CN115401364B - High-activity water-washing scaling powder and preparation process thereof - Google Patents
High-activity water-washing scaling powder and preparation process thereof Download PDFInfo
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- CN115401364B CN115401364B CN202111226367.1A CN202111226367A CN115401364B CN 115401364 B CN115401364 B CN 115401364B CN 202111226367 A CN202111226367 A CN 202111226367A CN 115401364 B CN115401364 B CN 115401364B
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- Prior art keywords
- acid
- flux
- water
- soldering flux
- activity water
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- 230000000694 effects Effects 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 238000005406 washing Methods 0.000 title claims abstract description 16
- 239000000843 powder Substances 0.000 title claims abstract description 14
- 230000004907 flux Effects 0.000 claims abstract description 48
- 238000005476 soldering Methods 0.000 claims abstract description 43
- 239000002562 thickening agent Substances 0.000 claims abstract description 36
- 239000002904 solvent Substances 0.000 claims abstract description 21
- 239000013543 active substance Substances 0.000 claims abstract description 20
- 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 18
- 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 18
- 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 18
- 239000002994 raw material Substances 0.000 claims abstract description 15
- -1 nitrogenous heterocyclic compound Chemical class 0.000 claims description 19
- 239000002253 acid Substances 0.000 claims description 15
- 238000001816 cooling Methods 0.000 claims description 13
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims description 12
- 238000002156 mixing Methods 0.000 claims description 12
- 238000006243 chemical reaction Methods 0.000 claims description 9
- 239000003921 oil Substances 0.000 claims description 8
- 150000007519 polyprotic acids Polymers 0.000 claims description 7
- 150000003505 terpenes Chemical class 0.000 claims description 6
- 235000007586 terpenes Nutrition 0.000 claims description 6
- 238000006386 neutralization reaction Methods 0.000 claims description 5
- 239000004094 surface-active agent Substances 0.000 claims description 4
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 3
- 125000005233 alkylalcohol group Chemical group 0.000 claims description 2
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 claims description 2
- 125000004185 ester group Chemical group 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 125000001424 substituent group Chemical group 0.000 claims description 2
- 150000001875 compounds Chemical class 0.000 claims 4
- RAXXELZNTBOGNW-UHFFFAOYSA-N imidazole Natural products C1=CNC=N1 RAXXELZNTBOGNW-UHFFFAOYSA-N 0.000 claims 3
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 claims 2
- SMWDFEZZVXVKRB-UHFFFAOYSA-N Quinoline Chemical compound N1=CC=CC2=CC=CC=C21 SMWDFEZZVXVKRB-UHFFFAOYSA-N 0.000 claims 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims 1
- WTKZEGDFNFYCGP-UHFFFAOYSA-N Pyrazole Chemical compound C=1C=NNC=1 WTKZEGDFNFYCGP-UHFFFAOYSA-N 0.000 claims 1
- 229910052799 carbon Inorganic materials 0.000 claims 1
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 claims 1
- 238000003466 welding Methods 0.000 abstract description 31
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 23
- 229910000679 solder Inorganic materials 0.000 abstract description 15
- 238000000034 method Methods 0.000 abstract description 11
- 230000008569 process Effects 0.000 abstract description 9
- 238000004140 cleaning Methods 0.000 abstract description 5
- 238000002844 melting Methods 0.000 abstract description 5
- 230000008018 melting Effects 0.000 abstract description 5
- 239000006185 dispersion Substances 0.000 abstract description 3
- 239000000463 material Substances 0.000 abstract description 3
