CN1951621A - Leadless solder paste and its preparation method - Google Patents
Leadless solder paste and its preparation method Download PDFInfo
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- CN1951621A CN1951621A CN 200610070003 CN200610070003A CN1951621A CN 1951621 A CN1951621 A CN 1951621A CN 200610070003 CN200610070003 CN 200610070003 CN 200610070003 A CN200610070003 A CN 200610070003A CN 1951621 A CN1951621 A CN 1951621A
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- soldering tin
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Abstract
The invention relates to a leadless solder paste, and relative production. Wherein, it is mixed by Sn-Cu-Ag tin substrate alloy powder and carrier medium. And it is characterized in that: it adds hydroxyl alkylamine into carrier medium, and uses hydroxyl alkylamine as active catalyst, to obtain the solder paste with high reliability, held welding property, and improved activity. The invention can improve the smooth of welding point.
Description
Technical field:
The present invention relates to the electronic product technical field of surface, is a kind of leadless soldering tin paste and preparation method thereof specifically, is mainly used in the electronic product surface mount, is particularly useful for using the electronic product of solder reflow process.
Background technology:
Traditional solder(ing) paste product is made up of tin-lead solder powder and solder flux, and tin-lead solder wherein is generally 63%Sn, the 37%Pb of 20-45 micron or 62%Sn, 36%Pb, the 2%Ag spherical powder constitutes; Solder flux generally is made of resin, activator, thixotropic agent, solvent, additive.Along with the development of electronics industry, electronic assemblies is increasingly sophisticated and accurate, and the kind of solder(ing) paste also increases thereupon, and the selection of solder(ing) paste not only will cooperate the needs of production, also it is also noted that the generation of side effect and avoids adverse consequences simultaneously.For fear of the harm of leaded solder(ing) paste, thereby select leadless soldering tin paste for use.Usually the alloy as lead-free solder has Sn-Ag system, Sn-Bi system, Sn-Zn system.Sn-Bi is that mechanical performance can not be satisfactory, and Sn-Zn is easy oxidation, thereby generally selects Sn-Cu-Ag system for use, but the performance that Sn-Cu-Ag ties up on wetability and the light characteristic is relatively poor, not as the SnPb alloy.
Summary of the invention:
The objective of the invention is to overcome the deficiency of above-mentioned prior art, and a kind of leadless soldering tin paste is provided, mainly solved existing leadless soldering tin paste wetability and the relatively poor problem of brightness.
Another object of the present invention has provided a kind of preparation method of leadless soldering tin paste.
In order to achieve the above object, the present invention is achieved in that a kind of leadless soldering tin paste, and it is to be mixed and made into by Sn-Cu-Ag kamash alloy powder and mounting medium, and its special character is to add hydroxy alkyl amine in mounting medium.
A kind of leadless soldering tin paste of the present invention, described mounting medium contains solvent alcohol ether 25-40%, rosin and derivative 50-68% thereof, crude vegetal thixotropic agent 5-12.5% by weight, organic acid for activating agent 0.5-2%, hydroxy alkyl amine 0.5-2.5%; Sn-Cu-Ag kamash alloy powder is general raw material, and the mixed proportion of mounting medium and Sn-Cu-Ag kamash alloy powder is 0.8-1.2: 8.8-9.2 by weight.
A kind of leadless soldering tin paste of the present invention, a kind of scheme preferably is: mounting medium comprises solvent alcohol ether 30-35%, rosin and derivative 55-63% thereof, crude vegetal thixotropic agent 6-10.5% by weight, organic acid for activating agent 0.7-1.5%, hydroxy alkyl amine 0.5-2.5%.
A kind of leadless soldering tin paste of the present invention, a kind of preferred version is: mounting medium comprises solvent alcohol ether 30.7%, rosin and derivative 60% thereof, crude vegetal thixotropic agent 7% by weight, organic acid for activating agent 0.8%, hydroxy alkyl amine 1.5%; Sn-Cu-Ag kamash alloy powder contains tin 96.5%, copper 0.5%, silver 3% by weight, and the mixed proportion of mounting medium and Sn-Cu-Ag kamash alloy powder is 0.82: 8.8 by weight.
