CN102554489A - Low-rosin halogen and lead-free solder paste and preparation method thereof - Google Patents

Low-rosin halogen and lead-free solder paste and preparation method thereof Download PDF

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CN102554489A
CN102554489A CN2011104591632A CN201110459163A CN102554489A CN 102554489 A CN102554489 A CN 102554489A CN 2011104591632 A CN2011104591632 A CN 2011104591632A CN 201110459163 A CN201110459163 A CN 201110459163A CN 102554489 A CN102554489 A CN 102554489A
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acid
halogen
percentage
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soldering tin
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潘惠凯
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NINGBO SHENGZHIDAO SOLDER MATERIAL CO Ltd
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NINGBO SHENGZHIDAO SOLDER MATERIAL CO Ltd
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Abstract

The invention relates to solder paste for welding electronic devices, in particular to low-rosin halogen and lead-free solder paste and a preparation method of the low-rosin halogen and lead-free solder paste. The low-rosin halogen and lead-free solder paste is composed of solder powder and an soldering flux, wherein the weight percentage of the solder powder is 88-90 percent; the weight percentage of the soldering flux is 10-12 percent; and the solder powder consists of the following components by weight percent: 95.3-97% of Sn, 2-2.5% of Ag, 0.5-1.5% of Zn and 0.5-0.7% of Cu. The solder paste does not contain lead or halogen, is beneficial for environmental protection, and can not damage the atmospheric layer, the heavy pollution to the environment is greatly reduced, the residual solder waste after welding is little, the solder paste is colourless and transparent, has stable performance under normal temperature, can not absorb moisture, does not contain halogen, has no corrosion after welding, is particularly suitable for the no-clean operation, and better conforms with the environmental protection requirements.

Description

A kind of low rosin halogen leadless soldering tin paste and preparation method thereof
Technical field
The present invention relates to a kind of solder(ing) paste that welds electronic installation, refer in particular to a kind of low rosin halogen leadless soldering tin paste and preparation method thereof.
Background technology
Traditional solder(ing) paste is made up of leypewter solder powder and scaling powder; Wherein the tin proportion of gold alloy solder glass putty is 63: 37; The spheric granules size is 25-45um, and scaling powder is made up of modified rosin resin, high medium-boiling solvent, thixotropic agent, activating agent, antioxidant preservative and other additive.In recent years; Because of traditional solder(ing) paste leaded; Harm environment and health are progressively banned use of, and leadless soldering tin paste has replaced traditional tin lead welding tin cream; Traditional in the market leadless soldering tin paste mainly contains Sn-Ag-Cu alloy, Sn-Ag alloy, Sn-Ag-Bi alloy, Sn-Bi alloy, Sn-Sb alloy but every kind of scolder all has certain limitation, can not reach ideal effect simultaneously at welding temperature/mechanical strength/aspects such as wetability/ageing resistance.Traditional solder(ing) paste film forming agent adopts the rosin synthetic mostly, and solvent adopts single high boiling solvent, makes that tin cream postwelding surface residue is more, influence outside and postwelding performance.What activating agent adopted is the halogen product, has destroyed atmospheric ozone layer, and has influenced the stability of postwelding product.
Summary of the invention
The technical problem that one, will solve
The objective of the invention is to solve that present lead-free solder paste postwelding residue is too high, the characteristics of combination property difference, solve present leadless soldering tin paste especially and contain halogen mostly, ozone layer is had the shortcoming of destruction.This type of solder(ing) paste postwelding residue is few, and is water white transparency, and stable performance under the normal temperature is nonhygroscopic, and halogen is added, and postwelding does not have corrosion, is specially adapted to exempt from cleaning operation, more compliance with environmental protection requirements.
