CN105234591A - Halogen-free soldering tin wire activator and preparation method thereof - Google Patents

Halogen-free soldering tin wire activator and preparation method thereof Download PDF

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Publication number
CN105234591A
CN105234591A CN201510651313.8A CN201510651313A CN105234591A CN 105234591 A CN105234591 A CN 105234591A CN 201510651313 A CN201510651313 A CN 201510651313A CN 105234591 A CN105234591 A CN 105234591A
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China
Prior art keywords
halogen
acid
activating agent
activator
solder stick
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Application number
CN201510651313.8A
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Chinese (zh)
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CN105234591B (en
Inventor
孙福林
张宇航
韩振峰
朱火清
康宇
高瑞军
谢鹏
潘凯华
林元华
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Guangdong Institute of welding technology (Guangdong Institute of China and Ukraine)
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Guangzhou Research Institute of Non Ferrous Metals
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Classifications

    • 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
    • B23K35/40Making 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 halogen-free soldering tin wire activator. The halogen-free soldering tin wire activator is composed of the following components in percentage by mass: 0.5-6% of an organic acid activator, 0.1-2% of a surfactant, 0.5-5% of an organic solvent and 90-96% of modified rosin. The preparation method thereof comprises the following steps: heating the modified rosin to 130-150 DEG C until the modified rosin is completely melted and keeps a constant temperature, sequentially adding the organic acid activator, the surfactant and the organic solvent and stirring to achieve uniformity and transparency, and standing for 5 minutes at a constant temperature and keeping no layering. The halogen-free soldering tin wire activator disclosed by the invention is free from any halogen, low in fume, smell and splashing during welding, high in activity, high in wettability, and high in surface insulation resistance after welding; and welding spots are full and bright.

