WO2016125901A1 - フラックス用活性剤、フラックス及びはんだ - Google Patents
フラックス用活性剤、フラックス及びはんだ Download PDFInfo
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- WO2016125901A1 WO2016125901A1 PCT/JP2016/053540 JP2016053540W WO2016125901A1 WO 2016125901 A1 WO2016125901 A1 WO 2016125901A1 JP 2016053540 W JP2016053540 W JP 2016053540W WO 2016125901 A1 WO2016125901 A1 WO 2016125901A1
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- group
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- 0 *CC(Br)=C(C*)I Chemical compound *CC(Br)=C(C*)I 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/22—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by the composition or nature of the material
- B23K35/36—Selection of non-metallic compositions, e.g. coatings, fluxes; Selection of soldering or welding materials, conjoint with selection of non-metallic compositions, both selections being of interest
- B23K35/3612—Selection of non-metallic compositions, e.g. coatings, fluxes; Selection of soldering or welding materials, conjoint with selection of non-metallic compositions, both selections being of interest with organic compounds as principal constituents
- B23K35/3616—Halogen compounds
-
- 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
- B23K35/3601—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 inorganic compounds as principal constituents
- B23K35/3603—Halide salts
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/22—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by the composition or nature of the material
- B23K35/24—Selection of soldering or welding materials proper
-
- 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
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C271/00—Derivatives of carbamic acids, i.e. compounds containing any of the groups, the nitrogen atom not being part of nitro or nitroso groups
- C07C271/06—Esters of carbamic acids
- C07C271/08—Esters of carbamic acids having oxygen atoms of carbamate groups bound to acyclic carbon atoms
- C07C271/10—Esters of carbamic acids having oxygen atoms of carbamate groups bound to acyclic carbon atoms with the nitrogen atoms of the carbamate groups bound to hydrogen atoms or to acyclic carbon atoms
- C07C271/16—Esters of carbamic acids having oxygen atoms of carbamate groups bound to acyclic carbon atoms with the nitrogen atoms of the carbamate groups bound to hydrogen atoms or to acyclic carbon atoms to carbon atoms of hydrocarbon radicals substituted by singly-bound oxygen atoms
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C271/00—Derivatives of carbamic acids, i.e. compounds containing any of the groups, the nitrogen atom not being part of nitro or nitroso groups
- C07C271/06—Esters of carbamic acids
- C07C271/08—Esters of carbamic acids having oxygen atoms of carbamate groups bound to acyclic carbon atoms
- C07C271/26—Esters of carbamic acids having oxygen atoms of carbamate groups bound to acyclic carbon atoms with the nitrogen atom of at least one of the carbamate groups bound to a carbon atom of a six-membered aromatic ring
- C07C271/28—Esters of carbamic acids having oxygen atoms of carbamate groups bound to acyclic carbon atoms with the nitrogen atom of at least one of the carbamate groups bound to a carbon atom of a six-membered aromatic ring to a carbon atom of a non-condensed six-membered aromatic ring
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C33/00—Unsaturated compounds having hydroxy or O-metal groups bound to acyclic carbon atoms
- C07C33/40—Halogenated unsaturated alcohols
- C07C33/42—Halogenated unsaturated alcohols acyclic
- C07C33/423—Halogenated unsaturated alcohols acyclic containing only double bonds as unsaturation
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C43/00—Ethers; Compounds having groups, groups or groups
- C07C43/02—Ethers
- C07C43/03—Ethers having all ether-oxygen atoms bound to acyclic carbon atoms
- C07C43/14—Unsaturated ethers
- C07C43/17—Unsaturated ethers containing halogen
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C43/00—Ethers; Compounds having groups, groups or groups
- C07C43/02—Ethers
- C07C43/03—Ethers having all ether-oxygen atoms bound to acyclic carbon atoms
- C07C43/14—Unsaturated ethers
- C07C43/17—Unsaturated ethers containing halogen
- C07C43/174—Unsaturated ethers containing halogen containing six-membered aromatic rings
- C07C43/176—Unsaturated ethers containing halogen containing six-membered aromatic rings having unsaturation outside the aromatic rings
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C69/00—Esters of carboxylic acids; Esters of carbonic or haloformic acids
- C07C69/62—Halogen-containing esters
- C07C69/63—Halogen-containing esters of saturated acids
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C69/00—Esters of carboxylic acids; Esters of carbonic or haloformic acids
- C07C69/76—Esters of carboxylic acids having a carboxyl group bound to a carbon atom of a six-membered aromatic ring
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/22—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by the composition or nature of the material
- B23K35/24—Selection of soldering or welding materials proper
- B23K35/26—Selection of soldering or welding materials proper with the principal constituent melting at less than 400 degrees C
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/22—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by the composition or nature of the material
- B23K35/24—Selection of soldering or welding materials proper
- B23K35/26—Selection of soldering or welding materials proper with the principal constituent melting at less than 400 degrees C
- B23K35/262—Sn as the principal constituent
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C13/00—Alloys based on tin
Definitions
- the present invention relates to a flux activator, a flux containing the same, and a solder.
