JP2004176179A - Water soluble treatment agent for improving solder wettability of electronic component terminal, and treatment method therefor - Google Patents
Water soluble treatment agent for improving solder wettability of electronic component terminal, and treatment method therefor Download PDFInfo
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本発明は、電子部品の製造や電子部品実装において該部品端子を半田接合する際に、半田の濡れ性を高めて確実な半田接合を可能にする水溶性の半田濡れ性向上処理剤と、該処理剤を用いた半田付け面の表面処理法に関するものである。 The present invention relates to a water-soluble solder wettability improving agent that enhances solder wettability and enables reliable solder joint when soldering the component terminals in the production and mounting of electronic components. The present invention relates to a surface treatment method for a soldering surface using a treatment agent.
電子部品端子に半田付けを行う際には、半田めっき表面の酸化物などを除去して半田の濡れ性を高めるため、所謂フラックス（またはペースト）で表面処理する方法が採用されており、また、これらの表面処理剤で半田めっき表面を予め被覆しておくことによって化成皮膜を形成し、酸化防止を図ることも行なわれている（特許文献１，２など）。 When soldering to electronic component terminals, a so-called flux (or paste) surface treatment method is used to remove oxides and the like on the solder plating surface and enhance solder wettability. It is also practiced to form a chemical conversion film by coating the surface of the solder plating in advance with these surface treatment agents to prevent oxidation (Patent Documents 1 and 2 and the like).
他方、最近では、環境汚染防止の意識が高まってくるにつれて、鉛主体の半田に代わって、鉛フリー半田の使用比率が急速に増大してきており、該鉛フリー半田としては、ニッケル合金や、錫−銅、錫−銀、錫−ビスマス、錫−亜鉛、錫−インジウムなどの錫合金が開発されている。ところが鉛を含有する従来の半田に比べると、電子部品保管時および電子部品実装におけるリフロー時に半田付け面に酸化皮膜が形成され易く、半田濡れ性が低下するという問題がある。 On the other hand, recently, as awareness of environmental pollution prevention has increased, the use ratio of lead-free solder has rapidly increased in place of lead-based solder, and nickel-based alloys and tin-based solders have been used as the lead-free solder. Tin alloys such as copper, tin-silver, tin-bismuth, tin-zinc, tin-indium, etc. have been developed. However, when compared with conventional lead-containing solder, there is a problem that an oxide film is easily formed on a soldering surface at the time of electronic component storage and reflow in electronic component mounting, and solder wettability is reduced.
そこで、こうした問題に対する解決策として例えば特許文献３には、鉛フリー半田を用いて半田付けを行う際に、ロジン系などの樹脂成分に活性剤と共に有機酸金属塩を添加したフラックスを使用することにより、鉛フリー半田の濡れ性を高め、半田付け性や接合強度を高める技術が開示されている。 Therefore, as a solution to such a problem, for example, Patent Document 3 discloses that when soldering using lead-free solder, a flux in which an organic acid metal salt is added to a resin component such as a rosin-based resin together with an activator is used. Accordingly, there is disclosed a technique for improving wettability of lead-free solder and improving solderability and joining strength.
しかしこれらのフラックスでも、鉛フリー半田を使用する際の接合性改善効果については必ずしも満足し得るものとは言えず、特に鉛フリー半田の濡れ性向上対策については一層の改善が求められる。
本発明は上記の様な問題に鑑みてなされたものであり、その目的は、電子部品保管時における端子に形成されるめっき部の酸化皮膜形成を抑制することによって、実装時に鉛フリー半田を用いた場合でも接合時の半田濡れ性を高めることができ、或いは、既に端子部に酸化皮膜が形成された電子部品に適用する場合は、当該酸化皮膜を簡単に除去することができ、実装に際して半田濡れ性を高めることのできる処理剤を提供し、更には、当該処理剤を使用することによって半田付けをより確実に実施し得るような処理法を提供することにある。 The present invention has been made in view of the above problems, and an object of the present invention is to use a lead-free solder at the time of mounting by suppressing the formation of an oxide film on a plated portion formed on a terminal during storage of an electronic component. Can improve the solder wettability at the time of bonding, or when applied to an electronic component with an oxide film already formed on the terminals, the oxide film can be easily removed, and the solder It is an object of the present invention to provide a processing agent capable of improving wettability, and to provide a processing method that can more reliably perform soldering by using the processing agent.
上記課題を解決することのできた本発明に係る半田濡れ性向上処理剤とは、
(A)有機酸アミン塩、
(B)一価アルコール類、グリコール類および極性非プロトン溶媒から選択される少なくとも１種、および
(C)非イオン界面活性剤
を必須成分として含有するところに特徴を有している。
With the solder wettability improving agent according to the present invention that was able to solve the above problems,
(A) an organic acid amine salt,
(B) at least one selected from monohydric alcohols, glycols and polar aprotic solvents, and
(C) It is characterized in that it contains a nonionic surfactant as an essential component.
上記有機酸アミン塩の有機酸として特に好ましいのは、下記一般式(I)で表される有機酸の少なくとも１種であり、また該有機酸アミン塩を構成する好ましいアミンは、下記一般式(II),(III)で表される少なくとも１種のアミンである。 Particularly preferred as the organic acid of the organic acid amine salt is at least one kind of organic acid represented by the following general formula (I), and a preferred amine constituting the organic acid amine salt is represented by the following general formula (I) At least one amine represented by (II) or (III).
Ｒ−ＣＯＯＨ……(I)
［式中、Ｒは炭素数６〜２２の直鎖状または分岐状の飽和または不飽和の脂肪
族、脂環族、もしくは芳香族の炭化水素基を表わす］
Ｒ１・Ｒ２・Ｒ３Ｎ……(II)
［式中、Ｒ１,Ｒ２,Ｒ３は、同一もしくは異なってもよく、水素または炭素数１
〜２２の直鎖状または分枝状の飽和もしくは不飽和の脂肪族、脂環族または
芳香族の炭化水素基を表わす］
Ｒ４・Ｒ５Ｎ-Ｒ６-ＮＲ７・Ｒ８……(III)
［式中、Ｒ４,Ｒ５,Ｒ７,Ｒ８は、水素または炭素数１〜２２の直鎖状または分枝
状の飽和もしくは不飽和の脂肪族、脂環族または芳香族の炭化水素、Ｒ６は
炭素数２〜８のアルキレン基を表わす］。
R-COOH ... (I)
[In the formula, R represents a linear or branched saturated or unsaturated aliphatic, alicyclic, or aromatic hydrocarbon group having 6 to 22 carbon atoms.]
