WO2007029589A1 - 錫および錫合金の水系酸化防止剤 - Google Patents

錫および錫合金の水系酸化防止剤 Download PDF

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Publication number
WO2007029589A1
WO2007029589A1 PCT/JP2006/317199 JP2006317199W WO2007029589A1 WO 2007029589 A1 WO2007029589 A1 WO 2007029589A1 JP 2006317199 W JP2006317199 W JP 2006317199W WO 2007029589 A1 WO2007029589 A1 WO 2007029589A1
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Prior art keywords
tin
antioxidant
solder
molecule
alkyl group
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PCT/JP2006/317199
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English (en)
French (fr)
Japanese (ja)
Inventor
Takashi Ouchi
Katsuyuki Tsuchida
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Nippon Mining & Metals Co., Ltd.
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Publication date
Application filed by Nippon Mining & Metals Co., Ltd. filed Critical Nippon Mining & Metals Co., Ltd.
Priority to CN2006800328749A priority Critical patent/CN101258268B/zh
Priority to JP2007534363A priority patent/JP4601670B2/ja
Publication of WO2007029589A1 publication Critical patent/WO2007029589A1/ja

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    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23GCLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
    • C23G1/00Cleaning or pickling metallic material with solutions or molten salts
    • C23G1/02Cleaning or pickling metallic material with solutions or molten salts with acid solutions
    • C23G1/04Cleaning or pickling metallic material with solutions or molten salts with acid solutions using inhibitors
    • C23G1/06Cleaning or pickling metallic material with solutions or molten salts with acid solutions using inhibitors organic inhibitors
    • C23G1/066Cleaning or pickling metallic material with solutions or molten salts with acid solutions using inhibitors organic inhibitors phosphorus-containing compounds
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/10Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
    • B22F1/102Metallic powder coated with organic material
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M137/00Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing phosphorus
    • C10M137/12Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing phosphorus having a phosphorus-to-carbon bond
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23FNON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
    • C23F11/00Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent
    • C23F11/08Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent in other liquids
    • C23F11/10Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent in other liquids using organic inhibitors
    • C23F11/167Phosphorus-containing compounds
    • C23F11/1673Esters of phosphoric or thiophosphoric acids
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23FNON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
    • C23F11/00Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent
    • C23F11/08Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent in other liquids
    • C23F11/10Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent in other liquids using organic inhibitors
    • C23F11/167Phosphorus-containing compounds
    • C23F11/1676Phosphonic acids
    • HELECTRICITY
    • H05ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05KPRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
    • H05K3/00Apparatus or processes for manufacturing printed circuits
    • H05K3/30Assembling printed circuits with electric components, e.g. with resistor
    • H05K3/32Assembling printed circuits with electric components, e.g. with resistor electrically connecting electric components or wires to printed circuits
    • H05K3/34Assembling printed circuits with electric components, e.g. with resistor electrically connecting electric components or wires to printed circuits by soldering
    • H05K3/3457Solder materials or compositions; Methods of application thereof
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2223/00Organic non-macromolecular compounds containing phosphorus as ingredients in lubricant compositions
    • C10M2223/06Organic non-macromolecular compounds containing phosphorus as ingredients in lubricant compositions having phosphorus-to-carbon bonds
    • C10M2223/061Metal salts
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2223/00Organic non-macromolecular compounds containing phosphorus as ingredients in lubricant compositions
    • C10M2223/06Organic non-macromolecular compounds containing phosphorus as ingredients in lubricant compositions having phosphorus-to-carbon bonds
    • C10M2223/063Ammonium or amine salts
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10NINDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2010/00Metal present as such or in compounds
    • C10N2010/02Groups 1 or 11
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10NINDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2010/00Metal present as such or in compounds
    • C10N2010/08Groups 4 or 14
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10NINDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2030/00Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
    • C10N2030/10Inhibition of oxidation, e.g. anti-oxidants
    • HELECTRICITY
    • H05ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05KPRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
    • H05K2203/00Indexing scheme relating to apparatus or processes for manufacturing printed circuits covered by H05K3/00
    • H05K2203/07Treatments involving liquids, e.g. plating, rinsing
    • H05K2203/0779Treatments involving liquids, e.g. plating, rinsing characterised by the specific liquids involved
    • H05K2203/0786Using an aqueous solution, e.g. for cleaning or during drilling of holes
    • HELECTRICITY
    • H05ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05KPRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
    • H05K2203/00Indexing scheme relating to apparatus or processes for manufacturing printed circuits covered by H05K3/00
    • H05K2203/12Using specific substances
    • H05K2203/122Organic non-polymeric compounds, e.g. oil, wax or thiol

