CN104175023A - Halogen-free soldering flux for lead-free solder paste - Google Patents

Halogen-free soldering flux for lead-free solder paste Download PDF

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Publication number
CN104175023A
CN104175023A CN201410179776.4A CN201410179776A CN104175023A CN 104175023 A CN104175023 A CN 104175023A CN 201410179776 A CN201410179776 A CN 201410179776A CN 104175023 A CN104175023 A CN 104175023A
Authority
CN
China
Prior art keywords
halogen
soldering flux
acid
free
unleaded
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201410179776.4A
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Chinese (zh)
Inventor
尹计深
戴爱斌
吕文慧
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Jiangsu Boqian New Materials Co Ltd
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Jiangsu Boqian New Materials Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
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Priority to CN201410179776.4A priority Critical patent/CN104175023A/en
Publication of CN104175023A publication Critical patent/CN104175023A/en
Pending legal-status Critical Current

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Classifications

    • BPERFORMING OPERATIONS; TRANSPORTING
    • B23MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23KSOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K35/00Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
    • B23K35/22Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by the composition or nature of the material
    • B23K35/36Selection 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
    • B23K35/3612Selection 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
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B23MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23KSOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K35/00Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
    • B23K35/22Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by the composition or nature of the material
    • B23K35/36Selection 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
    • B23K35/362Selection of compositions of fluxes

Abstract

The invention relates to the technical field of welding materials, in particular to a halogen-free soldering flux for lead-free solder paste. The halogen-free soldering flux for the lead-free solder paste comprises the following components in percentage by mass: 20 to 35 percent of solvent, 30 to 45 percent of rosin, 5 to 10 percent of surfactant, 10 to 20 percent of organic acid, 3 to 10 percent of antioxidant and 2 to 8 percent of thixotropic agent. According to the halogen-free soldering flux, a rosin mixture consisting of hydrogenated rosin and polymerized rosin at a weight ratio of 1:(1-3) is adopted, so that higher adhesive force of the solder paste is ensured; the proportion of the solvent and the rosin in the soldering flux is regulated, so that the viscosity range of the solder paste is wider; by the compounding of multiple organic acids, the prepared soldering flux is free of halogen, and has higher activity; the antioxidant for preparing the soldering flux is one or a combination of more than two of methylbenzotriazole, an antioxidant BHT, CHIMASSORB3030, benzimidazole and methylimidazole; the solder paste prepared from the soldering flux is long in service life, and has good de-molding effects.

Description

A kind of halogen-free soldering flux for unleaded soldering paste
Technical field
The present invention relates to technical field of welding materials, be specifically related to a kind of halogen-free soldering flux for unleaded soldering paste.
Background technology
Along with the develop rapidly of electronic technology, electronics and IT products are towards microminiaturized, integrated, multifunction future development, and surface installation technique has become the mainstream technology in Electronic Assemblies field.Solder(ing) paste is to be accompanied by a kind of Novel welding material that surface installation technique arises at the historic moment, and the quality of solder(ing) paste directly affects the quality of welding.Traditional solder(ing) paste product is mixed and is formed by tin slicker solder powder and scaling powder, and along with the progress of technology in recent years and the people growing interest to self and environment, unleaded glass putty has replaced tin slicker solder powder gradually.From there being lead welding tin cream to change to leadless soldering tin paste, some technical barriers when having adapted to environmental requirement, are also brought, traditional scaling powder mixes with unleaded glass putty the solder(ing) paste poor-performing making mutually, postwelding halogen residue thing is many, insulating properties is not high enough, bring great potential safety hazard to the dependability of product, cannot meet the demand of surface mounting technique.
Summary of the invention
The object of the invention is to for the problem that in prior art, solder(ing) paste content of halogen is high, high-temperature oxidation resistance is poor, provide that a kind of activity is high, halogen-free, thixotropy and high-temperature oxidation resistance is good, the wider halogen-free soldering flux for unleaded soldering paste of range of viscosities.
Technical solution of the present invention:
A kind of halogen-free soldering flux for unleaded soldering paste, is characterized in that: 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, diethylene glycol monobutyl ether acetate, diethylene glycol monobutyl ether, dipropylene glycol methyl ether, diethylene glycol monohexyl ether, nitroethane, 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, trimethyl butylene 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 at least one in thixotropic agent 7500, modified hydrogenated castor oil, ethylenebis stearic amide.
A kind of halogen-free soldering flux for unleaded soldering paste preparation technology, comprises the following steps:
(1) weigh according to the above ratio solvent, rosin and surfactant and join in reaction vessel, be heated to 100-120 DEG C, be stirred to completely and dissolve;
(2) after mixture step (1) being obtained is cooled to 80-100 DEG C, add organic acid and antioxidant, be stirred to completely and dissolve;
(3) after being cooled to 50-70 DEG C, mixture step (2) being obtained adds thixotropic agent, be stirred to completely and dissolve, be cooled to 20-25 DEG C, solid particle fineness in mixed solution is ground to below 10 μ m with three-roll grinder, makes halogen-free soldering flux for unleaded soldering paste of the present invention.
Beneficial effect of the present invention:
(1) to select weight ratio be Foral and the newtrex mixture rosin of 1:1 ~ 3 to scaling powder of the present invention, ensures that solder(ing) paste has good adhesion, by regulating the ratio of solvent and rosin in scaling powder, can obtain the wider solder(ing) paste of range of viscosities;
(2) scaling powder of the present invention is composite by multiple organic acid, and the scaling powder making is not only not halogen-containing but also have a higher activity;
(3) preparing scaling powder of the present invention antioxidant used is one or more combinations in methyl benzotriazazole, antioxidant BHT, CHIMASSORB 3030, benzimidazole, methylimidazole, the solder(ing) paste long service life that this scaling powder makes and have good stripping result.
Detailed description of the invention
Embodiment 1
By diethylene glycol monohexyl ether 48g, Foral 40g, newtrex 40g and TX-10 phosphate 12g join in reaction vessel, are heated to 100 DEG C, are stirred to completely and dissolve; 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, be stirred to completely and dissolve; Be cooled to 70 DEG C, add modified hydrogenated castor oil 12g, be stirred to completely and dissolve, be cooled to 23 DEG C, the solid particle fineness in mixed solution is ground to below 10 μ m with three-roll grinder, obtain halogen-free soldering flux for unleaded soldering paste 196g.
 
