CN102554518A - Halogen-free high-impedance soldering flux and preparation method - Google Patents
Halogen-free high-impedance soldering flux and preparation method Download PDFInfo
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- CN102554518A CN102554518A CN2012100187767A CN201210018776A CN102554518A CN 102554518 A CN102554518 A CN 102554518A CN 2012100187767 A CN2012100187767 A CN 2012100187767A CN 201210018776 A CN201210018776 A CN 201210018776A CN 102554518 A CN102554518 A CN 102554518A
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Abstract
The invention relates to a halogen-free high-impedance soldering flux and a preparation method. The halogen-free high-impedance soldering flux is characterized by containing the following components according to weight: 2-8% of organic acid activating agent, 0.1-2% of non-ionic surface active agent, 3-8% of organic solvent having a high boiling point, 0.01-0.5% corrosion inhibitor and the balance of modified rosin. The preparation method comprises the following steps: adding modified rosin into a container for heating and stirring until the modified rosin is completely fused; adding the organic acid activating agent, the non-ionic surface active agent, the corrosion inhibitor and the organic solvent having a high boiling point in sequence at a temperature of 130-150 DEG C, and continuing to stir for 20-30 minutes to obtain the soldering flux. The halogen-free high-impedance soldering flux has excellent welding assisting effect to lead-free solder, is halogen-free, has no harm to health and environment, causes little splashing, has less residue after welding, has high insulation resistance on the surface, and ensures the advantage and effect of reliability of electronic products after welding.
Description
Technical field
The present invention relates to a kind of Halogen high impedance scaling powder,, belong to the solderable material field of electronics, electric product especially for the Halogen high impedance scaling powder of lead-free soldering wire.
The invention still further relates to the preparation method of this Halogen high impedance scaling powder.
Background technology
In recent years because the appearance in succession that strengthens and prohibit plumbous decree day by day of human environmental consciousness; Electronic Packaging solder solder carries out the transition to lead-free brazing from traditional lead solder that has gradually; Sn-Cu system and the Sn-Ag-Cu brazing filler metal in the industry cycle is acknowledged as preferably and business-like lead-free brazing wherein; Yet their fusing point is than 183 ℃ high 30～45 ℃ of traditional Sn-Pb eutectic solder, and traditional Sn-Pb solder stick is difficult to satisfy the soldering demand of lead-free process with scaling powder.
For this reason; Each big electronics manufacturing enterprise and scolding tin manufactory are devoted to the research of lead-free brazing with the high activity scaling powder one after another; And obtained remarkable achievement, develop multiple lead-free soldering wire and use scaling powder, but multianalysis is found after the patent of the domestic lead-free soldering wire that occurs with scaling powder with research now; Present domestic lead-free soldering wire uses halogen contained compound or salts substances mostly with scaling powder; Yet such scaling powder postwelding halogen residue thing is many, has brought great potential safety hazard for the dependability of product, especially under high temperature and high humility situation; Like China's southern area environment temperature height and the big situation of air humidity during rainy season, such halogen-containing scaling powder makes the reliability of electronic product be faced with huge test.A kind of soldering flux in use for soft soldering wire like Chinese patent 200710022404.0 announcements; This patent has been used dibromo butene glycol, dibromo ethyl benzene and halide-containings such as brocide, amine salt; Postwelding halogen residue degree is high, yet constantly dwindles at the package dimension of electronics, electric product, under the more and more littler situation of components and parts pin-pitch; Directed moving usually takes place in the halogen residue thing of PCB surface in electric field environment; Cause surface insulation resistance to reduce, cause short circuit between the components and parts pin easily, finally cause components and parts to lose efficacy; The cleaning-free lead-free solder soldering fluid that Chinese patent 200810025124.X announces; This patent has been used halide-containings such as brocide, dibromo butene two pure and mild 5-chloro-salicylic acids, and postwelding halogen residue thing is many, perishable wiring board and solder joint in the components and parts use; Reduce the surface insulation resistance at wiring board and components and parts pin place; Short circuit between final initiation components and parts pin makes components and parts lose efficacy in the process under arms, can not satisfy the high reliability request of high-end electronic product.
