CN102513732B - Halogen-free cleaning-free rosin flux, and preparation and application thereof - Google Patents
Halogen-free cleaning-free rosin flux, and preparation and application thereof Download PDFInfo
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Abstract
The invention discloses a halogen-free cleaning-free rosin flux, and preparation and application thereof, and particularly relates to a flux suitable for surface mount lead-free welding paste, preparation of the flux and application of the flux. The flux comprises 20-50% (mass fraction, the same below) of rosin, 5-25% of film-forming agent, 30-50% of high boiling solvent, 3-8% of activator and 2-5% of thixotropic agent, and the flux does not contain any halogen. In order to control growth of interface IMC (intermediate compound) during welding, 0.3-1% of combined inhibitor is added. The welding paste prepared with the flux and lead-free tin-silver-copper powder has the advantages of excellent printing performance, fine weldability, less post-weld residue, thin and even welding spot interface IMC and excellent mechanical property, and is capable of meeting the requirement of high-end electronic products on packaging.
Description
Technical field
The invention belongs to Electronic Packaging soldering paste and use scaling powder field, be specifically related to the controllable halogen-free cleaning-free rosin flux of a kind of interface I MC and methods for making and using same thereof.
Background technology
Along with electronic product is to the future development of microminiaturization, slimming, high precision int, surface installation technique (SMT) becomes one of most popular technology and technique in Electronic Assemblies industry.Soldering paste is indispensable material in SMT, and its performance directly has influence on welding quality, is determining the quality of electronic product.
Scaling powder is the important composition composition of soldering paste, it is mainly made up of solvent, activating agent, film forming agent, corrosion inhibiter etc., the heterogeneity of scaling powder plays specific effect, and wherein the Main Function of corrosion inhibiter is to prevent active material corrosion solder metal and copper substrate in scaling powder.The solder metal of melting and Cu substrate can form interface I MC, and interface I MC is the key factor that affects welding spot reliability, the IMC ramp of welding process median surface, and blocked up IMC causes solder joint degradation, and reliability reduces.How to control the growth of interface I MC, obtaining desirable solder joint becomes the hot issue that people are concerned about.Research in the past concentrates on mostly carries out alloying, substrate surface processing etc. to scolder, to reach the object of improving IMC tissue topography, if YU D Q etc. is at Journal of Alloys and Compounds (2004,376 (1-2): 170-175) upper report: Sn-2.5Ag-0.7Cu alloy is carried out to rare earth RE alloying, add after rare earth scolder matrix and postwelding interface I MC refinement obvious, the corresponding raising of shear strength and hot strength; LIN Y C etc. above report at Scripta Materialia (2007,56 (1): 49-52): phosphorus content plays a decisive role to the growth of SnAgCu/Ni-P interface phase Ni-Sn-P, by the change of P content, IMC are grown and are controlled; And the document addressing this problem from the viewpoint of scaling powder really rarely has report.
Summary of the invention:
The object of invention is to develop a kind of New Flux and methods for making and using same thereof that unleaded SAC soldering paste is used that be suitable for, this scaling powder performance requirement comprises that scaling powder helps weldering performance good, the Solder-Paste Printing performance being made into developed scaling powder is good, postwelding is residual few, corrosivity is little, the growth of welding point interface IMC is controlled, and mechanical performance is good.Technical scheme of the present invention is directly to start with from scaling powder; by adding not organic acid and the organic amine activating agent containing any halogen; in not affecting wetability, reduce to a great extent the residual corrosivity of postwelding; in scaling powder, add compound corrosion inhibitor simultaneously; by the collaborative slow releasing function of corrosion inhibiter; form compact and complete diaphragm at substrate surface; stop or slowed down the diffusion of substrate atoms; thereby reach the object of controlling interface I MC growth (can effectively control thickness, grain size, uniformity etc.), the mechanical performance of solder joint also significantly improves.
A kind of SAC is soldering paste common resin type soldering flux without halogen, is prepared from: rosin 20～50%, resin film forming agent 5～25% by the composition of following mass percent, high boiling solvent 30～50%, activating agent 3～8%, thixotropic agent 2～5%, corrosion inhibiter 0.3～1%.
