KR102623878B1 - Thixotropic agents and fluxes and solder pastes containing them - Google Patents
Thixotropic agents and fluxes and solder pastes containing them Download PDFInfo
- Publication number
- KR102623878B1 KR102623878B1 KR1020187009710A KR20187009710A KR102623878B1 KR 102623878 B1 KR102623878 B1 KR 102623878B1 KR 1020187009710 A KR1020187009710 A KR 1020187009710A KR 20187009710 A KR20187009710 A KR 20187009710A KR 102623878 B1 KR102623878 B1 KR 102623878B1
- Authority
- KR
- South Korea
- Prior art keywords
- flux
- resin
- thixotropic agent
- amide wax
- acid
- Prior art date
Links
- 239000013008 thixotropic agent Substances 0.000 title claims abstract description 96
- 229910000679 solder Inorganic materials 0.000 title claims abstract description 92
- 230000004907 flux Effects 0.000 title claims abstract description 82
- 150000001408 amides Chemical class 0.000 claims abstract description 98
- 239000011347 resin Substances 0.000 claims abstract description 83
- 229920005989 resin Polymers 0.000 claims abstract description 83
- -1 saturated aliphatic monocarboxylic acids Chemical class 0.000 claims abstract description 70
- 238000009835 boiling Methods 0.000 claims abstract description 56
- 239000002612 dispersion medium Substances 0.000 claims abstract description 32
- 239000002253 acid Substances 0.000 claims abstract description 22
- 150000004985 diamines Chemical class 0.000 claims abstract description 21
- 150000001412 amines Chemical class 0.000 claims abstract description 18
- 150000007519 polyprotic acids Polymers 0.000 claims abstract description 18
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims abstract description 16
- 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 description 31
- 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 description 31
- 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 description 31
- 239000000843 powder Substances 0.000 claims description 26
- 125000004432 carbon atom Chemical group C* 0.000 claims description 21
- 238000000034 method Methods 0.000 claims description 18
- 239000002904 solvent Substances 0.000 claims description 15
- 238000002156 mixing Methods 0.000 claims description 7
- 238000004519 manufacturing process Methods 0.000 claims description 6
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical group OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 claims description 4
- 230000002194 synthesizing effect Effects 0.000 claims description 4
- 239000011248 coating agent Substances 0.000 claims 1
- 238000000576 coating method Methods 0.000 claims 1
- 239000000463 material Substances 0.000 claims 1
- 238000010298 pulverizing process Methods 0.000 claims 1
- 238000007665 sagging Methods 0.000 abstract description 25
- 238000010438 heat treatment Methods 0.000 abstract description 23
- 239000000203 mixture Substances 0.000 abstract description 13
- 230000003685 thermal hair damage Effects 0.000 abstract description 3
- 239000001993 wax Substances 0.000 description 89
- 238000002360 preparation method Methods 0.000 description 55
- 230000000052 comparative effect Effects 0.000 description 30
- 238000005476 soldering Methods 0.000 description 19
- 239000003963 antioxidant agent Substances 0.000 description 18
- NAQMVNRVTILPCV-UHFFFAOYSA-N hexane-1,6-diamine Chemical compound NCCCCCCN NAQMVNRVTILPCV-UHFFFAOYSA-N 0.000 description 18
- 239000002245 particle Substances 0.000 description 13
- OFOBLEOULBTSOW-UHFFFAOYSA-N Malonic acid Chemical compound OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 12
- LYCAIKOWRPUZTN-UHFFFAOYSA-N ethylene glycol Natural products OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 11
- CXMXRPHRNRROMY-UHFFFAOYSA-N sebacic acid Chemical compound OC(=O)CCCCCCCCC(O)=O CXMXRPHRNRROMY-UHFFFAOYSA-N 0.000 description 11
- ULQISTXYYBZJSJ-UHFFFAOYSA-N 12-hydroxyoctadecanoic acid Chemical compound CCCCCCC(O)CCCCCCCCCCC(O)=O ULQISTXYYBZJSJ-UHFFFAOYSA-N 0.000 description 10
- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid Chemical compound OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 description 10
- 125000001931 aliphatic group Chemical group 0.000 description 10
- 239000002184 metal Substances 0.000 description 10
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- 239000012190 activator Substances 0.000 description 7
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- 150000002148 esters Chemical class 0.000 description 7
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- 150000001875 compounds Chemical class 0.000 description 6
- 238000011156 evaluation Methods 0.000 description 6
- OJMIONKXNSYLSR-UHFFFAOYSA-N phosphorous acid Chemical compound OP(O)O OJMIONKXNSYLSR-UHFFFAOYSA-N 0.000 description 6
- 229940114072 12-hydroxystearic acid Drugs 0.000 description 5
- 239000001361 adipic acid Substances 0.000 description 5
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- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 5
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- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
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- ZUOUZKKEUPVFJK-UHFFFAOYSA-N diphenyl Chemical compound C1=CC=CC=C1C1=CC=CC=C1 ZUOUZKKEUPVFJK-UHFFFAOYSA-N 0.000 description 4
- QQVIHTHCMHWDBS-UHFFFAOYSA-N isophthalic acid Chemical compound OC(=O)C1=CC=CC(C(O)=O)=C1 QQVIHTHCMHWDBS-UHFFFAOYSA-N 0.000 description 4
- 238000002844 melting Methods 0.000 description 4
- 230000008018 melting Effects 0.000 description 4
- 239000012299 nitrogen atmosphere Substances 0.000 description 4
- BDJRBEYXGGNYIS-UHFFFAOYSA-N nonanedioic acid Chemical compound OC(=O)CCCCCCCC(O)=O BDJRBEYXGGNYIS-UHFFFAOYSA-N 0.000 description 4
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 4
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- 239000004952 Polyamide Substances 0.000 description 3
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 3
- 239000007983 Tris buffer Substances 0.000 description 3
- 125000003118 aryl group Chemical group 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 238000004140 cleaning Methods 0.000 description 3
- 238000004040 coloring Methods 0.000 description 3
- 239000010949 copper Substances 0.000 description 3
- 150000001991 dicarboxylic acids Chemical class 0.000 description 3
- QFTYSVGGYOXFRQ-UHFFFAOYSA-N dodecane-1,12-diamine Chemical compound NCCCCCCCCCCCCN QFTYSVGGYOXFRQ-UHFFFAOYSA-N 0.000 description 3
- NFHFRUOZVGFOOS-UHFFFAOYSA-N palladium;triphenylphosphane Chemical compound [Pd].C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1 NFHFRUOZVGFOOS-UHFFFAOYSA-N 0.000 description 3
- WQEPLUUGTLDZJY-UHFFFAOYSA-N pentadecanoic acid Chemical compound CCCCCCCCCCCCCCC(O)=O WQEPLUUGTLDZJY-UHFFFAOYSA-N 0.000 description 3
- 229920002647 polyamide Polymers 0.000 description 3
- 229920000647 polyepoxide Polymers 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- PUPZLCDOIYMWBV-UHFFFAOYSA-N (+/-)-1,3-Butanediol Chemical compound CC(O)CCO PUPZLCDOIYMWBV-UHFFFAOYSA-N 0.000 description 2
- IANQTJSKSUMEQM-UHFFFAOYSA-N 1-benzofuran Chemical compound C1=CC=C2OC=CC2=C1 IANQTJSKSUMEQM-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 2
- IBLKWZIFZMJLFL-UHFFFAOYSA-N 1-phenoxypropan-2-ol Chemical compound CC(O)COC1=CC=CC=C1 IBLKWZIFZMJLFL-UHFFFAOYSA-N 0.000 description 2
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- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical class [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 description 2
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- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- LVHBHZANLOWSRM-UHFFFAOYSA-N methylenebutanedioic acid Natural products OC(=O)CC(=C)C(O)=O LVHBHZANLOWSRM-UHFFFAOYSA-N 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- IJDNQMDRQITEOD-UHFFFAOYSA-N n-butane Chemical compound CCCC IJDNQMDRQITEOD-UHFFFAOYSA-N 0.000 description 1
- OFBQJSOFQDEBGM-UHFFFAOYSA-N n-pentane Natural products CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 description 1
- RXOHFPCZGPKIRD-UHFFFAOYSA-N naphthalene-2,6-dicarboxylic acid Chemical compound C1=C(C(O)=O)C=CC2=CC(C(=O)O)=CC=C21 RXOHFPCZGPKIRD-UHFFFAOYSA-N 0.000 description 1
- SLCVBVWXLSEKPL-UHFFFAOYSA-N neopentyl glycol Chemical compound OCC(C)(C)CO SLCVBVWXLSEKPL-UHFFFAOYSA-N 0.000 description 1
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- SSDSCDGVMJFTEQ-UHFFFAOYSA-N octadecyl 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoate Chemical compound CCCCCCCCCCCCCCCCCCOC(=O)CCC1=CC(C(C)(C)C)=C(O)C(C(C)(C)C)=C1 SSDSCDGVMJFTEQ-UHFFFAOYSA-N 0.000 description 1
- CSWFWSPPZMEYAY-UHFFFAOYSA-N octadecyl dihydrogen phosphite Chemical compound CCCCCCCCCCCCCCCCCCOP(O)O CSWFWSPPZMEYAY-UHFFFAOYSA-N 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
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- AQSJGOWTSHOLKH-UHFFFAOYSA-N phosphite(3-) Chemical class [O-]P([O-])[O-] AQSJGOWTSHOLKH-UHFFFAOYSA-N 0.000 description 1
- FAIAAWCVCHQXDN-UHFFFAOYSA-N phosphorus trichloride Chemical compound ClP(Cl)Cl FAIAAWCVCHQXDN-UHFFFAOYSA-N 0.000 description 1
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- 229910052697 platinum Inorganic materials 0.000 description 1
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- PZRKPUQWIFJRKZ-UHFFFAOYSA-N pyrimidine-2,4,5,6-tetramine Chemical compound NC1=NC(N)=C(N)C(N)=N1 PZRKPUQWIFJRKZ-UHFFFAOYSA-N 0.000 description 1
- 238000010526 radical polymerization reaction Methods 0.000 description 1
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- 229910052709 silver Inorganic materials 0.000 description 1
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- 239000000126 substance Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000010557 suspension polymerization reaction Methods 0.000 description 1
- TUNFSRHWOTWDNC-HKGQFRNVSA-N tetradecanoic acid Chemical compound CCCCCCCCCCCCC[14C](O)=O TUNFSRHWOTWDNC-HKGQFRNVSA-N 0.000 description 1
- LVEOKSIILWWVEO-UHFFFAOYSA-N tetradecyl 3-(3-oxo-3-tetradecoxypropyl)sulfanylpropanoate Chemical compound CCCCCCCCCCCCCCOC(=O)CCSCCC(=O)OCCCCCCCCCCCCCC LVEOKSIILWWVEO-UHFFFAOYSA-N 0.000 description 1
- UWHCKJMYHZGTIT-UHFFFAOYSA-N tetraethylene glycol Chemical compound OCCOCCOCCOCCO UWHCKJMYHZGTIT-UHFFFAOYSA-N 0.000 description 1
- 235000010384 tocopherol Nutrition 0.000 description 1
- 229960001295 tocopherol Drugs 0.000 description 1
- 229930003799 tocopherol Natural products 0.000 description 1
- 239000011732 tocopherol Substances 0.000 description 1
- LDHQCZJRKDOVOX-UHFFFAOYSA-N trans-crotonic acid Natural products CC=CC(O)=O LDHQCZJRKDOVOX-UHFFFAOYSA-N 0.000 description 1
- HVLLSGMXQDNUAL-UHFFFAOYSA-N triphenyl phosphite Chemical compound C=1C=CC=CC=1OP(OC=1C=CC=CC=1)OC1=CC=CC=C1 HVLLSGMXQDNUAL-UHFFFAOYSA-N 0.000 description 1
- XUHUMYVYHLHMCD-UHFFFAOYSA-N tris(2-cyclohexylphenyl) phosphite Chemical compound C1CCCCC1C1=CC=CC=C1OP(OC=1C(=CC=CC=1)C1CCCCC1)OC1=CC=CC=C1C1CCCCC1 XUHUMYVYHLHMCD-UHFFFAOYSA-N 0.000 description 1
- UKKLUBWWAGMMAG-UHFFFAOYSA-N tris(2-hydroxyethyl)azanium;bromide Chemical compound Br.OCCN(CCO)CCO UKKLUBWWAGMMAG-UHFFFAOYSA-N 0.000 description 1
- WGKLOLBTFWFKOD-UHFFFAOYSA-N tris(2-nonylphenyl) phosphite Chemical compound CCCCCCCCCC1=CC=CC=C1OP(OC=1C(=CC=CC=1)CCCCCCCCC)OC1=CC=CC=C1CCCCCCCCC WGKLOLBTFWFKOD-UHFFFAOYSA-N 0.000 description 1
- GVJHHUAWPYXKBD-IEOSBIPESA-N α-tocopherol Chemical compound OC1=C(C)C(C)=C2O[C@@](CCC[C@H](C)CCC[C@H](C)CCCC(C)C)(C)CCC2=C1C GVJHHUAWPYXKBD-IEOSBIPESA-N 0.000 description 1
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L77/00—Compositions of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Compositions of derivatives of such polymers
- C08L77/06—Polyamides derived from polyamines and polycarboxylic acids
-
- 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
- B23K35/362—Selection of compositions of fluxes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/16—Nitrogen-containing compounds
- C08K5/20—Carboxylic acid amides
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L91/00—Compositions of oils, fats or waxes; Compositions of derivatives thereof
- C08L91/06—Waxes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L93/00—Compositions of natural resins; Compositions of derivatives thereof
- C08L93/04—Rosin
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Electric Connection Of Electric Components To Printed Circuits (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
가열 처짐성 억제 성분을, 균일하고도 신속하게 분산시킴으로써, 플럭스나 솔더 페이스트에 첨가했을 때 플럭스 수지나 가열 처짐성 억제 성분의 열 손상을 일으키지 않고, 또 플럭스나 솔더 페이스트의 열 처짐성을 야기하지 않는 요변성제, 및 이것을 포함하는 플럭스 및 솔더 페이스트를 제공한다. 본 발명의 요변성제는, 포화 지방족 모노카복실산류, 하이드록시기 함유 지방족 모노카복실산류 및 다염기산류 중 적어도 어느 1종의 산류와, 다이아민류 및 테트라아민류 중 적어도 어느 1종의 아민류의 축합물인 아마이드 왁스와, 분자량이 최대 10000인 수지와, 비점이 적어도 180℃인 분산매체가 혼합되어서 포함되어 있는 것이며, 본 발명의 플럭스 및 솔더 페이스트는, 이 요변성제를 포함하고 있다.By dispersing the heat sagging suppressing component evenly and quickly, it does not cause thermal damage to the flux resin or heating sagging suppressing component when added to flux or solder paste, and does not cause thermal sagging of the flux or solder paste. A thixotropic agent, and a flux and solder paste containing the same are provided. The thixotropic agent of the present invention is an amide wax that is a condensate of at least one acid selected from saturated aliphatic monocarboxylic acids, hydroxyl group-containing aliphatic monocarboxylic acids, and polybasic acids, and at least one type of amine selected from diamines and tetraamines. It contains a mixture of a resin with a molecular weight of up to 10000 and a dispersion medium with a boiling point of at least 180°C, and the flux and solder paste of the present invention contain this thixotropic agent.
