JP6822440B2 - Cleaning agent composition for lead-free solder flux, cleaning method for lead-free solder flux - Google Patents
Cleaning agent composition for lead-free solder flux, cleaning method for lead-free solder flux Download PDFInfo
- Publication number
- JP6822440B2 JP6822440B2 JP2018096880A JP2018096880A JP6822440B2 JP 6822440 B2 JP6822440 B2 JP 6822440B2 JP 2018096880 A JP2018096880 A JP 2018096880A JP 2018096880 A JP2018096880 A JP 2018096880A JP 6822440 B2 JP6822440 B2 JP 6822440B2
- Authority
- JP
- Japan
- Prior art keywords
- lead
- free solder
- cleaning agent
- agent composition
- solder flux
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 229910000679 solder Inorganic materials 0.000 title claims description 58
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- OQIRZNNBUNOXTQ-UHFFFAOYSA-N n,n,n',n'-tetraethylpentane-1,5-diamine Chemical compound CCN(CC)CCCCCN(CC)CC OQIRZNNBUNOXTQ-UHFFFAOYSA-N 0.000 description 1
- TXXWBTOATXBWDR-UHFFFAOYSA-N n,n,n',n'-tetramethylhexane-1,6-diamine Chemical compound CN(C)CCCCCCN(C)C TXXWBTOATXBWDR-UHFFFAOYSA-N 0.000 description 1
- DNOJGXHXKATOKI-UHFFFAOYSA-N n,n,n',n'-tetramethylpentane-1,5-diamine Chemical compound CN(C)CCCCCN(C)C DNOJGXHXKATOKI-UHFFFAOYSA-N 0.000 description 1
- OAFOHGONKIXDDE-UHFFFAOYSA-N n,n,n',n'-tetrapropylhexane-1,6-diamine Chemical compound CCCN(CCC)CCCCCCN(CCC)CCC OAFOHGONKIXDDE-UHFFFAOYSA-N 0.000 description 1
- FTQWRYSLUYAIRQ-UHFFFAOYSA-N n-[(octadecanoylamino)methyl]octadecanamide Chemical compound CCCCCCCCCCCCCCCCCC(=O)NCNC(=O)CCCCCCCCCCCCCCCCC FTQWRYSLUYAIRQ-UHFFFAOYSA-N 0.000 description 1
- PHDLNXKJCPLCRO-UHFFFAOYSA-N n-[2-(diethylamino)ethyl]-n',n'-diethyl-n-methylethane-1,2-diamine Chemical compound CCN(CC)CCN(C)CCN(CC)CC PHDLNXKJCPLCRO-UHFFFAOYSA-N 0.000 description 1
- UICCSKORMGVRCB-UHFFFAOYSA-N n-[2-(diethylamino)ethyl]-n',n'-diethylethane-1,2-diamine Chemical compound CCN(CC)CCNCCN(CC)CC UICCSKORMGVRCB-UHFFFAOYSA-N 0.000 description 1
- JPJMSWSYYHNPLD-UHFFFAOYSA-N n-[2-(dimethylamino)ethyl]-n',n'-dimethylethane-1,2-diamine Chemical class CN(C)CCNCCN(C)C JPJMSWSYYHNPLD-UHFFFAOYSA-N 0.000 description 1
- FIDAJBOTMYEWMR-UHFFFAOYSA-N n-[2-(dipropylamino)ethyl]-n',n'-dipropylethane-1,2-diamine Chemical compound CCCN(CCC)CCNCCN(CCC)CCC FIDAJBOTMYEWMR-UHFFFAOYSA-N 0.000 description 1
- VMOWJORKYKVTSS-UHFFFAOYSA-N n-[2-[2-(dipropylamino)ethoxy]ethyl]-n-propylpropan-1-amine Chemical class CCCN(CCC)CCOCCN(CCC)CCC VMOWJORKYKVTSS-UHFFFAOYSA-N 0.000 description 1
- SALTZQPERQCAHK-UHFFFAOYSA-N n-[2-[2-[di(propan-2-yl)amino]ethoxy]ethyl]-n-propan-2-ylpropan-2-amine Chemical class CC(C)N(C(C)C)CCOCCN(C(C)C)C(C)C SALTZQPERQCAHK-UHFFFAOYSA-N 0.000 description 1
- DVVORTHDQVBZOO-UHFFFAOYSA-N n-[2-[di(propan-2-yl)amino]ethyl]-n',n'-di(propan-2-yl)ethane-1,2-diamine Chemical compound CC(C)N(C(C)C)CCNCCN(C(C)C)C(C)C DVVORTHDQVBZOO-UHFFFAOYSA-N 0.000 description 1
- 125000004108 n-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 125000004433 nitrogen atom Chemical group N* 0.000 description 1
- IOQPZZOEVPZRBK-UHFFFAOYSA-N octan-1-amine Chemical compound CCCCCCCCN IOQPZZOEVPZRBK-UHFFFAOYSA-N 0.000 description 1
- 239000002674 ointment Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000003002 pH adjusting agent Substances 0.000 description 1
- UKODFQOELJFMII-UHFFFAOYSA-N pentamethyldiethylenetriamine Chemical compound CN(C)CCN(C)CCN(C)C UKODFQOELJFMII-UHFFFAOYSA-N 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 229920006122 polyamide resin Polymers 0.000 description 1
- 229920000570 polyether Polymers 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 229920001451 polypropylene glycol Polymers 0.000 description 1
- XAEFZNCEHLXOMS-UHFFFAOYSA-M potassium benzoate Chemical compound [K+].[O-]C(=O)C1=CC=CC=C1 XAEFZNCEHLXOMS-UHFFFAOYSA-M 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000003449 preventive effect Effects 0.000 description 1
- 150000003139 primary aliphatic amines Chemical class 0.000 description 1
- 239000008213 purified water Substances 0.000 description 1
- HNJBEVLQSNELDL-UHFFFAOYSA-N pyrrolidin-2-one Chemical compound O=C1CCCN1 HNJBEVLQSNELDL-UHFFFAOYSA-N 0.000 description 1
- 150000003242 quaternary ammonium salts Chemical class 0.000 description 1
- 238000010405 reoxidation reaction Methods 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
- 125000006850 spacer group Chemical group 0.000 description 1
- 239000005720 sucrose Substances 0.000 description 1
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 1
- 229920003002 synthetic resin Polymers 0.000 description 1
- 239000000057 synthetic resin Substances 0.000 description 1
- 239000013008 thixotropic agent Substances 0.000 description 1
- ZIBGPFATKBEMQZ-UHFFFAOYSA-N triethylene glycol Chemical compound OCCOCCOCCO ZIBGPFATKBEMQZ-UHFFFAOYSA-N 0.000 description 1
- 238000004506 ultrasonic cleaning Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
- B08B3/04—Cleaning involving contact with liquid
- B08B3/08—Cleaning involving contact with liquid the liquid having chemical or dissolving effect
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
- C11D7/22—Organic compounds
- C11D7/26—Organic compounds containing oxygen
- C11D7/263—Ethers
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
- C11D7/22—Organic compounds
- C11D7/26—Organic compounds containing oxygen
- C11D7/265—Carboxylic acids or salts thereof
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
- C11D7/22—Organic compounds
- C11D7/32—Organic compounds containing nitrogen
- C11D7/3218—Alkanolamines or alkanolimines
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
- C11D7/50—Solvents
- C11D7/5004—Organic solvents
- C11D7/5022—Organic solvents containing oxygen
-
- C11D2111/14—
-
- C11D2111/22—
Description
本発明は、鉛フリーはんだフラックス用洗浄剤組成物、鉛フリーはんだフラックスの洗浄方法に関する。 The present invention relates to a lead-free solder flux cleaning agent composition and a method for cleaning lead-free solder flux.
