CN1927526A - Leadless solder for electronic industry and preparation method - Google Patents
Leadless solder for electronic industry and preparation method Download PDFInfo
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- CN1927526A CN1927526A CN 200610113439 CN200610113439A CN1927526A CN 1927526 A CN1927526 A CN 1927526A CN 200610113439 CN200610113439 CN 200610113439 CN 200610113439 A CN200610113439 A CN 200610113439A CN 1927526 A CN1927526 A CN 1927526A
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Abstract
The invention relates to a method for producing leadless soldering paste. Wherein, it is formed by 87-93% leadless tin solder powder and 7-13% welding flux; the leadless soldering powder is 25-45micrometer powder made from Cu, Ag, Ce, and Sn; the welding flux is formed by improved rosin, thixotropic agent, stabilizer, activator and solvent; first fusing the improved rosin, adding thixotropic agent, stabilizer, activator and solvent, to obtain welding flux; then mixing the leadless tin solder powder and welding flux in tin paste machine to be bottled. The invention has better protective property, less corrosion and high insulated property.
Description
Technical field
The present invention relates to a kind of leadless solder for electronic industry that is applicable to, belong to welding material.
The invention still further relates to the preparation method of this lead-free solder paste
Background technology
Along with electronic product high speed development day by day, the application of surface mounting technology is more extensive in recent years, and size is dwindled because this technology allows, high density, high-performance and cost are low.But traditional solder(ing) paste product is made up of tin-lead solder powder and scaling powder; heavy metal lead in the solder(ing) paste is after welding PCB; can intersperse among in the environment with discarded later on electronic product; through the long-term etch of acid rain, lead can permeate the ground, and dissolves in ground water regime; drink the back and can cause plumbous heavy poison at human or animal's cylinder accumulation for a long time; endangering the health of people and animal, just because of people recognize the importance of protection environment, so environmental regulation also is being gradually improved and strictness.Therefore, lead-free solder paste has been to avoid in microelectronics surface installation technique Application for Field, and existing lead-free tin cream kind is few, the easy drying that has, and the welding performance that has is undesirable.
Summary of the invention
Purpose of the present invention just for the shortcoming that overcomes above-mentioned prior art with not enough and provide a kind of have a good welds performance exempt to clean leadless solder for electronic industry, thereby provide quality product for electronics and IT products are unleaded.
The present invention also provides the preparation method of this lead-free solder paste.
The objective of the invention is to realize by following technical proposal:
A kind of leadless solder for electronic industry is characterized in that it is made up of the Pb-free solder powder and the scaling powder of following weight percentage: Pb-free solder powder 87~93%, and scaling powder 7~13%,
Described Pb-free solder powder is made up of following materials by weight percentage: Cu 0.01~2.0%, Ag0.01~4.0%, Ce 0.01~0.5% and surplus are 25~45 microns the powder that Sn makes,
The composition that described scaling powder is made up of following materials by weight percentage: modified rosin 35~45%, thixotropic agent 1~10%, stabilizing agent 0.5~8%, activator 0.5~15% and balance solvent.
Described modified rosin is disproportionated rosin, newtrex and Foral, or the combination of one or both arbitrary proportions in the above-mentioned raw materials; Described thixotropic agent be rilanit special or amide compound or two kinds of arbitrary proportions combination; Described stabilizing agent is calixarene compound or the paraffin or the combination of two kinds of arbitrary proportions; Described activator is the combination of adipic acid, decanedioic acid, perfluor adipic acid, perfluor decanedioic acid, dibromo butene glycol, isopropylamine or triethanolamine one or both or two or more arbitrary proportion wherein; Solvent is polyethylene glycol, 2-ethyl-1,3-hexylene glycol, triethylene glycol list ether and the positive ether of diglycol monotertiary, or the combination of one or both or two or more arbitrary proportion in the above-mentioned raw materials; Described amide compound is palmitic amide, the two stearic amides of second two supports, fatty acid amide or formamide; Described calixarene compound is to phenyl cup [6], to tert-butyl group cup [8] aromatic hydrocarbons or resorcinol cup [4] aromatic hydrocarbons.