Two, the technical scheme for solving the problems of the technologies described above
For solving the problems of the technologies described above, a kind of low rosin halogen leadless soldering tin paste of the present invention wherein, is made up of solder powder and scaling powder;
The percentage by weight of above-mentioned solder powder is 88~90%;
The percentage by weight of above-mentioned scaling powder is 10~12%;
Above-mentioned solder powder is by S n, A g, Z nAnd C uForm, its percentage by weight is followed successively by S nBe 95.3~97%, A gBe 2~2.5%, Z nBe 0.5~1.5% and C uBe 0.5~0.7%.
As optimization, above-mentioned scaling powder is that 8~15% organic acid for activating agent, percentage by weight are that 25~35% film forming agent, percentage by weight are that 6~10% thixotropic agent, percentage by weight are that 3~5% surfactant, percentage by weight are that 5~10% acid number conditioning agent, percentage by weight are that 2~3% lubrication humectant, percentage by weight are that 1~2% anti-oxidant and percentage by weight are 40~50% solvent composition by percentage by weight.
As optimization, above-mentioned organic acid for activating agent is one or more mixing in aliphatic, succinic acid, adipic acid, decanedioic acid, glutaric acid, itaconic acid, salicylic acid, dodecoic acid, tetradecylic acid, hexadecylic acid, stearic acid, tartaric acid, the DL-malic acid.This type of activator is heated and reaches the oxide that can remove solder surface after the uniform temperature rapidly, can decompose preferably again, reduces the corrosivity of postwelding, reaches good postwelding effect.
As optimization, above-mentioned aliphatic includes monoacid, binary acid, carboxylic acid.
As optimization, above-mentioned film forming agent is one or more mixing in celluosic resin, modified rosin, polyethylene glycol, the acrylic resin.The effect of film forming agent is to make tin cream generation viscosity and provide protective layer anti-oxidant.
As optimization, above-mentioned thixotropic agent is a rilanit special.The effect of thixotropic agent is the flowability that increases lotion, makes its thinning flowing under external force is sheared, and under static state can keep stable state, improves the printing and the demoulding property of tin cream.
As optimization, above-mentioned surfactant is one or more mixing in NPE, Brij, the diethylene glycol (DEG) APEO.This type of material can improve the scolding tin wetting power, reduces the surface tension of molten tin.
As optimization, above-mentioned acid number conditioning agent is one or more mixing in 12 diamines, triethanolamine, diethanol amine, the oleamide.Produce generation salt with the solder flux middle acid substance in this type of material ability, reduce corrosivity, in heating process, resolve into acid and organic amine again, improve and help the weldering performance.
As optimization, above-mentioned lubrication humectant is one or more mixing in propane diols, glycerine, the paraffin.This type of material mainly is to keep tin cream moistening, makes its not volatile exsiccation, increases the service life.
As optimization, above-mentioned anti-oxidant is one or more mixing among imidazoles, BTA, the BHT.Can effectively suppress activating agent, increase the service life corrosion of metal
As optimization, above-mentioned solvent is the multiple mixing in diglycol monotertiary octyl ether, diethylene glycol dibutyl ether, diethylene glycol monobutyl ether, phenmethylol, propane diols phenylate, the butyl glycol ether.The solvent of multiple different boiling can guarantee that solvent is effectively volatilized under different temperature, be more suitable for tin cream reflow soldering curve.
The present invention also provides a kind of preparation method of low rosin halogen leadless soldering tin paste:
Steps A: make solder powder:
A, with S n, A g, Z nAnd C uBe smelted into mixture;
B, with the said mixture centrifugal atomizing, obtain powdery granule;
C, filter out the powdery granule that size is 25~38um;
Step B: make scaling powder:
A, elder generation add heating for dissolving in the solvent with film forming agent, become mixed liquor;
B, in mixed liquor, add organic acid for activating agent, thixotropic agent, acid number conditioning agent, surfactant successively, apply out solvent;
C, mixed liquor is placed cooling;
Add acid number conditioning agent, lubrication humectant, anti-oxidant in d, the mixed liquor after cooling, stir and cooling;
E, cooled mixed liquor is refrigerated twenty four hours, subsequent use;
Step C: with solder powder and scaling powder according to 88~90: 12~10 mixed also stirs, and forms solder(ing) paste after the extracting vacuum.
