CN101104231A - Cleaning-free water base type scaling powder capable of restraining welding point interface compound growth - Google Patents
Cleaning-free water base type scaling powder capable of restraining welding point interface compound growth Download PDFInfo
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- CN101104231A CN101104231A CNA2007100093646A CN200710009364A CN101104231A CN 101104231 A CN101104231 A CN 101104231A CN A2007100093646 A CNA2007100093646 A CN A2007100093646A CN 200710009364 A CN200710009364 A CN 200710009364A CN 101104231 A CN101104231 A CN 101104231A
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Abstract
Disclosed is a cleaning-free water-based flux for constraining compound growth of solder joint interface, relating to a material for welding, in particular to a cleaning-free water- based flux that is used in the welding of micro-electronics and can constrain the compound growth of the solder joint interface. The invention provides a cleaning-free water-based flux, which can be effectively matched with solder without lead, with shiny welding points, good welding effect and good interface property, and can prevent the metal compound growth and constrain the compound growth of the solder joint interface. According to weight percent, the components are as following: organic reductant 0.1 percent to 0.3 percent; agent for constraining metal compound growth 0.01 percent to 1 percent; active organic manure 0.2 percent to 3 percent; surfactant 0.1 percent to 3 percent; corrosion inhibitor 0.1 percent; cosolvent 5 percent to 30 percent; the rest is water.
Description
Technical field
The present invention relates to a kind of material that is used to weld, especially relate to a kind of cleaning-free water base type scaling powder that is used for the suppressed welding point interface compound growth of microelectronics welding.
Background technology
Along with global problem of environmental pollution is increasingly serious, European Union has issued " waste electrical and electronic equipment (WEEE) " and " banning use of some harmful substance (RHOS) about electronic electric equipment " two decrees, from on July 1st, 2006, completely forbid leaded electronic product import.At present, mainly be to replace traditional SnPb alloy in the world, but the wetability of new alloy system is poorer than traditional SnPb alloy, easily oxidized with Sn-Ag and Sn-Ag-Cu eutectic system, the intermetallic compound undue growth at welding point interface place, welding back causes the solder joint mechanical performance to descend.Use traditional scaling powder, the welding effect extreme difference.
The more existing relevant reports of relevant lead-free solder soldering fluid.Publication number provides a kind of disposable film-formability water base type scaling powder for the application for a patent for invention of CN 1565791A.Contain by weight: 0.5%～8% water-soluble thermosetting resin, 0.5%～5% activator and 90%～99% deionized water, wherein activator is made up of surface active ingredient, organic acid and co-solvent.Be applied in the microelectronics welding production; can eliminate pollution and safety problem that organic type solvent scaling powder brings; can remove matting from again; and can form the water-insoluble film that one deck has certain adhesive force in PCB surface; play moistureproof damp proof protective effect, improved the insulation stability of electric equipment products effectively.The protection of use film forming, but must use a large amount of organic solvents to some oil-soluble macromolecule filmings, the easy moisture absorption of water soluble polymer film forming agent postwelding.Wherein a part just replaces to high boiling solvent with the solvent of traditional colophony type scaling powder, and the high-temperature operation with the adapted to leadless welding does not have great improvement on the whole, and is very poor to the welding effect of lead-free solder.Publication number provides a kind of water-soluble soldering flux dedicated for lead-free solder for the application for a patent for invention of CN1836825A, be made up of following weight percentage material: boric acid and organic acid for activating agent 5.0%～10.0%, non-ionic surface active agent or cationic surfactant 0.1%～1.0%, cosolvent 8.0%～20.0%, film forming agent 0.1%～1.0%, corrosion inhibiter 0.1%～0.5%, all the other are deionized water.This scaling powder does not contain rosin, non-halogen thing, environmental protection helps the weldering superior performance to lead-free solder, solder joint is full, sprawls evenly, corrode little, postwelding residue water soluble, after water cleans, dry copper coin, the surface insulation resistance of testing plank is all greater than 1.0 * 10
11Ω.Publication number provides a kind of cleaning-free lead-free solder soldering fluid for the Chinese patent of CN1562554, and it is made up of following materials by weight: organic acid for activating agent 1.0%～5.0%, improved resin 2.0%～8.0%, surfactant 0.2%～1.0%, high boiling solvent 2.0%～13.0%, wetting agent 1.0%～6.0%, all the other are solvent: isopropyl alcohol or deionized water.Use the bromide of nonionic covalent bond, welding back residue can cause bigger corrosivity.More existing scaling powders are only considered the spreadability problem of solder joint mostly, have ignored the compatibility of lead-free solder.Lead-free solder is after welding, and the intermetallic compound raised growth causes the solder joint mechanical performance to descend.The industrial nickel that plates 5～7 μ m thickness on copper base increases the mechanical performance of solder joint, but has increased the difficulty of cost and technology like this.