- 230000009471 action Effects 0.000 abstract description 2
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 27
- OFOBLEOULBTSOW-UHFFFAOYSA-N Malonic acid Chemical compound OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 18
- 229940051841 polyoxyethylene ether Drugs 0.000 description 12
- 229920000056 polyoxyethylene ether Polymers 0.000 description 12
- BWDBEAQIHAEVLV-UHFFFAOYSA-N 6-methylheptan-1-ol Chemical compound CC(C)CCCCCO BWDBEAQIHAEVLV-UHFFFAOYSA-N 0.000 description 10
- 235000015165 citric acid Nutrition 0.000 description 9
- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid Chemical compound OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 description 8
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 description 7
- WUOACPNHFRMFPN-UHFFFAOYSA-N alpha-terpineol Chemical compound CC1=CCC(C(C)(C)O)CC1 WUOACPNHFRMFPN-UHFFFAOYSA-N 0.000 description 7
- 229910052802 copper Inorganic materials 0.000 description 7
- 239000010949 copper Substances 0.000 description 7
- 235000019198 oils Nutrition 0.000 description 7
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 description 6
- 239000002585 base Substances 0.000 description 6
- 239000000155 melt Substances 0.000 description 6
- UBQKCCHYAOITMY-UHFFFAOYSA-N pyridin-2-ol Chemical compound OC1=CC=CC=N1 UBQKCCHYAOITMY-UHFFFAOYSA-N 0.000 description 6
- RTBFRGCFXZNCOE-UHFFFAOYSA-N 1-methylsulfonylpiperidin-4-one Chemical compound CS(=O)(=O)N1CCC(=O)CC1 RTBFRGCFXZNCOE-UHFFFAOYSA-N 0.000 description 5
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 5
- KDYFGRWQOYBRFD-UHFFFAOYSA-N Succinic acid Natural products OC(=O)CCC(O)=O KDYFGRWQOYBRFD-UHFFFAOYSA-N 0.000 description 5
- 239000003513 alkali Substances 0.000 description 5
- JFCQEDHGNNZCLN-UHFFFAOYSA-N anhydrous glutaric acid Natural products OC(=O)CCCC(O)=O JFCQEDHGNNZCLN-UHFFFAOYSA-N 0.000 description 5
- SQIFACVGCPWBQZ-UHFFFAOYSA-N delta-terpineol Natural products CC(C)(O)C1CCC(=C)CC1 SQIFACVGCPWBQZ-UHFFFAOYSA-N 0.000 description 5
- 238000001035 drying Methods 0.000 description 5
- 230000003472 neutralizing effect Effects 0.000 description 5
- 229940116411 terpineol Drugs 0.000 description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- 239000001361 adipic acid Substances 0.000 description 4
- 235000011037 adipic acid Nutrition 0.000 description 4
- 150000003839 salts Chemical class 0.000 description 4
- 238000009736 wetting Methods 0.000 description 4
- CUVLMZNMSPJDON-UHFFFAOYSA-N 1-(1-butoxypropan-2-yloxy)propan-2-ol Chemical compound CCCCOCC(C)OCC(C)O CUVLMZNMSPJDON-UHFFFAOYSA-N 0.000 description 3
- SBASXUCJHJRPEV-UHFFFAOYSA-N 2-(2-methoxyethoxy)ethanol Chemical compound COCCOCCO SBASXUCJHJRPEV-UHFFFAOYSA-N 0.000 description 3
- GCNTZFIIOFTKIY-UHFFFAOYSA-N 4-hydroxypyridine Chemical compound OC1=CC=NC=C1 GCNTZFIIOFTKIY-UHFFFAOYSA-N 0.000 description 3
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 3
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 3
- 238000009835 boiling Methods 0.000 description 3
- 235000014113 dietary fatty acids Nutrition 0.000 description 3
- 229930195729 fatty acid Natural products 0.000 description 3
- 239000000194 fatty acid Substances 0.000 description 3
- PMDHIMMPXRSDML-UHFFFAOYSA-N 2-methylpyridine-4-carboxylic acid Natural products CC1=CC(C(O)=O)=CC=N1 PMDHIMMPXRSDML-UHFFFAOYSA-N 0.000 description 2
- KWYJDIUEHHCHCZ-UHFFFAOYSA-N 3-[2-[bis(2-carboxyethyl)amino]ethyl-(2-carboxyethyl)amino]propanoic acid Chemical compound OC(=O)CCN(CCC(O)=O)CCN(CCC(O)=O)CCC(O)=O KWYJDIUEHHCHCZ-UHFFFAOYSA-N 0.000 description 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- VZCYOOQTPOCHFL-OWOJBTEDSA-N Fumaric acid Chemical compound OC(=O)\C=C\C(O)=O VZCYOOQTPOCHFL-OWOJBTEDSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 2
- 229920001214 Polysorbate 60 Polymers 0.000 description 2
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 125000004432 carbon atom Chemical group C* 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 229940028356 diethylene glycol monobutyl ether Drugs 0.000 description 2
