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CN114799618A - Zero-halogen low-voidage water-soluble flux paste and preparation method thereof - Google Patents

Zero-halogen low-voidage water-soluble flux paste and preparation method thereof Download PDF

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Publication number
CN114799618A
CN114799618A CN202210538176.7A CN202210538176A CN114799618A CN 114799618 A CN114799618 A CN 114799618A CN 202210538176 A CN202210538176 A CN 202210538176A CN 114799618 A CN114799618 A CN 114799618A
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water
soluble
voidage
zero
flux paste
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CN114799618B (en
Inventor
柳丽敏
武信
何欢
秦俊虎
王艳南
熊晓娇
钱斌
何禹浩
沈海斌
何江华
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Yunnan Tin Material Co ltd
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Yunnan Tin Material Co ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B23MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23KSOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K35/00Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
    • B23K35/22Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by the composition or nature of the material
    • B23K35/36Selection of non-metallic compositions, e.g. coatings, fluxes; Selection of soldering or welding materials, conjoint with selection of non-metallic compositions, both selections being of interest
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B23MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23KSOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K35/00Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
    • B23K35/22Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by the composition or nature of the material
    • B23K35/36Selection of non-metallic compositions, e.g. coatings, fluxes; Selection of soldering or welding materials, conjoint with selection of non-metallic compositions, both selections being of interest
    • B23K35/3612Selection 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
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B23MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23KSOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K35/00Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
    • B23K35/22Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by the composition or nature of the material
    • B23K35/36Selection of non-metallic compositions, e.g. coatings, fluxes; Selection of soldering or welding materials, conjoint with selection of non-metallic compositions, both selections being of interest
    • B23K35/3612Selection 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
    • B23K35/3613Polymers, e.g. resins
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B23MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23KSOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K35/00Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
    • B23K35/22Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by the composition or nature of the material
    • B23K35/36Selection of non-metallic compositions, e.g. coatings, fluxes; Selection of soldering or welding materials, conjoint with selection of non-metallic compositions, both selections being of interest
    • B23K35/362Selection of compositions of fluxes
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B23MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23KSOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K35/00Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
    • B23K35/40Making wire or rods for soldering or welding

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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 zero-halogen low-voidage water-soluble flux paste and a preparation method thereof, wherein the flux paste comprises the following components in percentage by mass: 18-35% of water-soluble resin, 0.5-3% of antioxidant 1010, 3-8% of amide substances, 10-20% of organic acid and 40-60% of alcohol ether substances. The soldering paste prepared by the soldering paste flux and the soldering powder has the advantages of good stability, good welding performance, no halogen, small welding voidage, cleaning of residues after welding by water, no corrosion after cleaning, no environmental pollution and the like.