プリント配線板に電子部品を表面実装する際、一般にはんだ付けが行われる。通常、はんだ付けの際には、はんだ及び母材表面の酸化膜を除去する、あるいははんだ及び母材表面の再酸化を防止し、充分なはんだ付け性を得る目的でフラックスが使用される。しかしながら、フラックスは腐食性であり、フラックス残渣は、プリント配線基板の品質を低下させる。そのため、フラックス残渣は洗浄除去する場合がある。 When surface mounting electronic components on a printed wiring board, soldering is generally performed. Usually, at the time of soldering, a flux is used for the purpose of removing the oxide film on the surface of the solder and the base material, or preventing the reoxidation of the surface of the solder and the base material and obtaining sufficient solderability. However, the flux is corrosive and the flux residue reduces the quality of the printed wiring board. Therefore, the flux residue may be washed and removed.
従来、表面実装部品のはんだ接合には、ロジンベースのフラックス（ロジンフラックス）が広く使用されており、このロジンフラックスの残渣は、フロン等のハロゲン化炭化水素で洗浄されていた。しかしながら、ハロゲン化炭化水素は、環境に対して極めて有害であることからその使用が規制されたため、ロジンフラックス残渣の洗浄剤として、ハロゲン化炭化水素等に代わるものが種々検討されている。例えば、引火の危険、環境への影響等が小さく、ロジンフラックス残渣の溶解力に優れるものとして、ポリオキシアルキレンアルキルエーテル系の非ハロゲン系有機溶剤等を含む洗浄剤が提案されている（特許文献１〜３）。 Conventionally, a rosin-based flux (rosin flux) has been widely used for solder bonding of surface mount components, and the residue of this rosin flux has been washed with a halogenated hydrocarbon such as freon. However, since the use of halogenated hydrocarbons has been restricted because they are extremely harmful to the environment, various alternatives to halogenated hydrocarbons and the like have been studied as cleaning agents for rosin flux residues. For example, a cleaning agent containing a polyoxyalkylene alkyl ether-based non-halogen organic solvent or the like has been proposed as one having a small risk of ignition, an impact on the environment, and an excellent dissolving power of a rosin flux residue (Patent Documents). 1-3).
また、環境問題への対策の一つとして、ハロゲン化炭化水素の代わりに水で洗浄することも検討されている。水洗浄が可能なフラックスとしては、ロジンフラックスのような疎水性のものでなく、ポリエーテル系樹脂等に活性剤、溶剤等を添加した水溶性フラックスがある。水溶性フラックスの残渣は吸湿性を有するため、洗浄が必須である。これは洗浄が必須ではないロジンフラックス残渣とは異なる特徴である。そのため、水溶性フラックスの残渣は、通常は水で洗浄されるが、洗浄が充分でない場合がある。 In addition, as one of the measures against environmental problems, washing with water instead of halogenated hydrocarbons is also being considered. The flux that can be washed with water is not a hydrophobic flux such as rosin flux, but a water-soluble flux obtained by adding an activator, a solvent, or the like to a polyether resin or the like. Since the residue of the water-soluble flux is hygroscopic, cleaning is essential. This is a feature different from rosin flux residues where cleaning is not essential. Therefore, the residue of the water-soluble flux is usually washed with water, but the washing may not be sufficient.
そこで、上記特許文献１〜３等の洗浄剤を水溶性フラックス残渣の洗浄剤として用いることが考えられる。しかし、これらの洗浄剤は水溶性フラックス残渣の除去を目的として検討されたわけではなく、また、水溶性フラックス残渣は、ロジンフラックス残渣と異なる特徴を有するため、上述のロジンフラックス用洗浄剤を用いても水溶性フラックス残渣を充分に洗浄することは困難であった。また、特許文献３の洗浄剤組成物には、アルキル基を有するアルカノールアミンが含有されるが、そのようなアミンは銅板等の金属基板を腐食する問題もあった。 Therefore, it is conceivable to use the cleaning agents of Patent Documents 1 to 3 and the like as the cleaning agent for the water-soluble flux residue. However, these cleaning agents have not been studied for the purpose of removing the water-soluble flux residue, and since the water-soluble flux residue has different characteristics from the rosin flux residue, the above-mentioned cleaning agent for rosin flux is used. However, it was difficult to sufficiently wash the water-soluble flux residue. Further, the cleaning agent composition of Patent Document 3 contains an alkanolamine having an alkyl group, and such an amine also has a problem of corroding a metal substrate such as a copper plate.
本発明は、ロジンフラックス又は水溶性フラックスをはんだ付けする際に生ずるフラックス残渣を短時間で洗浄することができ、さらに被洗浄物が複雑で微細な構造を有する実装基板等である場合にも優れた隙間洗浄性を有する鉛フリーはんだフラックス用洗浄剤組成物を提供することを主な目的とする。 The present invention can clean the flux residue generated when soldering rosin flux or water-soluble flux in a short time, and is also excellent when the object to be cleaned is a mounting substrate or the like having a complicated and fine structure. A main object of the present invention is to provide a cleaning agent composition for a lead-free solder flux having a gap cleaning property.
本発明者は、鋭意検討したところ、特定のグリコールエーテルを含む有機溶剤及びアミンに、ヒドロキシカルボン酸を含有する洗浄剤組成物が前記課題を解決することを見出し、本発明を完成させるに至った。すなわち、本発明は以下の鉛フリーはんだフラックス用洗浄剤組成物、及び鉛フリーはんだフラックスの洗浄方法に関する。 As a result of diligent studies, the present inventor has found that a cleaning agent composition containing a hydroxycarboxylic acid in an organic solvent and an amine containing a specific glycol ether solves the above-mentioned problems, and has completed the present invention. .. That is, the present invention relates to the following cleaning agent composition for lead-free solder flux and a method for cleaning lead-free solder flux.
１．ジエチレングリコールエチルメチルエーテル、ジエチレングリコールジエチルエーテル及びジプロピレングリコールジメチルエーテルからなる群より選ばれる少なくとも１種を含む有機溶剤（Ａ）、下記式（１）で表されるアルカノールアミン（Ｂ）、及びヒドロキシカルボン酸（Ｃ）を含む鉛フリーはんだフラックス用洗浄剤組成物。
２．（Ｂ）成分が、Ｎ，Ｎ−ビス（２−ヒドロキシエチル）−Ｎ−シクロヘキシルアミンである前項１の鉛フリーはんだフラックス用洗浄剤組成物。 2. 2. The cleaning agent composition for lead-free solder flux according to item 1 above, wherein the component (B) is N, N-bis (2-hydroxyethyl) -N-cyclohexylamine.
３．（Ｃ）成分が、クエン酸、イソクエン酸、酒石酸及びリンゴ酸からなる群より選ばれる少なくとも１種である前項１又は２の鉛フリーはんだフラックス用洗浄剤組成物。 3. 3. The cleaning agent composition for lead-free solder flux according to the above item 1 or 2, wherein the component (C) is at least one selected from the group consisting of citric acid, isocitric acid, tartaric acid and malic acid.
