TW201134562A - Cleaning method and cleaning device used in said cleaning method - Google Patents

Cleaning method and cleaning device used in said cleaning method Download PDF

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Publication number
TW201134562A
TW201134562A TW099146660A TW99146660A TW201134562A TW 201134562 A TW201134562 A TW 201134562A TW 099146660 A TW099146660 A TW 099146660A TW 99146660 A TW99146660 A TW 99146660A TW 201134562 A TW201134562 A TW 201134562A
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TW
Taiwan
Prior art keywords
pressure
cleaning
detergent composition
washing
kpa
Prior art date
Application number
TW099146660A
Other languages
Chinese (zh)
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TWI504450B (en
Inventor
Hirokazu Kawashimo
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Kao Corp
Sakura Seiki Co Ltd
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Publication of TW201134562A publication Critical patent/TW201134562A/en
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Publication of TWI504450B publication Critical patent/TWI504450B/en

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    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D7/00Compositions of detergents based essentially on non-surface-active compounds
    • C11D7/50Solvents
    • C11D7/5004Organic solvents
    • C11D7/5013Organic solvents containing nitrogen
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B08CLEANING
    • B08BCLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
    • B08B3/00Cleaning by methods involving the use or presence of liquid or steam
    • B08B3/04Cleaning involving contact with liquid
    • B08B3/08Cleaning involving contact with liquid the liquid having chemical or dissolving effect
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B08CLEANING
    • B08BCLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
    • B08B3/00Cleaning by methods involving the use or presence of liquid or steam
    • B08B3/04Cleaning involving contact with liquid
    • B08B3/10Cleaning involving contact with liquid with additional treatment of the liquid or of the object being cleaned, e.g. by heat, by electricity or by vibration
    • B08B3/12Cleaning involving contact with liquid with additional treatment of the liquid or of the object being cleaned, e.g. by heat, by electricity or by vibration by sonic or ultrasonic vibrations
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B23MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23KSOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K1/00Soldering, e.g. brazing, or unsoldering
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B23MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23KSOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K1/00Soldering, e.g. brazing, or unsoldering
    • B23K1/0008Soldering, e.g. brazing, or unsoldering specially adapted for particular articles or work
    • B23K1/0016Brazing of electronic components
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B23MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23KSOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K1/00Soldering, e.g. brazing, or unsoldering
    • B23K1/20Preliminary treatment of work or areas to be soldered, e.g. in respect of a galvanic coating
    • B23K1/206Cleaning
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D7/00Compositions of detergents based essentially on non-surface-active compounds
    • C11D7/22Organic compounds
    • C11D7/26Organic compounds containing oxygen
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D7/00Compositions of detergents based essentially on non-surface-active compounds
    • C11D7/22Organic compounds
    • C11D7/32Organic compounds containing nitrogen
    • HELECTRICITY
    • H05ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05KPRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
    • H05K3/00Apparatus or processes for manufacturing printed circuits
    • H05K3/0085Apparatus for treatments of printed circuits with liquids not provided for in groups H05K3/02 - H05K3/46; conveyors and holding means therefor
    • C11D2111/22
    • C11D2111/46
    • HELECTRICITY
    • H05ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05KPRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
    • H05K3/00Apparatus or processes for manufacturing printed circuits
    • H05K3/30Assembling printed circuits with electric components, e.g. with resistor
    • H05K3/32Assembling printed circuits with electric components, e.g. with resistor electrically connecting electric components or wires to printed circuits
    • H05K3/34Assembling printed circuits with electric components, e.g. with resistor electrically connecting electric components or wires to printed circuits by soldering
    • H05K3/3489Composition of fluxes; Methods of application thereof; Other methods of activating the contact surfaces

Abstract

The disclosed cleaning method involves a cleaning step for cleaning an object to be cleaned, wherein said cleaning step involves: an immersion step (step 1) in which the object to be cleaned having deposited flux residues is immersed in a cleaning tank with adjustable pressure containing a detergent of a particular composition; a pressure reduction step (step 2) in which the pressure in the cleaning tank is set to P1 (kPa); a reduced pressure maintaining step (step 3) in which, for 8 to 16 seconds, the pressure in the cleaning tank, which was reduced in the pressure reduction step, is continuously maintained at P1 ± 0.4 (kPa) and the temperature of the detergent composition inside the cleaning tank is continuously maintained at 50-70 DEG C; and a pressure increasing step (step 4) in which the pressure inside the cleaning tank is raised to P2 (kPa) after the pressure maintaining step is complete. Steps 2 through 4 are performed in 10-220 seconds.