Description

A kind of Halogen solder stick activating agent and preparation method thereof
Technical field
The present invention relates to a kind of solder stick activating agent, particularly a kind of Halogen solder stick activating agent and preparation method thereof.
Background technology
Traditional activating agent is mostly containing halogen, and corrosivity is strong, although can reach good welding effect, postwelding remains corrosivity, there is potential harmful effect to the mechanical property of product and electric property.Due to the easy moisture absorption of halogen, the activating agent made moist easily produces splashing, fried tin in welding process, affect welding quality, and the cleaning agent for cleaning postwelding residue volatilize after can damage the ozone layer, affect environment, do not meet environmental requirement.
In recent years, specify according to International Typographic Association and industry and the formulation of " fluxes for soft soldering requirement " (J-STD-004B), use for halogen proposes new regulation, requirement chlorine, bromine content are less than 900ppm, halogen total amount is less than 1500ppm, therefore, activating agent is non-halogen has been inexorable trend.But in the Halogen tin silk product occurred in the market, most active is poor, the rate of spread is low, a lot of enterprise blindly strengthens the percentage composition of activating agent in order to reach preferably active, the problem such as cause again that flue dust in welding use procedure is large, large, the postwelding of splashing remains on the high side, reliability reduction.
CN101049662A " no-lead soft soldering silk halogen-free solder flux and preparation method " discloses the following material composition of mass percent: organic acid activator 0.2 ~ 3%, non-ionic surface active agent 0.2 ~ 3%, surplus is modified rosin, its surfactant select dibromo butene glycol, dibromo ethyl benzene, bromide sixteen alkyls pyridine to close in FSN100 one or more.This solder flux content of halogen is higher, and postwelding is residual easily causes corrosion, causes surface insulation resistance to decline, especially runs into wet environment, cause the generation of short circuit leaky.
CN101157168A " lead-free solder thread-use colophony type non-halide element no-clean scaling powder " discloses the following material composition of mass percent: organic acid 4 ~ 18%, organic solvent 0.5 ~ 5%, and modified rosin is surplus; This scaling powder is not halogen-containing, but organic acid activator use amount is obviously on the high side, the Macrogol 2000 that its paste making agent uses, Macrogol 4000, one or more in Macrogol 6000, be heated in welding process and thermal cracking can occur, therefore welding fume is larger, affect to environment, using in the incomplete situation of exhaust equipment also has certain damage to health.
Summary of the invention
The object of the invention is to the defect overcoming prior art, provide a kind of Halogen solder stick activating agent, this activating agent has the features such as activity is good, welding fume is little, it is little to splash, the residual few corrosivity of the full light of solder joint, postwelding is low.
Another object of the present invention is the preparation method providing a kind of described Halogen solder stick activating agent.
Halogen solder stick activating agent of the present invention is made up of following component and mass percent: organic acid activator 0.5 ~ 6%; Surfactant 0.1 ~ 2%; Organic solvent 0.5 ~ 5%; Modified rosin 90 ~ 96%.
Preferred Halogen solder stick activating agent is made up of following component and mass percent: adipic acid: 1%; Suberic acid: 1%; FSN-100:0.3%; TX-10:0.7%; 200 ﹟ solvent naphthas: 0.5%; Turpentine oil: 0.5%; Foral 101:50%; Perhydrogenated rosin: 40% and 150 high-softening-point rosins: 6%.
Described organic acid activator is one or more in succinic acid, adipic acid, decanedioic acid, suberic acid or dimethylolpropionic acid.
Described surfactant is one or both in TX-10, OP-10, FC-4430 or FSN-100.
Described organic solvent is one or both in 120 ﹟ solvent naphthas, 200 ﹟ solvent naphthas, turpentine oil or mixed dibasic acid ester (DBE).
Described modified rosin is one or both in Foral 101, Foral 301, perhydrogenated rosin or 150 high-softening-point rosins.
Preparation method is: modified rosin is heated to 130 ~ 150 DEG C, melts maintenance constant temperature completely to it, adds organic acid activator, surfactant and organic solvent successively and is stirred to homogeneous transparent, constant temperature leave standstill 5 minutes not stratified.
Organic acid activator selected by the present invention is one or more in succinic acid, adipic acid, decanedioic acid, suberic acid or dimethylolpropionic acid, melting range is from 108 ~ 188 DEG C, boiling point Sum decomposition temperature is all below 240 DEG C, can continue to provide active in wider scope, remove metal pad surface film oxide, prevent metal surface from reoxidizing, effectively promote solder soaking on pad; Simultaneously major part (can have plumbous 245 DEG C, unleaded 260 DEG C) after welding again and decomposes or volatilization, and postwelding is residual few, and insulaion resistance is high, ensure that postwelding reliability.
Surfactant selected by the present invention is one or both in TX-10, OP-10, FC-4430 or FSN-100, is non-ionic surface active agent.Non-ionic surface active agent stability is high, acid and alkali-resistance, nontoxic, not containing halogen, can effectively reduce metal pad surface tension, cationic surfactant, anion surfactant, amphoteric surfactant have respective shortcoming or deficiency by contrast.What cationic surfactant had contains halogen, and what have has middle and high toxicity; Anion surfactant is acid and alkali-resistance not, unstable, is easily destroyed, and can not play completely and reduce capillary effect in the solder stick activating agent of slant acidity; Amphoteric ionic surfactant shows the performance of cationic surfactant in sour environment.
