CN105798482B - A kind of no-clean scaling powder of Halogen and preparation method thereof - Google Patents
A kind of no-clean scaling powder of Halogen and preparation method thereof Download PDFInfo
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- CN105798482B CN105798482B CN201610279314.9A CN201610279314A CN105798482B CN 105798482 B CN105798482 B CN 105798482B CN 201610279314 A CN201610279314 A CN 201610279314A CN 105798482 B CN105798482 B CN 105798482B
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- halogen
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/22—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by the composition or nature of the material
- B23K35/36—Selection 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/22—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by the composition or nature of the material
- B23K35/36—Selection 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
- B23K35/3612—Selection 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/40—Making wire or rods for soldering or welding
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- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Preventing Corrosion Or Incrustation Of Metals (AREA)
Abstract
The present invention provides the no-clean scaling powder of a kind of Halogen, including following component and mass percent thereof: activator 1～3%, film former 0.5～1.5%, cosolvent 20～35%, wetting agent 0.5～2%, water 60～72%；Described activator by organic acid and organic amine with (2～5): the mass ratio of 1 forms, described organic amine by diethanolamine and isophorone diamine with 1: the mass ratio of (3～8) forms.The invention belongs to scaling powder technical field, the present invention provide scaling powder can performance help weldering activity while avoid corrosion, and stability and wettability good, the consumption of activator is less, welding process is without splash phenomena, and the index such as the rate of spread of postwelding and surface insulation resistance is good.
Description
Technical field
The present invention relates to a kind of lead-free solder use scaling powder, particularly relate to a kind of Halogen no-clean scaling powder and
Preparation method.
Background technology
Along with the requirement of environmental protection, lead-free solder the most gradually replaces plumber's solder becomes the important materials of electronics industry.Unleaded
Solder has the advantages that fusing point is higher, oxidizable, wettability is poor, and fusing point height then welding temperature is high, thus brings scaling powder
Volatilization and loss are fast, cause scaling powder easily to lose efficacy, do not have good activation and protective effect.Therefore, tradition scaling powder without
Method meets the welding requirements of lead-free solder.
For lead-free solder, existing scaling powder mostly is organic solvent type scaling powder, the active component of the type scaling powder
Needing to dissolve in organic solvent, the consumption of organic solvent is big, and environmental benefit and safety are poor.If water base type scaling powder is complete
Entirely adopt and use water as solvent, owing to the boiling point of water is low, it is difficult to play the active effect of scaling powder, help it is thus typically necessary to add
Solvent.
The scaling powder of lead-free solder generally includes activator, film former, wetting agent, corrosion inhibiter, and each composition plays difference
Effect, but mutually influence.In scaling powder, play a crucial role is activator component, generally by organic acid and organic
Amine or organic amine hydrogen halogen composition, partial activation agents also includes surfactant, plays activity under certain welding temperature, with
The metal-oxide on lead-free solder surface reacts and then removes oxide film dissolving, ultimately forms good solder joint and realizes scaling powder
Effect.The activity of organic amine hydrogen halogen is high, has stronger oxide film dissolving ability, and prepared scaling powder welding effect is good, but
Have that postwelding halogen residue thing is many, corrode more serious shortcoming, easily bring potential safety hazard to welding product.Organic acid relies on it
The advantage of high reliability is widely deployed in the preparation of halogen-free scaling powder, but the more weak activity of organic acid is still not enough to fill
The oxide dividing ground to remove lead-free solder surface reaches moistening and requires and form solid and reliable solder joint, therefore, generally by organic
Acid and organic amine combine as activator.But the addition of organic acid easily brings the problem of corrosion, therefore in scaling powder often
Need to add corrosion inhibiter.
Chinese patent application 201310194831.2 discloses a kind of lead-free solder scaling powder, including: activator, surface
Activating agent, film former, cosolvent, corrosion inhibiter and deionized water；Activator is with 4.5: 1～8: 1 by organic acid and organic amine
Mass ratio mixing mixture, organic amine is hydramine, selected from diethanolamine, triethanolamine, triethylamine.This scaling powder is water base
Type cosolvent, Halogen, reach No clean requirement, but need to use corrosion inhibiter, and stability is not ideal enough.