Description

Zero-halogen low-voidage water-soluble flux paste and preparation method thereof
Technical Field
The invention relates to the technical field of soldering paste and a preparation method thereof, in particular to water-soluble soldering paste and a preparation method thereof.
Background
With the rapid development of the mechanical industry and the electronic industry and the increasingly fierce market competition, each enterprise pays more and more attention to the quality of products. On one hand, the solderability of various metal materials and electronic element leads and the cleaning problem after welding are common technical quality problems in enterprise production. Most flux paste used by the early-stage produced solder paste is rosin-type flux paste, and the flux has the problems of high viscosity, unsatisfactory flux-assisting effect, excessive PCB surface residue, difficulty in cleaning, unsatisfactory electrical performance and the like, and the product quality is seriously influenced. The residue, in addition to affecting the appearance of the PCB, may cause problems such as an increase in contact resistance, a decrease in insulation performance, and corrosion of the PCB. In addition, the cleaning agent of chlorofluorocarbon (CFC) is adopted for cleaning, and the CFC is not beneficial to environmental protection and is forbidden in many countries. The water-soluble solder paste is produced by transportation in order to meet the market demand, the residual of the solder paste after soldering is easy to clean, the solder paste can be cleaned only by water or warm water, and the solder paste is not corroded after being cleaned, so that the environmental pollution is avoided. On the other hand, in a welding finished product, the void ratio is a strict control index, the occurrence of the void influences the mechanical performance of a welding spot, the void is broken along with the increase of the welding spot during long-time work, the void formed during welding can directly influence the interface heat conduction effect, the spot overheating is easy to generate, and the reliability of the welding spot is reduced. Most of the existing water-soluble flux-cored pastes are non-rosin type, have poor activity and are easy to generate larger holes, and although the flux activity can be greatly improved and the hole rate can be reduced by adding halogen, the halogen can severely corrode electronic components, thereby affecting the reliability and the service life of products. Therefore, there is a need to develop a zero-halogen low-void water-soluble flux paste to solve the above problems.
Disclosure of Invention
The invention aims to solve the problems of excessive residual, difficult cleaning and large cavity of the existing solder paste after welding, and provides a zero-halogen low-voidage water-soluble soldering paste with low voidage, easy residual cleaning and low voidage.
The purpose of the invention is realized by the following technical scheme:
a zero-halogen low-voidage water-soluble flux paste comprises the following components by mass percent: 18-35% of water-soluble resin, 0.5-3% of antioxidant 1010, 3-8% of amide substances, 10-20% of organic acid and 40-60% of alcohol ether substances.
Further, the water-soluble resin is a water-soluble high molecular polymer.
Furthermore, the water-soluble high molecular polymer is one or two of polyvinylpyrrolidone, polyvinyl alcohol, polyethylene glycol, polyacrylamide, polyacrylic acid, polymethacrylic acid, polymaleic anhydride and polyquaternary ammonium salt.
Further, the amide substance is formed by mixing ethylene bis (12-hydroxy) stearic acid amide H and Bisamide LA according to the mass ratio of 1-2: 2-5.
Further, the organic acid is formed by mixing ricinoleic acid, palmitic acid and glycolic acid.
Further, the alcohol ether substance is formed by mixing a high-boiling point substance 2-benzyloxy ethanol and a low-boiling point substance diethylene glycol benzyl ether according to the mass ratio of 1-2: 2-3.
The preparation method of the zero-halogen low-voidage water-soluble flux paste comprises the following steps:
adding water-soluble resin, amide substances and alcohol ether substances into a container, heating to 160-180 ℃, stirring until the water-soluble resin, the amide substances and the alcohol ether substances are completely dissolved, stopping heating, adding an antioxidant 1010, dissolving, adding an organic acid, stirring until the organic acid is completely dissolved, pouring into the container, sealing, naturally cooling and solidifying to obtain the water-soluble flux-cored paste.
Compared with the prior art, the flux paste has at least the following advantages:
(1) the residues of the water-soluble tin paste after welding are easy to clean, and can be cleaned by water or warm water. The cleaning agent does not generate corrosion after cleaning, does not cause environmental pollution, reduces the production cost of customers, and meets the requirement of environmental protection;
(2) the flux paste does not contain halogen, and has good stability and wetting property;
(3) the solvent is prepared by compounding a high-boiling-point organic solvent and a low-boiling-point organic solvent, has good solubility, and can effectively reduce the voidage which is less than 12%.
The water-soluble flux paste prepared by the invention and the welding powder are prepared into the solder paste, and the solder paste has the advantages of good stability, good welding performance, no halogen, small welding voidage, water cleaning of residues after welding and the like.
Detailed Description
The present invention will be further illustrated with reference to the following examples.
Example 1
The zero-halogen low-voidage water-soluble flux paste comprises the following components in percentage by mass:
Figure BDA0003647258420000021
the method for preparing the water-soluble flux paste comprises the following steps: adding polymaleic anhydride, diethylene glycol benzyl ether, 2-benzyloxy ethanol, ethylene bis (12-hydroxy) stearic acid amide H and Bisamide LA into a container, heating to 180 ℃, stirring until the mixture is completely dissolved, stopping heating, adding an antioxidant 1010, keeping the temperature at about 150 ℃, adding organic acids of ricinoleic acid, palmitic acid and glycolic acid after the mixture is dissolved, stirring until the mixture is completely dissolved, pouring the mixture into the container, sealing, cooling and solidifying to obtain the water-soluble soldering paste, and preparing the water-soluble soldering paste and SnAg3.Cu0.5 soldering tin powder into the tin paste according to the mass ratio of 11.5: 88.5.