Description

201134562 六、發明說明: 【發明所屬之技術領域] 本發明係關於-種附著有助焊劑殘渣之被洗淨物之洗淨 方法、及使用該洗淨方法之電子零件之製造方法、以及該 洗淨方法用之洗淨裝置。 / 【先前技術】 先前,作為附著有助烊劑殘渔之被洗淨物之洗淨劑組人 物’已知含有乙二醇喊系化合物與胺系化合物之組合: T照專利文獻卜2等)、或進而含有界面活性劑之組合物 (參照專利文獻3、4等)等。 又,雖並非附著有助㈣_之被洗淨物之洗淨方法, 但作為用以除去附著於手錶之零件等上之研磨劑的洗淨方 法,揭不有將增加洗淨液周圍之麼力的操作與減少洗淨液 周圍之壓力的操作交替進杆 管進订複數次之洗淨方法(參照專利 獻5),作為具有微細之袋狀孔等間隙之零件之洗淨方 法’揭示有對液槽内反覆實施減壓與常麼之變壓(P— SWlng)洗淨法(參照專利文獻6等)。 專利文獻5中記載之洗淨方法中,作為洗淨劑組合物, 例如使用溶劑石油腦系洗淨液。專利文獻6中記載之洗淨 方法中’使用界面活性劑之稀釋液作為洗淨劑組合物將 :槽内減壓至所需壓力後,立即切換控制閥, 復到常壓。 a門阪 先前技術文獻 專利文獻 152501.doc 201134562 專利文獻1:曰本專利特開平9-87668號公報 專利文獻2:曰本專利特開2〇〇9_41〇94號公報 專利文獻3:日本專利特開平4_57897號公報 專利文獻4 :曰本專利特開平3_2274〇〇號公報 專利文獻5 :日本專利特開2〇〇1_17〇577號公報 專利文獻ό:曰本專利特開平6_29694〇號公報 【發明内容】 發明所欲解決之問題 於半導體裝置等電子零件之製造過程中,若於電路基板 上搭載零件(例如半導體晶片、晶片型電容器、其他電路 基板等),則有時會於上述電路基板與上述零件之間形成 空間(間隙)。用以搭載上述零件所使用之焊料中含有助焊 劑,但若於焊接後上述助焊劑以殘渣之形式長期殘留於上 述間隙中’則會產生遷移等,而成為電極間之短路等之原 因。 隨著電子零件之微細化及高密度化,大多使用例如覆晶 方式等之利用焊料凸塊之半導體晶片之安裝方法,而對安 裝要长更间之可罪性。因此,助焊劑殘渣之洗淨於電子零 件製造中的重要性進一步提高。 然隨著電子零件之微細化及高密度^匕,上述間隙進 " 進入上述較窄間隙中之助焊劑殘渣難以除去, 其結果’產生電子零件之生產性下降之問題。因此;期望 開發出-種”間隙中所殘留之助焊劑殘渣之除去性良好 之洗淨方法。 15250).doc 201134562 本發明提供-種不僅對於較窄 渔之洗淨心- ]料所存在之助祥劑殘 “ 較而,而且水之洗滌性亦良好,起泡 之附者有助焊劑殘渣之被洗淨物之洗淨方法·及:用: 淨方法之電子零件之製造方b 及使用錢 解決問題之技術手段 本發明之附著有助焊劑殘潰之被洗淨物的洗淨方法包括 使用洗淨劑組合物洗淨附著有助焊劑殘逢之被洗淨物之洗 ^步驟_h述洗淨步驟包括:將附著有助焊劑制之被洗 淨物次潰於收容於可調整壓力之洗淨槽内的上述洗淨劑組 合物中之浸潰步驟(第1步驟);將上述洗淨槽内之塵力減麼 至滿足下述式⑴之壓力P1(kPa)之減壓步驟(第2步驟);連 續8〜16秒鐘將上述減壓步驟中經減壓之上述洗淨槽内的壓 力保持在卩抓彳⑽),且將上述洗淨槽内之上述洗淨劑組 合物之溫度保持在50〜7(TC之減壓保持步驟(第3步驟);以 及經過上述減壓保持步驟後,使上述洗淨槽内之壓力為滿 足下述式(2)之壓力pjkPa)之升壓步驟(第4步驟)。以 10〜220秒鐘進行上述第2步驟〜第4步驟。 Π) (2) 0.1(kPa)^P1^7(kPa) 50(kPa)$ P2$ 120(kPa) 上述洗淨劑組合物含有2重量%以上i〇重量%以下之水 (成分A),50重量%以上未達97.75重量%之乙二醇醚(成分 B) ’及〇.〇5重量%以上5重量。/。以下之胺化合物(成分C)。 上述成分B係由下述通式(1)表示。 R]-0-(E0)m-R2 (1) 152501.doc 201134562 上述通式(1)中’ R1為碳數之烷基,R2為氫原子或碳 數1〜3之燒基,EO為氧伸乙基,m表示EO之平均加成莫耳 數’滿足 上述成分C係由下述通式(2)表示。 [化1] R3-n-(E〇)p-h (U-H ⑵ 上述通式(2)中,R3表示氫原子或碳數卜4之烷基,E〇為 氧伸乙基’ p、q分別表示E〇之平均加成莫耳數,滿足 1 各 p+q$ 4。 本發明之包含焊料凸塊之電子零件之製造方法包括:使 用含有助焊劑之焊料助焊劑於電子零件之基板上形成焊料 凸塊之步驟;以及利用本發明之上述被洗淨物之洗淨方法 洗淨源自上述助焊劑之上述助焊劑殘渣之步驟。 