Embodiment 2
A kind of halogen-free soldering flux for unleaded soldering paste, by diethylene glycol butyl ether 46g, Foral 30g, newtrex 50g and Surfynol 104E 14g join in reaction vessel, are heated to 108 DEG C, are stirred to completely and dissolve; 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, be stirred to completely and dissolve; Be cooled to 50 DEG C, add ethylenebis stearic amide 8g, be stirred to completely and dissolve, be cooled to 20 DEG C, the solid particle fineness in mixed solution is ground to below 10 μ m with three-roll grinder, obtain halogen-free soldering flux for unleaded soldering paste 194g.
 
Embodiment 3
A kind of halogen-free soldering flux for unleaded soldering paste, 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 completely and dissolve; 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, be stirred to completely and dissolve; Be cooled to 65 DEG C, add thixotropic agent 7500 10g, be stirred to completely and dissolve, be cooled to 22 DEG C, the solid particle fineness in mixed solution is ground to below 10 μ m with three-roll grinder, obtain halogen-free soldering flux for unleaded soldering paste 193g.
 
Embodiment 4
A kind of halogen-free soldering flux for unleaded soldering paste, by diethylene glycol monohexyl ether 48g, nitroethane 4g, Foral 40g, newtrex 40g, GE-511 8g and trimethyl butylene glycol 4g join in reaction vessel, are heated to 120 DEG C, are stirred to completely and dissolve; 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, be stirred to completely and dissolve; Be cooled to 60 DEG C, add ethylenebis stearic amide 9g, be stirred to completely and dissolve, be cooled to 21 DEG C, the solid particle fineness in mixed solution is ground to below 10 μ m with three-roll grinder, obtain halogen-free soldering flux for unleaded soldering paste 191g.
 
Embodiment 5
A kind of halogen-free soldering flux for unleaded soldering paste, by diethylene glycol monohexyl ether 48g, Foral 41g, newtrex 41g, GE-511 8g and trimethyl butylene glycol 5g join in reaction vessel, are heated to 110 DEG C, are stirred to completely and dissolve; 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, be stirred to completely and dissolve; Be cooled to 60 DEG C, add ethylenebis stearic amide 9g, be stirred to completely and dissolve, be cooled to 23 DEG C,, the solid particle fineness in mixed solution is ground to below 10 μ m with three-roll grinder, obtain halogen-free soldering flux for unleaded soldering paste 195g.
 
The scaling powder making by above embodiment and Sn-Ag-Cu are associated bronze and are mixed and made into solder(ing) paste, detect according to GB/T 9491-2002, 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: halogen-free soldering flux for unleaded soldering paste of the present invention is not halogen-containing, wetability well all reaches the more than 2 grades requirement of standard; Solder(ing) paste range of viscosities is wider; Surface insulation resistance value, far above standard-required, meets electric insulation requirement; 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.