- Solder used for joining electronic parts usually includes a solder alloy and a flux.
- the flux includes a resin component composed of a modified rosin, a synthetic resin, and the like, an activator, and, if necessary, a solvent component and other additives.
- an activator a halogen activator containing an organic halogen compound is known.
- Patent Document 1 describes a flux containing, as an activator, a halogen compound in which a halogen atom such as bromine or chlorine is introduced into an organic compound by a covalent bond.
- Patent Document 2 describes a flux containing an iodine carboxyl compound as an activator. It is known that these halogen compounds can improve the wettability of the solder by removing the oxide film on the solder surface or preventing re-oxidation and further reducing the surface tension of the solder.
- fluxes containing these halogen compound activators do not exhibit the above effects immediately after soldering, and it is also difficult to maintain the effect, so that the wettability of solder is sufficiently improved in the normal soldering process. There is a problem that it is difficult to do.
- the present invention has been made in view of the problems of the prior art as described above, and can improve the wettability of solder immediately after soldering, and can continuously improve the wettability of solder. It is an object of the present invention to provide a flux activator, a flux and a solder.
- the activator for flux of the present invention is represented by the following general formula 1 (wherein X 1 and X 2 are different halogen atoms, and R 1 and R 2 are respectively represented by the general formulas —OH, —O—R 3 , —O It is a group represented by either —C ( ⁇ O) —R 4 or —O—C ( ⁇ O) —NH—R 5 , and R 1 and R 2 are the same or different.
- R 3 , R 4 , and R 5 are each an aromatic hydrocarbon group having 1 to 18 carbon atoms or an aliphatic hydrocarbon group having 1 to 18 carbon atoms, and R 3 , R 4 and R 5 may be the same group or different groups.).
- X 1 may be Br or I
- X 2 may be Br or I
- the present invention concerning flux contains the activator for flux.
- the present invention concerning solder contains the flux.
- the wettability of solder can be improved immediately after soldering, and the wettability of solder can be continuously improved.
- the flux activator of the present embodiment (hereinafter also simply referred to as activator) includes a halogen compound represented by the following general formula 1.
- X 1 and X 2 are halogen atoms such as Br, I, Cl, F, and At, and are not particularly limited as long as they are different from each other, but are Cl, Br, and I. preferable.
- X 1 and X 2 are each preferably Br or I. That is, when X 1 is Br, X 2 is preferably I, and when X 1 is I, X 2 is preferably Br.
- a halogen compound represented by the following general formula (2) or (3) is preferable.
- R 1 and R 2 are each a general formula —OH, —O—R 3 , —O—C ( ⁇ O) —R 4 , or —O —C ( ⁇ O) —NH—R 5 is a group represented by any one, and R 1 and R 2 may be the same group or different groups.
- R 3 , R 4 and R 5 may be the same group or different groups, each of which is an aromatic hydrocarbon group having 1 to 18 carbon atoms, or an aliphatic hydrocarbon group having 1 to 18 carbon atoms. Group hydrocarbon group.
- R 3 , R 4 and R 5 are each, for example, a methyl group having 1 to 6 carbon atoms, an ethyl group or a propyl group; a linear or molecular chain alkyl group having 18 carbon atoms; an alkenyl having 2 to 6 carbon atoms A cyclohexyl group, a phenyl group, a cyclohexyl group, a phenyl group, or the like into which a substituent such as a methyl group, a hydroxy group, a methoxy group, a carboxyl group, an amino group, or a cyano group has been introduced.
- the oxide film on the solder surface can be removed or the formation of the oxide film can be suppressed by the action of the halogen atom, and the surface tension of the solder can be reduced. Therefore, the solder wettability can be improved.
- the effect of the halogen atom is different in the strength of the effect that can be exhibited for each halogen atom, the time until the effect, the sustainability of the effect, and the like.
- Br bromine
- Br can exert the above effect relatively immediately after soldering, but its heat resistance is low, so the effect is reduced by heating during soldering, and the wettability is continuously improved. It may not be effective.
- I iodine
- I (iodine) has relatively high heat resistance and has a long-lasting effect, but it takes time to remove the oxide film. Therefore, for example, in the process of soldering in a short time, there are cases where wettability cannot be improved.
- the activator of the present embodiment contains a halogen compound into which different halogen atoms are introduced, so that the effect of improving wettability can be exhibited immediately after soldering and can be exhibited continuously.
- R 1 and R 2 in the above general formulas (1) to (3) are respectively the general formulas —OH, —O—R 3 , —O—C ( ⁇ O) —R 4 , Or, it is a group represented by any of —O—C ( ⁇ O) —NH—R 5 .
- R 1 and R 2 may be the same group or different groups, but are preferably the same group.