本發明之洗淨裝置係本發明之被洗淨物之洗淨方法用之 洗淨裝置;且 具備用以使上述洗淨槽内之上述洗淨劑組合物之上述水 (成刀A)的含里為2重量%以上丨〇重量%以下之水分控制機 構。 發明之效果 本發明中’使用特定之洗淨劑組合物。&,以依序包括 咸壓步驟、減壓保持步驟、及升壓步驟之―系列步驟作為 循裒由於係於特定時間内進行該1循環,因此因壓力變 化而產生之物理力、與因減壓㈣步驟中之洗淨劑組合物 152501 .(J〇q 201134562 的/弗騰而屋生之物理力嘗對被办 對破洗#物之較窄間隙中所存在 的助焊劑殘渣發揮作用。因此, ]t Υ /Γ仔在 供—種不僅對於較窄 間隙中所存在之助焊劑殘渣 ^k 无淨性較向,而且水之洗滌 性亦良好,且起泡獲得抑t I 1 & 剌之附者有助焊劑殘渣之被洗淨 物之洗淨方法;及使用該洗淨 无净方法之包含焊料凸塊的電子 零件之製造方法。 【實施方式】 4上,< · q π坎岍便用之含有松 香或松香衍生物之松香系助焊劑,於本發明中 2回流方式及流動方式之焊接。本發明中所謂「悍料二 知劑」係指輝料與助烊劑之混合物,所謂「助焊劑殘査 係指使用助焊劑或谭料助焊劑進行焊接後於基板等上所殘 留之源自助谭劑的殘逢…於本發明中, 勺人 含船(Pb)焊料及無外焊料。 」匕3 本,明中所謂「因洗淨劑組合物之沸騰而產生之物理 」係指藉由洗淨劑組合物中所含有之水滞騰而產 =理:,所謂「洗淨劑組合物之冻騰」意指洗淨劑 曰所3有之水之沸騰。藉此,洗淨劑組合物中之 ::量越多’則該物理力越大’洗淨劑組合物令 置越少’則該物理力越小。 本發明之附著有助焊劑殘渣之被洗淨物的洗淨方 :亦有=僅簡稱為「洗淨方法J )中’使用分別含有特定 里之特定乙二醇醚及特定胺化合物且水之含量為2重量% 以上10重量%以下之洗淨劑組合物,於特定時間内進行依 152501.doc 201134562 序包括減虔步驟、減麼保柱半 保持步驟、及升>1步驟之-系列步 驟,且即便減屡之保持時間較短亦確保特定時間,藉此意 料發現對於中所殘留之助焊劑殘渣之洗淨性較 尚,起泡獲得抑制,水之洗滌杻 无綠性良好。進而,以上述一系 列步驟為1猶環,於反覆推分1 復進仃1循環之情形時,更加提高對 於較窄間隙中所存在之助.捏無丨X% Vjfc 助焊劑殘渣之洗淨性。因此,若於 包含焊料凸塊之電子零件之製造過程中使用本發明之洗淨 方法’則可期待提高電子零件之生產性或可靠性。 [被洗淨物之洗淨方法] 於本發明之洗淨方法中,例如依序進行洗淨步驟、使用 沖洗劑組合物洗務被洗淨物之沖洗步驟、及乾燥步驟。 [被洗淨物] 作為本發明之洗淨方法中較好地使狀被洗淨物,可列 舉包含電路基板等與焊接於電路基板等上之零件的製造中 間物’且該製造t間物於該電路基板與零件之間隙中含有 助焊劑殘渣。製造中間物為半導體封裝或半導體裝置等電 子零件之製造步驟中之製造中間物,例如包含藉由使用助 焊劑之焊接而於電路基板上搭載有半導體晶片、晶片型電 谷Is、及其他電路基板等者。 所謂被洗淨物之間隙係指例如電路基板與藉由焊接而搭 載於該電路基板上之上述零件之間的空間,且其高度(電 路基板與零件之最短距離)例如為5〜500 μπι、1〇〜250 μπι、 或2〇〜100 μΠ1之空間。間隙之寬度及深度依賴於所搭載之 零件或電路基板上之電極(焊點)的大小或間隔,寬度例如 152501.doc 201134562 為130〜20000 4瓜或13〇〜1〇〇〇〇 μιη,深度為13〇〜25〇〇〇洋爪 或 130〜10000 。 [洗淨步驟] 洗淨步驟包括:將附著有助焊劑殘渣之被洗淨物浸潰於 可調整壓力之收容於洗淨槽内的下述洗淨劑組合物中之浸 潰步驟(浸潰步驟亦稱為「第丨步驟」);將洗淨槽内之壓力 減壓至特定值之減壓步驟(減壓步驟亦稱為「第2步驟」); 連續特定時間將減壓步驟中經減壓之洗淨槽内的壓力保持 在特定壓力範圍内’且將洗淨槽内之洗淨劑組合物之溫度 保持在収溫度範圍内之減壓保持步驟(減壓保持步驟亦 稱為「第3步驟」);以及經過上述減壓保持步驟後將洗 =内之壓力升壓至特定值之升壓步驟(該步驟亦稱為 第4步驟」)。 洗淨步驟亦可更包括升壓後壓力保持步驟(第^步驟)及/ 或第5步驟。第4a步驟係於第4步驟之後進行,於洗淨 包括第5步驟之情形時於第5步驟之前進行。第4a步驟中, ==内之壓力保持在特定壓力範圍内且連續保持特定 、^第5步驟係於第4步驟之後進行,於洗淨步驟包 鈍步驟之情形時於第4a步驟 第 反覆―次至少依序包括上述第2步第^ 系列步驟。 U4步驟之一 伞赞明之洗淨方法中 行,亦可#… …”之用-個洗淨槽 使用兩個以上之洗淨槽進行。