Definitions

  • the present invention relates to an aqueous antioxidant for tin and a tin alloy, and a surface treatment method using the same. Furthermore, the present invention relates to an electronic component, a solder ball, a solder powder, a ball grid array using the solder ball, a solder paste using the solder powder, the electronic component processed with the aqueous anti-oxidation agent, It relates to a mounted product using them.
  • soldering is a technique for joining objects using a material having a relatively low melting point, and is widely used in joining and assembling electronic devices in the modern industry.
  • solder is Sn-Pb alloy, and its eutectic composition (63% Sn-remainder Pb) has a low melting point of 183 ° C, so soldering is 220-230 °. Since it is performed in C, it causes little thermal damage to electronic components and boards.
  • the Sn-Pb alloy also has good solderability and solidifies immediately during soldering, and does not easily crack or peel even when vibration is applied to the soldered part. Have it.
  • Pure Sn plating is the best lead-free plating in terms of cost and workability. It is considered promising. However, pure Sn plating has a problem that it is easy to generate a whisker due to the internal stress of the surface acid, and the solder wettability deteriorates over time. Is strongly demanded.
  • Sn—Zn alloys have melting points close to those of conventional Sn—Pb alloys, Sn—Zn alloys are advantageous in that it is not necessary to change current facilities and processes.
  • the plating film is excellent in mechanical strength and cost.
  • Zn is an active metal species, the solder wettability of Sn-Zn alloys, which are easily oxidized, is very poor. .
  • solder paste is used for surface mounting an electronic component on a substrate, and its usage is increasing in recent years.
  • the solder paste is generally composed of a solder alloy powder as a main component and added with a flux containing an adhesive, an activator, a thixotropic agent, a surfactant, a solvent, and the like.
  • Sn-Ag (Cu), Sn-Zn, and Sn-Bi alloys are being investigated as lead-free solder pastes. Because it is close to the eutectic temperature of a solder, it is considered as a promising alternative candidate.
  • solder paste using Sn-Zn alloy as solder powder causes an acid-oxidation reaction with the activator contained in the flux, resulting in solder wettability and storage stability.
  • an inert gas atmosphere is required during reflow.
  • Patent Document 1 exemplifies a phosphate ester type surfactant containing ethylene oxide and having an alkylphenol group having 8 to 30 carbon atoms as a lipophilic group.
  • Patent Document 2 describes that a phosphate ester containing a saturated or unsaturated alkyl group having 10 to 26 carbon atoms is preferable.
  • Patent Document 3 describes a phosphate ester containing a phenyl group or an alkyl group having 5 or less carbon atoms. In this case, the anti-oxidation function during humidification is excellent, but sufficient lubrication performance cannot be obtained. These are described in three patent documents. The phosphoric acid ester compounds listed are less effective in preventing discoloration and acidification during heating.
  • Patent Document 1 Japanese Patent Publication No. 5-22322
  • Patent Document 2 Japanese Patent Application Laid-Open No. 2004-137574
  • Patent Document 3 Japanese Patent No. 3155139
  • An object of the present invention is to provide an antioxidant exhibiting excellent solder wettability by treating tin or a tin alloy, which is excellent in antioxidant performance during heating or humidification. It is another object of the present invention to provide an anti-oxidation agent having excellent whisker characteristics and lubricity when an external load is applied.
  • the surface treatment agent in the case of a surface treatment agent containing a ⁇ compound having two or more phosphonic acid groups in one molecule and no ester bond in the molecule, the surface treatment agent is heated or calorieated. Excellent anti-humidity performance, wettability and whisker resistance in wet conditions, but insufficient whisker resistance and lubrication in areas where external stress is applied. However, sufficient characteristics were not obtained.
  • the present invention is as follows.
  • a compound having two or more phosphonic acid groups in one molecule and no ester bond in the molecule, and Z or a salt thereof, and a phosphate ester having an alkyl group having 6 to 10 carbon atoms An aqueous anti-oxidation agent for tin and tin alloys.
  • a compound having two or more phosphonic acid groups in one molecule and no ester bond in the molecule, and Z or a salt thereof are represented by the following formula (1), ( ⁇ ) or (III) Or a salt of Z or an alkali metal salt thereof, an ammonium salt, or an aminic compound thereof, and the compound according to any one of (1) to (3) above, Water-based antioxidant for tin and tin alloys.
  • x 3 and ⁇ O ⁇ oPH I 3 may be the same or different hydrogen atoms, or
  • Table 1 represents a lower alkyl group having 1 to 5 carbon atoms.
  • R 2 and R 4 each represent the following group (A), which may be the same or different, R 3 represents the following group (A), or a lower alkyl group having 1 to 5 carbon atoms, n is Represents an integer from 1 to 3.
  • X represents a hydrogen atom or a lower alkyl group having 1 to 5 carbon atoms
  • Y represents a hydrogen atom
  • a surface treatment method characterized by treating the surface of tin or a tin alloy with the aqueous acid / soaking agent according to any one of (1) to (4).
  • a solder ball or solder powder characterized by using a tin alloy which has been subjected to a surface treatment using the aqueous acid-rich inhibitor according to any one of (1) to (4).