- Examples of the halogen compound in which R 1 and R 2 are the same group represented by —OH include a halogen compound represented by the following formula (4).
- R 3 , R 4 and R 5 in the general formulas (1) to (3) are each an aromatic hydrocarbon group having 1 to 18 carbon atoms as described above, or An aliphatic hydrocarbon group having 1 to 18 carbon atoms.
- R 3, R 4, R 5 is preferably a phenyl group.
- halogen compound in which R 1 and R 2 are the same group represented by —O—R 3 and each R 3 is a phenyl group include, for example, the following general formula (5) And halogen compounds.
- each of R 6 and R 7 may be a hydrogen atom, a methyl group, a hydroxy group, a methoxy group, a carboxyl group, an amino group, or a cyano group. Each is a hydrogen atom or a methyl group.
- R 6 and R 7 may be the same group or different groups, but are preferably the same group.
- halogen compound in which R 1 and R 2 are the same group represented by —O—C ( ⁇ O) —R 4 and R 4 is a phenyl group include, for example, the following general formula ( And halogen compounds such as 6).
- R 8 and R 9 may each be a hydrogen atom, a methyl group, a hydroxy group, a methoxy group, a carboxyl group, an amino group, or a cyano group, A hydrogen atom and a methyl group.
- R 6 and R 7 may be the same group or different groups, but are preferably the same group.
- halogen compounds in which R 1 and R 2 are both the same group represented by —O—C ( ⁇ O) —NH—R 5 and each R 5 is a phenyl group include, for example, Halogen compounds such as the general formula (7) are exemplified.
- each of R 10 and R 11 may be a hydrogen atom, a methyl group, a hydroxy group, a methoxy group, a carboxyl group, an amino group, or a cyano group. Each is a hydrogen atom or a methyl group.
- R 10 and R 11 may be the same group or different groups, but are preferably the same group.
- both the R 1 and R 2 of the halogen compound represented by the general formula 3 are the general formula —O—R 3 and each R 3 phenyl
- a method for producing a diphenyl ether derivative (halogen compound represented by the following formula 8) as a group is exemplified.
- Infrared absorption spectrum (IR: apparatus name: Frontier GOLD spotlight 400, manufacturer: Perkin Elmer) by, check the peak derived from an ether bond to 1243cm -1, 3200 ⁇ broad from OH groups detected 2800cm around -1 It was confirmed that the diphenyl ether derivative represented by the above formula 8 was obtained by the disappearance of a simple peak.
- both of R 1 and R 2 of the halogen compound represented by the general formula 3 are the general formula —O—R 3 , and each R 3 is The manufacturing method of the distearyl ether derivative (halogen compound represented by following formula 9) which is a stearyl group is illustrated.
- R 1 and R 2 of the halogen compound represented by the above general formula 3 are both represented by the general formula —O—C ( ⁇ O) —R 4 using the halogen compound represented by the above general formula 4. Then, a method for producing a diphenyl ester derivative (halogen compound represented by the following formula 10) in which each R 4 is a phenyl group is exemplified.
- Infrared absorption spectrum (IR: apparatus name: Frontier GOLD spotlight 400, manufacturer: Perkin Elmer) by, check the peak derived from an ester bond in 1742 cm -1, 3200 ⁇ broad from OH groups detected 2800cm around -1 It was confirmed that it was a diphenyl ester derivative represented by the above formula 10 by the disappearance of a simple peak.
- both R 1 and R 2 of the halogen compound represented by the above formula 3 are the general formula —O—C ( ⁇ O) —R 4 .
- a method for producing a distearyl ester derivative (halogen compound represented by the following formula 11) in which each R 4 is a stearyl group is exemplified.
- both of R 1 and R 2 of the halogen compound represented by the above formula 3 are —O—C ( ⁇ O) —NH—R 5 .
- a method for producing a diphenylurethane derivative (halogen compound represented by Formula 12) in which each R 5 is a phenyl group is illustrated.
- IR infrared absorption spectrum
- isocyanates check the peak derived from the urethane bond to the peak and 1708 cm -1 derived from N-1-substituted amide N-H stretching vibration 3317cm -1, it appeared in the vicinity of 2275 ⁇ 2250 cm -1
- the origin peak disappeared, and the broad peak derived from the OH group detected in the vicinity of 3200 to 2800 cm ⁇ 1 disappeared, confirming the diphenylurethane derivative represented by the above formula 12.
- both of R 1 and R 2 of the halogen compound represented by the general formula 3 are —O—C ( ⁇ O) —NH—R 5.
- the use of the flux of this embodiment is not particularly limited, and can be used as, for example, solder paste, flux for solder such as cored solder, or post flux.
- the flux of this embodiment may use the said active agent 1 type or in mixture of 2 or more types.
- content in the flux of an activator is not specifically limited, For example, 0.1 to 10 mass%, Preferably 0.3 to 4 mass% etc. are mentioned.
