CN114571138B - Environment-friendly soldering flux and preparation method and application thereof - Google Patents
Environment-friendly soldering flux and preparation method and application thereof Download PDFInfo
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- CN114571138B CN114571138B CN202011384129.9A CN202011384129A CN114571138B CN 114571138 B CN114571138 B CN 114571138B CN 202011384129 A CN202011384129 A CN 202011384129A CN 114571138 B CN114571138 B CN 114571138B
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- 230000004907 flux Effects 0.000 title claims abstract description 72
- 238000005476 soldering Methods 0.000 title claims abstract description 59
- 238000002360 preparation method Methods 0.000 title description 14
- 238000007716 flux method Methods 0.000 title description 2
- 239000000203 mixture Substances 0.000 claims abstract description 39
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims abstract description 29
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 27
- 238000000034 method Methods 0.000 claims abstract description 25
- 239000004094 surface-active agent Substances 0.000 claims abstract description 25
- 230000008569 process Effects 0.000 claims abstract description 19
- 238000007747 plating Methods 0.000 claims abstract description 18
- 230000007797 corrosion Effects 0.000 claims abstract description 15
- 238000005260 corrosion Methods 0.000 claims abstract description 15
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 14
- 239000003112 inhibitor Substances 0.000 claims abstract description 13
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 20
- 239000011259 mixed solution Substances 0.000 claims description 18
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 15
- -1 compound organic acid Chemical class 0.000 claims description 14
- 229910007161 Si(CH3)3 Inorganic materials 0.000 claims description 13
- OFOBLEOULBTSOW-UHFFFAOYSA-N Malonic acid Chemical compound OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 claims description 12
- KDYFGRWQOYBRFD-UHFFFAOYSA-N succinic acid Chemical compound OC(=O)CCC(O)=O KDYFGRWQOYBRFD-UHFFFAOYSA-N 0.000 claims description 11
- AEMRFAOFKBGASW-UHFFFAOYSA-N Glycolic acid Chemical compound OCC(O)=O AEMRFAOFKBGASW-UHFFFAOYSA-N 0.000 claims description 10
- 235000005985 organic acids Nutrition 0.000 claims description 9
- 235000006408 oxalic acid Nutrition 0.000 claims description 9
- LCTONWCANYUPML-UHFFFAOYSA-N Pyruvic acid Chemical compound CC(=O)C(O)=O LCTONWCANYUPML-UHFFFAOYSA-N 0.000 claims description 8
- 229920001223 polyethylene glycol Polymers 0.000 claims description 7
- BJEPYKJPYRNKOW-REOHCLBHSA-N (S)-malic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O BJEPYKJPYRNKOW-REOHCLBHSA-N 0.000 claims description 6
- BJEPYKJPYRNKOW-UHFFFAOYSA-N alpha-hydroxysuccinic acid Natural products OC(=O)C(O)CC(O)=O BJEPYKJPYRNKOW-UHFFFAOYSA-N 0.000 claims description 6
- 239000001630 malic acid Substances 0.000 claims description 6
- 235000011090 malic acid Nutrition 0.000 claims description 6
- 239000002202 Polyethylene glycol Substances 0.000 claims description 5
- YXIWHUQXZSMYRE-UHFFFAOYSA-N 1,3-benzothiazole-2-thiol Chemical compound C1=CC=C2SC(S)=NC2=C1 YXIWHUQXZSMYRE-UHFFFAOYSA-N 0.000 claims description 4
- QRUDEWIWKLJBPS-UHFFFAOYSA-N benzotriazole Chemical compound C1=CC=C2N[N][N]C2=C1 QRUDEWIWKLJBPS-UHFFFAOYSA-N 0.000 claims description 4
- 239000012964 benzotriazole Substances 0.000 claims description 4
- 229940107700 pyruvic acid Drugs 0.000 claims description 4
- 239000001384 succinic acid Substances 0.000 claims description 4
- CMGDVUCDZOBDNL-UHFFFAOYSA-N 4-methyl-2h-benzotriazole Chemical compound CC1=CC=CC2=NNN=C12 CMGDVUCDZOBDNL-UHFFFAOYSA-N 0.000 claims description 3
- FBPFZTCFMRRESA-FSIIMWSLSA-N D-Glucitol Natural products OC[C@H](O)[C@H](O)[C@@H](O)[C@H](O)CO FBPFZTCFMRRESA-FSIIMWSLSA-N 0.000 claims description 3