Summary of the invention
The Halogen high impedance scaling powder that the object of the invention provides a kind of lead-free soldering wire to use for the shortcoming that overcomes above-mentioned prior art with deficiency just; Thereby can guarantee the postwelding reliability of electronic product, can satisfy the strict demand of hyundai electronics industry high reliability.
The present invention also provides the preparation method of this Halogen high impedance scaling powder.
The objective of the invention is to realize through following technical proposal:
A kind of Halogen high impedance scaling powder, it is made up of following weight percentages:
Described organic acid activator is one or both or the two or more combination in succinic acid, glutaric acid, adipic acid, suberic acid, decanedioic acid, dodecoic acid, tetradecylic acid, hexadecylic acid, maleic acid, itaconic acid or the salicylic acid;
Described non-ionic surface active agent is one or both or the two or more combination in OPEO, APES, NPE, isooctylphenol APEO, AEO, polyethyleneglycol resin acid ester or the polyethylene glycol monooleate;
Described high boiling organic solvent is one or both or the two or more combination in diethylene glycol monohexyl ether, triethylene glycol butyl ether, triethyl group carbitol ether or the tri ethylene glycol ethyl ether;
Described corrosion inhibiter is one or both or the two or more combination in BTA, hydroxybenzotriazole, methylbenzotrazole or the triethylamine;
Described modified rosin is one or both or the two or more combination in water-white rosin, newtrex, Foral or the acrylic rosin.
The preparation method of described Halogen high impedance scaling powder, it is undertaken by following step:
The surplus modified rosin is joined in the container heating and is stirred to fusing fully; Under 130～150 ℃ of temperature, add 2～8% organic acid activator, 0.1～2% non-ionic surface active agent, 0.01～0.5% corrosion inhibiter and 3～8% high boiling organic solvent successively; Continue to stir 20～30 minutes, process Halogen high impedance scaling powder.
The raw material that the present invention selects, organic acid activator wherein is nonhygroscopic, and sufficiently high activity is arranged; When welding, can remove solder effectively and welded the oxide of metal surface; Reduce the surface tension of solder, realize good welding, and in welding process, can in time decompose and volatilization; The postwelding noresidue does not have corrosion, and surface insulation resistance is high; Non-ionic surface active agent can be removed the oxide-film on solder surface effectively, reduces the surface tension of solder, improves the wetability of solder, improves the spreading ability of solder; Promote the mobile of solder and sprawl, obtain good soldered fitting, and this type of non-ionic surface active agent is not halogen-containing; Environmentally friendly, postwelding stability is high simultaneously, unionization; Surface insulation resistance is high, also is not subject to the influence of soda acid, and is also very good with the organic acid activator compatibility; High boiling organic solvent can make organic acid activator, corrosion inhibiter and non-ionic surface active agent in modified rosin, evenly distribute; Avoid in welding process, being splashed on the wiring board because of the organic acid activator skewness; Thereby reduce the corrosion of residue, and then improve surface insulation resistance wiring board; Corrosion inhibiter can reduce the corrosion of film of flux residue to wiring board in the active material generation redox reaction of postwelding and small amount of residual, improves the PCB surface insulaion resistance, thereby improves reliability; Modified rosin can form compact protective film on the solder joint surface in welding process solder joint is wrapped up, and secluding air prevents the oxidation once more of solder joint, and is solid-state under the postwelding normal temperature, and stable performance is non-conductive, and surface insulation resistance is high.
Owing to take technique scheme to make technology of the present invention compared with present technology have following advantage and effect:
A) scaling powder of the present invention has the splendid weldering effect that helps to Sn-Cu system and Sn-Ag-Cu series leadless solder, not only can effectively remove oxide-film, realize helping weldering fast, and not add halogen contained compound fully, and is nuisanceless to health and environment;
B) high boiling organic solvent that adds of scaling powder of the present invention can improve organic acid activator, non-ionic surface active agent and corrosion inhibiter modified rosin distribution; Make that scaling powder is basically very little in the welding process; The postwelding residue is few; Surface insulation resistance is high, has guaranteed the postwelding reliability of electronic product, can satisfy the strict demand of hyundai electronics industry to reliability;
C) scaling powder of the present invention is not for containing halogen, and the rate of spread>=80%, insulaion resistance are significantly greater than 1 * 10
12Ω reaches and is superior to SJ/T11273-2002 and exempts to clean insulaion resistance>=1 * 10 in the liquid scaling powder standard
8The standard of Ω is a kind of Halogen high impedance scaling powder.