４．（Ａ）成分を２．８〜７０重量％、（Ｂ）成分を０.０４〜５重量％、（Ｃ）成分を０．０１〜２重量％、及び水を５〜９７重量％含有する前項１〜３のいずれかの鉛フリーはんだフラックス用洗浄剤組成物。 4. The above item contains 2.8 to 70% by weight of the component (A), 0.04 to 5% by weight of the component (B), 0.01 to 2% by weight of the component (C), and 5 to 97% by weight of water. Cleaning agent composition for lead-free solder flux according to any one of 1 to 3.
５．温度２５℃における表面張力が１０〜６０ｄｙｎｅ／ｃｍである前項１〜４のいずれかの鉛フリーはんだフラックス用洗浄剤組成物。 5. The cleaning agent composition for lead-free solder flux according to any one of the above items 1 to 4, wherein the surface tension at a temperature of 25 ° C. is 10 to 60 dyne / cm.
６．前項１〜５のいずれかの鉛フリーはんだフラックス用洗浄剤組成物を、鉛フリーはんだフラックスが付着した被洗浄物に接触させて洗浄する、鉛フリーはんだフラックスの洗浄方法。 6. A method for cleaning a lead-free solder flux, wherein the cleaning agent composition for the lead-free solder flux according to any one of the above items 1 to 5 is brought into contact with an object to be cleaned to which the lead-free solder flux is attached.
本発明の鉛フリーはんだフラックス用洗浄剤組成物（以下、洗浄剤組成物ともいう）によれば、ロジンフラックス又は水溶性フラックスをはんだ付けする際に生じるフラックス残渣を短時間で洗浄でき、また被洗浄物が複雑で微細な構造を有する実装基板等である場合にも優れた隙間洗浄性を有する。更に前記洗浄剤組成物は金属基板を腐食させない効果も有する。 According to the lead-free solder flux cleaning agent composition of the present invention (hereinafter, also referred to as a cleaning agent composition), the flux residue generated when soldering a rosin flux or a water-soluble flux can be cleaned in a short time, and the surface is coated. It also has excellent gap cleaning properties even when the object to be cleaned is a mounting substrate or the like having a complicated and fine structure. Further, the cleaning agent composition also has an effect of not corroding the metal substrate.
本発明の洗浄剤組成物の洗浄対象である「鉛フリーはんだフラックス」とは、具体的には、鉛フリーはんだに由来する錫を含むフラックス残渣を意味し、例えば、（ア）粉状の鉛フリーはんだとフラックス組成物とからなるペーストではんだ付けした後に生ずるフラックス残渣や、（イ）鉛フリーはんだで形成された電極を、フラックス組成物を介してはんだ付けした後に生ずるフラックス残渣が挙げられる。 The "lead-free solder flux" to be cleaned of the cleaning agent composition of the present invention specifically means a flux residue containing tin derived from lead-free solder, for example, (a) powdery lead. Examples thereof include a flux residue generated after soldering with a paste composed of free solder and a flux composition, and (a) a flux residue generated after soldering an electrode formed of lead-free solder through a flux composition.
なお、「鉛フリーはんだ」としては、例えば、Ｓｎ−Ａｇ系はんだ、Ｓｎ−Ｃｕ系はんだ、Ｓｎ−Ａｇ−Ｃｕ系はんだ、Ｓｎ−Ｚｎ系はんだ、Ｓｎ−Ｓｂ系はんだ等が挙げられる。 Examples of the "lead-free solder" include Sn-Ag-based solder, Sn-Cu-based solder, Sn-Ag-Cu-based solder, Sn-Zn-based solder, Sn-Sb-based solder, and the like.
また、「フラックス組成物」としては、具体的には、例えば、樹脂酸類（天然ロジン、重合ロジン、α，β不飽和カルボン酸変性ロジン等）や合成樹脂類（アクリル樹脂、ポリアミド樹脂等）などのベース樹脂、活性剤（アジピン酸等の有機酸、ジエチルアミン臭化水素銀等のハロゲン系化合物等）、チキソトロピック剤（硬化ひまし油、ヒドロキシステアリン酸エチレンビスアミド等）、溶剤（ジエチレングリコールモノヘキシルエーテル、ジエチレングリコールモノブチルエーテル等）を主成分とする組成物が挙げられる。 Specifically, the "flux composition" includes, for example, resin acids (natural rosin, polymerized rosin, α, β unsaturated carboxylic acid-modified rosin, etc.), synthetic resins (acrylic resin, polyamide resin, etc.) and the like. Base resin, activator (organic acid such as adipic acid, halogen compound such as diethylamine hydrogen bromide), thixotropic agent (hardened castor oil, ethylene bisamide hydroxystearate, etc.), solvent (diethylene glycol monohexyl ether, diethylene glycol) Examples thereof include compositions containing monobutyl ether or the like as a main component.
本発明の洗浄剤組成物は、ジエチレングリコールエチルメチルエーテル、ジエチレングリコールジエチルエーテル及びジプロピレングリコールジメチルエーテルからなる群より選ばれる少なくとも１種を含む有機溶剤（Ａ）（以下、（Ａ）成分という）、下記式（１）で表されるアミン（Ｂ）（以下、（Ｂ）成分という）、及びヒドロキシカルボン酸（Ｃ）（以下、（Ｃ）成分という）を含むものである。 The cleaning agent composition of the present invention contains an organic solvent (A) containing at least one selected from the group consisting of diethylene glycol ethyl methyl ether, diethylene glycol diethyl ether and dipropylene glycol dimethyl ether (hereinafter referred to as component (A)), the following formula. It contains the amine (B) represented by (1) (hereinafter referred to as the component (B)) and the hydroxycarboxylic acid (C) (hereinafter referred to as the component (C)).
（Ａ）成分としては、ジエチレングリコールエチルメチルエーテル、ジエチレングリコールジエチルエーテル及びジプロピレングリコールジメチルエーテルからなる群より選ばれる少なくとも１種を含む。これらのジアルキルジアルキレングリコールは、表面張力及び粘度が低いため、基板の隙間に入りやすい傾向がある。 The component (A) contains at least one selected from the group consisting of diethylene glycol ethyl methyl ether, diethylene glycol diethyl ether and dipropylene glycol dimethyl ether. Since these dialkyldialkylene glycols have low surface tension and viscosity, they tend to easily enter the gaps of the substrate.