- KDYFGRWQOYBRFD-NUQCWPJISA-N butanedioic acid Chemical compound O[14C](=O)CC[14C](O)=O KDYFGRWQOYBRFD-NUQCWPJISA-N 0.000 claims description 3
- 239000000600 sorbitol Substances 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 3
- COGUOPIIFAMLES-UHFFFAOYSA-N 2-[(4-chlorophenyl)methyl]-1h-benzimidazole Chemical compound C1=CC(Cl)=CC=C1CC1=NC2=CC=CC=C2N1 COGUOPIIFAMLES-UHFFFAOYSA-N 0.000 claims description 2
- FBPFZTCFMRRESA-JGWLITMVSA-N D-glucitol Chemical compound OC[C@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-JGWLITMVSA-N 0.000 claims description 2
- 239000008367 deionised water Substances 0.000 claims description 2
- 229910021641 deionized water Inorganic materials 0.000 claims description 2
- 229940113115 polyethylene glycol 200 Drugs 0.000 claims description 2
- 229940068918 polyethylene glycol 400 Drugs 0.000 claims description 2
- 229940057847 polyethylene glycol 600 Drugs 0.000 claims description 2
- 239000002253 acid Substances 0.000 abstract description 13
- 239000002904 solvent Substances 0.000 abstract description 6
- 230000007613 environmental effect Effects 0.000 abstract description 5
- 230000006378 damage Effects 0.000 abstract description 4
- 239000000843 powder Substances 0.000 abstract description 3
- 150000007524 organic acids Chemical class 0.000 description 15
- 230000000052 comparative effect Effects 0.000 description 13
- SNGREZUHAYWORS-UHFFFAOYSA-N perfluorooctanoic acid Chemical compound OC(=O)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F SNGREZUHAYWORS-UHFFFAOYSA-N 0.000 description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- 229910052802 copper Inorganic materials 0.000 description 5
- 239000010949 copper Substances 0.000 description 5
- 238000003756 stirring Methods 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 238000003466 welding Methods 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- 239000005456 alcohol based solvent Substances 0.000 description 3
- NBVXSUQYWXRMNV-UHFFFAOYSA-N fluoromethane Chemical compound FC NBVXSUQYWXRMNV-UHFFFAOYSA-N 0.000 description 3
- 229910052736 halogen Inorganic materials 0.000 description 3
- 150000002367 halogens Chemical class 0.000 description 3
- 238000011056 performance test Methods 0.000 description 3
- 229910000679 solder Inorganic materials 0.000 description 3
- RSWGJHLUYNHPMX-UHFFFAOYSA-N Abietic-Saeure Natural products C12CCC(C(C)C)=CC2=CCC2C1(C)CCCC2(C)C(O)=O RSWGJHLUYNHPMX-UHFFFAOYSA-N 0.000 description 2
- FERIUCNNQQJTOY-UHFFFAOYSA-N Butyric acid Chemical compound CCCC(O)=O FERIUCNNQQJTOY-UHFFFAOYSA-N 0.000 description 2
- KHPCPRHQVVSZAH-HUOMCSJISA-N Rosin Natural products O(C/C=C/c1ccccc1)[C@H]1[C@H](O)[C@@H](O)[C@@H](O)[C@@H](CO)O1 KHPCPRHQVVSZAH-HUOMCSJISA-N 0.000 description 2
- 230000004913 activation Effects 0.000 description 2
- 239000013543 active substance Substances 0.000 description 2
- 230000032683 aging Effects 0.000 description 2
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 description 2
- 125000002917 halogen containing inorganic group Chemical group 0.000 description 2
- 230000036541 health Effects 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 2
- 239000002480 mineral oil Substances 0.000 description 2
- 235000010446 mineral oil Nutrition 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 230000001681 protective effect Effects 0.000 description 2
- YGSDEFSMJLZEOE-UHFFFAOYSA-N salicylic acid Chemical compound OC(=O)C1=CC=CC=C1O YGSDEFSMJLZEOE-UHFFFAOYSA-N 0.000 description 2
- KHPCPRHQVVSZAH-UHFFFAOYSA-N trans-cinnamyl beta-D-glucopyranoside Natural products OC1C(O)C(O)C(CO)OC1OCC=CC1=CC=CC=C1 KHPCPRHQVVSZAH-UHFFFAOYSA-N 0.000 description 2
- NQPDZGIKBAWPEJ-UHFFFAOYSA-N valeric acid Chemical compound CCCCC(O)=O NQPDZGIKBAWPEJ-UHFFFAOYSA-N 0.000 description 2
- RTBFRGCFXZNCOE-UHFFFAOYSA-N 1-methylsulfonylpiperidin-4-one Chemical compound CS(=O)(=O)N1CCC(=O)CC1 RTBFRGCFXZNCOE-UHFFFAOYSA-N 0.000 description 1
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 1