- the content of the activator is, for example, 0.3% by mass or more and 4% by mass or less, preferably 1% by mass or more and 3% by mass or less. Etc.
- the content of the activator is within the above range, the solder wettability is easily improved immediately after soldering, and the solder wettability is easily improved continuously.
- the flux of the present embodiment may contain a known activator component as an auxiliary activator in addition to the activator of the present embodiment.
- a known activator component for example, an organic acid, an amine halogen salt or the like can be used.
- the organic acid include glutaric acid, adipic acid, azelaic acid, sebacic acid, stearic acid, benzoic acid, and the like.
- the amine halogen salt include diethylamine, dibutylamine, tributylamine, diphenylguanidine, cyclohexylamine, and the like.
- examples of halogen include fluorine, chlorine, bromine, iodine, and astatine. However, fluorine is undesirable because it is highly corrosive and may impair reliability. Astatine is classified as halogen, but it is not practical because it has a very short half-life and can only exist in a nuclear reactor.
- the flux of this embodiment may contain a resin component, a solvent component, and the like.
- the resin component is not particularly limited as long as it is a known resin component used as a flux resin component, such as a synthetic resin or a natural resin. Examples thereof include polymerized rosin, hydrogenated rosin, natural rosin, disproportionated rosin, and acid-modified rosin.
- the content of the resin component in the flux is not particularly limited, and examples thereof include 20% by mass to 99% by mass, preferably 30% by mass to 99% by mass.
- the content of the resin component is, for example, 40% by mass or more and 99% by mass or less, preferably 60% by mass or more and 99% by mass or less. There are some.
- the solvent component is not particularly limited as long as it is a known component used as a solvent component of the flux.
- glycol ethers such as diethylene glycol monohexyl ether (hexyl diglycol), diethylene glycol dibutyl ether (dibutyl diglycol), diethylene glycol mono 2-ethylhexyl ether (2 ethylhexyl diglycol), diethylene glycol monobutyl ether (butyl diglycol); n- Aliphatic compounds such as hexane, isohexane and n-heptane; esters such as isopropyl acetate, methyl propionate and ethyl propionate; ketones such as methyl ethyl ketone, methyl-n-propyl ketone and diethyl ketone; ethanol and n-propanol And alcohols such as isopropanol and isobutanol.
- the solvent can be used alone or
- the content of the solvent component in the flux is not particularly limited, and examples include 0 mass% to 60 mass%, preferably 0 mass% to 40 mass%. *
- the flux of this embodiment may further contain additives such as a thixotropic agent, an antioxidant, a surfactant, an antifoaming agent, and a corrosion inhibitor.
- additives such as a thixotropic agent, an antioxidant, a surfactant, an antifoaming agent, and a corrosion inhibitor.
- the solder containing the flux of this embodiment is demonstrated.
- the flux of this embodiment can be a solder composition such as a solder paste or a solder such as a cored solder.
- the solder paste as the solder composition is configured by mixing the solder alloy powder and the flux of the present embodiment.
- the solder alloy is not particularly limited, and may be either a lead-free solder alloy or a leaded solder alloy, but a lead-free solder alloy is preferred from the viewpoint of environmental impact.
- Specific examples of lead-free solder alloys include alloys containing tin, silver, copper, zinc, bismuth, antimony, and the like.
- the solder paste as the solder composition is preferably mixed, for example, in an amount of 80% to 95% by mass of the solder alloy powder and 5% to 20% by mass of the flux.
- the cored solder as solder is composed of a thin cylindrical solder alloy having a central portion filled with the flux of the present embodiment.
- the flux content in the flux cored solder is preferably 1% by mass or more and 5% by mass or less.
- the flux containing the activator of the present embodiment is particularly preferably used as a flux for cored solder. If the wet solder is deteriorated in the cored solder, defects such as poor fillet formation, bridging between terminals, and horn standing tend to occur.
- the cored solder containing the flux according to the present embodiment can suppress a decrease in wettability immediately after soldering and can continuously improve the wettability, and thus can effectively suppress the above-described defect due to the decrease in wettability.
- the solder wettability can be improved immediately after soldering, and the solder wettability can be continuously improved.
- X 1 in the general formula 1 is Br or I
- X 2 when X 2 is Br or I can improve the wettability of the solder, especially in a short time from the soldering, and the solder wetting Sex can be improved more sustainably.
- the above case means that X 2 is I when X 1 is Br, and X 2 is Br when X 1 is I.