Summary of the invention
For solving problems of the prior art, composition and the consumption of activator are carried out by inventor by lot of experiments
Screening, unforeseeable discovery: by optimizing the component of organic amine, prepared scaling powder can be while performance helps weldering activity
Avoid corrosion, it is not necessary to add corrosion inhibiter, cost is relatively low, and stability and wettability good, the consumption of activator is less, solid content
Low, welding process is without splash phenomena, and the index such as the rate of spread of postwelding and surface insulation resistance is good.Based on above-mentioned discovery, thus
Complete the present invention.
The purpose of the present invention will be further illustrated by explained below.
The present invention provides the no-clean scaling powder of a kind of Halogen, including following component and mass percent thereof: activator 1～
3%, film former 0.5～1.5%, cosolvent 20～35%, wetting agent 0.5～2%, water 60～72%；Described activator is by having
Machine acid and organic amine are with (2～5): the mass ratio of 1 composition, described organic amine by diethanolamine and isophorone diamine with 1: (3～
8) mass ratio composition.
The combination of said components and the mass percent of each component, be that inventor is determined by lot of experiments, makes this
The scaling powder that invention provides has excellent performance.Isophorone diamine, is called for short IPDA, and chemical-resistance is excellent, is mainly used as
The firming agent of epoxy resin, coating crosslinking agent etc..Inventor is found by lot of experiments: by diethanolamine and isophorone diamine
By certain mass than mixing as organic amine, having excellent thermostability, the compatibility with other compositions such as cosolvent is good, in weldering
Termination process helps weldering activity volatilize by force and gradually, play the effect of corrosion inhibiter (avoiding corrosion), thus without adding in scaling powder
Add corrosion inhibiter, noresidue after welding.The binary such as resorcylic acid or multi-hydroxy carboxylic acid and above-mentioned organic amine with the use of, can
It is effective against reoxidizing of metal coating, promotes sprawling of lead-free solder.
Preferably, described water is deionized water.
Preferably, described activator is made up of with the mass ratio of 3: 1 organic acid and organic amine, and described organic amine is by diethanol
Amine and isophorone diamine form with the mass ratio of 1: 4.When the mass ratio of diethanolamine and isophorone diamine is beyond 1: (3～
8), when quality is than scope, weldering effect and stabilizing effect is helped to be deteriorated.
Preferably, described organic acid selected from resorcylic acid, dihydroxyphenyl acetic acid, malic acid, citric acid, malonic acid,
At least two in succinic acid, 1,3-propanedicarboxylic acid, adipic acid and dimer (fatty acid) yl.
It is highly preferred that described organic acid is made up of with the mass ratio of 2: 1: 1 resorcylic acid, malonic acid and 1,3-propanedicarboxylic acid.
Preferably, described cosolvent is made up of high boiling point cosolvent and low boiling cosolvent；Described high boiling point cosolvent selects
At least one in glycerol and diethylene glycol；Described low boiling cosolvent is selected from ethylene glycol, propylene glycol, butyl glycol ether and four
At least one in hydrogen furfuryl alcohol.High boiling solvent and low boiling point solvent are used in mixed way as cosolvent by the present invention, can be formed relatively
Wide boiling spread is to adapt to the variations in temperature of whole welding process so that under welding temperature, the solvent carrier of different boiling in
Stepped vapor away, it is ensured that activator gives full play to activity.
It is highly preferred that described high boiling point cosolvent is selected from butyl glycol ether selected from glycerol, described low boiling cosolvent.
Preferably, described wetting agent is in ethyl acetate, diethyl succinate, ethyl benzoate and polyatomic alcohol mixing ester
At least one.
Preferably, described film former is selected from Polyethylene Glycol, polyacrylic acid, carboxymethyl cellulose and polyvinyl pyrrolidone
In at least one.
