TW201529835A - Cleaning agent composition for removing solder flux residues - Google Patents
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本發明係關於焊料助焊劑殘餘物除去用洗淨劑組合物、焊料助焊劑殘餘物的洗淨方法以及電子部件的製造方法。 The present invention relates to a detergent composition for removing a flux flux residue, a method for cleaning a solder flux residue, and a method for producing an electronic component.
近年來,關於電子部件在印製電路佈線板、陶瓷基板上之安裝,自低消耗電力、高速處理之此類觀點出發,部件進行小型化,在焊料助焊劑之洗淨中需要進行洗淨之間隙逐漸變狹。另外,從環境安全方面出發,無鉛焊料逐漸使用起來,伴隨於此,使用了松香系助焊劑。 In recent years, regarding the mounting of electronic components on printed circuit boards and ceramic substrates, components have been miniaturized from the viewpoint of low power consumption and high-speed processing, and cleaning is required in the cleaning of solder fluxes. The gap gradually narrows. In addition, from the viewpoint of environmental safety, lead-free solder has been gradually used, and rosin-based flux has been used.
專利文獻1中,作為適合洗淨在經焊接之部件的間隙中殘留之助焊劑殘餘物的助焊劑用洗淨劑組合物,公開了含有特定二醇醚、烷醇胺、以及具有碳數1-6之烷基的烷基苯磺酸及/或其鹽、以及水的助焊劑用洗淨劑組合物。 Patent Document 1 discloses a detergent composition for a flux which is suitable for cleaning a flux residue remaining in a gap of a welded member, and contains a specific glycol ether, an alkanolamine, and a carbon number of 1 A detergent composition for a flux of -6 alkyl alkylbenzenesulfonic acid and/or a salt thereof and water.
專利文獻2中,作為不僅對於在狹窄間隙中存在之助焊劑殘餘物的洗淨性高、且利用水之清洗性亦良好、且發泡受到抑制的附著有助焊劑殘餘物之被洗淨物的洗淨方法,公開了使用包含2質量%以上且10質量%以下之水、50質量%以上且不足97.75質量%之二醇醚、以及0.05質量%以上且5質量%以下之胺化合物的洗淨劑,且利用特定洗淨條件及洗淨裝置進行洗淨的方法。 In the case of the patent document 2, the cleaning residue adhered to the flux residue is not only excellent in the detergency of the flux residue existing in the narrow gap, but also excellent in the cleaning property by water, and the foaming is suppressed. In the washing method, it is disclosed that the washing is carried out using water containing 2% by mass or more and 10% by mass or less, 50% by mass or more and less than 97.75% by mass, and 0.05% by mass or more and 5% by mass or less of the amine compound. A method of washing with a specific washing condition and a washing device.
專利文獻 Patent literature
專利文獻1:日本特許公開公報第2009-298940號 Patent Document 1: Japanese Patent Laid-Open Publication No. 2009-298940
專利文獻2:WO2011/081071 Patent Document 2: WO2011/081071
伴隨著近年之無鉛化,1)回流溫度之高溫化、2)焊料金屬中之錫含量增加成為使難以除去的松香酸等之錫鹽在助焊劑殘餘物中增加的誘因,因此存在殘留在現有洗淨劑中之問題。另一方面,洗淨性良好之物質會產生腐蝕用於電極之銅的此類問題。進而,自低消耗電力、高速處理之此類觀點出發,部件進行小型化,要洗淨之間隙逐漸變得狹窄。表面張力低之洗淨劑雖然浸透力高,能夠使狹窄間隙中之助焊劑殘餘物溶解,但由於清洗步驟中使用之水的表面張力高,因此會引起向間隙中浸透速度慢且無法充分清洗之此類問題。專利文獻1之洗淨劑中亦期望進一步提高洗淨性及清洗性。 With the lead-free in recent years, 1) the high temperature of the reflow temperature, and 2) the increase in the tin content in the solder metal is an incentive for increasing the tin salt of rosin acid or the like which is difficult to remove in the flux residue, and thus remains in the existing The problem in detergents. On the other hand, a substance having good detergency causes such a problem of corroding copper for an electrode. Further, from the viewpoint of low power consumption and high-speed processing, the components are miniaturized, and the gap to be washed is gradually narrowed. The detergent having a low surface tension has a high penetration force and can dissolve the flux residue in the narrow gap. However, since the surface tension of the water used in the washing step is high, the permeation rate into the gap is slow and cannot be sufficiently cleaned. Such problems. It is also desired to further improve the detergency and cleanability in the detergent of Patent Document 1.
因此,本發明在一或多個實施形態中,提供焊料助焊劑殘餘物除去用洗淨劑組合物,其對使用焊料助焊劑進行回流後之基板的洗淨性優異。另外,本發明在一或多個實施形態中,提供焊料助焊劑殘餘物除去用洗淨劑組合物,其對使用焊料助焊劑進行回流後之基板的洗淨性、以及向狹窄間隙中之浸透性以及清洗性優異,進而顯示出良好之抑制銅腐蝕性、抑制發泡性、以及安全性(易燃性降低)。 Therefore, in one or more embodiments of the present invention, a detergent composition for removing a flux flux residue is provided, which is excellent in the detergency of a substrate after reflow using a solder flux. Further, in one or more embodiments of the present invention, there is provided a detergent composition for removing a flux flux residue, which is excellent in the detergency of a substrate after reflow using a solder flux and in a narrow gap. It is excellent in the properties and cleanability, and exhibits excellent corrosion inhibition, foaming resistance, and safety (lower flammability).
本發明在一或多個實施形態中係關於焊料助焊劑殘餘物除去用洗淨劑組合物,其含有下述式(I)所示之化合物(成分A)、下述式(II)所示之化合物(成分B)、具有碳數1-6之烷基的烷基苯磺酸及/或其鹽(成分C)、以及水(成分D), 成分A之含量為88.0質量%以上且94.4質量%以下,成分A中,二乙二醇單丁醚之含量為90.0質量%以上且100.0質量%以下,成分B之含量為0.3質量%以上且5.0質量%以下,成分C之含量為0.3質量%以上且5.0質量%以下。 In one or more embodiments, the present invention relates to a detergent composition for removing a flux flux residue, which comprises a compound represented by the following formula (I) (component A) and represented by the following formula (II) a compound (ingredient B), an alkylbenzenesulfonic acid having an alkyl group having 1 to 6 carbon atoms, and/or a salt thereof (ingredient C), and water (ingredient D), The content of the component A is 88.0% by mass or more and 94.4% by mass or less. In the component A, the content of the diethylene glycol monobutyl ether is 90.0% by mass or more and 100.0% by mass or less, and the content of the component B is 0.3% by mass or more and 5.0. The content of the component C is 0.3% by mass or more and 5.0% by mass or less.
[上述式(I)中,R表示碳數3-7之烴基、n為1-5。] [In the above formula (I), R represents a hydrocarbon group having 3 to 7 carbon atoms, and n is 1 to 5. ]
[上述式(II)中,R1為氫原子、甲基、乙基或胺基乙基,R2為氫原子、羥乙基、羥丙基、甲基或乙基,R3為羥乙基或羥丙基。] [In the above formula (II), R 1 is a hydrogen atom, a methyl group, an ethyl group or an aminoethyl group, R 2 is a hydrogen atom, a hydroxyethyl group, a hydroxypropyl group, a methyl group or an ethyl group, and R 3 is a hydroxy group B. Base or hydroxypropyl. ]
本發明在其他一或多個實施形態中,關於焊料助焊劑殘餘物之洗淨方法,其具有利用本發明之洗淨劑組合物對具有回流後之焊料的被洗淨物進行洗淨的步驟。 According to still another embodiment of the present invention, in the method of cleaning a solder flux residue, the method of cleaning a material having a solder after reflow using the detergent composition of the present invention .
本發明在其他一或多個實施形態中,關於包括以下步驟的電子部件之製造方法,亦即,藉由使用助焊劑之焊接而將選自半導體晶片、晶片型電容器、以及電路基板中之至少一種部件搭載於電路基板上的步驟;以及藉由本發明的助焊劑殘餘物之洗淨方法對上述搭載物進行洗淨的步驟。 In another one or more embodiments, the present invention relates to a method of manufacturing an electronic component including the following steps, that is, at least one selected from the group consisting of a semiconductor wafer, a wafer type capacitor, and a circuit substrate by soldering using a flux. A step of mounting a component on a circuit board; and a step of cleaning the package by the method of cleaning the flux residue of the present invention.
根據本發明,在一或多個實施形態中,能夠提供對使用焊料助焊劑進行回流後之基板之洗淨性優異的焊料助焊劑殘餘物除去用洗淨劑組合物、使用其之洗淨方法、以及使用其的電子部件之製造方法。另外,根據本發明,在一或多個實施形態中,能夠提供對使用焊料助焊劑進行回流後之基板的洗淨性、以及向狹窄間隙中之浸透性及清洗 性優異、以及顯示出良好之抑制銅腐蝕性、抑制發泡性、以及安全性(易燃性的降低)的焊料助焊劑殘餘物除去用洗淨劑組合物、使用其之洗淨方法、以及使用其的電子部件之製造方法。 According to the present invention, in one or more embodiments, it is possible to provide a detergent flux-removing detergent composition excellent in detergency of a substrate after reflow using a solder flux, and a cleaning method using the same And a method of manufacturing an electronic component using the same. Further, according to the present invention, in one or more embodiments, it is possible to provide a cleansing property of a substrate after reflow using a solder flux, and a permeability and cleaning into a narrow gap. A detergent composition for removing solder flux residue which exhibits excellent copper corrosion resistance, foaming resistance, and safety (lower flammability), a cleaning method using the same, and a cleaning method using the same A method of manufacturing an electronic component using the same.
本發明基於如下見解:大量配合以二乙二醇單丁醚作為主要成分之二醇醚而製成的洗淨劑組合物,與先前技術相比,其洗淨性提高。另外,本發明亦基於如下見解:該洗淨劑組合物之抑制銅腐蝕性、抑制發泡性、以及安全性(易燃性的降低)良好,且除了洗淨性以外,在向狹窄間隙中之浸透性及清洗性亦能夠提高。 The present invention is based on the insight that a detergent composition prepared by blending a large amount of glycol ether containing diethylene glycol monobutyl ether as a main component has improved detergency as compared with the prior art. Further, the present invention is also based on the insight that the detergent composition has good copper corrosion resistance, foaming inhibition, and safety (decreased flammability), and is in a narrow gap in addition to the detergency. The permeability and cleaning properties can also be improved.
亦即,在本發明之一個實施形態中,關於焊料助焊劑殘餘物除去用洗淨劑組合物(以下,亦稱為「本發明之洗淨劑組合物」。),其含有上述式(I)所示之化合物(成分A)、上述式(II)所示之化合物(成分B)、具有碳數1-6之烷基的烷基苯磺酸及/或其鹽(成分C)、以及水(成分D),成分A之含量為88.0質量%以上且94.4質量%以下,成分A中,二乙二醇單丁醚之含量為90.0質量%以上且100.0質量%以下,成分B之含量為0.3質量%以上且5.0質量%以下,成分C之含量為0.3質量%以上且5.0質量%以下。 In one embodiment of the present invention, the detergent flux removal composition for solder flux residue (hereinafter also referred to as "the detergent composition of the present invention") contains the above formula (I). a compound (ingredient A), a compound represented by the above formula (II) (ingredient B), an alkylbenzenesulfonic acid having an alkyl group having 1 to 6 carbon atoms, and/or a salt thereof (ingredient C), and Water (component D), the content of the component A is 88.0% by mass or more and 94.4% by mass or less, and the content of the diethylene glycol monobutyl ether in the component A is 90.0% by mass or more and 100.0% by mass or less, and the content of the component B is 0.3% by mass or more and 5.0% by mass or less, and the content of the component C is 0.3% by mass or more and 5.0% by mass or less.