- Activator 1 Halogen compound activator represented by Formula 4 above: Diphenyl ether derivative activator represented by Formula 8 above: Distearyl ether derivative activator represented by Formula 9 above: Formula 10 above Diphenyl ester derivative activator 5: distearyl ester derivative activator represented by formula 11 above: diphenyl urethane derivative activator represented by formula 12 above: distearyl urethane derivative activity represented by formula 13 above Agent 8: Halogen compound activator represented by the following formula 14: Halogen compound represented by the following formula 15
- Thread solder solder alloy: SAC305 (Sn 96.5% by mass, Ag 3.0% by mass, Cu 0.5% by mass)) length 7 mm, diameter 1 on a degreased and cleaned copper plate (3 mm ⁇ 3 mm ⁇ 0.5 mm thickness) 0.0 mm) in a ring shape having a diameter of 2.0 mm was placed, and a piece of each flux (about 10 mg) was placed on the ring-shaped thread solder to prepare a test piece. Each test piece was placed on a solder bath heated to 300 ° C., the thread solder was melted, and after 5 seconds from melting, the test piece was removed from the solder bath. Each test piece was washed with flux using isopropyl alcohol, and the height of the solder was measured with a micrometer (manufactured by Mitutoyo Corporation). The spread ratio was calculated from the height of the solder by the following formula.
- Examples 1 to 7 had higher wettability because of higher spread ratio and less repelling than Comparative Examples 1 and 2.
- Examples 2 to 7 have slightly lower spreading ratios, but this is because an activator into which a substituent having a large molecular weight is introduced is used, so that the halogen content decreases. It is thought that.
- soldering test method Next, a flux cored solder (Examples 8 to 14 and Comparative Examples 3 and 4) was prepared with the fluxes (Examples 1 to 7 and Comparative Examples 1 and 2) using the above activators 1 to 7, A soldering test was performed. The flux content in the flux cored solder was 3.2%, and the wire diameter was adjusted and manufactured to 0.5 mm ⁇ .
- the bridge is a defective phenomenon in which the removal of the surface oxide film of the solder is insufficient, the fluidity is lowered, and the solder is connected between adjacent pins. Each substrate is visually observed.
- the slide speed is high (10 mm / sec)
- the slide speed is high (10 mm / sec)
- B was evaluated without bridge
- C was evaluated with bridge at a normal slide speed (6 mm / sec). The results are shown in Table 3.
- Example 8 both the formation of fillets and the occurrence of bridges were evaluated as A, and it was clear that soldering can be performed extremely well.
Abstract