Correspondingly, present invention also offers the preparation method of the no-clean scaling powder of Halogen, comprise the steps:
Organic acid, organic amine are added dissolving in part water by S1, obtain activating mixtures, standby；Described organic amine by
Diethanolamine and isophorone diamine are with 1: the mass ratio composition of (3～8)；
Cosolvent, wetting agent and excess water are mixed by S2, are heated to 40～50 DEG C, add film former, stirring, dissolve completely
After, cooling, add described activating mixtures, mixing, stand and filter, obtain scaling powder.
Preferably, described activator is made up of with the mass ratio of 3: 1 organic acid and organic amine, and described organic amine is by diethanol
Amine and isophorone diamine form with the mass ratio of 1: 4.
Compared with prior art, the invention has the beneficial effects as follows: the scaling powder water white transparency that the present invention provides, without halogen
Composition, without Colophonium composition, cost is relatively low, by organic acid and the synergism of organic amine, while performance helps weldering activity
Avoid corrosion, it is not necessary to adding corrosion inhibiter, stability and wettability are good, and the consumption of activator is less, and solid content is low, welding process
Without splash phenomena, the index such as the rate of spread of postwelding and surface insulation resistance is good.Use the scaling powder that the present invention provides to unleaded
After solder welding, the full light of pad surface, noresidue, reach the degree of No clean, corrosion-free, the rate of spread is up to 84.1%,
Surface insulation resistance is up to 5.2 × 1011Ω, stability, corrosion testing are the most qualified, and the welding that can meet various lead-free solder is wanted
Ask.
Detailed description of the invention
Below by specific embodiment, the present invention is described in further detail.
The no-clean scaling powder of embodiment one Halogen
A kind of no-clean scaling powder of Halogen, including following component and mass fraction thereof: 2,6-DHBA 1 part,
Malonic acid 0.5 part, 1,3-propanedicarboxylic acid 0.5 part, diethanolamine 0.13 part, isophorone diamine 0.53 part, PEG-4000 1 part, third
Triol 16 parts, butyl glycol ether 12 parts, ethyl benzoate 1 part, deionized water 67.33 parts.
Preparation method: resorcylic acid, malonic acid, 1,3-propanedicarboxylic acid, diethanolamine, isophorone diamine addition part are gone
Ionized water dissolves, obtains activating mixtures, standby；By glycerol, butyl glycol ether, ethyl benzoate and remaining go from
Sub-water mixes, and is heated to 45 DEG C, adds PEG-4000, stirring, after dissolving completely, is cooled to room temperature, adds described activation
Agent composition, mixing, stand and filter, obtain scaling powder.
The no-clean scaling powder of embodiment two Halogen
A kind of no-clean scaling powder of Halogen, including following component and mass fraction thereof: 2,6-DHBA 1 part,
Succinic acid 1 part, diethanolamine 0.2 part, isophorone diamine 0.8 part, polyacrylic acid 0.5 part, diethylene glycol 16 parts, butyl glycol ether
12 parts, ethyl acetate 1 part, deionized water 67.5 parts.
Preparation method: similar with embodiment one.
The no-clean scaling powder of embodiment three Halogen
The no-clean scaling powder of a kind of Halogen, including following component and mass fraction thereof: DL-malic acid 1 part, 1,3-propanedicarboxylic acid
0.5 part, 2,6-DHBA 0.3 part, diethanolamine 0.1 part, isophorone diamine 0.5 part, carboxymethyl cellulose 1 part,
Glycerol 16 parts, ethylene glycol 12 parts, polyatomic alcohol mixing ester (DBE) 1 part, ethyl acetate 0.5 part, deionized water 67.1 parts.
Preparation method: similar with embodiment one.
The no-clean scaling powder of comparative example one Halogen
A kind of no-clean scaling powder of Halogen, including following component and mass fraction thereof: 2,6-DHBA 1 part,
Malonic acid 0.5 part, 1,3-propanedicarboxylic acid 0.5 part, diethanolamine 0.66 part, PEG-4000 1 part, glycerol 16 parts, butyl glycol ether
12 parts, ethyl benzoate 1 part, deionized water 67.33 parts.