- JCGNDDUYTRNOFT-UHFFFAOYSA-N oxolane-2,4-dione Chemical compound O=C1COC(=O)C1 JCGNDDUYTRNOFT-UHFFFAOYSA-N 0.000 description 2
- SIOXPEMLGUPBBT-UHFFFAOYSA-N picolinic acid Chemical compound OC(=O)C1=CC=CC=N1 SIOXPEMLGUPBBT-UHFFFAOYSA-N 0.000 description 2
- WLJVNTCWHIRURA-UHFFFAOYSA-N pimelic acid Chemical compound OC(=O)CCCCCC(O)=O WLJVNTCWHIRURA-UHFFFAOYSA-N 0.000 description 2
- TYFQFVWCELRYAO-UHFFFAOYSA-N suberic acid Chemical compound OC(=O)CCCCCCC(O)=O TYFQFVWCELRYAO-UHFFFAOYSA-N 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 239000001384 succinic acid Substances 0.000 description 2
- KQTIIICEAUMSDG-UHFFFAOYSA-N tricarballylic acid Chemical compound OC(=O)CC(C(O)=O)CC(O)=O KQTIIICEAUMSDG-UHFFFAOYSA-N 0.000 description 2
- RPAJSBKBKSSMLJ-DFWYDOINSA-N (2s)-2-aminopentanedioic acid;hydrochloride Chemical class Cl.OC(=O)[C@@H](N)CCC(O)=O RPAJSBKBKSSMLJ-DFWYDOINSA-N 0.000 description 1
- BJEPYKJPYRNKOW-REOHCLBHSA-N (S)-malic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O BJEPYKJPYRNKOW-REOHCLBHSA-N 0.000 description 1
- QVCIPIYWPSPRFA-UHFFFAOYSA-N 1-hydroxypyrazole Chemical compound ON1C=CC=N1 QVCIPIYWPSPRFA-UHFFFAOYSA-N 0.000 description 1
- OKRROXQXGNEUSS-UHFFFAOYSA-N 1h-imidazol-1-ium-1-carboxylate Chemical compound OC(=O)N1C=CN=C1 OKRROXQXGNEUSS-UHFFFAOYSA-N 0.000 description 1
- KOPFEFZSAMLEHK-UHFFFAOYSA-N 1h-pyrazole-5-carboxylic acid Chemical compound OC(=O)C=1C=CNN=1 KOPFEFZSAMLEHK-UHFFFAOYSA-N 0.000 description 1
- HIXDQWDOVZUNNA-UHFFFAOYSA-N 2-(3,4-dimethoxyphenyl)-5-hydroxy-7-methoxychromen-4-one Chemical compound C=1C(OC)=CC(O)=C(C(C=2)=O)C=1OC=2C1=CC=C(OC)C(OC)=C1 HIXDQWDOVZUNNA-UHFFFAOYSA-N 0.000 description 1
- AMSDWLOANMAILF-UHFFFAOYSA-N 2-imidazol-1-ylethanol Chemical compound OCCN1C=CN=C1 AMSDWLOANMAILF-UHFFFAOYSA-N 0.000 description 1
- QCDWFXQBSFUVSP-UHFFFAOYSA-N 2-phenoxyethanol Chemical compound OCCOC1=CC=CC=C1 QCDWFXQBSFUVSP-UHFFFAOYSA-N 0.000 description 1
- GBISYXPXYCCKJU-UHFFFAOYSA-N C(C)(=O)O.C(C)(=O)O.C(C)(=O)O.OCCNCC Chemical compound C(C)(=O)O.C(C)(=O)O.C(C)(=O)O.OCCNCC GBISYXPXYCCKJU-UHFFFAOYSA-N 0.000 description 1
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 description 1
- 235000019501 Lemon oil Nutrition 0.000 description 1
- QPCDCPDFJACHGM-UHFFFAOYSA-N N,N-bis{2-[bis(carboxymethyl)amino]ethyl}glycine Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(=O)O)CCN(CC(O)=O)CC(O)=O QPCDCPDFJACHGM-UHFFFAOYSA-N 0.000 description 1
- 235000008331 Pinus X rigitaeda Nutrition 0.000 description 1
- 235000011613 Pinus brutia Nutrition 0.000 description 1
- 241000018646 Pinus brutia Species 0.000 description 1
- 241000779819 Syncarpia glomulifera Species 0.000 description 1
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 description 1
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 150000003973 alkyl amines Chemical class 0.000 description 1
- BJEPYKJPYRNKOW-UHFFFAOYSA-N alpha-hydroxysuccinic acid Natural products OC(=O)C(O)CC(O)=O BJEPYKJPYRNKOW-UHFFFAOYSA-N 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 229910052787 antimony Inorganic materials 0.000 description 1
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 description 1
- 229940111121 antirheumatic drug quinolines Drugs 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- KDYFGRWQOYBRFD-NUQCWPJISA-N butanedioic acid Chemical compound O[14C](=O)CC[14C](O)=O KDYFGRWQOYBRFD-NUQCWPJISA-N 0.000 description 1
- 150000001735 carboxylic acids Chemical class 0.000 description 1
- 239000012459 cleaning agent Substances 0.000 description 1
- 239000006184 cosolvent Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 239000010639 cypress oil Substances 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- YRIUSKIDOIARQF-UHFFFAOYSA-N dodecyl benzenesulfonate Chemical compound CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 YRIUSKIDOIARQF-UHFFFAOYSA-N 0.000 description 1