本發明之洗淨劑組合物的效果作用機理之詳細情況雖然有不明確之部分,但可推定如下所述。亦即,可認為二乙二醇單丁醚與焊料助焊劑之親和性高,因而藉由大量含有以二乙二醇單丁醚為主要成分之二醇醚(成分A),從而使洗淨劑組合物之表面張力變低,將狹窄間隙之焊料助焊劑殘餘物溶解且進行洗淨,結果,利用基於由特定烷醇 胺(成分B)及烷基苯磺酸或其鹽(成分C)所帶來之向焊料助焊劑殘餘物中之浸透而致的膨潤作用,從而使基於成分A之洗淨性得以提高。另外,亦認為利用水進行清洗時,藉由本發明之洗淨劑組合物中的特定烷醇胺(成分B)及烷基苯磺酸或其鹽(成分C)以及水(成分D),從而使二乙二醇單丁醚與清洗水之親和性得以提高,清洗性優異。而且,藉由將烷醇胺(成分B)設定為特定範圍的量,從而抑制銅的腐蝕。進而,藉由將各成分設定為特定量,從而良好地維持發泡性與安全性。但本發明亦可不限於該機理地進行解釋。 Although the details of the mechanism of action of the detergent composition of the present invention are not clear, they can be estimated as follows. In other words, diethylene glycol monobutyl ether is considered to have high affinity with the solder flux, so that the glycol ether (ingredient A) containing diethylene glycol monobutyl ether as a main component is contained in a large amount, so that the cleaning is performed. The surface tension of the agent composition is lowered, and the solder flux residue in the narrow gap is dissolved and washed, and as a result, the use is based on the specific alkanol. The swelling by the penetration of the amine (ingredient B) and the alkylbenzenesulfonic acid or its salt (ingredient C) into the solder flux residue improves the detergency based on the component A. Further, it is also considered that when washing with water, the specific alkanolamine (component B) and the alkylbenzenesulfonic acid or its salt (component C) and water (component D) in the detergent composition of the present invention are The affinity between diethylene glycol monobutyl ether and washing water is improved, and the cleaning property is excellent. Further, by setting the alkanolamine (component B) to a specific range, corrosion of copper is suppressed. Further, by setting each component to a specific amount, the foaming property and safety are favorably maintained. However, the invention may also be construed without being limited to this mechanism.
本發明中「助焊劑」係指在焊接中使用的含有松香或松香衍生物之松香系助焊劑,本發明中「焊接」包括回流方式及流體方式之焊接。本發明中「焊料助焊劑」係指焊料與助焊劑之混合物。若在電路基板上層疊其他部件(例如,半導體晶片、晶片型電容器、其他電路基板等)且搭載,則在上述電路基板與上述其他部件之間形成空間(間隙)。用於上述搭載之助焊劑藉由回流等而焊接後,亦會以助焊劑殘餘物之形式殘留在該間隙中。本發明中「焊料助焊劑殘餘物除去用洗淨劑組合物」係指,用於對使用助焊劑或焊料助焊劑進行焊接後之助焊劑殘餘物進行洗淨的洗淨劑組合物。自利用本發明之洗淨劑組合物之洗淨性及向狹窄間隙中之浸透性顯示出顯著效果的觀點出發,焊料較佳為無鉛(Pb)焊料。 In the present invention, "flux" means a rosin-based flux containing rosin or a rosin derivative used in welding, and "welding" in the present invention includes reflow type and fluid type welding. In the present invention, "solder flux" means a mixture of solder and flux. When another member (for example, a semiconductor wafer, a wafer type capacitor, or another circuit board) is mounted on a circuit board and mounted, a space (gap) is formed between the circuit board and the other member. The solder used for the above-described soldering is soldered by reflow or the like, and remains in the gap as a flux residue. In the present invention, the "cleaner composition for removing solder flux residue" means a detergent composition for cleaning a flux residue after soldering using a flux or a solder flux. The solder is preferably a lead-free (Pb) solder from the viewpoint of exhibiting a remarkable effect of the detergency of the detergent composition of the present invention and the permeability to a narrow gap.
本發明之洗淨劑組合物中的成分A為下述式(I)所示之一或多種(聚)乙二醇單烷基醚。 Component A in the detergent composition of the present invention is one or more (poly)ethylene glycol monoalkyl ethers represented by the following formula (I).
[式(I)中,R表示碳數3-7之烴基、n為1-5。] In the formula (I), R represents a hydrocarbon group having 3 to 7 carbon atoms, and n is 1 to 5. ]
上述式(I)中,自提高對殘留於間隙之助焊劑殘餘物的洗淨性的觀點出發,較佳R為碳數3-7之烴基、較佳為碳數3-6之烴基、更佳為 碳數4-6之烴基。R在一或多個實施形態中,包括丙基、丁基、戊基、己基。自提高對殘留於間隙之助焊劑殘餘物的洗淨性的觀點出發,平均加成莫耳數n為1-5、較佳為1-3、更佳為2或3。烴基較佳為烷基、烯基以及芳基,更佳為烷基。 In the above formula (I), from the viewpoint of improving the detergency of the flux residue remaining in the gap, R is preferably a hydrocarbon group having 3 to 7 carbon atoms, preferably a hydrocarbon group having 3 to 6 carbon atoms, and more preferably Good for A hydrocarbon group having 4 to 6 carbon atoms. R, in one or more embodiments, includes propyl, butyl, pentyl, hexyl. The average addition mole number n is from 1 to 5, preferably from 1 to 3, more preferably 2 or 3 from the viewpoint of improving the detergency of the flux residue remaining in the gap. The hydrocarbon group is preferably an alkyl group, an alkenyl group and an aryl group, more preferably an alkyl group.
本發明之洗淨劑組合物中的成分A至少包含二乙二醇單丁醚(式(I)中,R為丁基、n=2)。需要說明的是,在本發明中,丁基在沒有特別說明的情況下,係指正丁基。 Component A in the detergent composition of the present invention contains at least diethylene glycol monobutyl ether (in the formula (I), R is a butyl group, n = 2). In the present invention, the butyl group means n-butyl group unless otherwise specified.
作為除了二乙二醇單丁醚以外的成分A,在一或多個實施形態中,自提高對殘留於間隙之助焊劑殘餘物的洗淨性的觀點出發,較佳為二乙二醇單異丙醚、二乙二醇單異丁醚、二乙二醇單己醚等二乙二醇單烷基醚;二乙二醇單烯丙醚等二乙二醇單烯基醚;二乙二醇單苄醚等二乙二醇單芳基醚;三乙二醇單異丙醚、三乙二醇單丁醚、三乙二醇單異丁醚等三乙二醇單烷基醚;三乙二醇單烯丙醚等三乙二醇單烯基醚;四乙二醇單丁醚等四乙二醇單烷基醚;五乙二醇單丁醚等五乙二醇單烷基醚。在此等醚當中,自相同觀點出發,更佳為二乙二醇單異丙醚、二乙二醇單異丁醚、二乙二醇單己醚;三乙二醇單異丙醚。另外,除了二乙二醇單丁醚以外的成分A在一或多個實施形態中,自提高向狹窄間隙中之浸透性的觀點出發,較佳為三乙二醇單丁醚。 In the one or more embodiments, the component A other than the diethylene glycol monobutyl ether is preferably a diethylene glycol single from the viewpoint of improving the detergency of the flux residue remaining in the gap. Diethylene glycol monoalkyl ether such as diisopropyl ether, diethylene glycol monoisobutyl ether or diethylene glycol monohexyl ether; diethylene glycol monoalkenyl ether such as diethylene glycol monoallyl ether; a diethylene glycol monoaryl ether such as diol monobenzyl ether; a triethylene glycol monoalkyl ether such as triethylene glycol monoisopropyl ether, triethylene glycol monobutyl ether or triethylene glycol monoisobutyl ether; Triethylene glycol monoalkenyl ether such as triethylene glycol monoallyl ether; tetraethylene glycol monoalkyl ether such as tetraethylene glycol monobutyl ether; pentaethylene glycol monoalkyl group such as pentaethylene glycol monobutyl ether ether. Among these ethers, diethylene glycol monoisopropyl ether, diethylene glycol monoisobutyl ether, diethylene glycol monohexyl ether, and triethylene glycol monoisopropyl ether are more preferable from the same viewpoint. Further, in the one or more embodiments, the component A other than the diethylene glycol monobutyl ether is preferably triethylene glycol monobutyl ether from the viewpoint of improving the permeability to the narrow gap.
另外,就本發明之洗淨劑組合物中的成分A而言,作為除了二乙二醇單丁醚(閃點120℃)以外之成分,在一或多個實施形態中,自閃點高且安全性優異、對殘留於間隙之助焊劑殘餘物的洗淨性亦優異之此類觀點出發,較佳為二乙二醇單異丁醚(閃點112℃)、二乙二醇單己醚(閃點141℃)、二乙二醇單苄醚(閃點158℃)、三乙二醇單異丙醚、三乙二醇單丁醚(閃點156℃)、三乙二醇單異丁醚、三乙二醇單烯丙醚。在此等醚當中,自相同觀點出發,更佳為二乙二醇單丁醚、 二乙二醇單異丁醚、二乙二醇單己醚、三乙二醇單異丙醚。 Further, in the component A of the detergent composition of the present invention, as a component other than diethylene glycol monobutyl ether (flash point 120 ° C), in one or more embodiments, the self-flash point is high. Further, it is excellent in safety and excellent in the detergency of the flux residue remaining in the gap, preferably diethylene glycol monoisobutyl ether (flash point 112 ° C), diethylene glycol alone Ether (flash point 141 ° C), diethylene glycol monobenzyl ether (flash point 158 ° C), triethylene glycol monoisopropyl ether, triethylene glycol monobutyl ether (flash point 156 ° C), triethylene glycol single Isobutyl ether, triethylene glycol monoallyl ether. Among these ethers, from the same viewpoint, it is more preferably diethylene glycol monobutyl ether, Diethylene glycol monoisobutyl ether, diethylene glycol monohexyl ether, triethylene glycol monoisopropyl ether.
進而,就本發明之洗淨劑組合物中的成分A而言,作為除了二乙二醇單丁醚以外之成分,在一或多個實施形態中,自不僅距離閃點之安全性以及對殘留於間隙之助焊劑殘餘物的洗淨性優異,且水溶性優異且製劑化亦優異之此類觀點出發,較佳為二乙二醇單異丁醚、二乙二醇單苄醚、三乙二醇單異丙醚、三乙二醇單丁醚、三乙二醇單異丁醚、三乙二醇單烯丙醚。在此等醚當中,自相同觀點出發,更佳為二乙二醇單丁醚、二乙二醇單異丁醚、二乙二醇單苄醚、三乙二醇單異丙醚、三乙二醇單丁醚、三乙二醇單異丁醚、三乙二醇單烯丙醚,進一步較佳為二乙二醇單丁醚、二乙二醇單異丁醚、三乙二醇單異丙醚。 Further, in the component A of the detergent composition of the present invention, as a component other than diethylene glycol monobutyl ether, in one or more embodiments, safety from not only the distance from the flash point but also From the viewpoint of excellent detergency of the flux residue remaining in the gap, excellent water solubility, and excellent formulation, diethylene glycol monoisobutyl ether, diethylene glycol monobenzyl ether, and three are preferable. Ethylene glycol monoisopropyl ether, triethylene glycol monobutyl ether, triethylene glycol monoisobutyl ether, triethylene glycol monoallyl ether. Among these ethers, from the same viewpoint, it is more preferably diethylene glycol monobutyl ether, diethylene glycol monoisobutyl ether, diethylene glycol monobenzyl ether, triethylene glycol monoisopropyl ether, triethyl The diol monobutyl ether, triethylene glycol monoisobutyl ether, triethylene glycol monoallyl ether, further preferably diethylene glycol monobutyl ether, diethylene glycol monoisobutyl ether, triethylene glycol single Isopropyl ether.