A kind of leadless soldering tin paste of the present invention, the hydroxy radical content of its described hydroxy alkyl amine are 11-19%, and the amine value is 150-190.
A kind of leadless soldering tin paste of the present invention, its described mounting medium also contains additive, additive is one or more in releasing agent, antioxidant, polymerization inhibitor and the surfactant, its consumption is consumption routinely, and optimum amount is that benchmark is respectively releasing agent 0.3-0.8%, antioxidant 0.01-1.5%, polymerization inhibitor 0.01-4%, surfactant 0.3-1.8% by weight with the mounting medium; Described releasing agent can be silicone oil, liquid wax; Antioxidant can be triphenyl phosphorous oxide, BTA; Polymerization inhibitor can be resorcinol, hydroquinones; Surfactant can be polyoxyethylated alkyl phenol, poly amic acid.
A kind of leadless soldering tin paste of the present invention, its described solvent alcohol ether be in DGDE acetic acid esters, diethylene glycol monobutyl ether, diglycol monotertiary hexyl ether, diethylene glycol monobutyl ether acetic acid esters, 2-methyl-hexylene glycol, ethylene glycol monobutyl ether, propylene glycol monobutyl ether, polyethylene glycol butyl oxide, diethylene glycol dibutyl ether, the tripropylene glycol monobutyl ether one or both and two or more; Described rosin and derivative thereof be in newtrex, natural grease rosin, Foral, disproportionation rosin, partially polymerized rosin, Foral glyceride, the rosin pentaerythritol ester one or both and two or more; Described crude vegetal thixotropic agent be in rilanit special, modified hydrogenated castor oil, glycerine monofatty ester, the fatty acid glyceryl ester one or both and two or more; Described organic acid for activating agent is succinic acid, glutaric acid, adipic acid, salicylic acid, phthalic acid, tetrabutylammonium hydrogen bromic acid amine, diphenylguanidine hydrobromate, 2,3-two bromo-2-butene-1s, one or both in 4-glycol, the guanidine hydrochloride and two or more; Described hydroxy alkyl amine be in AEEA, monoethanolamine, diethanol amine, triethanolamine, N-hydroxyethyl piperazine, methylol diethyl triamine, methylol ethylenediamine, dihydroxy ethyl ethylenediamine, the ethoxy diethylenetriamine one or both and two or more.
The preparation method of a kind of leadless soldering tin paste of the present invention, earlier each component with mounting medium mixes by proportioning, heats until dissolving fully, leaves standstill naturally to room temperature, puts temperature into and be 1-10 ℃ refrigerating chamber, refrigerates stand-by after 48 hours; Then mounting medium and Sn-Cu-Ag kamash alloy powder are put with the ratio of 0.8-1.2: 8.8-9.2 and be stirred in the vacuum dispersion machine evenly, sealing is preserved in the Packaging Bottle of packing into then, and this storage temperature remains on 5-10 ℃ and gets final product.
Compared with the prior art a kind of leadless soldering tin paste of the present invention and preparation method thereof has outstanding substantive distinguishing features and marked improvement: 1, to have wetability strong for leadless soldering tin paste, the brightness height, good surface activity, lotion uniform and smooth, lotion have splendid thixotropy and higher viscosity, good slow curing; 2, under preservation condition, do not decompose down as the medium and the coexistence of scolding tin metal of carrier, keep the activity of media compositions, do not produce ionic halogen atom, the melting state fully decomposes down, makes the scolding tin wetability stronger, and brightness is higher, is kilter.
The specific embodiment:
In order to understand better and to implement, describe a kind of leadless soldering tin paste of the present invention and preparation method thereof in detail below in conjunction with embodiment.
Embodiment 1, accurately takes by weighing following various raw material, 30g newtrex and 30g disproportionation rosin, the modified hydrogenated castor oil of 7g, 0.8g glutaric acid and 2,3-two bromo-2-butene-1s, 4-glycol, 1.5g AEEA, 30g diethylene glycol dibutyl ether, 0.7g triphenyl phosphorous oxide; Above-mentioned each component is mixed by proportioning, heat after dissolving fully, generate the mounting medium of leadless soldering tin paste.Naturally leave standstill that to put temperature to the room temperature into be 5 ℃ refrigerating chamber, refrigerate stand-by after 48 hours; Then mounting medium and general Sn-Cu-Ag kamash alloy powder are put with 1.15: 8.85 weight ratio and be stirred in the vacuum dispersion machine evenly, sealing is preserved in the Packaging Bottle of packing into then, and this storage temperature remains on 8 ℃ and gets final product.