R 1 · R 2 · R 3 N ...... (II)
[Wherein, R 1 , R 2 , and R 3 may be the same or different;
Represents up to 22 linear or branched, saturated or unsaturated, aliphatic, alicyclic or aromatic hydrocarbon groups]
R 4 · R 5 NR 6 -NR 7 · R 8 (III)
[Wherein R 4 , R 5 , R 7 , and R 8 are hydrogen or a linear or branched saturated or unsaturated aliphatic, alicyclic, or aromatic hydrocarbon having 1 to 22 carbon atoms. , R 6 represents an alkylene group having 2 to 8 carbon atoms].
また、前記一価アルコール類として好ましく使用されるのは、下記一般式(IV)で示されるアルコールであり、また前記グリコール類として好ましいのは、下記一般式(V)で示されるグリコールまたはそのハーフエーテルである。 Also, preferably used as the monohydric alcohols are alcohols represented by the following general formula (IV), and preferable as the glycols are glycols represented by the following general formula (V) or a half thereof. It is ether.
Ｒ９-ＯＨ……(IV)
［式中、Ｒ９は、炭素数１〜８の直鎖状または分岐状の脂肪族、脂環族もしく
は芳香族の炭化水素基を表わす］
Ｒ10Ｏ-（Ｒ11-Ｏ）ｎＨ……(V)
［式中、Ｒ10は水素または炭素数１〜４のアルキル基、Ｒ11は炭素数２〜４の
アルキレン基、ｎは、１以上の整数を表わす］。
R 9 -OH ... (IV)
[Wherein, R 9 represents a linear or branched aliphatic, alicyclic, or aromatic hydrocarbon group having 1 to 8 carbon atoms]
R 10 O- (R 11 -O) n H ...... (V)
[Wherein, R 10 is hydrogen or an alkyl group having 1 to 4 carbon atoms, R 11 is an alkylene group having 2 to 4 carbon atoms, and n represents an integer of 1 or more].
また、前記極性非プロトン溶媒として好ましいのは、Ｎ−メチル−２−ピロリドン、ジメチルホルムアミド、ジメチルスルホキシド、ジオキサン、アセトンなどが例示される。 Preferred examples of the polar aprotic solvent include N-methyl-2-pyrrolidone, dimethylformamide, dimethylsulfoxide, dioxane, acetone and the like.
本発明に係る電子部品端子の表面処理法は、上記処理材を用いた表面処理法に関するもので、電子部品を製造するに当たり、電子部品の端子にめっきを施した後、該めっき表面を前記半田濡れ性向上処理剤で処理し、めっき表面の酸化を抑制し、或いは、電子部品実装において電子部品端子上に施しためっき皮膜に半田付けを行うに当たり、被半田付け面を、前記半田濡れ性向上処理剤で処理することにより、電子部品端子上に施しためっき表面に形成された酸化皮膜を除去するところに特徴を有している。 The surface treatment method for an electronic component terminal according to the present invention relates to a surface treatment method using the above-described processing material.In manufacturing an electronic component, after plating the terminal of the electronic component, the plated surface is soldered. Treating with a wettability improving agent to suppress oxidation of the plating surface, or, when soldering a plating film applied on an electronic component terminal in mounting an electronic component, improving the solder wettability on the surface to be soldered. It is characterized in that an oxide film formed on a plating surface provided on an electronic component terminal is removed by treating with a treating agent.
上記本発明の処理法を実施するに当たり、電子部品端子上に施される鉛フリーのめっきとしては、ニッケルまたは錫合金めっきが好ましく、これらのめっき表面には更に酸化防止などを目的として金、銀、白金などの貴金属めっきが施されていてもよい。また該錫合金めっきとして特に好ましいのは、錫を主体とし銅、銀、ビスマス、亜鉛、インジウムよりなる群から選択されるいずれかの金属を含む錫合金である。 In carrying out the processing method of the present invention, nickel or tin alloy plating is preferable as the lead-free plating applied to the electronic component terminals, and gold, silver, or the like is further provided on the surface of these platings for the purpose of preventing oxidation or the like. And a noble metal plating such as platinum. Particularly preferred as the tin alloy plating is a tin alloy containing tin as a main component and any metal selected from the group consisting of copper, silver, bismuth, zinc, and indium.
また本発明の処理法が適用される半田付けは、前述した如く公害防止の観点から鉛フリー半田を使用することが望ましく、該鉛フリー半田としても、錫を主体とし銅、銀、ビスマス、亜鉛、インジウムよりなる群から選択されるいずれかの金属を含む錫合金が好ましく使用される。 Further, the soldering to which the processing method of the present invention is applied is preferably a lead-free solder from the viewpoint of preventing pollution as described above. As the lead-free solder, tin is mainly used, and copper, silver, bismuth, and zinc are used. And a tin alloy containing any metal selected from the group consisting of indium is preferably used.
本発明の半田濡れ性向上技術を採用すれば、保存時の電子部品端子部の酸化を抑制し、或いは既に酸化皮膜が形成されている場合は、電子部品実装時の半田付け工程のリフロー時に酸化皮膜を除去することができるので、半田濡れ性を大幅に高めることができ、半田による接合性と信頼性を著しく向上させることができる。殊に本発明によれば、最近環境汚染防止の観点から急増してきている鉛フリー半田に対しても卓越した濡れ性を与えるので、その需要は今後益々増大していくものと期待される。 Employing the solder wettability improving technology of the present invention suppresses the oxidation of the electronic component terminal portion during storage or, if an oxide film has already been formed, oxidizes it during reflow in the soldering process when mounting the electronic component. Since the film can be removed, the solder wettability can be greatly increased, and the joining property and reliability by solder can be significantly improved. In particular, according to the present invention, excellent wettability is given even to lead-free solder, which has been rapidly increasing from the viewpoint of environmental pollution prevention in recent years, so that its demand is expected to increase further in the future.