- 239000004925 Acrylic resin Substances 0.000 description 1
- 229920000178 Acrylic resin Polymers 0.000 description 1
- 239000005711 Benzoic acid Substances 0.000 description 1
- 235000011054 acetic acid Nutrition 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- JFCQEDHGNNZCLN-UHFFFAOYSA-N anhydrous glutaric acid Natural products OC(=O)CCCC(O)=O JFCQEDHGNNZCLN-UHFFFAOYSA-N 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 235000010233 benzoic acid Nutrition 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 235000015165 citric acid Nutrition 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 239000010408 film Substances 0.000 description 1
- 235000019253 formic acid Nutrition 0.000 description 1
- 230000006870 function Effects 0.000 description 1
- 231100000206 health hazard Toxicity 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000000543 intermediate Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- FJKROLUGYXJWQN-UHFFFAOYSA-N papa-hydroxy-benzoic acid Natural products OC(=O)C1=CC=C(O)C=C1 FJKROLUGYXJWQN-UHFFFAOYSA-N 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 235000019260 propionic acid Nutrition 0.000 description 1
- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 229960004889 salicylic acid Drugs 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 235000011044 succinic acid Nutrition 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 229940005605 valeric acid Drugs 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
Classifications
-
- 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
- B23K35/362—Selection of compositions of fluxes
-
- 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
- B23K35/3613—Polymers, e.g. resins
Landscapes
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Electric Connection Of Electric Components To Printed Circuits (AREA)
Abstract
The invention discloses an environment-friendly scaling powder composition, which comprises acid, a surfactant, a film forming agent and a corrosion inhibitor. The environment-friendly soldering flux composition provided by the invention can meet the process requirements of medium-high speed tin plating, especially copper wire tin plating, is uniform and quick in tin plating, free of pinholes, less in tin residue, stable in performance, and in addition, the environment-friendly soldering flux is green and safe, free of volatile solvents, low in corrosiveness and less in harm to human bodies, and completely meets the requirements of environmental regulations such as RHOS 2.0 and REACH.
Description
Technical Field
The invention belongs to the technical field of soldering flux, and particularly relates to environment-friendly soldering flux as well as a preparation method and application thereof.
Background
The tinned copper wire is a basic material in the electronic industry, and is mainly used for producing lead wires of electronic components such as piezoresistors, thermistors and the like and jumpers of circuit boards of the whole machine, the thickness of a tin layer, the adhesion force with a base material and the like have important influences on the performance (such as conductivity, corrosion resistance, oxidation resistance and the like) of the copper wire, the service life of the copper wire can have important influences on the performance of the tin layer of the tinned copper wire except for a tinning process, and the performance of a tinning soldering flux.
The hot tinning process needs to use soldering flux to improve the welding quality, and the soldering flux mainly reacts chemically and physically in the tinning process and plays a role in quick tinning within 1-2 seconds. The flux contains chemicals that must react with the metal oxide film and form compounds that dissolve in the flux, while preventing oxidation, reducing surface tension, improving the surface activation properties of the solder, and increasing the lubricity of the solder to the substrate surface.