Preparation method: similar with embodiment one.
The present embodiment is with the difference of embodiment one: without isophorone diamine in organic amine.
The no-clean scaling powder of comparative example two Halogen
A kind of no-clean scaling powder of Halogen, including following component and mass fraction thereof: 2,6-DHBA 1 part,
Malonic acid 0.5 part, 1,3-propanedicarboxylic acid 0.5 part, isophorone diamine 0.66 part, PEG-4000 1 part, glycerol 16 parts, ethylene glycol
Butyl ether 12 parts, ethyl benzoate 1 part, deionized water 67.33 parts.
Preparation method: similar with embodiment one.
The present embodiment is with the difference of embodiment one: without diethanolamine in organic amine.
The no-clean scaling powder of comparative example three Halogen
A kind of no-clean scaling powder of Halogen, including following component and mass fraction thereof: 2,6-DHBA 1 part,
Malonic acid 0.5 part, 1,3-propanedicarboxylic acid 0.5 part, diethanolamine 0.33 part, isophorone diamine 0.33 part, PEG-4000 1 part, third
Triol 16 parts, butyl glycol ether 12 parts, ethyl benzoate 1 part, deionized water 67.33 parts.
Preparation method: similar with embodiment one.
The present embodiment is with the difference of embodiment one: in organic amine, the mass ratio of diethanolamine and isophorone diamine is
1∶1。
The performance test example of scaling powder
The scaling powder preparing embodiment one, embodiment two, comparative example one, comparative example two and comparative example three, according to " SJ/T
11389-2009 pb-free solder scaling powder " and " SJ/T 11273-2002 No clean liquid scaling powder " carry out performance detection, knot
Fruit is as shown in table 1.
The test result of table 1 scaling powder
As known from Table 1, the scaling powder various aspects of performance that the present invention provides is good, and wherein the rate of spread of embodiment one is up to
84.1%, surface insulation resistance is up to 5.2 × 1011Ω, therefore embodiment one is highly preferred embodiment of the present invention.Comparative example one,
Comparative example two and comparative example three provide not as the present invention at aspects such as corrosivity, splashing characteristic, surface insulation resistance, stability
Embodiment one and embodiment two.Visible, diethanolamine and isophorone diamine are remarkably improved than combination with specified weight and help weldering
The effect of agent.
Above content is to combine concrete preferred implementation further description made for the present invention, it is impossible to assert
Being embodied as of the present invention is confined to these explanations.For general technical staff of the technical field of the invention,
On the premise of present inventive concept, it is also possible to make some simple deduction or replace, all should be considered as belonging to the present invention's
Protection domain.
Claims (10)
1. the no-clean scaling powder of a Halogen, it is characterised in that: include the component of following mass percent: activator 1～
3%, film former 0.5～1.5%, cosolvent 20～35%, wetting agent 0.5～2%, water 60～72%；Described activator is by having
Machine acid and organic amine are with (2～5): the mass ratio of 1 composition, described organic amine by diethanolamine and isophorone diamine with 1:(3～
8) mass ratio composition.
The no-clean scaling powder of Halogen the most according to claim 1, it is characterised in that: described activator is by organic acid and has
Machine amine forms with the mass ratio of 3:1, and described organic amine is made up of with the mass ratio of 1:4 diethanolamine and isophorone diamine.
The no-clean scaling powder of Halogen the most according to claim 1, it is characterised in that: described organic acid is selected from dihydroxy benzenes
In formic acid, dihydroxyphenyl acetic acid, malic acid, citric acid, malonic acid, succinic acid, 1,3-propanedicarboxylic acid, adipic acid and dimer (fatty acid) yl extremely
Few two kinds.
The no-clean scaling powder of Halogen the most according to claim 3, it is characterised in that: described organic acid is by dihydroxy benzenes first
Acid, malonic acid and 1,3-propanedicarboxylic acid form with the mass ratio of 2:1:1.