The interpolation of organic solvent is characteristic of the present invention, organic solvent selected by the present invention is one or both in 120 ﹟ solvent naphthas, 200 ﹟ solvent naphthas, turpentine oil or mixed dibasic acid ester (DBE), all there is extremely strong dissolubility, other compositions can be made more uniformly to distribute in rosin, preventing is heated to produce because of component distributing inequality splashes, the viscosity of rosin can be reduced simultaneously, improve liquid rosin mobility, ensure that rosin being uniformly distributed in solder stick.
Modified rosin selected by the present invention is one or both in Foral 101, Foral 301, perhydrogenated rosin or 150 high-softening-point rosins.Foral antioxidant is good, fragility is little, heat endurance is high, compatibility, caking property, ageing-resistant performance are excellent, is highly suitable in solder stick activating agent and applies; The softening point of 150 high-softening-point rosins, at about 150 DEG C, has higher non-oxidizability, anti-crystallization at operating temperature 300 ~ 400 DEG C.
Activating agent of the present invention, not containing any halogen, during welding, flue dust is little, taste is little, it is little to splash and have good activity, and wettability is good, and postwelding surface insulation resistance is high, the full light of solder joint.
Detailed description of the invention
Embodiment 1
Halogen solder stick activating agent is by following component and mass percent: adipic acid: 2%; Succinic acid: 2%; TX-10:0.2%; FC-4430:0.3%; 120 ﹟ solvent naphthas: 5%; 150 high-softening-point rosins: 5% and Foral 101:85.5%.
150 high-softening-point rosins and Foral 101 are joined in reactor, is heated to 145 DEG C to all fusings; Add adipic acid, succinic acid, TX-10, FC-4430 and 120 ﹟ solvent naphthas successively; Constantly be stirred to homogeneous transparent, constant temperature leave standstill 5 minutes not stratified.
Embodiment 2
Component and mass percent: suberic acid: 3%; Decanedioic acid: 1%; TX-10:0.2%; FSN-100:0.3%; 200 ﹟ solvent naphthas: 5%; 150 high-softening-point rosins: 5% and Foral 301:85.5%.
150 high-softening-point rosins and Foral 301 are joined in reactor, is heated to 145 DEG C to all fusings; Add suberic acid, decanedioic acid, TX-10, FSN-100 and 200 ﹟ solvent naphthas successively; Constantly be stirred to homogeneous transparent, constant temperature leave standstill 5 minutes not stratified.
Embodiment 3
Component and mass percent: suberic acid: 4%; OP-10:0.2%; FSN-100:0.3%; 200 ﹟ solvent naphthas: 3%; DBE:2% and perhydrogenated rosin: 90.5%.
Perhydrogenated rosin is joined in reactor, be heated to 145 DEG C to all fusings; Add suberic acid, OP-10, FSN-100,200 ﹟ solvent naphtha and DBE successively; Constantly be stirred to homogeneous transparent, constant temperature leave standstill 5 minutes not stratified.
Embodiment 4
Component and mass percent: suberic acid: 2%; Adipic acid: 1%; Dimethylolpropionic acid: 1%; OP-10:0.2%; FC-4430:0.3%; 120 ﹟ solvent naphthas: 3%; Turpentine oil: 2%; 150 high-softening-point rosins: 5% and perhydrogenated rosin: 85.5%.
150 high-softening-point rosins and perhydrogenated rosin are joined in reactor, is heated to 145 DEG C to all fusings; Add suberic acid, adipic acid, dimethylolpropionic acid, OP-10, FC-4430,120 ﹟ solvent naphtha and turpentine oil successively; Constantly be stirred to homogeneous transparent, constant temperature leave standstill 5 minutes not stratified.
Embodiment 5
Component and mass percent: adipic acid: 1%; FSN-100:0.3%; OP-10:1.2%; 200 ﹟ solvent naphthas: 3%; Turpentine oil: 1%; Foral 101:50% and perhydrogenated rosin: 43.5%.
Perhydrogenated rosin and Foral 101 are joined in reactor, is heated to 145 DEG C to all fusings; Add adipic acid, FSN-100, OP-10,200 ﹟ solvent naphtha and turpentine oil successively; Constantly be stirred to homogeneous transparent, constant temperature leave standstill 5 minutes not stratified.
Embodiment 6
Component and mass percent: adipic acid: 1%; Suberic acid: 1%; FSN-100:0.3%; TX-10:0.7%; 200 ﹟ solvent naphthas: 0.5%; Turpentine oil: 0.5%; Foral 101:50%; Perhydrogenated rosin: 40% and 150 high-softening-point rosins: 6%.
Perhydrogenated rosin, Foral 101 and 150 high-softening-point rosin are joined in reactor, is heated to 145 DEG C to all fusings; Add adipic acid, suberic acid, FSN-100, TX-10,200 ﹟ solvent naphtha and turpentine oil successively; Constantly be stirred to homogeneous transparent, constant temperature leave standstill 5 minutes not stratified.
Embodiment 7
Component and mass percent: adipic acid: 2%; Suberic acid: 1%; Decanedioic acid: 1%; Dimethylolpropionic acid: 1%; FSN-100:0.2%; 200 ﹟ solvent naphthas: 1%; Turpentine oil: 1%; Foral 301:45%; Perhydrogenated rosin: 40% and 150 high-softening-point rosins: 7.8%.
Perhydrogenated rosin, Foral 301 and 150 high-softening-point rosin are joined in reactor, is heated to 145 DEG C to all fusings; Add adipic acid, suberic acid, decanedioic acid, dimethylolpropionic acid, FSN-100,200 ﹟ solvent naphtha and turpentine oil successively; Constantly be stirred to homogeneous transparent, constant temperature leave standstill 5 minutes not stratified.
According to the Halogen solder stick activating agent of the Ministry of Information Industry of China " the liquid scaling powder standard SJ/T11273-2002 of No clean " the above embodiment of standard testing, result shows, Halogen solder stick activating agent of the present invention is not containing halogen, outward appearance is orange-yellow, all have no irritating odor in welding process, splash little, postwelding remains less and sprawls evenly, and spreading ratio is all more than 80%, and postwelding insulaion resistance is all greater than 5.0 × 10 10Ω, copper corrosion test is all without penetrability corrosion, and meet the requirements of the standard completely, the performance of Halogen solder stick activating agent of the present invention has obvious advantage with traditional activating agent ratio.