With the continuous development of the electronic industry, the continuous updating of electronic products and the continuous upgrading of environmental protection regulations, the requirements of the market on soldering flux are increasing, and the development of the soldering flux is from the traditional rosin soldering flux to the synthetic soldering flux, the no-clean soldering flux, the water-soluble soldering flux and the like which appear in the 80 s, and then to the current lead-free halogen-free soldering flux and the like. All these types of soldering fluxes are based on alcohol solvents, and various auxiliary materials such as film forming agents, active agents, high-boiling point solvents, surfactants, corrosion inhibitors and the like are added to realize the applicability of the soldering fluxes to various processes. All of these types of fluxes have a commonality: alcohol solvents are taken as basic solvents or halogen-containing inorganic acids are taken as active agents, and the alcohol solvents mainly comprise ethanol, methanol, isopropanol or a mixture of the ethanol, the methanol and the isopropanol, and have the dangerous characteristics of low flash point, inflammability, explosiveness and the like; on the other hand, halogen-containing inorganic acid is easy to volatilize, and is easy to pollute water and soil, and health hazard is generated to human bodies.
The existing soldering flux applied to the field of tinned copper wires is mostly water-based halogen-containing soldering flux, but the existing soldering flux is high in damage to human bodies and environment due to halogen, and cannot meet the requirements of continuously-updated environmental regulations, such as RHOS 2.0, SONY 00259, HF, REACH and the like. In addition, a small amount of solvent or fluorocarbon surfactant (the raw material contains perfluorooctanoic acid (PFOA)) can be added into the emerging water-based halogen-free soldering flux, so that the increasingly-enhanced environment-friendly requirement cannot be met, and in the continuous copper wire tinning process, the water-based halogen-free soldering flux is easy to fry tin and cannot completely remove mineral oil attached on a copper wire, so that the tinning effect of the copper wire and the performance stability of a product can be influenced.
Disclosure of Invention
The invention provides a soldering flux composition, which comprises the following components in percentage by mass based on 100.0% of the total mass of the soldering flux composition: 2.0 to 10.0 percent of acid, 0.05 to 0.5 percent of surfactant, 1.0 to 10.0 percent of film forming agent and 0.05 to 0.5 percent of corrosion inhibitor.
According to an embodiment of the present invention, the flux composition comprises water. Illustratively, the balance of the flux composition, excluding the acid, surfactant, film former, corrosion inhibitor, is water.
According to an embodiment of the invention, the acid may be an organic acid, preferably a complex organic acid; the mass fraction of the acid in the composition may be 3.0-8.0%, for example 3.5%, 4%, 5%, 6%, 7%;
According to an embodiment of the present invention, the organic acid is selected from one, two, three or more of a monobasic acid or a dibasic acid. For example, at least one, e.g., two, three or more, of the organic acids is selected from formic acid, acetic acid, propionic acid, butyric acid, valeric acid, oxalic acid, malonic acid, succinic acid, glutaric acid, glycolic acid, citric acid, malic acid, pyruvic acid, benzoic acid, salicylic acid; preferably, the complex organic acid is selected from two, three or more of the above organic acids. Preferably, the combination of the compound organic acids may be oxalic acid and malic acid, succinic acid and glycolic acid, oxalic acid and succinic acid, oxalic acid, citric acid and malonic acid, glycolic acid, pyruvic acid and citric acid, malonic acid, succinic acid and malic acid;
According to embodiments of the present invention, the mass ratio between the organic acids in the complex organic acid may vary within a wide range. For example, when two organic acids are used in the compound organic acid, the mass ratio of the two organic acids is 1 (0.1-10), such as1 (0.2-6); when the compound organic acid is three organic acids, the mass ratio of the three organic acids is 1 (0.1-10), such as1 (0.2-6) (0.1-8), such as1 (1-4), and such as 1:2:4, 1:3:3, and 1:1:5.
According to the embodiment of the invention, the acid, particularly the compound organic acid, can be rapidly activated at high temperature and gradually decomposed or sublimated, so that the rapid tin-plating effect of the copper wire can be ensured, the residual amount of the compound organic acid in a tin bath can be reduced, and the waste of soldering flux is reduced; the tin plating method has the following two functions in the tin plating process: firstly, under the action of organic acid at high temperature, the surface oxide layer of the copper wire can be rapidly removed at the moment of contacting the copper wire, the surface of the copper wire is cleaned, a very thin protective film is formed, the copper wire is prevented from being oxidized again, and a pad is made for tin plating; secondly, by utilizing different activation temperatures and soldering assisting performances of the compound organic acid, the tin plating layer of the copper wire is ensured to have the characteristics of good brightness, plumpness, no pinholes and the like.