Summary of the invention
The objective of the invention is to characteristics at existing lead-free solder, provide a kind of lead-free solder that can effectively cooperate to use, the solder joint light can hinder the growth of intermetallic compound, the cleaning-free water base type scaling powder of the suppressed welding point interface compound growth that welding effect and interface performance are good.
Technical scheme of the present invention is directly from scaling powder, by scaling powder substrate is carried out surface modification, and diffusion suppresses to the atom between substrate and the scolder, thereby has hindered the growth of intermetallic compound.So both guarantee the good weldering performance that helps, improved the mechanical performance of solder joint again.
Composition of the present invention and content by mass percentage thereof are:
Organic reducing agent 0.1%～0.3% suppresses intermetallic compound growth agent 0.01%～1%, organic active agent 0.2%～3%, surfactant 0.1%～3%, corrosion inhibiter 0.1%, cosolvent 5%～30%, Yu Weishui.
The used organic reducing agent of the present invention is at least a in ascorbic acid, 4-hexyl resorcin, ascorbate, L-ascorbyl palmitate, arabo-ascorbic acid, phytic acid, Tea Polyphenols, vitamin E and the carrotene.
The used inhibition intermetallic compound growth agent of the present invention is the interface film forming agent, suppresses the intermetallic compound growth agent and be at least a among oxalic acid, ortho-aminobenzoic acid, oxine and the quinaldic acid.
The used organic active agent of the present invention does not comprise halogen, and by mass percentage, the organic active agent is made up of 50%～90% organic acid and 10%～50% organic amine.Organic acid mainly is at least a in aliphatic monoacid, aliphatic dibasic acid, aliphatic polyacid, tartaric acid, salicylic acid and the citric acid.Organic amine is hydramine, acid amides or fatty amine, and hydramine can be a kind of in monoethanolamine, diethanol amine and the triethanolamine etc., and acid amides is a urea, and fatty amine is the carbochain atomicity less than 12 monoamine or diamine; Organic amine also can be at least a in the three class amine.
The used surfactant of the present invention is a nonionic surface active agent, can be the OP series of surfactants, at least a in the TX series of surfactants, wherein with HMW and low-molecular-weight surfactant match be combined into good.
The used corrosion inhibiter of the present invention is a nitrogen-containing heterocycle compound.
The used cosolvent of the present invention is alcohol or the alcohol ether of boiling point more than 140 ℃, can be at least a in ethylene glycol, glycerine and the butyl glycol ether.
The present invention can adopt following method preparation: add cosolvent and water in having the reactor of agitator earlier, stir and add organic active agent, surfactant, corrosion inhibiter, the agent of inhibition intermetallic compound growth and reducing agent down, after be heated to 50～70 ℃, stir, leave standstill filtration, promptly get product of the present invention.
By the scaling powder of this method preparation, it helps the weldering performance can satisfy the J-STD-004 standard preferably.After the Sn3.5Ag0.5Cu scolder had welded, at 190 ℃ of 120h that anneal down, the thickness of the intermetallic compound of its boundary layer was 6.5～7.5 μ m, and the interface is also relatively milder, and the thickness of the intermetallic compounds layer of common scaling powder is 8～12 μ m.
