CN105014253A - Lead-free tin solder paste and preparation method thereof - Google Patents

Lead-free tin solder paste and preparation method thereof Download PDF

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Publication number
CN105014253A
CN105014253A CN201410179613.6A CN201410179613A CN105014253A CN 105014253 A CN105014253 A CN 105014253A CN 201410179613 A CN201410179613 A CN 201410179613A CN 105014253 A CN105014253 A CN 105014253A
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CN
China
Prior art keywords
acid
lead
free
soldering tin
rosin
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Pending
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CN201410179613.6A
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Chinese (zh)
Inventor
尹计深
戴爱斌
黄栋臣
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Jiangsu Boqian New Materials Co Ltd
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Jiangsu Boqian New Materials Co Ltd
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Priority to CN201410179613.6A priority Critical patent/CN105014253A/en
Publication of CN105014253A publication Critical patent/CN105014253A/en
Pending legal-status Critical Current

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Abstract

The invention discloses a lead-free tin solder paste and a preparation method thereof. The lead-free tin solder paste comprises the raw materials by mass percent: 80-90% of tin-silver-copper alloy tinpowder and 10-20% of lead-free flux, wherein the tin-silver-copper alloy tin powder comprises the componentsby mass percent: 0.3-3.0% of silver, 0.5-0.7% of copper and 96.5-99.0% of tin, and the lead-free flux comprises the componentsby mass percent: 20-35% of solvent, 30-45% of rosin, 5-10% of surface active agent, 10-20% of organic acid, 3-10% of antioxidant and 2-8% of thixotropic agent. The rosin which is a mixture of hydrogenated rosin and polymerized rosin according to a weight ratio of 1:(1-3) is adopted, so that the prepared lead-free tin solder paste is good in adhesive force and stability; by adjusting a ratio of the solvent to the rosin, the prepared lead-free tin solder paste has a wider viscosity range and good printing performance; with the compounding of various organic acid, the prepared lead-free tin solder paste is halogen-free, and the activity of the lead-free tin solder paste is improved greatly; the surface active agent is compounded with the solvent with high boiling point, low viscosity and low volatility, so that the prepared lead-free tin solder paste is long in printing time, and excellent in insulating property.

