder paste according to 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, the resin and the surfactant are completely dissolved to obtain a mixture 1;
(2) cooling the mixture 1 to 90-100 ℃, adding a certain amount of activating agent and antioxidant, and stirring until the activating agent and the antioxidant are completely dissolved to obtain a mixture 2;
(3) and 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 solder paste.
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