就本發明之洗淨劑組合物中的成分A之含量而言,在一或多個實施形態中,自提高對殘留於間隙之助焊劑殘餘物的洗淨性的觀點出發,其為88.0質量%以上、較佳為88.5質量%以上、更佳為89.0質量%以上、進一步較佳為89.4質量%以上。另外,就成分A之含量而言,在一或多個實施形態中,自相同觀點出發,其為94.4質量%以下、較佳為93.0質量%以下、更佳為92.0質量%以下、進一步較佳為91.0質量%以下。另外,就成分A之含量而言,在一或多個實施形態中,自相同觀點出發,其為88.0質量%以上且94.4質量%以下、較佳為88.5質量%以上且93.0質量%以下、更佳為89.0質量%以上且92.0質量%以下、進一步較佳為89.4質量%以上且91.0質量%以下。如上所述,成分A雖然包含二乙二醇單丁醚,但亦可以單獨為二乙二醇單丁醚,亦可包含除了二乙二醇單丁醚以外的上述式(I)所示之一或多種化合物。 In the one or more embodiments, the content of the component A in the detergent composition of the present invention is 88.0 by mass from the viewpoint of improving the detergency of the flux residue remaining in the gap. % or more, preferably 88.5 mass% or more, more preferably 89.0 mass% or more, further preferably 89.4 mass% or more. Further, the content of the component A is, in one or more embodiments, from the same viewpoint, it is 94.4% by mass or less, preferably 93.0% by mass or less, more preferably 92.0% by mass or less, further preferably It is 91.0% by mass or less. In addition, in one or more embodiments, the content of the component A is from 88.0% by mass to 94.4% by mass, preferably from 8.85% by mass to 93.0% by mass, more preferably from the same viewpoint. It is preferably 89.0% by mass or more and 92.0% by mass or less, and more preferably 89.4% by mass or more and 91.0% by mass or less. As described above, the component A contains diethylene glycol monobutyl ether, but may be diethylene glycol monobutyl ether alone or may contain the above formula (I) other than diethylene glycol monobutyl ether. One or more compounds.
就本發明之洗淨劑組合物中的二乙二醇單丁醚在成分A中的含量而言,在一或多個實施形態中,自提高對殘留於間隙之助焊劑殘餘物的洗淨性的觀點出發,其為90.0質量%以上、較佳為93.0質量%以 上、更佳為94.0質量%以上、進一步較佳為96.0質量%以上、更進一步較佳為98.0質量%以上。另外,就二乙二醇單丁醚在成分A中之含量而言,在一或多個實施形態中,自相同觀點出發,其為100.0質量%以下。 In the case of the content of the diethylene glycol monobutyl ether in the detergent composition of the present invention in the component A, in one or more embodiments, the cleaning of the flux residue remaining in the gap is improved. From the viewpoint of properties, it is 90.0% by mass or more, preferably 93.0% by mass. The amount is more preferably 94.0% by mass or more, further preferably 96.0% by mass or more, and still more preferably 98.0% by mass or more. Further, the content of the diethylene glycol monobutyl ether in the component A is, in one or more embodiments, 100.0% by mass or less from the same viewpoint.
就本發明之洗淨劑組合物中的二乙二醇單丁醚在洗淨劑組合物中的含量而言,在一或多個實施形態中,自提高對殘留於間隙之助焊劑殘餘物的洗淨性的觀點出發,其較佳為88.0質量%以上、更佳為88.5質量%以上、進一步較佳為89.0質量%以上、更進一步較佳為89.4質量%以上。另外,就二乙二醇單丁醚在洗淨劑組合物中之含量而言,在一或多個實施形態中,自相同觀點出發,較佳為94.4質量%以下、更佳為93.0質量%以下、進一步較佳為92.0質量%以下、更進一步較佳為91.0質量%以下。另外,就二乙二醇單丁醚之含量而言,在一或多個實施形態中,自相同觀點出發,其較佳為88.0質量%以上且94.4質量%以下、更佳為88.5質量%以上且93.0質量%以下、進一步較佳為89.0質量%以上且92.0質量%以下、更進一步較佳為89.4質量%以上且91.0質量%以下。 For the content of diethylene glycol monobutyl ether in the detergent composition of the present invention, in one or more embodiments, self-improving the flux residue remaining in the gap The viewpoint of the detergency is preferably 88.0% by mass or more, more preferably 88.5 mass% or more, further preferably 89.0 mass% or more, and still more preferably 89.4 mass% or more. Further, the content of the diethylene glycol monobutyl ether in the detergent composition is preferably, in one or more embodiments, from the same viewpoint, it is preferably 94.4% by mass or less, more preferably 93.0% by mass. The amount is more preferably 92.0% by mass or less, and still more preferably 91.0% by mass or less. In addition, in one or more embodiments, the content of diethylene glycol monobutyl ether is preferably 88.0% by mass or more and 94.4% by mass or less, and more preferably 88.5 % by mass or more from the same viewpoint. Further, it is 93.0% by mass or less, more preferably 89.0% by mass or more and 92.0% by mass or less, and still more preferably 89.4% by mass or more and 91.0% by mass or less.
在本發明之洗淨劑組合物中包含除了二乙二醇單丁醚以外的成分A的情況下,就其在成分A中的含量(在為多種的情況下為總含量)而言,在一或多個實施形態中,自不會妨礙提高對殘留於間隙之助焊劑殘餘物的洗淨性的觀點出發,較佳為10質量%以下、更佳為7.0質量%以下、進一步較佳為6.0質量%以下、更進一步較佳為4.0質量%以下、更進一步較佳為2.0質量%以下。 In the case where the component A other than diethylene glycol monobutyl ether is contained in the detergent composition of the present invention, the content thereof in the component A (in the case of a plurality of cases, the total content) is In one or more embodiments, from the viewpoint of preventing the improvement of the detergency of the flux residue remaining in the gap, it is preferably 10% by mass or less, more preferably 7.0% by mass or less, further preferably 6.0% by mass or less, more preferably 4.0% by mass or less, still more preferably 2.0% by mass or less.
在本發明之洗淨劑組合物中包含除了二乙二醇單丁醚以外的成分A的情況下,就其在洗淨劑組合物中之含量(在為多種之情況下為總含量)而言,在一或多個實施形態中,自不會妨礙提高對殘留於間隙之助焊劑殘餘物的洗淨性的觀點出發,較佳為8.0質量%以下、更佳為 6.0質量%以下、進一步較佳為5.0質量%以下。另外,在本發明之洗淨劑組合物中包含除了二乙二醇單丁醚以外的成分A的情況下,就其在洗淨劑組合物中之含量(在為多種之情況下為總含量)而言,在一或多個實施形態中,較佳為1.0質量%以上、更佳為2.0質量%以上、進一步較佳為3.0質量%以上。 In the case where the detergent composition of the present invention contains the component A other than diethylene glycol monobutyl ether, its content in the detergent composition (in a plurality of cases, the total content) In one or more embodiments, from the viewpoint of not impeding the improvement of the detergency of the flux residue remaining in the gap, it is preferably 8.0% by mass or less, more preferably 6.0% by mass or less, and more preferably 5.0% by mass or less. Further, in the case where the detergent composition of the present invention contains the component A other than diethylene glycol monobutyl ether, its content in the detergent composition (in a plurality of cases, the total content) In one or more embodiments, it is preferably 1.0% by mass or more, more preferably 2.0% by mass or more, and still more preferably 3.0% by mass or more.
本發明之洗淨劑組合物中的成分B為下述式(II)所示之一或多種烷醇胺。 Component B in the detergent composition of the present invention is one or more of the alkanolamines represented by the following formula (II).
[上述式(II)中,R1為氫原子、甲基、乙基或胺基乙基,R2為氫原子、羥乙基、羥丙基、甲基或乙基,R3為羥乙基或羥丙基。] [In the above formula (II), R 1 is a hydrogen atom, a methyl group, an ethyl group or an aminoethyl group, R 2 is a hydrogen atom, a hydroxyethyl group, a hydroxypropyl group, a methyl group or an ethyl group, and R 3 is a hydroxy group B. Base or hydroxypropyl. ]
作為成分B之烷醇胺,在一或多個實施形態中,可列舉出單乙醇胺、二乙醇胺、以及其烷基化物以及胺基烷基化物,自提高對殘留於間隙之助焊劑殘餘物的洗淨性的觀點出發,較佳為單乙醇胺、二乙醇胺、單甲基單乙醇胺、單甲基二乙醇胺、二甲基單乙醇胺、單乙基單乙醇胺、單乙基二乙醇胺以及單胺基乙基異丙醇胺,更佳為二乙醇胺、單乙基單乙醇胺、單甲基二乙醇胺以及單胺基乙基異丙醇胺,進一步較佳為單乙基單乙醇胺及單甲基二乙醇胺。 As the alkanolamine of the component B, in one or more embodiments, monoethanolamine, diethanolamine, an alkylate thereof, and an aminoalkylate may be mentioned, since the flux residue remaining in the gap is increased. From the viewpoint of detergency, preferred are monoethanolamine, diethanolamine, monomethylmonoethanolamine, monomethyldiethanolamine, dimethylmonoethanolamine, monoethylmonoethanolamine, monoethyldiethanolamine, and monoamine B. The isopropanolamine is more preferably diethanolamine, monoethylmonoethanolamine, monomethyldiethanolamine or monoaminoethylisopropanolamine, and further preferably monoethylmonoethanolamine and monomethyldiethanolamine.
就本發明之洗淨劑組合物中的成分B之含量而言,在一或多個實施形態中,自提高對殘留於間隙之助焊劑殘餘物的洗淨性的觀點出發,其為0.3質量%以上、較佳為0.5質量%以上、更佳為1.0質量%以上、進一步較佳為1.5質量%以上。另外,就成分B之含量而言,在一或多個實施形態中,自相同觀點出發,其為5.0質量%以下、較佳為4.5質量%以下、更佳為4.0質量%以下、進一步較佳為3.5質量%以 下。另外,就成分B之含量而言,在一或多個實施形態中,自相同觀點出發,其為0.3質量%以上且5.0質量%以下、較佳為0.5質量%以上且4.5質量%以下、更佳為1.0質量%以上且4.0質量%以下、進一步較佳為1.5質量%以上且3.5質量%以下。如上所述,成分B可為上述式(II)所示之單獨化合物,亦可包含上述式(II)所示之多種化合物。 In the one or more embodiments, the content of the component B in the detergent composition of the present invention is 0.3 mass from the viewpoint of improving the detergency of the flux residue remaining in the gap. % or more, preferably 0.5% by mass or more, more preferably 1.0% by mass or more, and still more preferably 1.5% by mass or more. In addition, in one or more embodiments, the content of the component B is 5.0% by mass or less, preferably 4.5% by mass or less, more preferably 4.0% by mass or less, further preferably from the same viewpoint. Is 3.5% by mass under. In addition, in one or more embodiments, the content of the component B is 0.3% by mass or more and 5.0% by mass or less, preferably 0.5% by mass or more and 4.5% by mass or less, more preferably from the same viewpoint. It is preferably 1.0% by mass or more and 4.0% by mass or less, and more preferably 1.5% by mass or more and 3.5% by mass or less. As described above, the component B may be a single compound represented by the above formula (II), or may contain a plurality of compounds represented by the above formula (II).
