CN105345314A - Scaling powder used for high-precision nanometer soldering paste - Google Patents
Scaling powder used for high-precision nanometer soldering paste Download PDFInfo
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- CN105345314A CN105345314A CN201510518008.1A CN201510518008A CN105345314A CN 105345314 A CN105345314 A CN 105345314A CN 201510518008 A CN201510518008 A CN 201510518008A CN 105345314 A CN105345314 A CN 105345314A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/22—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by the composition or nature of the material
- B23K35/36—Selection 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
- B23K35/3612—Selection 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/40—Making wire or rods for soldering or welding
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- Electric Connection Of Electric Components To Printed Circuits (AREA)
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Abstract
The invention discloses scaling powder used for high-precision nanometer soldering paste. The raw materials of the scaling powder comprise, by mass, 20%-30% of solvent, 30%-50% of rosin, 3%-8% of surfactant, 2%-5% of thixotropic agents, 5%-10% of organic acid, 2%-5% of organic amine and 2%-5% of inhibiter. Compared with the prior art, the scaling powder used for the high-precision nanometer soldering tin paste has the advantages that 1, each grain of tin powder is wrapped in the scaling powder and makes entire contact with the scaling powder, the tin powder cannot adhere to a net or a scraper in the printing process, and the defects of skipping printing and lessening soldering paste are decreased; 2, the friction among the tin powder is reduced through nanometer particles on the surface of the tin powder, and the printing service life of the soldering paste is prolonged; 3, the thixotropic agents forme a fine anti-setting net-shaped structure, and big crystals cannot be separated out to cause the phenomenon of false thickening; and 4, each grain of the tin powder in the soldering paste keeps in good contact with the scaling powder by adding polyamide resin nanometer powder, and the soldering efficiency of the scaling powder is improved.
Description
Technical field
The present invention relates to technical field of welding materials, be specifically related to a kind of high precision nanometer solder(ing) paste scaling powder.
Background technology
Along with the miniaturization of electronics and IT products, on pcb board, the packing density of components and parts is more and more higher, solder pad space length is more and more less, make various countries also more and more stricter to solder(ing) paste quality requirement, the solder pad space length of ultra fine-pitch and substituting at semiconductor die bond conductive silver glue, the solder(ing) paste of high precision more and more comes into one's own.
Select the scope of glass putty particle diameter according to pad size, along with the spacing of pad size is more and more less, only rely on reduction glass putty particle diameter can not deal with problems completely.The particle diameter of glass putty is less, surface area is larger, oxygen content is also larger, this just needs tin cream scaling powder to have good oxygen scavenging ability, activity easily makes scaling powder and glass putty before use chemical reaction occur and lose efficacy too by force, therefore, when not improving flux activity, raising flux activity and utilization rate can well address this problem.
The printing of ultra-fine size pad requires very strict to the demolding performace of tin cream, the method that traditional dependence thixotropic agent improves solder(ing) paste printing and the demoulding can not adapt to new needs completely.The stream of polyamide is utilized to become and anti-settling effect in prior art, solder(ing) paste is made to have splendid thixotropic property, meet the printing performance of solder(ing) paste, but along with the reduction day by day of pad and spacing dimension, polyamide particle diameter used on market is generally 20 μm, polyamide is that active temperature below fusing point stirs and produces netted thixotroping structure, diameter is less than to the 5#(15-25 μm of 20 μm), 6#(5-15 μm) powder solder(ing) paste, can not reach requirement completely.
Summary of the invention
The object of the invention is to solve above-mentioned technique not enough, utilize the property of nano particle, improve the active service efficiency of scaling powder, strengthen the demolding performace of solder(ing) paste, reach the requirement of accurate printing, welding, a kind of wetability, printing are provided, help weldering property, corrosion resistance good and the leadless soldering tin paste halogen-free flux of 5 ~ 45 μm of glass puttys can be adapted to.