The specific embodiment
Below in conjunction with concrete embodiment halogen high impedance scaling powder of the present invention is further specified.
Embodiment 1
Raw material:
Newtrex 92.70g, hexadecylic acid 2g, APES 0.5g, NPE 0.5g,
Isooctylphenol APEO 1g, hydroxybenzotriazole 0.1g, methylbenzotrazole 0.1g, triethylamine 0.1g and triethyl group carbitol ether 3g.
The 92.70g newtrex is joined in the container heating and is stirred to fusing fully; Under 130 ℃ of temperature, add 2g hexadecylic acid, 0.5g APES, 0.5g NPE, 1g isooctylphenol APEO, 0.1g hydroxybenzotriazole, 0.1g methylbenzotrazole, 0.1g triethylamine and 3g triethyl group carbitol ether successively; Continue to stir 30 minutes, process Halogen high impedance scaling powder.
Embodiment 2
Raw material:
Newtrex 48.5g, Foral 40g, glutaric acid 2g, adipic acid 2g, dodecoic acid 1g, AEO 0.5g, polyethyleneglycol resin acid ester 0.5g, triethylamine 0.5g, triethylene glycol butyl ether 2g and triethyl group carbitol ether 3g,
48.5g newtrex, 40g Foral are joined in the container heating and be stirred to fusing fully; Under 140 ℃ of temperature, add 2g glutaric acid, 2g adipic acid, 1g dodecoic acid, 0.5g AEO, 0.5g polyethyleneglycol resin acid ester, 0.5g triethylamine, 2g triethylene glycol butyl ether and 3g triethyl group carbitol ether successively; Continue to stir 25 minutes, process Halogen high impedance scaling powder.
Embodiment 3
Raw material:
Water-white rosin 42.4g, newtrex 20g, Foral 25g, suberic acid 3g, decanedioic acid 3g, APES 0.2g, NPE 0.3g, BTA 0.05g, hydroxybenzotriazole 0.05g, tri ethylene glycol ethyl ether 6g.
42.4g water-white rosin, 20g newtrex, 25g Foral are joined in the container heating and be stirred to fusing fully; Under 150 ℃ of temperature, add 3g suberic acid, 3g decanedioic acid, 0.2g APES, 0.3g NPE, 0.05g BTA, 0.05g hydroxybenzotriazole, 6g tri ethylene glycol ethyl ether successively; Continue to stir 20 minutes, process Halogen high impedance scaling powder.
Embodiment 4
Raw material:
Water-white rosin 44.59g, newtrex 40g, succinic acid 2g, tetradecylic acid 2g, itaconic acid 3g, OPEO 0.3g, polyethylene glycol monooleate 0.1g, BTA 0.01g, diethylene glycol monohexyl ether 2g, triethylene glycol butyl ether 3g and triethyl group carbitol ether 3g.
44.59g water-white rosin, 40g newtrex are joined in the container heating and be stirred to fusing fully; Under 135 ℃ of temperature, add 2g succinic acid, 2g tetradecylic acid, 3g itaconic acid, 0.3g OPEO, 0.1g polyethylene glycol monooleate, 0.01g BTA, 2g diethylene glycol monohexyl ether, 3g triethylene glycol butyl ether, 3g triethyl group carbitol ether successively and continue to stir 25 minutes, process Halogen high impedance scaling powder.
Embodiment 5
Raw material:
Foral 44.5g, acrylic rosin 40g, maleic acid 2g, salicylic acid 3g, hexadecylic acid 3g, OPEO 0.1g, hydroxybenzotriazole 0.1g, methylbenzotrazole 0.3g and triethylene glycol butyl ether 7g.