The comparative example 1, accurately take by weighing following various raw material, 30g newtrex and 30g disproportionation rosin, the modified hydrogenated castor oil of 7g, 0.8g glutaric acid and 2,3-two bromo-2-butene-1s, 4-glycol, 32.2g the additive of diethylene glycol dibutyl ether and conventional amount used mixes the back by proportioning and is the mounting medium of leadless soldering tin paste; Accurately take by weighing Sn-Cu-Ag kamash alloy powder then, the weight ratio of mounting medium and general Sn-Cu-Ag kamash alloy powder is 1.15: 8.85, and technology is made the Pb-free solder powder routinely then.
Embodiment 2, accurately take by weighing following mounting medium, the partially polymerized rosin of 28g natural grease rosin and 32g, 7g rilanit special, 0.8g salicylic acid and diphenylguanidine hydrobromate, 1.5g methylol ethylenediamine, 30g diglycol monotertiary hexyl ether, 0.7g BTA; Above-mentioned each component is mixed by proportioning, heat after dissolving fully, generate the mounting medium of leadless soldering tin paste.Naturally leave standstill that to put temperature to the room temperature into be 6 ℃ refrigerating chamber, refrigerate stand-by after 48 hours; Then mounting medium and general Sn-Cu-Ag kamash alloy powder are put with 1.1: 8.9 weight ratio and be stirred in the vacuum dispersion machine evenly, sealing is preserved in the Packaging Bottle of packing into then, and this storage temperature remains on 7 ℃ and gets final product.
The comparative example 2, accurately take by weighing following various raw material, the partially polymerized rosin of 28g natural grease rosin and 32g, 7g rilanit special, 0.8g salicylic acid and diphenylguanidine hydrobromate, the additive of 32.2g diglycol monotertiary hexyl ether and conventional amount used; Mix the back by proportioning and be the mounting medium of leadless soldering tin paste; Accurately take by weighing Sn-Cu-Ag kamash alloy powder then, the weight ratio of mounting medium and general Sn-Cu-Ag kamash alloy powder is 1.1: 8.9, and technology is made the Pb-free solder powder routinely then.
Embodiment 3, accurately take by weighing following various raw material, the 68g Foral, 5g glycerine monofatty ester and rilanit special, the 1g succinic acid, 1g monoethanolamine and diethanol amine, 25g DGDE acetic acid esters and diethylene glycol monobutyl ether acetic acid esters, wherein the hydroxy radical content of monoethanolamine and diethanol amine is 11-19%, and the amine value is 150-190; Above-mentioned each component is mixed by proportioning, heat after dissolving fully, generate the mounting medium of leadless soldering tin paste.Naturally leave standstill that to put temperature to the room temperature into be 1 ℃ refrigerating chamber, refrigerate stand-by after 48 hours; Then mounting medium and Sn-Cu-Ag kamash alloy powder are put with 0.8: 8.8 weight ratio and in the vacuum dispersion machine, be stirred to evenly, Sn-Cu-Ag kamash alloy powder contains tin 96.5%, copper 0.5%, silver 3% by weight percentage, sealing is preserved in the Packaging Bottle of packing into then, and this storage temperature remains on 5 ℃ and gets final product.
Embodiment 4, accurately take by weighing following various raw material, 50g Foral, hydrogenated rosin glyceride and rosin pentaerythritol ester, 5.5g rilanit special, modified hydrogenated castor oil and fatty acid glyceryl ester, the 2g adipic acid, 2.5g diethanol amine, triethanolamine and methylol diethyl triamine, 40g ethylene glycol monobutyl ether, propylene glycol monobutyl ether, polyethylene glycol butyl oxide; Above-mentioned each component is mixed by proportioning, heat after dissolving fully, generate the mounting medium of leadless soldering tin paste.Naturally leave standstill that to put temperature to the room temperature into be 10 ℃ refrigerating chamber, refrigerate stand-by after 48 hours; Then mounting medium and general Sn-Cu-Ag kamash alloy powder are put with 1.2: 9.2 weight ratio and be stirred in the vacuum dispersion machine evenly, sealing is preserved in the Packaging Bottle of packing into then, and this storage temperature remains on 10 ℃ and gets final product.