Claims (8)

1. a halogen-free soldering flux for unleaded soldering paste, is characterized in that: 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%.
2. a kind of halogen-free soldering flux for unleaded soldering paste as claimed in claim 1, is characterized in that: described solvent is one or more compositions in dibutyl ethylene glycol ether, diethylene glycol monobutyl ether acetate, diethylene glycol monobutyl ether, dipropylene glycol methyl ether, diethylene glycol monohexyl ether, nitroethane, diethylene glycol octyl ether, tripropylene glycol butyl ether, triethylene glycol butyl ether.
3. a kind of halogen-free soldering flux for unleaded soldering paste as claimed in claim 1, is characterized in that: described rosin is the mixture of Foral and newtrex, both part by weight are 1:1 ~ 3.
4. a kind of halogen-free soldering flux for unleaded soldering paste as claimed in claim 1, is characterized in that: described surfactant is one or both in TX-10 phosphate, rosin ether surface active agent, GE-511, trimethyl butylene glycol, Surfynol 104E.
5. a kind of halogen-free soldering flux for unleaded soldering paste as claimed in claim 1, 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.
6. a kind of halogen-free soldering flux for unleaded soldering paste as claimed in claim 1, is characterized in that: described antioxidant is one or more combinations in methyl benzotriazazole, antioxidant BHT, CHIMASSORB 3030, benzimidazole, methylimidazole.
7. a kind of halogen-free soldering flux for unleaded soldering paste as claimed in claim 1, is characterized in that: described thixotropic agent is at least one in thixotropic agent 7500, modified hydrogenated castor oil, ethylenebis stearic amide.
8. preparation a kind of halogen-free soldering flux for unleaded soldering paste as claimed in claim 1, comprises the following steps:
(1) weigh according to the above ratio solvent, rosin and surfactant and join in reaction vessel, be heated to 100-120 DEG C, be stirred to completely and dissolve;
(2) after mixture step (1) being obtained is cooled to 80-100 DEG C, add organic acid and antioxidant, be stirred to completely and dissolve;
(3) after being cooled to 50-70 DEG C, mixture step (2) being obtained adds thixotropic agent, be stirred to completely and dissolve, be cooled to 20-25 DEG C, solid particle fineness in mixed solution is ground to below 10 μ m with three-roll grinder, makes halogen-free soldering flux for unleaded soldering paste of the present invention.
CN201410179776.4A 2014-04-30 2014-04-30 Halogen-free soldering flux for lead-free solder paste Pending CN104175023A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201410179776.4A CN104175023A (en) 2014-04-30 2014-04-30 Halogen-free soldering flux for lead-free solder paste

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Application Number Priority Date Filing Date Title
CN201410179776.4A CN104175023A (en) 2014-04-30 2014-04-30 Halogen-free soldering flux for lead-free solder paste

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Cited By (16)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104722959A (en) * 2015-03-31 2015-06-24 北京航空航天大学 Soldering flux for aluminum alloy low-temperature brazing
CN105290647A (en) * 2015-11-13 2016-02-03 北京达博长城锡焊料有限公司 Organic scaling powder for frequency conversion refrigerator welding materials and preparing method
CN106670680A (en) * 2017-02-17 2017-05-17 广州适普电子有限公司 Scaling powder capable of preventing head-in-pillow effect and preparation method and application thereof
CN107088716A (en) * 2017-07-03 2017-08-25 中山翰华锡业有限公司 A kind of environment-friendly low-temperature noresidue tin cream and preparation method thereof
CN107447220A (en) * 2017-07-26 2017-12-08 苏州天承化工有限公司 A kind of chromium-free environment-friendly antioxidant and preparation method
CN107617832A (en) * 2017-10-20 2018-01-23 东莞市华粤焊锡制品有限公司 Anti- fried soldering tin cream scaling powder and preparation method thereof
CN107695561A (en) * 2017-11-03 2018-02-16 张家港市东大工业技术研究院 A kind of spray printing low viscosity leadless soldering tin paste and its preparation technology
CN108472771A (en) * 2016-01-15 2018-08-31 千住金属工业株式会社 Scaling powder
CN109093290A (en) * 2018-08-31 2018-12-28 安徽红桥金属制造有限公司 A kind of scaling powder that can be reduced weldment residue and improve welding efficiency
CN110303273A (en) * 2019-06-26 2019-10-08 浙江强力控股有限公司 Halogen-free low-temperature environment-protection soldering tin paste and preparation method thereof for heat radiation module
CN111906472A (en) * 2020-08-10 2020-11-10 云南锡业锡材有限公司 Solder wire soldering flux capable of reducing splashing and preparation method thereof
CN113210931A (en) * 2021-05-13 2021-08-06 北京达博长城锡焊料有限公司 Soldering flux for solder paste, preparation method thereof and halogen-free and lead-free solder paste
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
CN114273820A (en) * 2021-12-30 2022-04-05 云南锡业锡材有限公司 High-lead soldering tin paste soldering flux and preparation method thereof
CN114559181A (en) * 2022-04-13 2022-05-31 邢台福润德化工有限公司 Photovoltaic cleaning-free soldering flux and preparation method thereof
CN116174997A (en) * 2023-02-25 2023-05-30 东莞市千岛金属锡品有限公司 Lead-free halogen-free soldering paste and preparation process thereof