44.5g Foral, 40g acrylic rosin are joined in the container heating and is stirred to fusing fully; Under 135 ℃ of temperature, add 2g maleic acid, 3g salicylic acid, 3g hexadecylic acid, 0.1g OPEO, 0.1g hydroxybenzotriazole, 0.3g methylbenzotrazole and 7g triethylene glycol butyl ether successively; Continue to stir 25 minutes, process Halogen high impedance scaling powder.
The comparative example:
Raw material:
Foral 40.5g, newtrex 52.5g, succinic acid 1.8g, glutaric acid 3g, hexadecyltrimethylammonium chloride 0.2g, diethylamine hydrobromide 0.5g, cyclohexylamine hydrochloride 1.5g.
40.5g Foral, 52.5g newtrex are joined in the container heating and be stirred to fusing fully; Under 140 ℃ of temperature, add 1.8g succinic acid, 3g glutaric acid, 0.2g hexadecyltrimethylammonium chloride, 0.5g diethylamine hydrobromide and 1.5g cyclohexylamine hydrochloride successively; Continue to stir 25 minutes, process the high activity scaling powder.
Exempt to clean the test method of stipulating in the liquid scaling powder standard according to the SJ/T11273-2002 of China Ministry of Industry and Information, foregoing invention embodiment 1 to 5 and comparative example's performance is detected, each item testing result is seen table 1.
Table 1 embodiment 1 to 5 and comparative example's performance test results
Can find out that from table 1 embodiments of the invention 1 to 5 all do not contain halogen, the rate of spread>=80%, insulaion resistance are significantly greater than 1 * 10
12Ω meets and exceeds SJ/T11273-2002 and exempts to clean insulaion resistance>=1 * 10 in the liquid scaling powder standard
8The requirement of Ω; And containing 0.4% halogen in the Comparative Examples, postwelding can bring great potential safety hazard to the reliability that product uses, and insulaion resistance also is far smaller than the insulaion resistance of the embodiment of the invention.
Claims (2)
1. Halogen high impedance scaling powder, it is characterized in that: it is made up of following weight percentages:
Organic acid activator 2 ~ 8%
Non-ionic surface active agent 0.1 ~ 2%
High boiling organic solvent 3 ~ 8%
Corrosion inhibiter 0.01 ~ 0.5%
The modified rosin surplus
Described organic acid activator is one or both or the two or more combination in succinic acid, glutaric acid, adipic acid, suberic acid, decanedioic acid, dodecoic acid, tetradecylic acid, hexadecylic acid, maleic acid, itaconic acid or the salicylic acid;
Described non-ionic surface active agent is one or both or the two or more combination in OPEO, APES, NPE, isooctylphenol APEO, AEO, polyethyleneglycol resin acid ester or the polyethylene glycol monooleate;
Described high boiling organic solvent is one or both or the two or more combination in diethylene glycol monohexyl ether, triethylene glycol butyl ether, triethyl group carbitol ether or the tri ethylene glycol ethyl ether;
Described corrosion inhibiter is one or both or the two or more combination in BTA, hydroxybenzotriazole, methylbenzotrazole or the triethylamine;
Described modified rosin is one or both or the two or more combination in water-white rosin, newtrex, Foral or the acrylic rosin.