本発明の半田濡れ性向上処理剤は、上記の様に(A)有機酸アミン塩、(B)一価アルコール類、グリコール類および極性非プロトン溶媒から選択される少なくとも１種、(C)非イオン界面活性剤を必須成分として含有するもので、電子部品を製造する際に、該部品の端子部にめっきを施して水洗を行った後、上記処理剤を脱イオン水で例えば１０〜１００質量％に希釈した溶液を上記部品端子部に接触させ、該端子のめっき表面に緻密な撥水性の有機皮膜を形成させることにより、その撥水性によって端子部からの水切り性を向上させると共に、水洗後の酸化皮膜形成を抑制し、且つ緻密な有機皮膜によって保管時の酸化皮膜形成を防止する。こうした作用によって、電子部品実装時における半田付け工程における半田濡れ性を大幅に高めると共に、半田による接合を強固且つ確実にすることができる。 As described above, the solder wettability improving agent of the present invention comprises at least one selected from the group consisting of (A) an organic acid amine salt, (B) a monohydric alcohol, a glycol, and a polar aprotic solvent; It contains an ionic surfactant as an essential component, and when manufacturing an electronic component, after plating and rinsing the terminal portion of the component and washing with water, the above-mentioned treating agent is mixed with deionized water, for example, 10 to 100 mass%. % By contacting the above-mentioned component terminal portion with the above-mentioned terminal portion of the component to form a dense water-repellent organic film on the plating surface of the terminal. The formation of an oxide film during storage is prevented by the dense organic film. By such an operation, the solder wettability in the soldering step at the time of mounting the electronic component can be significantly increased, and the bonding by the solder can be made firm and reliable.
また電子部品実装を行う際に、部品端子部に既に酸化皮膜が形成されている場合は、当該部品端子部を本発明の処理剤で処理し、該端子部上に緻密な有機皮膜を形成させてから半田付けを行えば、該端子部上に形成された上記有機皮膜が、半田付けを行う際のリフロー時の加熱によりフラックスとして作用し、酸化皮膜を溶解除去することによって半田濡れ性を大幅に高める。 Also, when an electronic component is mounted, if an oxide film is already formed on the component terminal, the component terminal is treated with the treating agent of the present invention to form a dense organic film on the terminal. If soldering is performed afterwards, the organic film formed on the terminal portion acts as a flux due to heating during reflow during soldering, and dissolves and removes an oxide film to greatly improve solder wettability. Enhance.
以下、本発明に係る水溶性半田濡れ性向上処理剤の構成成分を主体にして詳細に説明していく。 Hereinafter, the present invention will be described in detail mainly on the components of the water-soluble solder wettability improving agent according to the present invention.
本発明の半田濡れ性向上処理剤は、上記の様に(A)有機酸アミン塩と(B)一価アルコール、グリコール類および極性非プロトン溶媒から選択される少なくとも１種、並びに(C)非イオン界面活性剤を必須成分として含有する。 As described above, the solder wettability improving agent of the present invention comprises (A) an organic acid amine salt and (B) at least one selected from monohydric alcohols, glycols and polar aprotic solvents, and (C) non-aprotic solvents. Contains an ionic surfactant as an essential component.
上記(A)有機酸アミン塩は、本発明における半田濡れ性向上処理剤の主成分となるもので、特に部品端子保管時の酸化防止と、熱処理時における酸化皮膜の溶解性を高める機能を果たす。該有機酸アミン塩を構成する好ましい有機酸としては、前記一般式(I)で示される有機酸が挙げられ、具体的にはカプリル酸、カプリン酸、ラウリン酸、ミリスチン酸、パルミチン酸、ステアリン酸、アラキジン酸、ベヘニン酸、イソステアリン酸、エライジン酸、オレイン酸、リノール酸、リノレン酸、エルカ酸、アゼライン酸、ドデカン二酸、安息香酸、フタル酸などが例示される。これらの有機酸は単独で使用し得るほか、必要により２種以上を適宜組合せて使用することができる。これら有機酸の中でも特に好ましいのは、オレイン酸、ミリスチン酸、パルミチン酸などである。 The above-mentioned (A) organic acid amine salt is a main component of the solder wettability improving agent in the present invention, and particularly has a function of preventing oxidation during storage of component terminals and enhancing solubility of an oxide film during heat treatment. . Preferred organic acids constituting the organic acid amine salt include the organic acids represented by the general formula (I), and specifically include caprylic acid, capric acid, lauric acid, myristic acid, palmitic acid, and stearic acid. Arachidic acid, behenic acid, isostearic acid, elaidic acid, oleic acid, linoleic acid, linolenic acid, erucic acid, azelaic acid, dodecanedioic acid, benzoic acid, phthalic acid and the like. These organic acids can be used alone or, if necessary, in combination of two or more. Among these organic acids, particularly preferred are oleic acid, myristic acid, palmitic acid and the like.
また該有機酸のアミン塩におけるアミンとしては、前記一般式(II),(III)で表されるアミンが挙げられ、好ましい具体例としては、モノプロピルアミン、モノブチルアミン、ジブチルアミン、トリブチルアミン、モノ−２−エチルヘキシルアミン、ジ−２−エチルヘキシルアミン、ベンジルアミン、シクロヘキシルアミン、ジシクロヘキシルアミン、ピペリジン、Ｎ−メチルピペリジン、２−ピペコリン、ピロリジン、３−メトキシプロピルアミン、モルホリン、ジメチルエタノールアミン、ジエチルエタノールアミンなどが例示される。 Examples of the amine in the amine salt of the organic acid include the amines represented by the general formulas (II) and (III). Preferred specific examples are monopropylamine, monobutylamine, dibutylamine, tributylamine, Mono-2-ethylhexylamine, di-2-ethylhexylamine, benzylamine, cyclohexylamine, dicyclohexylamine, piperidine, N-methylpiperidine, 2-pipecholine, pyrrolidine, 3-methoxypropylamine, morpholine, dimethylethanolamine, diethylethanol Examples include amines.
また、上記アミン(III)の好ましい具体例としては、エチレンジアミン、ジエチレントリアミン、１，４−ジアミノブタン、ジメチルアミノプロピルアミン、Ｎ−アミノプロピルモルホリン、ヒドロキシエチルアミノプロピルアミン、メタキシリレンジアミン、アミノエチルピペラジン、２−メチルイミダゾール、２−メチルイミダゾリン、２−フェニルイミダゾリンなどが例示される。 Preferred specific examples of the amine (III) include ethylenediamine, diethylenetriamine, 1,4-diaminobutane, dimethylaminopropylamine, N-aminopropylmorpholine, hydroxyethylaminopropylamine, metaxylylenediamine, and aminoethylpiperazine. , 2-methylimidazole, 2-methylimidazoline, 2-phenylimidazoline and the like.