Because the present invention adopts organic reducing agent, has antioxidation, therefore guaranteed the light of solder joint; Owing to suppress the adding of intermetallic compound growth agent, scolder with form one deck interface compound beds of precipitation at the interface, suppressed the atom diffusion of scolder and substrate, so hindered the growth of intermetallic compound; Owing to add the organic active agent, therefore can work to remove the copper coin surface film oxide; Because the adding of surfactant reduces the surface tension of solder metal and the surface energy of substrate, has therefore strengthened welding effect; Owing to add the stability that other cosolvents are regulated the boiling of welding process scaling powder, therefore guaranteed basic helping when welding performance, improved interface performance again.
The specific embodiment
Below in conjunction with embodiment the present invention is further detailed.
Embodiment 1: raw material is selected ascorbic acid 0.2g for use, oxalic acid 0.01g, adipic acid 1g, citric acid 0.5g, urea 0.5g, OP-10 0.1g, BTA 0.1g, ethylene glycol 15g, glycerine 5g, deionized water 77.6g.During preparation, in having the reactor of agitator, add cosolvent and deionized water earlier, stir the agent of adding organic active, surfactant, corrosion inhibiter, the agent of inhibition intermetallic compound growth and reducing agent down, after be heated to 60 ℃, stir, leave standstill filtration, promptly get scaling powder.The content of halogen of the scaling powder of gained＜0.01, the rate of spread 83.1%, aridity and copper coin corrosive nature are all qualified simultaneously.Do not have special odor when adopting this scaling powder welding and send, the solder joint surface-brightening uses the Sn3.5Ag0.5Cu scolder to weld, the intermetallic compounds layer thickness 7.4 μ m of 190 ℃ of 120h that anneal down.
Embodiment 2: raw material is selected L-ascorbyl palmitate 0.1g, oxalic acid 0.7g, oxine 0.3g, succinic acid 0.15g, triethanolamine 0.05g, T X-1002g, BTA 0.1g, ethylene glycol 30g, deionized water 66.6g for use.During preparation, in having the reactor of agitator, add cosolvent and deionized water earlier, stir the agent of adding organic active, surfactant, corrosion inhibiter, the agent of inhibition intermetallic compound growth and reducing agent down, after be heated to 50 ℃, stir, leave standstill filtration, promptly get scaling powder.After testing, the density of prepared scaling powder is 1.018g/L, content of halogen＜0.01, and the rate of spread 80.8%, aridity and copper coin corrosive nature are all qualified simultaneously.Do not have special odor when adopting this scaling powder welding and send, the solder joint surface-brightening uses the Sn3.5Ag0.5Cu scolder to weld, the intermetallic compounds layer thickness 7.0 μ m of 190 ℃ of 120 h that anneal down, and the interface is mild.
Embodiment 3: raw material is selected sodium ascorbate 0.3g for use, oxalic acid 0.1g, ortho-aminobenzoic acid 0.1g, acetate 0.1g, citric acid 0.5g, diethanol amine 0.1g, OP-10 1g, BTA 0.1g, glycerine 5g, deionized water 84.7g.During preparation, in having the reactor of agitator, add cosolvent and deionized water earlier, stir the agent of adding organic active, surfactant, corrosion inhibiter, the agent of inhibition intermetallic compound growth and reducing agent down, after be heated to 50 ℃, stir, leave standstill filtration, promptly get scaling powder.The content of halogen of prepared scaling powder＜0.01, the rate of spread 82.3%, aridity and copper coin corrosive nature are all qualified simultaneously.Do not have special odor when adopting this scaling powder welding and send, the solder joint surface-brightening uses the Sn3.5Ag0.5Cu scolder to weld, the intermetallic compounds layer thickness 7.1 μ m of 190 ℃ of 120h that anneal down.