Description
본 발명은, 전자부품의 납땜에 이용되는 플럭스(flux)나 솔더 페이스트(solder paste)에 혼합되어 이들의 열 처짐성(heat sagging)을 억제하는 요변성제, 및 이것을 함유하는 플럭스 및 솔더 페이스트에 관한 것이다.The present invention relates to a thixotropic agent that is mixed with flux or solder paste used for soldering electronic components to suppress heat sagging thereof, and to flux and solder paste containing the same. will be.
프린트 기판과 집적 회로, 저항, 및 컨덴서와 같은 전자부품의 납땜의 공업적 수법으로서, 플로우(flow) 방식과 리플로우(reflow) 방식이 알려져 있다. 플로우 방식은, 프린트 기판의 관통 구멍에, 전자부품의 리드 핀을 삽입하고, 프린트 기판의 하부면을 용융시킨 땜납에 침지시킴으로써 납땜하는 수법이다. 한편, 리플로우 방식은, 수지 성분, 용제 성분, 활성제, 요변성제 및 첨가제를 함유하는 플럭스와, 땜납 분말이 혼합된 솔더 페이스트를, 프린트 기판 상에 인쇄하고, 그 위에 전자부품을 탑재하고 나서, 열을 가해서 땜납을 용융시킴으로써 납땜하는 수법이다. 전자부품의 소형화·고밀도 실장화에 따라서, 리드 핀을 구비하지 않는 전자부품을 이용한 표면 실장 기술이 채용되게 되었기 때문에, 납땜에는 리플로우 방식이 주로 채용되고 있다.As industrial methods for soldering electronic components such as printed circuit boards, integrated circuits, resistors, and condensers, the flow method and the reflow method are known. The flow method is a method of soldering by inserting the lead pin of an electronic component into a through hole of a printed board and dipping the lower surface of the printed board into molten solder. On the other hand, in the reflow method, a solder paste mixed with a flux containing a resin component, a solvent component, an activator, a thixotropic agent, and an additive, and solder powder is printed on a printed circuit board, and electronic components are mounted thereon. This is a method of soldering by applying heat to melt the solder. With the miniaturization and high-density packaging of electronic components, surface mounting technology using electronic components without lead pins has been adopted, so the reflow method is mainly used for soldering.
리플로우 방식에 있어서, 솔더 페이스트를 프린트 기판에 인쇄한 후, 리플로우화로 내에서 프리히트(preheat)라고 불리는 예비가열이 행해진다. 이 프리히트는, 보통 150 내지 170℃에서 행해진다. 프리히트에 의해서, 용제 성분을 기화시키거나, 플럭스의 활성을 촉진시키거나 한다. 프리히트 후에, 메인 히트(main heat)라고 불리는 본 가열이 210 내지 260℃에서 행해진다. 프리히트에 의해서, 메인 히트에서 프린트 기판이나 전자부품에 가해지는 열충격이 완화된다.In the reflow method, after solder paste is printed on a printed board, preliminary heating called preheat is performed in a reflow furnace. This preheat is usually performed at 150 to 170°C. Preheating vaporizes solvent components or promotes flux activity. After preheat, main heating, called main heat, is carried out at 210 to 260°C. By preheating, the thermal shock applied to the printed circuit board or electronic components from the main heat is alleviated.
프리히트에 있어서는, 인쇄된 솔더 페이스트가 연화되어, 프린트 기판 상의 전자부품 아래나 그것의 주위로 흐르는 현상, 소위 열 처짐성을 일으키는 일이 있다. 열 처짐성은, 메인 히트에 있어서 땜납 볼(ball)이나 땜납 브리지(bridge)를 유발하므로, 납땜 불량의 원인이 되고 있다. 이 열 처짐성을 억제하기 위하여, 가열 처짐성 억제 성분인 왁스형태 생성물을, 요변성제로서 함유하고 있는 플럭스와, 땜납 분말을 혼화시킨 솔더 페이스트(크림 땜납)가 특허문헌 1에 기재되어 있다. 이 왁스형태 생성물은, 고급지방족 모노카복실산, 다염기산 및 다이아민을 탈수 반응시킴으로써 얻어진다.In preheating, the printed solder paste may soften and flow under or around electronic components on the printed board, causing so-called thermal sagging. Heat sagging causes solder balls and solder bridges in the main heat, which causes soldering defects. In order to suppress this heat sagging, a solder paste (cream solder) is described in Patent Document 1 in which a flux containing a wax-like product, which is a heat sagging suppressing component, as a thixotropic agent, and solder powder are mixed. This wax-like product is obtained by subjecting higher aliphatic monocarboxylic acids, polybasic acids, and diamines to a dehydration reaction.
납을 함유하는 땜납은, 인체에 유해하고 자연 환경을 오염시키므로, 납을 함유하지 않는 땜납을 포함하고 있는 무연 솔더 페이스트가, 많이 채용되고 있다. 특허문헌 2에, 가열 처짐성 억제 성분인 폴리아마이드를 함유하는 첨가제가 첨가된 플럭스를 이용해서 조제된 무연 솔더 페이스트가 개시되어 있다. 이 가열 처짐성 억제 성분은, 탄소수 14 이상의 다염기산과 다이아민의 축합반응에 의해서 얻어진 생성물이다. 또 플럭스의 용매로서 에틸렌 비스스테아릴아마이드를 이용하고 있다. 무연 솔더 페이스트의 프리히트는, 예를 들면 190℃라고 하는 고온조건에서 행해진다. 그 때문에 무연 솔더 페이스트는, 더한층 열 처짐성을 일으키기 쉽다.Since solder containing lead is harmful to the human body and pollutes the natural environment, lead-free solder paste containing solder that does not contain lead is widely used. Patent Document 2 discloses a lead-free solder paste prepared using a flux to which an additive containing polyamide, which is a heat sagging suppressing component, was added. This heating sagging suppressing component is a product obtained by a condensation reaction between a polybasic acid having 14 carbon atoms or more and diamine. Additionally, ethylene bisstearylamide is used as a flux solvent. Preheating of lead-free solder paste is performed under high temperature conditions, for example, 190°C. Therefore, lead-free solder paste is more prone to thermal sagging.
가열 처짐성 억제 성분은, 상온에서 분말 형태나 작은 덩어리 형태를 이루고 있기 때문에, 이것을 플럭스에 균일하게 분산시키기 위하여, 고온에서 장시간 가열 처리하고, 이것을 용융시키면서 혼합시킬 필요가 있다. 이 고온이면서도 장시간의 가열 처리 때문에, 가열 처짐성 억제 성분이 열화되거나, 플럭스에 함유되는 수지 성분이 분해·변질되고, 플럭스가 착색되거나 하는 열 손상을 일으킨다. 한편, 이 열 손상을 회피하기 위하여, 가열 처리 시간을 단축시키거나, 온도를 내리거나 하면, 가열 처짐성 억제 성분의 분산 불량을 일으켜 버린다.Since the heat sagging suppressing component is in the form of powder or small lumps at room temperature, in order to uniformly disperse it in the flux, it is necessary to heat it at a high temperature for a long time and mix it while melting it. Due to this high temperature and long-time heat treatment, the heat sagging suppressing component deteriorates, the resin component contained in the flux decomposes and deteriorates, and heat damage such as coloring of the flux occurs. On the other hand, in order to avoid this heat damage, if the heat treatment time is shortened or the temperature is lowered, poor dispersion of the heat sagging suppressing component will occur.
본 발명은 상기 과제를 해결하기 위하여 이루어진 것으로, 가열 처짐성 억제 성분을, 균일하고도 신속하게 분산시킴으로써, 플럭스나 솔더 페이스트에 첨가했을 때 플럭스 수지나 가열 처짐성 억제 성분의 열 손상을 일으키지 않고, 또 플럭스나 솔더 페이스트의 열 처짐성을 야기시키지 않는 요변성제, 및 이것을 함유하는 플럭스 및 솔더 페이스트를 제공하는 것을 목적으로 한다.The present invention was made to solve the above problems, by uniformly and quickly dispersing the heat sagging suppressing component, so that when added to flux or solder paste, thermal damage to the flux resin or heating sagging suppressing component is not caused, Another object is to provide a thixotropic agent that does not cause thermal sagging of flux or solder paste, and a flux and solder paste containing the same.
상기 목적을 달성하기 위하여 이루어진, 본 발명의 요변성제는, 포화 지방족 모노카복실산류, 하이드록시기 함유 지방족 모노카복실산류, 및 다염기산류 중 적어도 어느 1종의 산류와, 다이아민류 및 테트라아민류 중 적어도 어느 1종의 아민류의 축합물인 아마이드 왁스와, 분자량이 최대 10000인 수지와, 비점이 적어도 180℃인 분산매체가 혼합되어서 함유되어 있는 것이다.The thixotropic agent of the present invention, made to achieve the above object, comprises at least one acid selected from saturated aliphatic monocarboxylic acids, hydroxyl group-containing aliphatic monocarboxylic acids, and polybasic acids, and at least one selected from diamines and tetraamines. It contains a mixture of amide wax, which is a condensate of one type of amine, a resin with a molecular weight of up to 10,000, and a dispersion medium with a boiling point of at least 180°C.
요변성제는, 상기 아마이드 왁스가 탄소수 12 내지 22의 상기 포화 지방족 모노카복실산류 및/또는 탄소수 12 내지 22의 상기 하이드록시기 함유 지방족 모노카복실산류를 몰비로 합계 a몰(1≤a≤3)과, 탄소수 2 내지 12의 상기 다염기산류를 몰비로 b몰(0 <b≤5)과, 탄소수 2 내지 14의 상기 다이아민류 및/또는 탄소수 2 내지 14의 상기 테트라아민류를 몰비로 합계 c몰(1≤c≤6)로 하는 상기 축합물이며, 1 내지 40질량%의 상기 아마이드 왁스와, 20 내지 60질량%의 상기 수지와, 20 내지 60질량%의 상기 분산매체가 함유되어 있는 것이 바람직하다. 또한, 요변성제의 특성을 훼손시키지 않는 한, 요변성제는, 상기 아마이드 왁스에, 상기 다염기산류를 함유하지 않고 축합된 다른 아마이드 왁스(b=0)가 함유되어 있어도 된다.The thixotropic agent is a mixture of the amide wax and the saturated aliphatic monocarboxylic acids having 12 to 22 carbon atoms and/or the hydroxy group-containing aliphatic monocarboxylic acids having 12 to 22 carbon atoms in a molar ratio of a total of a mole (1≤a≤3). , a total of b moles (0 <b≤5) of the polybasic acids having 2 to 12 carbon atoms in a molar ratio and c moles of the diamines having 2 to 14 carbon atoms and/or the tetraamines having 2 to 14 carbon atoms in a molar ratio (1 ≤c≤6), and preferably contains 1 to 40% by mass of the amide wax, 20 to 60% by mass of the resin, and 20 to 60% by mass of the dispersion medium. Additionally, as long as the properties of the thixotropic agent are not impaired, the thixotropic agent may contain another amide wax (b=0) condensed with the amide wax without containing the polybasic acid.
요변성제는, 예를 들면, 상기 수지가 로진계 수지이며, 상기 분산매체가 글리콜 에터류인 것을 들 수 있다.As for the thixotropic agent, for example, the resin is a rosin-based resin and the dispersion medium is glycol ethers.
본 발명의 플럭스는, 상기 요변성제, 플럭스 수지 및 용제가 함유되어 있는 것이다.The flux of the present invention contains the above thixotropic agent, flux resin, and solvent.
본 발명의 솔더 페이스트는, 상기 플럭스 및 땜납이 함유되어 있는 것이다.The solder paste of the present invention contains the above flux and solder.
본 발명의 요변성제의 제조 방법은, 포화 지방족 모노카복실산류, 하이드록시기 함유 지방족 모노카복실산류 및 다염기산류 중 적어도 어느 1종의 산류와, 다이아민류 및 테트라아민류 중 적어도 어느 1종의 아민류를 축합시켜서 아마이드 왁스를 합성하는 공정과, 상기 아마이드 왁스, 분자량이 최대 10000인 수지 및 비점이 적어도 180℃인 분산매체를 혼합하는 공정을 포함한다.The method for producing a thixotropic agent of the present invention involves condensing at least one acid selected from saturated aliphatic monocarboxylic acids, hydroxyl group-containing aliphatic monocarboxylic acids, and polybasic acids, and at least one type of amine selected from diamines and tetraamines. It includes a process of synthesizing an amide wax, and a process of mixing the amide wax, a resin with a molecular weight of up to 10,000, and a dispersion medium with a boiling point of at least 180°C.
본 발명의 요변성제는, 가열 처짐성 억제 성분인 아마이드 왁스가, 수지와 분산매체에, 균일하게 분산되어 있는 것이므로, 플럭스나 솔더 페이스트에 이 요변성제를 첨가할 때의 가열 처리 시간을 단축시킬 수 있다. 또한, 가열 처리 시간의 단축에 의해서, 플럭스 수지 등의 열 손상을 억제시킬 수 있다.In the thixotropic agent of the present invention, amide wax, which is a heat sagging suppressing component, is uniformly dispersed in the resin and the dispersion medium, so the heat treatment time when adding this thixotropic agent to flux or solder paste can be shortened. there is. Additionally, by shortening the heat treatment time, heat damage to the flux resin and the like can be suppressed.
본 발명의 플럭스 및 솔더 페이스트는, 상기 요변성제를 함유하고 있으므로, 리플로우화로 내에서의 프리히트에 의해서 열 처짐성을 일으키지 않는다.Since the flux and solder paste of the present invention contain the above thixotropic agent, they do not cause heat sagging due to preheating in a reflow furnace.
본 발명의 요변성제의 제조 방법에 따르면, 적은 공정으로 신속하게 그리고 간편하게 아마이드 왁스를 요변성제에 분산시킬 수 있다.According to the method for producing a thixotropic agent of the present invention, amide wax can be quickly and easily dispersed in the thixotropic agent in a few steps.
이하, 본 발명을 실시하기 위한 형태를 상세히 설명하지만, 본 발명의 범위는 이들 형태로 한정되는 것은 아니다.Hereinafter, modes for carrying out the present invention will be described in detail, but the scope of the present invention is not limited to these modes.
본 발명의 요변성제는, 아마이드 왁스와, 수지와, 분산매체가 혼합되어서 함유되어 있는 것이다.The thixotropic agent of the present invention contains a mixture of amide wax, resin, and dispersion medium.
아마이드 왁스는, (a) 포화 지방족 모노카복실산류 및 하이드록시기 함유 지방족 모노카복실산류, 및 (b) 다염기산류 중 적어도 어느 1종의 산류와, (c) 다이아민류 및 테트라아민류 중 적어도 어느 1종의 아민류가, (a):(b):(c) = 1 내지 3:0 내지 5:1 내지 6의 몰비로, 탈수 축합된 축합물이다. 이 아마이드 왁스는 가열 처짐성 억제 성분이다.Amide wax is (a) at least one type of acid from saturated aliphatic monocarboxylic acids and hydroxy group-containing aliphatic monocarboxylic acids, (b) polybasic acids, and (c) at least one type from diamines and tetraamines. It is a condensate in which amines are dehydrated and condensed at a molar ratio of (a):(b):(c) = 1 to 3:0 to 5:1 to 6. This amide wax is an ingredient that inhibits heat sagging.