これら一般式(II),(III)で表されるアミンも、単独で使用し得るほか、必要により２種以上を適宜組合せて使用できる。 The amines represented by the general formulas (II) and (III) can be used alone or in combination of two or more as needed.
上記アミンの中でも特に好ましいのは、ジシクロへキシルアミン、モルホリン、ジメチルアミノプロピルアミン等である。 Among the above amines, particularly preferred are dicyclohexylamine, morpholine, dimethylaminopropylamine and the like.
上記有機酸と上記アミンの好ましいモル比は０．９：１〜１：０．９である。本発明の処理剤は、上記有機酸アミン塩を任意の比率で含むことができるが、半田濡れ性向上処理剤中に占める該有機酸アミン塩の好ましい含有量は５質量％以上、９０質量％以下である。該有機酸アミン塩の含有率が５質量％未満では、部品端子保管時の酸化防止作用や熱処理時の酸化皮膜の溶解性が不足気味となり、逆に９０質量％を超えると、(B)一価アルコール類、グリコール類、極性非プロトン溶媒や(C)非イオン界面活性剤の含有率が相対的に不足気味となって、処理液の安定性や水に対する溶解性が悪くなる。処理液の安定性や水に対する溶解性を低下させることなく、部品端子保管時の酸化防止作用や熱処理時の酸化皮膜の溶解性を確保する上で特に好ましい有機酸アミン塩の配合量は、１０質量％以上、８０質量％以下である。 The preferred molar ratio of the organic acid to the amine is from 0.9: 1 to 1: 0.9. The treating agent of the present invention can contain the above-mentioned organic acid amine salt in an arbitrary ratio, and the preferable content of the organic acid amine salt in the solder wettability improving treating agent is 5% by mass or more and 90% by mass or more. It is as follows. If the content of the organic acid amine salt is less than 5% by mass, the antioxidant effect at the time of storage of the component terminals and the solubility of the oxide film at the time of heat treatment tend to be insufficient. The contents of the polyhydric alcohols, glycols, polar aprotic solvent and (C) nonionic surfactant tend to be relatively insufficient, and the stability of the treatment liquid and the solubility in water deteriorate. The amount of the organic acid amine salt which is particularly preferable for ensuring the antioxidant action at the time of storing the component terminals and the solubility of the oxide film at the time of heat treatment without reducing the stability of the processing solution and the solubility in water is 10%. It is not less than 80% by mass and not less than 80% by mass.
本発明で使用する一価アルコール類およびグリコール類とは、前記一般式(IV)で示される一価アルコール類および一般式(V)で示されるグリコール類であり、一価アルコール類の具体例としては、プロピルアルコール、イソプロピルアルコール、ブチルアルコール、シクロヘキサノールなどが例示され、またグリコール類の具体例としては、エチレングリコール、ポリエチレングリコール、ポリプロピレングリコール、３−メチル−１，３−ブタンジオール等のグリコール；メチルセロソルブ、ブチルカルビトール、３−メトキシ−３−メチル−１−ブタノール(ソルフィット)等のグリコールハーフエーテルが例示される。また極性非プロトン溶媒類としては、Ｎ−メチル−２−ピロリドン、ジメチルホルムアミド、ジメチルスルホキシド、ジオキサン、アセトンなどが例示される。 Monohydric alcohols and glycols used in the present invention are monohydric alcohols represented by the general formula (IV) and glycols represented by the general formula (V), and specific examples of the monohydric alcohols Is exemplified by propyl alcohol, isopropyl alcohol, butyl alcohol, cyclohexanol and the like. Specific examples of glycols include glycols such as ethylene glycol, polyethylene glycol, polypropylene glycol and 3-methyl-1,3-butanediol; Glycol half ethers such as methyl cellosolve, butyl carbitol and 3-methoxy-3-methyl-1-butanol (Solfit) are exemplified. Examples of polar aprotic solvents include N-methyl-2-pyrrolidone, dimethylformamide, dimethylsulfoxide, dioxane, acetone and the like.
これら一価アルコール類、グリコール類および極性非プロトン溶媒類も各々単独で使用し得るほか、必要により２種以上を適宜組合せて使用することができる。 These monohydric alcohols, glycols and polar aprotic solvents can be used alone, respectively, and if necessary, two or more kinds can be used in appropriate combination.
上記一価アルコール類、グリコール類および極性非プロトン溶媒から選択される少なくとも１種の使用量は、半田濡れ性向上処理剤全量中に占める比率で１質量％以上、４０質量％以下の範囲とするのがよい。それらの配合量が１質量％未満では、処理液の安定性や水に対する溶解性、更には補助的な熱処理時の酸化皮膜の溶解性が不足気味となり、また５０質量％を超えて過度に多くなると、前記有機酸アミン塩の含有量が相対的に少なくなって、部品端子保管時の酸化防止作用や、熱処理時における酸化皮膜の溶解性が悪くなる傾向が生じてくる。処理剤の安定性と熱処理時における酸化皮膜の溶解性を最大限有効に発揮させる上でより好ましい使用量は、２質量％以上、４０質量％以下である。 The amount of use of at least one selected from the above monohydric alcohols, glycols and polar aprotic solvents is in the range of 1% by mass or more and 40% by mass or less in the total amount of the solder wettability improving agent. Is good. If the compounding amount is less than 1% by mass, the stability of the treatment liquid and the solubility in water, and further the solubility of the oxide film during the auxiliary heat treatment may be insufficient, and may exceed 50% by mass. Then, the content of the organic acid amine salt becomes relatively small, and the antioxidant action during storage of the component terminals and the solubility of the oxide film during heat treatment tend to deteriorate. In order to maximize the stability of the treatment agent and the solubility of the oxide film during the heat treatment, a more preferable use amount is 2% by mass or more and 40% by mass or less.