Technical solution of the present invention:
A kind of high-accuracy nanometer solder(ing) paste scaling powder, it is characterized in that: raw materials used and mass percent is: solvent, rosin, surfactant, thixotropic agent, organic acid, organic amine, corrosion inhibiter, and its mass percent is: 20%30%:30%50%:3%8%:2%5%:5%10%:2%5%:2%5%.
Described solvent is one or more combinations in diethylene glycol list octyl ether, tripropylene glycol butyl ether, isopropyl alcohol.
Described rosin is more than two or three combination in disproportionated rosin, maleic rosin, perhydro rosin.
Described surfactant is one or both compositions in OP-10 emulsifying agent, polyoxyethylene glycerol ether.
Described thixotropic agent is polyamide nano-powder.
Described polyamide nano-powder is obtained by following preparation process: polyamide and alcohol solvent join in autoclave by 3:7 mass ratio by (1), and add account for total amount 1% hydroxyethylcellulose as anticoagulant, constantly stir while being heated to 150 ~ 170 DEG C, until polyamide dissolves completely;
(2) continue stir and be cooled to 70 DEG C with 2 DEG C/min speed, separate out the polyamide resin powders particle that particle diameter is 20 ~ 50nm;
(3) stop stirring, after being cooled to room temperature, take out material in autoclave, be separated polyamide resin powders and alcohol solvent, after dry, obtain pure polyamide nano-powder;
(4) as thixotropic agent, the content of polyamide in tin cream scaling powder is 2%-5%.
Described organic acid is one or more combinations in salicylic acid, malic acid, 16 acid, 24 acid.
Described organic amine is one or both combinations in triethanolamine, diethanol amine.
Described corrosion inhibiter is BTA.
A preparation for high precision nanometer solder(ing) paste scaling powder, is characterized in that: comprise the following steps:
One, above-mentioned raw materials is taken in proportion for subsequent use;
Two, solvent, rosin are added in reaction vessel, be heated to 115 DEG C 125 DEG C and be stirred to dissolve completely;
Three, be cooled to 75 DEG C 85 DEG C, add organic acid, organic amine, corrosion inhibiter, control temperature is stirred at 75 DEG C 85 DEG C and fully mixes;
Four, continue to be cooled to 20 DEG C 25 DEG C, add surfactant, thixotropic agent, stir and be evacuated to and mix, obtained mixed solution;
Five, with three-roll grinder, the solid particle in gained mixed solution in step 4 is ground to less than 5 μm, i.e. obtained scaling powder of the present invention, and preserves with stainless steel or plastic containers sealing.
The technology of the present invention and existing technics comparing, tool has the following advantages:
1, in order to reach good thixotropic property, the production technology of current scaling powder generally uses the derivative of rilanit special as thixotropic agent, polyamide is exactly the most frequently used one, the thixotropic agent powdered granule diameter that market uses is generally 20 μm, this is less than 20 μm of (5# for glass putty particle diameter, solder(ing) paste 6#), glass putty can produce little agglomeration (as shown in Figure 1), in printing process, the lubrication of scaling powder is lacked between glass putty and glass putty, the friction aggravation printing lost of life, in welding process, each glass putty is different from the contact surface of scaling powder, part glass putty produces oxidation because helping weldering not enough, form little tin ball phenomenon, use the solder(ing) paste of nanometer technology scaling powder, due to anti-settling cancellated finer and closely woven, guarantee each glass putty all in the parcel of scaling powder, contact completely with scaling powder (as shown in Figure 2), due to the principle of quantum mechanics of nano particle, the nano particle that surface energy is larger can stop glass putty to produce well and reunite, and in printing process, not easily sticky net glues scraper, reduce bite, the defect such as few tin cream,
2, for greater particle size glass putty, common scaling powder is because thixotropic agent particle is larger, be as good as with ordinary solid performance, long-time printing can cause the friction between glass putty and other solid particles, friction extremely to a certain degree, particle surface is roughening, and in printing, easily heating makes active material in glass putty and scaling powder produce chemical reaction solder(ing) paste to be lost efficacy, reduces the printing life-span of solder(ing) paste; The solder(ing) paste that with the addition of nano particle forms fine and closely woven network structure on every solder powder surface, solder powder surface coverage one deck nano particle (as shown in Figure 3), according to principle of quantum mechanics, in the motion process of the very large nano particle printing of surface energy, show great activity, the solid material for making clothes of the larger particles such as glass putty is not easily sticked on printed steel mesh, and the nano particle on glass putty surface decreases the friction between glass putty and glass putty, improves the printing life-span of solder(ing) paste;
3, existing tin cream scaling powder production technology generally no longer stirs in cooling procedure, easily like this in cooling procedure, separates out uncontrollable crystalline size, makes scaling powder produce false thick phenomenon; The present invention, after all raw materials all mix, still stirs with the comparatively slow-speed of revolution, and make scaling powder keep motion state, thixotropic agent can form finer and closely woven anti-settling network structure, is unlikely the larger crystallization of precipitation, causes false thick phenomenon;
4, in the tin cream scaling powder of different formulations, add polyamide nanometer powder, use nano particle technique for packing, make every glass putty in solder(ing) paste keep the contact good with scaling powder, that improves scaling powder helps weldering efficiency.