According to embodiments of the invention, the surfactant may also be present in the composition in an amount of 0.1-0.4%, for example 0.2%, 0.3%;
according to an embodiment of the present invention, the surfactant may be selected from fluorosilicone surfactants;
According to an embodiment of the present invention, the fluorosilicone surfactant has the formula (CH3)3SiO[SiO(CH3)2]p[CH3SiOC2H4CF3]q[CH3SiC3H6O(C2H4O)r(C3H6O)sHO]tSi(CH3)3, wherein p=1-5, q=3-8, r=2-6, s=6-15, t=2-5; for example, as (CH3)3SiO[SiO(CH3)2]2[CH3SiOC2H4CF3]5[CH3SiC3H6O(C2H4O)2(C3H6O)6HO]3Si(CH3)3、(CH3)3SiO[SiO(CH3)2]4[CH3SiOC2H4CF3]3[CH3SiC3H6O(C2H4O)6(C3H6O)6HO]2Si(CH3)3、(CH3)3SiO[SiO(CH3)2]2[CH3SiOC2H4CF3]7[CH3SiC3H6O(C2H4O)5(C3H6O)9HO]3Si(CH3)3、(CH3)3SiO[SiO(CH3)2]3[CH3SiOC2H4CF3]4[CH3SiC3H6O(C2H4O)6(C3H6O)7HO]5Si(CH3)3、(CH3)3SiO[SiO(CH3)2]5[CH3SiOC2H4CF3]3[CH3SiC3H6O(C2H4O)4(C3H6O)10HO]4Si(CH3)3;
According to an embodiment of the present invention, the fluorosilicone surfactant has a fluorocarbon chain hydrophobe and a carbosilicon chain hydrophobe.
According to an embodiment of the invention, the fluorosilicone surfactant is free of perfluorooctanoic acid (PFOA).
According to the embodiment of the invention, the fluorosilicone surfactant can reduce the surface tension of water to below 23 mN.m -1, does not contain perfluorooctanoic acid (PFOA), can effectively prevent tin explosion and enables tin liquid to be uniformly plated on copper wires;
According to the preferred embodiment of the invention, the surfactant can effectively reduce the surface tension of liquid, effectively clean mineral oil on copper wires, improve the thermal stability and chemical stability of the environment-friendly soldering flux, and improve the wettability of the environment-friendly soldering flux to solder. Preferably, the fluorosilicone surfactant has fluorocarbon and carbo-silicon chain hydrophobe, can improve wettability and permeability, can also show high surface activity at low concentration, and has good thermal stability.
According to embodiments of the invention, the film former may be present in the composition in a mass fraction of 2-8%, for example 3%, 3.5%, 4%, 5%, 6%, 7%;
according to an embodiment of the present invention, the film forming agent is selected from one of acrylic resin, modified rosin resin, polyethylene glycol and sorbitol; the polyethylene glycol is selected from polyethylene glycols with a number average molecular weight of 200-1000, for example, one selected from polyethylene glycol 200, polyethylene glycol 400 and polyethylene glycol 600;
According to the embodiment of the invention, the film forming agent is used for forming a very thin protective film on the copper wire after soldering, so that the copper wire is prevented from being oxidized again, and the tinning effect is deteriorated.
According to an embodiment of the invention, the corrosion inhibitor is selected from at least one of benzotriazole, methylbenzotriazole, 2-p-chlorobenzyl benzimidazole or mercaptobenzothiazole; preferably benzotriazole or methylbenzotriazole.
According to the embodiment of the invention, the corrosion inhibitor can reduce corrosion of the environment-friendly soldering flux to the copper wire in the tinning process, and ensure the service life of the copper wire and the stability of the process.
According to an embodiment of the invention, the water is preferably deionized water.
