CN114367761A - Halogen-free lead-free soldering paste with low residues after soldering and preparation method thereof - Google Patents
Halogen-free lead-free soldering paste with low residues after soldering and preparation method thereof Download PDFInfo
- Publication number
- CN114367761A CN114367761A CN202210158532.2A CN202210158532A CN114367761A CN 114367761 A CN114367761 A CN 114367761A CN 202210158532 A CN202210158532 A CN 202210158532A CN 114367761 A CN114367761 A CN 114367761A
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- Prior art keywords
- solder
- free
- soldering
- halogen
- rosin
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Links
- 238000005476 soldering Methods 0.000 title claims abstract description 84
- 238000002360 preparation method Methods 0.000 title abstract description 15
- 229910000679 solder Inorganic materials 0.000 claims abstract description 106
- 230000004907 flux Effects 0.000 claims abstract description 40
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 33
- 239000000956 alloy Substances 0.000 claims abstract description 33
- RSWGJHLUYNHPMX-UHFFFAOYSA-N Abietic-Saeure Natural products C12CCC(C(C)C)=CC2=CCC2C1(C)CCCC2(C)C(O)=O RSWGJHLUYNHPMX-UHFFFAOYSA-N 0.000 claims abstract description 28
- 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 claims abstract description 28
- 229920005989 resin Polymers 0.000 claims abstract description 28
- 239000011347 resin Substances 0.000 claims abstract description 28
- 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 claims abstract description 28
- 239000000843 powder Substances 0.000 claims abstract description 26
- 239000013008 thixotropic agent Substances 0.000 claims abstract description 23
- 229920001187 thermosetting polymer Polymers 0.000 claims abstract description 19
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910052718 tin Inorganic materials 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 9
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000004094 surface-active agent Substances 0.000 claims abstract description 8
- 229910052727 yttrium Inorganic materials 0.000 claims abstract description 7
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000012190 activator Substances 0.000 claims abstract description 6
- 239000010949 copper Substances 0.000 claims abstract description 6
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 5
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229910052802 copper Inorganic materials 0.000 claims abstract description 5
- 229910052703 rhodium Inorganic materials 0.000 claims abstract description 5
- 239000010948 rhodium Substances 0.000 claims abstract description 5
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229910052709 silver Inorganic materials 0.000 claims abstract description 5
- 239000004332 silver Substances 0.000 claims abstract description 5
- 229910052726 zirconium Inorganic materials 0.000 claims abstract description 5
- 229910052763 palladium Inorganic materials 0.000 claims abstract description 4
- 238000003756 stirring Methods 0.000 claims description 32
- XLJMAIOERFSOGZ-UHFFFAOYSA-M cyanate Chemical compound [O-]C#N XLJMAIOERFSOGZ-UHFFFAOYSA-M 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 10
- 229920000877 Melamine resin Polymers 0.000 claims description 9
- 239000004640 Melamine resin Substances 0.000 claims description 9
- 230000003213 activating effect Effects 0.000 claims description 9
- 239000003795 chemical substances by application Substances 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 9
- 238000000227 grinding Methods 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 8
- 238000005303 weighing Methods 0.000 claims description 8
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 6
- 239000003960 organic solvent Substances 0.000 claims description 6
- 229920000642 polymer Polymers 0.000 claims description 5
- QIGBRXMKCJKVMJ-UHFFFAOYSA-N Hydroquinone Chemical compound OC1=CC=C(O)C=C1 QIGBRXMKCJKVMJ-UHFFFAOYSA-N 0.000 claims description 4
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 claims description 4
- PXKLMJQFEQBVLD-UHFFFAOYSA-N bisphenol F Chemical compound C1=CC(O)=CC=C1CC1=CC=C(O)C=C1 PXKLMJQFEQBVLD-UHFFFAOYSA-N 0.000 claims description 4
- 239000004359 castor oil Substances 0.000 claims description 4
- 235000019438 castor oil Nutrition 0.000 claims description 4
- ZEMPKEQAKRGZGQ-XOQCFJPHSA-N glycerol triricinoleate Natural products CCCCCC[C@@H](O)CC=CCCCCCCCC(=O)OC[C@@H](COC(=O)CCCCCCCC=CC[C@@H](O)CCCCCC)OC(=O)CCCCCCCC=CC[C@H](O)CCCCCC ZEMPKEQAKRGZGQ-XOQCFJPHSA-N 0.000 claims description 4
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims description 4