例如 洗淨槽實施本發明之洗淨方法之情形時,第5:用一 了 於第5步驟中 I52501.doc 201134562 可不進行第i步驟,而反覆進行 可。 人乐2步驟〜第4步驟即 之情形時Γ兩個以上之洗淨槽實施本發明之洗淨方法 β於第5步驟中反覆進行卜 驟,亦可於铱c土 人弟1梦驟〜第4步 15步驟巾之反覆絲為χ次之情料, =步驟〜 2 ^ V ; #"x 1 °^2 2 °# # ^ ^ ^ ^ ^ ’ P匕括上述第2步驟〜第4步驟之一系列步 尤提高對於較窄間隙中所存在之助焊劑殘渣之洗淨性 且縮短洗淨時間之觀點而言,較佳為以15〜H)0秒鐘進行, 更佳為以15〜50秒鐘進行,進而較佳為心〜⑽秒鐘進行。 (第1步驟) 广先’:步驟中,首先於收容有洗淨劑組合物之洗淨槽内 才又入附著有助焊劑殘渣之被洗淨物,於洗淨劑組合物中浸 潰被洗淨物。 若為可浸潰被洗淨物之量,則洗淨劑組合物對洗淨槽之 填充量並無特別限制。 作為洗淨槽,例如可使用具備加熱機構、超音波振盪器 等之耐壓容器等。洗淨槽内與連接於真空泵等抽吸裝置之 空氣配管相連通,空氣配管包含未與抽吸裝置連接之分支 管。可藉由設置於該分支管中之切換控制閥之開閉控制, 而將洗淨槽内減壓至所需壓力或升壓至所需壓力。上述洗 淨槽之一例例如揭示於日本專利特開平6_29694〇號公報 中。 152501.doc -10- 201134562 於第1步驟中,就提高洗淨性之觀點而言,填充於洗淨 槽内之洗淨劑組合物之溫度,於即將開始減壓之前,較佳 為50〜70C,更佳為55〜70。(:,進而較佳為60~70。(:。具體 而δ,將調整為} 〇〜4〇〇c之洗淨劑組合物填充至上述洗淨 槽内後,進行加熱,使其成為上述較佳範圍内之溫度。洗 淨劑組合物之加熱視需要使用洗淨槽中所具備之加熱機構 進行即可。洗淨劑組合物之溫度係利用洗淨槽内所設置之 溫度計測定。 (第2步驟) 其次,將洗淨槽内之壓力減壓至Pi(kPa)。Ρι滿足關係式 0.1(kPa)$ p丨彡 7(kPa)。 於第2步驟中,就提高對於被洗淨物之較窄間隙中所存 在之助焊劑殘渣之洗淨性且縮短洗淨時間之觀點而言,更 佳為對洗淨槽内進行減壓,直至達到較佳為〇1〜_小 更佳為0.1〜5(kPa)、進而較佳為〜以㈣)之範圍内的壓 力。 於第2步驟中,可藉由減壓而於更窄之間隙中強制性地 混入洗淨劑組合物’因此可將阻礙較窄間隙中所存在之助 焊劑殘逢與洗淨劑組合物接觸的空氣自上述間隙迫出,且 洗淨劑組合物中所含溶存氣體亦可脫氣。故而,本發明之 洗淨方法適合作為混入較窄間隙令之助谭劑殘渣的洗淨方 法。 於第2步驟中,就同時實現提高對於較窄間隙中所存在 之助煤劑殘渣之洗淨性與縮短洗淨時間之觀點而言,使洗 I52501.doc 201134562 淨槽内之壓力為P1(kPa)所需之減壓 r 1 坚碍間,更佳為洗淨槽内 之壓力的減壓開始後1秒以上12 _ ζυ杉以内,更佳為1秒以上 60秒以内,進而較佳為】秒 办以内,進一步佳為1秒 以上15秒以内。 〜 於第2步驟中,就㈣實現提高對於較窄間隙中所存在 之助焊劑㈣之洗淨性與縮短洗淨時間之觀點而言,使洗 淨槽内之壓力為Pl(kPa)之_速度較佳為i5〜3Q(kpa/s), 更佳為17〜30(kPa/s),進而較佳為18〜3〇(kpa/s)。 就提高對於較窄間隙中所存在之助烊劑錢之洗淨性之 觀點而言,更具體而言,就藉由洗淨劑組合物之沸騰而獲 得較高之物理力及抑制洗淨劑組合物中之水的蒸發即抑 制洗淨槽内之水之減少,抑制因洗淨劑組合物之組成變動 所引起的洗淨性下降之觀點而言,第2步驟中之洗淨劑組 合物之溫度與第1步驟相同,較佳為5〇〜7(rc,更佳為 55〜70°C,進而較佳為6〇〜7〇t。洗淨劑组合物之加熱視需 要使用洗淨槽令所具備之加熱機構進行即可。即,於第2 步驟中,較佳為保持第1步驟中調整為上述較佳範圍内之 溫度的洗淨劑組合物之該溫度。第2步驟中之洗淨劑組合 物之上述溫度係利用洗淨槽内所設置之溫度計例如每1秒 測定之溫度的平均值。該平均值可根據下述第3步驟中之 洗淨劑組合物的平均溫度之算式而求出。 (第3步驟) 其次,於減壓保持步驟中’連續8〜16秒鐘將上述減壓步 驟争經減壓之洗淨槽内的壓力保持在p〗±〇 4 kPaT,且將 152501.doc 12 201134562 洗淨槽内之洗淨劑組合物的溫度保持在5〇〜70〇C下。 於第3步驟中,就保持洗淨劑組合物之穩定之沸騰狀態 之觀點而言’洗淨槽内之壓力必須為〇 ,就相同 之觀點而言’第3步驟中之洗淨槽内之壓力的變動幅度較 佳為P1:t〇_3(kPa),更佳為Pl±0 2(kPa),進而較佳為 Pi±0.1 (kPa)。