2. the preparation method of a Halogen high impedance scaling powder as claimed in claim 1 is characterized in that it is undertaken by following step:
The surplus modified rosin is joined in the container heating and is stirred to fusing fully; Under 130 ~ 150 ℃ of temperature, add 2 ~ 8% organic acid activator, 0.1 ~ 2% non-ionic surface active agent, 0.01 ~ 0.5% corrosion inhibiter and 3 ~ 8% high boiling organic solvents successively; Continue to stir 20 ~ 30 minutes, process Halogen high impedance scaling powder.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2012100187767A CN102554518A (en) | 2012-01-19 | 2012-01-19 | Halogen-free high-impedance soldering flux and preparation method |
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| CN2012100187767A CN102554518A (en) | 2012-01-19 | 2012-01-19 | Halogen-free high-impedance soldering flux and preparation method |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105215579A (en) * | 2015-11-13 | 2016-01-06 | 广东中实金属有限公司 | Halogen-free scaling powder and preparation method in a kind of automatic welding machine people solder stick |
| CN105234591A (en) * | 2015-10-10 | 2016-01-13 | 广州有色金属研究院 | Halogen-free soldering tin wire activator and preparation method thereof |
| CN105458552A (en) * | 2015-12-31 | 2016-04-06 | 深圳市兴鸿泰锡业有限公司 | High-performance tin wire soldering flux for automatic tin soldering and preparation method of high-performance tin wire soldering flux |
| CN105772979A (en) * | 2016-04-13 | 2016-07-20 | 苏州伊飞特电子科技有限公司 | High flux environment-friendly tin wire and preparation method thereof |
| CN107498208A (en) * | 2017-08-24 | 2017-12-22 | 广东中实金属有限公司 | A kind of lead-free soldering wire for being applied to drag welding technology |
| CN108262577A (en) * | 2018-01-26 | 2018-07-10 | 东莞市固晶电子科技有限公司 | A kind of powder particle scaling powder and preparation method thereof |
| CN113677814A (en) * | 2019-04-11 | 2021-11-19 | 哈利玛化成株式会社 | Flux, solder paste, and electronic circuit board |
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| JP2002001581A (en) * | 2000-06-21 | 2002-01-08 | Fujikura Ltd | Flux for non-lead soft solder |
| CN101049663A (en) * | 2007-05-09 | 2007-10-10 | 昆山成利焊锡制造有限公司 | Soldering flux in use for soft soldering wire, and preparation method |
| CN101049662A (en) * | 2007-05-09 | 2007-10-10 | 昆山成利焊锡制造有限公司 | Soldering flux without halogen in use for soft welding wire without lead, and preparation method |
| CN101879671A (en) * | 2010-06-13 | 2010-11-10 | 汕头市骏码凯撒有限公司 | Halogen-free flux and method for preparing same |
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2012
- 2012-01-19 CN CN2012100187767A patent/CN102554518A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002001581A (en) * | 2000-06-21 | 2002-01-08 | Fujikura Ltd | Flux for non-lead soft solder |
| CN101049663A (en) * | 2007-05-09 | 2007-10-10 | 昆山成利焊锡制造有限公司 | Soldering flux in use for soft soldering wire, and preparation method |
| CN101049662A (en) * | 2007-05-09 | 2007-10-10 | 昆山成利焊锡制造有限公司 | Soldering flux without halogen in use for soft welding wire without lead, and preparation method |
| CN101879671A (en) * | 2010-06-13 | 2010-11-10 | 汕头市骏码凯撒有限公司 | Halogen-free flux and method for preparing same |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105234591A (en) * | 2015-10-10 | 2016-01-13 | 广州有色金属研究院 | Halogen-free soldering tin wire activator and preparation method thereof |
| CN105215579A (en) * | 2015-11-13 | 2016-01-06 | 广东中实金属有限公司 | Halogen-free scaling powder and preparation method in a kind of automatic welding machine people solder stick |
| CN105458552A (en) * | 2015-12-31 | 2016-04-06 | 深圳市兴鸿泰锡业有限公司 | High-performance tin wire soldering flux for automatic tin soldering and preparation method of high-performance tin wire soldering flux |
| CN105458552B (en) * | 2015-12-31 | 2018-07-17 | 深圳市兴鸿泰锡业有限公司 | A kind of automatic soldering high-performance solder stick scaling powder and preparation method thereof |
| CN105772979A (en) * | 2016-04-13 | 2016-07-20 | 苏州伊飞特电子科技有限公司 | High flux environment-friendly tin wire and preparation method thereof |
| CN107498208A (en) * | 2017-08-24 | 2017-12-22 | 广东中实金属有限公司 | A kind of lead-free soldering wire for being applied to drag welding technology |
| CN108262577A (en) * | 2018-01-26 | 2018-07-10 | 东莞市固晶电子科技有限公司 | A kind of powder particle scaling powder and preparation method thereof |
| CN113677814A (en) * | 2019-04-11 | 2021-11-19 | 哈利玛化成株式会社 | Flux, solder paste, and electronic circuit board |
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Application publication date: 20120711 |