- WLJVNTCWHIRURA-UHFFFAOYSA-N pimelic acid Chemical compound OC(=O)CCCCCC(O)=O WLJVNTCWHIRURA-UHFFFAOYSA-N 0.000 claims description 4
- BJEPYKJPYRNKOW-REOHCLBHSA-N (S)-malic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O BJEPYKJPYRNKOW-REOHCLBHSA-N 0.000 claims description 2
- RTBFRGCFXZNCOE-UHFFFAOYSA-N 1-methylsulfonylpiperidin-4-one Chemical compound CS(=O)(=O)N1CCC(=O)CC1 RTBFRGCFXZNCOE-UHFFFAOYSA-N 0.000 claims description 2
- PVFQHGDIOXNKIC-UHFFFAOYSA-N 4-[2-[3-[2-(4-hydroxyphenyl)propan-2-yl]phenyl]propan-2-yl]phenol Chemical compound C=1C=CC(C(C)(C)C=2C=CC(O)=CC=2)=CC=1C(C)(C)C1=CC=C(O)C=C1 PVFQHGDIOXNKIC-UHFFFAOYSA-N 0.000 claims description 2
- DKPFZGUDAPQIHT-UHFFFAOYSA-N Butyl acetate Natural products CCCCOC(C)=O DKPFZGUDAPQIHT-UHFFFAOYSA-N 0.000 claims description 2
- CNRKMCUYINLDNN-UHFFFAOYSA-N C1(=CC=CC=C1)C.C(C(C)C)C(=O)CC(C)C Chemical compound C1(=CC=CC=C1)C.C(C(C)C)C(=O)CC(C)C CNRKMCUYINLDNN-UHFFFAOYSA-N 0.000 claims description 2
- KDYFGRWQOYBRFD-UHFFFAOYSA-N Succinic acid Natural products OC(=O)CCC(O)=O KDYFGRWQOYBRFD-UHFFFAOYSA-N 0.000 claims description 2
- RNFAKTRFMQEEQE-UHFFFAOYSA-N Tripropylene glycol butyl ether Chemical compound CCCCOC(CC)OC(C)COC(O)CC RNFAKTRFMQEEQE-UHFFFAOYSA-N 0.000 claims description 2
- BJEPYKJPYRNKOW-UHFFFAOYSA-N alpha-hydroxysuccinic acid Natural products OC(=O)C(O)CC(O)=O BJEPYKJPYRNKOW-UHFFFAOYSA-N 0.000 claims description 2
- JFCQEDHGNNZCLN-UHFFFAOYSA-N anhydrous glutaric acid Natural products OC(=O)CCCC(O)=O JFCQEDHGNNZCLN-UHFFFAOYSA-N 0.000 claims description 2
- KDYFGRWQOYBRFD-NUQCWPJISA-N butanedioic acid Chemical compound O[14C](=O)CC[14C](O)=O KDYFGRWQOYBRFD-NUQCWPJISA-N 0.000 claims description 2
- 238000001816 cooling Methods 0.000 claims description 2
- 235000014113 dietary fatty acids Nutrition 0.000 claims description 2
- 239000000839 emulsion Substances 0.000 claims description 2
- 229930195729 fatty acid Natural products 0.000 claims description 2
- 239000000194 fatty acid Substances 0.000 claims description 2
- 150000004665 fatty acids Chemical class 0.000 claims description 2
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 claims description 2
- 239000001630 malic acid Substances 0.000 claims description 2
- 235000011090 malic acid Nutrition 0.000 claims description 2
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 claims description 2
- 229940068918 polyethylene glycol 400 Drugs 0.000 claims description 2
- 239000007787 solid Substances 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 2
- 235000021355 Stearic acid Nutrition 0.000 claims 1
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims 1
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims 1
- 239000008117 stearic acid Substances 0.000 claims 1
- 230000002829 reductive effect Effects 0.000 abstract description 14
- 239000011135 tin Substances 0.000 abstract description 14
- 238000002844 melting Methods 0.000 abstract description 11
- 230000008018 melting Effects 0.000 abstract description 11
- 229910001128 Sn alloy Inorganic materials 0.000 abstract description 10
- 230000008569 process Effects 0.000 abstract description 8
- 239000002904 solvent Substances 0.000 abstract description 8
- 230000000694 effects Effects 0.000 abstract description 6
- 229910052751 metal Inorganic materials 0.000 abstract description 6
- 239000002184 metal Substances 0.000 abstract description 6
- 239000000758 substrate Substances 0.000 abstract description 6
- 238000007711 solidification Methods 0.000 abstract description 5
- 230000008023 solidification Effects 0.000 abstract description 5
- 238000009736 wetting Methods 0.000 abstract description 5
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 abstract description 4
- 238000007334 copolymerization reaction Methods 0.000 abstract description 4
- 238000002425 crystallisation Methods 0.000 abstract description 4
- 230000008025 crystallization Effects 0.000 abstract description 4
- 229910052761 rare earth metal Inorganic materials 0.000 abstract description 4
- 230000003647 oxidation Effects 0.000 abstract description 3
- 238000007254 oxidation reaction Methods 0.000 abstract description 3
- 238000006243 chemical reaction Methods 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 238000003466 welding Methods 0.000 description 16
- 239000003963 antioxidant agent Substances 0.000 description 7
- 230000003078 antioxidant effect Effects 0.000 description 7
- 239000004643 cyanate ester Substances 0.000 description 7
- 239000000463 material Substances 0.000 description 6
- 239000002245 particle Substances 0.000 description 6
- 150000004820 halides Chemical class 0.000 description 4