Embodiment 5, accurately take by weighing following mounting medium, the 60g Foral, the 7g rilanit special, 0.8g glutaric acid, 1.5g dihydroxy ethyl ethylenediamine, 30g tripropylene glycol monobutyl ether, 0.7g silicone oil, triphenyl phosphorous oxide and resorcinol, above-mentioned each component is mixed by proportioning, heat after dissolving fully, generate the mounting medium of leadless soldering tin paste.Naturally leave standstill that to put temperature to the room temperature into be 4 ℃ refrigerating chamber, refrigerate stand-by after 48 hours; Then mounting medium and Sn-Cu-Ag kamash alloy powder are put with 0.82: 8.8 weight ratio and in the vacuum dispersion machine, be stirred to evenly, Sn-Cu-Ag kamash alloy powder contains tin 96.5%, copper 0.5%, silver 3% by weight percentage, sealing is preserved in the Packaging Bottle of packing into then, and this storage temperature remains on 6 ℃ and gets final product.
Embodiment 6, accurately take by weighing following mounting medium, the 55g newtrex, 12.5g fatty acid glyceryl ester, 0.5g phthalic acid, 0.5g N-hydroxyethyl piperazine, 31.5g diethylene glycol monobutyl ether and 2-methyl-hexylene glycol, above-mentioned each component is mixed by proportioning, heat after dissolving fully, generate the mounting medium of leadless soldering tin paste.Naturally leave standstill that to put temperature to the room temperature into be 8 ℃ refrigerating chamber, refrigerate stand-by after 48 hours; Then mounting medium and general Sn-Cu-Ag kamash alloy powder are put with 0.9: 9.0 weight ratio and be stirred in the vacuum dispersion machine evenly, sealing is preserved in the Packaging Bottle of packing into then, and this storage temperature remains on 9 ℃ and gets final product.
Embodiment 7, accurately take by weighing following mounting medium, 63g newtrex and natural rosin, the 6g glycerine monofatty ester, 0.7g tetrabutylammonium hydrogen bromic acid amine and guanidine hydrochloride, 1.3g dihydroxy ethyl ethylenediamine and ethoxy diethylenetriamine, 29g tripropylene glycol monobutyl ether, above-mentioned each component is mixed by proportioning, heat after dissolving fully, generate the mounting medium of leadless soldering tin paste.Naturally leave standstill that to put temperature to the room temperature into be 2 ℃ refrigerating chamber, refrigerate stand-by after 48 hours; Then mounting medium and Sn-Cu-Ag kamash alloy powder are put with 1.0: 9.0 weight ratio and in the vacuum dispersion machine, be stirred to evenly, Sn-Cu-Ag kamash alloy powder contains tin 96.5%, copper 0.5%, silver 3% by weight percentage, sealing is preserved in the Packaging Bottle of packing into then, and this storage temperature remains on 7.5 ℃ and gets final product.
Embodiment 8, accurately take by weighing following mounting medium, 52g Foral, 10.5g rilanit special, 1.5g succinic acid, 0.8g AEEA, 35g tripropylene glycol monobutyl ether, 0.2g silicone oil, wherein the hydroxy radical content of AEEA is 11-19%, and the amine value is 150-190; Above-mentioned each component is mixed by proportioning, heat after dissolving fully, generate the mounting medium of leadless soldering tin paste.Naturally leave standstill that to put temperature to the room temperature into be 3 ℃ refrigerating chamber, refrigerate stand-by after 48 hours; Then mounting medium and general Sn-Cu-Ag kamash alloy powder are put with 0.95: 9.1 weight ratio and be stirred in the vacuum dispersion machine evenly, sealing is preserved in the Packaging Bottle of packing into then, and this storage temperature remains on 8 ℃ and gets final product.