Embodiment 4: raw material is selected 4-hexyl resorcin 0.1g, oxalic acid 0.01g, quinaldic acid 0.1g, succinic acid 1.4g, monoethanolamine 1.5g, OP-10 3g, BTA 0.1g, glycerine 3g, butyl glycol ether 10g, pure water 80.79g for use.During preparation, in having the reactor of agitator, add cosolvent and deionized water earlier, stir the agent of adding organic active, surfactant, corrosion inhibiter, the agent of inhibition intermetallic compound growth and reducing agent down, after be heated to 50 ℃, stir, leave standstill filtration, promptly get scaling powder.The content of halogen of prepared scaling powder＜0.01, the rate of spread 85.3%, aridity and copper coin corrosive nature are all qualified simultaneously.Do not have special odor when adopting this scaling powder welding and send, the solder joint surface-brightening uses the Sn3.5Ag0.5Cu scolder to weld, the intermetallic compounds layer thickness 7.5 μ m of 190 ℃ of 120h that anneal down.
Embodiment 5: raw material is selected arabo-ascorbic acid 0.1g for use, phytic acid 0.05g, oxalic acid 0.01g, quinaldic acid 0.1g, tartaric acid 1.4g, lauryl amine 1.5g, OP-4 0.5g, BTA 0.1g, glycerine 3g, ethylene glycol 10g, pure water 83.24g.During preparation, in having the reactor of agitator, add cosolvent and deionized water earlier, stir the agent of adding organic active, surfactant, corrosion inhibiter, the agent of inhibition intermetallic compound growth and reducing agent down, after be heated to 50 ℃, stir, leave standstill filtration, promptly get scaling powder.The content of halogen of prepared scaling powder＜0.01, the rate of spread 85.0%, aridity and copper coin corrosive nature are all qualified simultaneously.Do not have special odor when adopting this scaling powder welding and send, the solder joint surface-brightening uses the Sn3.5Ag0.5Cu scolder to weld, the intermetallic compounds layer thickness 7.2 μ m of 190 ℃ of 120h that anneal down.
Embodiment 6: raw material is selected Tea Polyphenols 0.1g for use, oxalic acid 0.05g, salicylic acid 0.4g, citric acid 0.8g, methylamine 1.5g, TX-100 0.5g, TX-10 0.5g, BTA 0.1g, glycerine 3g, ethylene glycol 10g, deionized water 83.05g.During preparation, in having the reactor of agitator, add cosolvent and deionized water earlier, stir the agent of adding organic active, surfactant, corrosion inhibiter, the agent of inhibition intermetallic compound growth and reducing agent down, after be heated to 70 ℃, stir, leave standstill filtration, promptly get scaling powder.The content of halogen of prepared scaling powder＜0.01, the rate of spread 82.8%, aridity and copper coin corrosive nature are all qualified simultaneously.Do not have special odor when adopting this scaling powder welding and send, the solder joint surface-brightening uses the Sn3.5Ag0.5Cu scolder to weld, the intermetallic compounds layer thickness 7.4 μ m of 190 ℃ of 120h that anneal down.
Embodiment 7: raw material is selected vitamin E 0.05g for use, carrotene 0.05g, oxalic acid 0.05g, formic acid 0.3g, succinic acid 0.8g, hexamethylene diamine 1g, OP-10 1g, BTA 0.1g, glycerine 3g, ethylene glycol 10g, deionized water 83.65g.During preparation, in having the reactor of agitator, add cosolvent and deionized water earlier, stir the agent of adding organic active, surfactant, corrosion inhibiter, the agent of inhibition intermetallic compound growth and reducing agent down, after be heated to 50 ℃, stir, leave standstill filtration, promptly get scaling powder.The content of halogen of prepared scaling powder＜0.01, the rate of spread 80.9%, aridity and copper coin corrosive nature are all qualified simultaneously.Do not have special odor when adopting this scaling powder welding and send, the solder joint surface-brightening uses the Sn3.5Ag0.5Cu scolder to weld, the intermetallic compounds layer thickness 7.4 μ m of 190 ℃ of 120h that anneal down.