- 230000004048 modification Effects 0.000 description 4
- 238000012986 modification Methods 0.000 description 4
- 239000013543 active substance Substances 0.000 description 3
- 230000007797 corrosion Effects 0.000 description 3
- 238000005260 corrosion Methods 0.000 description 3
- 238000009413 insulation Methods 0.000 description 3
- JYEUMXHLPRZUAT-UHFFFAOYSA-N 1,2,3-triazine Chemical compound C1=CN=NN=C1 JYEUMXHLPRZUAT-UHFFFAOYSA-N 0.000 description 2
- 229910052779 Neodymium Inorganic materials 0.000 description 2
- 229910052797 bismuth Inorganic materials 0.000 description 2
- JWVAUCBYEDDGAD-UHFFFAOYSA-N bismuth tin Chemical compound [Sn].[Bi] JWVAUCBYEDDGAD-UHFFFAOYSA-N 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 230000009477 glass transition Effects 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 229910052745 lead Inorganic materials 0.000 description 2
- 239000000696 magnetic material Substances 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 230000001681 protective effect Effects 0.000 description 2
- 230000002285 radioactive effect Effects 0.000 description 2
- MIMUSZHMZBJBPO-UHFFFAOYSA-N 6-methoxy-8-nitroquinoline Chemical compound N1=CC=CC2=CC(OC)=CC([N+]([O-])=O)=C21 MIMUSZHMZBJBPO-UHFFFAOYSA-N 0.000 description 1
- OFGKGZXVFIMMDC-UHFFFAOYSA-N F.OC(CC(O)(O)O)NCCN Chemical compound F.OC(CC(O)(O)O)NCCN OFGKGZXVFIMMDC-UHFFFAOYSA-N 0.000 description 1
- -1 Sn Ag Cu Inorganic materials 0.000 description 1
- 229910007637 SnAg Inorganic materials 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 239000003431 cross linking reagent Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 230000000670 limiting effect Effects 0.000 description 1
- MUJIDPITZJWBSW-UHFFFAOYSA-N palladium(2+) Chemical compound [Pd+2] MUJIDPITZJWBSW-UHFFFAOYSA-N 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 238000003892 spreading Methods 0.000 description 1
- 230000007480 spreading Effects 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 150000003746 yttrium Chemical class 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
- B23K35/24—Selection of soldering or welding materials proper
- B23K35/26—Selection of soldering or welding materials proper with the principal constituent melting at less than 400 degrees C
- B23K35/262—Sn as the principal constituent
-
- 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
- B23K35/02—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by mechanical features, e.g. shape
- B23K35/0222—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by mechanical features, e.g. shape for use in soldering, brazing
- B23K35/0244—Powders, particles or spheres; Preforms made therefrom
- B23K35/025—Pastes, creams, slurries
-
- 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
- B23K35/22—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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Landscapes
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Electric Connection Of Electric Components To Printed Circuits (AREA)
Abstract
The application provides a halogen-free lead-free solder paste with low residues after soldering, which comprises solder alloy powder and soldering flux, wherein the solder alloy powder comprises tin, silver, copper, zirconium, yttrium, rhodium and palladium, the strength, hardness and heat resistance of a tin alloy can be obviously improved by adding yttrium, the melting point of a solder wire is improved, the oxidation resistance and ductility of the tin alloy are enhanced, the solidification crystallization state of the solder can be improved by adding trace rare earth elements into the tin alloy, the melting point of the solder wire is increased, the tensile strength and toughness of the solder are improved, the soldering flux comprises rosin, thermosetting resin, thixotropic agent, activator, surfactant and solvent, the copolymerization of the rosin and the thermosetting resin is used as a main body, so that the tin wetting capacity of a metal surface can be improved, the extension toughness of the solder wire can be improved, the existence of residues after soldering can be effectively reduced, the substrate is prevented from being corroded, and the final effect of a product is influenced, the preparation method of the halogen-free lead-free soldering paste with low residues after soldering, provided by the invention, has the advantages that the soldering flux and the solder alloy powder are prepared in sequence, the process is simple and convenient, the reaction is mild, no harmful gas is generated in the process, and the preparation method is suitable for mass production.