即’減壓保持步驟中之洗淨槽内之壓力較佳 為實質上固定,更佳為固定。再者,洗淨槽内之壓力係利 用測壓計而測定。 就保持洗淨劑組合物之穩定之沸騰狀態之觀點而言,第 3步驟中之洗淨劑組合物之溫度,於洗淨槽内之壓力為 PpO.VkPa)之情形時,必須為5〇〜7〇。〇,就藉由沸騰之物 理力而提高對於間隙中所存在之助焊劑殘渣之洗淨性之觀 點而言,於洗淨槽内之壓力匕為〇 之情形時,較 佳為50〜70°C,於洗淨槽内之壓力Ρι超過5 kpa且為7 kpa以 下之情形時,較佳為60〜70。(:。 第3步驟中之洗淨劑組合物之溫度可於5〇〜7〇。〇之溫度範 圍内變化,但就保持洗淨劑組合物之穩定之沸騰狀態之觀 點而言,其變動幅度以第3步驟中之洗淨劑组合物的溫度 之平均值為基準,車交佳為幻.。。。㈣,更佳為士〇5。。以 内’進而較佳為±0.2。(:以内。即,本發明之洗淨方法中, 第3步驟中之洗淨劑組合物的溫度較佳為實質上固定,更 佳為固定。 第3步驟中之洗淨劑組合物之溫0係利用洗淨槽内所 設置之溫度計例如每1秒而測定。第3步驟中之洗淨劑組合 152501.doc 201134562 物之/皿度的平均值Tx(時間平均保持溫度)可根 求出。 r遴式而 時間平均保持溫度Τχ=Σ(Τί* ti)· [、’句化之别之保持溫度設為Ti,將該溫度下保掊 間設為ti]。 ”守及- 於第3步驟中’就提高對於較窄㈣中所存在之助焊劑 殘潰之洗淨性之觀點而言,洗淨劑組合物之海騰狀態必須 為8移以上。又,就同時實現提高對於間隙中所存在之助 焊劑殘渔之洗淨性與縮短洗淨時間之觀點而言,減壓之保 持:間(第3步驟之時間)必須為16秒以下。因此,就同時實 現提尚對於間隙中所存在之助焊劑殘邊之洗淨性與縮短洗 淨時間之觀點而言,減塵之保持時間為8〜16秒,就相同之 理由而5,較佳為8〜15秒,更佳為9〜13秒。 減磨之保持時間於第2步驟(減慶步驟)中,係自洗淨样 内之I力達到Pl之時間點開始計算。第2步驟中,於洗淨 槽内之屡力例如減屋至5(kPa)之情形時,^為聊小自 洗淨槽内之壓力達到5(kPa)之時間點開始測量減塵之保持 =間。於第3步财’即便洗淨槽内之壓力上升或下降, 一要為P^G.VkPa)之範圍内的值,則亦可作為洗淨槽内之 愿力保持在減壓狀態而計算減壓之保持時間。 較佳為-邊對洗淨劑組合物施加超音波振動—邊進行第 3步驟。藉由經過第2步驟’而將間隙中所存在之空氣自上 述間隙迫出’藉此使助焊劑殘渣與洗淨劑組合物良好地接 觸’且若於對洗淨劑組合物中之溶存氣體進行脫氣後,對 I52501.doc 201134562 洗淨劑組合物施加超音波振動,則提 之助焊劑殘清之洗淨性, m中所存在 佳。 故了期待縮紐洗淨時間,因此較 就提高對於間隙中所存在之 被洗淨物損傷之觀點而言,第3步驟:f=淨性及抑制 予之超音波之頻率及超立波之Λ 合物賦 ,Η Λ 超曰波之此里密度較佳為20〜400 他、(Μ〜4.〇 w/cm2 HZ、G.2〜2.G W/cm2。 超曰波振動之賦予例如#南丨 振堡器進行。 係利用配置於洗淨槽内之超音波 不:之洗淨方法中,對洗淨劑組合物賦予超音波振動 =僅限^於第3步驟期間。對洗淨劑組合物賦予超音波振 動可於第1步驟〜第5步驟中之至少, 接”⑽甲之至广個步驟期間進行。就 ::間隙中所存在之助輝劑殘逢之洗淨性之觀點而 二 淨劑組合物賦予超音波振動較佳為於第!步驟〜第 5步驟之所有步驟中進行。 (第4步驟) ^,將洗淨槽内之壓力升屋至⑽叫^滿足關 5〇^P2S12〇(kPa) 〇 :第4步驟中’就提高對於間隙中所存在之助焊劑殘漬 二孑性之觀點而言’洗淨槽内之壓力較佳為HO〗… 之範圍内的壓力’更佳為8〇〜1〇2㈣之範圍内的壓力,進 而,佳為常塵。再者’所謂常壓係指未特別減麼或加塵時 之堅力’通常與大氣壓相等,大致41氣壓⑽!雄⑽。 ;第4 ^驟中’就同時實現提高對於較窄間隙中所存在 I52501.doc • 15· 201134562 之助焊劑殘渣之洗淨性與縮短洗淨時間之觀點而言,使洗 淨槽内之壓力成為P2(kPa)所需之升壓時間較佳為洗淨槽内 之壓力升麼開始後冰以上60秒以内,更佳為冰以上輝 以内’進而較佳為i秒以上10秒以内。 就提高對於較窄間隙中所存在之助焊劑録之洗淨性之 觀點而言,第4步驟中之洗淨劑組合物之溫度較佳為盘上 述第3步驟中之洗淨劑組合物的溫度相等,具體而言,較 佳為50〜7(TC ’更具體而言,較佳為與上述第3步驟中之保 持溫度相同之溫度。洗淨劑組合物之加熱視需要使用洗淨 槽中具備之加熱機構進行即可。第4步驟中之洗淨劑組合 物之上述溫度係利用洗淨槽内所設置之溫度計例如每… 所測定之溫度的平均值。該平均值可根據第3步驟中之洗 淨劑組合物之平均溫度的上述算式而求出。 (第4a步驟) 就提高對於較窄間隙中所存在之助焊劑殘渣之洗淨性之 觀點而言’本發明之洗淨方法較佳為更包括在第斗步驟 後、下述第5步驟之前進行升壓後壓力保持步驟(該步驟亦 稱為「第4a步驟」),其係將洗淨槽内之壓力p“呆持在 韻㈣之範圍内、且與P2±04(kPa)相等或高於 p2±〇.4(kPa)之壓力歷時8〜16秒鐘。尤其是於第4步驟中對 洗淨劑組合物施加超音波振動之情形時,就提高洗淨性之 觀點而言’本發明之洗淨方法較佳為包括上述第43步驟。 例如,於第4步驟中之洗淨槽内之壓力P2(kPa)低於常塵 之情形時’開放洗淨槽’使洗淨槽内之壓力與洗淨槽外之 I52501.doc 201134562 壓力平衡,將洗淨槽内之壓力與洗淨槽外之壓力的平衡狀 態保持特定時間即可。 於第3步驟中之洗淨槽内的壓力為p]±〇 4(kpa)之情形 時,尤其是就進行反覆洗淨時之效率性之觀點而言,第牦 步驟中之洗淨槽内之洗淨劑組合物的溫度較佳為 〜7〇t:。第4a步驟中之洗淨槽内之洗淨劑組合物的溫度 可於50〜70t之範圍内變動,更佳為與第4步驟中之洗淨劑 組合物的溫度相同之溫度。第4a步驟中之洗淨劑組合物之 t述溫度係利用洗淨槽内所設置之溫度計例如每!秒所測 定之溫度的平均值。該平均值可根據第3步驟令之洗淨劑 組合物之平均溫度的上述算式而求出。 第4a步驟中,就同時實現提高料間隙中所存在之助谭 劑殘逢之洗淨性與縮短洗淨時間之觀點而言,將洗淨槽内 之愚力p3保持在P2±0.4(kPa)或50〜12〇 kpa之範圍内之高於 ㈣撕a)的壓力之時間較佳為8〜_,更佳為8〜⑽, 進而較佳為9〜16秒。 上發牛明之洗淨方法包括第#步驟之情形時,若將包括 就同l 述第^步驟之一系列步驟作為1循環,則 淨性盘^見提高對於較窄間隙中所存在之助焊劑殘漬之洗 行上述U唐卢± 权佳為以20〜230秒鐘進 ㈣^ 較佳為以25〜UG秒鐘進行,更佳為以25〜60 R進仃,進而較佳為以25〜5〇秒鐘進行。 (第5步驟) 就提高對於較窄間隙中所存在之助焊劑殘^ 152501.doc 17 201134562 觀點而g ’本發明之'φ总 n a之“方法較佳為包括進而反覆進行 5〇次上述第2步驟〜第4步驟之反覆步驟(第5步驟)。第5 步驟中反覆進行之第2〜第4步驟以與第5步驟之前進行之上 ϋ第2日〜第4步驟相同之條件進行即可。具體而纟,就同時 貫現提向對於較窄問陏由π + 水t所存在之助焊劑殘渣之洗淨性盥 縮短洗淨時間之觀點而言,於反覆進行之第2步驟中,較 佳為將洗淨槽内之磨力減屢至…㈣之範圍内之屢 力,其減料間較佳為減壓開始後1秒以上120秒以内,洗 Γ劑組合物之溫度較佳為nc。又,就相同之觀點而 於反覆進订之第3步驟中,較佳為將洗淨槽内之壓力 保持在Pl±G.4(kPa)之屋力,更佳為將洗淨槽内之Μ力保持 在P!±〇.i(kpa)之屋力,洗淨劑組合物之溫度於洗淨槽内之 磨力為P1±G.4(kPa)之情形時,較佳為5㈣。c,洗淨劑組 口物之咖度更佳為固^,減壓之保持時間較佳為8〜⑽。 就相同之觀點而言’於反覆進行之第4步驟中,藉由升磨 達到之壓力較佳為常壓,洗淨劑組合物之溫度較佳 50〜70〇C。 再者,由於在每次結束上述第2〜第*步驟而更換洗淨槽 之情形時’必需進一步實施將被洗淨物浸潰於洗淨劑組合 物中之步驟(第1步驟),®此將「進而反覆進行1〜50次至 ^上述第2〜第4步驟之步驟」替換成「進而反覆進行卜5〇 次上述第1〜第4步驟之步驟」。又,於本發明之洗淨方法包 括上述第4a步驟之情形時’較佳為於第5步驟中所進行之 各第4步驟之後亦進行第4a步驟。於第5步驟包括第4a步驟 152501.doc 201134562 之情形時,將反覆進行之第2〜第4步驟作為⑽環時較佳 為於至少-個反覆循環後進行第4a步驟,就同時實現提高 對於較窄間隙中所存在之助焊劑殘潰之洗淨性與縮短洗淨 時間之觀點而言,更佳為於第5步驟中之所有循環後進行 第4a步驟,,於第5步驟中,較佳為反覆進行㈣次至 少包括上述第2步驟〜第_驟之】循環’較佳為反覆進行 1〜50次包括上述第1步驟〜第步驟之U盾環,或較佳為反 覆進行卜50次包括上述第2步驟〜第心步驟之工循環。 反覆次數⑷步驟中之上述循環數)根據被洗淨物之間 隙形狀及助焊劑殘渣之狀態而有所不同,但就提高對於間 隙中所存在之助焊劑殘渣之洗淨性及生產性之觀點而言, 較佳為㈣次,更佳為2〜35次,進而較佳為㈣次。藉由 以較短時間反覆進行上述第2步驟〜第4步驟、上述^步驟 〜第4a步,驟、或上述第2步驟〜第43步驟,而使由於壓力變 化而產生之物理力、與由於減璧保持步驟中之洗淨劑組合 物之沸騰而產生之物理力反覆附加於被洗淨物。