The preparation method of lead-free solder paste is characterized in that it is undertaken by following step:
(a) will 35~45% modified rosins add in the container heating and be stirred to fusing fully, under 130~230 ℃ of temperature, add the stirring solvent 5~15 minutes of 1~10% thixotropic agent, 0.5~8% stabilizing agent, 0.5~15% activator and surplus;
(b) behind the cool to room temperature with container closure, and to insert temperature be 1~10 ℃ refrigerating chamber, refrigerates 48 hours and make scaling powder,
(c) at last with 7~13% scaling powders and 87~93% be that 25~45 microns Pb-free solder powder that Sn makes is packed into after solder paste stirrer stirs 10~20 minutes by Cu 0.01~2.0%, Ag 0.01~4.0%, Ce 0.01~0.5% and surplus, divide to install to be sealed in 5~10 ℃ in the Packaging Bottle and to preserve the tin cream products.
Select SnAgCuCe Pb-free solder powder in the lead-free solder paste of the present invention for use, it all reaches lead-free solder and uses standard in raw material mechanical property, solder joint stretching, shearing test, QFP lead-in wire 45 ° of tension tests, slice component solder joint shearing test and wetability, chemical composition, the rate of spread, fusing point, metallographic and performances, can be composite with scaling powder; The scaling powder of selecting for use, wherein modification perfume is disproportionated rosin, newtrex and Foral, it is solid-state that modified rosin is at normal temperatures, unionization, form good, the transparent organic film of air-tightness after the soldering, bump can be wrapped up, completely cut off contacting of atmosphere and other Korrosionsmediums, have the excellent protection performance, solved activity and corrosive contradiction of scaling powder well; The thixotropic agent of selecting for use is rilanit special or amide compound, amide compound is palmitic amide, the two stearic amides of second two supports, fatty acid amide or formamide, it can strengthen the thinning behavior of shear force of soldering paste fluid, improve the printing performance of soldering paste, make soldering paste be easy to demoulding, and the phenomenon of not caving in; The stabilizing agent of selecting for use is calixarene compound or paraffin, calixarene compound is to phenyl cup [6], to tert-butyl group cup [8] aromatic hydrocarbons or resorcinol cup [4] aromatic hydrocarbons, stabilizing agent can strengthen the thick stability of rosin colloidal sol, and it is stable that soldering paste is preserved, and it is rotten to be difficult for layering; The activator of selecting for use is adipic acid, decanedioic acid, perfluor adipic acid, perfluor decanedioic acid, dibromo butene glycol, isopropylamine or triethanolamine, can remove the oxide-film of mother metal and solder surface, the metal on mother metal surface is partly exposed, help mother metal and scolder and under brazing temperature, sprawl, reach good soldering purpose; The activating agent solvent of selecting for use is polyethylene glycol, 2-ethyl-1, in 3-hexylene glycol, triethylene glycol list ether and the positive ether of diglycol monotertiary, the residual corrosivity of postwelding is little, good insulation preformance, a kind of ionization environment can be provided, make the ionization in solvent of rosin and organic acid go on a tour from H
+Ion, solvent also plays a kind of carrier function simultaneously, in welding process, carries free H
+The ion remaval oxide-film carries other scaling powder composition and plays the weldering effect that helps, and solvent also can play the effect of regulating scaling powder concentration and viscosity.
Raw material of the present invention is the commercially available prod.
Product test result of the present invention is as follows:
Test No. | 1 | 2 | 3 | 4 | 5 | 6 |
The rate of spread | 83.2% | 80.1% | 81.4% | 82.1% | 82.4% | 83.1% |
Bronze mirror corrosivity | Do not penetrate | Do not penetrate | Do not penetrate | Do not penetrate | Do not penetrate | Do not penetrate |
Has the good rate of spread from above-mentioned result of the test product of the present invention as can be seen, so suitable welding; The residual corrosivity of postwelding is little, is to be fit to well weld in the microelectronics surface installation technique field use material.
Owing to take technique scheme to make the technology of the present invention compared with the prior art have following advantage and effect:
(a) have the excellent protection performance, solved activity and corrosive contradiction of scaling powder well,
(b) strengthen the thinning behavior of shear force of soldering paste fluid, improve the printing performance of soldering paste, make soldering paste be easy to demoulding, and the phenomenon of not caving in,
(c) strengthen the thick stability of rosin colloidal sol, it is stable that soldering paste is preserved, and it is rotten to be difficult for layering,
(d) have the good rate of spread, the residual corrosivity of postwelding is little, good insulation preformance.