Description
Technical Field
The invention belongs to the technical field of welding materials, and particularly relates to a low-residue halogen-free lead-free soldering paste after welding and a preparation method thereof.
Background
With the rapid development of the electronic industry, the demand of thermally sensitive low-temperature welding application fields such as intelligent hardware radiators, LED lighting component mounting, solar photovoltaic and the like is rapidly increased. Lead-free solder paste is widely used as a connecting material of electronic components and circuit boards. The reflow soldering temperature of the solder paste prepared by the lead-free alloy solders such as Sn Ag Cu, SnAg and the like used at present is generally over 230 ℃, and the solder paste can not meet the requirement of low-temperature soldering. Is not suitable for the welding process of the heat sensitive electronic element. Therefore, the tin-bismuth system lead-free tin paste with lower melting point becomes the preferred material in the field of low-temperature welding, but the prior tin-bismuth system lead-free tin paste has low activity, so that the surface oxide layer of the bonding pad cannot be removed, and the poor phenomena of insufficient soldering, tombstoning, tin ball, no wetting and the like are caused in the welding process. In order to solve the above problems, in the prior art, a halide (such as ammonium bifluoride, tetrahydroxypropyl ethylenediamine hydrofluoride, etc.) with strong corrosiveness is mainly used as an active agent to remove black oxide formed in the welding process, which not only corrodes the welding point and the substrate, reduces the surface insulation resistance and affects the electrical performance of the welding point, but also fails to solve the problem of storage stability of the solder paste.
Therefore, there is a need for a halogen-free lead-free solder paste with high surface insulation resistance, strong wettability, high spreading rate, and low residue after soldering.
Disclosure of Invention
The invention provides the halogen-free lead-free soldering paste with low residues after welding, aiming at solving the defects that in the prior art, halide with high corrosivity is used as an active agent, so that the halide corrodes a welding spot and a substrate and the surface insulation resistance is reduced;
the second purpose of the invention is to provide a preparation method of the halogen-free lead-free solder paste with low residue after soldering.
In order to achieve the first purpose, the invention adopts the technical scheme that:
a low-residue halogen-free lead-free solder paste after soldering comprises the following components: 93.1-96.1 wt% of solder alloy powder and 2.4-7.0 wt% of soldering flux;
the solder alloy powder comprises the following components: 1.7-3.1 wt% of silver, 2.1-3.6 wt% of copper, 6.5-8.7 wt% of zirconium, 4.1-5.7 wt% of yttrium, 0.11-0.25 wt% of rhodium, 0.09-0.19 wt% of palladium and the balance of tin, wherein the strength, hardness and heat resistance of the tin alloy can be obviously improved by adding yttrium, the melting point of the tin wire is improved, the oxidation resistance and ductility of the tin alloy are enhanced, the solidification crystallization state of the solder can be improved by adding trace rare earth elements into the tin alloy, the melting point of the tin wire is increased, the tensile strength and toughness of the solder are improved, signal interference caused by decay is reduced because no radioactive isotope elements such as Bi, Pb and Co are added, and signal interference caused by material nonlinearity is reduced because no magnetic materials such as Fe, Co, Ni, Nd and the like are added;
the soldering flux comprises the following components: 33-42.5 wt% of rosin, 8.5-11.6 wt% of activating agent, 2.7-4.1 wt% of thixotropic agent, 11.5-15.2 wt% of thermosetting resin, 1.2-3.2 wt% of surfactant and the balance of organic solvent; the thermosetting resin is prepared by compounding cyanate resin and melamine resin according to the weight ratio of 1-2:3-4, and copolymerization of rosin and the thermosetting resin is used as a main body, so that the tin wetting capacity of the metal surface can be improved, the extending toughness of a solder wire can be improved, the existence of residues after welding can be effectively reduced, and the final effect of a product is prevented from being influenced by corrosion of a substrate.