Described rosin is that one or more in Foral, water-white rosin, disproportionated rosin, newtrex, gum rosin, ester gum combine.
Described resin film forming agent is that one or more in acrylic resin, tristerin, polyethylene glycol, epoxy resin combine.
Described high boiling solvent is that one or more in ethylene glycol, glycerine, diethylene glycol (DEG), methyl carbitol, ethylene glycol monobutyl ether, dibutyl ethylene glycol ether, triethylene glycol butyl ether, ethyl acetate, dimethyl succinate, diethyl succinate, N-methyl-2 pyrrolidones combine.
Described activating agent is oleic acid, stearic acid, succinic acid, glutaric acid, adipic acid, SA, malic acid, citric acid, salicylic acid, di-propionic acid, dimethyl succinic acid, 2, and one or more in 3-dihydroxy formic acid, maleic anhydride, succinic acid amine, monoethanolamine, diethanol amine, triethanolamine, tetradecy lamine combine.
Described thixotropic agent is that one or more in rilanit special, ethylene bis stearic acid amide, thixotropic agent 6500, thixotropic agent 6650 combine.
Described corrosion inhibiter is that two or more in BTA, imidazoles, 2-ethyl imidazol(e), 2-mercaptobenzothiazole, oxine combines.
The preparation method of described scaling powder, specific as follows:
(1) load weighted rosin, resin film forming agent are added in high boiling solvent, be heated to 110～130 DEG C, and be stirred to formation homogeneous mixture;
(2) mixture temperature step (1) being obtained drops to 75-80 DEG C, and load weighted activating agent, thixotropic agent, corrosion inhibiter are added wherein, is constantly stirred to completely and dissolves under 75-80 DEG C of insulation;
(3) step (2) gained mixture is cooled to room temperature rapidly with 30-50 DEG C/min, makes scaling powder.
Described flux application is in the preparation of soldering paste and corresponding surface encapsulation welding procedure for electronic product packaging.Described soldering paste is unleaded SAC soldering paste.
Advantage and the good effect of invention
This scaling powder not containing halide, selects organic acid that activity is moderate, organic amine as activating agent, and scaling powder corrosivity is little, helps weldering property superior.According to the character of lead-free solder and Fundamentals of Welding; science is chosen raw material; selected activating agent, solvent adopt composite mode; can in whole welding process, all work, and all decompose and vapor away in the time that welding completes, postwelding residue is few; needn't clean; selected resin film forming agent and rosin compatibility are good, form the uniform electrical insulating property resin protection film of one deck after welding on pcb board surface, can play waterproof, erosion-resisting effect simultaneously.This scaling powder is controlled the growth of interface I MC by adding compound corrosion inhibitor, and in soldering paste welding process, the active material of scaling powder cleans the oxide-film of Cu substrate, has also increased the diffusion of substrate Cu atom when improving wetability.Composite by corrosion inhibiter, the diaphragm of they and the each self-forming of Cu can be complementary, compactness and the integrality of the polymerization passivation layer of substrate surface are ensured, thereby stop or slowed down substrate Cu atom to the diffusion in scolder matrix, also reduced diffusion and the reaction speed of scolder matrix element to substrate, make like this reaction diffusion phase of IMC obviously be suppressed, crystal boundary diffusion and body diffusion phase are also suppressed, the growth rate of IMC reduces, final acquisition is thin and even, the IMC layer that crystal grain is tiny, thereby improve Interface Microstructure performance, improve the mechanical performance of solder joint.If the amount that corrosion inhibiter adds is very little, do not have good protective effect, added residual increase at most, the addition of compound corrosion inhibitor is between 0.3%～1%.
Brief description of the drawings
Fig. 1 is scaling powder prepared by embodiment 1;
Fig. 2 is scaling powder prepared by embodiment 2;
Fig. 3 is scaling powder prepared by embodiment 3.
Detailed description of the invention
Be intended to further illustrate the present invention below in conjunction with embodiment, and unrestricted the present invention.