The specific embodiment
Embodiment 1
Disproportionated rosin 20kg, newtrex 11kg and Foral 4kg are added in the container, and heating is also stirred until fusing fully, adds rilanit special 5kg, palmitic amide 5kg under 230 ℃ of temperature; Paraffin 0.5kg; Adipic acid 5kg, decanedioic acid 5kg, perfluor adipic acid 0.5kg, perfluor decanedioic acid 0.5kg, dibromo butene glycol 1kg, triethanolamine 3kg and polyethylene glycol 8kg, 2-ethyl-1,3-hexylene glycol 12kg, the positive ether 4.5kg of diglycol monotertiary, triethylene glycol list ether 15kg stirred after 5 minutes, behind the cool to room temperature with container closure, and to insert temperature be 1 ℃ refrigerating chamber, refrigerate 48 hours and make scaling powder, get at last above-mentioned scaling powder 7kg and 93kg by Cu 0.01kg, Ag 4kg, 25 microns the unleaded glass putty that Ce 0.01kg and Sn 95.98kg make was packed the solder paste stirrer stirring into after 10 minutes, divided to install to 10 ℃ of preservations of sealing tin cream products in the Packaging Bottle.
Embodiment 2
Disproportionated rosin 25kg, newtrex 15kg and Foral 5kg are added in the container, and heating is also stirred until fusing fully, adds rilanit special 4kg under 210 ℃ of temperature; To phenyl cup [6] 6kg, paraffin 2g; Dibromo butene glycol 0.5kg and polyethylene glycol 2kg, 2-ethyl-1,3-hexylene glycol 15kg, the positive ether 10.5kg of diglycol monotertiary, triethylene glycol list ether 15kg stirred after 8 minutes, behind the cool to room temperature with container closure, and to insert temperature be 5 ℃ refrigerating chamber, refrigerate 48 hours and make scaling powder, 30 microns the unleaded glass putty of being made by Cu 1.0kg, Ag 0.1kg, Ce 0.1kg and Sn 98.8kg of getting above-mentioned scaling powder 10kg and the 90kg at last solder paste stirrer of packing into stirred after 12 minutes, divided to install in the Packaging Bottle sealing and preserve the tin cream products for 8 ℃.
Embodiment 3
Disproportionated rosin 30kg and Foral 10kg are added in the container, and heating is also stirred until fusing fully, adds the two stearic amide 1kg of second two supports under 200 ℃ of temperature; To tert-butyl group cup [8] aromatic hydrocarbons 5kg; Adipic acid 5kg, decanedioic acid 5kg, perfluor adipic acid 1kg, isopropylamine 0.5kg and polyethylene glycol 5kg, 2-ethyl-1,3-hexylene glycol 15kg, the positive ether 8kg of diglycol monotertiary, triethylene glycol list ether 14.5kg stirred after 10 minutes, behind the cool to room temperature with container closure, and to insert temperature be 8 ℃ refrigerating chamber, refrigerate 48 hours and make scaling powder, get at last above-mentioned scaling powder 13kg and 87kg by Cu 2.0kg, Ag0.01kg, 45 microns the unleaded glass putty that Ce 0.5kg and Sn 97.49kg make was packed the solder paste stirrer stirring into after 14 minutes, divided to install to 5 ℃ of preservations of sealing tin cream products in the Packaging Bottle.
Embodiment 4
Newtrex 25kg and Foral 18kg are added in the container, and heating is also stirred until fusing fully, adds rilanit special 8kg under 180 ℃ of temperature; Paraffin 3kg; Adipic acid 3kg, decanedioic acid 5kg, perfluor decanedioic acid 0.5kg, dibromo butene glycol 2.5kg and polyethylene glycol 3kg, 2-ethyl-1,3-hexylene glycol 17kg, triethylene glycol list ether 15kg stirred after 12 minutes, behind the cool to room temperature with container closure, and to insert temperature be 10 ℃ refrigerating chamber, refrigerate 48 hours and make scaling powder, get at last above-mentioned scaling powder 10kg and 90kg by Cu 0.05kg, Ag 2kg, 25 microns the unleaded glass putty that Ce 0.05kg and Sn 97.9kg make was packed the solder paste stirrer stirring into after 16 minutes, divided to install to 7 ℃ of preservations of sealing tin cream products in the Packaging Bottle.
Embodiment 5
Disproportionated rosin 35kg is added in the container, and heating is also stirred until fusing fully, adds rilanit special 10kg 150 ℃ of temperature; Paraffin 8kg; Adipic acid 15kg and 2-ethyl-1,3-hexylene glycol 32kg stirred after 14 minutes, behind the cool to room temperature with container closure, and to insert temperature be 8 ℃ refrigerating chamber, refrigerate 48 hours and make scaling powder, 45 microns the unleaded glass putty of being made by Cu 1.5kg, Ag3.0kg, Ce 0.2kg and Sn 95.3kg of getting above-mentioned scaling powder 11kg and the 89kg at last solder paste stirrer of packing into stirred after 18 minutes, divided to install in the Packaging Bottle sealing and preserve the tin cream products for 5 ℃.