  • a compound having two or more phosphonic acid groups in one molecule and no ester bond in the molecule, and Z or a salt thereof, and a phosphate ester having an alkyl group having 6 to 10 carbon atoms By surface-treating tin or a tin alloy with the water-based antioxidant of the present invention containing bismuth, it has excellent anti-oxidation performance during heating and humidification, exhibits good solder wettability, and has excellent whisker characteristics and lubrication when an external load is applied. It becomes tin or a tin alloy which is excellent in properties. Therefore, the water-based antioxidant of the present invention is suitable as an antioxidant for the tin- or tin-alloy-attached portion of the fitting portion between the FPC or FFC and the connector.
  • tin alloys are more preferred because they do not contain lead in terms of environmental pollution and other problems.
  • Sn alloy that does not contain lead Sn alloy such as solder alloy containing one or more of Zn, Bi, Cu, In, Ag and Sb.
  • the composition of the antioxidant of the present invention comprises a phosphoric acid ester having a specific alkyl group and a compound having two or more phosphonic acid groups in one molecule and no ester bond in the molecule.
  • This is an aqueous solution. It is difficult to dissolve a compound having two or more phosphonic acid groups in one molecule and not containing an ester bond in the molecule and a phosphate ester having an alkyl group. It is necessary to select the number of carbon atoms in the alkyl group. It was confirmed that the solubility in aqueous solution was low when the alkyl group of the phosphate ester having an alkyl group had 11 or more carbon atoms.
  • a compound having two or more phosphonic acid groups in one molecule and no ester bond in the molecule, and Z or a salt thereof may be contained singly or in combination.
  • the total content is preferably 0. OlgZL or more. 0. Less than OlgZL, the effect is small.
  • there is no upper limit of the content because the properties do not deteriorate even if the content is too high, but the content is more preferably 0.01 to 500 g / L due to cost problems. More preferably, 0.1 to: LOOgZL.
  • the force of a compound having two or more phosphonic acid groups in one molecule is more detailed than that of a compound having one phosphonic acid group in one molecule. It turned out to be excellent.
  • the number of phosphonic acid groups in one molecule is preferably 2 to 6 because of cost issues.
  • ⁇ 3 and ⁇ 3 each represent the same or different and Yogu hydrogen atom, or a lower alkyl group of 1 to 5 carbon atoms.
  • R 2 and R 4 each represent the following group (A), which may be the same or different, R 3 represents the following group (A), or a lower alkyl group having 1 to 5 carbon atoms, n is Represents an integer from 1 to 3.
  • X represents a hydrogen atom or a lower alkyl group having 1 to 5 carbon atoms
  • Y represents a hydrogen atom
  • Child a lower alkyl group having 1 to 5 carbon atoms, Yc xll alkyl group, hydroxyl group, or amino group.
  • ethylenediaminetetrakismethylenephosphonic acid, diethylenetriamine pentakismethylenephosphonic acid, etc. are particularly preferred as the compound represented by the above general formula (III).
  • 1-hydroxyethane 1,1-diphosphonic acid is particularly preferred.
  • the alkali metal salt of the above compound is preferably a sodium salt, potassium salt or the like.
  • the salt with an amine compound is preferably a triethylamine salt or a triethanolamine salt!
  • the phosphate ester having an alkyl group having 6 to 10 carbon atoms may be a mixture of a monoalkyl ester and a dialkyl ester, preferably a monoalkyl ester or a dialkyl ester! /. When it is obtained as a mixture of monoalkyl ester and dialkyl ester in production, it can be used as it is without separation, and in the case of a mixture, it may be a mixture in any proportion.
  • the phosphate ester examples include monohexyl phosphate ester, dihexyl phosphate ester, mono 2-ethylhexyl phosphate ester, di-2-ethylhexyl phosphate ester, monooctyl phosphate ester, dioctyl phosphate ester, monoiso Decyl phosphate ester, diisodecyl phosphate ester and the like are preferable.
  • the content of the antioxidant is preferably from 0.01 to LOOgZL, more preferably from 0.1 to LOg / L. When the content is less than 0. Olg / L, the film formation is insufficient, and when it exceeds lOOgZL, the stability of the liquid is remarkably lowered.
  • the anti-oxidation agent of the present invention comprises a compound having two or more phosphonic acid groups in one molecule and containing no ester bond in the molecule, Z or a salt thereof, and 6 to 10 carbon atoms.
  • a phosphate ester having an alkyl group can be used by dissolving in an aqueous solvent.
  • aqueous solvent water is preferable in consideration of solubility and cost, but alcohols, glycols, ketones and the like may be contained in addition to water.
  • the aqueous antioxidant of the present invention further improves the acid resistance of the surface to be treated by adjusting the pH to 5 or less.
  • the pH of the anti-oxidation agent is more preferably ⁇ 1 to 5 in view of the influence on the material and the like.
  • As the pH adjuster generally available acids and alkalis can be used.
  • the acid resistance of the surface to be treated is further improved. Even if the addition amount of the surfactant is less than 0. OlgZL or exceeds 1OgZL, the effect of improving acid resistance cannot be obtained.
  • the addition amount of the surfactant is preferably 0.1 to LOg / L.
  • surfactant one or more of commercially available ion-based, cationic, non-ionic, and amphoteric surfactants can be appropriately selected and used.
  • cationic surfactant sulfate ester type, sulfonate salt type, phosphate ester salt type, sulfosuccinate type, etc.