The cyanate ester resin is one or more of bisphenol A type cyanate ester, bisphenol F type cyanate ester, bisphenol M type cyanate ester and phenolic cyanate ester, and the triazine network formed after curing by using the cyanate ester has excellent mechanical property and high glass transition temperature (T)g260 ℃) is added into the soldering flux, the cyanate resin is copolymerized and modified by the melamine resin, and the melting point of the system is improved after modification, so that the residues after welding can be effectively reduced.
The melamine resin is a high molecular polymer of 1,3, 5-triazine-2, 4, 6-triamine and formaldehyde, the solid content of the high molecular polymer in the melamine resin emulsion is 30-70%, and the high molecular polymer is used as a cross-linking agent of cyanate ester resin under a slightly acidic condition, so that the fluidity and the stability of a solder paste system during construction can be effectively improved.
The activator is one or a combination of more of succinic acid, glutaric acid, pimelic acid and malic acid, and the activator without halide is used, so that the corrosivity of the soldering paste on a base material is reduced, the residues after soldering are reduced, the excessive corrosion caused after soldering is avoided, the use is influenced, and the cleaning cost is saved.
The thixotropic agent is two or more of hydroquinone, dodecahydroxystearic acid, hydrogenated castor oil, modified hydrogenated castor oil and fatty acid amide, the viscosity and the printing performance of the solder paste are adjusted by adding the thixotropic agent, the viscosity of the solder paste is increased under an unstressed state so as to keep the inherent shape, prevent the collapse of the solder paste and prevent the trailing, adhesion, collapse and the like in the printing process.
The rosin is any one of water white rosin, perhydrogenated rosin and disproportionated rosin, does not play a role of a protective film at normal temperature, but is activated at high temperature of reflow soldering, quickly removes an oxide film on the surfaces of solder and a parent metal in a short time, forms a protective film for preventing metal from reoxidizing on the surface of the solder, is favorable for inhibiting the generation of the oxide film on the surface of the solder during the heating period of the reflow soldering, and ensures that the solder paste can still keep good soldering activity under continuous high-temperature baking.
The surface active agent is a halogen-free active agent ST-200 and polyethylene glycol 400 which are compounded according to the weight ratio of 1: 1-3.
The organic solvent is one or a combination of more of tripropylene glycol butyl ether, toluene isobutyl ketone, ethyl acetate and butyl acetate.
In order to achieve the second object, the invention adopts the technical scheme that:
the preparation method of the post-soldering low-residue halogen-free lead-free solder paste comprises the following steps:
s1, weighing the components according to the weight percentage for later use;
s2, adding an organic solvent into a container, heating to 140 ℃ below zero, adding rosin, adding thermosetting resin after dissolving, and stirring until the thermosetting resin is completely dissolved;
s3, keeping the temperature at 140 ℃ and adding a thixotropic agent and stirring until the thixotropic agent is completely dissolved;
s4, cooling the temperature to 60-80 ℃, adding an antioxidant and an activator, and stirring for 40-60 min;
s5, grinding the mixture by a grinder at the rotating speed of 4000-;
and S6, adding the soldering flux and the solder alloy powder into the stirrer, and mixing and stirring for 40-60 minutes to obtain the solder.
Compared with the prior art, the invention has the following advantages:
1. the application provides a low-residue halogen-free lead-free soldering paste after soldering, which comprises 93.1-96.6 wt% of solder alloy powder and 2.4-7.6 wt% of soldering flux, wherein the solder alloy powder is prepared from tin, silver, copper, zirconium, yttrium, rhodium and palladium, the strength, hardness and heat resistance of a tin alloy can be obviously improved by adding yttrium, the melting point of a soldering wire is improved, the oxidation resistance and ductility of the tin alloy are enhanced, the solidification crystallization state of the solder can be improved by adding trace rare earth elements into the tin alloy, the melting point of the soldering wire is increased, the tensile strength and toughness of the solder are improved, signal interference caused by decay is reduced by not adding radioactive isotope elements such as Bi, Pb, Co and the like, and signal interference caused by nonlinearity of materials is reduced by not adding magnetic materials such as Fe, Co, Ni, Nd and the like Thixotropic agent, activator, surfactant, solvent, resin and thermosetting resinThe copolymerization of the resin is taken as a main body, so that the tin wetting capacity of the metal surface can be improved, the extending toughness of the solder wire can be improved, the existence of residues after welding can be effectively reduced, the substrate is prevented from being corroded, and the final effect of the product is influencedg260 ℃) is added into the soldering flux, the cyanate resin is copolymerized and modified by the melamine resin, and the melting point of the system is improved after modification, so that the residues after welding can be effectively reduced.