Description
例えば、特許文献1には、臭素、塩素などのハロゲン原子が共有結合によって有機化合物中に導入されているハロゲン化合物を活性剤として含むフラックスが記載されている。また、特許文献2には、ヨウ素系カルボキシル化合物を活性剤として含むフラックスが記載されている。
これらのハロゲン化合物は、はんだ表面の酸化膜を除去し、あるいは、再酸化を防止し、さらに、はんだの表面張力を低下させることで、はんだの濡れ性を向上させうることが知られている。
本実施形態のフラックス用活性剤(以下、単に活性剤とも言う。)は、下記一般式1で表されるハロゲン化合物を含む。
但し、下記一般式(2)及び(3)中、R1、R2は、それぞれが一般式-OH、-O-R3、-O-C(=O)-R4、又は、-O-C(=O)-NH-R5の何れかで表される基であり、R1、R2は同一の基であっても異なる基であってもよい。
また、R3、R4、R5は、同一の基であっても異なる基であってもよく、それぞれが炭素数1~18の芳香族炭化水素基、又は、炭素数1~18の脂肪族炭化水素基である。
R3、R4、R5は、それぞれが、例えば、炭素数1~6のメチル基、エチル基、プロピル基;炭素数18の直鎖または分子鎖状アルキル基;炭素数2~6のアルケニル基、シクロヘキシル基、フェニル基;メチル基、ヒドロキシ基、メトキシ基、カルボキシル基、アミノ基、シアノ基等の置換基が導入されたシクロヘキシル基、フェニル基等であってもよい。
前記X1、X2が、互いに異なるハロゲン原子であることによって、上述のような効果が得られるのは、以下のような理由によるためであると考えられる。
例えば、ハロゲン原子の中でもBr(臭素)は比較的はんだ付け直後から上記効果を発揮しうるが、耐熱性が低いため、はんだ付け時の加熱によって効果が低下していき、持続的に濡れ性向上効果が発揮できない場合がある。
これらの問題を解消するために、例えば、はんだ付け温度を上げてはんだ付けの時間を短くすることや、Brの含有量を増やすことが考えられる。しかし、はんだ付け温度を上げると、基板や電子部品への熱ダメージが大きくなり、また、フラックス残渣の焦げつきが生じるおそれがある。また、Brの含有量を増やすことはフラックス残渣の絶縁性が低下する原因になるおそれがある。
R1、R2は同一の基であっても異なる基であってもよいが、好ましくは同一の基である。
中でも、R3、R4、R5は、フェニル基であることが好ましい。
また、R6、R7は同一の基であっても異なる基であってもよいが、好ましくは同一の基である。
また、R6、R7は同一の基であっても異なる基であってもよいが、好ましくは同一の基である。
また、R10、R11は同一の基であっても異なる基であってもよいが、好ましくは同一の基である。
温度計、スターラーピースを備えた反応容器へ、トルエン50g、酸化銀(I)8.7g、ベンジルブロミド6.1g、上記式4で表されるハロゲン化合物を5.0g加えた。その後、内温40℃で24時間反応させた。
ガスクロマトグラフ(GC:装置名GC-2010、製造元:島津製作所)で原料である上記ハロゲン化合物(式4)のピークが消失していることを確認後、メタノール10g添加し、3hr撹拌した。その後、エバポレーターにより溶媒を留去した。酢酸エチル40gを添加後、2hr撹拌し、析出している黒色固体をろ別した。再度エバポレーターにより溶媒を除去後、IPA50g添加し、内温5~10℃で一晩撹拌させた。析出している固体をろ別し乾燥させ、白色固体を1.43g(収率17.7%)得た。赤外吸収スペクトル(IR:装置名:Frontier GOLD spotlight 400、製造元:Perkin Elmer)により、1243cm-1にエーテル結合由来のピークを確認し、3200~2800cm-1付近に検出されるOH基由来のブロードなピークが消失していることで、上記式8で表されるジフェニルエーテル誘導体であることを確認した。
上記式8で表されるジフェニルエーテル誘導体の合成における反応条件のうち、ベンジルブロミド6.13gを1-ブロモオクタデカン12.0gに変更した以外は同様の手順で合成した。それにより白色固体を1.68g(収率12.8%)得た。赤外吸収スペクトル(IR)により、1231cm-1にエーテル結合由来のピークを確認し、2850、2960cm-1にC-H伸縮運動によるピークを確認し、さらに、3200~2800cm-1付近に検出されるOH基由来のブロードなピークが消失していることで、上記式9で表されるジステアリルエーテル誘導体であることを確認した。
温度計、スターラーピースを備えた反応容器へ、トルエン50g、トリエチルアミン3.6g、4,4-ジメチルアミノピリジン(DMAP)0.21g、上記式4で表されるハロゲン化合物を5.0g加えた。そこに、ベンゾイルクロライド4.27gをトルエン10gに溶解させた溶液を15分かけて滴下した。滴下終了後、内温40℃で72時間反応させた。
ガスクロマトグラフ(GC:装置名GC-2010、製造元:島津製作所)で原料である上記ハロゲン化合物(式4)のピークが消失していることを確認後、純水50gを添加した。5分撹拌後、下層を抜き取り、再度純水50g添加し、分液操作を行った。上層の溶媒をエバポレーターにより溶媒を留去することで、粘性の高い液体を得た。IPA70gとトルエン1gを添加し、撹拌すると、固形分が析出した。そのまま、一晩室温で撹拌した。析出している固体をろ別し乾燥させ、白色固体を4.51g(収率52.7%)得た。赤外吸収スペクトル(IR:装置名:Frontier GOLD spotlight 400、製造元:Perkin Elmer)により、1742cm-1にエステル結合由来のピークを確認し、3200~2800cm-1付近に検出されるOH基由来のブロードなピークが消失していることで、上記式10で表されるジフェニルエステル誘導体であることを確認した。
上記式10で表されるジフェニルエステル誘導体の合成における反応条件のうち、ベンゾイルクロライド4.27gをステアリルクロライド10.36gに変更した以外は同様の手順で合成した。それにより白色固体を9.14g(収率64.8%)得た。赤外吸収スペクトル(IR)により、1742cm-1にエステル結合由来のピークを確認し、2850、2960cm-1にC-H伸縮運動によるピークを確認し、さらに、3200~2800cm-1付近に検出されるOH基由来のブロードなピークが消失していることで、上記式11で表されるステアリルエステル誘導体であることを確認した。