The no-clean scaling powder of Halogen the most according to claim 1, it is characterised in that: described cosolvent is by high boiling point hydrotropy
Agent and low boiling cosolvent composition；At least one in glycerol and diethylene glycol of described high boiling point cosolvent；Described low boiling
At least one in ethylene glycol, propylene glycol, butyl glycol ether and tetrahydrofurfuryl alcohol of some cosolvent.
The no-clean scaling powder of Halogen the most according to claim 5, it is characterised in that: described high boiling point cosolvent is selected from third
Triol, described low boiling cosolvent is selected from butyl glycol ether.
The no-clean scaling powder of Halogen the most according to claim 1, it is characterised in that: described wetting agent is selected from acetic acid second
At least one in ester, diethyl succinate, ethyl benzoate and polyatomic alcohol mixing ester.
The no-clean scaling powder of Halogen the most according to claim 1, it is characterised in that: described film former is selected from poly-second two
At least one in alcohol, polyacrylic acid, carboxymethyl cellulose and polyvinyl pyrrolidone.
9. the preparation method of the no-clean scaling powder of a Halogen as claimed in claim 1, it is characterised in that: include walking as follows
Rapid:
Organic acid, organic amine are added dissolving in part water by S1, obtain activating mixtures, standby；
Cosolvent, wetting agent and excess water are mixed by S2, are heated to 40～50 DEG C, add film former, stir, after dissolving completely,
Cooling, adds described activating mixtures, mixing, stands and filters, obtains scaling powder.
The preparation method of the no-clean scaling powder of Halogen the most according to claim 9, it is characterised in that: described activator
Be made up of with the mass ratio of 3:1 organic acid and organic amine, described organic amine by diethanolamine and isophorone diamine with the matter of 1:4
Amount is than composition.
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| CN106271219A (en) * | 2016-08-26 | 2017-01-04 | 王泽陆 | A kind of No clean high-temperature electronic brazing flux and preparation method thereof |
| CN106392377A (en) * | 2016-10-07 | 2017-02-15 | 常州市鼎升环保科技有限公司 | Preparation method for washing-free scaling powder |
| CN107498214B (en) * | 2016-11-29 | 2019-06-14 | 广东剑鑫科技股份有限公司 | Dedicated cleaning-free scaling powder of the outer PIN of network transformer and preparation method thereof |
| CN106392378A (en) * | 2016-12-06 | 2017-02-15 | 周潇潇 | Environment-friendly scaling powder |
| CN107962318A (en) * | 2017-12-01 | 2018-04-27 | 苏州市宽道模具机械有限公司 | A kind of scaling powder and preparation method thereof |
| CN109940311A (en) * | 2017-12-20 | 2019-06-28 | 海太半导体（无锡）有限公司 | A kind of low-temperature catalyzed scaling powder |
| CN108817733A (en) * | 2018-08-31 | 2018-11-16 | 安徽红桥金属制造有限公司 | A kind of halogen-free scaling powder and preparation method thereof |
| CN113199170B (en) * | 2021-04-25 | 2022-10-25 | 江苏海瑞电源有限公司 | Gel type storage battery soldering flux and preparation method thereof |
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| US5334260B1 (en) * | 1993-02-05 | 1995-10-24 | Litton Systems Inc | No-clean, low-residue, volatile organic conpound free soldering flux and method of use |
| US5443660A (en) * | 1994-10-24 | 1995-08-22 | Ford Motor Company | Water-based no-clean flux formulation |
| CN1233499C (en) * | 2002-10-18 | 2005-12-28 | 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 |
| CN100496867C (en) * | 2007-05-11 | 2009-06-10 | 北京工业大学 | Cleaning-free soldering flux without halogen and rosin for solder without lead |
| CN101327552A (en) * | 2008-07-31 | 2008-12-24 | 东莞永安科技有限公司 | Low solid content halogenide-free water-based type cleaning-free scaling powder |
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