Claims (10)
1. cleaning-free water base type scaling powder that can suppress welding point interface compound growth is characterized in that its composition and content by mass percentage thereof are:
Organic reducing agent 0.1%～0.3% suppresses intermetallic compound growth agent 0.01%～1%, organic active agent 0.2%～3%, surfactant 0.1%～3%, corrosion inhibiter 0.1%, cosolvent 5%～30%, Yu Weishui.
2. a kind of cleaning-free water base type scaling powder that suppresses welding point interface compound growth as claimed in claim 1 is characterized in that organic reducing agent is at least a in ascorbic acid, 4-hexyl resorcin, ascorbate, L-ascorbyl palmitate, arabo-ascorbic acid, phytic acid, Tea Polyphenols, vitamin E and the carrotene.
3. a kind of cleaning-free water base type scaling powder that suppresses welding point interface compound growth as claimed in claim 1 is characterized in that suppressing the intermetallic compound growth agent and is at least a among oxalic acid, ortho-aminobenzoic acid, oxine and the quinaldic acid.
4. a kind of cleaning-free water base type scaling powder that suppresses welding point interface compound growth as claimed in claim 1 is characterized in that by mass percentage, and the organic active agent is made up of 50%～90% organic acid and 10%～50% organic amine; Organic acid is at least a in aliphatic monoacid, aliphatic dibasic acid, aliphatic polyacid, tartaric acid, salicylic acid and the citric acid.
5. a kind of cleaning-free water base type scaling powder that suppresses welding point interface compound growth as claimed in claim 1, it is characterized in that organic amine is hydramine, acid amides or fatty amine, hydramine is selected from a kind of in monoethanolamine, diethanol amine and the triethanolamine, acid amides is a urea, and fatty amine is the carbochain atomicity less than 12 monoamine or diamine.
6. a kind of cleaning-free water base type scaling powder that suppresses welding point interface compound growth as claimed in claim 1 is characterized in that organic amine is at least a in the three class amine.
7. a kind of cleaning-free water base type scaling powder that suppresses welding point interface compound growth as claimed in claim 1, it is characterized in that surfactant is a nonionic surface active agent, be selected from the OP series of surfactants, at least a in the TX series of surfactants.
8. a kind of cleaning-free water base type scaling powder that suppresses welding point interface compound growth as claimed in claim 1 is characterized in that corrosion inhibiter is a nitrogen-containing heterocycle compound.
9. a kind of cleaning-free water base type scaling powder that suppresses welding point interface compound growth as claimed in claim 1 is characterized in that cosolvent is alcohol or the alcohol ether of boiling point more than 140 ℃.
10. a kind of cleaning-free water base type scaling powder that suppresses welding point interface compound growth as claimed in claim 9 is characterized in that described alcohol or alcohol ether are selected from least a in ethylene glycol, glycerine and the butyl glycol ether.
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| CNB2007100093646A CN100457375C (en) | 2007-08-11 | 2007-08-11 | Cleaning-free water base type scaling powder capable of restraining welding point interface compound growth |
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| CNB2007100093646A CN100457375C (en) | 2007-08-11 | 2007-08-11 | Cleaning-free water base type scaling powder capable of restraining welding point interface compound growth |
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| CN101104231A true CN101104231A (en) | 2008-01-16 |
| CN100457375C CN100457375C (en) | 2009-02-04 |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102357749A (en) * | 2011-10-18 | 2012-02-22 | 苏州之侨新材料科技有限公司 | Water-based halogen-free soldering flux used for lead-free soldering tin |