Three, beneficial effect of the present invention
The not leaded and halogen of solder(ing) paste of the present invention helps environmental protection, and can not damage atmosphere; A huge sum of money that also greatly reduces environment pollutes, and solder(ing) paste postwelding residue of the present invention is few, and is water white transparency; Stable performance under the normal temperature, nonhygroscopic, halogen is added; Postwelding does not have corrosion, is specially adapted to exempt from cleaning operation, more compliance with environmental protection requirements.Film forming agent of the present invention is that multiple modified fibre resin is synthetic, is prone to decompose, and resistance to oxidation, what activating agent adopted is the composite side's surfactant system of halogen, has improved reliability of products and environmental standard greatly.
Description of drawings
Fig. 1 is a solder(ing) paste preparation method's of the present invention process chart.
The specific embodiment
Embodiment one:
Solder powder: S n, A g, Z n, C uFour kinds of materials are according to 95.8% S n, 2% A g, 1.5% Z n, 0.7%. C uMelting mixes, and centrifugal atomizing, filters out the powder of 25-38um particle.
The percentage by weight of scaling powder is:
Film forming agent contains 30%: wherein, contain 15% celluosic resin, 10% modified rosin, 5% polyethylene glycol;
The organic acid for activating agent contains 10%: wherein, contain 4% succinic acid, 4% adipic acid, 2% itaconic acid;
Surfactant contains 4%: wherein, contain 4% NPE;
Thixotropic agent contains 6%: wherein, contain 6% rilanit special;
The acid number conditioning agent contains 5%: wherein, contain 3% diethanol amine, 2% oleamide;
Lubrication humectant contains 3%: wherein, containing 3% has paraffin;
Anti-oxidant contains 2%: wherein, contain 2% BTA;
Solvent contains 40%: wherein, contain 15% propane diols phenylate, 5% butyl glycol ether, 15% diglycol monotertiary octyl ether, 5% phenmethylol.
Earlier celluosic resin, modified rosin, polyethylene glycol are added heating for dissolving in diglycol monotertiary octyl ether, propane diols phenylate, butyl glycol ether, the phenmethylol; Add succinic acid, adipic acid, itaconic acid, rilanit special, oleamide, Nonyl pheno alcohol more successively, apply out solvent, place again and cool to 130 degree; Add diethanol amine, paraffin, BTA again; After stirring cooling, put into refrigerating box refrigeration twenty four hours again after, take out and use.
Solder powder and scaling powder are stirred by 90: 10 mixed, just form moist solder(ing) paste after the extracting vacuum, its specification is following:
Figure BDA0000127933470000051
Embodiment two:
Solder powder: S n, A g, Z n, C uFour kinds of materials are according to 95.8% S n, 2% A g, 1.5% Z n, 0.7%. C uMelting mixes, and centrifugal atomizing, filters out the powder of 25-38um particle.
The percentage by weight of scaling powder is:
Film forming agent contains 35%: wherein, contain 15% celluosic resin, 10% modified rosin, 5% polyethylene glycol, 5% acrylic resin;
The organic acid for activating agent contains 8%: wherein, contain 4% glutaric acid, 4% decanedioic acid;
Surfactant contains 3%: wherein, contain 3% diethylene glycol (DEG) APEO;
Thixotropic agent contains the rilanit special of 6%:6%;
The acid number conditioning agent contains 5%: wherein, contain 4% triethanolamine, 1% oleamide;
Lubrication humectant contains 2%: wherein, contain 2% glycerine;
Anti-oxidant contains 1%: wherein, contain 1% BHT;
Solvent contains 40%: wherein, contain 15% propane diols phenylate, 5% butyl glycol ether, 15% diethylene glycol monobutyl ether, 5% phenmethylol;
Earlier celluosic resin, modified rosin, polyethylene glycol, acrylic resin are added heating for dissolving in diethylene glycol monobutyl ether, propane diols phenylate, butyl glycol ether, the phenmethylol; Add glutaric acid, decanedioic acid, rilanit special, oleamide, diethylene glycol (DEG) APEO more successively, apply out solvent, place again and cool to 130 degree; Add triethanolamine, glycerine, BHT again; After stirring cooling, put into refrigerating box refrigeration twenty four hours again after, take out and use.