本發明之洗淨劑組合物中的成分C包含一或多種具有碳數1-6之烷基的烷基苯磺酸及/或其鹽。在烷基苯磺酸中可具有多個烷基,在此情況下,多個烷基之碳數的總計為碳數1-6。就成分C之烷基苯磺酸及/或其鹽中之烷基的碳數而言,在一或多個實施形態中,自提高對殘留於間隙之助焊劑殘餘物的洗淨力的觀點出發,其為1-6、較佳為1-4、更佳為1-3、進一步較佳為1或2、更進一步較佳為1。作為具有碳數1-6之烷基的烷基苯磺酸之鹽,自允許作為洗淨劑組合物之觀點出發,較佳為鈉、鉀等鹼金屬鹽、銨鹽、有機胺鹽,自半導體品質之穩定性的觀點出發,進一步較佳為金屬離子不會殘留之銨鹽、有機胺鹽。另外,有機胺鹽亦可為基於成分B之鹽。 The component C in the detergent composition of the present invention contains one or more alkylbenzenesulfonic acids having an alkyl group having 1 to 6 carbon atoms and/or a salt thereof. The alkylbenzenesulfonic acid may have a plurality of alkyl groups, and in this case, the total number of carbon atoms of the plurality of alkyl groups is 1-6. With respect to the carbon number of the alkyl group in the alkylbenzenesulfonic acid of the component C and/or its salt, in one or more embodiments, the viewpoint of improving the detergency of the flux residue remaining in the gap Starting, it is 1-6, preferably 1-4, more preferably 1-3, still more preferably 1 or 2, still more preferably 1. The salt of an alkylbenzenesulfonic acid having an alkyl group having 1 to 6 carbon atoms is preferably an alkali metal salt such as sodium or potassium, an ammonium salt or an organic amine salt, from the viewpoint of allowing the composition to be a detergent. From the viewpoint of the stability of the semiconductor quality, an ammonium salt or an organic amine salt in which metal ions do not remain is more preferable. Further, the organic amine salt may also be a salt based on the component B.
作為在成分C中包含之烷基苯磺酸及/或其鹽,在一或多個實施形態中,自提高對殘留於間隙之助焊劑殘餘物的洗淨力的觀點出發,可列舉出甲苯磺酸、二甲苯磺酸、乙基苯磺酸、丙基苯磺酸、異丙基苯磺酸、丁基苯磺酸、戊基苯磺酸、己基苯磺酸、2,4-二甲基苯磺酸、二丙基苯磺酸、及/或其鹽,其可為鄰位、間位、對位中之任一者。成分C在一或多個實施形態中,自相同觀點出發,更佳為對甲苯磺酸、二甲苯磺酸、乙基苯磺酸、丁基苯磺酸、及/或其鹽,進一步較佳為對甲苯磺酸。 The alkylbenzenesulfonic acid and/or its salt contained in the component C may, in one or more embodiments, be a toluene from the viewpoint of improving the detergency of the flux residue remaining in the gap. Sulfonic acid, xylenesulfonic acid, ethylbenzenesulfonic acid, propylbenzenesulfonic acid, cumenesulfonic acid, butylbenzenesulfonic acid, pentylbenzenesulfonic acid, hexylbenzenesulfonic acid, 2,4-dimethyl Alkylbenzenesulfonic acid, dipropylbenzenesulfonic acid, and/or a salt thereof, which may be any of an ortho, meta or para. In one or more embodiments, component C is more preferably p-toluenesulfonic acid, xylenesulfonic acid, ethylbenzenesulfonic acid, butylbenzenesulfonic acid, and/or a salt thereof from the same viewpoint, and further preferably. For p-toluenesulfonic acid.
就本發明之洗淨劑組合物中的成分C之含量而言,在一或多個實施形態中,其為0.3質量%以上且5.0質量%以下,自提高對殘留於間 隙之助焊劑殘餘物的洗淨力的觀點出發,較佳為0.4質量%以上、更佳為0.5質量%以上,而且,自提高洗淨劑組合物在間隙中之浸透性的觀點出發,較佳為4.5質量%以下、更佳為4.0質量%以下、進一步較佳為3.0質量%以下。如上所述,成分C可為單獨化合物,亦可包含多種化合物。就在成分C為鹽之情況下的成分C之含量而言,換算成酸型而計算其含量。 In one or more embodiments, the content of the component C in the detergent composition of the present invention is 0.3% by mass or more and 5.0% by mass or less. From the viewpoint of the cleaning power of the flux residue, it is preferably 0.4% by mass or more, more preferably 0.5% by mass or more, and from the viewpoint of improving the permeability of the detergent composition in the gap, It is preferably 4.5% by mass or less, more preferably 4.0% by mass or less, still more preferably 3.0% by mass or less. As described above, the component C may be a single compound or may contain a plurality of compounds. The content of the component C in the case where the component C is a salt is calculated in terms of an acid form.
本發明之洗淨劑組合物中的成分D為水。水可使用蒸餾水、離子交換水、或超純水等。就本發明之洗淨劑組合物中的成分D之含量而言,在一或多個實施形態中,自降低易燃性之觀點出發,較佳為5.0質量%以上、更佳為5.5質量%以上、進一步較佳為6.5質量%以上。另外,就成分D之含量而言,在一或多個實施形態中,自提高對殘留於間隙之助焊劑殘餘物的洗淨力的觀點出發,較佳為10.0質量%以下、更佳為9.0質量%以下、進一步較佳為8.0質量%以下。就成分D之含量而言,在一或多個實施形態中,自提高對殘留於間隙之助焊劑殘餘物的洗淨力的觀點以及降低易燃性的觀點出發,較佳為5.0質量%以上且10.0質量%以下、更佳為5.5質量%以上且9.0質量%以下、進一步較佳為6.5質量%以上且8.0質量%以下。 Component D in the detergent composition of the present invention is water. As the water, distilled water, ion-exchanged water, or ultrapure water can be used. In one or more embodiments, the content of the component D in the detergent composition of the present invention is preferably 5.0% by mass or more, and more preferably 5.5% by mass from the viewpoint of reducing flammability. The above is more preferably 6.5 mass% or more. In addition, the content of the component D is preferably 10.0% by mass or less, more preferably 9.0, from the viewpoint of improving the detergency of the flux residue remaining in the gap in one or more embodiments. The mass% or less is more preferably 8.0 mass% or less. In one or more embodiments, the content of the component D is preferably 5.0% by mass or more from the viewpoint of improving the detergency of the flux residue remaining in the gap and reducing the flammability. Further, it is 10.0% by mass or less, more preferably 5.5% by mass or more and 9.0% by mass or less, further preferably 6.5% by mass or more and 8.0% by mass or less.
就成分A與成分D之質量比〔A/D〕而言,在一或多個實施形態中,自提高對殘留於間隙之助焊劑殘餘物的洗淨性的觀點出發,較佳為10.0以上、更佳為11.0以上、進一步較佳為12.0以上。就成分A與成分D之質量比〔A/D〕而言,在一或多個實施形態中,自提高對殘留於間隙之助焊劑殘餘物的洗淨性的觀點以及降低閃點而提高安全性的觀點出發,較佳為19.0以下、更佳為17.0以下、進一步較佳為14.0以下。 In the one or more embodiments, the mass ratio [A/D] of the component A to the component D is preferably 10.0 or more from the viewpoint of improving the detergency of the flux residue remaining in the gap. More preferably, it is 11.0 or more, and further preferably 12.0 or more. In the mass ratio [A/D] of the component A to the component D, in one or more embodiments, the safety is improved from the viewpoint of improving the detergency of the flux residue remaining in the gap and reducing the flash point. From the viewpoint of properties, it is preferably 19.0 or less, more preferably 17.0 or less, still more preferably 14.0 or less.
就本發明之洗淨劑組合物中成分A、B以及C的質量比(成分A/成 分B/成分C)而言,在一或多個實施形態中,自提高洗淨劑組合物之處置性以及提高對殘留於間隙之助焊劑殘餘物的洗淨力的觀點出發,較佳為89.7-99.4/0.3-5.4/0.3-5.4、更佳為91.0-98.6/1.0-5.0/0.4-4.0、進一步較佳為94.0-98.0/1.5-4.0/0.5-2.0。其中,成分A、成分B、成分C之總計為100.0。 The mass ratio of the components A, B and C in the detergent composition of the present invention (ingredient A/forming In the case of the component B or the component C), it is preferred from the viewpoint of improving the handleability of the detergent composition and improving the detergency of the flux residue remaining in the gap in one or more embodiments. 89.7-99.4/0.3-5.4/0.3-5.4, more preferably 91.0-98.6/1.0-5.0/0.4-4.0, further preferably 94.0-98.0/1.5-4.0/0.5-2.0. The total of the component A, the component B, and the component C was 100.0.
就本發明之洗淨劑組合物中成分A、B、C以及D的總含量而言,在一或多個實施形態中,自提高對殘留於間隙之助焊劑殘餘物的洗淨力的觀點出發,較佳為98.0質量%以上且100質量%以下、更佳為99.0質量%以上且100質量%以下、進一步較佳為99.5質量%以上且100質量%以下、進一步更佳為99.7質量%以上且100質量%以下。因此,就本發明之洗淨劑組合物而言,在一或多個實施形態中,可在較佳為0質量%以上且2.0質量%以下、更佳為0質量%以上且1.0質量%以下、進一步較佳為0質量%以上且0.3質量%以下、進一步更佳為0質量%以上且0.1質量%以下的範圍內包含其他成分。 With respect to the total content of the components A, B, C and D in the detergent composition of the present invention, in one or more embodiments, the viewpoint of improving the detergency of the flux residue remaining in the gap The starting point is preferably 98.0% by mass or more and 100% by mass or less, more preferably 99.0% by mass or more and 100% by mass or less, further preferably 99.5% by mass or more and 100% by mass or less, and still more preferably 99.7% by mass or more. And 100% by mass or less. Therefore, in the one or more embodiments, the detergent composition of the present invention may preferably be 0% by mass or more and 2.0% by mass or less, more preferably 0% by mass or more and 1.0% by mass or less. Further, it is more preferably 0% by mass or more and 0.3% by mass or less, and still more preferably 0% by mass or more and 0.1% by mass or less.
作為本發明之洗淨劑組合物中的其他成分,在一或多個實施形態中,自提高清洗性之觀點出發,可列舉出聚伸烷基二醇烷基胺型非離子界面活性劑。作為聚伸烷基二醇烷基胺型非離子界面活性劑,在一或多個實施形態中,可列舉出下述式(III)所示之化合物。 The other component in the detergent composition of the present invention may, in one or more embodiments, be a polyalkylene glycol alkylamine type nonionic surfactant from the viewpoint of improving the cleaning property. The polyalkylene glycol alkylamine type nonionic surfactant may, in one or more embodiments, be a compound represented by the following formula (III).