因此,更 加提高對於較窄間隙中所存在之助焊劑錢之洗淨性。 (水含量之調整) 於本發明之洗淨方法中,亦可於用以洗淨一個被洗淨物 ,洗淨步驟之中途,於洗淨槽内之洗淨劑組合物中添加 , 為了洗淨複數個被洗淨物而連續使用洗淨槽之情 ^時亦可於用以洗淨各被洗淨物之洗淨步驟之中途及/ 或^前’於洗淨槽内之洗淨劑組合物中添加水。本發明之 先淨方法中,使洗淨劑組合物沸騰’因此尤其是於第5步 152501.doc •19· 201134562 驟中,反覆進行第2步驟〜第 組合物中之水含量會降,之過程中,彳時洗淨劑 用之洗净劑組合物中之各成分厅使 离之、、条渔w ± 0己比例之變動’維持較 同之洗淨性,較佳為於第丨步 前及/或t途,於洗淨槽内之洗之任一步驟之 制,先淨劑組合物中添加水,抑 制洗淨劑組合物之組成之變動。 例如利用水分感測器等水分 ^ _ T〜夂第1步驟〜第5步驟中 任-步驟之前及/或中途的洗淨劑組合物中之水之濃产, 根據測定值將水補給至洗淨槽内之洗淨劑組合物即可。為 了準確地敎洗淨劑組合物中之水之濃度,較佳為於㈣ _、循環泵、超音波__洗淨劑組合物之狀 態下測定水之濃度。 有關水分感測器之檢測器之類型並無特別限制,例如可 為近紅外線分光型、電容導電率型、導電率型之任一種。 對洗淨槽内之洗淨劑組合物補給水係藉由例如使副槽内 之洗淨劑組合物與洗淨槽内之洗淨劑組合物循環而進行, 該副槽具備連接於洗淨槽且根據洗淨槽中設置之水分感測 器的測定值而進行開閉之電磁閥。為了洗淨複數個被洗淨 物而連續使用洗淨槽之情形時,水之補給較佳為例如於為 了將被洗淨物移至沖洗槽中而自洗淨槽提起並除去液體期 間、且將其他被洗淨物投入至洗淨槽内之前進行。較佳為 水分感測器不僅設置於洗淨槽亦設置於副槽。 上述洗淨劑組合物中之水含量之調整可使用例如圖3所 示之洗淨裝置進行。 152501.doc •20- 201134562 如圖3所示,上述洗淨裝置包含:洗淨槽u,其含有可 將先淨劑組合物蓄積於内部,可調整内部壓力之壓力調整 部(未圖示)及可敎洗淨槽η之内部所蓄積之洗淨劑植合 物的水之濃度之水分計15;副槽14,其可f積洗淨劑組合 物,循環管路18,其具備可將洗淨槽u與副槽Μ連通,可 根據水分計i 5之測定值而開閉流路之閥} 7 (例如電磁闕); 以及送液部(泵等,未圖示),其根據水分計Η之測定值, 經由循環管路18使洗淨槽11内之洗淨劑組合物與副槽14内 之洗淨劑組合物循環。 该洗淨裝置中’若水分計15之測定值並非特定範圍内之 值’則可使閥17打開,並且送液部動作,經由循環管路18 14内之洗淨劑組合物與洗淨仙内之洗淨組合物循 環直至洗淨槽n内之洗淨組合物之水的濃度成為特定範圍 内之值。就確保對於助焊劑殘渣之較高之洗淨性之觀點而 言,上述特^範圍必須為2重量%以上师量%以下,就相 同之觀點而言’較佳為3〜8重量%,$而較佳為Η重量 %。又’特定範圍内之值較佳為洗淨槽_之洗淨組合物 之水的濃度之初始值。 於圖3所示洗淨裝置中,水分控制機構包含副槽14、水 分計15、及具備閥17之循環管路18。較佳為不僅洗淨槽 11,而且副槽14亦具備水分計16。上述洗淨裝置可進而: 有對洗淨槽U内經過洗淨步驟之被洗淨物進行預沖洗之第 1洗務槽12、及進行完卫沖洗之第2洗務槽13。 如此’若對用以洗淨被洗淨物之洗淨劑組合物補給水, 152501.doc •21 · 201134562 則亦可將洗淨劑組合物用於其他被洗淨物之洗淨因此較 為經濟。 (預備洗淨) 本發明之洗淨方法中,洗淨步驟亦可進而包括於糾步 驟之前,例如於與進行第丨步驟〜第5步驟之洗淨槽不同的 洗淨槽中所收容之洗淨劑組合物中浸潰被洗淨物一定時間 之步驟。上述洗淨劑組合物可與第丨步驟七步驟中所使 用之下述洗淨劑組合物相同,亦可為下述洗淨劑組合物以 外之先前公知的用以洗淨附著有助焊劑殘渣之被洗淨物的 洗淨劑組合物。對洗淨劑組合物之浸潰時間例如較佳為 1〜10分鐘。 [沖洗步驟] 沖洗步驟係洗條附著於被洗淨物上之洗淨劑組合物、殘 留之助焊劑殘/查、或再附著之助焊劑殘渣等污垢的步驟, 於本發月之/先淨方法均不包括第4&步驟及第5步驟之情形 時,係於第4步驟之後進行,於本發明之洗淨方法包括第 4a步驟但不包括第5步驟之情形時,係於第乜步驟之後進 行,於本發明之洗淨方法包括第5步驟之情形時,係於第5 步驟之後進行。沖洗步驟可使用一個沖洗槽進行,亦可使 用兩個以上之沖洗槽進行。 沖洗步驟除了例如將洗淨劑組合物換成沖洗劑組合物以 外,其他係藉由經過與上述洗淨步驟中之第丨步驟〜第4步 驟为別相同之條件之步驟而進行。