A kind of leadless soldering tin paste of the present invention, its performance test is as follows:
1, wetability test:
This test is implemented according to the appendix 10 of the JIS-Z-3284 method that is used for solder(ing) paste.Metallic membrane is placed on the test film that cleaned in advance, and solder(ing) paste is coated on the metal otter board, to be full of the hole of web plate.After removing web plate, the heat run sheet and behind solder fusing 5 seconds kinds stop heating, the expansion degree of cooling scolder and check scolder is represented degree of expansion according to following classification on horizontal level.
The wetting base material test film in 1 solder(ing) paste fusing back, and launch greatlyyer than surface covered
The All Ranges of 2 coating solder(ing) pastes is by solder
Most of zone of 3 coating solder(ing) pastes is by solder
4 test films are not by solder, and the scolder of fusing is rendered as one or more solder balls.
2, microscope figure is adopted in the brightness test.
Test result such as table 1:
Table 1
| Mounting medium hydroxyl alkylamine | The wetability measure of merit | Brightness | |
| Embodiment 1 | 1.5% AEEA | 1 | Good |
| Embodiment 2 | 1.5% methylol ethylenediamine | 1 | Good |
| The comparative example 1 | Do not have | 3 | Generally |
| The comparative example 2 | Do not have | 3 | Generally |
As can be known from Table 1, all less than the pad of solder(ing) paste and coating, in contrast, embodiment 1,2 maintains high wetting activity in wetting expansion shown in the comparative example, show as from the solder test film of solder(ing) paste fusing, and launch greatlyyer than surface covered; Can find out that from microscope figure embodiment 1,2 brightness are higher.
Claims (10)
1, a kind of leadless soldering tin paste, it is to be mixed and made into by Sn-Cu-Ag kamash alloy powder and mounting medium, it is characterized in that adding in mounting medium hydroxy alkyl amine.
2, a kind of leadless soldering tin paste according to claim 1, it is characterized in that mounting medium contains solvent alcohol ether 25-40%, rosin and derivative 50-68% thereof, crude vegetal thixotropic agent 5-12.5% by weight, organic acid for activating agent 0.5-2%, hydroxy alkyl amine 0.5-2.5%; The mixed proportion of mounting medium and Sn-Cu-Ag kamash alloy powder is 0.8-1.2: 8.8-9.2 by weight.
3, a kind of leadless soldering tin paste according to claim 1 and 2, the hydroxy radical content that it is characterized in that described hydroxy alkyl amine is 11-19%, the amine value is 150-190.
4, according to claim 1 or 2 or 3 described a kind of leadless soldering tin pastes, it is characterized in that mounting medium also contains additive, additive is one or more in releasing agent, antioxidant, polymerization inhibitor and the surfactant.
5, a kind of leadless soldering tin paste according to claim 2, it is characterized in that described solvent alcohol ether be in DGDE acetic acid esters, diethylene glycol monobutyl ether, diglycol monotertiary hexyl ether, diethylene glycol monobutyl ether acetic acid esters, 2-methyl-hexylene glycol, ethylene glycol monobutyl ether, propylene glycol monobutyl ether, polyethylene glycol butyl oxide, diethylene glycol dibutyl ether, the tripropylene glycol monobutyl ether one or both and two or more.
6, a kind of leadless soldering tin paste according to claim 2, it is characterized in that described rosin and derivative thereof be in newtrex, natural grease rosin, Foral, disproportionation rosin, partially polymerized rosin, Foral glyceride, the rosin pentaerythritol ester one or both and two or more.
7, a kind of leadless soldering tin paste according to claim 2, it is characterized in that described crude vegetal thixotropic agent be in rilanit special, modified hydrogenated castor oil, glycerine monofatty ester, the fatty acid glyceryl ester one or both and two or more.
8, a kind of leadless soldering tin paste according to claim 2, it is characterized in that described organic acid for activating agent is succinic acid, glutaric acid, adipic acid, salicylic acid, phthalic acid, tetrabutylammonium hydrogen bromic acid amine, diphenylguanidine hydrobromate, 2,3-two bromo-2-butene-1s, one or both in 4-glycol, the guanidine hydrochloride and two or more.