- 229940071161 dodecylbenzenesulfonate Drugs 0.000 description 1
- 125000006575 electron-withdrawing group Chemical group 0.000 description 1
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 1
- TUEYHEWXYWCDHA-UHFFFAOYSA-N ethyl 5-methylthiadiazole-4-carboxylate Chemical compound CCOC(=O)C=1N=NSC=1C TUEYHEWXYWCDHA-UHFFFAOYSA-N 0.000 description 1
- 239000010642 eucalyptus oil Substances 0.000 description 1
- 229940044949 eucalyptus oil Drugs 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 150000004665 fatty acids Chemical class 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 239000001530 fumaric acid Substances 0.000 description 1
- 235000011087 fumaric acid Nutrition 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 238000009499 grossing Methods 0.000 description 1
- 150000002460 imidazoles Chemical class 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 239000010501 lemon oil Substances 0.000 description 1
- 239000001630 malic acid Substances 0.000 description 1
- 235000011090 malic acid Nutrition 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 235000006408 oxalic acid Nutrition 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 229960003330 pentetic acid Drugs 0.000 description 1
- 229960005323 phenoxyethanol Drugs 0.000 description 1
- 239000001739 pinus spp. Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 150000003217 pyrazoles Chemical class 0.000 description 1
- 150000003222 pyridines Chemical class 0.000 description 1
- 150000003248 quinolines Chemical class 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 238000003892 spreading Methods 0.000 description 1
- 230000007480 spreading Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000011975 tartaric acid Substances 0.000 description 1
- 235000002906 tartaric acid Nutrition 0.000 description 1
- 239000013008 thixotropic agent Substances 0.000 description 1
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 description 1
- 229940036248 turpentine Drugs 0.000 description 1
- 238000004506 ultrasonic cleaning 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
Abstract
The invention relates to B23K, in particular to a high-activity water-washing scaling powder and a preparation process thereof. The soldering flux is prepared from the following raw materials in percentage by weight: 8-15 wt% of active agent, 7-12 wt% of thickener and the balance of solvent. The flux provided by the invention can promote the welding activity and improve the water washability by selecting the polycarboxylic active agent and adding the solvent containing the rosin derivative to adjust the viscosity and the dispersion compatibility during welding. By adding the thickener with both activity and washability, the activity in the low-temperature reflow process can be further improved, the cleaning of residual soldering flux with poor water solubility such as rosin derivatives and the like is promoted, and the residual soldering flux can be quickly and completely cleaned under the action of pure water. The soldering flux provided by the invention has high welding reliability, is environment-friendly, has no pollution, has high weldability to various base materials, avoids melting solder into balls, and has neat and bright welding spots and firm adhesion.
Description
Technical Field
The invention relates to B23K, in particular to a high-activity water-washing scaling powder and a preparation process thereof.
Background
The soldering flux is an auxiliary agent for removing metal oxide on the surface of a bonding pad in a welding process and promoting welding, and after the welding is finished, residual soldering flux such as water cleaning type soldering flux and the like needs to be removed through an oil-based or water-based cleaning agent, and the problems that the residual soldering flux is more after welding due to the fact that the water cleaning type soldering flux comprises resin with high content such as rosin and the like exist.