Description

A kind of leadless soldering tin paste and preparation method thereof
Technical field
The present invention relates to technical field of soldering paste, be specifically related to a kind of leadless soldering tin paste and preparation method thereof.
Background technology
Solder(ing) paste is the paste mixture be mixed to form by solder powder, scaling powder and surfactant, thixotropic agent etc., is auxiliary material very important during current electronic product is produced.Along with the high speed development of electronics and information industry, electronic product more and more changes to light, thin, short, little and high-effect direction, Electronic Assembly Foundation is towards while high accuracy, high density, high reliability future development, internationalization environmental consciousness also improves thereupon, higher requirement be it is also proposed to the solder(ing) paste played a crucial role in Electronic Assemblies, lead-free and halogen-free, low-temperature energy-saving, shaping precise treatment, use high reliability to become the developing direction of current solder(ing) paste.At present, in various leadless soldering tin paste, a kind of solder compositions that Sn/Ag/Cu alloy is accepted extensively the most by industry, but the performance of its each side is not also very desirable, and as also there is solder(ing) paste failure welding, activity is low, wetability is poor, containing defects such as halogens.
Summary of the invention
The object of the invention is to for above-mentioned deficiency, provide a kind of there is excellent printing performance, the demoulding is clean, solderability good, wetability is strong, halogen-free, postwelding bronze mirror is without penetrability corrosion and the high leadless soldering tin paste of welding spot reliability and preparation method thereof.
The technology of the present invention solution:
A kind of leadless soldering tin paste, raw material comprises: tin-silver-copper alloy glass putty, and lead-free soldering flux, is characterized in that: material quality percentage is: 80% ~ 90%:10% ~ 20%.
In described tin-silver-copper alloy glass putty, mass percent is silver: 0.3% ~ 3.0%, copper: 0.5% ~ 0.7%, tin: 96.5% ~ 99.0%.
In described lead-free soldering flux, each component and mass percent are: solvent: rosin: surfactant: organic acid: antioxidant: thixotropic agent=20% ~ 35%:30% ~ 45%:5% ~ 10%:10% ~ 20%:3% ~ 10%:2% ~ 8%.
Described solvent is one or more compositions in dibutyl ethylene glycol ether, butyl acetate, diethylene glycol monobutyl ether, dipropylene glycol methyl ether, diethylene glycol monohexyl ether, diethylene glycol octyl ether, tripropylene glycol butyl ether, triethylene glycol butyl ether.
Described rosin is the mixture of Foral and newtrex, and both part by weight are 1:1 ~ 3.
Described surfactant is one or both in TX-10 phosphate, rosin ether surface active agent, GE-511, trimethylbutene glycol, Surfynol 104E.
Described organic acid is at least two or more combinations in itaconic acid, stearic acid, decanedioic acid, succinic acid, adipic acid, glutaric acid, suberic acid, tetradecylic acid, di-propionic acid, p-tert-butyl benzoic acid, dimethyl succinic acid.
Described antioxidant is one or more combinations in methyl benzotriazazole, antioxidant BHT, CHIMASSORB 3030, benzimidazole, methylimidazole.
Described thixotropic agent is the one in thixotropic agent 7500, modified hydrogenated castor oil, ethylenebis stearic amide.
A kind of Pb-free solder ointment preparation, comprises the following steps:
The first step, weighs solvent, rosin and surfactant according to the above ratio and joins in reaction vessel, is stirred to and dissolves completely after being heated to 100-120 DEG C;
Second step, the mixture first step obtained adds organic acid and antioxidant after being cooled to 80-100 DEG C, is stirred to and dissolves completely;
3rd step, the mixture obtained by second step adds thixotropic agent after being cooled to 50-70 DEG C, is stirred to and dissolves completely, is cooled to room temperature, with three-roll grinder, the solid particle fineness in mixed solution is ground to less than 10 μm, obtains scaling powder;
4th step, under normal temperature and pressure, the scaling powder obtain the 3rd step and Pb-free coating glass putty load solder paste stirrer and stir 5 minutes with the speed of 15 revs/min;
5th step, extracting vacuum, continues stirring 15 minutes, namely obtains leadless soldering tin paste of the present invention.
Beneficial effect of the present invention:
(1) the present invention selects weight ratio to be Foral and the newtrex mixture rosin of 1:1 ~ 3, obtained solder(ing) paste adhesion and having good stability, by regulating the ratio of solvent and rosin, obtained solder(ing) paste has wider range of viscosities and good printing performance;
(2) the present invention adopts multiple organic acid composite, and obtained leadless soldering tin paste is halogen-free, and the activity of solder(ing) paste improves greatly;
(3) the present invention selects higher boiling, low viscosity, the solvent complex surfactant of low volatility, and obtained solder(ing) paste printing time is longer, and insulating properties is excellent.
detailed description of the invention