Accompanying drawing explanation
Fig. 1 is the netted anti-sink structure schematic diagram that conventional polyamide and glass putty are formed.
Fig. 2 is the anti-settling network structure schematic diagram of nanometer polyamide resin of the present invention.
Fig. 3 is the netted anti-sink structure schematic diagram that nanometer scaling powder of the present invention produces in 4# powder tin cream.
Wherein: 1-glass putty; A 2-polyamide material; 3-solvent.
Specific embodiment
Embodiment 1:
1, get polyamide 4g, ethanol 10g, hydroxyethylcellulose 0.14g joins in autoclave, do not stop while being heated to 150 ~ 170 DEG C to stir, until polyamide dissolves completely; Continue stir and be cooled to 70 DEG C with 2 DEG C/min speed, stop stirring being cooled to room temperature, take out material in autoclave, separated powder and solvent, after dry, obtain pure polyamide nano particle 4g;
2, diethylene glycol list octyl ether 28.5g, perhydro rosin 35g, disproportionated rosin 15g are added in reaction vessel, be heated to 115 DEG C of stirrings, until rosin is dissolved in diethylene glycol list octyl ether completely; Be cooled to 75 DEG C, add 16 sour 3g, 24 sour 2.5g, triethanolamine 2g, BTA 3.5g, is stirred well to and mixes; Be cooled to 20 DEG C, add polyoxyethylene glycerol ether 5.5g, polyamide nanometer powder 4g, stir and be evacuated to it and mix, with three-roll grinder, the solid particle in mixed solution is ground to less than 10 μm, i.e. the obtained halogen-free nanometer scaling powder 100g of leadless soldering tin paste.
Embodiment 2:
1, get polyamide 5g, ethanol 11.7g, hydroxyethylcellulose 0.17g joins in autoclave, do not stop while being heated to 150 ~ 170 DEG C to stir, until polyamide dissolves completely; Continue stir and be cooled to 70 DEG C with 2 DEG C/min speed, stop stirring being cooled to room temperature, take out material in autoclave, separated powder and solvent, after dry, obtain pure polyamide nano particle 5g;
2, triethylene glycol butyl ether 30g, perhydro rosin 34g, maleic rosin 13g are added in reaction vessel, be heated to 117 DEG C of stirrings, directly cause rosin and be dissolved in completely in solvent; Be cooled to 77 DEG C, add salicylic acid 4g, 24 sour 3g, triethanolamine 2g, BTA 2.5g, be stirred well to and mix; Be cooled to 22 DEG C, add polyoxyethylene glycerol ether 6.5g, rilanit special 5g, stir and be evacuated to it and mix, with three-roll grinder, the solid particle in mixed solution is ground to less than 10 μm, i.e. the obtained halogen-free nanometer scaling powder 100g of leadless soldering tin paste.