Example 2
The zero-halogen low-voidage water-soluble flux paste comprises the following components in percentage by mass:
Figure BDA0003647258420000031
the method for preparing the water-soluble flux paste comprises the following steps: adding polyquaternium, diethylene glycol benzyl ether, 2-benzyloxy ethanol, ethylene bis (12-hydroxy) stearic acid amide H and Bisamide LA into a container, heating to 160 ℃, stirring until the mixture is completely dissolved, stopping heating, adding an antioxidant 1010, keeping the temperature at about 150 ℃, adding organic acids ricinoleic acid, palmitic acid and glycolic acid after the mixture is dissolved, stirring until the mixture is completely dissolved, pouring the mixture into the container, sealing, cooling and solidifying to obtain the water-soluble soldering paste. And preparing the water-soluble flux paste and SnAg3.0Cu0.5 solder powder into solder paste according to the mass ratio of 11.5: 88.5.
Example 3
The zero-halogen low-voidage water-soluble flux paste comprises the following components in percentage by mass:
Figure BDA0003647258420000032
the method for preparing the water-soluble flux paste comprises the following steps: adding polyvinylpyrrolidone, diethylene glycol benzyl ether, 2-benzyloxy ethanol, ethylene bis (12-hydroxy) stearic acid amide H and Bisamide LA into a container, heating to 170 ℃, stirring until the mixture is completely dissolved, stopping heating, adding an antioxidant 1010, keeping the temperature at about 150 ℃, adding organic acids of ricinoleic acid, palmitic acid and glycolic acid after the mixture is dissolved, stirring until the mixture is completely dissolved, pouring the mixture into the container, sealing, cooling and solidifying to obtain the water-soluble soldering paste, and preparing the water-soluble soldering paste and SnAg3.0Cu0.5 soldering tin powder into tin paste according to the mass ratio of 11.5: 88.5.
Example 4
The zero-halogen low-voidage water-soluble flux paste comprises the following components in percentage by mass:
Figure BDA0003647258420000041
the method for preparing the flux paste comprises the following steps: adding polyacrylamide, diethylene glycol benzyl ether, 2-benzyloxy ethanol, ethylene bis (12-hydroxy) stearamide H and Bisamide LA into a container, heating to 180 ℃, stirring until the materials are completely dissolved, stopping heating, adding an antioxidant 1010, keeping the temperature at about 150 ℃, adding organic acids of ricinoleic acid, palmitic acid and glycolic acid after the materials are dissolved, stirring until the materials are completely dissolved, pouring the materials into the container, sealing, cooling and solidifying to obtain the water-soluble soldering paste, and preparing the water-soluble soldering paste and SnAg3.0Cu0.5 soldering tin powder into the soldering paste according to the mass ratio of 11.5: 88.5.
Example 5
The zero-halogen low-voidage water-soluble flux paste comprises the following components in percentage by mass:
Figure BDA0003647258420000042
the method for preparing the flux paste comprises the following steps: adding polyacrylic acid, polyvinyl alcohol, diethylene glycol benzyl ether, 2-benzyloxy-ethanol, ethylene bis (12-hydroxy) stearic acid amide H and Bisamide LA into a container, heating to 170 ℃, stirring until the mixture is completely dissolved, stopping heating, adding an antioxidant 1010, keeping the temperature at about 150 ℃, adding organic acids ricinoleic acid, palmitic acid and glycolic acid after the mixture is dissolved, stirring until the mixture is completely dissolved, pouring the mixture into the container, sealing, cooling and solidifying to obtain the water-soluble soldering paste, and preparing the water-soluble soldering paste and SnAg3.0Cu0.5 soldering tin powder into tin paste according to the mass ratio of 11.5: 88.5.
Example 6
The zero-halogen low-voidage water-soluble flux paste comprises the following components in percentage by mass:
Figure BDA0003647258420000051
the method for preparing the flux paste comprises the following steps: adding polymethacrylic acid, diethylene glycol benzyl ether, 2-benzyloxy ethanol, ethylene bis (12-hydroxy) stearamide H and Bisamide LA into a container, heating to 170 ℃, stirring until the materials are completely dissolved, stopping heating, adding an antioxidant 1010, keeping the temperature at about 150 ℃, adding organic acids of ricinoleic acid, palmitic acid and glycolic acid after the materials are dissolved, stirring until the materials are completely dissolved, pouring the materials into the container, sealing, cooling and solidifying to obtain the water-soluble soldering paste, and preparing the water-soluble soldering paste and SnAg3.0Cu0.5 soldering tin powder into the soldering paste according to the mass ratio of 11.5: 88.5.
A commercially available water-soluble SnAg3.0Cu0.5 tin paste A and a commercially available water-soluble SnAg3.0Cu0.5 tin paste B were taken to perform comparative tests with the tin pastes in the above examples: after SMT automatic solder paste printing, surface mounting and reflow soldering, detecting the solderability of soldering points, counting the yield and testing the void ratio; the spreading ratio test was carried out in accordance with JIS Z3197. The test results are given in the following table:
comparison table for testing performance of solder paste
Figure BDA0003647258420000052
The spreading rate is an important index for measuring the wettability of the solder paste to the bonding pad, and the larger the spreading rate is, the better the wettability is. As can be seen from the above table, compared with the existing commercially available solder paste A and solder paste B, the solder paste of the invention has the advantages of significantly reduced voidage, relatively large reflow soldering yield and expansion rate, and no halogen in the solder paste, which indicates that the solder paste of the invention has good wettability, and is a zero-halogen, energy-saving, environment-friendly and low-voidage solder paste.
The above examples are merely illustrative of the preferred embodiments of the present invention, and are not intended to limit the scope of the present invention, and various modifications and improvements made to the technical solutions of the present invention by those skilled in the art without departing from the technical scope of the present invention should fall within the protection scope defined by the claims of the present invention.