温度計、スターラーピースを備えた反応容器へ、シクロヘキサン50g、トルエン10g、1,4-ジアザビシクロ[2.2.2]オクタン(DABCO)0.1g、イソシアン酸フェニル4.47g、上記式4で表されるハロゲン化合物を5.0g加えた。その後内温65℃で24時間反応させた。GCで原料である上記ハロゲン化合物のピークが消失していることを確認後、メタノール20g追加し、室温で一晩反応させた。析出している固体をろ別した。ろ別した固体にIPAを加え、3時間撹拌した。再度ろ別し、白色固体6.27g(収率69.2%)得た。赤外吸収スペクトル(IR)により、3317cm-1にN-1置換アミドN-H伸縮振動由来のピーク及び1708cm-1にウレタン結合由来のピークを確認し、2275~2250cm-1付近に出現するイソシアネート由来のピークが消失し、及び3200~2800cm-1付近に検出されるOH基由来のブロードなピークが消失していることで、上記式12で表されるジフェニルウレタン誘導体であることを確認した。
上記式12で表されるジフェニルウレタン誘導体の合成における反応条件のうち、イソシアン酸フェニル4.47gをイソシアン酸ステアリル7.57g、上記式4で表されるハロゲン化合物5.0gを3.0gに変更した以外は同様の手順で合成した。それにより白色固体を9.14g(収率64.8%)得た。赤外吸収スペクトル(IR)により、3346cm-1にN-1置換アミドN-H伸縮振動由来のピーク、2849、2917cm-1にC-H伸縮運動によるピーク、1688cm-1にウレタン結合由来のピーク及び、1528cm-1に鎖状N-1置換アミド由来のピークを確認し、2275~2250cm-1付近に出現するイソシアネート由来のピークが消失し、3200~2800cm-1付近に検出されるOH基由来のブロードなピークが消失していることで、上記式13で表されるジステアリルウレタン誘導体であることを確認した。
活性剤のフラックス中における含有量は特に限定されるものではないが、例えば、0.1質量%以上10質量%以下、好ましくは0.3質量%以上4質量%以下等が挙げられる。
本実施形態のフラックスをやに入りはんだ用のフラックスとして用いる場合には、上記活性剤の含有量は、例えば、0.3質量%以上4質量%以下、好ましくは1質量%以上3質量%以下等であることが挙げられる。
上記活性剤の含有量が上記範囲である場合には、はんだ付け直後からはんだの濡れ性を向上させやすく、且つはんだの濡れ性を持続的に向上させやすくなるため好ましい。
樹脂成分としては、合成樹脂、天然樹脂など、フラックスの樹脂成分として用いられる公知の樹脂成分であれば特に限定されるものではない。例えば、重合ロジン、水添ロジン、天然ロジン、不均化ロジン、酸変性ロジン等が挙げられる。
本実施形態のフラックスをやに入りはんだ用のフラックスとして用いる場合には、上記樹脂成分の含有量は、例えば、40質量%以上99質量%以下、好ましくは60質量%以上99質量%以下等であることが挙げられる。
本実施形態のフラックスは上述のとおり、ソルダーペーストなどのはんだ組成物、やに入りはんだ等のはんだ用いることができる。
はんだ合金としては、特に限定されるものではなく、無鉛のはんだ合金、有鉛のはんだ合金のいずれでもよいが、環境への影響の観点から無鉛のはんだ合金が好ましい。
具体的には、無鉛のはんだ合金としては、スズ、銀、銅、亜鉛、ビスマス、アンチモン等を含む合金等が挙げられ、より具体的には、Sn/Ag、Sn/Ag/Cu、Sn/Cu、Sn/Ag/Bi、Sn/Bi、Sn/Ag/Cu/Bi、Sn/Sb、Sn/Zn/Bi、Sn/Zn、Sn/Zn/Al、Sn/Ag/Bi/In、Sn/Ag/Cu/Bi/In/Sb、In/Ag等の合金が挙げられる。
やに入りはんだの中のフラックスの含有量は1質量%以上5質量%以下であることが好ましい。
本実施形態の活性剤を含むフラックスは、やに入りはんだ用のフラックスとして用いられることが特に好ましい。
やに入りはんだは、濡れ性が低下すると、フィレットの形成不良、端子間におけるブリッジ、ツノ立ちという不良が発生しやすくなる。
本実施形態のフラックスを含むやに入りはんだは、濡れ性低下をはんだ付け直後から抑制でき、且つ持続的に濡れ性を向上させうるため、濡れ性低下による上記不良を効果的に抑制しうる。
尚、本発明において上記場合は、X1がBrである場合にX2はIであり、X1がIである場合にX2はBrであることを意味する。
活性剤として下記の活性剤1乃至6を用い、表1に示す配合比のフラックスを作製した。各原料を加熱容器に投入して、180℃まで加熱し、全原料が溶解して分散したことを確認した。その後、室温にまで冷却して、均一なフラックスを得た。ここで、水素添加ロジンとして荒川化学工業社製「KR-612」を、酸変性ロジンとして荒川化学工業社製「パインクリスタル KE-604」、有機酸としてアジピン酸を用いた。
活性剤2:上記式8で表されるジフェニルエーテル誘導体
活性剤3:上記式9で表されるジステアリルエーテル誘導体
活性剤4:上記式10で表されるジフェニルエステル誘導体
活性剤5:上記式11で表されるジステアリルエステル誘導体
活性剤6:上記式12で表されるジフェニルウレタン誘導体
活性剤7:上記式13で表されるジステアリルウレタン誘導体
活性剤8:下記式14で表されるハロゲン化合物
活性剤9:下記式15で表されるハロゲン化合物
以下の方法で、各フラックスの濡れ性を評価した。
脱脂洗浄した銅板(3mm×3mm×0.5mm厚)上に、糸はんだ(はんだ合金:SAC305(Sn96.5質量%、Ag3.0質量%、Cu0.5質量%)長さ約7mm、径1.0mm)を径2.0mmのリング状にしたものを置き、このリング状の糸はんだの上に、各フラックスをひとかけら(約10mg)乗せて試験片を作製した。
各試験片を300℃に加熱したはんだ槽の上に置き、糸はんだを溶融させ、溶融後5秒間経過した後、試験片をはんだ槽の上からはずした。
各試験片をイソプロピルアルコールを用いフラックスを洗浄し、はんだの高さをマイクロメーター(ミツトヨ社製)で測定した。該はんだの高さから以下の計算式で広がり率を求めた。