本発明に係る半田濡れ性向上処理剤における更に他の必須成分である非イオン界面活性剤は、一価アルコール類、グリコール類および極性非プロトン溶媒から選択される少なくとも１種と共同して、液状処理剤としての安定性や水に対する溶解性を高める作用を有しており、上記成分（A），(B)と共に混合溶解して水に可溶化するものであれば全ての非イオン界面活性剤を使用できるが、好ましい具体例としては、ポリオキシエチレンアルキルフェニルエーテル、ポリオキシアルキルエーテル、ポリオキシエチレン・ポリオキシプロピレンブロックポリマー、ポリオキシ脂肪酸エステル、ソルビタン脂肪酸エステルなどが挙げられる。 The nonionic surfactant which is still another essential component in the solder wettability improving agent according to the present invention is a liquid in cooperation with at least one selected from monohydric alcohols, glycols and polar aprotic solvents. All nonionic surfactants have the effect of increasing the stability as a treatment agent and the solubility in water, and can be mixed and dissolved with the above components (A) and (B) and solubilized in water. Can be used, and preferred specific examples include polyoxyethylene alkylphenyl ether, polyoxyalkyl ether, polyoxyethylene / polyoxypropylene block polymer, polyoxy fatty acid ester, and sorbitan fatty acid ester.
半田濡れ性向上処理剤中に占める該非イオン界面活性剤の好ましい含有量は、１質量％以上、５０質量％以下であり、１質量％未満では処理剤の安定性や水に対する溶解性が悪くなり、５０質量％を超えて過度に多くなると、前記有機酸アミン塩の含有量が相対的に少なくなって、部品端子保管時の酸化防止作用や熱処理時における酸化皮膜の溶解性が低下傾向を示す様になる。これら非イオン界面活性剤の作用を最大限有効に発揮させる上でより好ましい非イオン界面活性剤の含有量は、２質量％以上、４０質量％以下である。 The preferred content of the nonionic surfactant in the treatment agent for improving solder wettability is 1% by mass or more and 50% by mass or less. When the content is less than 1% by mass, the stability of the treatment agent and the solubility in water are deteriorated. If the content is excessively larger than 50% by mass, the content of the organic acid amine salt becomes relatively small, and the antioxidant action at the time of storing the component terminals and the solubility of the oxide film at the time of heat treatment tend to decrease. Looks like. A more preferable content of the nonionic surfactant for maximally and effectively exerting the action of the nonionic surfactant is 2% by mass or more and 40% by mass or less.
本発明の処理剤は、上記の如く(A)有機酸アミン塩と、(B)一価アルコール類、グリコール類および極性非プロトン溶媒から選択される少なくとも１種、並びに(C)非イオン界面活性剤を必須成分として含有するが、上記以外の成分として、部品端子保管時の酸化防止効果を高める作用を有するアクリル系樹脂やポリエステル系樹脂、ウレタン系樹脂などの水分散性あるいは水溶性有機樹脂や、熱処理時における酸化皮膜の溶解性改善効果を有する天然ロジン、ロジンエステル、ロジン変性マレイン酸系樹脂などを、必要に応じて適量配合することも勿論可能である。 The treating agent of the present invention is, as described above, (A) an organic acid amine salt, (B) at least one selected from monohydric alcohols, glycols and polar aprotic solvents, and (C) nonionic surfactant Contains an agent as an essential component, but as a component other than the above, a water-dispersible or water-soluble organic resin such as an acrylic resin, a polyester resin, or a urethane resin having an effect of increasing the antioxidant effect at the time of storing component terminals, Natural rosin, rosin ester, rosin-modified maleic resin having an effect of improving the solubility of the oxide film at the time of heat treatment, and the like can be naturally added in an appropriate amount, if necessary.
なお本発明の上記処理剤は、前記(A),(B),(C)各成分の種類や配合率を適正に制御することで水溶性としたものであることを必須とする。その理由は、部品端子にめっきした後、水洗後、乾燥なしでそのまま本発明の処理剤で処理することができ、乾燥時の酸化を防止できるからである。また、処理後に保管し、または熱処理時の酸化防止後に皮膜を除去する際にも、水洗によって容易に除去できるからである。 In addition, it is essential that the treatment agent of the present invention is made water-soluble by appropriately controlling the types and mixing ratios of the components (A), (B), and (C). The reason for this is that, after plating on the component terminal, it can be treated with the treating agent of the present invention without drying after washing with water, and oxidation during drying can be prevented. Also, when the film is stored after the treatment or the film is removed after the oxidation is prevented during the heat treatment, the film can be easily removed by washing with water.
本発明に係る上記水溶性半田濡れ性向上処理剤を、各種電子部品の端子部分に適用すると、該端子部分を構成する銅、銅合金、半田、無電解半田、ニッケル、銀、亜鉛、錫合金などの表面に耐食性、耐水性、耐薬品性などに優れた化成皮膜が形成され、当該端子部に設けられるめっき表面の発錆や耐久劣化を長期的に防止できる。 When the water-soluble solder wettability improving agent according to the present invention is applied to terminal portions of various electronic components, copper, copper alloy, solder, electroless solder, nickel, silver, zinc, and tin alloy constituting the terminal portions A chemical conversion film having excellent corrosion resistance, water resistance, chemical resistance and the like is formed on the surface of the terminal and the like, and rusting and durability deterioration of the plating surface provided on the terminal portion can be prevented for a long time.
また、既に酸化皮膜が形成された電子部品端子部に、例えば、錫−銅、錫−銀、錫−ビスマス、錫−亜鉛、錫−インジウムなどに代表される鉛フリー半田を用いて半田付けを行う際に、接合対象面を該処理剤で処理すると、その表面に形成されている酸化皮膜は速やかに溶解して端子表面が清浄化されると共に、その表面の鉛フリー半田等に対する濡れ性が著しく高められ、確実且つ安定した半田接合を実現できると共に、接合部の信頼性を大幅に高めることができる。 In addition, for example, tin-copper, tin-silver, tin-bismuth, tin-zinc, tin-indium, and the like are soldered to the electronic component terminal portion on which the oxide film is already formed. When the surface to be joined is treated with the treating agent, the oxide film formed on the surface is quickly dissolved to clean the terminal surface, and the wettability of the surface to lead-free solder or the like is reduced. It is remarkably enhanced, and a reliable and stable solder joint can be realized, and the reliability of the joint can be greatly improved.