Solder powder and scaling powder stir by 88: 12 mixed, just form moist solder(ing) paste after the extracting vacuum, and its specification is following:
Figure BDA0000127933470000061
Embodiment three:
Solder powder: S n, A g, Z n, C uFour kinds of materials are according to 96.3% S n, 2.5% A g, 0.5% Z n, 0.7%. C uMelting mixes, and centrifugal atomizing, filters out the powder of 25-38um particle.
The percentage by weight of scaling powder is:
Film forming agent contains 25%: wherein, contain 10% celluosic resin, 10% modified rosin, 5% polyethylene glycol;
The organic acid for activating agent contains 8%: wherein, contain 4% succinic acid, 4% DL-malic acid;
Surfactant contains 3%: wherein, contain 3% Brij;
Thixotropic agent contains 6%: wherein, contain 6% rilanit special;
The acid number conditioning agent contains 5%: wherein, contain 4% triethanolamine, 1% oleamide;
Lubrication humectant contains 2%: wherein, contain 2% propane diols;
Anti-oxidant contains 1%: wherein, contain 1% imidazoles;
Solvent contains 50%: wherein, contain 15% propane diols phenylate, 15% butyl glycol ether, 15% diethylene glycol monobutyl ether, 5% phenmethylol;
Earlier celluosic resin, modified rosin, polyethylene glycol are added heating for dissolving in diethylene glycol monobutyl ether, propane diols phenylate, butyl glycol ether, the phenmethylol; Add succinic acid, DL-malic acid, rilanit special, oleamide, Brij more successively, apply out solvent, place again and cool to 130 degree; Add triethanolamine, propane diols, imidazoles again; After stirring cooling, put into refrigerating box refrigeration twenty four hours again after, take out and use.
Scaling powder and solder powder stir by 11: 89 mixed, just form moist solder(ing) paste after the extracting vacuum, and its specification is following:
Figure BDA0000127933470000081

Claims (12)

1. one kind low rosin halogen leadless soldering tin paste is characterized in that: be made up of solder powder and scaling powder;
The percentage by weight of said solder powder is 88~90%;
The percentage by weight of said scaling powder is 10~12%;
Said solder powder is by S n, A g, Z nAnd the Cu composition, its percentage by weight is followed successively by S nBe 95.3~97%, A gBe 2~2.5%, Z nBe 0.5~1.5% and C uBe 0.5~0.7%.
2. low rosin halogen leadless soldering tin paste according to claim 1 is characterized in that: said scaling powder is that 8~15% organic acid for activating agent, percentage by weight are that 25~35% film forming agent, percentage by weight are that 6~10% thixotropic agent, percentage by weight are that 3~5% surfactant, percentage by weight are that 5~10% acid number conditioning agent, percentage by weight are that 2~3% lubrication humectant, percentage by weight are that 1~2% anti-oxidant and percentage by weight are 40~50% solvent composition by percentage by weight.
3. low rosin halogen leadless soldering tin paste according to claim 2 is characterized in that: said organic acid for activating agent is one or more mixing in aliphatic, succinic acid, adipic acid, decanedioic acid, glutaric acid, itaconic acid, salicylic acid, dodecoic acid, tetradecylic acid, hexadecylic acid, stearic acid, tartaric acid, the DL-malic acid.
4. low rosin halogen leadless soldering tin paste according to claim 3, it is characterized in that: said aliphatic includes monoacid, binary acid, carboxylic acid.