According to an embodiment of the present invention, the flux comprises the following components: the total mass of the composition is 100.0%, and the composition comprises 2.0-10.0% of compound organic acid, 0.05-0.5% of surfactant, 1.0-10.0% of film forming agent and 0.05-0.5% of corrosion inhibitor.
The invention also provides a preparation method of the soldering flux composition, which comprises the following steps: the flux composition is obtained by mixing a film forming agent, an acid (preferably a compound acid), a surfactant, a corrosion inhibitor and water.
According to embodiments of the present invention, the mixing may be carried out using a compounding process conventional in the art, such as stirring.
According to an embodiment of the present invention, the preparation method includes: sequentially adding the film forming agent, the acid, the surfactant and the corrosion inhibitor into water, and mixing to obtain the soldering flux composition.
According to an embodiment of the invention, the preparation method comprises the following steps:
(1) Mixing the film forming agent with water to obtain a first mixed solution;
(2) Mixing the acid with the first mixed solution to obtain a second mixed solution;
(3) Mixing the surfactant with the second mixed solution to obtain a third mixed solution;
(4) And mixing the corrosion inhibitor with the third mixed solution to obtain the soldering flux composition.
The invention also provides application of the soldering flux composition in a tinning process, preferably in a copper wire tinning process.
The invention also provides a tin plating method, which comprises the step of using the soldering flux composition in a tin plating process.
Advantageous effects
The soldering flux composition provided by the invention is environment-friendly, and the synergistic effect of the components ensures that the composition has the characteristics of quick tin application, no tin frying, no pinholes, less tin bath residues, good gloss and the like, and can ensure the continuous stability of a copper wire tinning process.
In addition, the soldering flux composition is green, safe and environment-friendly, does not contain PFOA intermediates, does not cause environmental pollution, has little harm to human health and little corrosiveness, and meets the requirements of environmental regulations such as RHOS 2.0, SONY 00259, HF, REACH and the like. The preparation method of the scaling powder composition has simple and easily controlled technological conditions, and the prepared environment-friendly scaling powder has stable performance and is suitable for large-scale industrial production.
The preparation method of the environment-friendly soldering flux provided by the invention has the advantages of simple process and strong operability, and can be widely applied to copper wire hot tinning processes.
Definition of terms
The numerical ranges recited in the specification and claims are equivalent to at least each specific integer number recited therein unless otherwise stated. For example, the numerical range "1-20" corresponds to the numerical range "1-10" in which each of the integer numbers 1,2, 3, 4, 5, 6,7, 8, 9, 10, and the numerical range "11-20" in which each of the integer numbers 11, 12, 13, 14, 15, 16, 17, 18, 19, 20 is recited. For example, p=1 to 5 is described herein, and p may be any number selected from 1,2, 3, 4, and 5. Furthermore, when a range of numerical values is defined as a "number" or can be a non-integer, it is understood that two endpoints of the range, each integer within the range, and each fraction within the range are recited. For example, a "number of 0 to 10" should be understood to describe not only each integer of 0, 1,2, 3, 4, 5, 6,7, 8, 9 and 10, but also at least the sum of each integer with 0.1, 0.2, 0.3, 0.4, 0.5, 0.6, 0.7, 0.8, 0.9, respectively.
It should be understood that "more" as described herein shall mean an integer greater than 3, such as greater than or equal to 4, such as 4, 5, 6, 7, 8, 9, or 10.
Detailed Description
The technical scheme of the invention will be further described in detail below with reference to specific embodiments. It is to be understood that the following examples are illustrative only and are not to be construed as limiting the scope of the invention. All techniques implemented based on the above description of the invention are intended to be included within the scope of the invention.
Unless otherwise indicated, the starting materials and reagents used in the following examples were either commercially available or may be prepared by known methods.
Example 1
The environment-friendly soldering flux comprises the following components in percentage by mass of 100.0 percent:
At room temperature, adding sorbitol into a stirring kettle, adding water and stirring uniformly to obtain a first mixed solution; adding oxalic acid and malic acid into the first mixed solution, and uniformly stirring to obtain a second mixed solution; (CH3)3SiO[SiO(CH3)2]2[CH3SiOC2H4CF3]5[CH3SiC3H6O(C2H4O)2(C3H6O)6HO]3Si(CH3)3 is added into the second mixed solution and stirred uniformly to obtain a third mixed solution; and adding the benzotriazole into the third mixed solution, and uniformly stirring to obtain the soldering flux composition.