[式(III)中,R4表示碳數8-18之烴基、EO表示氧化乙烯基、n以及m分別表示EO之平均加成莫耳數。] In the formula (III), R 4 represents a hydrocarbon group having a carbon number of 8 to 18, EO represents an oxyethylene group, and n and m each represent an average addition molar number of EO. ]
上述式(III)中,自提高清洗性之觀點出發,R4較佳為碳數10-14之烴基,自相同觀點出發,n+m較佳為3以上且6以下。 In the above formula (III), R 4 is preferably a hydrocarbon group having 10 to 14 carbon atoms from the viewpoint of improving the cleaning property, and from the same viewpoint, n + m is preferably 3 or more and 6 or less.
作為本發明之洗淨劑組合物中的其他成分,在其他一或多個實 施形態中,自抑制發泡性之觀點出發,可列舉出碳數10-18的具有或不具有不飽和鍵之烴。作為烴,在一或多個實施形態中,自相同觀點出發,可列舉出十二碳烯、十四碳烯。 As other components in the detergent composition of the present invention, in one or more other In the embodiment, from the viewpoint of suppressing foaming property, a hydrocarbon having 10 to 18 carbon atoms with or without an unsaturated bond can be cited. As a hydrocarbon, in one or more embodiments, dodecene and tetradecene are mentioned from the same viewpoint.
作為本發明之洗淨劑組合物中的其他成分,在其他一或多個實施形態中,可列舉出下述式(IV)所示之非離子界面活性劑。 The other component in the detergent composition of the present invention may, for example, be a nonionic surfactant represented by the following formula (IV).
[式(IV)中,R5表示碳數8-18之烴基、EO表示氧化乙烯基、PO表示氧化丙烯基。p、q、以及r分別表示EO、PO之平均加成莫耳數,分別為0-15之數,p及r不同時為0,且在q>0之情況下qp+r30,在q=0之情況下r=0。] In the formula (IV), R 5 represents a hydrocarbon group having a carbon number of 8 to 18, EO represents an oxyethylene group, and PO represents an oxypropylene group. p, q, and r represent the average addition moles of EO and PO, respectively, which are 0-15, and p and r are different at 0, and q is 0. p+r 30, r=0 in the case of q=0. ]
進一步而言,作為其他成分,本發明之洗淨劑組合物可在不損害本發明效果之範圍內根據需要適當地並用通常用於洗淨劑中的羥乙基胺基乙酸、羥乙基亞胺基二乙酸、乙二胺四乙酸等胺基羧酸鹽等具有螯合力的化合物、防腐劑、防銹劑、殺菌劑、抗菌劑、矽酮系消泡劑、抗氧化劑、椰子油脂肪酸甲酯或乙酸苄酯等酯或醇類等。 Further, as the other component, the detergent composition of the present invention can be used in combination with hydroxyethylaminoacetic acid or hydroxyethyl group which is usually used in a detergent as appropriate within the range which does not impair the effects of the present invention. Chelating compound, preservative, rust inhibitor, bactericide, antibacterial agent, anthrone ketone antifoaming agent, antioxidant, coconut oil fatty acid A, such as amino carboxylic acid such as aminodiacetic acid and ethylenediaminetetraacetic acid An ester or an alcohol such as an ester or a benzyl acetate.
在本發明之洗淨劑組合物含有矽酮系消泡劑的情況下,作為其含量,較佳為發揮出抑制發泡性之效果的有效量,更佳為0.01質量%以上且0.6質量%以下、進一步較佳為0.03質量%以上且0.5質量%以下、更進一步較佳為0.05質量%以上且0.3質量%以下。 In the case where the detergent composition of the present invention contains an anthrone-based antifoaming agent, the content thereof is preferably an effective amount which exhibits an effect of suppressing foaming property, and more preferably 0.01% by mass or more and 0.6% by mass. In the following, it is more preferably 0.03 mass% or more and 0.5 mass% or less, and still more preferably 0.05 mass% or more and 0.3 mass% or less.
本發明中之洗淨劑組合物的製備方法沒有任何限定,可藉由混合成分A、成分B、成分C以及成分D進行製備。 The preparation method of the detergent composition in the present invention is not limited, and it can be prepared by mixing the component A, the component B, the component C, and the component D.
就本發明之洗淨劑組合物的pH而言,在一或多個實施形態中,自提高對殘留於間隙之助焊劑殘餘物的洗淨力的觀點出發,較佳為pH8以上且pH14以下。pH可根據需要藉由按照所需量適當地配合硝 酸、硫酸等無機酸、羥基羧酸、多元羧酸、胺基聚羧酸、胺基酸等除了成分C以外之有機酸、以及其金屬鹽或銨鹽、氨、氫氧化鈉、氫氧化鉀、胺等除了成分B以外之鹼性物質而進行調整。 In the one or more embodiments, the pH of the detergent composition of the present invention is preferably pH 8 or higher and pH 14 or lower from the viewpoint of improving the cleaning power of the flux residue remaining in the gap. . The pH can be appropriately mixed with the nitrate according to the required amount as needed. An organic acid other than the component C such as an inorganic acid such as an acid or a sulfuric acid, a hydroxycarboxylic acid, a polyvalent carboxylic acid, an amine polycarboxylic acid or an amino acid, and a metal salt or an ammonium salt thereof, ammonia, sodium hydroxide or potassium hydroxide. The amine or the like is adjusted in addition to the basic substance other than the component B.
本發明在其他實施形態中,關於焊料助焊劑殘餘物之洗淨方法(以下,亦稱為本發明之洗淨方法),其包括使具有回流後之焊料的被洗淨物與本發明之洗淨劑組合物接觸的步驟。本發明之洗淨方法在一或多個實施形態中,具有利用本發明之洗淨劑組合物對具有回流後之焊料的被洗淨物進行洗淨的步驟。作為使被洗淨物與本發明之洗淨劑組合物接觸的方法、或者利用本發明之洗淨劑組合物對被洗淨物進行洗淨的方法,在一或多個實施形態中,可列舉出在超音波洗淨裝置之浴槽內進行接觸的方法;將洗淨劑組合物以噴霧狀射出且進行接觸的方法(噴淋方式)等。本發明之洗淨劑組合物可直接用於洗淨而無需稀釋。本發明之洗淨方法較佳包括以下步驟:使洗淨劑組合物與被洗淨物接觸後,用水進行沖洗且乾燥。若為本發明之洗淨方法,則能夠有效對殘留於焊接後之部件之間隙中的助焊劑殘餘物進行洗淨。自基於本發明之洗淨方法之洗淨性及向狹窄間隙中之浸透性表現出顯著效果的觀點出發,焊料較佳為無鉛(Pb)焊料。本發明之洗淨方法在一或多個實施形態中,自容易發揮本發明之洗淨劑組合物的洗淨力的觀點出發,較佳在本發明之洗淨劑組合物與被洗淨物接觸時照射超音波,更佳該超音波較強。作為上述超音波,在一或多個實施形態中,較佳26-72Hz、80-1500W,更佳36-72Hz、80-1500W。 In another embodiment of the present invention, a method of cleaning a solder flux residue (hereinafter also referred to as a cleaning method of the present invention) includes: washing a solder having a reflowed solder and the washing of the present invention The step of contacting the detergent composition. In one or more embodiments, the cleaning method of the present invention has a step of washing the washed product having the solder after reflow using the detergent composition of the present invention. As a method of bringing the object to be washed into contact with the detergent composition of the present invention or a method of washing the object to be washed by the detergent composition of the present invention, in one or more embodiments, A method of contacting in a bath of an ultrasonic cleaning device, a method of spraying the detergent composition in a spray form and bringing it into contact (spraying method), and the like are exemplified. The detergent composition of the present invention can be used directly for washing without dilution. The cleaning method of the present invention preferably comprises the steps of: after contacting the detergent composition with the object to be washed, rinsing with water and drying. According to the cleaning method of the present invention, it is possible to effectively clean the flux residue remaining in the gap between the welded components. The solder is preferably a lead-free (Pb) solder from the viewpoint of the detergency of the cleaning method according to the present invention and the permeability to the narrow gap. In one or more embodiments, the cleaning method of the present invention is preferably a detergent composition and a laundry according to the present invention from the viewpoint of easily exhibiting the detergency of the detergent composition of the present invention. When the contact is irradiated with ultrasonic waves, it is better that the ultrasonic wave is stronger. As the above ultrasonic wave, in one or more embodiments, it is preferably 26-72 Hz, 80-1500 W, more preferably 36-72 Hz, or 80-1500 W.
本發明之洗淨劑組合物在一或多個實施形態中,用於電子部件之洗淨中。作為被洗淨物,在一或多個實施形態中,可列舉出具有回流後之焊料的被洗淨物,在其他一或多個實施形態中,可列舉出將部 件焊接而得的電子部件之製造中間物,或者可列舉出在焊接後之部件之間隙中包含助焊劑殘餘物的製造中間物。上述製造中間物為在包含半導體組件或半導體裝置之電子部件之製造步驟中的中間製造物,例如,包括在電路基板上藉由使用助焊劑之焊接而搭載有半導體晶片、晶片型電容器、以及電路基板等而製成的物體。被洗淨物中之間隙係指,例如,在電路基板與經焊接而搭載至該電路基板上之部件(半導體晶片、晶片型電容器、電路基板等)之間所形成的空間,且高度(部件間之距離)為例如5-500μm、10-250μm、或20-100μm的空間。間隙之寬度及深度依賴於所搭載之部件以及電路基板上之電極(land,接合區)的大小或間隔。 The detergent composition of the present invention is used in the cleaning of electronic components in one or more embodiments. In one or more embodiments, the object to be washed may be a washed object having solder after reflow, and in one or more embodiments, a part may be mentioned. An intermediate for manufacturing an electronic component obtained by soldering, or a manufacturing intermediate containing a flux residue in a gap between the components after soldering. The above-described manufacturing intermediate is an intermediate product in a manufacturing step of an electronic component including a semiconductor component or a semiconductor device, and includes, for example, a semiconductor wafer, a wafer type capacitor, and a circuit mounted on a circuit substrate by soldering using a flux. An object made of a substrate or the like. The gap in the object to be cleaned is, for example, a space formed between a circuit board and a member (a semiconductor wafer, a chip capacitor, a circuit board, or the like) that is mounted on the circuit board by soldering, and the height (parts) The distance between them is, for example, a space of 5 to 500 μm, 10 to 250 μm, or 20 to 100 μm. The width and depth of the gap depend on the size and spacing of the components to be mounted and the electrodes (land) on the circuit substrate.