5. low rosin halogen leadless soldering tin paste according to claim 2 is characterized in that: said film forming agent is one or more mixing in celluosic resin, modified rosin, polyethylene glycol, the acrylic resin.
6. low rosin halogen leadless soldering tin paste according to claim 2, it is characterized in that: said thixotropic agent is a rilanit special.
7. low rosin halogen leadless soldering tin paste according to claim 2 is characterized in that: said surfactant is one or more mixing in NPE, Brij, the diethylene glycol (DEG) APEO.
8. low rosin halogen leadless soldering tin paste according to claim 2 is characterized in that: said acid number conditioning agent is one or more mixing in 12 diamines, triethanolamine, diethanol amine, the oleamide.
9. low rosin halogen leadless soldering tin paste according to claim 2 is characterized in that: said lubrication humectant is one or more mixing in propane diols, glycerine, the paraffin.
10. low rosin halogen leadless soldering tin paste according to claim 2 is characterized in that: said anti-oxidant is one or more mixing among imidazoles, BTA, the BHT.
11. low rosin halogen leadless soldering tin paste according to claim 2 is characterized in that: said solvent is the multiple mixing in diglycol monotertiary octyl ether, diethylene glycol dibutyl ether, diethylene glycol monobutyl ether, phenmethylol, propane diols phenylate, the butyl glycol ether.
12. the preparation method of one kind low rosin halogen leadless soldering tin paste is characterized in that:
Steps A: make solder powder:
A, with S n, A g, Z nAnd C uBe smelted into mixture;
B, with said mixture centrifugal atomizing, obtain powdery granule;
C, filter out the powdery granule that size is 25~38um;
Step B: make scaling powder:
A, elder generation add heating for dissolving in the solvent with film forming agent, become mixed liquor;
B, in mixed liquor, add organic acid for activating agent, thixotropic agent, acid number conditioning agent, surfactant successively, apply out solvent;
C, mixed liquor is placed cooling;
Add acid number conditioning agent, lubrication humectant, anti-oxidant in d, the mixed liquor after cooling, stir and cooling;
E, cooled mixed liquor is refrigerated twenty four hours, subsequent use;
Step C: with solder powder and scaling powder according to 88~90: 12~10 mixed also stirs, and forms solder(ing) paste after the extracting vacuum.
CN2011104591632A 2011-12-28 2011-12-31 Low-rosin halogen and lead-free solder paste and preparation method thereof Pending CN102554489A (en)

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CN102909493A (en) * 2012-11-20 2013-02-06 邸园园 Soldering flux
CN103706961A (en) * 2012-09-28 2014-04-09 钟广飞 Halogen-free tin paste
CN104526186A (en) * 2014-12-26 2015-04-22 苏州龙腾万里化工科技有限公司 Novel scaling powder for SnZn series lead-free brazing filler metal
CN106392364A (en) * 2016-10-28 2017-02-15 广东中实金属有限公司 Lead-free solder paste used for jet printing technology and preparation method of lead-free solder paste
CN107755921A (en) * 2017-09-18 2018-03-06 广东省焊接技术研究所(广东省中乌研究院) A kind of water-based organic aluminium soldering paste into lotion and its comprising this into lotion
CN108274159A (en) * 2018-02-07 2018-07-13 合肥安力电力工程有限公司 A kind of circuit welding environment protection soldering fluid and preparation method thereof
CN108406166A (en) * 2018-03-13 2018-08-17 广东省焊接技术研究所(广东省中乌研究院) A kind of halogen-free spray printing tin cream scaling powder and preparation method thereof
