CN101690997B - Non-halogen cleaning-free soldering flux - Google Patents

Non-halogen cleaning-free soldering flux Download PDF

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Publication number
CN101690997B
CN101690997B CN2009103081847A CN200910308184A CN101690997B CN 101690997 B CN101690997 B CN 101690997B CN 2009103081847 A CN2009103081847 A CN 2009103081847A CN 200910308184 A CN200910308184 A CN 200910308184A CN 101690997 B CN101690997 B CN 101690997B
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China
Prior art keywords
acid
soldering flux
cleaning
free soldering
halogen
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Expired - Fee Related
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CN2009103081847A
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Chinese (zh)
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CN101690997A (en
Inventor
朱岳恩
丁建设
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Ningbo Xihan Tin Solder Co Ltd
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Ningbo Xihan Tin Solder Co Ltd
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Abstract

The invention provides a non-halogen cleaning-free soldering flux, which comprises the following compositions in percentage by weight: 0.5 to 5 percent of stannous oxalate, 0.5 to 20 percent of organic acid activator, 0.1 to 1 percent of surfactant, 0 to 3 percent of cosolvent, and the balance of solvent. Because of adopting the stannous oxalate as an activator, and having synergistic action with the organic acid activator and no halogen, the soldering flux has the advantages of no irritant odour, less smoke, no environmental pollution, strong wetting power and excellent weldability. When the soldering flux is used for welding, a printed package board has less solid residue, clean layout and low ionic contamination, and needs no cleaning after the welding; and the printed package board has high insulation resistance after the welding, which can meet the cleaning-free requirement of the printing package board.