Claims (7)

1. a Halogen solder stick activating agent, is characterized in that being made up of following component and mass percent: organic acid activator 0.5 ~ 6%; Surfactant 0.1 ~ 2%; Organic solvent 0.5 ~ 5%; Modified rosin 90 ~ 96%.
2. Halogen solder stick activating agent according to claim 1, is characterized in that being made up of following component and mass percent: adipic acid: 1%; Suberic acid: 1%; FSN-100:0.3%; TX-10:0.7%; 200 ﹟ solvent naphthas: 0.5%; Turpentine oil: 0.5%; Foral 101:50%; Perhydrogenated rosin: 40% and 150 high-softening-point rosins: 6%.
3. Halogen solder stick activating agent according to claim 1, is characterized in that organic acid activator is one or more in succinic acid, adipic acid, decanedioic acid, suberic acid or dimethylolpropionic acid.
4. Halogen solder stick activating agent according to claim 1, is characterized in that surfactant is one or both in TX-10, OP-10, FC-4430 or FSN-100.
5. Halogen solder stick activating agent according to claim 1, is characterized in that organic solvent is one or both in 120 ﹟ solvent naphthas, 200 ﹟ solvent naphthas, turpentine oil or commercially available mixed dibasic acid ester (DBE).
6. Halogen solder stick activating agent according to claim 1, is characterized in that modified rosin is one or both in Foral 101, Foral 301, perhydrogenated rosin or 150 high-softening-point rosins.
7. the preparation method of Halogen solder stick activating agent as claimed in claim 1, modified rosin is it is characterized in that to be heated to 130 ~ 150 DEG C, maintenance constant temperature is melted completely to it, add organic acid activator, surfactant and organic solvent successively and be stirred to homogeneous transparent, constant temperature leave standstill 5 minutes not stratified.
CN201510651313.8A 2015-10-10 2015-10-10 A kind of Halogen solder stick activating agent and preparation method thereof Expired - Fee Related CN105234591B (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106624463A (en) * 2016-11-30 2017-05-10 重庆微世特电子材料有限公司 Activating agent used for water-based soldering flux and preparing method of activating agent
CN108788521A (en) * 2018-06-28 2018-11-13 广东剑鑫科技股份有限公司 A kind of transformer scaling powder and preparation method thereof
CN114005663A (en) * 2021-09-26 2022-02-01 深圳市岑科实业有限公司 NR inductor, tin wire and manufacturing method of NR inductor
CN114871629A (en) * 2022-06-21 2022-08-09 浙江亚通焊材有限公司 Solder wire containing nickel ball and preparation method thereof

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106624463A (en) * 2016-11-30 2017-05-10 重庆微世特电子材料有限公司 Activating agent used for water-based soldering flux and preparing method of activating agent
CN108788521A (en) * 2018-06-28 2018-11-13 广东剑鑫科技股份有限公司 A kind of transformer scaling powder and preparation method thereof
CN108788521B (en) * 2018-06-28 2021-08-10 广东剑鑫科技股份有限公司 Transformer flux and preparation method thereof
CN114005663A (en) * 2021-09-26 2022-02-01 深圳市岑科实业有限公司 NR inductor, tin wire and manufacturing method of NR inductor
CN114871629A (en) * 2022-06-21 2022-08-09 浙江亚通焊材有限公司 Solder wire containing nickel ball and preparation method thereof

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