また、（Ａ）成分としては、隙間洗浄性を損なわない限り、他のグリコールエーテルを併用しても良い。他のグリコールエーテルとしては、特に限定されないが、例えば、ジエチレングリコールモノメチルエーテル、ジエチレングリコールジメチルエーテル、ジエチレングリコールモノエチルエーテル、ジエチレングリコールモノｎ−プロピルエーテル、ジエチレングリコールジｎ−プロピルエーテル、ジエチレングリコールメチルプロピルエーテル、ジエチレングリコールエチルプロピルエーテル、ジエチレングリコールモノｎ−ブチルエーテル、ジエチレングリコールジｎ−ブチルエーテル、ジエチレングリコールメチルブチルエーテル、ジエチレングリコールエチルブチルエーテル、ジエチレングリコールプロピルブチルエーテル、ジエチレングリコールモノｎ−ペンチルエーテル、ジエチレングリコールジｎ−ペンチルエーテル、ジエチレングリコールメチルペンチルエーテル、ジエチレングリコールエチルペンチルエーテル、ジエチレングリコールプロピルペンチルエーテル、ジエチレングリコールブチルペンチルエーテル、ジエチレングリコールモノｎ−ヘキシルエーテル等のジエチレングリコールエーテル類；ジプロピレングリコールモノメチルエーテル、これらに対応するトリもしくはテトラエチレングリコールエーテル類等が挙げられ、これらは１種を単独で、または２種以上を組み合わせて用いることができ、その含有量も特に限定されないが、本発明の洗浄剤組成物を１００重量％として、４０重量％以下が好ましい。 Further, as the component (A), another glycol ether may be used in combination as long as the gap cleaning property is not impaired. The other glycol ether is not particularly limited, but for example, diethylene glycol monomethyl ether, diethylene glycol dimethyl ether, diethylene glycol monoethyl ether, diethylene glycol mono n-propyl ether, diethylene glycol din-propyl ether, diethylene glycol methylpropyl ether, diethylene glycol ethylpropyl ether, etc. Diethylene glycol mono n-butyl ether, diethylene glycol din-butyl ether, diethylene glycol methyl butyl ether, diethylene glycol ethyl butyl ether, diethylene glycol propyl butyl ether, diethylene glycol mono n-pentyl ether, diethylene glycol di n-pentyl ether, diethylene glycol methyl pentyl ether, diethylene glycol ethyl pentyl ether, diethylene glycol propyl Diethylene glycol ethers such as pentyl ether, diethylene glycol butyl pentyl ether, diethylene glycol mono n-hexyl ether; dipropylene glycol monomethyl ether, corresponding tri or tetraethylene glycol ethers, etc. may be mentioned, and these may be used alone. Alternatively, two or more kinds can be used in combination, and the content thereof is not particularly limited, but the cleaning agent composition of the present invention is preferably 100% by weight, preferably 40% by weight or less.
（Ａ）成分の含有量としては、特に限定されないが、隙間洗浄性の点から、通常は本発明の洗浄剤組成物を１００重量％として、２．８〜７０重量％、好ましくは５〜７０重量％、より好ましくは２０〜７０重量％である。 The content of the component (A) is not particularly limited, but from the viewpoint of crevice cleaning property, the cleaning agent composition of the present invention is usually 100% by weight, 2.8 to 70% by weight, preferably 5 to 70% by weight. By weight%, more preferably 20-70% by weight.
（Ｂ）成分は、下記式（１）で表されるアルカノールアミンであり、金属基板を腐食せず、かつフラックスの洗浄性も発揮するために必要な成分である。 The component (B) is an alkanolamine represented by the following formula (1), which is a component necessary for not corroding the metal substrate and exhibiting the detergency of the flux.
（ｎは１〜３の整数、Ｒは炭素数１〜４のアルキル基又はヒドロキシアルキル基を表す） (N represents an integer of 1 to 3, R represents an alkyl group or a hydroxyalkyl group having 1 to 4 carbon atoms)
前記式（１）で表されるアルカノールアミンとしては、例えば、Ｎ−ヒドロキシエチルーＮ−メチルーＮ−シクロヘキシルアミン、Ｎ−エチルーＮ−（２−ヒドロキシエチル）−Ｎ−シクロヘキシルアミン、Ｎ，Ｎ−ビス（２−ヒドロキシメチル）−Ｎ−シクロヘキシルアミン、Ｎ，Ｎ−ビス（２−ヒドロキシエチル）−Ｎ−シクロヘキシルアミン等が挙げられる。これらは単独でも２種以上を組み合わせても良い。これらの中でも、隙間洗浄性の点から、Ｎ，Ｎ−ビス（２−ヒドロキシエチル）−Ｎ−シクロヘキシルアミンが好ましい。 Examples of the alkanolamine represented by the formula (1) include N-hydroxyethyl-N-methyl-N-cyclohexylamine, N-ethyl-N- (2-hydroxyethyl) -N-cyclohexylamine, N, N-. Examples thereof include bis (2-hydroxymethyl) -N-cyclohexylamine and N, N-bis (2-hydroxyethyl) -N-cyclohexylamine. These may be used alone or in combination of two or more. Among these, N, N-bis (2-hydroxyethyl) -N-cyclohexylamine is preferable from the viewpoint of crevice cleaning property.
（Ｂ）成分の含有量としては、特に限定されないが、隙間洗浄性の点から、通常は本発明の洗浄剤組成物を１００重量％として、０．０４〜５重量％、好ましくは０．０４〜３重量％、より好ましくは０．１〜２重量％である。 The content of the component (B) is not particularly limited, but from the viewpoint of crevice cleaning property, the cleaning agent composition of the present invention is usually 100% by weight, 0.04 to 5% by weight, preferably 0.04. It is ~ 3% by weight, more preferably 0.1 to 2% by weight.
本発明の洗浄剤組成物は、（Ｂ）成分以外のアルカノールアミン（Ｂ−１）（以下、（Ｂ−１）成分という）、又は脂肪族アミン（Ｂ−２）（以下、（Ｂ−２）成分という）等を併用しても良い。（Ｂ−１）成分としては、特に限定されないが、例えば、ジエタノールアミン、Ｎ−メチルジエタノールアミン、Ｎ−エチルジエタノールアミン、Ｎ−ｎ−ブチルジエタノールアミン、Ｎ−ｔ−ブチルジエタノールアミン、トリエタノールアミン、Ｎ−（β−アミノエチル）エタノールアミン、Ｎ−（β−アミノエチル）イソプロパノールアミン等が挙げられる。また（Ｂ−２）成分としては、特に限定されないが、例えば、オクチルアミン、デシルアミン、ドデシルアミン、テトラデシルアミン、ヘキサデシルアミン、２−エチルヘキシルアミン等の第１級脂肪族アミン、Ｎ，Ｎ，Ｎ’，Ｎ’−テトラメチルペンタメチレンジアミン、Ｎ，Ｎ，Ｎ’，Ｎ’−テトラエチルペンタメチレンジアミン、Ｎ，Ｎ，Ｎ’，Ｎ’−テトライソプロピルペンタメチレンジアミン、Ｎ，Ｎ，Ｎ’，Ｎ’−テトラ−ｎ−プロピルペンタメチレンジアミン、Ｎ，Ｎ，Ｎ’，Ｎ’−テトラメチルヘキサメチレンジアミン、Ｎ，Ｎ，Ｎ’，Ｎ’−テトラエチルヘキサメチレンジアミン、Ｎ，Ｎ，Ｎ’，Ｎ’−テトライソプロピルヘキサメチレンジアミン、Ｎ，Ｎ，Ｎ’，Ｎ’−テトラ−ｎ−プロピルヘキサメチレンジアミン等の第３級ジアミン；ビス（２−ジメチルアミノエチル）エーテル、ビス（２−ジエチルアミノエチル）エーテル、ビス（２−ジイソプロピルアミノエチル）エーテル、ビス（２−ジ−ｎ−プロピルアミノエチル）エーテル等のジアミノアルキルエーテル；１，１，７，７−テトラメチルジエチレントリアミン、１，１，７，７−テトラエチルジエチレントリアミン、１，１，７，７−テトライソプロピルジエチレントリアミン、１，１，７，７−テトラ−ｎ−プロピルジエチレントリアミン、Ｎ，Ｎ，Ｎ’，Ｎ’’，Ｎ’’−ペンタメチルジエチレントリアミン、４−メチル−１，１，７，７−テトラエチルジエチレントリアミン、４−メチル−１，１，７，７−テトライソプロピルジエチレントリアミン、４−メチル−１，１，７，７−テトラ−ｎ−プロピルジエチレントリアミン等のトリアミン等が挙げられる。これらは単独でも２種以上を組み合わせても良い。（Ｂ−１）成分及び（Ｂ−２）成分の含有量としては、特に限定されないが、金属基板を腐食させない点から、本発明の洗浄剤組成物を１００重量％として、２重量％以下にすることが好ましい。 