2. The preparation method of the halogen-free lead-free soldering paste with low residues after soldering, provided by the invention, has the advantages that the soldering flux and the solder alloy powder are prepared in sequence, the process is simple and convenient, the reaction is mild, no harmful gas is generated in the process, and the preparation method is suitable for mass production.
Detailed Description
The technical solution of the present invention will be described below with reference to examples 1 to 6.
Example 1
A low-residue halogen-free lead-free solder paste after soldering, which comprises 93.10 wt% of solder alloy powder and 6.90 wt% of soldering flux, wherein the component ratio of the solder alloy powder is shown in Table 2, the component ratio of the soldering flux is shown in Table 3, and the preparation method comprises the following steps:
weighing the components according to the weight percentages in the tables 2 and 3 for later use; firstly, adding a solvent into a container, heating to 120 ℃, adding rosin, stirring until the rosin is completely dissolved, adding thermosetting resin, keeping the temperature at 120 ℃, adding a thixotropic agent into the container, keeping the temperature and stirring until the thixotropic agent is completely dissolved;
reducing the temperature to 70 ℃, adding an antioxidant and an activating agent, keeping the temperature and stirring for 45 minutes; grinding the mixture by a grinder at the rotating speed of 4000r/min until the particle size is less than 20 microns to obtain the soldering flux; adding soldering flux and solder alloy components into a solder paste stirrer, mixing and stirring for 60 minutes, and refrigerating to obtain the low-residue halogen-free lead-free solder paste after soldering.
Example 2
A low-residue halogen-free lead-free solder paste after soldering, which comprises the following components by weight, 94.50 wt% of solder alloy powder and 5.50 wt% of soldering flux, wherein the component ratio of the solder alloy powder is shown in Table 2, the component ratio of the soldering flux is shown in Table 3, and the preparation method comprises the following steps:
weighing the components according to the weight percentages in the tables 2 and 3 for later use; firstly, adding a solvent into a container, heating to 120 ℃, adding rosin, stirring until the rosin is completely dissolved, adding thermosetting resin, keeping the temperature at 120 ℃, adding a thixotropic agent into the container, keeping the temperature and stirring until the thixotropic agent is completely dissolved;
reducing the temperature to 70 ℃, adding an antioxidant and an activating agent, keeping the temperature and stirring for 45 minutes; grinding the mixture by a grinder at the rotating speed of 4000r/min until the particle size is less than 20 microns to obtain the soldering flux; adding soldering flux and solder alloy components into a solder paste stirrer, mixing and stirring for 60 minutes, and refrigerating to obtain the low-residue halogen-free lead-free solder paste after soldering.
Example 3
A low-residue halogen-free lead-free solder paste after soldering, which comprises 95.90 wt% of solder alloy powder and 4.10 wt% of soldering flux, wherein the component ratio of the solder alloy powder is shown in Table 2, the component ratio of the soldering flux is shown in Table 3, and the preparation method comprises the following steps:
weighing the components according to the weight percentages in the tables 2 and 3 for later use; firstly, adding a solvent into a container, heating to 120 ℃, adding rosin, stirring until the rosin is completely dissolved, adding thermosetting resin, keeping the temperature at 120 ℃, adding a thixotropic agent into the container, keeping the temperature and stirring until the thixotropic agent is completely dissolved;
reducing the temperature to 70 ℃, adding an antioxidant and an activating agent, keeping the temperature and stirring for 45 minutes; grinding the mixture by a grinder at the rotating speed of 4000r/min until the particle size is less than 20 microns to obtain the soldering flux; adding soldering flux and solder alloy components into a solder paste stirrer, mixing and stirring for 60 minutes, and refrigerating to obtain the low-residue halogen-free lead-free solder paste after soldering.
Example 4
A low-residue halogen-free lead-free solder paste after soldering, which comprises 96.10 wt% of solder alloy powder and 3.90 wt% of soldering flux, wherein the component ratio of the solder alloy powder is shown in Table 2, the component ratio of the soldering flux is shown in Table 3, and the preparation method comprises the following steps:
weighing the components according to the weight percentages in the tables 2 and 3 for later use; firstly, adding a solvent into a container, heating to 120 ℃, adding rosin, stirring until the rosin is completely dissolved, adding thermosetting resin, keeping the temperature at 120 ℃, adding a thixotropic agent into the container, keeping the temperature and stirring until the thixotropic agent is completely dissolved;
reducing the temperature to 70 ℃, adding an antioxidant and an activating agent, keeping the temperature and stirring for 45 minutes; grinding the mixture by a grinder at the rotating speed of 4000r/min until the particle size is less than 20 microns to obtain the soldering flux; adding soldering flux and solder alloy components into a solder paste stirrer, mixing and stirring for 60 minutes, and refrigerating to obtain the low-residue halogen-free lead-free solder paste after soldering.