CN108555474A (en) * 2018-04-03 2018-09-21 深圳市同方电子新材料有限公司 A kind of halogen-free environmental-friendly lead-free tin cream and preparation method thereof
CN109014656A (en) * 2018-08-24 2018-12-18 云南科威液态金属谷研发有限公司 A kind of halogen-free scaling powder and its preparation method and application
CN109676284A (en) * 2018-12-13 2019-04-26 上海锡喜材料科技有限公司 Weld-aiding cream and preparation method thereof
CN110560962A (en) * 2019-08-30 2019-12-13 西安理工大学 tin-bismuth series soldering paste and preparation method thereof
CN110753787A (en) * 2017-06-20 2020-02-04 马勒国际有限公司 Piston for an internal combustion engine with liquid metal cooling
CN111922551A (en) * 2020-08-12 2020-11-13 昆山联金科技发展有限公司 Sn-Zn lead-free soldering paste and preparation method thereof
CN113305470A (en) * 2021-05-28 2021-08-27 华天科技(西安)有限公司 Cleaning soldering flux and preparation method and use method thereof
CN114769943A (en) * 2022-04-27 2022-07-22 深圳市福特佳电子有限公司 Flux paste, solder paste and soldering method
CN115971726A (en) * 2022-12-19 2023-04-18 浙江亚通新材料股份有限公司 Scaling powder for lead-free solder and lead-free solder paste
CN115971724A (en) * 2022-12-27 2023-04-18 云南锡业锡材有限公司 Halogen-free water-soluble flux paste and preparation method thereof
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CN103706961A (en) * 2012-09-28 2014-04-09 钟广飞 Halogen-free tin paste
CN103706961B (en) * 2012-09-28 2016-08-03 钟广飞 Halogen-free tin paste
CN102909493A (en) * 2012-11-20 2013-02-06 邸园园 Soldering flux
CN104526186A (en) * 2014-12-26 2015-04-22 苏州龙腾万里化工科技有限公司 Novel scaling powder for SnZn series lead-free brazing filler metal
CN106392364A (en) * 2016-10-28 2017-02-15 广东中实金属有限公司 Lead-free solder paste used for jet printing technology and preparation method of lead-free solder paste
CN110753787A (en) * 2017-06-20 2020-02-04 马勒国际有限公司 Piston for an internal combustion engine with liquid metal cooling
CN107755921A (en) * 2017-09-18 2018-03-06 广东省焊接技术研究所(广东省中乌研究院) A kind of water-based organic aluminium soldering paste into lotion and its comprising this into lotion
CN107755921B (en) * 2017-09-18 2020-04-21 广东省焊接技术研究所(广东省中乌研究院) Aqueous organic paste forming body and aluminum soldering paste containing same
CN108274159A (en) * 2018-02-07 2018-07-13 合肥安力电力工程有限公司 A kind of circuit welding environment protection soldering fluid and preparation method thereof
CN108406166A (en) * 2018-03-13 2018-08-17 广东省焊接技术研究所(广东省中乌研究院) A kind of halogen-free spray printing tin cream scaling powder and preparation method thereof
CN108555474B (en) * 2018-04-03 2021-07-09 深圳市同方电子新材料有限公司 Halogen-free environment-friendly lead-free tin paste and preparation method thereof
CN108555474A (en) * 2018-04-03 2018-09-21 深圳市同方电子新材料有限公司 A kind of halogen-free environmental-friendly lead-free tin cream and preparation method thereof
CN109014656A (en) * 2018-08-24 2018-12-18 云南科威液态金属谷研发有限公司 A kind of halogen-free scaling powder and its preparation method and application
CN109676284A (en) * 2018-12-13 2019-04-26 上海锡喜材料科技有限公司 Weld-aiding cream and preparation method thereof
CN110560962A (en) * 2019-08-30 2019-12-13 西安理工大学 tin-bismuth series soldering paste and preparation method thereof
CN111922551A (en) * 2020-08-12 2020-11-13 昆山联金科技发展有限公司 Sn-Zn lead-free soldering paste and preparation method thereof
CN113305470A (en) * 2021-05-28 2021-08-27 华天科技(西安)有限公司 Cleaning soldering flux and preparation method and use method thereof
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Application publication date: 20120711