포화 지방족 모노카복실산류는, 탄소수 12 내지 22인 것이 바람직하다. 구체적으로, 라우르산, 미리스트산, 펜타데실산, 팔미트산, 마르가르산(margaric acid), 스테아르산, 노나데칸산, 아라키드산, 베헨산 등을 들 수 있다. 또 하이드록시기 함유 지방족 모노카복실산류는, 탄소수 12 내지 22인 것이 바람직하다. 구체적으로, 12-하이드록시스테아르산, 다이하이드록시스테아르산을 들 수 있다. 이들 포화 지방족 모노카복실산류 및 하이드록시기 함유 지방족 모노카복실산류는 단독으로 사용해도 되고, 복수를 사용해도 된다.Saturated aliphatic monocarboxylic acids preferably have 12 to 22 carbon atoms. Specifically, lauric acid, myristic acid, pentadecylic acid, palmitic acid, margaric acid, stearic acid, nonadecanoic acid, arachidic acid, behenic acid, etc. can be mentioned. Moreover, the hydroxy group-containing aliphatic monocarboxylic acids preferably have 12 to 22 carbon atoms. Specifically, 12-hydroxystearic acid and dihydroxystearic acid can be mentioned. These saturated aliphatic monocarboxylic acids and hydroxy group-containing aliphatic monocarboxylic acids may be used individually or in plural.
다염기산류는, 탄소수 2 내지 12의 이염기산 이상의 카복실산인 것이 바람직하고, 다이카복실산인 것이 보다 바람직하다. 이러한 다이카복실산으로서, 옥살산, 말론산, 숙신산, 글루타르산, 아디프산, 피멜산, 수베르산, 아젤라산, 세바스산, 1,10-데칸다이카복실산 및 1, 12-도데칸다이카복실산과 같은 지방족 다이카복실산; 프탈산, 아이소프탈산 및 테레프탈산과 같은 방향족 다이카복실산;1,2-사이클로헥산다이카복실산, 1,3-사이클로헥산다이카복실산, 1,4-사이클로헥산다이카복실산 및 사이클로헥실숙신산과 같은 지환식 다이카복실산을 들 수 있다. 이들 다염기산류는 단독으로 사용해도 되고, 복수를 사용해도 된다.Polybasic acids are preferably dibasic acids or higher carboxylic acids having 2 to 12 carbon atoms, and more preferably dicarboxylic acids. Such dicarboxylic acids include oxalic acid, malonic acid, succinic acid, glutaric acid, adipic acid, pimelic acid, suberic acid, azelaic acid, sebacic acid, 1,10-decanedicarboxylic acid, and 1,12-dodecanedicarboxylic acid. Aliphatic dicarboxylic acids; aromatic dicarboxylic acids such as phthalic acid, isophthalic acid and terephthalic acid; alicyclic dicarboxylic acids such as 1,2-cyclohexanedicarboxylic acid, 1,3-cyclohexanedicarboxylic acid, 1,4-cyclohexanedicarboxylic acid and cyclohexylsuccinic acid. You can. These polybasic acids may be used individually or in plural form.
다이아민류는, 탄소수 2 내지 14인 것이 바람직하다. 구체적으로, 에틸렌다이아민, 1,3-프로판다이아민, 1,4-부탄다이아민, 헥사메틸렌다이아민, 메타자일렌다이아민, 트라이렌다이아민, 파라자일렌다이아민, 페닐렌다이아민, 아이소포론다이아민, 1,10-데칸다이아민, 1,12-도데칸다이아민, 4,4-다이아미노다이사이클로헥실메탄, 4,4-다이아미노다이페닐메탄을 들 수 있다. 또 테트라아민류는, 탄소수 2 내지 14인 것이 바람직하다. 구체적으로, 부탄-1,1,4,4-테트라아민, 피리미딘-2,4,5,6-테트라아민을 들 수 있다. 이들 다이아민류 및 테트라아민류는 단독으로 사용해도 되고, 복수를 사용해도 된다.Diamines preferably have 2 to 14 carbon atoms. Specifically, ethylenediamine, 1,3-propanediamine, 1,4-butanediamine, hexamethylenediamine, metaxylenediamine, trylenediamine, para-xylenediamine, phenylenediamine, Examples include isophoronediamine, 1,10-decanediamine, 1,12-dodecanediamine, 4,4-diaminodicyclohexylmethane, and 4,4-diaminodiphenylmethane. Moreover, tetraamines preferably have 2 to 14 carbon atoms. Specifically, butane-1,1,4,4-tetraamine and pyrimidine-2,4,5,6-tetraamine can be mentioned. These diamines and tetraamines may be used individually or in plural.
다이아민류 및 테트라아민류의 양은, 포화 지방족 모노카복실산 또는 하이드록시기 함유 지방족 모노카복실산의 몰수와, 다염기산류의 몰수에 따라서, 카복시기의 총수와 아미노기의 총수가 당량이 되도록, 조정된다. 예를 들면, 지방족 모노카복실산 2몰에 대하여, 다염기산류인 지방족 다이카복실산 n몰(n=0 내지 5)일 경우, 다이아민류를 (n+1)몰로 하면, 산과 아민이 당량이 된다.The amounts of diamines and tetraamines are adjusted so that the total number of carboxyl groups and the total number of amino groups are equivalent, depending on the number of moles of saturated aliphatic monocarboxylic acid or hydroxy group-containing aliphatic monocarboxylic acid and the number of moles of polybasic acid. For example, in the case of n moles (n=0 to 5) of aliphatic dicarboxylic acids, which are polybasic acids, for 2 moles of aliphatic monocarboxylic acids, if the diamines are (n+1) moles, the acid and amine are equivalent.
이 아마이드 왁스는, 다른 분자량을 갖는 복수의 화합물의 혼합물로서 얻어진다. 아마이드 왁스는, 하기 화학식 (I)로 표시되는 것이 바람직하다:This amide wax is obtained as a mixture of a plurality of compounds having different molecular weights. The amide wax is preferably represented by the following formula (I):
A-C-(B-C)m-A ···（I)AC-(BC) m -A···(I)
(식 (Ｉ) 중, A는 포화 지방족 모노카복실산 및/또는 하이드록시기 함유 포화 지방족 모노카복실산의 탈수산기 잔기, B는 다염기산의 탈수산기 잔기, C는 다이아민 및/또는 테트라아민의 탈수소잔기, m은 0≤m≤5이다). 또한, 아마이드 왁스는, 단일 화합물이어도 되고, 혼합물이어도 된다.(In formula (I), A is the dehydroxyl group residue of a saturated aliphatic monocarboxylic acid and/or a hydroxy group-containing saturated aliphatic monocarboxylic acid, B is the dehydroxyl group residue of a polybasic acid, C is the dehydrogenation residue of diamine and/or tetraamine, m is 0≤m≤5). Additionally, the amide wax may be a single compound or a mixture.
요변성제에 함유되는 수지의 분자량은, 10000 이하인 것이 바람직하고, 5000 이하인 것이 보다 바람직하고, 3000 이하인 것이 더한층 바람직하다. 10000 이하의 분자량을 갖는 수지를 이용함으로서, 요변성제를 조제할 때의 가열 시에, 적당하게 연화되어서 분체 형태 또는 작은 덩어리 형태의 아마이드 왁스가 수지에 의해 균일하게 피복된다. 그것에 의해, 아마이드 왁스를 요변성제 중에 균일하게 분산시킬 수 있다. 한편, 수지의 분자량이 10000을 초과하면, 수지의 점도가 지나치게 높아져, 아마이드 왁스의 표면이 부분적으로밖에 수지로 피복되지 않으므로, 요변성제 중에 균일하게 분산되기 어려워진다. 또, 여기에서 말하는 분자량이란, 중량평균 분자량을 말한다. 이러한 분자량은, 겔 침투 크로마토그래피법에 의해 측정되어, 폴리스타이렌 환산으로 구해지는 것이다.The molecular weight of the resin contained in the thixotropic agent is preferably 10,000 or less, more preferably 5,000 or less, and even more preferably 3,000 or less. By using a resin having a molecular weight of 10,000 or less, when heated when preparing the thixotropic agent, it is appropriately softened and the amide wax in the form of powder or small lumps is uniformly coated with the resin. Thereby, the amide wax can be uniformly dispersed in the thixotropic agent. On the other hand, if the molecular weight of the resin exceeds 10000, the viscosity of the resin becomes too high and the surface of the amide wax is only partially covered with the resin, making it difficult to disperse uniformly in the thixotropic agent. In addition, the molecular weight referred to here refers to the weight average molecular weight. This molecular weight is measured by gel permeation chromatography and calculated in terms of polystyrene.
요변성제를 납땜에 이용하는 것의 관점에서, 이러한 수지로서 로진계 수지가 바람직하다. 로진계 수지는, 170 내지 174℃의 융점을 지니고 있으므로, 150 내지 190℃에서 행해지는 프리히트에서 활성화되어, 납땜해야 할 금속 표면의 산화막을 제거할 수 있다. 또 로진계 수지는 상온에서 불활성이므로, 납땜 후의 세정을 요하지 않는다. 로진계 수지로서, 구체적으로 검 로진, 톨 로진, 우드 로진, 및 이들의 유도체를 들 수 있다. 이들의 유도체로서는, 중합 로진, 아크릴화 로진, 수소첨가 로진, 불균화 로진, 폼일화 로진, 로진 에스터, 로진 변성 말레산 수지, 로진 변성 페놀 수지 및 로진 변성 알키드 수지 등을 들 수 있다.From the viewpoint of using a thixotropic agent in soldering, rosin-based resins are preferred as such resins. Since the rosin-based resin has a melting point of 170 to 174°C, it is activated in a preheat performed at 150 to 190°C and can remove the oxide film on the surface of the metal to be soldered. Additionally, since rosin-based resin is inert at room temperature, cleaning after soldering is not required. As the rosin-based resin, specific examples include gum rosin, tall rosin, wood rosin, and derivatives thereof. Examples of these derivatives include polymerized rosin, acrylated rosin, hydrogenated rosin, disproportionated rosin, formylated rosin, rosin ester, rosin-modified maleic acid resin, rosin-modified phenolic resin, and rosin-modified alkyd resin.
로진계 수지로서 구체적으로, 검 로진, 톨 로진, 우드 로진, 및 이들의 유도체를 들 수 있다. 이들의 유도체로서는, 중합 로진, 아크릴화 로진, 수소 첨가 로진, 불균화 로진, 폼일화 로진, 로진 에스터, 로진 변성 말레산 수지, 로진 변성 페놀 수지 및 로진 변성 알키드 수지 등을 들 수 있다.Specific examples of rosin-based resins include gum rosin, tall rosin, wood rosin, and derivatives thereof. Examples of these derivatives include polymerized rosin, acrylated rosin, hydrogenated rosin, disproportionated rosin, formylated rosin, rosin ester, rosin-modified maleic acid resin, rosin-modified phenolic resin, and rosin-modified alkyd resin.
분자량 10000 이하의 수지로서, 로진계 수지 외에, 터펜계 수지, 석유계 수지, 아크릴계 수지, 에폭시 수지 및 에스터계 수지를 들 수 있다. 이들 수지는, 혼합되어 있어도 된다.Resins with a molecular weight of 10000 or less include, in addition to rosin-based resins, terpene-based resins, petroleum-based resins, acrylic resins, epoxy resins, and ester-based resins. These resins may be mixed.
터펜 수지로서, 터펜 수지, 터펜페놀 수지, 변성 터펜 수지, 수첨 터펜 수지 및 수첨 터펜페놀 수지를 들 수 있다.Examples of the terpene resin include terpene resin, terpene phenol resin, modified terpene resin, hydrogenated terpene resin, and hydrogenated terpene phenol resin.
석유계 수지로서는, 지방족 또는 방향족 석유수지, 수첨 석유수지, 변성 석유수지, 지환식 석유수지 및 쿠마론·인덴석유수지를 들 수 있다.Examples of petroleum resins include aliphatic or aromatic petroleum resins, hydrogenated petroleum resins, modified petroleum resins, alicyclic petroleum resins, and coumarone/indene petroleum resins.
아크릴계 수지로서, 중합성 불포화기를 갖는 모노머, 예를 들면 (메타)아크릴산, 및 이의 에스터, 크로톤산, 이타콘산, (무수)말레산, 및 이의 에스터, 및 (메타)아크릴로나이트릴, (메타)아크릴 아마이드, 염화 비닐 및 아세트산 비닐을, 과산화물 등의 촉매의 존재 하, 괴상중합법, 액상중합법, 현탁 중합법 또는 유화 중합법으로 라디컬 중합에 의해 중합된 것을 들 수 있다.As the acrylic resin, monomers having a polymerizable unsaturated group, such as (meth)acrylic acid, and esters thereof, crotonic acid, itaconic acid, (maleic anhydride) maleic acid, and esters thereof, and (meth)acrylonitrile, (meth) ) Acrylamide, vinyl chloride, and vinyl acetate are polymerized by radical polymerization using bulk polymerization, liquid phase polymerization, suspension polymerization, or emulsion polymerization in the presence of a catalyst such as peroxide.
에폭시계 수지로서, 폴리에폭사이드, 방향족계 폴리에폭시 화합물, 다가 페놀의 글리시딜에터체, 다가 페놀의 글리시딜에스터체, 글리시딜 방향족 폴리아민, 지환식계 폴리에폭시 화합물, 지방족계 폴리에폭시 화합물 및 다가 지방산의 폴리글리시딜에스터체를 들 수 있다.As epoxy resins, polyepoxide, aromatic polyepoxy compound, glycidyl ether form of polyhydric phenol, glycidyl ester form of polyhydric phenol, glycidyl aromatic polyamine, alicyclic polyepoxy compound, aliphatic polyepoxy. Examples include compounds and polyglycidyl esters of polyvalent fatty acids.
에스터계 수지는, 다가 카복실산과 다가 알코올과의 축합반응에 의해 형성된 것이다. 다가 카복실산으로서, 테레프탈산, 아이소프탈산, 프탈산, 2,6-나프탈렌다이카복실산, 아디프산, 세바스산, 데칸다이카복실산, 아젤라산, 도데카다이카복실산, 사이클로헥산다이카복실산등을 들 수 있다. 또한, 다가 알코올로서, 에틸렌글리콜, 프로판다이올, 부탄다이올, 펜탄다이올, 헥산다이올, 네오펜틸글리콜, 1,4-사이클로헥산다이메탄올, 데칸다이올, 2-에틸-부틸-1-프로판다이올 및 비스페놀A를 들 수 있다.Ester resin is formed through a condensation reaction between polyhydric carboxylic acid and polyhydric alcohol. Examples of polyhydric carboxylic acids include terephthalic acid, isophthalic acid, phthalic acid, 2,6-naphthalenedicarboxylic acid, adipic acid, sebacic acid, decanedicarboxylic acid, azelaic acid, dodecadicarboxylic acid, and cyclohexanedicarboxylic acid. In addition, as polyhydric alcohols, ethylene glycol, propanediol, butanediol, pentanediol, hexanediol, neopentyl glycol, 1,4-cyclohexanedimethanol, decanediol, 2-ethyl-butyl-1- Propanediol and bisphenol A are included.