Example 5
A low-residue halogen-free lead-free solder paste after soldering, which comprises 94.80 wt% of solder alloy powder and 5.20 wt% of soldering flux, wherein the component ratio of the solder alloy powder is shown in Table 2, the component ratio of the soldering flux is shown in Table 3, and the preparation method comprises the following steps:
weighing the components according to the weight percentages in the tables 2 and 3 for later use; firstly, adding a solvent into a container, heating to 120 ℃, adding rosin, stirring until the rosin is completely dissolved, adding thermosetting resin, keeping the temperature at 120 ℃, adding a thixotropic agent into the container, keeping the temperature and stirring until the thixotropic agent is completely dissolved;
reducing the temperature to 70 ℃, adding an antioxidant and an activating agent, keeping the temperature and stirring for 45 minutes; grinding the mixture by a grinder at the rotating speed of 4000r/min until the particle size is less than 20 microns to obtain the soldering flux; adding soldering flux and solder alloy components into a solder paste stirrer, mixing and stirring for 60 minutes, and refrigerating to obtain the low-residue halogen-free lead-free solder paste after soldering.
Example 6
A low-residue halogen-free lead-free solder paste after soldering, which comprises 93.60 wt% of solder alloy powder and 6.40 wt% of soldering flux, wherein the component ratio of the solder alloy powder is shown in Table 2, the component ratio of the soldering flux is shown in Table 3, and the preparation method comprises the following steps:
weighing the components according to the weight percentages in the tables 2 and 3 for later use; firstly, adding a solvent into a container, heating to 120 ℃, adding rosin, stirring until the rosin is completely dissolved, adding thermosetting resin, keeping the temperature at 120 ℃, adding a thixotropic agent into the container, keeping the temperature and stirring until the thixotropic agent is completely dissolved;
reducing the temperature to 70 ℃, adding an antioxidant and an activating agent, keeping the temperature and stirring for 45 minutes; grinding the mixture by a grinder at the rotating speed of 4000r/min until the particle size is less than 20 microns to obtain the soldering flux; adding soldering flux and solder alloy components into a solder paste stirrer, mixing and stirring for 60 minutes, and refrigerating to obtain the low-residue halogen-free lead-free solder paste after soldering.
Table 1: weight ratios of the components of the solder pastes of examples 1 to 6
| Components | Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Example 6 |
| Solder alloy powder | 93.10％ | 94.50％ | 95.90％ | 96.10％ | 94.80％ | 93.60％ |
| Soldering flux | 6.90％ | 5.50％ | 4.10％ | 3.90％ | 5.20％ | 6.40％ |
Table 2: composition by weight proportions of solder alloy powders of examples 1 to 6
| Components | Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Example 6 |
| Tin (Sn) | 81.98％ | 82.63％ | 80.90％ | 83.44％ | 81.48％ | 82.49％ |
| Silver (Ag) | 3.10％ | 2.90％ | 2.50％ | 2.10％ | 1.90％ | 1.80％ |
| Copper (Cu) | 2.10％ | 2.30％ | 2.80％ | 2.50％ | 3.40％ | 3.20％ |
| Zirconium | 8.40％ | 6.80％ | 8.70％ | 7.20％ | 7.60％ | 6.50％ |
| Yttrium salt | 4.10％ | 5.10％ | 4.80％ | 4.50％ | 5.20％ | 5.70％ |
| Rhodium | 0.13％ | 0.15％ | 0.21％ | 0.11％ | 0.25％ | 0.18％ |
| Palladium (II) | 0.19％ | 0.12％ | 0.09％ | 0.15％ | 0.17％ | 0.13％ |
Table 3: the flux of examples 1-6 has the following composition by weight
The performance of the low-residue halogen-free lead-free solder paste prepared in examples 1-6 after soldering and the commercial lead-free solder paste of comparative example were tested, and the test results are shown in Table 4:
table 4: examples 1-6 and comparative examples test results
As can be seen from the table, the application provides a low-residue halogen-free lead-free solder paste after soldering, the solidification crystallization state of solder can be improved by adding trace rare earth elements into tin alloy, the melting point of a solder wire is increased, the tensile strength and toughness of the solder are improved, the copolymerization of rosin and thermosetting resin is adopted as a main body, the tin wetting capacity of the metal surface can be improved, the extending toughness of the solder wire can be improved, the existence of residues after soldering can be effectively reduced, the corrosion of a substrate is avoided, the final effect of a product is influenced, and a triazine network formed after the solidification of the cyanate has excellent mechanical property and high glass transition temperature (T & ltT & gt)g260 ℃) is added into the soldering flux, the cyanate resin is copolymerized and modified by the melamine resin, and the melting point of the system is improved after modification, so that the residues after welding can be effectively reduced.