Embodiment 1
Tripropylene glycol butyl ether 52g, Foral 40g, newtrex 40g, GE-511 8g and trimethylbutene glycol 4g are joined in reaction vessel, is heated to 120 DEG C, is stirred to and dissolves completely; Be cooled to 100 DEG C, add tetradecylic acid 18g, succinic acid 2g, adipic acid 4g, glutaric acid 8g, suberic acid 3g, antioxidant BHT 2g and methylimidazole 10g, is stirred to and dissolves completely; Be cooled to 60 DEG C, add ethylenebis stearic amide 9g, be stirred to and dissolve completely, be cooled to room temperature, with three-roll grinder, the solid particle fineness in mixed solution is ground to less than 10 μm, obtains scaling powder 193g.
Pb-free coating glass putty 442.5g is mixed with scaling powder 57.5g, stirs 5 minutes with the mixing speed of 15 revs/min, extracting vacuum, continue stirring 15 minutes, namely obtain leadless soldering tin paste 500g.
Embodiment 2
By dibutyl ethylene glycol ether 58g, Foral 36g, newtrex 40g and rosin ether surface active agent 10g join in reaction vessel, are heated to 116 DEG C, are stirred to and dissolve completely; Be cooled to 80 DEG C, add di-propionic acid 14g, succinic acid 4g, adipic acid 5g, glutaric acid 7g, suberic acid 2g, methyl benzotriazazole 2g and methylimidazole 12g, is stirred to and dissolves completely; Be cooled to 65 DEG C, add thixotropic agent 7500 10g, be stirred to and dissolve completely, be cooled to room temperature, with three-roll grinder, the solid particle fineness in mixed solution is ground to less than 10 μm, obtains scaling powder 195g.
Pb-free coating glass putty 442.0g is mixed with scaling powder 58.0g, stirs 5 minutes with the mixing speed of 15 revs/min, extracting vacuum, continue stirring 15 minutes, namely obtain leadless soldering tin paste 500g.
Embodiment 3
Diethylene glycol monohexyl ether 48g, Foral 41g, newtrex 41g, GE-511 8g and trimethylbutene glycol 5g are joined in reaction vessel, is heated to 110 DEG C, is stirred to and dissolves completely; Be cooled to 90 DEG C, add tetradecylic acid 18g, succinic acid 2g, adipic acid 4g, glutaric acid 8g, suberic acid 4g, antioxidant BHT 2g and methylimidazole 10g, is stirred to and dissolves completely; Be cooled to 60 DEG C, add ethylenebis stearic amide 9g, be stirred to and dissolve completely, be cooled to room temperature, with three-roll grinder, the solid particle fineness in mixed solution is ground to less than 10 μm, obtains scaling powder 192g.
Pb-free coating glass putty 443.5g is mixed with scaling powder 56.5g, stirs 5 minutes with the mixing speed of 15 revs/min, extracting vacuum, continue stirring 15 minutes, namely obtain leadless soldering tin paste 500g.
Embodiment 4
Diethylene glycol monohexyl ether 48g, Foral 40g, newtrex 40g and TX-10 phosphate 12g are joined in reaction vessel, is heated to 100 DEG C, is stirred to and dissolves completely; Be cooled to 85 DEG C, add tetradecylic acid 16g, succinic acid 3g, adipic acid 6g, glutaric acid 9g, suberic acid 2g, methyl benzotriazazole 2g and methylimidazole 10g, is stirred to and dissolves completely; Be cooled to 70 DEG C, add modified hydrogenated castor oil 12g, be stirred to and dissolve completely, be cooled to room temperature, with three-roll grinder, the solid particle fineness in mixed solution is ground to less than 10 μm, obtains scaling powder 191g.
Pb-free coating glass putty 441.5g is mixed with scaling powder 58.5g, stirs 5 minutes with the mixing speed of 15 revs/min, extracting vacuum, continue stirring 15 minutes, namely obtain leadless soldering tin paste 500g.
Embodiment 5
By butyl 46g, Foral 30g, newtrex 50g and Surfynol 104E 14g joins in reaction vessel, is heated to 108 DEG C, is stirred to and dissolves completely; Be cooled to 90 DEG C, add p-tert-butyl benzoic acid 12g, stearic acid 4g, succinic acid 4g, adipic acid 7g, glutaric acid 8g, suberic acid 2g, CHIMASSORB 3030 3g and benzimidazole 12g, is stirred to and dissolves completely; Be cooled to 50 DEG C, add ethylenebis stearic amide 8g, be stirred to and dissolve completely, be cooled to room temperature, with three-roll grinder, the solid particle fineness in mixed solution is ground to less than 10 μm, obtains scaling powder 194g.
Pb-free coating glass putty 443.0g is mixed with scaling powder 57.0g, stirs 5 minutes with the mixing speed of 15 revs/min, extracting vacuum, continue stirring 15 minutes, namely obtain leadless soldering tin paste 500g.
The solder(ing) paste obtained by above embodiment detects according to SJ/T 11186-2009 standard, and properties testing result is as table 1.
Table 1 embodiment 1 ~ 5 performance test results
As can be seen from Table 1: leadless soldering tin paste range of viscosities of the present invention is wider; Halogen-free, wetability is strong, and tin sweat(ing) is few; Surface insulation resistance value is far above the standard-required of electron trade; Postwelding bronze mirror corrodes without penetrability; The maximum bridging spacing that cold/heat is caved in is 0.06/0.10mm, has good printing, thixotropic property, meets the requirement of high density thin space Full Vision technique completely; Meanwhile, after continuous printing 8h, viscosity B coefficent value is little, ensure that the stability of printing performance during long-time presswork.