CN109676284a discloses a soldering paste and a method for manufacturing the same. The paste formulation comprises: 8-15% of rosin, a solvent, a thixotropic agent, organic acid, a surfactant and organic amine, and has the advantages of low reflux temperature, less flux paste residues, strong activity, low corrosion and capability of effectively improving the reliability of chip packaging.
The soldering paste has the advantages that the soldering paste adopts low rosin content, so that most of the soldering paste is volatilized in the reflow process, the amount of residues is reduced, the residues are difficult to clean rapidly by using water, and the current soldering paste is difficult to promote the formation of neat and smooth welding spots.
Disclosure of Invention
In order to solve the above problems, the first aspect of the present invention provides a high-activity water-washed flux, which is prepared from the following raw materials in percentage by weight: 8-15 wt% of active agent, 7-12 wt% of thickener and the balance of solvent.
In the welding process, the surface of a base material such as Cu, ni, au, pb is provided with an oxide layer to influence the formation and wetting of welding spots, so that an active agent is needed to remove the oxide layer to improve the welding activity, and the inventor finds that when a chain acid with a proper carboxyl number is added, the welding activity can be promoted, the wettability of a melt in the welding process can be promoted, but when the adhesive is used for low-temperature welding, the effect of the chain carboxylic acid is softer and the activity is poorer. In one embodiment, the active agent comprises a chain acid having a number of carboxyl groups ranging from 2 to 5. Preferably, the weight ratio of the chain acid having 2 to 3 carboxyl groups to the chain acid having 4 to 5 carboxyl groups is (2 to 6): 1. the chain acid has 10 or less carbon atoms. Examples of chain acids include, but are not limited to, oxalic acid, malonic acid, succinic acid, glutaric acid, adipic acid, suberic acid, pimelic acid, citric acid, tricarballylic acid, N-hydroxyethyl ethylamine triacetic acid, ethylenediamine tetraacetic acid, diethylenetriamine pentaacetic acid.
The inventor finds that when the thickening agent is obtained by adding acid with a certain carboxyl number and the nitrogenous heterocyclic compound through an acid-base neutralization mode, compared with the method of separately adding polybasic acid and the nitrogenous heterocyclic compound, the thickening agent can effectively promote the activity of low-temperature welding when the thickening agent acts with an active agent, reduce the melting and balling of a melt in the welding process, and promote the wetting of the melt on the surface of a substrate. The inventor discovers that the thickener provided by the invention can also promote the residual cosolvent in welding to be quickly cleaned by water, so that a clean, flat and smooth welding spot is obtained. In one embodiment, the thickener is prepared from a polyacid and a nitrogen-containing heterocyclic compound by acid-base neutralization.
The inventor finds that the thickening agent obtained by using polybasic acid with the carboxyl number of 2-4 contains redundant carboxylate radicals, so that the low-temperature welding activity of the active agent is further promoted, the compatibility with the active agent is also promoted, and the welding residues are promoted to be quickly cleaned by water. In one embodiment, the polyacid has a carboxyl number of 2 to 4 and the polyacid has 10 or less carbon atoms. Examples of the acid include malic acid, fumaric acid, adipic acid, tartaric acid, and citric acid.
In addition, the inventors have found that it is necessary to control the structure of the nitrogen-containing heterocyclic compound, particularly, to use a structure containing an electron withdrawing group such as a hydroxyl group, which promotes compatibility of a thickener with a relatively low water-soluble substance such as a rosin derivative or a terpene oil in a solvent, promotes water solubility and wetting uniformity, and that it is difficult to form a homogeneous phase with a flux to affect wetting effect even when an antimony-containing solder is used, if an alkylamine such as triethanolamine is used for the acid-base neutralization of the resulting thickener. In one embodiment, the nitrogen-containing heterocyclic compound is at least one selected from the group consisting of imidazoles, pyridines, pyrazoles, quinolines.
In one embodiment, the substituents of the nitrogen-containing heterocyclic compound include at least one of hydroxyl, carboxyl, carbonyl, and ester groups. Examples thereof include 4-hydroxypyridine, 2-carboxypyridine, 2-methyl-4-carboxypyridine, 3-carboxypyrazole, imidazole-1-carboxylic acid, 1- (2-hydroxyethyl) imidazole, and 1-hydroxypyrazole.