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CN102489897A (en) * 2011-11-16 2012-06-13 苏州之侨新材料科技有限公司 Low-temperature lead-free soldering flux for tin-bismuth series
CN102794582A (en) * 2012-08-15 2012-11-28 北京工业大学 Soldering flux matched with high-melting-point solder and preparation method thereof
CN102990242A (en) * 2011-09-13 2013-03-27 郴州金箭焊料有限公司 Low-temperature halogen-free lead-free solder paste

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US4478650A (en) * 1983-10-19 1984-10-23 At&T Technologies, Inc. Water soluble flux
JP2007069260A (en) * 2005-09-09 2007-03-22 Uchihashi Estec Co Ltd Flux composition for resin flux cored solder, and resin flux cored solder
CN101934437A (en) * 2010-09-30 2011-01-05 常州市亚太微电子材料有限公司 Unleaded solder paste and preparation method thereof
CN102990242A (en) * 2011-09-13 2013-03-27 郴州金箭焊料有限公司 Low-temperature halogen-free lead-free solder paste
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Cited By (22)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104722959A (en) * 2015-03-31 2015-06-24 北京航空航天大学 Soldering flux for aluminum alloy low-temperature brazing
CN105290647A (en) * 2015-11-13 2016-02-03 北京达博长城锡焊料有限公司 Organic scaling powder for frequency conversion refrigerator welding materials and preparing method
CN105290647B (en) * 2015-11-13 2017-08-29 北京达博长城锡焊料有限公司 Frequency conversion refrigerator welding material organic scaling powder and preparation method
CN108472771A (en) * 2016-01-15 2018-08-31 千住金属工业株式会社 Scaling powder
US11571772B2 (en) 2016-01-15 2023-02-07 Senju Metal Industry Co., Ltd. Flux
CN108472771B (en) * 2016-01-15 2019-05-28 千住金属工业株式会社 Scaling powder
CN106670680A (en) * 2017-02-17 2017-05-17 广州适普电子有限公司 Scaling powder capable of preventing head-in-pillow effect and preparation method and application thereof
CN106670680B (en) * 2017-02-17 2018-11-23 广州适普电子有限公司 A kind of anti-pillow effect scaling powder and its preparation method and application
CN107088716A (en) * 2017-07-03 2017-08-25 中山翰华锡业有限公司 A kind of environment-friendly low-temperature noresidue tin cream and preparation method thereof
CN107088716B (en) * 2017-07-03 2020-01-24 中山翰华锡业有限公司 Environment-friendly low-temperature residue-free solder paste and preparation method thereof
CN107447220A (en) * 2017-07-26 2017-12-08 苏州天承化工有限公司 A kind of chromium-free environment-friendly antioxidant and preparation method
CN107617832A (en) * 2017-10-20 2018-01-23 东莞市华粤焊锡制品有限公司 Anti- fried soldering tin cream scaling powder and preparation method thereof
CN107695561A (en) * 2017-11-03 2018-02-16 张家港市东大工业技术研究院 A kind of spray printing low viscosity leadless soldering tin paste and its preparation technology
CN109093290A (en) * 2018-08-31 2018-12-28 安徽红桥金属制造有限公司 A kind of scaling powder that can be reduced weldment residue and improve welding efficiency
CN110303273A (en) * 2019-06-26 2019-10-08 浙江强力控股有限公司 Halogen-free low-temperature environment-protection soldering tin paste and preparation method thereof for heat radiation module
CN111906472A (en) * 2020-08-10 2020-11-10 云南锡业锡材有限公司 Solder wire soldering flux capable of reducing splashing and preparation method thereof
CN113210931A (en) * 2021-05-13 2021-08-06 北京达博长城锡焊料有限公司 Soldering flux for solder paste, preparation method thereof and halogen-free and lead-free solder paste
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
CN114273820A (en) * 2021-12-30 2022-04-05 云南锡业锡材有限公司 High-lead soldering tin paste soldering flux and preparation method thereof
CN114559181A (en) * 2022-04-13 2022-05-31 邢台福润德化工有限公司 Photovoltaic cleaning-free soldering flux and preparation method thereof
CN116174997A (en) * 2023-02-25 2023-05-30 东莞市千岛金属锡品有限公司 Lead-free halogen-free soldering paste and preparation process thereof
CN116174997B (en) * 2023-02-25 2023-08-25 东莞市千岛金属锡品有限公司 Lead-free halogen-free soldering paste and preparation process thereof

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