Claims (10)

1. a leadless soldering tin paste, raw material comprises: tin-silver-copper alloy glass putty, and lead-free soldering flux, is characterized in that: material quality percentage is: 80% ~ 90%:10% ~ 20%.
2. a kind of leadless soldering tin paste as claimed in claim 1, is characterized in that: in described tin-silver-copper alloy glass putty, mass percent is silver: 0.3% ~ 3.0%, copper: 0.5% ~ 0.7%, tin: 96.5% ~ 99.0%.
3. a kind of leadless soldering tin paste as claimed in claim 1, is characterized in that: in described lead-free soldering flux, each component and mass percent are: solvent: rosin: surfactant: organic acid: antioxidant: thixotropic agent=20% ~ 35%:30% ~ 45%:5% ~ 10%:10% ~ 20%:3% ~ 10%:2% ~ 8%.
4. a kind of leadless soldering tin paste as claimed in claim 3, is characterized in that: described solvent is one or more compositions in dibutyl ethylene glycol ether, butyl acetate, diethylene glycol monobutyl ether, dipropylene glycol methyl ether, diethylene glycol monohexyl ether, diethylene glycol octyl ether, tripropylene glycol butyl ether, triethylene glycol butyl ether.
5. a kind of leadless soldering tin paste as claimed in claim 3, it is characterized in that: described rosin is the mixture of Foral and newtrex, both part by weight are 1:1 ~ 3.
6. a kind of leadless soldering tin paste as claimed in claim 3, is characterized in that: described surfactant is one or both in TX-10 phosphate, rosin ether surface active agent, GE-511, trimethylbutene glycol, Surfynol 104E.
7. a kind of leadless soldering tin paste as claimed in claim 3, is characterized in that: described organic acid is at least two or more combinations in itaconic acid, stearic acid, decanedioic acid, succinic acid, adipic acid, glutaric acid, suberic acid, tetradecylic acid, di-propionic acid, p-tert-butyl benzoic acid, dimethyl succinic acid.
8. a kind of leadless soldering tin paste as claimed in claim 3, is characterized in that: described antioxidant is one or more combinations in methyl benzotriazazole, antioxidant BHT, CHIMASSORB 3030, benzimidazole, methylimidazole.
9. a kind of leadless soldering tin paste as claimed in claim 3, is characterized in that: described thixotropic agent is the one in thixotropic agent 7500, modified hydrogenated castor oil, ethylenebis stearic amide.
10. preparation a kind of leadless soldering tin paste as claimed in claim 1, comprises and comprising the following steps:
The first step, weighs solvent, rosin and surfactant according to the above ratio and joins in reaction vessel, is stirred to and dissolves completely after being heated to 100-120 DEG C;
Second step, the mixture first step obtained adds organic acid and antioxidant after being cooled to 80-100 DEG C, is stirred to and dissolves completely;
3rd step, the mixture obtained by second step adds thixotropic agent after being cooled to 50-70 DEG C, is stirred to and dissolves completely, is cooled to room temperature, with three-roll grinder, the solid particle fineness in mixed solution is ground to less than 10 μm, obtains scaling powder;
4th step, under normal temperature and pressure, the scaling powder obtain the 3rd step and Pb-free coating glass putty load solder paste stirrer and stir 5 minutes with the speed of 15 revs/min;
5th step, extracting vacuum, continues stirring 15 minutes, namely obtains leadless soldering tin paste of the present invention.
CN201410179613.6A 2014-04-30 2014-04-30 Lead-free tin solder paste and preparation method thereof Pending CN105014253A (en)