The cleaning composition of the present invention comprises an alkanolamine (B-1) other than the component (B) (hereinafter referred to as a component (B-1)) or an aliphatic amine (B-2) (hereinafter, (B-2). ) Ingredients) and the like may be used in combination. The component (B-1) is not particularly limited, but is, for example, diethanolamine, N-methyldiethanolamine, N-ethyldiethanolamine, Nn-butyldiethanolamine, Nt-butyldiethanolamine, triethanolamine, N- (β). Examples thereof include −aminoethyl) ethanolamine and N- (β-aminoethyl) isopropanolamine. The component (B-2) is not particularly limited, but for example, primary aliphatic amines such as octylamine, decylamine, dodecylamine, tetradecylamine, hexadecylamine, and 2-ethylhexylamine, N, N, N', N'-tetramethylpentamethylenediamine, N, N, N', N'-tetraethylpentamethylenediamine, N, N, N', N'-tetraisopropylpentamethylenediamine, N, N, N', N'-Tetra-n-propylpentamethylenediamine, N, N, N', N'-tetramethylhexamethylenediamine, N, N, N', N'-tetraethylhexamethylenediamine, N, N, N', Tertiary diamines such as N'-tetraisopropylhexamethylenediamine, N, N, N', N'-tetra-n-propylhexamethylenediamine; bis (2-dimethylaminoethyl) ether, bis (2-diethylaminoethyl) ) Diaminoalkyl ethers such as ethers, bis (2-diisopropylaminoethyl) ethers, bis (2-di-n-propylaminoethyl) ethers; 1,1,7,7-tetramethyldiethylenetriamines, 1,1,7, 7-Tetraethyldiethylenetriamine, 1,1,7,7-tetraisopropyldiethylenetriamine, 1,1,7,7-tetra-n-propyldiethylenetriamine, N, N, N', N'', N''-pentamethyldiethylenetriamine , 4-Methyl-1,1,7,7-Tetraethyldiethylenetriamine, 4-Methyl-1,1,7,7-Tetraisopropyldiethylenetriamine, 4-Methyl-1,1,7,7-Tetra-n-propyldiethylenetriamine Such as triamine and the like. These may be used alone or in combination of two or more. The contents of the component (B-1) and the component (B-2) are not particularly limited, but from the viewpoint of not corroding the metal substrate, the cleaning agent composition of the present invention is set to 100% by weight and is 2% by weight or less. It is preferable to do so.
（Ｃ）成分としては、特に限定されず各種公知のものを使用でき、例えば、クエン酸、イソクエン酸、リンゴ酸、酒石酸等が挙げられる。また前記酸の塩を用いてもよく、塩としてはナトリウム塩、カリウム塩、アンモニウム塩、アルカノールアミン塩等が挙げられる。これらは単独でも２種以上を組み合わせても良い。これらの中でも、フラックス残渣洗浄性の点から、クエン酸、イソクエン酸及びリンゴ酸からなる群より選ばれる少なくとも１種が好ましく、クエン酸がより好ましい。 The component (C) is not particularly limited, and various known substances can be used, and examples thereof include citric acid, isocitric acid, malic acid, and tartaric acid. Further, the salt of the acid may be used, and examples of the salt include sodium salt, potassium salt, ammonium salt, alkanolamine salt and the like. These may be used alone or in combination of two or more. Among these, at least one selected from the group consisting of citric acid, isocitric acid and malic acid is preferable, and citric acid is more preferable, from the viewpoint of flax residue detergency.
（Ｃ）成分の含有量としては、特に限定されないがフラックス残渣溶解性の点から、通常は本発明の洗浄剤組成物を１００重量％として、０．０１〜２重量％、好ましくは０．１〜２重量％、より好ましくは０．１〜１重量％である。 The content of the component (C) is not particularly limited, but from the viewpoint of flux residue solubility, the cleaning composition of the present invention is usually 100% by weight, 0.01 to 2% by weight, preferably 0.1. It is ~ 2% by weight, more preferably 0.1 to 1% by weight.
本発明の洗浄剤組成物は、更に水を含有するものでもある。水としては、例えば純水、イオン交換水、精製水等が挙げられる。また、水の混合については１回でも複数回に分けても良い。水の含有量も特に限定されないが、洗浄剤の非危険物化の点から、通常は本発明の洗浄剤組成物を１００重量％として、５〜９７重量％、好ましくは２０〜９０重量％、より好ましくは２０〜５０重量％である。 The cleaning agent composition of the present invention also contains water. Examples of water include pure water, ion-exchanged water, purified water and the like. Further, the mixing of water may be divided into once or a plurality of times. The content of water is also not particularly limited, but from the viewpoint of non-hazardous substances of the cleaning agent, usually, the cleaning agent composition of the present invention is 100% by weight, and is 5 to 97% by weight, preferably 20 to 90% by weight. It is preferably 20 to 50% by weight.
また、本発明の洗浄剤組成物には、必要に応じて非ハロゲン系有機溶剤を含有させても良く、例えば、１，３−ジメチル−２−イミダゾリジノン、１，３−ジエチル−２−イミダゾリジノン、１，３−ジプロピル−２−イミダゾリジノン、Ｎ−メチル−２−ピロリドン等の窒素原子を含有する溶剤；ヘキサン、ヘプタン、オクタン等の炭化水素；メタノール、エタノール、ベンジルアルコール等のアルコール；アセトン、メチルエチルケトン等のケトン；ジエチルエーテル、テトラヒドロフラン、グリコールエーテル類等のエーテル；酢酸エチル、酢酸メチル等のエステル等が挙げられ、これらは単独でも２種以上を組み合わせても良い。 Further, the cleaning agent composition of the present invention may contain a non-halogen organic solvent, if necessary, for example, 1,3-dimethyl-2-imidazolidinone, 1,3-diethyl-2-. Solvents containing nitrogen atoms such as imidazolidinone, 1,3-dipropyl-2-imidazolidinone, N-methyl-2-pyrrolidone; hydrocarbons such as hexane, heptane, octane; methanol, ethanol, benzyl alcohol, etc. Examples include alcohol; ketones such as acetone and methyl ethyl ketone; ethers such as diethyl ether, tetrahydrofuran and glycol ethers; esters such as ethyl acetate and methyl acetate, and these may be used alone or in combination of two or more.
なお、本発明の洗浄剤組成物には、本発明の所期の効果を損なわない程度において、各種公知の添加剤、例えばノニオン性界面活性剤（（Ａ）成分に相当するものを除く）、アニオン性界面活性剤、カチオン性界面活性剤等の各種界面活性剤等を添加しても良い。 The cleaning composition of the present invention includes various known additives such as nonionic surfactants (excluding those corresponding to the component (A)) to the extent that the intended effects of the present invention are not impaired. Various surfactants such as anionic surfactants and cationic surfactants may be added.