Claims (7)

1. The zero-halogen low-voidage water-soluble flux paste is characterized in that the flux paste comprises the following components in percentage by mass: 18-35% of water-soluble resin, 0.5-3% of antioxidant 1010, 3-8% of amide substances, 10-20% of organic acid and 40-60% of alcohol ether substances.
2. The zero-halogen low-voidage water-soluble flux paste according to claim 1, wherein the water-soluble resin is a water-soluble high molecular polymer.
3. The zero-halogen low-voidage water-soluble flux paste according to claim 2, wherein the water-soluble high molecular polymer is one or two of polyvinylpyrrolidone, polyvinyl alcohol, polyethylene glycol, polyacrylamide, polyacrylic acid, polymethacrylic acid, polymaleic anhydride and polyquaternium.
4. The zero-halogen low-voidage water-soluble flux paste according to claim 1, wherein the amide substance is a mixture of ethylene bis (12-hydroxy) stearic acid amide H and Bisamide LA in a mass ratio of 1-2: 2-5.
5. The zero-halogen low-voidage water-soluble flux paste as claimed in claim 1, wherein the organic acid is a mixture of ricinoleic acid, palmitic acid and glycolic acid.
6. The zero-halogen low-voidage water-soluble flux paste according to claim 1, wherein the alcohol ether substance is a mixture of a high boiling point substance 2-benzyloxy ethanol and a low boiling point substance diethylene glycol benzyl ether in a mass ratio of 1-2: 2-3.
7. The method for preparing the zero-halogen low-voidage water-soluble flux paste according to any one of claims 1 to 6, wherein the method comprises the following steps: adding water-soluble resin, amide substances and alcohol ether substances into a container, heating to 160-180 ℃, stirring until the water-soluble resin, the amide substances and the alcohol ether substances are completely dissolved, stopping heating, adding an antioxidant 1010, dissolving, adding an organic acid, stirring until the organic acid is completely dissolved, pouring into the container, sealing, naturally cooling and solidifying to obtain the soldering paste.
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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116727922A (en) * 2022-11-11 2023-09-12 苏州优诺电子材料科技有限公司 Special tin paste with self-corrosion inhibition effect for OPS (optical surface bonding) pad and application of special tin paste
CN116833622A (en) * 2023-08-08 2023-10-03 云南锡业新材料有限公司 Needle cylinder flux paste with good spot coating stability and preparation method thereof
CN118789159A (en) * 2024-08-12 2024-10-18 深圳市华远金属有限公司 Anti-splash laser solder paste and preparation method thereof
CN119501370A (en) * 2025-01-07 2025-02-25 云南锡业新材料有限公司 A zero-halogen low-void SnBi soldering paste and preparation method thereof
CN119501370B (en) * 2025-01-07 2025-12-26 云南锡业新材料有限公司 A zero-halogen, low-void SnBi-based solder paste and its preparation method

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101347875A (en) * 2008-08-19 2009-01-21 深圳悍豹科技有限公司 Middle-temperature energy-saving leadless solder paste special for tuners
US20210031311A1 (en) * 2018-02-28 2021-02-04 Senju Metal Industry Co., Ltd. Flux and solder paste
WO2021166972A1 (en) * 2020-02-18 2021-08-26 千住金属工業株式会社 Flux and solder paste

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101347875A (en) * 2008-08-19 2009-01-21 深圳悍豹科技有限公司 Middle-temperature energy-saving leadless solder paste special for tuners
US20210031311A1 (en) * 2018-02-28 2021-02-04 Senju Metal Industry Co., Ltd. Flux and solder paste
WO2021166972A1 (en) * 2020-02-18 2021-08-26 千住金属工業株式会社 Flux and solder paste

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116727922A (en) * 2022-11-11 2023-09-12 苏州优诺电子材料科技有限公司 Special tin paste with self-corrosion inhibition effect for OPS (optical surface bonding) pad and application of special tin paste
CN116833622A (en) * 2023-08-08 2023-10-03 云南锡业新材料有限公司 Needle cylinder flux paste with good spot coating stability and preparation method thereof
CN118789159A (en) * 2024-08-12 2024-10-18 深圳市华远金属有限公司 Anti-splash laser solder paste and preparation method thereof
CN119501370A (en) * 2025-01-07 2025-02-25 云南锡业新材料有限公司 A zero-halogen low-void SnBi soldering paste and preparation method thereof
CN119501370B (en) * 2025-01-07 2025-12-26 云南锡业新材料有限公司 A zero-halogen, low-void SnBi-based solder paste and its preparation method

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