  • quaternary ammonium salt type Amine salt type isotropic non-ionic surfactants include: products with higher alcohol ethylene oxide, products with higher alcohol propylene oxide, alkylphenol ethylene oxide adducts, polyoxyethylene polyoxypropylene Block polymers 1, ethyleneoxyamine polyoxyethylene polyoxypropylene block polymers, higher aliphatic amine amine oxide adducts, aliphatic amide ethylene oxide carbonates, etc., are amphoteric surfactants such as amino acid type and betaine type. Etc. are preferred.
  • one or more of one-on or two-on Is preferably selected and used.
  • nonionic surfactants the higher glycol ethylene oxide adducts, higher alcohol propylene oxide adducts, alkyl phenol ethylene oxide adducts, polyoxyethylene polyoxypropylene block polymers are particularly preferred for the polyethylene glycol type. Etc. can be particularly preferably used.
  • a sulfate ester salt type and a phosphate ester salt type are particularly preferable.
  • the antioxidant of the present invention may contain an additive in an amount within a range that does not impair the original properties for the purpose of imparting desired performance.
  • additives include preservatives and pH buffering agents, and conventionally known additives can be used.
  • any method that forms a film on the surface of tin or tin alloy may be used.
  • tin or tin alloy may be used. Examples include a method of simply immersing in an antioxidant, a method of applying an antioxidant using a shower or a device such as an air coater, blade coater, rod coater, knife coater, gravure coater, reverse coater, cast coater, etc. .
  • the temperature of the antioxidant during the surface treatment is preferably 15 to 80 ° C, more preferably 30 to 70 ° C.
  • the surface of the conductor of the connection terminal portion of the electronic component is tinned or tin-plated and then surface-treated to provide excellent oxidation resistance, solder wettability, and whisker resistance.
  • An electronic component with good lubricity can be obtained.
  • the electronic component in the present invention includes a substrate.
  • a solder ball using a tin alloy treated with the anti-oxidation agent of the present invention has excellent oxidation resistance and is disposed as a ball grid array as an electrical connection member or in an electronic component. It can be used favorably as a mounted product connected to.
  • a tin alloy powder is treated with the antioxidant of the present invention, and a flux containing an adhesive, an activator, a thixotropic agent, a surfactant, a solvent, and the like is added to the solder paste. It can also be used. This solder paste is excellent in oxidation resistance and whisker resistance. Conventionally known pressure-sensitive adhesives, activators, thixotropic agents, surfactants and solvents can be used.
  • Comparative Example 2 As a comparative example, as shown in Table 2, six types of aqueous solutions were prepared in the same manner as in the examples (Comparative Examples 1 to 6). Since Comparative Example 7 was not treated with antioxidant, no antioxidant was prepared. Further, as Comparative Example 8, the power obtained by changing the hexyl phosphate of the solution of Example 2 to oleyl phosphate was suspended in brown, and the active ingredient was completely dissolved.
  • hexyl phosphate ester, 2-ethylhexyl phosphate ester, isodecyl phosphate ester and butyl phosphate ester are all mixtures of monoalkyl phosphate ester and dialkyl phosphate ester.
  • Nitrilotrismethylenephosphonic acid 1 / L 2 Hexyl phosphate: 0.5g / L
  • Nonylphenol ethylene oxide 12 mol adduct 1 g / L
  • Nitrilotrismethylenephosphonic acid K salt 1 g / s 6 Hexyl phosphate: 0.5 g / L
  • Nitrilotrismethylenephosphonic acid 1 g / L 2
  • Nitryltrismethylenephosphonic acid K salt 1 g / L 6
  • This substrate was tinned with a thickness of about 5 m (plating bath: Tincoat K (manufactured by Nikko Metal Plating Co., Ltd.)), plating conditions: cathode current density 2AZdm 2 , temperature 20 ° C , Liquid flow and force sword rocking).
  • This tinned base material (hereinafter referred to as "Sn base material”) was immersed in the above antioxidant for 10 seconds at a bath temperature of 60 ° C, then washed with water and dried to obtain a test substrate. It was.
  • test boards were heat-treated in an electric furnace maintained at 220 ° C for 1 hour in the air atmosphere, and then solder wettability (zero cross time) with lead-free solder was measured by the meniscograph method based on the following measurement conditions .
  • the evaluation criteria are as follows.
  • Zero crossing time 1 second or more and less than 3 seconds
  • Zero crossing time 3 seconds or more and less than 5 seconds
  • test boards were PCT-treated (temperature standing at 105 ° C, humidity 100% for 16 hours), and solder wettability (zero cross time) with lead-free solder was measured by meniscograph method. The measurement was performed in the same manner as the term of heat resistance and acidity.
  • the evaluation criteria are as follows.
  • Zero crossing time 1 second or more and less than 3 seconds
  • Zero crossing time 3 seconds or more and less than 5 seconds
  • the substrate was left for 24 hours in a constant temperature and humidity atmosphere at a temperature of 85 ° C and a humidity of 85%. Thereafter, after the substrate was sufficiently dried, the surface was observed with a scanning electron microscope (SEM). As a result, no whisker was generated in any of the examples and comparative examples.
  • SEM scanning electron microscope
  • the evaluation criteria are as follows.
  • the lubricity of the surface of the test substrate was evaluated by the coefficient of static friction.
  • Sn-Zn substrate Sn-Zn plated substrate