분산매체의 비점은, 180℃ 이상인 것이 바람직하고, 220℃ 이상인 것이 보다 바람직하며, 260℃ 이상인 것이 더한층 바람직하다. 분산매체의 비점이 180℃ 이상인 것에 의해, 요변성제를 조제할 때의 가열 온도에서 휘발되지 않으므로, 수지에 피복된 아마이드 왁스가 분산매체 중에 편재되는 일 없이 분산된다. 그 결과, 요변성제 중에 아마이드 왁스를 균일하게 분산시킬 수 있다. 게다가, 프린트 기판용의 솔더 페이스트에 포함되어 있는 공정 땜납의 융점(약 180℃) 이상의 비점을 지니고 있는 것에 의해, 납땜 시의 온도에서, 분산매체가 즉석에서 휘발되지 않고, 이 요변성제를 포함하는 솔더 페이스트 중에 아마이드 왁스를 균일하게 분산시킬 수 있다.The boiling point of the dispersion medium is preferably 180°C or higher, more preferably 220°C or higher, and even more preferably 260°C or higher. Since the boiling point of the dispersion medium is 180°C or higher, it does not volatilize at the heating temperature used when preparing the thixotropic agent, so the amide wax coated with the resin is dispersed without being unevenly distributed in the dispersion medium. As a result, the amide wax can be uniformly dispersed in the thixotropic agent. Furthermore, since it has a boiling point higher than the melting point (approximately 180°C) of the eutectic solder contained in the solder paste for printed circuit boards, the dispersion medium does not volatilize immediately at the temperature during soldering, and the dispersion medium containing this thixotropic agent does not volatilize immediately. Amide wax can be uniformly dispersed in solder paste.
한편 비점이 180℃ 미만이면, 프리히트나 납땜 시의 가열에 의해 분산매체가 용이하게 휘발되어 버려, 아마이드 왁스가 솔더 페이스트 중에 균일하게 분산되기 어려워져 버린다.On the other hand, if the boiling point is less than 180°C, the dispersion medium is easily volatilized by heating during preheating or soldering, making it difficult for the amide wax to be uniformly dispersed in the solder paste.
비점이 180℃ 이상인 분산매체로서, 모노올 및/또는 폴리올이 바람직하다. 구체적으로, 메틸다이글리콜(비점 194℃), 메틸트라이글리콜(비점 248℃), 메틸폴리글리콜(비점 295℃), 에틸렌글리콜(비점 197℃), 다이에틸렌글리콜(비점 244℃), 트라이에틸렌글리콜(비점 287℃), 프로필렌글리콜(비점 188℃), 다이프로필렌글리콜(비점 232℃), 아이소프로필다이글리콜(비점 207℃), 부틸다이글리콜(비점 255℃), 부틸트라이글리콜(비점 271℃), 아이소부틸다이글리콜(비점 220℃), 헥실글리콜(비점 208℃), 헥실다이글리콜(비점 260℃), 헥실렌글리콜(비점 197℃), 1,3-부탄다이올(비점 208℃), 1,5-펜탄다이올(비점 242℃), 1-페녹시-2-프로판올(비점 243℃), 2-에틸헥실글리콜(비점 229℃), 2-에틸헥실다이글리콜(비점 272℃), 페닐글리콜(비점 245℃), 페닐다이글리콜(비점 283℃), 벤질글리콜(비점 256℃), 벤질다이글리콜(비점 302℃), 메틸프로필렌다이글리콜(비점 187℃), 메틸프로필렌트라이글리콜(비점 242℃), 프로필프로필렌다이글리콜(비점 212℃), 부틸프로필렌다이글리콜(비점 212℃), 부틸프로필렌트라이글리콜(비점 274℃), 페닐프로필렌글리콜(비점 243℃), 다이메틸트라이글리콜(비점 216℃), 다이에틸다이글리콜(비점 189℃), 다이부틸다이글리콜(비점 255℃), 다이에틸렌글리콜모노메틸에터(비점 194℃), 트라이에틸렌글리콜모노메틸에터(비점 248℃), 프로필렌글리콜페닐에터(비점 243℃), 다이에틸렌글리콜모노부틸에터아세테이트(비점 247℃), 테트라에틸렌글리콜(비점 328℃), 2-에틸-1,3-헥산다이올(비점 244℃), α-터피네올(비점 217℃)을 들 수 있다.As a dispersion medium with a boiling point of 180°C or higher, monool and/or polyol are preferred. Specifically, methyl diglycol (boiling point 194°C), methyl triglycol (boiling point 248°C), methyl polyglycol (boiling point 295°C), ethylene glycol (boiling point 197°C), diethylene glycol (boiling point 244°C), triethylene glycol. (boiling point 287°C), propylene glycol (boiling point 188°C), dipropylene glycol (boiling point 232°C), isopropyl diglycol (boiling point 207°C), butyl diglycol (boiling point 255°C), butyl triglycol (boiling point 271°C) , Isobutyl diglycol (boiling point 220°C), hexyl glycol (boiling point 208°C), hexyl diglycol (boiling point 260°C), hexylene glycol (boiling point 197°C), 1,3-butanediol (boiling point 208°C), 1,5-pentanediol (boiling point 242°C), 1-phenoxy-2-propanol (boiling point 243°C), 2-ethylhexyl glycol (boiling point 229°C), 2-ethylhexyldiglycol (boiling point 272°C), Phenyl glycol (boiling point 245°C), phenyl diglycol (boiling point 283°C), benzyl glycol (boiling point 256°C), benzyl diglycol (boiling point 302°C), methylpropylene diglycol (boiling point 187°C), methylpropylene triglycol (boiling point 242°C), propylpropylene diglycol (boiling point 212°C), butylpropylene diglycol (boiling point 212°C), butylpropylene triglycol (boiling point 274°C), phenylpropylene glycol (boiling point 243°C), dimethyl triglycol (boiling point 216) ℃), diethyldiglycol (boiling point 189℃), dibutyldiglycol (boiling point 255℃), diethylene glycol monomethyl ether (boiling point 194℃), triethylene glycol monomethyl ether (boiling point 248℃), propylene Glycol phenyl ether (boiling point 243°C), diethylene glycol monobutyl ether acetate (boiling point 247°C), tetraethylene glycol (boiling point 328°C), 2-ethyl-1,3-hexanediol (boiling point 244°C), and α-terpineol (boiling point 217°C).
본 발명의 요변성제는, 아마이드 왁스와 수지와 분산매체가 미리 혼합되어서 포함되어 있는 것이므로, 요변성제를 플럭스에 첨가할 때, 아마이드 왁스가 신속하게 그리고 원활하게 분산된다. 그것에 의해 플럭스를 조제하는 가열 시간을 단축할 수 있다. 그 결과, 요변성제나 플럭스에 포함되는 수지조성물이 분해되거나 변질되거나 하는 열 손상을 일으키지 않는다.Since the thixotropic agent of the present invention contains a premix of amide wax, resin, and dispersion medium, when the thixotropic agent is added to the flux, the amide wax is quickly and smoothly dispersed. Thereby, the heating time for preparing the flux can be shortened. As a result, the resin composition contained in the thixotropic agent or flux does not cause thermal damage such as decomposition or deterioration.
본 발명의 요변성제는, 예를 들면 다음과 같이 해서 조제된다.The thixotropic agent of the present invention is prepared, for example, as follows.
탄소수 12 내지 22의 포화 지방족 모노카복실산 및/또는 탄소수 12 내지 22의 하이드록시기 함유 지방족 모노카복실산을 몰비로 합계 1 내지 3몰 당량, 바람직하게는 2 내지 3몰 당량과, 다염기산류인 탄소수 2 내지 12의 지방족 다이카복실산을 몰비로 1 내지 5몰 당량, 바람직하게는 2 내지 3몰 당량과, 다이아민류인 탄소수 2 내지 14의 지방족다이아민 및/또는 테트라아민류인 탄소수 2 내지 14의 지방족 테트라아민을 몰비로 합계 1 내지 6몰 당량, 바람직하게는 3 내지 4몰 당량을, 무용매에서, 160 내지 300℃로 가열하면서 2 내지 10시간, 탈수 축합반응시킨다. 그것에 의해, 포화 지방족 모노카복실산 및/또는 하이드록시기 함유 지방족 모노카복실산과, 지방족 다이카복실산과, 지방족다이아민 및/또는 지방족 테트라아민이 탈수 축합되어 생성된 탈수 축합물인 아마이드 왁스를 얻을 수 있다. 이 아마이드 왁스를 분쇄기에 투입하고, 평균 입자 직경 20㎛ 이하의 분체 형태 또는 작은 덩어리 형태가 되도록 분쇄한다.A total of 1 to 3 mole equivalents, preferably 2 to 3 mole equivalents, of saturated aliphatic monocarboxylic acids having 12 to 22 carbon atoms and/or hydroxy group-containing aliphatic monocarboxylic acids having 12 to 22 carbon atoms, and 2 to 12 carbon atoms of polybasic acids. 1 to 5 molar equivalents, preferably 2 to 3 molar equivalents, of aliphatic dicarboxylic acid, and aliphatic diamines having 2 to 14 carbon atoms and/or aliphatic tetraamines having 2 to 14 carbon atoms, which are diamines, in molar ratio. A total of 1 to 6 molar equivalents, preferably 3 to 4 molar equivalents, are subjected to a dehydration condensation reaction in the absence of a solvent while heating to 160 to 300°C for 2 to 10 hours. As a result, amide wax, which is a dehydration condensation product produced by dehydration condensation of a saturated aliphatic monocarboxylic acid and/or a hydroxyl group-containing aliphatic monocarboxylic acid, an aliphatic dicarboxylic acid, and an aliphatic diamine and/or an aliphatic tetraamine, can be obtained. This amide wax is put into a grinder and pulverized to form a powder or small lump with an average particle diameter of 20 ㎛ or less.
다음에, 아마이드 왁스의 1 내지 40질량%, 바람직하게는 10 내지 30질량%와, 10000 이하의 분자량을 지니는 수지의 20 내지 60질량%, 바람직하게는 30 내지 50질량%와, 180℃ 이상의 비점을 지니는 분산매체의 20 내지 60질량%, 바람직하게는 30 내지 50질량%를 혼합한다. 요변성제를 포함하는 플럭스가 납땜에 이용될 경우, 수지로서 로진계 수지가 바람직하다. 또 분산매체로서 글리콜 에터류가 바람직하다. 이 혼합물을 90 내지 110℃로 가열하는 것에 의해, 아마이드 왁스와 수지를 연화되게 한다. 이 온도를 유지하면서 1 내지 2시간 가열 분산시키고, 냉각시킴으로써 요변성제를 얻는다. 얻어지는 요변성제는 담황색 내지 갈색을 띠는 점조성을 지니는 페이스트 형태이다.Next, 1 to 40% by mass, preferably 10 to 30% by mass, of amide wax, 20 to 60% by mass, preferably 30 to 50% by mass of resin having a molecular weight of 10000 or less, and a boiling point of 180°C or higher. 20 to 60% by mass, preferably 30 to 50% by mass, of the dispersion medium having is mixed. When a flux containing a thixotropic agent is used for soldering, a rosin-based resin is preferred as the resin. Also, glycol ethers are preferred as the dispersion medium. By heating this mixture to 90 to 110° C., the amide wax and resin are softened. The thixotropic agent is obtained by heating and dispersing for 1 to 2 hours while maintaining this temperature and cooling. The resulting thixotropic agent is in the form of a paste with a light yellow to brown consistency.
요변성제의 본래의 물성을 훼손시키지 않는 한, 전술한 화합물 이외에, 방향족 모노카복실산, 방향족 다이카복실산, 방향족 다이아민류, 및/또는 방향족 테트라아민류가, 요변성제에 포함되어 있어도 된다. 또 아마이드 왁스의 탈수 축합물은, 1종류라도 되고, 복수 종류의 혼합물이어도 된다. 또한 요변성제의 특성을 훼손시키지 않는 한, 고비점 용제가 요변성제에 포함되어 있어도 된다.As long as the original physical properties of the thixotropic agent are not impaired, the thixotropic agent may contain aromatic monocarboxylic acids, aromatic dicarboxylic acids, aromatic diamines, and/or aromatic tetraamines in addition to the above-described compounds. Additionally, the dehydration condensate of amide wax may be one type or a mixture of multiple types. Additionally, a high boiling point solvent may be included in the thixotropic agent as long as it does not impair the properties of the thixotropic agent.
또한, 아마이드 왁스의 열안정성을 높이기 위하여, 아마이드 왁스 합성 시에 산화방지제를 첨가하는 것도 효과적이다. 이 산화방지제는, 아마이드 왁스 성분과의 상용성이 양호하지 않으면 안 된다. 그 이유로서, 산화방지제는, 아마이드 왁스 성분의 열안정성을 높이므로, 분리되어서는 그 목적을 달성하지 못한다. 산화방지제로서는 페놀계 산화방지제, 포스파이트계 산화방지제, 황계 산화방지제를 들 수 있다.Additionally, in order to increase the thermal stability of amide wax, it is effective to add an antioxidant when synthesizing amide wax. This antioxidant must have good compatibility with the amide wax component. For that reason, since antioxidants increase the thermal stability of the amide wax component, their purpose cannot be achieved if they are separated. Antioxidants include phenol-based antioxidants, phosphite-based antioxidants, and sulfur-based antioxidants.