ノニオン性界面活性剤としては、例えば、一般式（２）：Ｒ２−Ｏ−（ＣＨ２−ＣＨ２−Ｏ）ｅ−Ｈ（式中、Ｒ２は炭素数８〜２０のアルキル基を、ｅは０〜２０の整数を表す。）で表される化合物や、脂肪酸アミドのエチレンオキサイド付加物、ソルビタン脂肪酸エステル、ショ糖脂肪酸エステル、脂肪酸アルカノールアミド、これらの対応するポリオキシプロピレン系界面活性剤等が挙げられ、これらは単独でも２種以上を組み合わせても良い。 The nonionic surfactant includes, for example, the general formula (2): R 2 -O- ( CH 2 -CH 2 -O) e-H ( wherein, R 2 is an alkyl group having 8 to 20 carbon atoms, e represents an integer from 0 to 20), ethylene oxide adducts of fatty acid amides, sorbitan fatty acid esters, sucrose fatty acid esters, fatty acid alkanolamides, and their corresponding polyoxypropylene-based surfactants. Etc., and these may be used alone or in combination of two or more.
アニオン性界面活性剤としては、例えば、硫酸エステル系アニオン性界面活性剤（高級アルコールの硫酸エステル塩、アルキル硫酸エステル塩、ポリオキシエチレンアルキル硫酸エステル塩等）、スルホン酸塩系アニオン性界面活性剤（アルキルスルホン酸塩、アルキルベンゼンスルホン酸塩等）等が挙げられ、これらは単独でも２種以上を組み合わせても良い。 Examples of the anionic surfactant include sulfate ester-based anionic surfactants (sulfate ester salts of higher alcohols, alkyl sulfate ester salts, polyoxyethylene alkyl sulfate ester salts, etc.), and sulfonate-based anionic surfactants. (Alkyl sulfonate, alkyl benzene sulfonate, etc.) and the like can be mentioned, and these may be used alone or in combination of two or more.
カチオン性界面活性剤としては、例えば、アルキル化アンモニウム塩、４級アンモニウム塩等が挙げられ、これらは単独でも２種以上を組み合わせても良い。 Examples of the cationic surfactant include alkylated ammonium salts and quaternary ammonium salts, which may be used alone or in combination of two or more.
両性界面活性剤としては、アミノ酸型、ベタイン型両性界面活性剤等が挙げられ、これらは単独でも２種以上を組み合わせても良い。 Examples of the amphoteric tenside include amino acid type and betaine type amphoteric tenside agents, and these may be used alone or in combination of two or more.
本発明の洗浄剤組成物には、各種公知の添加剤を配合しても良い。添加剤としては特に限定されないが、例えば、キレート剤、酸化防止剤、酸化還元剤、スケール防止剤、防錆剤、ｐＨ調整剤、消泡剤等が挙げられる。 Various known additives may be added to the cleaning composition of the present invention. The additive is not particularly limited, and examples thereof include a chelating agent, an antioxidant, an oxidation reducing agent, an antioxidant, a rust preventive, a pH adjuster, and an antifoaming agent.
本発明の洗浄剤組成物の物性としては、特に限定されないが、例えば、表面張力が温度２５℃で、通常１０〜６０ｄｙｎｅ／ｃｍ程度であり、好ましくは１０〜５０ｄｙｎｅ／ｃｍ程度であり、より好ましくは１０〜４０ｄｙｎｅ／ｃｍである。表面張力が当該範囲とすることで、隙間洗浄性が良好となりやすい。 The physical properties of the cleaning agent composition of the present invention are not particularly limited, but for example, the surface tension is usually about 10 to 60 dyne / cm at a temperature of 25 ° C., preferably about 10 to 50 dyne / cm, more preferably. Is 10 to 40 dyne / cm. By setting the surface tension within this range, the gap cleaning property tends to be good.
また、本発明の洗浄剤組成物は引火点を有さず、非危険物である。 Further, the cleaning agent composition of the present invention does not have a flash point and is a non-dangerous substance.
また、本発明の洗浄剤組成物には、必要に応じて該（Ａ）成分以外の非ハロゲン系有機溶剤を含有させることができる。例えば、窒素含有化合物系溶剤（１，３−ジメチル−２−イミダゾリジノン、１，３−ジエチル−２−イミダゾリジノン、１，３−ジプロピル−２−イミダゾリジノン、Ｎ−メチル−２−ピロリドン等）、炭化水素系溶剤（ヘキサン、ヘプタン、オクタン等）、アルコール系溶剤（メタノール、エタノール、ベンジルアルコール等）、ケトン系溶剤（アセトン、メチルエチルケトン等）、エーテル系溶剤（ジエチルエーテル、テトラヒドロフラン、グリコールエーテル類等）、エステル系溶剤（酢酸エチル、酢酸メチル等）等が挙げられ、これらは単独でも２種以上を組み合わせても良い。 In addition, the cleaning agent composition of the present invention may contain a non-halogen organic solvent other than the component (A), if necessary. For example, nitrogen-containing compound solvents (1,3-dimethyl-2-imidazolidinone, 1,3-diethyl-2-imidazolidinone, 1,3-dipropyl-2-imidazolidinone, N-methyl-2-. Pyrrolidone, etc.), hydrocarbon solvents (hexane, heptane, octane, etc.), alcohol solvents (methanol, ethanol, benzyl alcohol, etc.), ketone solvents (acetone, methyl ethyl ketone, etc.), ether solvents (diethyl ether, tetrahydrofuran, glycol, etc.) (Ethers, etc.), ester solvents (ethyl acetate, methyl acetate, etc.) and the like can be mentioned, and these may be used alone or in combination of two or more.
＜鉛フリーはんだフラックスの除去方法＞
本発明の鉛フリーはんだフラックスの除去方法は、本発明の洗浄剤組成物を鉛フリーハンダフラックスが付着した被洗浄物に接触させることにより、前記フラックスを除去できるものである。
<How to remove lead-free solder flux>
The method for removing lead-free solder flux of the present invention can remove the flux by bringing the cleaning agent composition of the present invention into contact with an object to be cleaned to which lead-free solder flux is attached.
本発明の洗浄剤組成物の利用態様は特に限定されず、各種公知の方法を採用できる。例えば、スプレー装置を使用して洗浄剤組成物を鉛フリーハンダフラックスが付着した被洗浄物にスプレーで吹き付ける方法（特開２００７−０９６１２７号公報参照）、洗浄剤組成物に被洗浄物を浸漬して超音波洗浄する方法、直通式洗浄装置（登録商標「ダイレクトパス」、荒川化学工業（株）製、特許第２６２１８００号等）を用いる方法等が挙げられる。 The mode of use of the cleaning agent composition of the present invention is not particularly limited, and various known methods can be adopted. For example, a method of spraying the cleaning agent composition onto the object to be cleaned to which lead-free solder flux is attached using a spray device (see Japanese Patent Application Laid-Open No. 2007-09612), and immersing the cleaning agent composition in the cleaning agent composition. A method of ultrasonic cleaning, a method of using a direct cleaning device (registered trademark "Direct Path", manufactured by Arakawa Chemical Industry Co., Ltd., Patent No. 2621800, etc.) and the like can be mentioned.