Example 2
The environment-friendly soldering flux comprises the following components in percentage by mass of 100.0 percent:
The preparation method is described in example 1.
Example 3
The environment-friendly soldering flux comprises the following components in percentage by mass of 100.0 percent:
The preparation method is described in example 1.
Example 4
The environment-friendly soldering flux comprises the following components in percentage by mass of 100.0 percent:
The preparation method is described in example 1.
Example 5
The environment-friendly soldering flux comprises the following components in percentage by mass of 100.0 percent:
The preparation method is described in example 1.
Example 6
The environment-friendly soldering flux comprises the following components in percentage by mass of 100.0 percent:
The preparation method is described in example 1.
Example 7
The environment-friendly soldering flux comprises the following components in percentage by mass of 100.0 percent:
The preparation method is described in example 1.
Comparative example 1
The components are sequentially dissolved in water to obtain the soldering flux.
Comparative example 2
Comparative example 3
Comparative example 4
Performance test examples
In the performance tests of the samples of examples 1 to 7 and comparative examples 1 to 4, the relative wetting force, the aging test (baking at 190 ℃ C. For 4 hours, the tin layer does not fall off and does not change color), the solderability and the tin plating pinhole phenomenon test were respectively carried out by using copper wires with the diameter of 0.5mm as base materials, and the test standards are mainly referred to GB/T4909-2009 and GB/T4910-2009, and the test results are shown in Table 1.
Table 1 results of Performance test of examples 1-7 and comparative examples 1-4
As can be seen from table 1: in comparison with the comparative examples, the respective properties of the samples of examples 1 to 7 of the present invention, such as relative wettability, solderability, and pinhole phenomenon at high-speed tin plating, are superior to those of comparative examples 1 to 4. And, the pinhole phenomenon of comparative example 2 is superior to comparative example 1 in relative wettability, solderability and high speed tin plating, and it is proved that the welding performance of a single organic acid system is superior to that of the conventional halogen soldering flux, while the pinhole phenomenon of comparative examples 3 and 4 is superior to that of comparative example 2 in solderability and high speed tin plating, and it is proved that the welding performance of the compound organic acid solvent type soldering flux is superior to that of the single organic acid system. In addition, the welding effect of the compound organic acid water-based environment-friendly soldering flux provided by the invention is better than that of the compound organic acid solvent-based soldering flux in comparative examples 3 and 4. Therefore, the environment-friendly soldering flux provided by the embodiment of the invention has the characteristics of quick tin application, few pinholes, environmental protection, little harm to human health, little corrosiveness, capability of easily passing an aging test and the like, and meets the high-speed tin plating process requirement of 200m/min copper wires.
The embodiments of the present invention have been described above. However, the present invention is not limited to the above embodiments. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (11)
1. A flux composition comprising, based on 100.0% of the total mass of the flux composition, the following components: 0.1 to 0.4 percent of compound organic acid, 3.0 to 6.0 percent of surfactant, and 0.2 to 0.5 percent of film forming agent;
in the soldering flux composition, the balance of water is water except the combination of the compound organic acid, the surfactant, the film forming agent and the corrosion inhibitor;
The combination of the compound organic acid is selected from one of a combination of 3.0% oxalic acid and 1.5% malic acid, a combination of 1.0% succinic acid and 2.0% glycolic acid, a combination of 3.0% oxalic acid and 0.5% succinic acid, a combination of 2.0% oxalic acid, 1.0% citric acid and 0.5% malonic acid, a combination of 2.5% glycolic acid, 1.0% pyruvic acid and 0.5% citric acid, a combination of 1.5% oxalic acid, 1.5% pyruvic acid and 0.5% malonic acid, a combination of 2.5% malonic acid, 0.5% succinic acid and 0.5% malic acid;
The surfactant is a fluorosilicone surfactant, and the chemical formula is (CH3)3SiO[SiO(CH3)2]p[CH3SiOC2H4CF3]q[CH3SiC3H6O(C2H4O)r(C3H6O)sHO]tSi(CH3)3,, wherein p=1-5, q=3-8, r=2-6, s=6-15 and t=2-5;
The film forming agent is selected from one of polyethylene glycol and sorbitol;
the corrosion inhibitor is at least one selected from benzotriazole, methylbenzotriazole, 2-p-chlorobenzyl benzimidazole or mercaptobenzothiazole.