本發明之電子部件的製造方法包括以下步驟:藉由使用助焊劑之焊接而將選自半導體晶片、晶片型電容器、以及電路基板中之至少一種部件搭載於電路基板上的步驟;以及藉由本發明之洗淨方法對上述搭載物進行洗淨的步驟。就使用助焊劑之焊接而言,在一或多個實施形態中,利用無鉛焊料進行,可為回流方式亦可為流體方式。電子部件包括未搭載半導體晶片之半導體組件、搭載有半導體晶片之半導體組件、以及半導體裝置。本發明之電子部件的製造方法藉由進行本發明之洗淨方法,從而降低殘留於焊接後之部件之間隙中的助焊劑殘餘物,且抑制由於助焊劑殘餘物殘留所導致之電極間短路或黏接不良,由此,能夠進行可靠性高的電子部件之製造。另外,藉由進行本發明之洗淨方法,從而易於對殘留於焊接後之部件之間隙中的助焊劑殘餘物進行洗淨,由此,能夠縮短洗淨時間,且能夠提高電子部件之製造效率。 A method of manufacturing an electronic component according to the present invention includes the steps of: mounting at least one member selected from the group consisting of a semiconductor wafer, a wafer type capacitor, and a circuit substrate on a circuit substrate by soldering using a flux; and by the present invention The cleaning method is a step of washing the above-mentioned mounted object. In the case of soldering using a flux, in one or more embodiments, the lead-free solder may be used, and the reflow method may be a fluid method. The electronic component includes a semiconductor component in which a semiconductor wafer is not mounted, a semiconductor component on which a semiconductor wafer is mounted, and a semiconductor device. The method for producing an electronic component of the present invention reduces the flux residue remaining in the gap of the soldered component by performing the cleaning method of the present invention, and suppresses the short circuit between the electrodes due to the residue of the flux residue or The adhesion is poor, whereby the manufacture of highly reliable electronic components can be performed. Further, by performing the cleaning method of the present invention, it is easy to wash the flux residue remaining in the gap between the welded components, whereby the cleaning time can be shortened, and the manufacturing efficiency of the electronic component can be improved. .
本發明亦關於以下所述之一或多個實施形態。 The invention also relates to one or more of the embodiments described below.
<1>一種焊料助焊劑殘餘物除去用洗淨劑組合物,其含有下述式 (I)所示之化合物(成分A)、下述式(II)所示之化合物(成分B)、具有碳數1-6之烷基的烷基苯磺酸及/或其鹽(成分C)、以及水(成分D),成分A之含量為88.0質量%以上且94.4質量%以下,成分A中,二乙二醇單丁醚之含量為90.0質量%以上且100.0質量%以下,成分B之含量為0.3質量%以上且5.0質量%以下,成分C之含量為0.3質量%以上且5.0質量%以下。 <1> A detergent composition for removing a flux flux residue, which contains the following formula a compound (component A) represented by the formula (I), a compound represented by the following formula (II) (component B), an alkylbenzenesulfonic acid having an alkyl group having 1 to 6 carbon atoms, and/or a salt thereof (component C) And water (component D), the content of the component A is 88.0% by mass or more and 94.4% by mass or less, and the content of the diethylene glycol monobutyl ether in the component A is 90.0% by mass or more and 100.0% by mass or less, and the component B The content of the component C is 0.3% by mass or more and 5.0% by mass or less, and the content of the component C is 0.3% by mass or more and 5.0% by mass or less.
[上述式(I)中,R表示碳數3-7之烴基,n為1-5。] [In the above formula (I), R represents a hydrocarbon group having 3 to 7 carbon atoms, and n is 1 to 5. ]
[上述式(II)中,R1為氫原子、甲基、乙基或胺基乙基,R2為氫原子、羥乙基、羥丙基、甲基或乙基,R3為羥乙基或羥丙基。] [In the above formula (II), R 1 is a hydrogen atom, a methyl group, an ethyl group or an aminoethyl group, R 2 is a hydrogen atom, a hydroxyethyl group, a hydroxypropyl group, a methyl group or an ethyl group, and R 3 is a hydroxy group B. Base or hydroxypropyl. ]
<2>根據<1>所述之洗淨劑組合物,其中,成分A之含量較佳為88.0質量%以上、更佳為88.5質量%以上、進一步較佳為89.0質量%以上、進一步更佳為89.4質量%以上。 <2> The detergent composition according to <1>, wherein the content of the component A is preferably 88.0% by mass or more, more preferably 88.5 mass% or more, further preferably 89.0 mass% or more, and further preferably further It is 89.4% by mass or more.
<3>根據<1>或<2>所述之洗淨劑組合物,其中,成分A之含量較佳為94.4質量%以下、更佳為93.0質量%以下、進一步較佳為92.0質量%以下、進一步更佳為91.0質量%以下。 <3> The detergent composition according to <1> or <2>, wherein the content of the component A is preferably 94.4% by mass or less, more preferably 93.0% by mass or less, still more preferably 92.0% by mass or less. Further, it is more preferably 91.0% by mass or less.
<4>根據<1>至<3>中任一項所述之洗淨劑組合物,其中,成分A之含量較佳為88.5質量%以上且93.0質量%以下、更佳為89.0質量%以上且92.0質量%以下、進一步較佳為89.4質量%以上且91.0質量%以下。 The detergent composition according to any one of the aspects of the present invention, wherein the content of the component A is preferably 88.5 mass% or more and 93.0 mass% or less, more preferably 89.0 mass% or more. Further, it is 92.0% by mass or less, and more preferably 89.4% by mass or more and 91.0% by mass or less.
<5>根據<1>至<4>中任一項所述之洗淨劑組合物,其中,作為成分A中之一者的二乙二醇單丁醚在成分A中的含量較佳為93.0質量%以 上、更佳為94.0質量%以上、進一步較佳為96.0質量%以上、更進一步較佳為98.0質量%以上、且為100.0質量%以下。 The detergent composition according to any one of <1> to <4>, wherein the content of diethylene glycol monobutyl ether as one of the components A in the component A is preferably 93.0% by mass The amount is more preferably 94.0% by mass or more, further preferably 96.0% by mass or more, still more preferably 98.0% by mass or more, and 100.0% by mass or less.
<6>根據<1>至<5>中任一項所述之洗淨劑組合物,其中,作為成分A中之一者的二乙二醇單丁醚的含量較佳為88.0質量%以上、更佳為88.5質量%以上、進一步較佳為89.0質量%以上、更進一步較佳為89.4質量%以上。 The detergent composition according to any one of the above-mentioned items, wherein the content of diethylene glycol monobutyl ether as one of the components A is preferably 88.0% by mass or more. More preferably, it is 88.5 mass% or more, further preferably 89.0 mass% or more, and still more preferably 89.4 mass% or more.
<7>根據<1>至<6>中任一項所述之洗淨劑組合物,其中,作為成分A中之一者的二乙二醇單丁醚的含量較佳為94.4質量%以下、更佳為93.0質量%以下、進一步較佳為92.0質量%以下、更進一步較佳為91.0質量%以下。 The detergent composition according to any one of the above-mentioned items, wherein the content of diethylene glycol monobutyl ether as one of the components A is preferably 94.4% by mass or less. More preferably, it is 93.0 mass% or less, further preferably 92.0 mass% or less, and still more preferably 91.0 mass% or less.
<8>根據<1>至<7>中任一項所述之洗淨劑組合物,其中,作為成分A中之一者的二乙二醇單丁醚的含量較佳為88.0質量%以上且94.4質量%以下、更佳為88.5質量%以上且93.0質量%以下、進一步較佳為89.0質量%以上且92.0質量%以下、更進一步較佳為89.4質量%以上且91.0質量%以下。 The detergent composition according to any one of the above-mentioned items, wherein the content of the diethylene glycol monobutyl ether as one of the components A is preferably 88.0% by mass or more. Further, it is 94.4% by mass or less, more preferably 88.5 mass% or more and 93.0 mass% or less, further preferably 89.0 mass% or more and 92.0 mass% or less, and still more preferably 89.4 mass% or more and 91.0 mass% or less.
<9>根據<1>至<8>中任一項所述之洗淨劑組合物,其中,在包含除了二乙二醇單丁醚以外之成分A的情況下,其在成分A中之含量較佳為10質量%以下、更佳為7.0質量%以下、進一步較佳為6.0質量%以下、更進一步較佳為4.0質量%以下、更進一步較佳為2.0質量%以下。 The detergent composition according to any one of <1> to <8> wherein, in the case of the component A other than diethylene glycol monobutyl ether, it is in the component A. The content is preferably 10% by mass or less, more preferably 7.0% by mass or less, still more preferably 6.0% by mass or less, still more preferably 4.0% by mass or less, and still more preferably 2.0% by mass or less.
<10>根據<1>至<9>中任一項所述之洗淨劑組合物,其中,在包含除了二乙二醇單丁醚以外之成分A的情況下,其含量較佳為8.0質量%以下、更佳為6.0質量%以下、進一步較佳為5.0質量%以下。 The detergent composition according to any one of <1> to <9> wherein, in the case of the component A other than diethylene glycol monobutyl ether, the content is preferably 8.0. The mass% or less, more preferably 6.0% by mass or less, further preferably 5.0% by mass or less.
<11>根據<1>至<10>中任一項所述之洗淨劑組合物,其中,在包含除了二乙二醇單丁醚以外之成分A的情況下,其含量較佳為1.0質量%以上、更佳為2.0質量%以上、進一步較佳為3.0質量%以上。 The detergent composition according to any one of <1> to <10> wherein, in the case of the component A other than diethylene glycol monobutyl ether, the content is preferably 1.0. The mass% or more, more preferably 2.0% by mass or more, further preferably 3.0% by mass or more.
<12>根據<1>至<11>中任一項所述之洗淨劑組合物,其中,式(I)中,R較佳為碳數3-6之烴基、更佳為碳數4-6之烴基。 The detergent composition according to any one of <1> to <11>, wherein, in the formula (I), R is preferably a hydrocarbon group having a carbon number of 3 to 6, more preferably a carbon number of 4 a hydrocarbon group of -6.
<13>根據<1>至<12>中任一項所述之洗淨劑組合物,其中,式(I)中,平均加成莫耳數n較佳為1-3、更佳為2或3。 The detergent composition according to any one of <1> to <12> wherein, in the formula (I), the average addition molar number n is preferably 1-3, more preferably 2 Or 3.
<14>根據<1>至<13>中任一項所述的洗淨劑組合物,其中,成分B之含量較佳為0.3質量%以上、更佳為0.5質量%以上、進一步較佳為1.0質量%以上、進一步更佳為1.5質量%以上。 The detergent composition according to any one of the aspects of the present invention, wherein the content of the component B is preferably 0.3% by mass or more, more preferably 0.5% by mass or more, further preferably 1.0% by mass or more, and more preferably 1.5% by mass or more.
<15>根據<1>至<14>中任一項所述之洗淨劑組合物,其中,成分B之含量較佳為5.0質量%以下、更佳為4.5質量%以下、進一步較佳為4.0質量%以下、進一步更佳為3.5質量%以下。 The detergent composition according to any one of the aspects of the present invention, wherein the content of the component B is preferably 5.0% by mass or less, more preferably 4.5% by mass or less, further preferably 4.0% by mass or less, and more preferably 3.5% by mass or less.
<16>根據<1>至<15>中任一項所述之洗淨劑組合物,其中,成分B之含量較佳為0.5質量%以上且4.5質量%以下、更佳為1.0質量%以上且4.0質量%以下、進一步較佳為1.5質量%以上且3.5質量%以下。 The detergent composition according to any one of the aspects of the present invention, wherein the content of the component B is preferably 0.5% by mass or more and 4.5% by mass or less, more preferably 1.0% by mass or more. It is 4.0% by mass or less, and more preferably 1.5% by mass or more and 3.5% by mass or less.
<17>根據<1>至<16>中任一項所述之洗淨劑組合物,其中,成分C之含量較佳為0.4質量%以上、更佳為0.5質量%以上。 The detergent composition according to any one of <1> to <16>, wherein the content of the component C is preferably 0.4% by mass or more, more preferably 0.5% by mass or more.
<18>根據<1>至<17>中任一項所述之洗淨劑組合物,其中,成分C之含量較佳為4.5質量%以下、更佳為4.0質量%以下、進一步較佳為3.0質量%以下。 The detergent composition according to any one of the aspects of the present invention, wherein the content of the component C is preferably 4.5% by mass or less, more preferably 4.0% by mass or less, further preferably 3.0% by mass or less.