本発明の洗浄剤組成物を用いて鉛フリーハンダフラックスを除去した後、得られた洗浄物は水で濯がれることが好ましい。特に、本発明の除去方法としては、本発明の洗浄剤組成物を、鉛フリーハンダフラックスにスプレー吹き付けすることにより洗浄物を得た後、当該洗浄物に水をスプレー吹き付けする方法が好ましい。 After removing the lead-free solder flux using the cleaning agent composition of the present invention, it is preferable that the obtained cleaning product is rinsed with water. In particular, as the removal method of the present invention, a method of spraying the cleaning agent composition of the present invention onto a lead-free solder flux to obtain a cleaning product and then spraying water onto the cleaning product is preferable.
また、濯ぎ処理は、複数回繰り返し行ってもよい。例えば、前記洗浄物に対して、プレ濯ぎ処理した後、仕上げの濯ぎ処理を行うことにより、洗浄物表面に付着した洗浄剤組成物を効果的に除去できる。 Moreover, the rinsing treatment may be repeated a plurality of times. For example, the cleaning agent composition adhering to the surface of the cleaning product can be effectively removed by performing a finishing rinsing treatment after the pre-rinsing treatment on the cleaning product.
プレ濯ぎ処理は、純水等を用いた従来のプレすすぎ処理の方法に準じて行えばよい。 The pre-rinsing treatment may be performed according to the conventional pre-rinsing treatment method using pure water or the like.
仕上げすすぎ処理は、従来の方法に従って行えばよい。例えば、プレすすぎ処理物に対して純水等を用いて処理する方法が挙げられる。 The finish rinsing process may be performed according to a conventional method. For example, a method of treating the pre-rinsed product with pure water or the like can be mentioned.
プレすすぎ処理後及び／又は仕上げすすぎ処理後に、必要に応じて乾燥処理を行っても良い。 After the pre-rinse treatment and / or after the finish rinse treatment, a drying treatment may be performed if necessary.
なお、濯ぎ工程が、当該被洗浄物に水をスプレー吹き付けする態様で行われる場合には、低発泡性の観点より、本発明の洗浄剤組成物としては、前記の各種界面活性剤を含まない方が好ましい。 When the rinsing step is performed by spraying water onto the object to be cleaned, the cleaning composition of the present invention does not contain the above-mentioned various surfactants from the viewpoint of low foaming property. Is preferable.
以下、本発明を、実施例及び比較例を通じて詳細に説明するが、それらによって本発明の範囲が制限されないことはもとよりである。 Hereinafter, the present invention will be described in detail through Examples and Comparative Examples, but it goes without saying that the scope of the present invention is not limited by them.
（鉛フリーはんだフラックス用洗浄剤組成物の調製）
表１に示す各成分を混合し（重量％基準）、実施例１〜１０及び比較例１〜６の鉛フリーはんだフラックス用洗浄剤組成物を調製した。
(Preparation of cleaning agent composition for lead-free solder flux)
Each component shown in Table 1 was mixed (based on weight%) to prepare a cleaning agent composition for lead-free solder flux of Examples 1 to 10 and Comparative Examples 1 to 6.
［金属基板の腐食（変色の有無確認）］
２００ｍｌのビーカーに。実施例１の鉛フリーはんだフラックス用洗浄剤組成物を１５０ｇ採り、アルミ板（アルミ板Ａ１０５０Ｐ（ＪＩＳ Ｈ３１００に規定）、寸法：７０ｍｍ×１５０ｍｍ×０．８ｍｍ）を入れ、６０℃で１０分間浸漬させた。冷却後、アルミ板を取り出し、よく水洗した後、窒素ブローにて液滴を除去した。アルミ板の変色有無を目視で確認した。また、実施例２〜１０、および比較例１〜６の鉛フリーはんだフラックス用洗浄剤組成物についても同様に評価した。結果を表１に示す（以下同様）。
（評価基準）
○：アルミ板の変色がない ×：アルミ板の変色がある
[Corrosion of metal substrate (confirmation of discoloration)]
In a 200 ml beaker. Take 150 g of the lead-free solder flux cleaning agent composition of Example 1, put an aluminum plate (aluminum plate A1050P (specified in JIS H3100), dimensions: 70 mm x 150 mm x 0.8 mm), and soak at 60 ° C. for 10 minutes. It was. After cooling, the aluminum plate was taken out, washed well with water, and then droplets were removed by blowing nitrogen. The presence or absence of discoloration of the aluminum plate was visually confirmed. Further, the cleaning agent compositions for lead-free solder flux of Examples 2 to 10 and Comparative Examples 1 to 6 were also evaluated in the same manner. The results are shown in Table 1 (the same applies hereinafter).
(Evaluation criteria)
◯: No discoloration of aluminum plate ×: Discoloration of aluminum plate
〔水溶性フラックス残渣の作製〕
市販の水溶性フラックス（製品名「ＷＦ−６３１７」、千住金属工業（株）製）３０重量部と、鉛フリーはんだ粉末（９６．５Ｓｎ３．０Ａｇ０．５Ｃｕ、２０−３８μｍ、三井金属鉱業（株）製）７０重量部を混合しソルダペーストを調製した。前記ソルダペーストを軟膏缶に入れ、温度２７０℃のホットプレート上で加熱溶融させた後、冷却し、ソルダペーストから分離した水溶性フラックス残渣を採取した。前記フラックス残渣を鉛フリー水溶性はんだではんだ付けした後に生じた残渣のモデルとして用いた。
[Preparation of water-soluble flux residue]
30 parts by weight of commercially available water-soluble flux (product name "WF-6317", manufactured by Senju Metal Industry Co., Ltd.) and lead-free solder powder (96.5 Sn3.0Ag 0.5Cu, 20-38 μm, Mitsui Mining & Smelting Co., Ltd.) (Manufactured) 70 parts by weight was mixed to prepare a solder paste. The solder paste was placed in an ointment can, heated and melted on a hot plate at a temperature of 270 ° C., cooled, and the water-soluble flux residue separated from the solder paste was collected. The flux residue was used as a model of the residue generated after soldering with lead-free water-soluble solder.
前記フラックス残渣の一部を採取し、波長分散型蛍光Ｘ線分析装置（製品名「ＺＳＸ１００ｅ」、（株）リガク製）を用いて錫濃度を測定した。結果、５重量％となる錫が検出された。 A part of the flux residue was collected, and the tin concentration was measured using a wavelength dispersive fluorescent X-ray analyzer (product name "ZSX100e", manufactured by Rigaku Co., Ltd.). As a result, 5% by weight of tin was detected.
〔洗浄用モデル基板の作製〕
土台のガラスエポキシ基板（縦４０ｃｍ×横４０ｃｍ×厚み１ｍｍ）上に、高さ３０μｍとなるレジストバンプを数個形成しスペーサーとなるガラス小板（縦１６ｃｍ×横１６ｃｍ×厚み０．５ｍｍ）を１枚上から接着することにより隙間洗浄用の基板を形成した。その後、当該ガラス小板間の凹部に前記水溶性フラックス残渣をメタノールで濃度１５％に希釈した液を１０μｌ供給し、洗浄用モデル基板を作製した。
[Preparation of model substrate for cleaning]
On the base glass epoxy substrate (length 40 cm x width 40 cm x thickness 1 mm), a glass small plate (length 16 cm x width 16 cm x thickness 0.5 mm) that serves as a spacer by forming several resist bumps with a height of 30 μm is 1 A substrate for cleaning the gap was formed by adhering from the top of the sheet. Then, 10 μl of a solution obtained by diluting the water-soluble flux residue with methanol to a concentration of 15% was supplied to the recesses between the glass plates to prepare a model substrate for cleaning.