Description

A kind of non-halogen cleaning-free soldering flux
Technical field
The present invention relates to the scaling powder in the electronic material.
Background technology
Scaling powder is the critical material that guarantees welding quality, it should have the higher weldering that helps, and can not produce corrosion to materials to be welded again, also will satisfy the especially requirement of reliability aspect of a series of machinery, electric property simultaneously, therefore, the quality of scaling powder directly affects quality of welded.
In soldering technology, because having very outstanding helping, the chemical substance of some Halogen welds activity and low-cost advantage, therefore the scaling powder that uses at present is made up of rosin, resin, halide activating agent etc. mostly, this class scaling powder solderability is better, cost is low, but the electronic product of its postwelding is if continued to keep the activity of Halogen chemicals, its ionic pollution degree will exceed standard, then produce phenomenons such as chronic electricity leakage and corrosion, shorten the life-span of electronic product, even can have a strong impact on the reliability of electronic product.
For overcoming the above problems, need with hydrocarbon compound (CFCs) class of fluorine, chlorine substituent or contain volatile organic compound (VOC) class cleaning agent to clean, and the destruction that a large amount of dischargings of CFCs can cause ozone layer, according to Montreal Convention, progressively it bans use of industry.VOC disperses in atmosphere, and a large amount of science data prove, CO2, CH4 etc. contain all kinds of gases of C, is the main arch-criminal who causes global warming and greenhouse, border, destruction border.
After the forbidding CFCs, the notion that proposes washing one period was arranged once, the washing scaling powder is also after a while popular.But at first, the one, because water has had a strong impact on the reliability requirement of electronic product in the hydropexis problem in some electronic devices and components slit, the 2nd, the processing of cleaning industrial wastewater later also is to bother very much, thereby can't promote.
No-clean scaling powder can reduce cost, and shortens the production cycle, reduces the technological process of production, has important economic benefit and social benefit, has become the important directions of electron trade development.But many " exempting to clean " more of notions so far lay particular emphasis on the reliability aspect of guaranteeing electronic product, and it is still not enough that environmental protection factor aspect is considered.
Begin in recent years to release some new international standards (IEC61249-2-21, JPCA-ES01, IPC4101B), new standard is clearer and more definite to the definition of Halogen, the one, scaling powder has been proposed stricter restriction, not only limit the content of free halogen, but also limited the content of halides; The 2nd, clearly defined content and halogen total content, the i.e. bromine≤900PPM of chlorine element and bromo element in the electronic welding material; Chlorine≤900PPM; Bromine+chlorine≤1500PPM is so the non-halogen process of electronic welding is had higher requirement to scaling powder.
Summary of the invention
Technical problem to be solved by this invention provides a kind of non-halogen cleaning-free soldering flux and solves postwelding residue that existing scaling powder exists too much and difficult problems such as electric property reliability deficiency of bringing because of the existence of halogen and solder joint corrosion, simultaneously, take into account the negative effect that reduces as far as possible the environment generation.
The present invention solves the problems of the technologies described above the technical scheme that is adopted:
A kind of non-halide cleaning-free welding flux, the percentage by weight of each component is:
Stannous oxalate 0.5%~5%
Organic acid activator 0.5~20%
Cosolvent 0~3%
Surfactant 0.1~1%
The solvent surplus
Because the organic acid activator is active obviously not as the halide activator, finds among the present invention to select for use stannous oxalate as activator, collaborative organic acid activator uses, and can reach stronger activation effect.Stannous oxalate has strong reducing power, can react with the oxide of mother metal and solder surface, removes the oxide-film of mother metal and solder surface, plays the effect that replaces the halide activating agent.
Above-mentioned organic acid activator can be selected succinic acid, dimethyl succinic acid, succinic anhydride, itaconic acid, fumaric acid, adipic acid, glutaric acid, azelaic acid, decanedioic acid, benzoic acid, phthalic acid, malic acid, stearic one or more mixtures.
Above-mentioned cosolvent is ethers or esters solvent, can select ethylene glycol monobutyl ether, one or more of propylene glycol monomethyl ether, diethylene glycol monoethyl ether, diethylene glycol dimethyl ether, diethylene glycol monobutyl ether, diethylene glycol monobutyl ether, ethyl acetate, butyl acetate, dimethyl succinate, diethyl succinate.Cosolvent can play surfactant and wetting agent, and can increase surface insulation resistance.
Above-mentioned surfactant can select that OP-5, OP-7, OP-10's is a kind of.This type of surfactant belongs to nonionic surface active agent, can effectively reduce the surface tension of scolder between pad, strengthens wetability.
Above-mentioned solvent is one or more mixing of ethanol, isopropyl alcohol, methyl alcohol.
Compared with prior art, the invention has the advantages that:
Since adopt stannous oxalate as activator, and act synergistically with the organic acid for activating agent, not halogen-containing, therefore having no irritating odor, smog is few, and is free from environmental pollution, and wetting power is strong, and solderability is superior.When being used to weld, solid residue is few on the printing component palette, clean layout, and ionic pollution degree is low, and postwelding need not clean, and the insulaion resistance height of postwelding printing assembly plate, can satisfy the cleaning requirement of exempting from of printing component palette.
The specific embodiment
Below in conjunction with embodiment the present invention is further described.
Embodiment 1:
Non-halogen cleaning-free soldering flux, the percentage by weight of each component is:
Stannous oxalate 3
Dimethyl succinic acid 1
Itaconic acid 0.2
Fumaric acid 0.2
Diethylene glycol dimethyl ether 3
OP-7 0.25
The isopropyl alcohol surplus
Concrete preparation method: get above-mentioned each composition, in having the reactor of agitator, add solvent earlier, add the thermal control temperature under the solvent fusing point, stir adding stannous oxalate, organic acid activator, cosolvent, it is transparent to be stirred to solution, is non-halogen cleaning-free soldering flux.
This scaling powder is detected its rate of spread 〉=85%, surface insulation resistance value S.I.R 〉=1 * 10 with the JISZ 3197-1999 of Japanese Industrial Standards 12Ω.
Embodiment 2:
Non-halogen cleaning-free soldering flux, the percentage by weight of each component is:
Stannous oxalate 0.5
Succinic acid 4
Adipic acid 3
Malic acid 3
OP-10 1
Ethanol 15
The isopropyl alcohol surplus
The preparation method is identical with embodiment 1.
This scaling powder is detected its rate of spread 〉=85%, surface insulation resistance value S.I.R 〉=1 * 10 with the JISZ 3197-1999 of Japanese Industrial Standards 12Ω.
Embodiment 3:
Non-halogen cleaning-free soldering flux, the percentage by weight of each component is:
Stannous oxalate 1.5
Phthalic acid 1.5
Succinic anhydride 3
Azelaic acid 4
OP-7 0.1
Ethanol 15
Methyl alcohol 35
The isopropyl alcohol surplus
The preparation method is identical with embodiment 1.
This scaling powder is detected its rate of spread 〉=85%, surface insulation resistance value S.I.R 〉=1 * 10 with the JISZ 3197-1999 of Japanese Industrial Standards 12Ω.
Embodiment 4:
Non-halogen cleaning-free soldering flux, the percentage by weight of each component is:
Stannous oxalate 4
Dimethyl succinic acid 5
Benzoic acid 1
OP-5 0.5
Butyl acetate 1
Diethyl succinate 1
Isopropyl alcohol 30
The methyl alcohol surplus
The preparation method is identical with embodiment 1.
This scaling powder is detected its rate of spread 〉=85%, surface insulation resistance value S.I.R 〉=1 * 10 with the JISZ 3197-1999 of Japanese Industrial Standards 12Ω.
Embodiment 5:
Non-halogen cleaning-free soldering flux, the percentage by weight of each component is:
Stannous oxalate 5
Fumaric acid 2
Glutaric acid 2
OP-7 0.3
Butyl acetate 1
Diethyl succinate 1.5
The isopropyl alcohol surplus
The preparation method is identical with embodiment 1.
This scaling powder is detected its rate of spread 〉=85%, surface insulation resistance value S.I.R 〉=1 * 10 with the JISZ 3197-1999 of Japanese Industrial Standards 12Ω.
Embodiment 6:
Non-halogen cleaning-free soldering flux, the percentage by weight of each component is:
Stannous oxalate 3
Decanedioic acid 10
Stearic acid 5
Benzoic acid 5
OP-10 0.5
Diethylene glycol dimethyl ether 0.5
Isopropyl alcohol 20
The ethanol surplus
The preparation method is identical with embodiment 1.
This scaling powder is detected its rate of spread 〉=85%, surface insulation resistance value S.I.R 〉=1 * 10 with the JISZ 3197-1999 of Japanese Industrial Standards 12Ω.
Embodiment 7:
Non-halogen cleaning-free soldering flux, the percentage by weight of each component is:
Stannous oxalate 1
Succinic anhydride 1.5
Fumaric acid 2
Malic acid 0.5
OP-5 0.3
The isopropyl alcohol surplus
The preparation method is identical with embodiment 1.
This scaling powder is detected its rate of spread 〉=85%, surface insulation resistance value S.I.R 〉=1 * 10 with the JISZ 3197-1999 of Japanese Industrial Standards 12Ω.
Embodiment 8:
Non-halogen cleaning-free soldering flux, the percentage by weight of each component is:
Stannous oxalate 3
Dimethyl succinic acid 0.25
Succinic anhydride 0.25
Diethylene glycol monobutyl ether 1.2
Butyl acetate 1.3
OP-7 0.8
The isopropyl alcohol surplus
The preparation method is identical with embodiment 1.
This scaling powder is detected its rate of spread 〉=85%, surface insulation resistance value S.I.R 〉=1 * 10 with the JISZ 3197-1999 of Japanese Industrial Standards 12Ω.
Embodiment 9:
Non-halogen cleaning-free soldering flux, the percentage by weight of each component is:
Stannous oxalate 2.5
Succinic acid 2.5
Dimethyl succinic acid 0.5
Adipic acid 5
Diethyl succinate 1
OP-7 0.8
Ethanol 25
The isopropyl alcohol surplus
The preparation method is identical with embodiment 1.
This scaling powder is detected its rate of spread 〉=85%, surface insulation resistance value S.I.R 〉=1 * 10 with the JISZ 3197-1999 of Japanese Industrial Standards 12Ω.
Embodiment 10
Non-halogen cleaning-free soldering flux, the percentage by weight of each component is:
Stannous oxalate 2.5
Azelaic acid 2
Malic acid 2
Diethylene glycol dimethyl ether 0.5
Two diethyl phthalates 0.5
OP-10 1
The methyl alcohol surplus
The preparation method is identical with embodiment 1.
This scaling powder is detected its rate of spread 〉=85%, surface insulation resistance value S.I.R 〉=1 * 10 with the JISZ 3197-1999 of Japanese Industrial Standards 12Ω.