Embodiment 1
A kind of Electronic Packaging lead-free solder paste scaling powder, its component and content (wt%) are:
Concrete compound method: weigh methyl carbitol, diethylene glycol (DEG), glycerine and insert in the beaker container of 500 milliliters, by methyl carbitol: diethylene glycol (DEG): glycerine=18: the ratio of 16: 4 is prepared 76 grams of solvents; In above-mentioned joined solvent, add successively 70 grams of Forals, 30 grams of Macrogol 2000s, be heated to 115 DEG C, and be stirred to formation homogeneous mixture; Mixture temperature is dropped to 78 DEG C, 5.6 grams of succinic acid, 4.4 grams of glutaric acids, 3 grams of succinic acid amine, 10 grams of rilanit specials, 0.6 gram of BTA, 0.4 gram of 2-mercaptobenzothiazole are added wherein successively, be constantly stirred to completely and dissolve 78 DEG C of insulations; Be cooled to rapidly room temperature with 50 DEG C/min, make required scaling powder.
The scaling powder (Fig. 1) that the present embodiment is prepared, the thickness lotion that is translucent, pH value is 5.6, density is 1.06g/cm
3.This scaling powder and unleaded Sn3.0Ag0.5Cu solder powder are made into soldering paste in 11.5: 88.5 by mass percentage and weld, solder joint is full, surface-brightening, the rate of spread is 82.5%, postwelding is less residual and be transparence and can exempt cleaning, welding point interface IMC even compact, average thickness is 3.8 μ m, shear strength reaches 45.34Mpa.
Embodiment 2
A kind of Electronic Packaging lead-free solder paste scaling powder, its component and content (wt%) are:
Concrete compound method: weigh dibutyl ethylene glycol ether, diethyl succinate and insert in the beaker container of 500 milliliters, by dibutyl ethylene glycol ether: diethyl succinate=23: 8.4 ratio is prepared 62.8 grams of solvents; In above-mentioned joined solvent, add successively 80 grams of newtrexes, 16 grams of Forals, 16 grams of acrylic resins, 8 grams of tristerins, be heated to 130 DEG C, and be stirred to formation homogeneous mixture; Mixture temperature is dropped to 80 DEG C, by 4.4 gram 2, restrain oneself diacid, 3 grams of maleic anhydrides, 1.2 grams of diethanol amine, 4 grams of ethylene bis stearic acid amides, 1.3 grams of BTAs, 0.3 gram of oxine of 3-dihydroxy formic acid, 3 adds wherein successively, is constantly stirred to completely and dissolves 80 DEG C of insulations; Be cooled to rapidly room temperature with 35 DEG C/min, make required scaling powder.
The scaling powder (Fig. 2) that the present embodiment is prepared, is faint yellow thickness lotion, and pH value is 6.3, and density is 1.06g/cm
3.This scaling powder and unleaded Sn3.0Ag0.5Cu solder powder are made into soldering paste in 11.5: 88.5 by mass percentage and weld, the full light of solder joint, the rate of spread is 83.4%, the residual little and water white transparency of postwelding, can exempt cleaning, welding point interface IMC even compact, average thickness is 3.4 μ m, shear strength reaches 48.01Mpa.
Embodiment 3
A kind of Electronic Packaging lead-free solder paste scaling powder, its component and content (wt%) are:
Concrete compound method: weigh ethylene glycol, triethylene glycol butyl ether and insert in the beaker container of 500 milliliters, by ethylene glycol: triethylene glycol butyl ether=17: 25 ratio is prepared 84 grams of solvents; In above-mentioned joined solvent, add successively 30 grams of water-white rosin, 50 grams of newtrexes, 14 grams of tristerins, be heated to 130 DEG C, and be stirred to formation homogeneous mixture; Mixture temperature is dropped to 80 DEG C, 2 grams of stearic acid, 2 grams of citric acids, 8 grams of succinic acid, 0.4 gram of triethanolamine, 9 grams of rilanit specials, 0.3 gram of imidazoles, 0.3 gram of oxine are added wherein successively, be constantly stirred to completely and dissolve 80 DEG C of insulations; Be cooled to rapidly room temperature with 40 DEG C/min, make required scaling powder
The scaling powder (Fig. 3) that the present embodiment is prepared, is faint yellow thickness lotion, and pH value is 6.1, and density is 1.02g/cm
3.While adopting this scaling powder welding, postwelding is residual few, and solder joint is full, surface-brightening, and the rate of spread is 81.2%, and welding point interface IMC thickness is 4.0 μ m, and shear strength reaches 45.01Mpa.