보다 구체적인 산화방지제로서는, 페놀계 산화방지제로서, 부틸화하이드록시톨루엔, 4-하이드록시메틸-2,6-다이-t-부틸페놀, 2,6-다이-t-부틸-4-에틸페놀, n-옥타데실-β-(4'-하이드록시-3',5'-다이-t-부틸페닐)프로피오네이트, 토코페롤, 2,4,비스(옥틸티오메틸)-6-t-메틸페놀, 2,4-비스[(도데실티오)메틸]-6-메틸페놀, 2,2'-메틸렌 비스(4-메틸-6-t-부틸페놀), 2,2'-메틸렌 비스(4-에틸-6-t-부틸페놀), 4,4'-메틸렌 비스(2,6-다이-t-부틸페놀), 4,4'-부틸리덴 비스(6-t-부틸-m-크레졸), 1,1-비스(2'-메틸-4'-하이드록시-5'-t-부틸-페닐)부탄, 4,4'-티오비스(6-t-부틸-m-크레졸), 4,4'-티오비스(3-메틸-6-t-부틸페놀), N,N'-헥사메틸렌 비스(3,5-다이-t-부틸-4-하이드록시하이드로신나마이드), 3,5-다이-t-부틸-4-하이드록시벤질포스폰산모노에틸에스터 칼슘염, 헥사메틸렌 비스(3,5-다이-t-부틸-4-하이드록시하이드로신나메이트), 트라이에틸렌글리콜 비스-3-(3-t-부틸-4-하이드록시-5-메틸페닐)프로피오네이트, 2,2'-옥사마이드 비스[에틸3-(3,5-다이-t-부틸-4-하이드록시페닐)프로피오네이트], 2,2'-에틸리덴 비스(4,6-다이-t-부틸페놀), N,N'-1,3-프로판다이일비스(3,5-다이-t-부틸-4-하이드록시하이드로신나마이드), 2,4-다이메틸-6-(1-메틸펜타데실)페놀, 1,1,3-트리스(2-메틸-4-하이드록시-5-t-부틸페닐)부탄), 2-t-부틸-6-(3-t-부틸-2-하이드록시-5-메틸벤질)-4-메틸페닐아크릴레이트, 1,3,5-트라이메틸-2,4,6-트리스(3,5-다이-t-부틸-4-하이드록시벤질)벤젠, 테트라키스[메틸렌-3-(3',5)다이-t-부틸-4'-하이드록시페닐]프로피오네이트]메탄, 2,2'-메틸렌 비스[6-(1-메틸사이클로헥실)-p-크레졸], 비스[3,3-비스(4'-하이드록시-3'-t-부틸페닐)부탄산]글리콜 에스터, 1,4-벤젠다이카복실산 비스 [2-(1,1-다이메틸에틸)-6-[[3-(1,1-다이메틸에틸)-2-하이드록시-5-메틸페닐]메틸]-4-메틸페닐]에스터, N,N'-비스 {3-(3,5-다이-t-부틸-4-하이드록시페닐)프로피오닐}하이드라진, 3,9-비스 [2-{3-(3-t-부틸-4-하이드록시-5-메틸페닐)프로피오닐옥시}-1,1-다이메틸에틸]-2,4,8,10-테트라옥사스피로[5,5]운데칸, 4,4'-바이페닐렌다이포스핀산 테트라키스(2,4-다이-t-부틸페닐), 1,3,5-트리스(3',5-다이-t-부틸-4'-하이드록시벤질)-s-트라이아진-2,4,6(1H,3H,5H)-트라이온, 1,3,5-트리스(4-t-부틸-3-하이드록시-2,6-다이메틸벤질)-1,3,5-트라이아진-2,4,6-(1H,3H,5H)-트라이온, 2,6-다이-t-부틸-4-{4,6-비스(옥틸티오)-1,3,5-트라이아진-2-일아미노}페놀, 1,3,5-트리스(2-프로페닐) 1,3,5-트라이아진-2,4,6(1H,3H,5H)-트라이온, 2-[4,6-다이(2,4-자일릴)-1,3,5-트라이아진-2-일]-5-옥틸옥시페놀, 2,2-메틸렌 비스(4-메틸6-노닐페놀)과 2,6-비스(2-하이드록시-3-노닐-5-메틸벤질)-P-크레졸의 혼합물, 4-메틸페놀과 아이소부틸렌과 다이사이클로펜타다이엔의 반응 생성물 및 2-[1-(2-하이드록시-3,5-다이-t-펜틸페닐)에틸]-4,6-다이-t-펜틸페닐아크릴레이트를 들 수 있다.More specific antioxidants include phenol-based antioxidants, such as butylated hydroxytoluene, 4-hydroxymethyl-2,6-di-t-butylphenol, 2,6-di-t-butyl-4-ethylphenol, n-octadecyl-β-(4'-hydroxy-3',5'-di-t-butylphenyl)propionate, tocopherol, 2,4,bis(octylthiomethyl)-6-t-methylphenol , 2,4-bis[(dodecylthio)methyl]-6-methylphenol, 2,2'-methylene bis(4-methyl-6-t-butylphenol), 2,2'-methylene bis(4- Ethyl-6-t-butylphenol), 4,4'-methylene bis(2,6-di-t-butylphenol), 4,4'-butylidene bis(6-t-butyl-m-cresol) , 1,1-bis(2'-methyl-4'-hydroxy-5'-t-butyl-phenyl)butane, 4,4'-thiobis(6-t-butyl-m-cresol), 4, 4'-thiobis(3-methyl-6-t-butylphenol), N,N'-hexamethylene bis(3,5-di-t-butyl-4-hydroxyhydrocinnamide), 3,5- Di-t-butyl-4-hydroxybenzylphosphonic acid monoethyl ester calcium salt, hexamethylene bis (3,5-di-t-butyl-4-hydroxyhydrocinnamate), triethylene glycol bis-3-( 3-t-butyl-4-hydroxy-5-methylphenyl)propionate, 2,2'-oxamide bis[ethyl 3-(3,5-di-t-butyl-4-hydroxyphenyl)propionate Nate], 2,2'-ethylidene bis(4,6-di-t-butylphenol), N,N'-1,3-propanediylbis(3,5-di-t-butyl-4- Hydroxyhydrocinnamide), 2,4-dimethyl-6-(1-methylpentadecyl)phenol, 1,1,3-tris(2-methyl-4-hydroxy-5-t-butylphenyl)butane ), 2-t-butyl-6-(3-t-butyl-2-hydroxy-5-methylbenzyl)-4-methylphenylacrylate, 1,3,5-trimethyl-2,4,6-tris (3,5-di-t-butyl-4-hydroxybenzyl)benzene, tetrakis[methylene-3-(3',5)di-t-butyl-4'-hydroxyphenyl]propionate]methane , 2,2'-methylene bis[6-(1-methylcyclohexyl)-p-cresol], bis[3,3-bis(4'-hydroxy-3'-t-butylphenyl)butanoic acid]glycol Ester, 1,4-benzenedicarboxylic acid bis [2-(1,1-dimethylethyl)-6-[[3-(1,1-dimethylethyl)-2-hydroxy-5-methylphenyl]methyl] -4-methylphenyl] ester, N,N'-bis {3-(3,5-di-t-butyl-4-hydroxyphenyl)propionyl}hydrazine, 3,9-bis [2-{3-( 3-t-butyl-4-hydroxy-5-methylphenyl) propionyloxy}-1,1-dimethylethyl]-2,4,8,10-tetraoxaspiro[5,5]undecane, 4, 4'-biphenylenediphosphinic acid tetrakis(2,4-di-t-butylphenyl), 1,3,5-tris(3',5-di-t-butyl-4'-hydroxybenzyl) -s-triazine-2,4,6(1H,3H,5H)-trione, 1,3,5-tris(4-t-butyl-3-hydroxy-2,6-dimethylbenzyl)- 1,3,5-triazine-2,4,6-(1H,3H,5H)-trione, 2,6-di-t-butyl-4-{4,6-bis(octylthio)-1 ,3,5-triazine-2-ylamino}phenol, 1,3,5-tris(2-propenyl) 1,3,5-triazine-2,4,6(1H,3H,5H)- Trione, 2-[4,6-di(2,4-xylyl)-1,3,5-triazin-2-yl]-5-octyloxyphenol, 2,2-methylene bis(4-methyl A mixture of 6-nonylphenol) and 2,6-bis(2-hydroxy-3-nonyl-5-methylbenzyl)-p-cresol, the reaction product of 4-methylphenol, isobutylene, and dicyclopentadiene and 2-[1-(2-hydroxy-3,5-di-t-pentylphenyl)ethyl]-4,6-di-t-pentylphenylacrylate.
포스파이트계 산화방지제로서, 트리스(노닐페닐)포스파이트, 트리스(믹스트, 모노 및 다이노닐페닐)포스파이트, 다이스테아릴펜타에리트리톨 다이포스파이트, 사이클릭네오펜탄테트라일 비스(옥타데실포스파이트), 4,4'-아이소프로필리덴다이페놀알킬(C12 내지 C15)포스파이트, 트리스(2,4-다이-t-부틸페닐)포스파이트, 4,4'-부틸리덴-비스(3-메틸-6-t-부틸페닐-다이-트라이데실포스파이트), 1,1,3-트리스(2-메틸-4-다이-트라이데실포스파이트-5-t-부틸-페닐)부탄과 다이페닐포스파이트의 혼합물, 4,4'-바이페닐렌다이포스핀산 테트라키스(2,4-다이-t-부틸페닐), 사이클릭네오펜탄테트라일비스(2,4-다이-t-부틸페닐포스파이트), 트리스(사이클로헥실페닐)포스파이트, 2-t-부틸-α-(3-t-부틸-4-하이드록시페닐)-p-쿠메닐비스(p-노닐페닐)포스파이트, 트리스-[2-(2,4,8,10-테트라부틸-5,7-다이옥사-6-포스포-다이벤조-{a,c}사이클로헵텐-6-일-옥시)에틸]아민, 비스-[2-메틸-4,6-비스-(1,1-다이메틸에틸)페닐]에틸포스파이트, 3,9-비스{2,4-비스(1-메틸-1-페닐에틸)페녹시}-2,4,8,10-테트라옥사-3,9-다이포스파스피로[5,5]운데칸, 6-[3-(3-t-부틸-4-하이드록시-5-메틸페닐)프로폭시-2,4,8,10-테트라-t-부틸벤즈[d,f][1,3,2]다이옥사포스페핀, 9,10-다이하이드로-9-옥사-10-포스파페난트렌-10-옥사이드, (삼염화인과 바이페닐)의 프리델 크라프츠 부가물과 4,6-다이-t-부틸-m-크레졸의 축합에 의해 합성되는 바이페닐을 지니는 4,6-다이-t-부틸-m-크레질포스포나이트 축합물, 3,9-비스(2,6-다이-t-부틸-4-메틸페녹시)-2,4,8,10-테트라옥사-3,9-다이포스파스피로[5,5]운데칸, 2,4,8,10-테트라키스(1,1-다이메틸에틸)-6-(2-에틸헥실옥시)-12H-다이벤조[d,g][1,3,2]다이옥사포스포신, 및 카베톡시메틸다이에틸포스포네이트를 들 수 있다.Phosphite-based antioxidants include tris(nonylphenyl)phosphite, tris(mixed, mono, and dinonylphenyl)phosphite, distearylpentaerythritol diphosphite, and cyclic neopentanetetriyl bis(octadecyl phosphite). ), 4,4'-isopropylidene diphenolalkyl (C 12 to C 15 ) phosphite, tris (2,4-di-t-butylphenyl) phosphite, 4,4'-butylidene-bis ( 3-methyl-6-t-butylphenyl-di-tridecylphosphite), 1,1,3-tris(2-methyl-4-di-tridecylphosphite-5-t-butyl-phenyl)butane Mixture of diphenylphosphites, 4,4'-biphenylenediphosphinic acid tetrakis(2,4-di-t-butylphenyl), cyclicneopentanetetraylbis(2,4-di-t-butyl) phenyl phosphite), tris(cyclohexylphenyl) phosphite, 2-t-butyl-α-(3-t-butyl-4-hydroxyphenyl)-p-cumenylbis(p-nonylphenyl) phosphite, tris-[2-(2,4,8,10-tetrabutyl-5,7-dioxa-6-phospho-dibenzo-{a,c}cyclohepten-6-yl-oxy)ethyl]amine, Bis-[2-methyl-4,6-bis-(1,1-dimethylethyl)phenyl]ethylphosphite, 3,9-bis{2,4-bis(1-methyl-1-phenylethyl)phenok Si}-2,4,8,10-tetraoxa-3,9-diphosphaspiro[5,5]undecane, 6-[3-(3-t-butyl-4-hydroxy-5-methylphenyl ) Propoxy-2,4,8,10-tetra-t-butylbenz[d,f][1,3,2]dioxaphosphepine, 9,10-dihydro-9-oxa-10-phosphene Nanthrene-10-oxide, 4,6-di-bearing biphenyl, synthesized by condensation of Friedel-Krafts adduct of (phosphorus trichloride and biphenyl) with 4,6-di-t-butyl-m-cresol. t-butyl-m-crezyllphosphonite condensate, 3,9-bis(2,6-di-t-butyl-4-methylphenoxy)-2,4,8,10-tetraoxa-3, 9-diphosphaspiro[5,5]undecane, 2,4,8,10-tetrakis(1,1-dimethylethyl)-6-(2-ethylhexyloxy)-12H-dibenzo[ d,g][1,3,2]dioxaphosphosine, and carbetoxymethyldiethylphosphonate.
황계 산화방지제로서, 3,3'-티오다이프로피온산다이라우릴, 3,3'-티오다이프로피온산다이미리스틸, 3,3'-티오다이프로피온산다이스테아릴, 다이옥타데실다이설파이드를 들 수 있다.Examples of sulfur-based antioxidants include dilauryl 3,3'-thiodipropionate, dimyristyl 3,3'-thiodipropionate, distearyl 3,3'-thiodipropionate, and dioctadecyl disulfide. .
아마이드 왁스 등과의 상용성이 우수한 산화방지제로서, 포스파이트계 산화방지제가 바람직하고, 그 중에서도, 트리스(믹스트, 모노 및 다이노닐페닐)포스파이트, 다이스테아릴펜타에리트리톨 다이포스파이트, 트리스(2,4-다이-t-부틸페닐)포스파이트, 3,9-비스{2,4-비스(1-메틸-1-페닐에틸)페녹시}-2,4,8,10-테트라옥사-3,9-다이포스파스피로[5,5]운데칸, 6-[3-(3-t-부틸-4-하이드록시-5-메틸페닐)프로폭시-2,4,8,10-테트라-t-부틸벤즈[d,f][1,3,2]다이옥사포스페핀 및/또는 3,9-비스(2,6-다이-t-부틸-4-메틸페녹시)-2,4,8,10-테트라옥사-3,9-다이포스파스피로[5,5]운데칸이 보다 바람직하다.As antioxidants with excellent compatibility with amide waxes, etc., phosphite-based antioxidants are preferable, and among them, tris (mixed, mono, and dinonylphenyl) phosphites, distearyl pentaerythritol diphosphites, and tris (2 ,4-di-t-butylphenyl)phosphite, 3,9-bis{2,4-bis(1-methyl-1-phenylethyl)phenoxy}-2,4,8,10-tetraoxa-3 ,9-diphosphaspiro[5,5]undecane, 6-[3-(3-t-butyl-4-hydroxy-5-methylphenyl)propoxy-2,4,8,10-tetra-t -Butylbenz[d,f][1,3,2]dioxaphosphepine and/or 3,9-bis(2,6-di-t-butyl-4-methylphenoxy)-2,4,8 , 10-Tetraoxa-3,9-diphosphaspiro[5,5]undecane is more preferred.
이들 산화방지제는, 아마이드 왁스의 합성 후에 한번에 첨가해도 되고, 그것의 합성 전후에 나누어서 첨가해도 된다. 한번에 첨가할 경우, 99.98 내지 95질량%의 아마이드 왁스에, 0.02 내지 5질량%의 산화방지제를 첨가해서 혼합할 수 있다. 나누어서 첨가할 경우, 아마이드 왁스의 합성 전에, 예를 들면 다염기산류 및 다이아민류에, 0.01 내지 1질량%의 산화방지제를 첨가해서 아마이드 왁스를 합성하고, 얻어진 아마이드 왁스에 0.01 내지 4.99질량%의 산화방지제를 첨가하는 것이 바람직하다. 나누어서 첨가할 경우더라도 한번에 첨가할 경우와 마찬가지로, 아마이드 왁스의 99.98 내지 95질량%에 상용하고 있는 산화방지제가, 총량으로 0.02 내지 5질량%인 것이 바람직하다.These antioxidants may be added all at once after the synthesis of the amide wax, or may be added separately before and after the synthesis of the amide wax. When added at once, 0.02 to 5% by mass of antioxidant can be added and mixed to 99.98 to 95% by mass of amide wax. When adding in portions, before synthesizing the amide wax, for example, 0.01 to 1% by mass of an antioxidant is added to polybasic acids and diamines to synthesize the amide wax, and 0.01 to 4.99% by mass of the antioxidant is added to the obtained amide wax. It is desirable to add. Even when adding in portions, it is preferable that the total amount of antioxidants used in 99.98 to 95% by mass of the amide wax is 0.02 to 5% by mass, as in the case of adding at once.