この様に本発明の処理剤および処理法によれば、電子部品用端子部に汎用されているニッケルめっき等に対して優れた酸化防止効果を享受できると共に、既に形成されていることのある酸化膜は効率よく溶解除去することができ、鉛フリー半田に対しても卓越した濡れ性を与えることができる。よって、電子部品端子部に例えばニッケルめっきを施す際に、該ニッケルめっき表面の酸化防止用等として行われることのある金めっき処理なども省略可能となる。また、その様な金めっき処理（あるいは銀、白金などの貴金属めっき処理）が既に施されている場合は、その表面に本発明の処理法をそのまま適用すればよく、更には、それら貴金属めっきが極薄で部分的にニッケルめっき等が露出している様な場合でも、本発明の処理法を適用することで支障なく確実な半田接合を行うことができる。 As described above, according to the treating agent and the treating method of the present invention, it is possible to enjoy an excellent antioxidant effect on nickel plating and the like, which are widely used for terminal parts for electronic components, and to prevent oxidation that may have already been formed. The film can be efficiently dissolved and removed, and can provide excellent wettability to lead-free solder. Therefore, when, for example, nickel plating is applied to the electronic component terminal portion, it is possible to omit a gold plating process or the like that is sometimes performed for preventing oxidation of the nickel plating surface. When such a gold plating treatment (or a plating treatment of a noble metal such as silver or platinum) has already been performed, the treatment method of the present invention may be applied to the surface as it is. Even in the case where the nickel plating or the like is extremely thin and partially exposed, application of the processing method of the present invention enables reliable solder bonding without any trouble.
本発明が適用される上記電子部品の種類には特に制限がなく、要は半田接合される端子部、特に鉛フリー半田により接合される端子部を有するものであれば全て有効に適用することができ、代表的なものとしてはプリント基板のリードフレームなどが例示される。 The type of the electronic component to which the present invention is applied is not particularly limited. In short, any type of electronic component having a terminal portion joined by soldering, particularly a terminal portion joined by lead-free solder can be effectively applied. A typical example is a lead frame of a printed circuit board.
また本発明は、特に鉛フリー半田を用いた電子部材のロウ付けに有効に活用されるが、依然として一部で実用化されている鉛含有半田に適用した場合でも、同様に優れた濡れ性向上作用や酸化防止作用を発揮し得るものであり、これらへの適用を排除するものではない。 In addition, the present invention is particularly effectively used for brazing electronic members using lead-free solder. However, even when the present invention is applied to a lead-containing solder which is still partially used, similarly excellent wettability can be improved. It can exert an action and an antioxidant action, and does not exclude application to these.
本発明の半田濡れ性向上処理剤を金属表面に施すには、金属と処理液とを接触させればよく、接触させる方法としては、浸漬、噴霧、塗布などを採用すればよい。接触させる際の処理液の温度は、０〜１００℃の範囲が適当であり、浸漬時間は数秒〜数十分が適当である。 In order to apply the solder wettability improving treatment agent of the present invention to a metal surface, the metal and the treatment liquid may be brought into contact with each other, and the contact may be made by immersion, spraying, coating, or the like. The temperature of the treatment liquid at the time of contact is suitably in the range of 0 to 100 ° C., and the immersion time is suitably several seconds to tens of minutes.
以下、実施例を挙げて本発明をより具体的に説明するが、本発明はもとより下記実施例によって制限を受けるものではなく、前・後記の趣旨に適合し得る範囲で適当に変更を加えて実施することも勿論可能であり、それらはいずれも本発明の技術的範囲に包含される。 Hereinafter, the present invention will be described more specifically with reference to Examples. However, the present invention is not limited to the following Examples, and may be appropriately modified within a range that can be adapted to the purpose of the preceding and the following. It is of course possible to carry out them, and all of them are included in the technical scope of the present invention.
実施例１［水溶性半田濡れ性向上処理剤(a)の製造］
有機酸として、オレイン酸３９４ｇと、アミンとしてジシクロヘキシルアミン２５６ｇを撹拌混合し、４０〜６０℃の温度で３０分間反応させた。次いで可溶化剤としてモノエチレングリコール２５０ｇと、非イオン界面活性剤として「ノイゲンEA-102」(第一工業製薬社製のポリオキシエチレンオクチルフェニルエーテル)１００ｇを加え、均一になるまで混合して水溶性半田濡れ性向上処理剤(a)１ｋｇを得た。この半田濡れ性向上処理剤(a)を脱イオン水で９０質量％に希釈し、処理液とした。
Example 1 [Production of water-soluble solder wettability improving agent (a)]
394 g of oleic acid as an organic acid and 256 g of dicyclohexylamine as an amine were stirred and mixed, and reacted at a temperature of 40 to 60 ° C. for 30 minutes. Next, 250 g of monoethylene glycol as a solubilizing agent and 100 g of "Neugen EA-102" (polyoxyethylene octylphenyl ether manufactured by Daiichi Kogyo Seiyaku Co., Ltd.) as a nonionic surfactant were added, mixed until uniform, and dissolved in water. 1 kg of a wettability improving treatment agent (a) was obtained. The treatment agent (a) for improving solder wettability was diluted to 90% by mass with deionized water to obtain a treatment liquid.
この処理液にニッケルめっき直後の電子部品端子部を浸漬し、乾燥させた後２５℃で５００時間放置し、めっき皮膜の酸化抑制を確認するための試料とした。 The electronic component terminal portion immediately after nickel plating was immersed in this treatment solution, dried, and then left at 25 ° C. for 500 hours to obtain a sample for confirming suppression of oxidation of the plating film.
実施例２
後述する対照例１で用いたのと同じ電子部品用の試験片を、上記実施例１で得た処理液に浸漬し、乾燥した後、電子部品実装におけるリフロー時の加熱条件を想定して２５０℃まで加熱し乾燥した。
Example 2
The same test piece for an electronic component as used in Comparative Example 1 to be described later was immersed in the treatment liquid obtained in Example 1 and dried. C. and dried.