Claims (6)

1. non-halogen cleaning-free soldering flux, its characteristic is: the percentage by weight of each component is: stannous oxalate 0.5~5%, organic acid activator 0.5~20%, surfactant 0.1~1%, cosolvent 0~3%, surplus is a solvent.
2. non-halogen cleaning-free soldering flux as claimed in claim 1 is characterized in that: described organic acid activator is succinic acid, dimethyl succinic acid, succinic anhydride, itaconic acid, fumaric acid, adipic acid, glutaric acid, azelaic acid, decanedioic acid, benzoic acid, phthalic acid, malic acid, stearic two kinds or multiple mixture.
3. non-halogen cleaning-free soldering flux as claimed in claim 1 or 2 is characterized in that: described cosolvent is ethers or esters solvent.
4. non-halogen cleaning-free soldering flux as claimed in claim 3, it is characterized in that: described cosolvent is an ethylene glycol monobutyl ether, one or both mixtures of propylene glycol monomethyl ether, diethylene glycol monoethyl ether, diethylene glycol dimethyl ether, diethylene glycol monobutyl ether, ethyl acetate, butyl acetate, dimethyl succinate, diethyl succinate.
5. non-halogen cleaning-free soldering flux as claimed in claim 1 or 2 is characterized in that: described surfactant is a kind of among OP-5, OP-7, the OP-10.
6. non-halogen cleaning-free soldering flux as claimed in claim 1 or 2 is characterized in that: described solvent is one or more mixtures of ethanol, isopropyl alcohol, methyl alcohol.
CN2009103081847A 2009-10-12 2009-10-12 Non-halogen cleaning-free soldering flux Expired - Fee Related CN101690997B (en)

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CN101690997B true CN101690997B (en) 2011-06-15

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Families Citing this family (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102794458B (en) * 2012-08-24 2014-11-05 济南大学 Hollow silver particle and preparation method thereof
CN104384752B (en) * 2014-09-23 2016-06-08 明光旭升科技有限公司 A kind of soldering flux being applied to sensor
CN107584233A (en) * 2017-09-29 2018-01-16 苏州宙璎电子有限公司 A kind of environmentally friendly cleaning-free water base scaling powder
CN109175793A (en) * 2018-09-14 2019-01-11 深圳市中南环保科技控股有限公司 Solvent type no-clean scaling powder
CN108994485B (en) * 2018-10-26 2021-01-05 众潮电科(深圳)有限公司 Soldering flux and preparation method thereof
CN110449768A (en) * 2019-09-02 2019-11-15 重庆理工大学 A kind of halogen-free no rosin solvent type scaling powder free of cleaning
CN110449773A (en) * 2019-09-02 2019-11-15 重庆理工大学 A kind of multifunctional solvent type scaling powder free of cleaning

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1110205A (en) * 1994-04-06 1995-10-18 化学工业部晨光化工研究院成都分院 Non-halogen non-rosin type low solid content non-cleaning scaling powder
CN1404959A (en) * 2002-10-18 2003-03-26 深圳市唯特偶化工开发实业有限公司 Halogen-free low-solid-contained water-base washing-free scaling powder
CN101412168A (en) * 2008-11-26 2009-04-22 华南理工大学 Scaling powder for aluminium soldering tin wire core and preparation method thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1110205A (en) * 1994-04-06 1995-10-18 化学工业部晨光化工研究院成都分院 Non-halogen non-rosin type low solid content non-cleaning scaling powder
CN1404959A (en) * 2002-10-18 2003-03-26 深圳市唯特偶化工开发实业有限公司 Halogen-free low-solid-contained water-base washing-free scaling powder
CN101412168A (en) * 2008-11-26 2009-04-22 华南理工大学 Scaling powder for aluminium soldering tin wire core and preparation method thereof

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