Embodiment 3:
1, get polyamide 5g, ethanol 11.7g, hydroxyethylcellulose 0.17g joins in autoclave, do not stop while being heated to 150 ~ 170 DEG C to stir, until polyamide dissolves completely; Continue stir and be cooled to 70 DEG C with 2 DEG C/min speed, stop stirring being cooled to room temperature, take out material in autoclave, separated powder and solvent, after dry, obtain pure polyamide nano particle 5g;
2, triethylene glycol butyl ether 28g, perhydro rosin 30g, disproportionated rosin 13g, maleic rosin 5g are added in reaction vessel, be heated to 119 DEG C of stirrings, until rosin is dissolved in solvent completely; Be cooled to 79 DEG C, add 24 sour 7g, diethanol amine 2g, BTA 3.5g, is stirred well to and mixes; Be cooled to 22 DEG C, add polyoxyethylene glycerol ether 6.5g, polyamide 5g, stir and be evacuated to it and mix, with three-roll grinder, the solid particle in mixed solution is ground to less than 5 μm, i.e. the obtained halogen-free nanometer scaling powder 100g of leadless soldering tin paste.
The preparation of the conventional tin cream scaling powder of embodiment 4():
Triethylene glycol butyl ether 28g, perhydro rosin 30g, disproportionated rosin 12g, maleic rosin 5g are added in reaction vessel, is heated to 121 DEG C of stirrings, until rosin is dissolved in solvent completely; Be cooled to 81 DEG C, add 16 sour 5g, salicylic acid 2.5g, diethanol amine 2g, BTA 3.5g, is stirred well to and mixes; Be cooled to 25 DEG C, add OP-10 emulsifying agent 7g, rilanit special 5g, stir and be evacuated to it and mix, with three-roll grinder, the solid particle in mixed solution is ground to less than 10 μm, i.e. obtained conventional lead-free solder(ing) paste halogen-free flux 100g.
Four scaling powder samples that four embodiments are obtained press glass putty respectively: the percentage by weight of scaling powder=88.5%:11.5% mixes with SAC305 glass putty (6#), and make solder(ing) paste, and test according to Its Relevant Technology Standards, its test result is as shown in table 1.
Contrasted from test data of experiment in table 1, compared with the solder(ing) paste adopting the technology of the present invention product to make scaling powder makes the solder(ing) paste of scaling powder with employing prior art products, in the application of fine powder solder(ing) paste, the stability of its properties promotes all to some extent, and the storage life of product and service life are all longer.
Same formula scaling powder performance test contrast prepared by table 1 two kinds of techniques
Four obtained for four embodiments scaling powder samples are pressed glass putty respectively: the percentage by weight of scaling powder=88.5%:11.5% mixes with SAC305 glass putty (4#), makes solder(ing) paste, and it is as shown in table 2 to carry out testing its test result according to Its Relevant Technology Standards.
Contrasted from test data of experiment in table 2, compared with the solder(ing) paste adopting the technology of the present invention product to make scaling powder makes the solder(ing) paste of scaling powder with employing prior art products, in the application of conventional powder solder(ing) paste, its demolding performace promotes to some extent, and storage life and the service life of product extend all to some extent.
Same formula scaling powder performance test contrast prepared by table 2 two kinds of techniques
Claims (10)
1. a high-accuracy nanometer solder(ing) paste scaling powder, it is characterized in that: raw materials used and mass percent is: solvent, rosin, surfactant, thixotropic agent, organic acid, organic amine, corrosion inhibiter, and its mass percent is: 20% 30%:30% 50%:3% 8%:2% 5%:5% 10%:2% 5%:2% 5%.
2. a kind of high-accuracy nanometer solder(ing) paste scaling powder according to claim 1, is characterized in that: described solvent is one or more combinations in diethylene glycol list octyl ether, tripropylene glycol butyl ether, isopropyl alcohol.
3. a kind of high-accuracy nanometer solder(ing) paste scaling powder according to claim 1, is characterized in that: described rosin is more than two or three combination in disproportionated rosin, maleic rosin, perhydro rosin.
4. a kind of high-accuracy nanometer solder(ing) paste scaling powder according to claim 1, is characterized in that: described surfactant is one or both compositions in OP-10 emulsifying agent, polyoxyethylene glycerol ether.