Embodiment 6
Newtrex 45kg is added in the container, and heating is also stirred until fusing fully, adds rilanit special 2kg, fatty acid amide or formamide 3kg under 130 ℃ of temperature; Resorcinol cup [4] aromatic hydrocarbons 2kg, paraffin 2kg; Adipic acid 3.5kg, decanedioic acid 2.5kg, perfluor adipic acid 1kg, dibromo butene glycol 5kg, isopropylamine 1kg and 2-ethyl-1,3-hexylene glycol 18kg, triethylene glycol list ether 15kg stirs 15 minutes after evenly, behind the cool to room temperature with container closure, behind the cool to room temperature with container closure, and to insert temperature be 8 ℃ refrigerating chamber, refrigerate 48 hours and make scaling powder, get at last above-mentioned scaling powder 10kg and 90kg by Cu 0.5kg, Ag 3kg, 25 microns the unleaded glass putty that Ce 0.01kg and Sn 96.49kg make was packed the solder paste stirrer stirring into after 20 minutes, divided to install to 7 ℃ of preservations of sealing tin cream products in the Packaging Bottle.
Claims (9)
1, a kind of leadless solder for electronic industry is characterized in that it is made up of the Pb-free solder powder and the scaling powder of following weight percentage: Pb-free solder powder 87~93%, and scaling powder 7~13%,
Described Pb-free solder powder is made up of following materials by weight percentage: Cu 0.01~2.0%, Ag0.01~4.0%, Ce 0.01~0.5% and surplus are 25~45 microns the powder that Sn makes,
The composition that described scaling powder is made up of following materials by weight percentage: modified rosin 35~45%, thixotropic agent 1~10%, stabilizing agent 0.5~8%, activator 0.5~15% and balance solvent.
2, lead-free solder paste according to claim 1 is characterized in that described modified rosin is disproportionated rosin, newtrex and Foral, or the combination of one or both arbitrary proportions in the above-mentioned raw materials.
3, lead-free solder paste according to claim 1 is characterized in that described thixotropic agent is rilanit special or the amide compound or the combination of two kinds of arbitrary proportions.
4, lead-free solder paste according to claim 1 is characterized in that described stabilizing agent is calixarene compound or the paraffin or the combination of two kinds of arbitrary proportions.
5, lead-free solder paste according to claim 1 is characterized in that described activator is the combination of adipic acid, decanedioic acid, perfluor adipic acid, perfluor decanedioic acid, dibromo butene glycol, isopropylamine or triethanolamine one or both or two or more arbitrary proportion wherein.
6, lead-free solder paste according to claim 1, it is characterized in that described solvent is polyethylene glycol, 2-ethyl-1,3-hexylene glycol, triethylene glycol list ether and the positive ether of diglycol monotertiary, or the combination of one or both or two or more arbitrary proportions in the above-mentioned raw materials.
7, lead-free solder paste according to claim 3 is characterized in that described amide compound is palmitic amide, the two stearic amides of second two supports, fatty acid amide or formamide.
8, lead-free solder paste according to claim 4 is characterized in that described calixarene compound is to phenyl cup [6], to tert-butyl group cup [8] aromatic hydrocarbons or resorcinol cup [4] aromatic hydrocarbons.
9, the preparation method of lead-free solder paste according to claim 1 is characterized in that it is undertaken by following step:
(a) will 35~45% modified rosins add in the container heating and be stirred to fusing fully, under 130~230 ℃ of temperature, add the stirring solvent 5~15 minutes of 1~10% thixotropic agent, 0.5~8% stabilizing agent, 0.5~15% activator and surplus;
(b) behind the cool to room temperature with container closure, and to insert temperature be 1~10 ℃ refrigerating chamber, refrigerates 48 hours and make scaling powder,
(c) at last with 7~13% scaling powders and 87~93% be that 25~45 microns Pb-free solder powder that Sn makes is packed into after solder paste stirrer stirs 10~20 minutes by Cu 0.01~2.0%, Ag 0.01~4.0%, Ce 0.01~0.5% and surplus, divide to install to be sealed in 5~10 ℃ in the Packaging Bottle and to preserve the tin cream products.