9, according to claim 1 or 2 or 3 described a kind of leadless soldering tin pastes, it is characterized in that described hydroxy alkyl amine be in AEEA, monoethanolamine, diethanol amine, triethanolamine, N-hydroxyethyl piperazine, methylol diethyl triamine, methylol ethylenediamine, dihydroxy ethyl ethylenediamine, the ethoxy diethylenetriamine one or both and two or more.
10, the preparation method of the described a kind of leadless soldering tin paste of claim 1, each component raw material with the mounting medium part mix by proportioning earlier, heat until dissolving fully, leave standstill naturally to room temperature, put temperature into and be 1-10 ℃ refrigerating chamber, refrigerate stand-by after 48 hours; Then mounting medium and Sn-Cu-Ag kamash alloy powder are put with the ratio of 0.8-1.2: 8.8-9.2 and be stirred in the vacuum dispersion machine evenly, sealing is preserved in the Packaging Bottle of packing into then, and this storage temperature remains on 5-10 ℃ and gets final product.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102107340A (en) * | 2009-12-24 | 2011-06-29 | 汉高股份有限及两合公司 | Solder paste composition, solder paste and soldering flux |
| CN102166689A (en) * | 2011-03-30 | 2011-08-31 | 浙江强力焊锡材料有限公司 | Halogen-free lead-free soldering paste and soldering flux used by same |
| CN104308388A (en) * | 2010-11-26 | 2015-01-28 | 深圳市晨日科技有限公司 | Die-bond soldering paste for high-power LED and preparation method of die-bond soldering paste |
| CN107309577A (en) * | 2016-04-27 | 2017-11-03 | 赛伦（厦门）新材料科技有限公司 | One kind is applied to signal distributor solder(ing) paste and preparation method thereof |
| CN110418692A (en) * | 2017-03-31 | 2019-11-05 | 三菱综合材料株式会社 | Engagement formed body and its manufacturing method |
| CN111151910A (en) * | 2020-01-07 | 2020-05-15 | 杭州乔泰电子有限公司 | Lead-free soldering paste |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JPH10249577A (en) * | 1997-03-10 | 1998-09-22 | Nippon Superia Shiya:Kk | Soldering cream |
| JP2002086292A (en) * | 2000-02-08 | 2002-03-26 | Showa Denko Kk | Solder paste |
| CN1295054C (en) * | 2003-08-20 | 2007-01-17 | 中国科学院金属研究所 | Sn-Ag-Cu-X eutectic alloy leadless welding materials for electronic elements |
| CN1318182C (en) * | 2004-03-17 | 2007-05-30 | 上海博物馆 | Chlorine free soldering flux and its application in bronze historical relics soldering repair |
| CN100336626C (en) * | 2005-08-12 | 2007-09-12 | 北京工业大学 | Rosin halogen-free scaling powder for lead-free soldering paste |
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2006
- 2006-10-27 CN CNB2006100700038A patent/CN100425385C/en not_active Expired - Fee Related
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102107340A (en) * | 2009-12-24 | 2011-06-29 | 汉高股份有限及两合公司 | Solder paste composition, solder paste and soldering flux |
| CN104308388A (en) * | 2010-11-26 | 2015-01-28 | 深圳市晨日科技有限公司 | Die-bond soldering paste for high-power LED and preparation method of die-bond soldering paste |
| CN102166689A (en) * | 2011-03-30 | 2011-08-31 | 浙江强力焊锡材料有限公司 | Halogen-free lead-free soldering paste and soldering flux used by same |
| CN102166689B (en) * | 2011-03-30 | 2013-05-22 | 浙江强力焊锡材料有限公司 | Halogen-free lead-free soldering paste and soldering flux used by same |
| CN107309577A (en) * | 2016-04-27 | 2017-11-03 | 赛伦（厦门）新材料科技有限公司 | One kind is applied to signal distributor solder(ing) paste and preparation method thereof |
| CN110418692A (en) * | 2017-03-31 | 2019-11-05 | 三菱综合材料株式会社 | Engagement formed body and its manufacturing method |
| CN111151910A (en) * | 2020-01-07 | 2020-05-15 | 杭州乔泰电子有限公司 | Lead-free soldering paste |
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