5. a kind of high-accuracy nanometer solder(ing) paste scaling powder according to claim 1, is characterized in that: described thixotropic agent is polyamide nano-powder.
6. a kind of high-accuracy nanometer solder(ing) paste scaling powder according to claim 5, it is characterized in that: described polyamide nano-powder is obtained by following preparation process: polyamide and alcohol solvent join in autoclave by 3:7 mass ratio by (1), and add account for total amount 1% hydroxyethylcellulose as anticoagulant, constantly stir while being heated to 150 ~ 170 DEG C, until polyamide dissolves completely;
(2) continue stir and be cooled to 70 DEG C with 2 DEG C/min speed, separate out the polyamide resin powders particle that particle diameter is 20 ~ 50nm;
(3) stop stirring, after being cooled to room temperature, take out material in autoclave, be separated polyamide resin powders and alcohol solvent, after dry, obtain pure polyamide nano-powder;
(4) as thixotropic agent, the content of polyamide in tin cream scaling powder is 2%-5%.
7. a kind of high-accuracy nanometer solder(ing) paste scaling powder according to claim 1, is characterized in that: described organic acid is one or more combinations in salicylic acid, malic acid, 16 acid, 24 acid.
8. a kind of high-accuracy nanometer solder(ing) paste scaling powder according to claim 1, is characterized in that: described organic amine is one or both combinations in triethanolamine, diethanol amine.
9. a kind of high-accuracy nanometer solder(ing) paste scaling powder according to claim 1, is characterized in that: described corrosion inhibiter is BTA.
10. a preparation for high precision nanometer solder(ing) paste scaling powder, is characterized in that: comprise the following steps:
One, above-mentioned raw materials is taken in proportion for subsequent use;
Two, solvent, rosin are added in reaction vessel, be heated to 115 DEG C 125 DEG C and be stirred to dissolve completely;
Three, be cooled to 75 DEG C 85 DEG C, add organic acid, organic amine, corrosion inhibiter, control temperature is stirred at 75 DEG C 85 DEG C and fully mixes;
Four, continue to be cooled to 20 DEG C 25 DEG C, add surfactant, thixotropic agent, stir and be evacuated to and mix, obtained mixed solution;
Five, with three-roll grinder, the solid particle in gained mixed solution in step 4 is ground to less than 5 μm, i.e. obtained scaling powder of the present invention, and preserves with stainless steel or plastic containers sealing.
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| 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 |
| CN107442969A (en) * | 2017-09-08 | 2017-12-08 | 苏州汉尔信电子科技有限公司 | A kind of nanometer weld-aiding cream and low-temperature environment-friendly type nanometer solder(ing) paste and preparation method thereof |
| CN109676284A (en) * | 2018-12-13 | 2019-04-26 | 上海锡喜材料科技有限公司 | Weld-aiding cream and preparation method thereof |
| CN110869162A (en) * | 2017-07-12 | 2020-03-06 | 千住金属工业株式会社 | Flux for soldering and solder paste |
| CN111390429A (en) * | 2020-04-21 | 2020-07-10 | 深圳市唯特偶新材料股份有限公司 | Soldering paste with three-proofing effect for film forming after welding and preparation method thereof |
| CN111872599A (en) * | 2020-07-01 | 2020-11-03 | 潮州三环（集团）股份有限公司 | Modified tin powder and tin paste |
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| 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 |
| CN110869162A (en) * | 2017-07-12 | 2020-03-06 | 千住金属工业株式会社 | Flux for soldering and solder paste |
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| CN109676284A (en) * | 2018-12-13 | 2019-04-26 | 上海锡喜材料科技有限公司 | Weld-aiding cream and preparation method thereof |
| CN111390429A (en) * | 2020-04-21 | 2020-07-10 | 深圳市唯特偶新材料股份有限公司 | Soldering paste with three-proofing effect for film forming after welding and preparation method thereof |
| CN111872599A (en) * | 2020-07-01 | 2020-11-03 | 潮州三环（集团）股份有限公司 | Modified tin powder and tin paste |
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