In one embodiment, the molar ratio of the fatty acid to the nitrogen-containing heterocyclic compound is (0.8 to 1.1): 1, there may be mentioned 0.8: 1. 0.82: 1. 0.85: 1. 0.88: 1. 0.9: 1. 0.95: 1. 0.99: 1.1:1. 1.05: 1. 1.1:1.
the salt obtained by neutralizing the acid and alkali with the main components of the thickener of the invention, which is mainly obtained by neutralizing the acid and alkali with the main components of carboxyl and amino, can be obtained by melting reaction without limitation or solution reaction in water which is well known in the art, wherein the reaction is reversible, the obtained salt can also obtain a small amount of acid and nitrogen-containing heterocycle in water, and the acid-base neutralization is carried out in inert gas atmosphere such as nitrogen, argon and the like. In one embodiment, the thickener is prepared by a melt reaction and/or a solution reaction.
In one embodiment, the melt reaction is a melt mixing of the polyacid and the nitrogen-containing heterocyclic compound at 200-220 ℃ and cooling.
In one embodiment, the solution reaction is obtained by adding polybasic acid and nitrogen-containing heterocyclic compound into water, reacting at 45-60 ℃ and drying. Wherein during the drying process, salt crystallization can be observed along with evaporation and cooling of water, and the salt is obtained by filtration.
In order to reduce the precipitation of the active agent in the welding process and promote the dissolution, the inventor adopts rosin derivatives, terpene oil and alcohol ether to jointly adjust the compatibility and dispersion of the soldering flux in the solder, reduce corrosion and promote the obtainment of a flat and smooth welding spot. In one embodiment, the solvent comprises one or more of rosin derivatives, terpene oils, alcohol ethers, alkyl alcohols. Preferably rosin derivatives, terpene oils, alcohol ethers, in a weight ratio of 1: (0.1-0.3): (0.3-0.5).
Examples of rosin derivatives include, but are not limited to, hydrogenated rosin, disproportionated rosin, hydrogenated rosin alcohol; examples of terpene oils include, but are not limited to, eucalyptus oil, pine needle oil, lemon oil, cypress oil, turpentine, terpineol; examples of alcohol ethers include, but are not limited to, ethylene glycol monophenyl ether, diethylene glycol methyl ether, diethylene glycol monobutyl ether, dipropylene glycol monobutyl ether, tetraethylene glycol monomethyl ether.
In one embodiment, the raw materials for preparing the soldering flux further comprise 1-4wt% of surfactant. The surfactant is not particularly limited in the present invention, and examples thereof include isooctanol polyoxyethylene ether, polyoxyethylene sorbitan fatty acid ester, dodecylbenzene sulfonate, and alkylphenol polyoxyethylene ether, preferably isooctanol polyoxyethylene ether, polyoxyethylene sorbitan fatty acid ester, and alkylphenol polyoxyethylene ether.
The second aspect of the invention provides a preparation process of the high-activity water-washing scaling powder, which comprises the following steps: and mixing the raw materials for preparing the soldering flux at 110-170 ℃ and cooling to obtain the soldering flux. The addition temperature of the feedstock of the present invention may be determined by the boiling point, e.g., a low boiling point feedstock such as propylene glycol may be added below the boiling point.
Compared with the prior art, the invention has the following beneficial effects:
(1) The flux provided by the invention can promote the welding activity and improve the water washability by selecting the polycarboxylic active agent and adding the solvent containing the rosin derivative to adjust the viscosity and the dispersion compatibility during welding.
(2) By adding the thickener with both activity and washability, the activity in the low-temperature reflow process can be further improved, the cleaning of residual soldering flux with poor water solubility such as rosin derivatives and the like is promoted, and the residual soldering flux can be quickly and completely cleaned under the action of pure water.
(3) The soldering flux provided by the invention has high welding reliability, is environment-friendly, has no pollution, has high weldability to various base materials such as Cu, ni, au, pb and the like, avoids the melting of solder into balls, and has neat and bright obtained welding spots and firm attachment.
Drawings
Fig. 1 is a photograph of the soldering flux provided in example 1 after low temperature soldering.