The above description is only exemplary of the present application and should not be taken as limiting the present application, as any modification, equivalent replacement, or improvement made within the spirit and principle of the present application should be included in the protection scope of the present application.
Claims (9)
1. A low-residue halogen-free lead-free solder paste after soldering is characterized by comprising the following components: 93.1-96.1 wt% of solder alloy powder and 2.4-7.0 wt% of soldering flux;
the solder alloy powder comprises the following components: 1.7-3.1 wt% silver, 2.1-3.6 wt% copper, 6.5-8.7 wt% zirconium, 4.1-5.7 wt% yttrium, 0.11-0.25 wt% rhodium and 0.09-0.19 wt% palladium with the balance tin;
the soldering flux comprises the following components: 33-42.5 wt% of rosin, 8.5-11.6 wt% of activating agent, 2.7-4.1 wt% of thixotropic agent, 11.5-15.2 wt% of thermosetting resin, 1.2-3.2 wt% of surfactant and the balance of organic solvent; the thermosetting resin is compounded by cyanate resin and melamine resin according to the weight ratio of 1-2: 3-4.
2. The low residue post-solder halogen-free lead-free solder paste of claim 1, wherein: the cyanate resin is one or a combination of bisphenol A cyanate, bisphenol F cyanate and bisphenol M cyanate.
3. The low residue post-solder halogen-free lead-free solder paste of claim 1, wherein: the melamine resin is a high molecular polymer of 1,3, 5-triazine-2, 4, 6-triamine and formaldehyde, and the solid content of the high molecular polymer in the melamine resin emulsion is 30-70%.
4. The low residue post-solder halogen-free lead-free solder paste of claim 1, wherein: the activating agent is one or a combination of more of succinic acid, glutaric acid, pimelic acid and malic acid.
5. The low residue post-solder halogen-free lead-free solder paste of claim 1, wherein: the thixotropic agent is two or more of hydroquinone, dodecahydroxy stearic acid, hydrogenated castor oil, modified hydrogenated castor oil and fatty acid amide.
6. The low residue post-solder halogen-free lead-free solder paste of claim 1, wherein: the rosin is any one of water white rosin, perhydrogenated rosin and disproportionated rosin.
7. The low residue post-solder halogen-free lead-free solder paste of claim 1, wherein: the surfactant is a halogen-free surfactant ST-200 and polyethylene glycol 400 which are compounded according to the weight ratio of 1: 1-3.
8. The low residue post-solder halogen-free lead-free solder paste of claim 1, wherein: the organic solvent is one or a combination of more of tripropylene glycol butyl ether, toluene isobutyl ketone, ethyl acetate and butyl acetate.
9. The method for preparing the post-solder low residue halogen-free lead-free solder paste as claimed in any of claims 1-8, comprising the steps of:
s1, weighing the components according to the weight percentage for later use;
s2, adding an organic solvent into a container, heating to 140 ℃ below zero, adding rosin, adding thermosetting resin after dissolving, and stirring until the thermosetting resin is completely dissolved;
s3, keeping the temperature at 140 ℃ and adding a thixotropic agent and stirring until the thixotropic agent is completely dissolved;
s4, cooling the temperature to 60-80 ℃, adding a surfactant and an activator, and stirring for 40-60 min;
s5, grinding the mixture by a grinder at the rotating speed of 4000-;
and S6, adding the soldering flux and the solder alloy powder into the stirrer, and mixing and stirring for 40-60 minutes to obtain the solder.
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Denomination of invention: A halogen-free lead-free solder paste with low residue after welding and its preparation method Granted publication date: 20230818 Pledgee: Zhongshan Branch of Bank of Communications Co.,Ltd. Pledgor: ZHONGSHAN TIN-KING Co.,Ltd. Registration number: Y2024980026094 |