実施例３［水溶性半田濡れ性向上処理剤(b)の製造］
有機酸としてミリスチン酸４５０ｇ、アミンとしてジブチルアミン２５５ｇを使用し、これらを均一に撹拌混合した後、４０〜６０℃の温度で３０分間反応させた。次いでこれに、可溶化剤としてブチルアルコール１００ｇと、非イオン界面活性剤として「ノイゲンＳＤ−８０」（第一工業製薬社製のポリオキシエチレンデシルエーテル）１９５ｇを加え、均一になるまで混合することにより、水溶性半田濡れ性向上処理剤(b)１ｋｇを得た。得られた半田濡れ性向上処理剤(b)を脱イオン水で９０質量％に希釈して処理液とした。この処理液にニッケルめっき直後の電子部品端子部を浸漬し、乾燥させた後２５℃で５００時間放置し、めっき皮膜の酸化抑制効果を確認するための試料とした。
Example 3 [Production of water-soluble solder wettability improving agent (b)]
450 g of myristic acid as an organic acid and 255 g of dibutylamine as an amine were uniformly stirred and mixed, and then reacted at a temperature of 40 to 60 ° C. for 30 minutes. Next, 100 g of butyl alcohol as a solubilizing agent and 195 g of "Neugen SD-80" (polyoxyethylene decyl ether manufactured by Daiichi Kogyo Seiyaku Co., Ltd.) as a nonionic surfactant are added and mixed until uniform. As a result, 1 kg of a water-soluble solder wettability improving agent (b) was obtained. The obtained solder wettability improving agent (b) was diluted to 90% by mass with deionized water to obtain a treating solution. The electronic component terminal portion immediately after nickel plating was immersed in this treatment liquid, dried, and allowed to stand at 25 ° C. for 500 hours to prepare a sample for confirming the effect of suppressing oxidation of the plating film.
実施例４
後記対照例１で用いたのと同じ試験片を、上記実施例３で得た処理液に浸漬してから乾燥した後、電子部品実装におけるリフロー時の加熱条件を想定して２５０℃まで加熱し乾燥した。
Example 4
The same test piece as used in Comparative Example 1 described below was immersed in the treatment liquid obtained in Example 3 described above, dried, and then heated to 250 ° C. assuming heating conditions during reflow in electronic component mounting. Dried.
実施例５［水溶性半田濡れ性向上処理剤(c)の製造］
有機酸としてパルミチン酸２５６ｇ、アミンとしてジベンジルアミン１９７ｇを使用し、これらを均一に撹拌混合した後、４０〜６０℃の温度で３０分間反応させた。次いでこれに、可溶化剤としてブチルアルコール１００ｇと、プロピレングリコール２００ｇ、および非イオン界面活性剤として「ノイゲンＳＤ−８０」(第一工業製薬社製のポリオキシエチレンデシルエーテル)２４７ｇを加え、均一になるまで混合することにより、水溶性半田濡れ性向上処理剤(c)１ｋｇを製造した。該半田濡れ性向上処理剤(c)を、脱イオン水で希釈することなくそのままで処理液とした。
Example 5 [Production of water-soluble solder wettability improving agent (c)]
256 g of palmitic acid as an organic acid and 197 g of dibenzylamine as an amine were uniformly stirred and mixed, and then reacted at a temperature of 40 to 60 ° C. for 30 minutes. Next, 100 g of butyl alcohol as a solubilizing agent, 200 g of propylene glycol, and 247 g of "Neugen SD-80" (a polyoxyethylene decyl ether manufactured by Daiichi Kogyo Seiyaku Co., Ltd.) as a nonionic surfactant were added, and the mixture was homogenized. By mixing until complete, 1 kg of a water-soluble solder wettability improving treatment agent (c) was produced. The treatment agent (c) for improving solder wettability was used as it was without dilution with deionized water.
この処理液にニッケルめっき直後の電子部品端子部を浸漬してから乾燥させ、２５℃で５００時間放置することにより、めっき皮膜の酸化抑制効果を確認するための試料とした。 The terminal part of the electronic component immediately after nickel plating was immersed in this treatment liquid, dried, and left at 25 ° C. for 500 hours to obtain a sample for confirming the effect of suppressing the oxidation of the plating film.
実施例６
後記対照例１で用いたのと同じ試験片を、上記実施例５で得た処理液に浸漬してから乾燥した後、電子部品実装におけるリフロー時の加熱条件を想定して２５０℃まで加熱して乾燥した後、２５℃で５００時間放置した。
Example 6
The same test piece as used in Comparative Example 1 described below was immersed in the treatment liquid obtained in Example 5 described above, dried, and then heated to 250 ° C. assuming heating conditions during reflow in electronic component mounting. After drying, it was left at 25 ° C. for 500 hours.
実施例７［水溶性半田濡れ性向上処理剤(d)の製造］
有機酸としてイソステアリン酸２８４ｇとオレイン酸１４１ｇ、アミンとしてメタキシリレンジアミン１０２ｇを使用し、これらを均一に撹拌混合した後、４０〜６０℃の温度で３０分間反応させた。次いでこれに、可溶化剤としてブチルアルコール１００ｇとトリエチレングリコール２００ｇ、および非イオン界面活性剤として「ノイゲンＳＤ−８０」(同前)１７３ｇ加え、均一になるまで混合することにより、水溶性半田濡れ性向上処理剤(d)１ｋｇを得た。
Example 7 [Production of water-soluble solder wettability improving agent (d)]
284 g of isostearic acid and 141 g of oleic acid were used as the organic acid, and 102 g of meta-xylylenediamine was used as the amine. After uniformly stirring and mixing these, they were reacted at a temperature of 40 to 60 ° C. for 30 minutes. Next, 100 g of butyl alcohol and 200 g of triethylene glycol as a solubilizing agent and 173 g of "Neugen SD-80" (the same as above) as a nonionic surfactant were added thereto, and mixed until uniform to obtain a water-soluble solder wet. 1 kg of a property improving treatment agent (d) was obtained.
この半田濡れ性向上処理剤(d)を、脱イオン水で８０質量％に希釈して処理液とした。この処理液にニッケルめっき直後の電子部品端子部を浸漬してから乾燥させ、２５℃で５００時間放置し、めっき皮膜の酸化抑制効果を確認するための試料とした。 The treatment agent (d) for improving the solder wettability was diluted to 80% by mass with deionized water to prepare a treatment liquid. The terminal part of the electronic component immediately after nickel plating was immersed in this treatment liquid, dried, and left at 25 ° C. for 500 hours to obtain a sample for confirming the effect of suppressing oxidation of the plating film.
実施例８
後記対照例１で用いたのと同じ試験片を、上記実施例７で得た処理液に浸漬してから乾燥した後、電子部品実装におけるリフロー時の加熱条件を想定して２５０℃まで加熱し乾燥した。
Example 8
The same test piece as used in Comparative Example 1 described below was immersed in the treatment liquid obtained in Example 7 described above, dried, and then heated to 250 ° C. assuming heating conditions during reflow in electronic component mounting. Dried.