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CN101508061A (en) * | 2009-03-30 | 2009-08-19 | 汕头市骏码凯撒有限公司 | Welding flux for SnAgCu alloy solder powder and preparation method thereof |
CN101879671A (en) * | 2010-06-13 | 2010-11-10 | 汕头市骏码凯撒有限公司 | Halogen-free flux and method for preparing same |
CN101642855B (en) * | 2009-08-19 | 2012-02-22 | 浙江一远电子材料研究院 | Rear-earth-containing halogen free Sn-Ag-C series tinol |
CN102369083A (en) * | 2009-03-30 | 2012-03-07 | 荒川化学工业株式会社 | Flux composition for lead-free solder, and lead-free solder composition |
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CN111590235A (en) * | 2020-06-11 | 2020-08-28 | 中山翰华锡业有限公司 | Low-dielectric-loss high-reliability soldering paste and preparation method thereof |
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- 2006-09-28 CN CN 200610113439 patent/CN1927526A/en active Pending
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CN102369083B (en) * | 2009-03-30 | 2014-08-20 | 荒川化学工业株式会社 | Flux composition for lead-free solder, and lead-free solder composition |
CN101508061A (en) * | 2009-03-30 | 2009-08-19 | 汕头市骏码凯撒有限公司 | Welding flux for SnAgCu alloy solder powder and preparation method thereof |
CN101642855B (en) * | 2009-08-19 | 2012-02-22 | 浙江一远电子材料研究院 | Rear-earth-containing halogen free Sn-Ag-C series tinol |
CN101879671A (en) * | 2010-06-13 | 2010-11-10 | 汕头市骏码凯撒有限公司 | Halogen-free flux and method for preparing same |
CN101879671B (en) * | 2010-06-13 | 2012-09-19 | 汕头市骏码凯撒有限公司 | Halogen-free flux and method for preparing same |
CN102785039B (en) * | 2012-07-30 | 2015-04-15 | 东莞永安科技有限公司 | Solder paste and preparation method thereof |
CN102785039A (en) * | 2012-07-30 | 2012-11-21 | 东莞永安科技有限公司 | Solder paste and preparation method thereof |
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CN102922162B (en) * | 2012-11-01 | 2014-11-26 | 青岛英太克锡业科技有限公司 | Aluminum welding tin paste and preparation method thereof |
WO2015081622A1 (en) * | 2013-12-04 | 2015-06-11 | 马鑫 | Nano-/micro-particle mixed lead-free solder paste having size effects, and method for preparation thereof |
CN104107989A (en) * | 2014-06-23 | 2014-10-22 | 上海嘉浩新材料科技有限公司 | High-temperature semiconductor solid crystal solder paste and preparation method thereof |
CN104741821A (en) * | 2015-04-17 | 2015-07-01 | 哈尔滨工业大学 | Micro-nano copper particle filled Sn based soldering paste for high-temperature packaging of electronic module and preparation method of soldering paste |
CN104785949A (en) * | 2015-05-12 | 2015-07-22 | 昆山成利焊锡制造有限公司 | Solder powder doped with tin-plated alloyed powder and soldering paste containing solder powder |
CN106607650A (en) * | 2015-10-23 | 2017-05-03 | 东莞市天铖锡业有限公司 | Rare earth cerium solder alloy soldering paste |
CN106825982B (en) * | 2017-02-07 | 2019-04-16 | 深圳市斯特纳新材料有限公司 | A kind of anti-collapse leadless soldering tin paste of low viscosity and preparation method thereof |
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CN106686900A (en) * | 2017-02-24 | 2017-05-17 | 广东成德电子科技股份有限公司 | Method for processing printed circuit board by using calixarene |
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CN110524139A (en) * | 2019-08-06 | 2019-12-03 | 界首市南都华宇电源有限公司 | A kind of scaling powder of low-corrosiveness |
CN111590235A (en) * | 2020-06-11 | 2020-08-28 | 中山翰华锡业有限公司 | Low-dielectric-loss high-reliability soldering paste and preparation method thereof |
CN111590235B (en) * | 2020-06-11 | 2022-04-01 | 中山翰华锡业有限公司 | Low-dielectric-loss high-reliability soldering paste and preparation method thereof |
CN114367762A (en) * | 2020-06-11 | 2022-04-19 | 中山翰华锡业有限公司 | Solder alloy powder, low dielectric loss high reliability soldering paste and preparation method thereof |
CN114367762B (en) * | 2020-06-11 | 2023-08-18 | 中山翰华锡业有限公司 | Solder alloy powder, low dielectric loss and high reliability solder paste and preparation method thereof |
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