<19>根據<1>至<18>中任一項所述之洗淨劑組合物,其中,成分D之含量較佳為5.0質量%以上、更佳為5.5質量%以上、進一步較佳為6.5質量%以上。 The detergent composition according to any one of the aspects of the present invention, wherein the content of the component D is preferably 5.0% by mass or more, more preferably 5.5% by mass or more, and still more preferably 6.5 mass% or more.
<20>根據<1>至<19>中任一項所述之洗淨劑組合物,其中,成分D之含量較佳為10.0質量%以下、更佳為9.0質量%以下、進一步較佳為8.0質量%以下。 The detergent composition according to any one of the aspects of the present invention, wherein the content of the component D is preferably 10.0% by mass or less, more preferably 9.0% by mass or less, further preferably 8.0% by mass or less.
<21>根據<1>至<20>中任一項所述之洗淨劑組合物,其中,成分D之含量較佳為5.0質量%以上且10.0質量%以下、更佳為5.5質量%以 上且9.0質量%以下、進一步較佳為6.5質量%以上且8.0質量%以下。 The detergent composition according to any one of <1> to <20>, wherein the content of the component D is preferably 5.0% by mass or more and 10.0% by mass or less, more preferably 5.5% by mass. The amount is 9.0% by mass or less, and more preferably 6.5 mass% or more and 8.0 mass% or less.
<22>根據<1>至<21>中任一項所述之洗淨劑組合物,其中,成分A與成分D之質量比〔成分A/成分D〕較佳為10.0以上、更佳為11.0以上、進一步較佳為12.0以上。 The detergent composition according to any one of <1> to <21>, wherein the mass ratio of the component A to the component D [component A/component D] is preferably 10.0 or more, more preferably 11.0 or more, further preferably 12.0 or more.
<23>根據<1>至<22>中任一項所述之洗淨劑組合物,其中,成分A與成分D之質量比〔成分A/成分D〕較佳為19.0以下、更佳為17.0以下、進一步較佳為14.0以下。 The detergent composition according to any one of the above aspects, wherein the mass ratio of the component A to the component D [component A/component D] is preferably 19.0 or less, more preferably 17.0 or less, further preferably 14.0 or less.
<24>根據<1>至<22>中任一項所述之洗淨劑組合物,其中,成分A、B以及C之質量比(成分A/成分B/成分C)較佳為89.7-99.4/0.3-5.4/0.3-5.4、更佳為91.0-98.6/1.0-5.0/0.4-4.0、進一步較佳為94.0-98.0/1.5-4.0/0.5-2.0,成分A、成分B以及成分C之總計為100.0。 The detergent composition according to any one of <1> to <22> wherein the mass ratio of the components A, B and C (component A/component B/component C) is preferably 89.7- 99.4/0.3-5.4/0.3-5.4, more preferably 91.0-98.6/1.0-5.0/0.4-4.0, further preferably 94.0-98.0/1.5-4.0/0.5-2.0, component A, component B and component C The total is 100.0.
<25>根據<1>至<23>中任一項所述之洗淨劑組合物,其亦包含聚伸烷基二醇烷基胺型非離子界面活性劑。 <25> The detergent composition according to any one of <1> to <23> which further comprises a polyalkylene glycol alkylamine type nonionic surfactant.
<26>根據<1>至<25>中任一項所述之洗淨劑組合物,其中,焊料為無鉛(Pb)焊料。 The detergent composition according to any one of <1> to <25> wherein the solder is a lead-free (Pb) solder.
<27>一種焊料助焊劑殘餘物之洗淨方法,其具有以下步驟:利用<1>至<26>中任一項所述之洗淨劑組合物對具有回流後之焊料的被洗淨物進行洗淨。 <27> A method of cleaning a solder flux residue, which has the following steps: using the detergent composition according to any one of <1> to <26> for a washed product having a solder after reflow Wash it out.
<28>根據<27>所述之洗淨方法,其中,被洗淨物為利用焊料焊接部件而得的電子部件之製造中間物。 <28> The cleaning method according to <27>, wherein the object to be cleaned is an intermediate material for manufacturing an electronic component obtained by using a solder joint member.
<29>一種電子部件之製造方法,其包括以下步驟:藉由使用助焊劑之焊接而將選自半導體晶片、晶片型電容器、以及電路基板中之至少一種部件搭載於電路基板上的步驟;以及藉由<27>或<28>所述之助焊劑殘餘物之洗淨方法對該搭載物進行洗淨的步驟。 <29> A method of manufacturing an electronic component, comprising the steps of: mounting at least one member selected from the group consisting of a semiconductor wafer, a wafer type capacitor, and a circuit substrate on a circuit board by soldering using a flux; The step of washing the mounted material by the method of cleaning the flux residue as described in <27> or <28>.
<30><1>至<26>中任一項所述之洗淨劑組合物在電子部件之洗淨 中的應用。 The detergent composition according to any one of <1> to <26>, which is washed in the electronic component Application in .
混合下述表1及表2所示之成分A-D、以及根據需要使用之其他成分(表1以及表2),製備出實施例1-16、比較例1-16之洗淨劑組合物。下述表1及表2之成分A-D以及其他成分的數值表示在所製備之洗淨劑組合物中的含量(質量%)。 The detergent compositions of Examples 1 to 16 and Comparative Examples 1 to 16 were prepared by mixing the components A-D shown in the following Tables 1 and 2 and the other components (Table 1 and Table 2) as needed. The values of the components A-D and other components in the following Tables 1 and 2 indicate the content (% by mass) in the prepared detergent composition.
作為其他成分而在表1及表2中以「*1」「*2」及「*3」表示之物質為下述化合物。 The substances represented by "*1", "*2" and "*3" in Tables 1 and 2 as the other components are the following compounds.
成分*1:下述式(III)所示之聚伸烷基二醇烷基胺型非離子界面活性劑。其中,使用R4為碳數12之烴基、n+m為4的化合物。 Component *1: a polyalkylene glycol alkylamine type nonionic surfactant represented by the following formula (III). Among them, a compound in which R 4 is a hydrocarbon group having 12 carbon atoms and n + m is 4 is used.
[式(III)中,R4表示碳數8-18之烴基、EO表示氧化乙烯基、n及m分別表示EO之平均加成莫耳數。] In the formula (III), R 4 represents a hydrocarbon group having a carbon number of 8 to 18, EO represents an oxyethylene group, and n and m each represent an average addition molar number of EO. ]
成分*2:下述式(IV)所示之聚氧乙烯氧丙烯烷基醚型非離子界面活性劑。其中,使用R5為碳數12或14之烴基、p=5、q=2、r=5的化合物。 Component *2: A polyoxyethylene oxypropylene alkyl ether type nonionic surfactant represented by the following formula (IV). Among them, a compound in which R 5 is a hydrocarbon group having 12 or 14 carbon atoms, p = 5, q = 2, and r = 5 is used.
[式(IV)中,R5表示碳數8-18之烴基、EO表示氧化乙烯基、PO表示氧化丙烯基。p、q及r分別表示EO、PO之平均加成莫耳數,分別為0-15之數,p及r不同時為0,且在q>0之情況下qp+r30、在q=0之情況下r=0。] In the formula (IV), R 5 represents a hydrocarbon group having a carbon number of 8 to 18, EO represents an oxyethylene group, and PO represents an oxypropylene group. p, q, and r represent the average addition moles of EO and PO, respectively, which are 0-15, and p and r are different at 0, and q is 0. p+r 30. In the case of q=0, r=0. ]
成分*3:上述式(IV)所示之聚氧乙烯氧丙烯烷基醚型非離子界面活性劑。其中,使用R5為碳數12之仲烴基、p=7、q=r=0的化合物。 Component *3: a polyoxyethylene oxypropylene alkyl ether type nonionic surfactant represented by the above formula (IV). Among them, a compound in which R 5 is a secondary hydrocarbon group having 12 carbon atoms and p = 7 and q = r = 0 is used.
使用所製備的實施例1-16及比較例1-16之洗淨劑組合物,對於測試基板之洗淨性(洗淨性1及2)、玻璃毛細管試驗、清洗性、腐蝕性、發泡性、以及安全性進行試驗且進行評價。表1及表2中顯示其結果。 Using the prepared detergent compositions of Examples 1 to 16 and Comparative Examples 1 to 16, the test substrate was cleaned (detergency 1 and 2), glass capillary test, cleaning property, corrosiveness, foaming Sex, and safety were tested and evaluated. The results are shown in Tables 1 and 2.
在以下條件下進行洗淨測試基板之洗淨性試驗。 The detergency test of the cleaning test substrate was carried out under the following conditions.
使用了搭載有10個晶片電容器(0816)之測試基板(50mm×50mm、晶片電容器與基板之間隙為約50μm)。焊劑使用無鉛ECO SOLDER M705-BPS(千住金屬工業(股)製),回流爐使用ECO-REFLOW SNR825(千住金屬工業(股)製),在回流峰溫度240℃、焊料熔融時間45秒、氮氣氣氛下(氧氣濃度100ppm),進行焊料連接。 A test substrate (50 mm × 50 mm, and a gap between the wafer capacitor and the substrate of about 50 μm) equipped with 10 wafer capacitors (0816) was used. The flux used was lead-free ECO SOLDER M705-BPS (manufactured by Senju Metal Industry Co., Ltd.), and the reflow furnace used ECO-REFLOW SNR825 (manufactured by Senju Metal Industry Co., Ltd.) at a reflow peak temperature of 240 ° C, a solder melting time of 45 seconds, and a nitrogen atmosphere. Lower (oxygen concentration: 100 ppm), solder connection.
洗淨進行噴霧洗淨。對於測試基板之晶片電容器,將焊接面朝上,以扇形噴嘴VVP9060(IKEUCHI製)、壓力0.3MPa(流量6公升/分鐘),由上至下(距離5cm)進行噴霧,使測試基板以0.5米/分鐘進行左右移動,進行2分鐘洗淨。洗淨後,在各進行1次之條件下進行預沖洗及終沖洗。以水平對置距離為27cm之密實錐形噴嘴(full-cone nozzle)J050(IKEUCHI製)、壓力0.3MPa(流量0.6公升/分鐘),在噴嘴間之中間將測試基板固定2分鐘。在終沖洗後,利用送風乾燥機(85℃、15分鐘)對測試基板進行乾燥。另外,所使用之各洗淨劑組合物及沖洗用離子交換水加熱至60℃。 Wash and spray to wash. For the wafer capacitor of the test substrate, the soldering surface is facing up, and the fan-shaped nozzle VVP9060 (manufactured by IKEUCHI) is pressed at a pressure of 0.3 MPa (flow rate: 6 liters/min), and sprayed from top to bottom (distance: 5 cm) to make the test substrate 0.5 m. /minute to move left and right, and wash for 2 minutes. After washing, pre-rinsing and final washing were carried out under the conditions of one each. The test substrate was fixed for 2 minutes between the nozzles with a full-cone nozzle (manufactured by IKEUCHI) having a horizontally opposed distance of 27 cm and a pressure of 0.3 MPa (flow rate of 0.6 liter/min). After the final rinse, the test substrate was dried using a blow dryer (85 ° C, 15 minutes). Further, each of the detergent compositions used and the ion exchange water for washing were heated to 60 °C.