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Manufacturing & Machinery (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Preventing Corrosion Or Incrustation Of Metals (AREA)
PCT/JP2006/317199 2005-09-07 2006-08-31 錫および錫合金の水系酸化防止剤 WO2007029589A1 (ja)

Priority Applications (2)

Application Number Priority Date Filing Date Title
CN2006800328749A CN101258268B (zh) 2005-09-07 2006-08-31 锡和锡合金的水系抗氧化剂
JP2007534363A JP4601670B2 (ja) 2005-09-07 2006-08-31 錫および錫合金の水系酸化防止剤

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JP2005-258826 2005-09-07
JP2005258826 2005-09-07

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JP (1) JP4601670B2 (ko)
KR (1) KR100964063B1 (ko)
CN (1) CN101258268B (ko)
TW (1) TW200712257A (ko)
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Cited By (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2007197791A (ja) * 2006-01-27 2007-08-09 Daiwa Fine Chemicals Co Ltd (Laboratory) めっき後処理剤組成物
JP2010525169A (ja) * 2007-04-18 2010-07-22 エントン インコーポレイテッド 金属表面の強化
JP2012506488A (ja) * 2008-10-21 2012-03-15 アトテツク・ドイチユラント・ゲゼルシヤフト・ミツト・ベシユレンクテル・ハフツング 金属又は金属合金表面の耐食性を増加させるための後処理組成物
WO2012118075A1 (ja) * 2011-03-02 2012-09-07 千住金属工業株式会社 フラックス
JP2012255205A (ja) * 2011-05-13 2012-12-27 C Uyemura & Co Ltd 錫又は錫合金めっき皮膜用後処理剤、及び錫又は錫合金めっき皮膜の処理方法
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