본 발명의 플럭스는, 상기 요변성제와, 플럭스 수지와, 용제를 적어도 포함하고 있다. 이 플럭스 수지로서, 요변성제에 포함되는 수지로서 열거한 상기 수지를 들 수 있다. 또한 상기 수지 대신에, 또는 부가해서, ε-카프로락탐, γ-락탐, 및 δ-락탐과 같은 환상 아마이드가 중합 또는 공중합된 폴리아마이드를 들 수 있다. 폴리아마이드가 함유되어 있는 것에 의해, 플럭스의 내열성이 향상된다.The flux of the present invention contains at least the thixotropic agent, flux resin, and solvent. Examples of this flux resin include the resins listed above as resins contained in thixotropic agents. Also, instead of or in addition to the above resins, polyamides obtained by polymerizing or copolymerizing cyclic amides such as ε-caprolactam, γ-lactam, and δ-lactam can be used. Containing polyamide improves the heat resistance of the flux.
플럭스에 포함되는 용제로서, 요변성제에 포함되는 분산매체로서 열거한 상기 모노올 및/또는 폴리올을 들 수 있다. 플럭스 수지 및 용제는, 요변성제에 포함되는 수지 및 분산매체와, 각각 동종인 것이 바람직하다. 그것에 의해, 요변성제와 플럭스의 상용성이 양호해지므로, 요변성제에 포함되는 아마이드 왁스가, 플럭스 중에 균일하게 그리고 신속하게 분산된다.Solvents contained in the flux include the monools and/or polyols listed above as dispersion media contained in the thixotropic agent. The flux resin and solvent are preferably of the same type as the resin and dispersion medium contained in the thixotropic agent. As a result, the compatibility between the thixotropic agent and the flux becomes good, so the amide wax contained in the thixotropic agent is dispersed uniformly and quickly in the flux.
요변성제의 함유량은, 5 내지 50질량%인 것이 바람직하고, 10 내지 40질량%인 것이 보다 바람직하며, 10 내지 30질량%인 것이 더한층 바람직하다. 요변성제가 5질량% 미만이면, 아마이드 왁스의 양이 부족하고, 솔더 페이스트의 열 처짐성을 억제할 수 없다. 한편 요변성제가 50질량%를 초과하면, 아마이드 왁스의 함유량이 과다로 된다. 그 때문에, 플럭스 조제 시에 가열 용융시킨 후의 냉각에 의해서, 아마이드 왁스가 작은 덩어리 형태로 석출되어 버려, 플럭스 중에의 균일한 분산을 방해하게 되어버린다.The content of the thixotropic agent is preferably 5 to 50 mass%, more preferably 10 to 40 mass%, and even more preferably 10 to 30 mass%. If the thixotropic agent is less than 5% by mass, the amount of amide wax is insufficient and the thermal sagging of the solder paste cannot be suppressed. On the other hand, if the thixotropic agent exceeds 50% by mass, the amide wax content becomes excessive. Therefore, when preparing the flux, the amide wax is precipitated in the form of small lumps when heated and melted and then cooled, which prevents uniform dispersion in the flux.
또한, 플럭스 수지의 함유량은, 25 내지 65질량%인 것이 바람직하고, 30 내지 60질량%인 것이 보다 바람직하며, 35 내지 55질량%인 것이 더한층 바람직하다. 또한 용제는, 20 내지 50질량%인 것이 바람직하고, 20 내지 45질량%인 것이 보다 바람직하며, 25 내지 45질량%인 것이 더한층 바람직하다.Moreover, the content of the flux resin is preferably 25 to 65 mass%, more preferably 30 to 60 mass%, and even more preferably 35 to 55 mass%. Moreover, the solvent is preferably 20 to 50 mass%, more preferably 20 to 45 mass%, and even more preferably 25 to 45 mass%.
플럭스에, 활성제가 포함되어 있어도 된다. 그것에 의해, 구리와 같은 납땜해야 할 금속의 표면을 덮고 있는 산화막이 신속하게 제거되므로, 솔더 페이스트에 포함되는 땜납과 금속의 표면의 젖음성이 향상되어, 확실히 납땜할 수 있다. 그 결과, 땜납 브리지나 땜납 볼과 같은 납땜 불량을 방지할 수 있다. 활성제로서, 예를 들면, 다이페닐구아니딘 브로민화수소산염, 사이클로헥실아민 브로민화수소산염, 다이에틸아민염산염, 트리에탄올아민 브로민화수소산염, 및 모노에탄올아민 브로민화수소산염과 같은 유기 아민의 할로겐화 수소산염; 말론산, 숙신산, 말레산, 글루타르산, 수베르산, 아디프산 및 세바스산과 같은 유기산, 특히 다이카복실산; 구연산, 1,2-하이드록시스테아르산 및 1,2-하이드록시올레산과 같은 하이드록시지방산; 테트라브로모메탄, 1,1,2,2-테트라브로모부탄, 1,2-다이브로모-2-부텐, 2,3-다이브로모-1-프로판올, 1,2-다이브로모-2,3-부탄다이올, 트랜스-2,3-다이브로모-2-부텐-1,4-다이올, 2,2-비스(브로모메틸)-1,3-프로판다이올과 같은 유기 할로겐 화합물을 들 수 있다.The flux may contain an activator. As a result, the oxide film covering the surface of the metal to be soldered, such as copper, is quickly removed, so the wettability of the surface of the solder and metal contained in the solder paste is improved, allowing reliable soldering. As a result, soldering defects such as solder bridges and solder balls can be prevented. As an activator, hydrogen halides of organic amines such as, for example, diphenylguanidine hydrobromide, cyclohexylamine hydrobromide, diethylamine hydrochloride, triethanolamine hydrobromide, and monoethanolamine hydrobromide. acid salt; Organic acids such as malonic acid, succinic acid, maleic acid, glutaric acid, suberic acid, adipic acid and sebacic acid, especially dicarboxylic acids; Hydroxy fatty acids such as citric acid, 1,2-hydroxystearic acid, and 1,2-hydroxyoleic acid; Tetrabromomethane, 1,1,2,2-tetrabromobutane, 1,2-dibromo-2-butene, 2,3-dibromo-1-propanol, 1,2-dibromo-2,3 -Organic halogen compounds such as butanediol, trans-2,3-dibromo-2-butene-1,4-diol, and 2,2-bis(bromomethyl)-1,3-propanediol. You can.
활성제의 함유량은, 0.1 내지 5질량%인 것이 바람직하고, 0.5 내지 3질량%인 것이 보다 바람직하다. 0.1질량% 미만이면, 충분한 효과가 얻어지지 않는다. 5질량%를 초과하면, 납땜 후에 세정을 필요로 할 뿐만 아니라, 세정에 의해서도 전부 제거하지 못한 활성제 때문에, 땜납이나 금속 표면이 부식되어서 전기적 접합이 끊겨 버린다.The content of the activator is preferably 0.1 to 5 mass%, and more preferably 0.5 to 3 mass%. If it is less than 0.1% by mass, sufficient effect cannot be obtained. If it exceeds 5% by mass, not only will cleaning be required after soldering, but the solder and metal surfaces will corrode due to the activator that cannot be completely removed even by cleaning, resulting in loss of electrical connection.
플럭스는, 요변성제와, 플럭스 수지와, 용제와, 필요에 따라서 활성제를, 혼합하고, 80 내지 120℃로 가열하면서 1 내지 3시간, 교반함으로써, 조제할 수 있다. 가열 온도 및 교반 시간은, 플럭스에 포함되는 각 성분의 비나, 요변성제의 평균 입자 직경과 같은 조건에 의해 적당히 설정된다. 얻어지는 플럭스는, 담황색 내지 갈색의 페이스트 형태이다.Flux can be prepared by mixing a thixotropic agent, a flux resin, a solvent, and, if necessary, an activator, and stirring the mixture for 1 to 3 hours while heating to 80 to 120°C. The heating temperature and stirring time are appropriately set depending on conditions such as the ratio of each component contained in the flux and the average particle diameter of the thixotropic agent. The resulting flux is in the form of a light yellow to brown paste.
플럭스는, 후술하는 바와 같이, 땜납 분말이 혼합됨으로써, 솔더 페이스트를 조제하는데 사용된다. 또한, 실 땜납의 중심축을 따라서 메워넣어지거나, 납땜해야 할 금속 표면에 도포나 인쇄에 의해서 부착시키거나 해서 사용된다.Flux is used to prepare solder paste by mixing solder powder, as described later. Additionally, it is used by filling it along the central axis of the thread solder or by attaching it to the metal surface to be soldered by applying or printing.
본 발명의 솔더 페이스트는, 상기 플럭스와, 땜납을 포함하고 있는 것이다. 그것에 의해, 가열 처짐성 억제 성분인 아마이드 왁스를 포함한 요변성제를, 솔더 페이스트에 분산시킬 수 있다.The solder paste of the present invention contains the above flux and solder. Thereby, the thixotropic agent containing amide wax, which is a heat sagging suppressing component, can be dispersed in the solder paste.
땜납은, 1 내지 20㎛의 평균 입자 직경을 지니는 땜납 분말인 것이 바람직하다. 땜납 분말로서, 공정 땜납과 같은 Sn-Pb계 땜납 분말; Sn-Cu계, Sn-Ag계, Sn-Zn계 및 Sn-Ag-Cu계와 같은 무연 땜납 분말을 들 수 있다. 본 발명의 솔더 페이스트는, 가열 처짐성 억제 성분인 아마이드 왁스가 균일하게 분산되어 있으므로, 고온조건의 프리히트를 요하는 무연 땜납 분말을 포함하고 있어도, 열 처짐성을 일으키지 않는다.The solder is preferably a solder powder having an average particle diameter of 1 to 20 μm. As solder powder, Sn-Pb solder powder such as eutectic solder; Lead-free solder powders such as Sn-Cu-based, Sn-Ag-based, Sn-Zn-based, and Sn-Ag-Cu-based solder powders may be included. Since the amide wax, which is a heat sagging suppressing component, is uniformly dispersed in the solder paste of the present invention, it does not cause heat sagging even if it contains lead-free solder powder that requires preheating under high temperature conditions.
본 발명의 솔더 페이스트는, 상기 플럭스에 땜납 분말을 투입하고, 교반, 혼합함으로써 조제된다. 솔더 페이스트 중, 땜납 분말은 65 내지 95질량%인 것이 바람직하고, 80 내지 95질량%인 것이 보다 바람직하다. 땜납 분말이 65질량% 미만이면, 솔더 페이스트 중의 땜납 분말의 함유량이 과소해져, 기판 상의 한정된 면적 내에서 확실히 납땜할 수 없다. 한편, 95질량%를 초과하면, 땜납 분말의 함유량이 과다가 되므로, 페이스트가 형성되지 않아, 취급하기 곤란해져 버린다.The solder paste of the present invention is prepared by adding solder powder to the flux, stirring and mixing. In the solder paste, the solder powder is preferably 65 to 95% by mass, and more preferably 80 to 95% by mass. If the solder powder is less than 65% by mass, the content of solder powder in the solder paste becomes too small, making it impossible to reliably solder within a limited area on the substrate. On the other hand, if it exceeds 95% by mass, the solder powder content becomes excessive, so a paste is not formed and handling becomes difficult.
솔더 페이스트는, 리플로우 방식에 의한 납땜에 적합하게 사용된다. 솔더 페이스트는, 프린트 기판에 배치된 금속배선 상의 납땜해야 할 위치에, 인쇄에 의해서 부착된다. 인쇄는, 스크린 인쇄, 잉크젯 인쇄, 오프셋, 그라비어 인쇄, 및/또는 플렉소 인쇄에 의해 행할 수 있다.Solder paste is suitably used for soldering by the reflow method. The solder paste is applied by printing to the position to be soldered on the metal wiring arranged on the printed board. Printing can be performed by screen printing, inkjet printing, offset, gravure printing, and/or flexo printing.
솔더 페이스트 상에, 금속배선에 전기적 접속되는 전자부품이 탑재된다. 이 프린트 기판이, 리플로우화로 내에 투입된다. Sn-Pb계 땜납 분말을 포함하는 솔더 페이스트의 경우, 리플로우화로 내에서, 150 내지 170℃에서 60 내지 120초의 프리히트가 행해진 후, 180 내지 185℃에서 30 내지 50초의 메인 히트가 행해진다. 한편, 무연 땜납 분말을 포함하는 솔더 페이스트의 경우, 프리히트 및 메인 히트는 각기, 170 내지 190℃에서 60 내지 120초, 및 210 내지 260℃에서 30 내지 50초이다. 그것에 의해, 땜납 분말이 용융되어, 금속배선과 전자부품이, 통전 가능하게 전기적 접합된다. 그 후 냉각되어, 필요에 따라서 세정이 행해진다.Electronic components electrically connected to metal wiring are mounted on the solder paste. This printed board is put into a reflow furnace. In the case of a solder paste containing Sn-Pb solder powder, in a reflow furnace, a preheat is performed at 150 to 170°C for 60 to 120 seconds, followed by a main heat at 180 to 185°C for 30 to 50 seconds. . Meanwhile, in the case of a solder paste containing lead-free solder powder, the preheat and main heat are 60 to 120 seconds at 170 to 190°C and 30 to 50 seconds at 210 to 260°C, respectively. As a result, the solder powder is melted, and the metal wiring and the electronic component are electrically connected to enable current conduction. Afterwards, it is cooled and washed as needed.
솔더 페이스트의 사용 방법으로서 리플로우 방식을 들었지만, 땜납조 내에서 용융시킨 솔더 페이스트에, 프린트 기판의 한쪽 면을 침지시킴으로써 납땜을 행하는 플로우 방식에 사용해도 되고, 주걱으로 퍼내어 납땜해야 할 개소에 도포하고, 전자부품을 탑재시킨 후, 땜납 인두로, 솔더 페이스트를 용융시켜서 납땜을 행하는 수동 작업에 사용해도 된다.The reflow method has been mentioned as a method of using solder paste, but it can also be used in the flow method, which performs soldering by immersing one side of the printed board in solder paste melted in a solder tank, or scooped out with a spatula and applied to the area to be soldered. After mounting the electronic components, it may be used for manual work in which solder is performed by melting the solder paste with a soldering iron.
본 발명의 요변성제는, 도전성 도료 및 도전성 접착제와 같이 금속분말을 많이 포함하는 도전성 페이스트에 혼합되어서 사용되어도 된다. 도전성 페이스트는, 금, 은, 구리, 백금 및 팔라듐과 같은 0.01 내지 10㎛의 평균 입자 직경을 지니는 금속분말이, 페이스트 수지와, 용매에 분산되어 있는 것이다. 도전성 페이스트는, 수지 필름과 같은 대상물에 도포되고, 예를 들면 150 내지 200℃의 고온으로 소결됨으로써 대상물을 도전성 물질로 코팅할 수 있다. 그것에 의해, 예를 들면, 가요성 프린트배선판이나, 필름 안테나를 제조한다. 본 발명의 요변성제에 따르면, 고온의 소결이어도, 도전성 페이스트의 열 처짐성을 야기시키지 않는다.The thixotropic agent of the present invention may be used mixed in a conductive paste containing a large amount of metal powder, such as a conductive paint or a conductive adhesive. A conductive paste is a metal powder having an average particle diameter of 0.01 to 10 μm, such as gold, silver, copper, platinum, and palladium, dispersed in a paste resin and a solvent. The conductive paste can be applied to an object such as a resin film and sintered at a high temperature of, for example, 150 to 200°C to coat the object with a conductive material. Thereby, for example, flexible printed wiring boards and film antennas are manufactured. According to the thixotropic agent of the present invention, even high temperature sintering does not cause thermal sagging of the conductive paste.