〔隙間洗浄性〕
前記モデル基板を実施例１の鉛フリーはんだフラックス用洗浄剤組成物（液温５０℃）でスプレー洗浄（圧力０．２ＭＰａ、温度５０℃、１分）した。水を用いたスプレー洗浄（圧力は０．２ＭＰａ、１分）で基板を濯ぎ、窒素ブローにて液滴を除去した後、８０℃の循風乾燥機で１０分間乾燥させた。乾燥後の基板に残ったフラックス残渣を光学顕微鏡（（株）キーエンス製 ＶＨＸ６０００）で観察した。評価基準を以下に示す。また、実施例２〜１０、および比較例１〜６の鉛フリーはんだフラックス用洗浄剤組成物についても同様に評価した。
（評価基準）
◎：フラックス残渣がない（図１参照）
○：フラックス残渣が若干あるが、基板の電気的信頼性に影響を及ぼさないレベル
△：フラックス残渣が若干あり、基板の電気的信頼性に若干影響を及ぼすレベル
×：フラックス残渣がある（図２参照）
[Gap cleaning property]
The model substrate was spray-cleaned (pressure 0.2 MPa, temperature 50 ° C., 1 minute) with the lead-free solder flux cleaning agent composition (liquid temperature 50 ° C.) of Example 1. The substrate was rinsed by spray washing with water (pressure: 0.2 MPa, 1 minute), droplets were removed by nitrogen blowing, and then dried in a circulation dryer at 80 ° C. for 10 minutes. The flux residue remaining on the substrate after drying was observed with an optical microscope (VHX6000 manufactured by KEYENCE CORPORATION). The evaluation criteria are shown below. Further, the cleaning agent compositions for lead-free solder flux of Examples 2 to 10 and Comparative Examples 1 to 6 were also evaluated in the same manner.
(Evaluation criteria)
⊚: No flux residue (see Fig. 1)
◯: Level where there is some flux residue but does not affect the electrical reliability of the substrate Δ: Level where there is some flux residue and slightly affects the electrical reliability of the substrate ×: There is flux residue (Fig. 2) reference)
表１における略称は、以下の化合物を示す。
・ＤＥＤＧ：ジエチレングリコールジエチルエーテル
・ＭＥＤＧ：ジエチレングリコールエチルメチルエーテル
・ＤＰＤＭ：ジプロピレングリコールジメチルエーテル
・ＢＤＧ ：ジエチレングリコールモノｎ−ブチルエーテル
・ＣＨＥ−２０：Ｎ，Ｎ−ビス（２−ヒドロキシエチル）−Ｎ−シクロヘキシルアミン（商品名：『アミノアルコール ＣＨＥ−２０』、日本乳化剤（株）製）
・ＭＢＤ ：Ｎ−ｎ−ブチルジエタノールアミン
The abbreviations in Table 1 indicate the following compounds.
-DEDG: Diethylene glycol diethyl ether-MEDG: Diethylene glycol ethyl methyl ether-DPDM: Dipropylene glycol dimethyl ether-BDG: Diethylene glycol mono n-butyl ether-CHE-20: N, N-bis (2-hydroxyethyl) -N-cyclohexylamine ( Product name: "Amino alcohol CHE-20", manufactured by Nippon Emulsion Co., Ltd.)
MBD: Nn-butyldiethanolamine
〔ロジンフラックス残渣を供給したモデル基板に対する隙間洗浄性〕
市販のロジン系フラックスが含有されたソルダペースト（製品名「パインソルダー ＶＡＰＹ―ＬＦ２１９」、荒川化学工業（株）製）を用いて、［００５５］〜［００５７］と同様の方法でモデル基板を作製した（今回の製品はソルダペーストのため、ソルダペーストの調整過程を省略する）。前記モデル基板で実施例４の鉛フリーはんだフラックス用洗浄剤組成物で洗浄したところ、同様に優れた隙間洗浄性を示すことがわかった。
[Gap cleaning property for model substrates supplied with rosin flux residue]
A model substrate was prepared in the same manner as in [0055] to [0057] using a commercially available solder paste containing a rosin-based flux (product name "Pine Solder VAPY-LF219", manufactured by Arakawa Chemical Industry Co., Ltd.). (Since this product is a solder paste, the solder paste adjustment process is omitted). When the model substrate was washed with the lead-free solder flux cleaning agent composition of Example 4, it was found that the model substrate also exhibited excellent gap cleaning performance.
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| JPH0457899A (en) | 1990-06-27 | 1992-02-25 | Arakawa Chem Ind Co Ltd | Detergent for rosing solder flux and method for washing rosin solder flux using said detergent |
| JP2813862B2 (en) | 1994-07-05 | 1998-10-22 | 荒川化学工業株式会社 | Detergent composition |
| US5571340A (en) * | 1994-09-09 | 1996-11-05 | Fry's Metals, Inc. | Rosin-free, low VOC, no-clean soldering flux and method using the same |
| JPH0959698A (en) * | 1995-08-23 | 1997-03-04 | Asahi Chem Ind Co Ltd | Detergent composition for metal mask |
| US5733378A (en) * | 1996-02-26 | 1998-03-31 | Austin American Technology | Method for cleaning printed circuit boards |
| US7435711B2 (en) * | 2003-08-27 | 2008-10-14 | Kaken Tech Co., Ltd. | Cleaning agent for removing solder flux and method for cleaning solder flux |
| JP2005112887A (en) * | 2003-10-03 | 2005-04-28 | Kaken Tec Kk | Detergent composition for flux and method for washing using the same |
| WO2007119392A1 (en) * | 2006-03-17 | 2007-10-25 | Arakawa Chemical Industries, Ltd. | Cleaner composition for removal of lead-free soldering flux, rinsing agent for removal of lead-free soldering flux, and method for removal of lead-free soldering flux |
| KR101530321B1 (en) * | 2007-08-08 | 2015-06-19 | 아라까와 가가꾸 고교 가부시끼가이샤 | Cleaner composition for removing lead-free soldering flux, and method for removing lead-free soldering flux |
| KR20090020199A (en) | 2007-08-23 | 2009-02-26 | 주식회사 코오롱 | Polishing pad and method of manufacturing the same |
| JP5556658B2 (en) * | 2008-08-27 | 2014-07-23 | 荒川化学工業株式会社 | Cleaning composition for lead-free solder flux removal and lead-free solder flux removal system |
| WO2011019189A2 (en) | 2009-08-11 | 2011-02-17 | 동우 화인켐 주식회사 | Resist stripping solution composition, and method for stripping resist by using same |
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| KR101128865B1 (en) * | 2010-10-01 | 2012-03-26 | 에이케이켐텍 주식회사 | Formulation of cleaner for removing residual flux after reflow and cleaning method by using it |
| JP2018127573A (en) | 2017-02-10 | 2018-08-16 | 荒川化学工業株式会社 | Rinse agent for electronic material |
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