Claims (3)
1. an Electronic Packaging lead-free solder paste scaling powder, its component and quality percentage composition are:
Concrete compound method: weigh methyl carbitol, diethylene glycol (DEG), glycerine and insert in the beaker container of 500 milliliters, by methyl carbitol: the ratio of diethylene glycol (DEG): glycerine=18:16:4 is prepared 76 grams of solvents; In above-mentioned joined solvent, add successively 70 grams of Forals, 30 grams of Macrogol 2000s, be heated to 115 DEG C, and be stirred to formation homogeneous mixture; Mixture temperature is dropped to 78 DEG C, 5.6 grams of succinic acid, 4.4 grams of glutaric acids, 3 grams of succinic acid amine, 10 grams of rilanit specials, 0.6 gram of BTA, 0.4 gram of 2-mercaptobenzothiazole are added wherein successively, be constantly stirred to completely and dissolve 78 DEG C of insulations; Be cooled to rapidly room temperature with 50 DEG C/min, make required scaling powder.
2. an Electronic Packaging lead-free solder paste scaling powder, its component and quality percentage composition are:
Concrete compound method: weigh dibutyl ethylene glycol ether, diethyl succinate and insert in the beaker container of 500 milliliters, prepare 62.8 grams of solvents by the ratio of dibutyl ethylene glycol ether: diethyl succinate=23:8.4; In above-mentioned joined solvent, add successively 80 grams of newtrexes, 16 grams of Forals, 16 grams of acrylic resins, 8 grams of tristerins, be heated to 130 DEG C, and be stirred to formation homogeneous mixture; Mixture temperature is dropped to 80 DEG C, by 4.4 gram 2, restrain oneself diacid, 3 grams of maleic anhydrides, 1.2 grams of diethanol amine, 4 grams of ethylene bis stearic acid amides, 1.3 grams of BTAs, 0.3 gram of oxine of 3-dihydroxy formic acid, 3 adds wherein successively, is constantly stirred to completely and dissolves 80 DEG C of insulations; Be cooled to rapidly room temperature with 35 DEG C/min, make required scaling powder.
3. an Electronic Packaging lead-free solder paste scaling powder, its component and quality percentage composition are:
Concrete compound method: weigh ethylene glycol, triethylene glycol butyl ether and insert in the beaker container of 500 milliliters, by ethylene glycol: the ratio of triethylene glycol butyl ether=17:25 is prepared 84 grams of solvents; In above-mentioned joined solvent, add successively 30 grams of water-white rosin, 50 grams of newtrexes, 14 grams of tristerins, be heated to 130 DEG C, and be stirred to formation homogeneous mixture; Mixture temperature is dropped to 80 DEG C, 2 grams of stearic acid, 2 grams of citric acids, 8 grams of succinic acid, 0.4 gram of triethanolamine, 9 grams of rilanit specials, 0.3 gram of imidazoles, 0.3 gram of oxine are added wherein successively, be constantly stirred to completely and dissolve 80 DEG C of insulations; Be cooled to rapidly room temperature with 40 DEG C/min, make required scaling powder.
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| CN201110421368.1A CN102513732B (en) | 2011-12-15 | 2011-12-15 | Halogen-free cleaning-free rosin flux, and preparation and application thereof |
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| CN201110421368.1A CN102513732B (en) | 2011-12-15 | 2011-12-15 | Halogen-free cleaning-free rosin flux, and preparation and application thereof |
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| WO2011027659A1 (en) * | 2009-09-03 | 2011-03-10 | 株式会社村田製作所 | Soldering paste, bonding method using same, and bonding structure |
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| EP3878596A4 (en) * | 2018-11-06 | 2022-10-19 | Senju Metal Industry Co., Ltd. | Flux, method for applying flux, and method for mounting solder ball |
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