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Cited By (18)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106002000A (en) * 2016-06-23 2016-10-12 深圳市唯特偶新材料股份有限公司 Soldering paste and preparation method thereof
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
CN106271186A (en) * 2016-08-31 2017-01-04 苏州恩斯泰金属科技有限公司 A kind of solder(ing) paste
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
CN108057965A (en) * 2017-11-29 2018-05-22 东莞永安科技有限公司 Leadless soldering tin paste of welding quality and preparation method thereof can be improved
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
CN108788512A (en) * 2018-08-24 2018-11-13 东莞市仁信电子有限公司 A kind of low voidage leadless environment-friendly solder(ing) paste of low melting point
CN110303274A (en) * 2019-06-26 2019-10-08 浙江强力控股有限公司 Remain heat cure solder(ing) paste and preparation method thereof
CN110303272A (en) * 2019-06-26 2019-10-08 浙江强力控股有限公司 Brass base, Ni-based needle tubing halogen-free environmental solder(ing) paste and preparation method thereof
CN110405377A (en) * 2019-07-10 2019-11-05 深圳市博士达焊锡制品有限公司 A kind of semiconductor high temperature print solder paste
CN111360347A (en) * 2020-03-06 2020-07-03 深圳市唯特偶新材料股份有限公司 Method for improving welding performance of 5G communication module
CN111360446A (en) * 2020-04-28 2020-07-03 深圳市邦大科技有限公司 Halogen-free lead-free 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
EP3848149A1 (en) * 2020-01-09 2021-07-14 3S Silicon Tech, Inc. Solder paste composition and soldering method using the same
CN114029649A (en) * 2021-12-24 2022-02-11 南京青锐风新材料科技有限公司 Compound solvent modified lead-free soldering paste for jet printing and preparation method thereof
CN114101972A (en) * 2021-10-29 2022-03-01 江苏正能电子科技有限公司 SMT soldering paste with high wetting dispersibility and weather resistance and preparation 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
CN115365703A (en) * 2022-08-19 2022-11-22 大连海外华昇电子科技有限公司 Water-soluble soldering flux and preparation method thereof

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Cited By (21)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106002000A (en) * 2016-06-23 2016-10-12 深圳市唯特偶新材料股份有限公司 Soldering paste and preparation method thereof
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
CN106271186B (en) * 2016-08-31 2019-11-08 苏州恩斯泰金属科技有限公司 A kind of solder(ing) paste
CN106271186A (en) * 2016-08-31 2017-01-04 苏州恩斯泰金属科技有限公司 A kind of solder(ing) paste
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
CN108057965A (en) * 2017-11-29 2018-05-22 东莞永安科技有限公司 Leadless soldering tin paste of welding quality and preparation method thereof can be improved
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
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
CN108788512A (en) * 2018-08-24 2018-11-13 东莞市仁信电子有限公司 A kind of low voidage leadless environment-friendly solder(ing) paste of low melting point
CN110303272A (en) * 2019-06-26 2019-10-08 浙江强力控股有限公司 Brass base, Ni-based needle tubing halogen-free environmental solder(ing) paste and preparation method thereof
CN110303274A (en) * 2019-06-26 2019-10-08 浙江强力控股有限公司 Remain heat cure solder(ing) paste and preparation method thereof
CN110405377A (en) * 2019-07-10 2019-11-05 深圳市博士达焊锡制品有限公司 A kind of semiconductor high temperature print solder paste
EP3848149A1 (en) * 2020-01-09 2021-07-14 3S Silicon Tech, Inc. Solder paste composition and soldering method using the same
CN111360347B (en) * 2020-03-06 2022-07-05 深圳市唯特偶新材料股份有限公司 Method for improving welding performance of 5G communication module
CN111360347A (en) * 2020-03-06 2020-07-03 深圳市唯特偶新材料股份有限公司 Method for improving welding performance of 5G communication module
CN111360446A (en) * 2020-04-28 2020-07-03 深圳市邦大科技有限公司 Halogen-free lead-free 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
CN114101972A (en) * 2021-10-29 2022-03-01 江苏正能电子科技有限公司 SMT soldering paste with high wetting dispersibility and weather resistance and preparation method thereof
CN114029649A (en) * 2021-12-24 2022-02-11 南京青锐风新材料科技有限公司 Compound solvent modified lead-free soldering paste for jet printing and preparation 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
CN115365703A (en) * 2022-08-19 2022-11-22 大连海外华昇电子科技有限公司 Water-soluble soldering flux and preparation method thereof

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