2. The flux composition of claim 1, wherein the fluorosilicone surfactant is selected from one of (CH3)3SiO[SiO(CH3)2]2[CH3SiOC2H4CF3]5[CH3SiC3H6O(C2H4O)2(C3H6O)6HO]3Si(CH3)3、(CH3)3SiO[SiO(CH3)2]4[CH3SiOC2H4CF3]3[CH3SiC3H6O(C2H4O)6(C3H6O)6HO]2Si(CH3)3、(CH3)3SiO[SiO(CH3)2]2[CH3SiOC2H4CF3]7[CH3SiC3H6O(C2H4O)5(C3H6O)9HO]3Si(CH3)3、(CH3)3SiO[SiO(CH3)2]3[CH3SiOC2H4CF3]4[CH3SiC3H6O(C2H4O)6(C3H6O)7HO]5Si(CH3)3、(CH3)3SiO[SiO(CH3)2]5[CH3SiOC2H4CF3]3[CH3SiC3H6O(C2H4O)4(C3H6O)10HO]4Si(CH3)3.
3. The soldering flux composition according to claim 1 or 2, wherein the surfactant is present in the composition in a mass fraction of 0.1-0.3%.
4. The soldering flux composition according to claim 1, wherein the film forming agent is present in the composition in a mass fraction of 3-4%.
5. The soldering flux composition according to claim 1, wherein the polyethylene glycol is selected from polyethylene glycols having a number average molecular weight of 200-1000.
6. The soldering flux composition according to claim 1, wherein the polyethylene glycol is selected from one of polyethylene glycol 200, polyethylene glycol 400 and polyethylene glycol 600.
7. The flux composition of claim 1, wherein the water is deionized water.
8. A method of preparing the flux composition of any one of claims 1-7, comprising the steps of:
(1) Mixing the film forming agent with water to obtain a first mixed solution;
(2) Mixing the combination of the compound organic acids with the first mixed solution to obtain a second mixed solution;
(3) Mixing the surfactant with the second mixed solution to obtain a third mixed solution;
(4) And mixing the corrosion inhibitor with the third mixed solution to obtain the soldering flux composition.
9. Use of the flux composition of any one of claims 1-7 in a tin plating process.
10. The use according to claim 9, wherein the flux composition is used in a copper wire tinning process.
11. A method of tin plating comprising tin plating using the flux composition of any one of claims 1-7.
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| CN101362264A (en) * | 2008-09-28 | 2009-02-11 | 厦门大学 | No-cleaning welding flux for environmental protection type lead-free solder and preparation method thereof |
| CN102357749A (en) * | 2011-10-18 | 2012-02-22 | 苏州之侨新材料科技有限公司 | Water-based halogen-free soldering flux used for lead-free soldering tin |
| CN102618362A (en) * | 2012-02-27 | 2012-08-01 | 深圳市优宝惠新材料科技有限公司 | Friction-reducing lubricating coating composition |
| CN109261069A (en) * | 2018-09-19 | 2019-01-25 | 九江学院 | A kind of quaternary fluorine silicon cationic surfactant and its synthetic method |
| CN109970781A (en) * | 2019-05-09 | 2019-07-05 | 九江学院 | A kind of synthetic method of fluorine silicon zwitterionic surfactant |
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| CN101362264A (en) * | 2008-09-28 | 2009-02-11 | 厦门大学 | No-cleaning welding flux for environmental protection type lead-free solder and preparation method thereof |
| CN102357749A (en) * | 2011-10-18 | 2012-02-22 | 苏州之侨新材料科技有限公司 | Water-based halogen-free soldering flux used for lead-free soldering tin |
| CN102618362A (en) * | 2012-02-27 | 2012-08-01 | 深圳市优宝惠新材料科技有限公司 | Friction-reducing lubricating coating composition |
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