Fig. 2 is a photograph of the soldering flux provided in example 2 after low temperature soldering.
Fig. 3 is a photograph of the soldering flux provided in example 1 after soldering and cleaning.
Detailed Description
Examples
Example 1
The example provides a water-washing scaling powder, which comprises the following preparation raw materials in percentage by weight: 10wt% of an active agent, 9wt% of a thickening agent and the balance of a solvent, wherein the active agent comprises malonic acid, glutaric acid and ethylenediamine tetraacetic acid, and the weight ratio is 1:3:1, the thickener comprises the following components in a molar ratio of 0.99: the thickener is prepared by neutralizing citric acid and 2-hydroxypyridine with acid and alkali, wherein the preparation method of the thickener comprises the steps of adding the citric acid and the 2-hydroxypyridine into water, reacting at 50 ℃ and drying, and the solvent is hydrogenated terpineol, terpineol and diethylene glycol methyl ether, and the weight ratio is 1:0.2:0.36, the raw materials for preparing the soldering flux also comprise 3 weight percent of isooctyl alcohol polyoxyethylene ether.
The example also provides a preparation process of the water-washing scaling powder, which comprises the following steps: mixing glutaric acid, ethylenediamine tetraacetic acid, a thickening agent, a solvent and isooctyl alcohol polyoxyethylene ether at 160 ℃, cooling to 120 ℃, adding malonic acid, mixing, preserving heat for 5min, and cooling to obtain the soldering flux.
Example 2
The example provides a water-washing scaling powder, which comprises the following preparation raw materials in percentage by weight: 14wt% of an active agent, 11wt% of a thickening agent and the balance of a solvent, wherein the active agent comprises malonic acid, succinic acid and ethylenediamine tetrapropionic acid, and the weight ratio is 0.6:2.4:1, the thickener comprises the following components in a molar ratio of 0.8: the thickener is prepared by neutralizing citric acid and 4-hydroxypyridine with acid and alkali, wherein the preparation method of the thickener comprises the steps of melting and mixing the citric acid and the 4-hydroxypyridine at 210 ℃ and cooling, and the solvent is hydrogenated rosin alcohol, terpineol, diethylene glycol monobutyl ether and dipropylene glycol monobutyl ether, and the weight ratio is 1:0.13:0.34, the raw materials for preparing the soldering flux also comprise 4 weight percent of isooctyl alcohol polyoxyethylene ether.
The example also provides a preparation process of the water-washing scaling powder, which comprises the following steps: and (3) mixing succinic acid with ethylenediamine tetrapropionic acid, a thickening agent, a solvent and isooctyl alcohol polyoxyethylene ether at 160 ℃, cooling to 120 ℃, adding malonic acid, mixing, preserving heat for 5min, and cooling to obtain the soldering flux.
Example 3
The example provides a water-washing scaling powder, which comprises the following preparation raw materials in percentage by weight: 8wt% of an active agent, 7wt% of a thickening agent and the balance of a solvent, wherein the active agent comprises malonic acid, adipic acid and ethylenediamine tetraacetic acid, and the weight ratio is 1:2:1, the thickener comprises the following components in a molar ratio of 1.1: the preparation method of the thickener comprises the steps of adding citric acid and 2-hydroxypyridine into water, reacting at 45-60 ℃ and drying, wherein the solvent is hydrogenated terpineol and terpineol dipropylene glycol monobutyl ether, and the weight ratio is 1:0.2:0.3, the raw materials for preparing the soldering flux also comprise 2 weight percent of isooctyl alcohol polyoxyethylene ether.
The example also provides a preparation process of the water-washing scaling powder, which comprises the following steps: mixing adipic acid, ethylenediamine tetraacetic acid, a thickening agent, a solvent and isooctyl alcohol polyoxyethylene ether at 160 ℃, cooling to 120 ℃, adding malonic acid, mixing, preserving heat for 5min, and cooling to obtain the soldering flux.