[[ 실시예Example ]]
(요변성제의 조제)(Preparation of thixotropic agent)
본 발명을 적용하는 요변성제를 조제한 조제예 1 내지 4 및 이 요변성제를 포함하는 실시예 1 내지 4의 플럭스, 및 본 발명의 적용 외의 요변성제를 조제한 비교조제예 1 내지 5 및 이 요변성제를 포함하는 비교예 1 내지 5의 플럭스를, 각기 나타낸다.Preparation Examples 1 to 4 in which a thixotropic agent to which the present invention is applied and the fluxes of Examples 1 to 4 containing this thixotropic agent, and Comparative Preparation Examples 1 to 5 in which a thixotropic agent other than the present invention is prepared and this thixotropic agent are prepared. The fluxes of Comparative Examples 1 to 5 included are shown separately.
(조제예 1) 아마이드 왁스와 수지와 분산매체를 함유한 요변성제의 조제(Preparation Example 1) Preparation of a thixotropic agent containing amide wax, resin, and dispersion medium.
교반기, 온도계, 분수기를 구비한 반응 장치에, (a) 하이드록시기 함유 지방족 모노카복실산인 12-하이드록시스테아르산 1000.0질량부와, (b) 지방족 다이카복실산인 세바스산 1010.0질량부를 첨가하고, 80 내지 100℃로 가온시켜 12-하이드록시스테아르산을 용해시켰다. 거기에, (c) 다이아민인 헥사메틸렌다이아민 780.5질량부를 첨가하고, 질소분위기 하, 210 내지 220℃에서 3 내지 5시간, 탈수시키면서 축합반응을 행하여 아마이드화시켜, 산가 3.2, 아민가 2.4의 아마이드 왁스를 얻었다(몰비로 (a):(b):(c)=2몰:2.7몰:3.3몰). 얻어진 아마이드 왁스를, 분쇄기에 투입해서 평균 입자 직경 20㎛ 이하로 분쇄하였다. 그 다음에, 이 아마이드 왁스 20질량%, 로진계 수지인 파인 크리스탈 KE-604(아라카와카가쿠쿄고(荒川化學工業) 주식회사 제품, 분자량 350) 40질량%, 및 헥실다이글리콜 40질량%를 혼합하고, 90 내지 110℃로 가열하면서 1 내지 2시간 가열 분산시키고, 그 후 냉각시켰다. 그것에 의해 조제예 1의 요변성제를 얻었다.To a reaction apparatus equipped with a stirrer, thermometer, and fountain, (a) 1000.0 parts by mass of 12-hydroxystearic acid, which is a hydroxyl group-containing aliphatic monocarboxylic acid, and (b) 1,010.0 parts by mass of sebacic acid, which is an aliphatic dicarboxylic acid, are added, and 80.0 parts by mass are added. 12-hydroxystearic acid was dissolved by heating to 100°C. To this, (c) 780.5 parts by mass of hexamethylenediamine, which is a diamine, was added, and a condensation reaction was performed under a nitrogen atmosphere at 210 to 220° C. for 3 to 5 hours while dehydrating to amidize, resulting in an amide wax with an acid value of 3.2 and an amine value of 2.4. was obtained (molar ratio (a):(b):(c)=2 mole:2.7 mole:3.3 mole). The obtained amide wax was put into a grinder and pulverized to an average particle diameter of 20 μm or less. Next, 20% by mass of this amide wax, 40% by mass of Fine Crystal KE-604 (produced by Arakawa Chemical Engineering Co., Ltd., molecular weight 350), which is a rosin-based resin, and 40% by mass of hexyl diglycol were mixed. , heat-dispersed for 1 to 2 hours while heating to 90 to 110°C, and then cooled. As a result, the thixotropic agent of Preparation Example 1 was obtained.
(조제예 2) 아마이드 왁스와 수지와 분산매체를 함유한 요변성제의 조제(Preparation Example 2) Preparation of a thixotropic agent containing amide wax, resin, and dispersion medium.
조제예 1의 헥사메틸렌다이아민 대신에, (c) 메타자일렌다이아민 915.1질량부를 이용한 것 이외에는, 조제예 1과 마찬가지로 해서, 산가 4.2, 아민가 3.6의 아마이드 왁스를 얻었다(몰비로 (a):(b):(c)=2몰:2.7몰:3.3몰). 얻어진 아마이드 왁스를, 분쇄기에 투입해서 평균 입자 직경 20㎛ 이하로 분쇄하였다. 그 다음에, 이 아마이드 왁스 20질량%, 로진계 수지인 파인 크리스탈 KE-604(아라카와카가쿠쿄고 주식회사 제품) 40질량%, 및 헥실다이글리콜 40질량%를 혼합하고, 90 내지 110℃로 가열하면서 1 내지 2시간 가열 분산시키고, 그 후 냉각시켰다. 그것에 의해 조제예 2의 요변성제를 얻었다.An amide wax with an acid value of 4.2 and an amine value of 3.6 was obtained in the same manner as in Preparation Example 1, except that 915.1 parts by mass of (c) metaxylenediamine was used instead of the hexamethylenediamine in Preparation Example 1 (molar ratio (a): (b):(c)=2 moles:2.7 moles:3.3 moles). The obtained amide wax was put into a grinder and pulverized to an average particle diameter of 20 μm or less. Next, 20% by mass of this amide wax, 40% by mass of Fine Crystal KE-604 (produced by Arakawa Chemical Technology Co., Ltd.), which is a rosin-based resin, and 40% by mass of hexyldiglycol were mixed, and heated to 90 to 110°C. It was heated and dispersed for 1 to 2 hours and then cooled. As a result, the thixotropic agent of Preparation Example 2 was obtained.
(조제예 3) 아마이드 왁스와 수지와 분산매체를 함유한 요변성제의 조제(Preparation Example 3) Preparation of a thixotropic agent containing amide wax, resin, and dispersion medium
조제예 1의 헥사메틸렌다이아민 대신에, (c) 1, 12-도데칸다이아민 1345.7질량부를 이용한 것 이외에는, 조제예 1과 마찬가지로 해서, 산가 4.2, 아민가 3.6의 아마이드 왁스를 얻었다(몰비로 (a):(b):(c)=2몰:2.7몰:3.3몰). 얻어진 아마이드 왁스를, 분쇄기에 투입해서 평균 입자 직경 20㎛ 이하로 분쇄하였다. 그 다음에, 이 아마이드 왁스의 20질량%, 로진계 수지인 파인 크리스탈 KR-85(아라카와카가쿠쿄고 주식회사 제품, 분자량 300)의 40질량%, 및 다이에틸렌글리콜모노부틸에터아세테이트의 40질량%를 혼합하고, 90 내지 110℃로 가열하면서 1 내지 2시간 가열 분산시키고, 그 후 냉각시켰다. 그것에 의해 조제예 3의 요변성제를 얻었다.In the same manner as Preparation Example 1, except that 1345.7 parts by mass of (c) 1,12-dodecanediamine was used instead of the hexamethylenediamine in Preparation Example 1, an amide wax with an acid value of 4.2 and an amine value of 3.6 was obtained (in molar ratio (a) ):(b):(c)=2 moles:2.7 moles:3.3 moles). The obtained amide wax was put into a grinder and pulverized to an average particle diameter of 20 μm or less. Next, 20% by mass of this amide wax, 40% by mass of Fine Crystal KR-85 (produced by Arakawa Chemical Co., Ltd., molecular weight 300), which is a rosin-based resin, and 40% by mass of diethylene glycol monobutyl ether acetate. were mixed, heated and dispersed at 90 to 110°C for 1 to 2 hours, and then cooled. As a result, the thixotropic agent of Preparation Example 3 was obtained.
(조제예 4) 아마이드 왁스와 수지와 분산매체를 함유한 요변성제의 조제(Preparation Example 4) Preparation of thixotropic agent containing amide wax, resin and dispersion medium
교반기, 온도계, 분수기를 구비한 반응 장치에, (a) 지방족 모노카복실산인 스테아르산 568.0질량부와, (b) 지방족 다이카복실산인 아디프산 438.0질량부를 첨가하고, 80 내지 100℃로 가온시켜 스테아르산을 용융시켰다. 거기에, (c) 다이아민인 헥사메틸렌다이아민 464.0질량부를 첨가하고, 질소분위기 하, 240 내지 280℃에서 3 내지 5시간, 탈수시키면서 축합반응을 행하여 아마이드화시켜, 산가 8.8, 아민가 7.8의 아마이드 왁스를 얻었다(몰비로 (a):(b):(c)=2몰:2.7몰:3.3몰).To a reaction apparatus equipped with a stirrer, thermometer, and fountain, (a) 568.0 parts by mass of stearic acid, which is an aliphatic monocarboxylic acid, and (b) 438.0 parts by mass of adipic acid, which is an aliphatic dicarboxylic acid, are added, and heated to 80 to 100° C. to dissolve stear. The acid was melted. There, (c) 464.0 parts by mass of hexamethylenediamine, which is a diamine, was added, and a condensation reaction was performed under a nitrogen atmosphere at 240 to 280° C. for 3 to 5 hours while dehydrating to amidize, resulting in an amide wax with an acid value of 8.8 and an amine value of 7.8. was obtained (molar ratio (a):(b):(c)=2 mole:2.7 mole:3.3 mole).
얻어진 아마이드 왁스를, 분쇄기에 투입해서 평균 입자 직경 20㎛ 이하로 분쇄하였다. 그 다음에, 이 아마이드 왁스의 20질량%, 로진계 수지인 파인 크리스탈(crystal)KR-85(아라카와카가쿠쿄고 주식회사 제품) 40질량% 및 다이에틸렌글리콜모노부틸에터아세테이트 40질량%를 혼합하고, 90 내지 110℃로 가열하면서 1 내지 2시간 가열 분산시키고, 그 후 냉각시켰다. 그것에 의해 조제예 4의 요변성제를 얻었다.The obtained amide wax was put into a grinder and pulverized to an average particle diameter of 20 μm or less. Next, 20% by mass of this amide wax, 40% by mass of rosin-based resin Fine Crystal KR-85 (manufactured by Arakawa Chemical Co., Ltd.), and 40% by mass of diethylene glycol monobutyl ether acetate were mixed. , heat-dispersed for 1 to 2 hours while heating to 90 to 110°C, and then cooled. As a result, the thixotropic agent of Preparation Example 4 was obtained.
(비교조제예 1) 아마이드 왁스만으로 이루어진 요변성제의 조제(Comparative Preparation Example 1) Preparation of a thixotropic agent consisting only of amide wax
교반기, 온도계, 분수기를 구비한 반응 장치에, 하이드록시기 함유 지방족 모노카복실산인 12-하이드록시스테아르산 1000.0질량부와, 지방족 다이카복실산인 세바스산 1010.0질량부를 첨가하고, 80 내지 100℃로 가온시켜 12-하이드록시스테아르산을 용해시켰다. 거기에, 다이아민인 헥사메틸렌다이아민 780.5질량부를 첨가하고, 질소분위기 하, 210 내지 220℃에서 3 내지 5시간, 탈수시키면서 축합반응을 행하여 아마이드화시켜, 산가 3.6, 아민가 2.8의 아마이드 왁스를 얻었다. 얻어진 아마이드 왁스를, 분쇄기에 투입해서 평균 입자 직경 20㎛ 이하로 분쇄시켜, 아마이드 왁스만으로 이루어진 비교 조제예 1의 요변성제를 얻었다.1000.0 parts by mass of 12-hydroxystearic acid, an aliphatic monocarboxylic acid containing a hydroxyl group, and 1010.0 parts by mass of sebacic acid, an aliphatic dicarboxylic acid, were added to a reaction apparatus equipped with a stirrer, thermometer, and fountain, and heated to 80 to 100°C. 12-Hydroxystearic acid was dissolved. 780.5 parts by mass of hexamethylenediamine, a diamine, was added thereto, and a condensation reaction was carried out while dehydrating in a nitrogen atmosphere at 210 to 220° C. for 3 to 5 hours to carry out amidation, thereby obtaining an amide wax with an acid value of 3.6 and an amine value of 2.8. The obtained amide wax was put into a grinder and pulverized to an average particle diameter of 20 μm or less to obtain the thixotropic agent of Comparative Preparation Example 1 consisting only of amide wax.
(비교조제예 2) 아마이드 왁스만으로 이루어진 요변성제의 조제(Comparative Preparation Example 2) Preparation of a thixotropic agent consisting only of amide wax
조제예 1의 헥사메틸렌다이아민 대신에 메타자일렌다이아민 915.1질량부를 이용한 것 이외에는, 실시예 1과 마찬가지로 해서, 산가 4.8, 아민가 4.4의 아마이드 왁스를 얻었다. 얻어진 아마이드 왁스를, 분쇄기에 투입해서 평균 입자 직경 20㎛ 이하로 분쇄시켜, 아마이드 왁스만으로 이루어진 비교조제예 2의 요변성제를 얻었다.An amide wax with an acid value of 4.8 and an amine value of 4.4 was obtained in the same manner as in Example 1, except that 915.1 parts by mass of metaxylenediamine was used instead of the hexamethylenediamine in Preparation Example 1. The obtained amide wax was placed in a grinder and pulverized to an average particle diameter of 20 μm or less to obtain a thixotropic agent of Comparative Preparation Example 2 consisting only of amide wax.
(비교조제예 3) 아마이드 왁스만으로 이루어진 요변성제의 조제(Comparative Preparation Example 3) Preparation of a thixotropic agent consisting only of amide wax
조제예 1의 헥사메틸렌다이아민 대신에 1, 12-도데칸다이아민 1345.7질량부를 이용한 것 이외에는, 조제예 1과 마찬가지로 해서, 산가 4.6, 아민가 4.1의 아마이드 왁스를 얻었다. 얻어진 아마이드 왁스를, 분쇄기에 투입해서 평균 입자 직경 20㎛ 이하로 분쇄시켜, 아마이드 왁스만으로 이루어진 비교조제예 3의 요변성제를 얻었다.An amide wax with an acid value of 4.6 and an amine value of 4.1 was obtained in the same manner as in Preparation Example 1, except that 1345.7 parts by mass of 1,12-dodecanediamine was used instead of the hexamethylenediamine in Preparation Example 1. The obtained amide wax was put into a grinder and pulverized to an average particle diameter of 20 μm or less to obtain a thixotropic agent of Comparative Preparation Example 3 consisting only of amide wax.