自乾燥後之測試基板中剝離晶片電容器,利用光學顯微鏡確認有無助焊劑殘餘物之殘留。評價基準如下所述。表1及表2之「洗淨性1」欄中顯示其結果。 The wafer capacitor was peeled off from the dried test substrate, and the presence or absence of the residue of the flux was confirmed by an optical microscope. The evaluation criteria are as follows. The results are shown in the column of "Detergency 1" in Tables 1 and 2.
A:10個中有殘餘物的為0個 A: 0 of the 10 residues
B:10個中有殘餘物的為1個 B: 1 of the 10 residues
C:10個中有殘餘物的為2個以上 C: 2 or more of the remaining residues are more than 2
利用與上述洗淨性試驗(洗淨性1)相同之方法,將洗淨時間縮短至1分鐘而進行評價。表1及表2之「洗淨性2」欄中顯示其結果。 The washing time was shortened to 1 minute by the same method as the above-described detergency test (detergency 1), and the evaluation was performed. The results are shown in the column of "Detergency 2" in Tables 1 and 2.
在氮氣氣氛下在銅板上對ECO SOLDER M705-BPS(千住金屬工業(股)製)進行250℃、30分鐘加熱,分離且採集液狀助焊劑殘餘物。對DRUMMOND製Glass Microcap(玻璃毛細管)(長度32mm、內徑140μm)填充按照上述方法製得之助焊劑殘餘物,將一個開口部密封,製成了試驗片。在100mL燒杯中加入各洗淨劑組合物及清洗用離子交換水各100g,加熱至60℃。將試驗片浸漬於各洗淨劑組合物中且照射5分鐘超音波(40kHz、200W),然後移至清洗用離子交換水中且照射5分鐘超音波(40kHz、200W)後取出。利用光學顯微鏡觀察取出之試驗片,測定溶解之助焊劑殘餘物距離開口部的距離,算出5點之平均值。可評價為:助焊劑殘餘物溶解後之距離愈長,則溶解速度愈快、洗淨性愈良好。表1及表2中顯示其結果。 ECO SOLDER M705-BPS (manufactured by Senju Metal Industry Co., Ltd.) was heated at 250 ° C for 30 minutes on a copper plate under a nitrogen atmosphere to separate and collect a liquid flux residue. A glass microcapacitor (glass capillary) (length 32 mm, inner diameter 140 μm) manufactured by DRUMMOND was filled with the flux residue prepared by the above method, and one opening was sealed to prepare a test piece. 100 g of each of the detergent composition and the ion exchange water for washing was placed in a 100 mL beaker and heated to 60 °C. The test piece was immersed in each of the detergent compositions and irradiated for 5 minutes for ultrasonic waves (40 kHz, 200 W), and then transferred to ion-exchange water for washing and irradiated for 5 minutes for ultrasonic waves (40 kHz, 200 W), and then taken out. The taken test piece was observed with an optical microscope, and the distance of the dissolved flux residue from the opening was measured, and the average value of 5 points was calculated. It can be evaluated that the longer the distance after the flux residue is dissolved, the faster the dissolution rate and the better the detergency. The results are shown in Tables 1 and 2.
在氮氣氣氛下,在銅板上對ECO SOLDER M705-BPS(千住金屬工業(股)製)進行250℃、30分鐘加熱,分離且採集液狀助焊劑殘餘物。將該助焊劑殘餘物與各洗淨劑組合物混合,製成1質量%混合液。滴加約0.1g利用上述方法製成之混合液至見方之蓋玻片(18mm×18mm、松浪硝子工業(股)製)上,在其上重疊另一張見方之蓋玻片,利用夾子(口寬19mm、Kokuyo(股)製)夾住一邊且固定,製成試驗片。在100mL燒杯中加入清洗用離子交換水100g且加熱至60℃。用 鑷子保持試驗片,邊在清洗用離子交換水中上下搖動10次邊浸漬1分鐘,取出。利用真空乾燥機(120℃、15分鐘)對取出後之試驗片進行乾燥。觀察試驗片,計算直至見方之蓋玻片間沒有殘留物時的清洗次數。可評價為:清洗次數愈少,則清洗性愈良好。表1及表2中顯示其結果。另外,將經由5次清洗仍無法清洗乾淨之情況設為「>5」。 Under a nitrogen atmosphere, ECO SOLDER M705-BPS (manufactured by Senju Metal Industry Co., Ltd.) was heated on a copper plate at 250 ° C for 30 minutes to separate and collect a liquid flux residue. The flux residue was mixed with each detergent composition to prepare a 1% by mass mixed liquid. About 0.1 g of the mixture prepared by the above method was added dropwise to a cover slip (18 mm × 18 mm, manufactured by Songlang Glass Industry Co., Ltd.), and another cover glass was overlapped thereon, using a clip ( A test piece was prepared by sandwiching one side and fixing it by a width of 19 mm and a Kokuyo (manufactured by Kokuyo Co., Ltd.). 100 g of ion-exchanged water for washing was placed in a 100 mL beaker and heated to 60 °C. use While holding the test piece, the tweezers were immersed for 1 minute while shaking up and down for 10 times in the ion exchange water for washing, and taken out. The taken-out test piece was dried using a vacuum dryer (120 ° C, 15 minutes). The test piece was observed, and the number of times of washing until there was no residue between the coverslips of the square was calculated. It can be evaluated that the less the number of cleanings, the better the cleaning performance. The results are shown in Tables 1 and 2. In addition, the case where the cleaning cannot be performed after 5 times of cleaning is set to ">5".
將各洗淨劑組合物裝滿至1L燒杯中且加熱至60℃,向其中放入厚1mm之銅板(30mm×50mm)且浸漬10分鐘。然後,利用離子交換水進行充分清洗,且利用送風乾燥機(85℃、15分鐘)進行乾燥,觀察銅板之表面狀態。評價基準如下所述。表1及表2中顯示其結果。 Each of the detergent compositions was filled in a 1 L beaker and heated to 60 ° C, and a copper plate (30 mm × 50 mm) having a thickness of 1 mm was placed therein and immersed for 10 minutes. Then, it was sufficiently washed with ion-exchanged water, and dried by a blow dryer (85 ° C, 15 minutes) to observe the surface state of the copper plate. The evaluation criteria are as follows. The results are shown in Tables 1 and 2.
A:無變色 A: no discoloration
B:有變色 B: There is discoloration
在氮氣氣氛下在銅板上對ECO SOLDER M705-BPS(千住金屬工業(股)製)進行250℃、30分鐘加熱,分離且採集液狀助焊劑殘餘物。利用離子交換水將在上述條件下製成的含有助焊劑殘餘物1質量%之各洗淨劑組合物稀釋10倍,將其50mL加入至200mL帶塞容量瓶中,加熱至60℃,上下激烈振盪30次。測定1分鐘後之泡高度,以下述基準進行評價。表1及表2中顯示其結果。 ECO SOLDER M705-BPS (manufactured by Senju Metal Industry Co., Ltd.) was heated at 250 ° C for 30 minutes on a copper plate under a nitrogen atmosphere to separate and collect a liquid flux residue. Each of the detergent compositions containing 1% by mass of the flux residue prepared under the above conditions was diluted 10 times with ion-exchanged water, and 50 mL of the detergent composition was added to a 200 mL stoppered volumetric flask, and heated to 60 ° C. Oscillation 30 times. The bubble height after 1 minute was measured and evaluated based on the following criteria. The results are shown in Tables 1 and 2.
A:無泡 A: no bubble
B:不足5mL B: less than 5mL
C:5mL以上 C: 5mL or more
根據各洗淨劑組合物之閃點進行如下所述之評價。需要說明的是,若在水沸點之100℃下進行點火,則形成火災之危險性變高。以比水沸點高10℃之110℃為基準,基於閃點而進行安全性評價。表1及 表2中顯示其結果。 The evaluation as described below was carried out based on the flash point of each detergent composition. In addition, when ignition is performed at 100 ° C of the boiling point of water, the risk of fire formation becomes high. The safety evaluation was performed based on the flash point based on 110 ° C which is 10 ° C higher than the boiling point of water. Table 1 and The results are shown in Table 2.
A:閃點為110℃以上 A: The flash point is above 110 °C
B:閃點不足110℃ B: The flash point is less than 110 ° C
如上述表1及表2所示,實施例1-16之洗淨劑組合物與比較例1-10、12-16之洗淨劑組合物相比,顯示出優異之洗淨性,且玻璃毛細管試驗之結果(浸透性)及清洗性亦顯示出大體上優異之結果。另外,實施例1-13之洗淨劑組合物與比較例11之洗淨劑組合物相比,安全性方面較優異(閃點高)。 As shown in the above Tables 1 and 2, the detergent compositions of Examples 1 to 16 exhibited superior detergency and glass compared with the detergent compositions of Comparative Examples 1-10 and 12-16. The results of the capillary test (permeability) and cleanability also showed generally excellent results. Further, the detergent compositions of Examples 1 to 13 were superior in safety (high flash point) as compared with the detergent composition of Comparative Example 11.
如上述表1及表2所示,添加有聚伸烷基二醇烷基胺型非離子界 面活性劑的實施例8之洗淨劑組合物,其清洗性特別優異。另外,含有烴或矽酮系消泡劑的實施例7及12之洗淨劑組合物,其低發泡性特別優異。 As shown in Tables 1 and 2 above, a polyalkylene glycol alkylamine type nonionic boundary is added. The detergent composition of Example 8 of the surfactant was particularly excellent in cleanability. Further, the detergent compositions of Examples 7 and 12 containing a hydrocarbon or an anthrone-based antifoaming agent are particularly excellent in low foaming property.
藉由使用本發明,焊接後之部件的殘留於間隙之助焊劑殘餘物的洗淨能夠良好地進行,因而例如能夠縮短電子部件之製造過程中的助焊劑殘餘物之洗淨步驟以及提高所製造之電子部件的性能可靠性,且能夠提高半導體裝置之生產性。 By using the present invention, the cleaning of the flux residue remaining in the gap of the welded component can be performed satisfactorily, and thus, for example, the step of cleaning the flux residue in the manufacturing process of the electronic component can be shortened and the manufacturing can be improved. The performance reliability of the electronic component can improve the productivity of the semiconductor device.
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JP2012018982A (en) * | 2010-07-06 | 2012-01-26 | Tosoh Corp | Resist stripping agent and stripping method using the same |
JP2012032757A (en) * | 2010-07-06 | 2012-02-16 | Tosoh Corp | Resist stripping agent and stripping method using the same |
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WO2012144438A1 (en) * | 2011-04-18 | 2012-10-26 | ライオン株式会社 | Liquid detergent |
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- 2014-12-08 CN CN201410743519.9A patent/CN104694273B/en active Active
- 2014-12-09 KR KR1020140175567A patent/KR102225717B1/en active IP Right Grant
- 2014-12-10 TW TW103143097A patent/TWI576427B/en active
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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TWI714910B (en) * | 2017-11-14 | 2021-01-01 | 日商千住金屬工業股份有限公司 | Flux, cored solder and flux-coated mass |
US11413711B2 (en) | 2017-11-14 | 2022-08-16 | Senju Metal Industry Co., Ltd. | Flux, resin flux cored solder, and flux coated pellet |
Also Published As
Publication number | Publication date |
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KR20150067737A (en) | 2015-06-18 |
JP2015113379A (en) | 2015-06-22 |
KR102225717B1 (en) | 2021-03-09 |
TWI576427B (en) | 2017-04-01 |
JP6158060B2 (en) | 2017-07-05 |
CN104694273A (en) | 2015-06-10 |
CN104694273B (en) | 2019-08-09 |
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