対照例１
電子部品端子部にニッケルめっきを施した後、水洗してから乾燥し、大気中に２５℃で５００時間放置することにより、ニッケルめっき表面に酸化皮膜を形成させた。
Comparative Example 1
After nickel plating was applied to the terminal of the electronic component, it was washed with water, dried, and left in the air at 25 ° C. for 500 hours to form an oxide film on the nickel plating surface.
対照例２
上記対照例１と同様の酸化皮膜処理を行った後、２５０℃で加熱した。
Comparative Example 2
After the same oxide film treatment as in Control Example 1 above, heating was performed at 250 ° C.
比較例１
上記対照例１の酸化皮膜処理を行った後、該酸化皮膜処理面に、ロジン；２０質量％、ジエチルアミン塩酸塩；０．２質量％、イソプロピルアルコール；７９．８質量％のロジン系フラックスを塗布した。
Comparative Example 1
After performing the oxide film treatment of Comparative Example 1, a rosin-based flux of rosin; 20% by mass, diethylamine hydrochloride; 0.2% by mass, isopropyl alcohol; 79.8% by mass was applied to the oxide film-treated surface. did.
上記実施例１〜８の電子部品端子部と、対照例１，２および比較例１で得た酸化皮膜処理物について、夫々の半田濡れ性を調べた。なお半田としては、Ｓｎ；９６質量％、Ａｇ；３．５質量％、Ｃｕ；０．５質量％よりなる鉛フリーの錫合金を使用した。また、半田濡れ性の評価にはメニスコグラフ法を採用し、下記の条件により半田濡れ時間(秒)の平均値（ｎ＝５）で判断した。結果を表１に示す。 The solder wettability of each of the electronic component terminal portions of Examples 1 to 8 and the oxide film-treated products obtained in Comparative Examples 1 and 2 and Comparative Example 1 was examined. As the solder, a lead-free tin alloy consisting of 96 mass% of Sn, 3.5 mass% of Ag, and 0.5 mass% of Cu was used. In addition, the meniscograph method was adopted for the evaluation of solder wettability, and the average value (n = 5) of the solder wet time (second) was determined under the following conditions. Table 1 shows the results.
［半田濡れ性評価実験条件］
半田付け温度；２５０℃、浸漬速度；２５ｍｍ／ｓｅｃ、
浸漬深さ；８ｍｍ、浸漬時間；１０秒。
[Solder wettability evaluation experiment conditions]
Soldering temperature: 250 ° C, immersion speed: 25mm / sec,
Immersion depth: 8 mm, immersion time: 10 seconds.
表１からも明らかな様に、本発明の半田濡れ性向上処理剤を使用すると、電子部品保管時における端子部の酸化を抑制し得ると共に、既に形成されている酸化皮膜は積極的に除去することができ、実装時における半田付け工程で、通常のロジン系フラックスより半田濡れ性を大幅に高め得ることが分る。 As is clear from Table 1, when the solder wettability improving agent of the present invention is used, the oxidation of the terminal portion during the storage of the electronic component can be suppressed, and the already formed oxide film is positively removed. It can be seen that, in the soldering process at the time of mounting, the solder wettability can be greatly improved as compared with a normal rosin-based flux.
Claims (10)
Ｒ−ＣＯＯＨ……(I)
［式中、Ｒは炭素数６〜２２の直鎖状または分岐状の飽和または不飽和の脂肪族、脂環
族、もしくは芳香族の炭化水素基を表わす］
Ｒ１・Ｒ２・Ｒ３Ｎ……(II)
［式中、Ｒ１,Ｒ２,Ｒ３は、同一もしくは異なってもよく、水素または炭素数１〜２２の
直鎖状または分枝状の飽和もしくは不飽和の脂肪族、脂環族または芳香族の炭化水素
基を表わす］
Ｒ４・Ｒ５Ｎ-Ｒ６-ＮＲ７・Ｒ８……(III)
［式中、Ｒ４,Ｒ５,Ｒ７,Ｒ８は、水素または炭素数１〜２２の直鎖状または分枝状の飽和
もしくは不飽和の脂肪族、脂環族または芳香族の炭化水素、Ｒ６は炭素数２〜８のア
ルキレン基を表わす］。 The organic acid of the organic acid amine salt is at least one kind of organic acid represented by the following general formula (I), and the amine of the organic acid amine salt is represented by the following general formulas (II) and (III). The treating agent according to claim 1, which is at least one kind of amine.
R-COOH ... (I)
[In the formula, R represents a straight-chain or branched saturated or unsaturated aliphatic, alicyclic, or aromatic hydrocarbon group having 6 to 22 carbon atoms.]
R 1 · R 2 · R 3 N ...... (II)
[Wherein, R 1 , R 2 , and R 3 may be the same or different, and may be hydrogen or a linear or branched saturated or unsaturated aliphatic, alicyclic, or aromatic having 1 to 22 carbon atoms. Represents a group hydrocarbon group]
R 4 · R 5 NR 6 -NR 7 · R 8 (III)
[Wherein R 4 , R 5 , R 7 , and R 8 are hydrogen or a linear or branched saturated or unsaturated aliphatic, alicyclic, or aromatic hydrocarbon having 1 to 22 carbon atoms. , R 6 represents an a alkylene group having 2 to 8 carbon atoms.
Ｒ９-ＯＨ……(IV)
［式中、Ｒ９は、炭素数１〜８の直鎖状または分岐状の脂肪族、脂環族もしくは芳香族
の炭化水素基を表わす］
Ｒ10Ｏ-（Ｒ11-Ｏ）ｎＨ……(V)
［式中、Ｒ10は水素または炭素数１〜４のアルキル基、Ｒ11は炭素数２〜４のアルキレ
ン基、ｎは、１以上の整数を表わす］。 The treatment according to claim 1 or 2, wherein the monohydric alcohol is an alcohol represented by the following general formula (IV), and the glycol is a glycol represented by the following general formula (V) or a half ether thereof. Agent.
R 9 -OH ... (IV)
[Wherein R 9 represents a linear or branched aliphatic, alicyclic or aromatic hydrocarbon group having 1 to 8 carbon atoms]
R 10 O- (R 11 -O) n H ...... (V)
[Wherein, R 10 is hydrogen or an alkyl group having 1 to 4 carbon atoms, R 11 is an alkylene group having 2 to 4 carbon atoms, and n represents an integer of 1 or more].
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