Example 4
The example provides a water-washing scaling powder, which comprises the following preparation raw materials in percentage by weight: 10wt% of an active agent, 9wt% of a thickening agent and the balance of a solvent, wherein the active agent comprises malonic acid, glutaric acid and ethylenediamine tetraacetic acid, and the weight ratio is 1:3:1, the thickener comprises the following components in a molar ratio of 0.99: the thickener is prepared by neutralizing citric acid and triethylamine with acid and alkali, wherein the preparation method of the thickener comprises the steps of adding the citric acid and the triethylamine into water, reacting at 50 ℃ and drying, and the solvent is hydrogenated rosin alcohol, terpineol and diethylene glycol methyl ether, and the weight ratio is 1:0.2:0.36, the raw materials for preparing the soldering flux also comprise 3 weight percent of isooctyl alcohol polyoxyethylene ether.
The example also provides a preparation process of the water-washing scaling powder, which comprises the following steps: mixing glutaric acid, ethylenediamine tetraacetic acid, a thickening agent, a solvent and isooctyl alcohol polyoxyethylene ether at 160 ℃, cooling to 120 ℃, adding malonic acid, mixing, preserving heat for 5min, and cooling to obtain the soldering flux.
Evaluation of Performance
The soldering flux provided by the embodiment and Sn42Bi58 are prepared according to the weight ratio of 12:88 as solder paste, the following experiment was performed.
1. Activity: three solder pastes are printed on each copper sheet, after welding is carried out at 120 ℃ for 5 minutes and at 180 ℃ for 5 minutes, the spreading condition of the solder pastes and the leveling and smoothing condition of the obtained solder joints in the welding process are observed, wherein the solder pastes provided in the examples 1-3 are melted into a complete block and evenly spread on the copper sheet without shrinkage to form balls, the solder joints obtained in the examples 1-2 are leveled and smoothed and spread on the copper sheet without tin balls, the solder joints are similar to the examples 1 and 2, the solder joints are leveled and smoothed without tin balls, the solder joints provided in the examples 1-3 are evenly spread, and the solder joints provided in the example 4 are leveled.
2. Water washability: three solder pastes were printed on each copper sheet, and after soldering at 120 ℃ for 5 minutes and 180 ℃ for 5 minutes, ultrasonic cleaning was performed in pure water at 50 ℃ for 3 minutes, and flux residue was observed, wherein the results of example 1 are shown in fig. 3, and it was found that all flux residues were cleaned, and that examples 2, 3 were identical to example 1, and no flux residue was found.
The test result shows that the soldering flux provided by the invention has good low-temperature activity and rapid water washability, and the obtained welding spots are smooth and smooth, can be used for welding difficult-to-weld metal substrates such as nickel, gold, palladium and the like besides copper, and further shows that the soldering flux has high activity.
Claims (8)
1. The high-activity water-washing scaling powder is characterized by comprising the following raw materials in percentage by weight: 8-15 wt% of an active agent, 7-12 wt% of a thickening agent and the balance of a solvent;
the thickener is prepared from polybasic acid and nitrogenous heterocyclic compound through acid-base neutralization;
the carboxyl number of the polybasic acid is 2-4, and the carbon number of the polybasic acid is less than or equal to 10;
the molar ratio of the polybasic acid to the nitrogen-containing heterocyclic compound is (0.8-1.1): 1.
2. the high-activity water-washing flux according to claim 1, wherein the nitrogen-containing heterocyclic compound is at least one selected from the group consisting of imidazole-based compounds, pyridine-based compounds, pyrazole-based compounds, quinoline-based compounds.
3. The high activity water-washable flux of claim 1, wherein the substituents of the nitrogen-containing heterocyclic compound comprise at least one of hydroxyl, carboxyl, carbonyl, ester groups.
4. The high activity water-washable flux of claim 1, wherein the thickener is prepared by melt reaction and/or solution reaction.
5. The high activity water-washable flux of any of claims 1-4, wherein the active agent comprises a chain acid having a carboxyl number of 2-5.
6. The high activity water-washable flux of any one of claims 1-5, wherein the solvent comprises one or more of rosin derivatives, terpene oils, alcohol ethers, alkyl alcohols.
7. The high-activity water-washing soldering flux according to any one of claims 1 to 6, wherein the raw materials for preparing the soldering flux further comprise 1 to 4wt% of a surfactant.
8. A process for preparing the high-activity water-washed flux according to any one of claims 1 to 7, comprising: and mixing the preparation raw materials of the soldering flux at 110-170 ℃ and cooling to obtain the soldering flux.
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