(비교조제예 4) 아마이드 왁스만으로 이루어진 요변성제의 조제(Comparative Preparation Example 4) Preparation of a thixotropic agent consisting only of amide wax
교반기, 온도계, 분수기를 구비한 반응 장치에, 지방족 모노카복실산인 스테아르산 568.0질량부와, 지방족 다이카복실산인 아디프산 438.0질량부를 가하고, 80 내지 100℃로 가온시켜 스테아르산을 용융시켰다. 거기에, 다이아민인 헥사메틸렌다이아민 464.0질량부를 첨가하고, 질소분위기 하, 240 내지 280℃에서 3 내지 5시간, 탈수시키면서 축합반응을 행하여 아마이드화시켜, 산가 8.2, 아민가 7.4의 아마이드 왁스를 얻었다. 얻어진 아마이드 왁스를, 분쇄기에 투입해서 평균 입자 직경 20㎛ 이하로 분쇄시켜, 아마이드 왁스만으로 이루어진 비교조제예 4의 요변성제를 얻었다.568.0 parts by mass of stearic acid, an aliphatic monocarboxylic acid, and 438.0 parts by mass of adipic acid, an aliphatic dicarboxylic acid, were added to a reaction apparatus equipped with a stirrer, thermometer, and fountain, and the mixture was heated to 80 to 100°C to melt the stearic acid. 464.0 parts by mass of hexamethylenediamine, a diamine, was added thereto, and a condensation reaction was performed under a nitrogen atmosphere at 240 to 280° C. for 3 to 5 hours while dehydrating to amidize the wax, thereby obtaining an amide wax with an acid value of 8.2 and an amine value of 7.4. The obtained amide wax was put into a grinder and pulverized to an average particle diameter of 20 μm or less to obtain a thixotropic agent of Comparative Preparation Example 4 consisting only of amide wax.
(비교조제예 5) 아마이드 왁스와 고분자량 아크릴수지와 저비점 분산매체를 함유한 요변성제의 조제(Comparative Preparation Example 5) Preparation of a thixotropic agent containing amide wax, high molecular weight acrylic resin, and low boiling point dispersion medium.
조제예 1과 마찬가지로 해서, 산가 3.6, 아민가 2.6의 아마이드 왁스를 얻었다. 얻어진 아마이드 왁스를, 분쇄기에 투입해서 평균 입자 직경 20㎛ 이하로 분쇄하였다. 그 다음에, 이 아마이드 왁스의 20질량%, 고분자량의 아크릴수지로서 DEGALAN LP 63/11(Evonik Industries사 제품, 분자량 30000) 40질량%, 저비점의 분산매체인 메틸아이소부틸케톤(비점 117℃) 40질량%를 혼합하고, 90 내지 110℃로 가열하면서 1 내지 2시간 가열 분산시키고, 그 후 냉각시킴으로써 비교조제예 5의 요변성제를 얻었다.In the same manner as Preparation Example 1, amide wax with an acid value of 3.6 and an amine value of 2.6 was obtained. The obtained amide wax was put into a grinder and pulverized to an average particle diameter of 20 μm or less. Next, 20% by mass of this amide wax, 40% by mass of DEGALAN LP 63/11 (manufactured by Evonik Industries, molecular weight 30000) as a high molecular weight acrylic resin, and methyl isobutyl ketone (boiling point 117°C) as a low boiling point dispersion medium. The thixotropic agent of Comparative Preparation Example 5 was obtained by mixing 40% by mass, dispersing by heating at 90 to 110°C for 1 to 2 hours, and then cooling.
(플럭스의 조제)(Preparation of flux)
플럭스 수지, 활성제, 용제 그리고 조제예 1 내지 4 및 비교조제예 1 내지 5에서 얻어진 요변성제를 표 1의 비율로 배합해서 혼합하고, 80 내지 120℃에서 1 내지 3시간, 가열 용융시켰다. 그 후 취출해서 방치함으로써 상온(25℃)으로 냉각시켜, 실시예 1 내지 4 및 비교예 1 내지 5의 플럭스를 얻었다.The flux resin, activator, solvent, and thixotropic agent obtained in Preparation Examples 1 to 4 and Comparative Preparation Examples 1 to 5 were mixed in the ratios shown in Table 1 and heated and melted at 80 to 120°C for 1 to 3 hours. After that, it was taken out and left to cool to room temperature (25°C) to obtain fluxes of Examples 1 to 4 and Comparative Examples 1 to 5.
(분산성 평가)(Dispersibility evaluation)
실시예 1 내지 4 및 비교예 1 내지 5의 플럭스에 포함되는 아마이드 왁스의 분산성을 육안으로 확인하였다. 조제한 플럭스를 유리판에 도포하고, 덩어리가 확인되지 않은 것을 ○, 덩어리가 확인된 것을 ×로 하였다.The dispersibility of the amide wax included in the fluxes of Examples 1 to 4 and Comparative Examples 1 to 5 was visually confirmed. The prepared flux was applied to a glass plate, and those in which no lumps were observed were marked as ○, and those in which lumps were found were marked as ×.
(색감 평가)(Color evaluation)
실시예 1 내지 4 및 비교예 1 내지 5의 플럭스의 색감을 육안으로 확인하였다. 플럭스 중의 수지 성분의 열 손상을 나타내는 판단으로서, 무색 내지 담황색인 것을 ○, 황색 내지 갈색인 것을 ×로 하였다.The color of the fluxes of Examples 1 to 4 and Comparative Examples 1 to 5 was confirmed with the naked eye. As a judgment indicating the heat damage of the resin component in the flux, colorless to light yellow was assigned ○, and yellow to brown was assigned ○.
분산성 평가, 색감 평가의 결과를 표 2에 나타낸다.The results of the dispersibility evaluation and color evaluation are shown in Table 2.
표 2로부터 명확한 바와 같이, 본 발명을 적용하는 조제예 1 내지 4의 요변성제를 포함하는 실시예 1 내지 4의 플럭스는, 본 발명의 적용 외의 비교조제예 1 내지 4의 아마이드 왁스만으로 이루어진 요변성제를 포함하는 비교예 1 내지 4의 플럭스에 비교해서, 아마이드 왁스의 덩어리가 확인되지 않은 점으로부터, 분산성이 우수하였다. 또한, 플럭스의 착색이 거의 보이지 않았다. 비교조제예 5의 요변성제가, 고분자량의 수지 및 저비점의 분산매체를 포함하고 있기 때문에, 비교예 5의 플럭스는, 분산성이 낮고, 착색되어 있는 것이 확인되었다.As is clear from Table 2, the fluxes of Examples 1 to 4 containing the thixotropic agent of Preparation Examples 1 to 4 in which the present invention is applied are the thixotropic agent consisting only of amide wax in Comparative Preparation Examples 1 to 4 other than the application of the present invention. Compared to the fluxes of Comparative Examples 1 to 4 containing, the dispersibility was excellent in that no lumps of amide wax were observed. Additionally, almost no coloring of the flux was observed. Since the thixotropic agent of Comparative Preparation Example 5 contained a high molecular weight resin and a low boiling point dispersion medium, it was confirmed that the flux of Comparative Example 5 had low dispersibility and was colored.
상기 실시예에 따르면, 본 발명의 요변성제는 아마이드 왁스의 분산성을 높일 수 있으므로, 이 요변성제를 가해서 플럭스를 조제할 때, 가열 처리 시간을 극히 단축시킬 수 있고, 플럭스의 착색을 일으키지 않는다는 것이 나타났다.According to the above examples, the thixotropic agent of the present invention can increase the dispersibility of amide wax, so when preparing flux by adding this thixotropic agent, the heat treatment time can be extremely shortened and coloring of the flux is not caused. appear.
(솔더 페이스트의 조제)(Preparation of solder paste)
실시예 1의 플럭스의 11질량%와, 무연 땜납 합금 분말(Sn 96.5% - Ag 3.0% - Cu 0.5%; 미츠이킨조쿠코교(三井金屬鑛業) 주식회사 제품)의 89 질량%를, 페이스트 혼련기(솔더소프너)에서 혼련시키고, 솔더 페이스트를 조제하였다. 이것과 마찬가지로 해서, 실시예 2 내지 4의 플럭스를 포함하는 솔더 페이스트를 조제하였다. 이 솔더 페이스트를 납땜에 이용하였다.11 mass% of the flux of Example 1 and 89 mass% of lead-free solder alloy powder (Sn 96.5% - Ag 3.0% - Cu 0.5%; manufactured by Mitsui Kinzoku Kogyo Co., Ltd.) were mixed in a paste kneader ( It was kneaded in a solder softener and a solder paste was prepared. In the same manner, solder pastes containing the fluxes of Examples 2 to 4 were prepared. This solder paste was used for soldering.
본 발명의 요변성제는, 아마이드 왁스의 분산성이 우수하므로, 요변성제 첨가 시의 가열 처리 시간을 짧게 할 수 있고, 플럭스, 솔더 페이스트 및 실 땜납의 조제나 사용에 적합하다.Since the thixotropic agent of the present invention has excellent amide wax dispersibility, the heat treatment time when adding the thixotropic agent can be shortened, and it is suitable for the preparation and use of flux, solder paste, and thread solder.
본 발명의 플럭스는, 땜납 분말과 혼합함으로써, 솔더 페이스트를 조제하는데 이용될 수 있다.The flux of the present invention can be used to prepare solder paste by mixing it with solder powder.
본 발명의 솔더 페이스트는, 특히 플로우 방식에 의한 납땜에 적합하게 이용될 수 있다.The solder paste of the present invention can be particularly suitably used for soldering by the flow method.
본 발명의 요변성제의 제조 방법은, 플럭스나 솔더 페이스트에 첨가하는 요변성제를 제조하는데 이용될 수 있다.The method for producing a thixotropic agent of the present invention can be used to produce a thixotropic agent added to flux or solder paste.
Claims (6)
포화 지방족 모노카복실산류, 하이드록시기 함유 지방족 모노카복실산류 및 다염기산류 중 적어도 어느 1종의 산류와, 다이아민류 및 테트라아민류 중 적어도 어느 1종의 아민류의 축합물이고, 분체 형태로 된 아마이드 왁스의 분쇄물과,
분자량이 최대 10000인 수지와,
비점이 적어도 180℃인 분산매체가,
혼합되어서 포함되어 있고,
상기 아마이드 왁스의 분쇄물이 상기 수지로 피복되어 있고, 상기 수지 및 상기 분산매체에 분산되어 있는 것을 특징으로 하는 플럭스용 요변성제.As a thixotropic agent for flux,
It is a condensate of at least one type of acid from saturated aliphatic monocarboxylic acids, hydroxyl group-containing aliphatic monocarboxylic acids, and polybasic acids, and at least one type of amine from diamines and tetraamines, and is an amide wax in powder form. pulverized material,
A resin with a molecular weight of up to 10000,
A dispersion medium with a boiling point of at least 180°C,
It is mixed and included,
A thixotropic agent for flux, characterized in that a pulverized product of the amide wax is coated with the resin and dispersed in the resin and the dispersion medium.
상기 아마이드 왁스의 분쇄물이, 탄소수 12 내지 22의 상기 포화 지방족 모노카복실산류 및/또는 탄소수 12 내지 22의 상기 하이드록시기 함유 지방족 모노카복실산류를 몰비로 합계 a몰(1≤a≤3)과, 탄소수 2 내지 12의 상기 다염기산류를 몰비로 b몰 (0 <b≤5)과, 탄소수 2 내지 14의 상기 다이아민류 및/또는 탄소수 2 내지 14의 상기 테트라아민류를 몰비로 합계 c몰(1≤c≤6)로 하는 상기 축합물이며,
1 내지 40질량%의 상기 아마이드 왁스와, 20 내지 60질량%의 상기 수지와, 20 내지 60질량%의 상기 분산매체가 포함되어 있는 것을 특징으로 하는 플럭스용 요변성제.According to paragraph 1,
The pulverized product of the amide wax contains a total of a mole (1≤a≤3) of the saturated aliphatic monocarboxylic acids having 12 to 22 carbon atoms and/or the hydroxy group-containing aliphatic monocarboxylic acids having 12 to 22 carbon atoms in a molar ratio. , a total of b moles (0 <b≤5) of the polybasic acids having 2 to 12 carbon atoms in a molar ratio and c moles of the diamines having 2 to 14 carbon atoms and/or the tetraamines having 2 to 14 carbon atoms in a molar ratio (1 ≤c≤6), which is the above condensate,
A thixotropic agent for flux, comprising 1 to 40% by mass of the amide wax, 20 to 60% by mass of the resin, and 20 to 60% by mass of the dispersion medium.
포화 지방족 모노카복실산류, 하이드록시기 함유 지방족 모노카복실산류 및 다염기산류 중 적어도 어느 1종의 산류와, 다이아민류 및 테트라아민류 중 적어도 어느 1종의 아민류를 축합시켜서 아마이드 왁스를 합성하는 공정과,
상기 아마이드 왁스를 분체 형태가 되도록 분쇄하여 분쇄물로 하는 공정과,
상기 아마이드 왁스, 분자량이 최대 10000인 수지 및 비점이 적어도 180℃인 분산매체를 혼합하여 상기 아마이드 왁스의 상기 분쇄물을 상기 수지로 피복하면서 상기 수지 및 상기 분산매체에 분산시키는 공정을 포함하는 것을 특징으로 하는 플럭스용 요변성제의 제조 방법.A method for producing a thixotropic agent for flux, comprising:
A process for synthesizing amide wax by condensing at least one acid selected from saturated aliphatic monocarboxylic acids, hydroxyl group-containing aliphatic monocarboxylic acids, and polybasic acids, and at least one type of amine selected from diamines and tetraamines;
A process of pulverizing the amide wax into powder form to obtain pulverized product;
A process of mixing the amide wax, a resin having a molecular weight of up to 10000, and a dispersion medium having a boiling point of at least 180° C. and dispersing the pulverized amide wax in the resin and the dispersion medium while coating the pulverized amide wax with the resin. A method for producing a thixotropic agent for flux.
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| KR20210031870A (en) * | 2018-08-10 | 2021-03-23 | 가부시키가이샤 코키 | Flux and solder paste |
| JP7097611B2 (en) * | 2018-09-04 | 2022-07-08 | 株式会社弘輝 | Flux and solder materials |
| JP2020116611A (en) * | 2019-01-24 | 2020-08-06 | 株式会社弘輝 | Flux and solder paste |
| JP6777872B1 (en) * | 2019-05-27 | 2020-10-28 | 千住金属工業株式会社 | Flux and solder paste |
| CN116529021B (en) * | 2020-11-18 | 2024-03-08 | 千住金属工业株式会社 | Soldering flux and soldering paste |
| JP6947998B1 (en) * | 2020-11-18 | 2021-10-13 | 千住金属工業株式会社 | Flux and solder paste |
| CN114453795B (en) * | 2021-12-10 | 2023-09-29 | 江苏广昇新材料有限公司 | Halogen-free soldering flux for lead-free solder paste |
| JP7236022B1 (en) * | 2022-07-25 | 2023-03-09 | 千住金属工業株式会社 | Method for manufacturing flux, solder paste and bonded body |
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- 2016-10-06 WO PCT/JP2016/079746 patent/WO2017065076A1/en active Application Filing
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005144520A (en) * | 2003-11-18 | 2005-06-09 | Ito Seiyu Kk | Thixotropy application agent for solder paste, and solder paste |
| JP2012086269A (en) | 2010-09-24 | 2012-05-10 | Arakawa Chem Ind Co Ltd | Rosin-based flux for soldering and solder paste |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20230078829A (en) * | 2020-11-18 | 2023-06-02 | 센주긴조쿠고교 가부시키가이샤 | Flux and Solder Paste |
| KR102645403B1 (en) | 2020-11-18 | 2024-03-11 | 센주긴조쿠고교 가부시키가이샤 | flux and solder paste |
Also Published As
| Publication number | Publication date |
|---|---|
| KR20180068972A (en) | 2018-06-22 |
| JP6801879B2 (en) | 2020-12-16 |
| JPWO2017065076A1 (en) | 2018-08-09 |
| CN108136549B (en) | 2021-03-23 |
| WO2017065076A1 (en) | 2017-04-20 |
| CN108136549A (en) | 2018-06-08 |
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