H:はんだの高さ=(試験後の基板の厚さ)-(試験前の基板の厚さ)
D:試験に用いたはんだを球とみなした場合の直径(mm)=2.2(mm)
結果を表2に示す。
尚、実施例1に比べると実施例2~7では、やや広がり率が低いが、これは、分子量の大きい置換基が導入された活性剤を使用しているため、ハロゲン含有割合が低下するためであると考えられる。
次に、上記活性剤1乃至7を用いたフラックス(実施例1~7、および比較例1、2)で、やに入りはんだ(実施例8乃至14、比較例3、4)を作製し、はんだ付け試験を行った。やに入りはんだの中のフラックスの含有量は3.2%とし、線径を0.5mmφとなるように調整、製造した。
基板のランドにはんだが濡れて、且つピン部品のリードの周辺に山の裾野のように、はんだ接合が形成される状態をフィレットが形成された状態であるとする。
目視にて各基板を観察し、基板のパッドのすべてにはんだが濡れて良好な状態である場合にはA、イモはんだ付けが生じる場合にはB、基板のパッドの一部ではんだがはじかれてフィレットの形状が不均一な状態であった場合にはCと評価した。
尚、イモはんだ付けが生じた状態とは、ランドにはんだが濡れているが、その形状が山の裾野のようにならず、団子状に形成された状態を意味する。
ブリッジとは、はんだの表面酸化膜の除去が不十分で、流動性が低下し、隣接するピン間ではんだが繋がってしまう不良現象をいう。
目視にて各基板を観察し、スライド速度が速い場合(10mm/秒)でブリッジ無しをA、スライド速度が速い場合(10mm/秒)ではブリッジ有りだが、通常のスライド速度(6mm/秒)でブリッジ無しをB、通常のスライド速度(6mm/秒)でブリッジ有りをCと評価した。結果を表3に示す。
Claims (4)
- 前記X1はBr又はIであり、前記X2はBr又はIである請求項1に記載のフラックス用活性剤。
- 請求項1又は2に記載のフラックス用活性剤を含むフラックス。
- 請求項3に記載のフラックスを含むはんだ。
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2015
- 2015-02-05 JP JP2015021528A patent/JP5816947B1/ja active Active
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2016
- 2016-02-05 MY MYPI2017702698A patent/MY182814A/en unknown
- 2016-02-05 TW TW105104149A patent/TWI665047B/zh active
- 2016-02-05 PL PL16746731T patent/PL3254800T3/pl unknown
- 2016-02-05 CN CN201680004703.9A patent/CN107107278B/zh active Active
- 2016-02-05 US US15/546,868 patent/US10702956B2/en active Active
- 2016-02-05 EP EP16746731.5A patent/EP3254800B1/en active Active
- 2016-02-05 KR KR1020177014391A patent/KR102356003B1/ko active IP Right Grant
- 2016-02-05 WO PCT/JP2016/053540 patent/WO2016125901A1/ja active Application Filing
- 2016-02-05 SG SG11201705919WA patent/SG11201705919WA/en unknown
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WO2019216291A1 (ja) * | 2018-05-08 | 2019-11-14 | 株式会社弘輝 | フラックス及びはんだ材料 |
KR20200130492A (ko) * | 2018-05-08 | 2020-11-18 | 가부시키가이샤 코키 | 플럭스 및 땜납 재료 |
KR102234323B1 (ko) | 2018-05-08 | 2021-03-30 | 가부시키가이샤 코키 | 플럭스 및 땜납 재료 |
US11833621B2 (en) | 2018-05-08 | 2023-12-05 | Koki Company Limited | Flux and solder material |
Also Published As
Publication number | Publication date |
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MY182814A (en) | 2021-02-05 |
EP3254800A4 (en) | 2018-07-11 |
PL3254800T3 (pl) | 2021-07-19 |
KR20170108937A (ko) | 2017-09-27 |
US20180015576A1 (en) | 2018-01-18 |
JP5816947B1 (ja) | 2015-11-18 |
TWI665047B (zh) | 2019-07-11 |
EP3254800B1 (en) | 2020-11-11 |
EP3254800A1 (en) | 2017-12-13 |
CN107107278A (zh) | 2017-08-29 |
KR102356003B1 (ko) | 2022-01-25 |
JP2016140915A (ja) | 2016-08-08 |
TW201636147A (zh) | 2016-10-16 |
CN107107278B (zh) | 2019-09-03 |
SG11201705919WA (en) | 2017-08-30 |
US10702956B2 (en) | 2020-07-07 |
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