| CN103028868A (en) * | 2011-09-30 | 2013-04-10 | 罗门哈斯电子材料有限公司 | Polyamine, carboxylic acid flux composition and method of soldering |
| CN103286477A (en) * | 2013-05-22 | 2013-09-11 | 中南大学 | Soldering flux for lead-free solder and preparation method of soldering flux |
| CN103785975A (en) * | 2014-02-20 | 2014-05-14 | 苏州龙腾万里化工科技有限公司 | Soldering flux for improving corrosion inhibition |
| CN104139252A (en) * | 2014-06-24 | 2014-11-12 | 超威电源有限公司 | Flux for lead-acid battery |
| CN106041367A (en) * | 2016-07-14 | 2016-10-26 | 四川美亚达光电科技有限公司 | Soldering flux for light-emitting diode |
| 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 |
| CN108422127A (en) * | 2017-11-13 | 2018-08-21 | 天能集团（河南）能源科技有限公司 | A kind of aqueous scaling powder of lead-acid accumulator |
| CN108620764A (en) * | 2017-03-24 | 2018-10-09 | 苏州昭舜物联科技有限公司 | Low temperature solder connects with soldering paste and preparation method |
| CN109048122A (en) * | 2018-08-17 | 2018-12-21 | 佛山朝鸿新材料科技有限公司 | A kind of preparation method of the disposable flux material of high activity |
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| JPH0716787A (en) * | 1993-06-30 | 1995-01-20 | Taiyo Yuden Co Ltd | Solder paste |
| JPH10249581A (en) * | 1997-03-10 | 1998-09-22 | Jitsuo Adachi | Flux for welding, and coated electrode and flux-cared welding wire using the flux |
| CN100352598C (en) * | 2003-07-03 | 2007-12-05 | 梁树华 | Wash-free film forming water-based type welding flux |
| CN1290662C (en) * | 2004-03-30 | 2006-12-20 | 深圳市唯特偶化工开发实业有限公司 | Welding flux agent of solder with no lead and free from cleaning |
| US7378523B2 (en) * | 2005-08-25 | 2008-05-27 | National Starch And Chemical Investment Holding Corporation | Quinolinols as fluxing and accelerating agents for underfill compositions |
| CN100408257C (en) * | 2006-04-21 | 2008-08-06 | 北京工业大学 | Water-soluble soldering flux dedicated for lead-free solder |
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- 2007-08-11 CN CNB2007100093646A patent/CN100457375C/en not_active Expired - Fee Related
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| CN103028868B (en) * | 2011-09-30 | 2015-07-01 | 罗门哈斯电子材料有限公司 | Polyamine, carboxylic acid flux composition and method of soldering |
| CN103028868A (en) * | 2011-09-30 | 2013-04-10 | 罗门哈斯电子材料有限公司 | Polyamine, carboxylic acid flux composition and method of soldering |
| CN102357749A (en) * | 2011-10-18 | 2012-02-22 | 苏州之侨新材料科技有限公司 | Water-based halogen-free soldering flux used for lead-free soldering tin |
| CN103286477A (en) * | 2013-05-22 | 2013-09-11 | 中南大学 | Soldering flux for lead-free solder and preparation method of soldering flux |
| CN103785975A (en) * | 2014-02-20 | 2014-05-14 | 苏州龙腾万里化工科技有限公司 | Soldering flux for improving corrosion inhibition |
| CN104139252B (en) * | 2014-06-24 | 2016-03-02 | 超威电源有限公司 | A kind of lead-acid accumulator scaling powder |
| CN104139252A (en) * | 2014-06-24 | 2014-11-12 | 超威电源有限公司 | Flux for lead-acid battery |
| CN106041367A (en) * | 2016-07-14 | 2016-10-26 | 四川美亚达光电科技有限公司 | Soldering flux for light-emitting diode |
| CN108620764A (en) * | 2017-03-24 | 2018-10-09 | 苏州昭舜物联科技有限公司 | Low temperature solder connects with soldering paste and preparation method |
| CN108620764B (en) * | 2017-03-24 | 2022-03-08 | 苏州昭舜物联科技有限公司 | Soldering paste for low-temperature soldering and preparation method thereof |
| 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 |
| CN108422127A (en) * | 2017-11-13 | 2018-08-21 | 天能集团（河南）能源科技有限公司 | A kind of aqueous scaling powder of lead-acid accumulator |
| CN109048122A (en) * | 2018-08-17 | 2018-12-21 | 佛山朝鸿新材料科技有限公司 | A kind of preparation method of the disposable flux material of high activity |
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