即,於沖洗步驟之一例 中’將經過洗淨步驟之被洗淨物浸潰於收容於沖洗槽中之 152501.doc •22- 201134562 沖洗劑組合物令之後,進行依序包括減壓步驟 步驟、及升壓步驟之-系列步驟。該一系列步驟可包= 上述洗淨步驟中之第4a步驟(升錢座力保持步驟)相對庫 的步驟。除了沖洗步驟之第仏步驟中將洗淨劑組合物換成 沖洗劑組合物以外,亦以與洗淨步驟之第4a步驟相同之條 件進订X,較佳為於沖洗步驟中,將洗淨步驟中之 ^所使用之洗淨劑組合物換成沖洗劑組合物,反覆進行 咸壓步驟、減壓保持步驟、及升壓步驟之-系列牛 :驟更佳為反覆進行包括減壓步驟、減壓保持步驟、升壓 升壓後壓力保持步驟之一系列步驟。關於各步驟 =度、星力、時間、循環數、"盾環所花費之時間、 超曰波振動之賦予等條件’亦可與洗淨步驟中相同。 沖洗步驟中之第2〜第4步驟之反覆次數或第2〜第4a牛驟 =覆次數根據上述污垢之程度而適#決定即可二 良好之洗滌性與提高生產性 ,兼八 更佳為W。次,進而較佳為2 3 §,較佳為1〜5〇次’ 次。於使用稽數個沖洗槽之;〜:人,更進而較佳為3〜30 吸双1u汗洗槽之情形時,各 洗次數總計為上述次數即可。 s 仃之沖 上述沖洗劑組合物中通常 水等’拫據污垢之程度,較佳使用將=為使用離子交換 水、較佳為離子交換水加以以而料 劑組合物與 稀釋液。於使用該稀釋液作為;洗淨:組合物之 述冲洗步驟包括使用稀釋液之沖洗步 < 月形時,上 為離子交換水作為沖洗刹組合物之完巧3驟用水、較佳 工冲洗步騾,為了將 I5250i.doc •23· 201134562 該等加以區別,而將使用稀釋液之沖洗步驟稱為預沖洗步 驟。預沖洗步驟及完工沖洗步驟分別例如使用與洗淨步驟 中所使用之洗淨槽相同的洗淨槽作為沖洗槽而進行。 若於完工沖洗步驟後,污垢及/或洗淨劑組合物未殘留 於被洗淨物,則預沖洗步驟中所使用之沖洗劑組合物中之 洗淨劑組合物的水以外之有效成分之含量並無特別限制, 較佳為0.0001〜10重量。/〇,更佳為〇 〇〇〇1〜8重量%,進而軾 佳為0.0001〜5重量0/〇。 預沖洗步驟中所使用之沖洗劑組合物中可含有下述洗淨 劑組合物以外之先前公知之用以洗淨附著有助焊劑殘渣的 被洗淨物之洗淨劑組合物。於沖洗劑組合物中包含下述洗 淨劑組合物、或上述公知洗淨劑組合物之任一情形時/就[Technical Field] The present invention relates to a method for cleaning a washed object to which a flux residue adheres, a method for producing an electronic component using the cleaning method, and the washing method A cleaning method for the net method. / [Prior Art] Previously, a group of detergents containing a detergent-attached material that was attached to a smuggled fish was known to contain a combination of an ethylene glycol-based compound and an amine-based compound: T, Patent Document 2, etc. Or a composition containing a surfactant (refer patent documents 3, 4, etc.), etc.. Moreover, although it is not attached to the method of cleaning the washed matter of (4)_, is it a cleaning method for removing the abrasive attached to the parts of the wristwatch or the like, and does it increase the surrounding of the washing liquid? The operation of the force and the operation of reducing the pressure around the cleaning liquid are alternately applied to the tube tube for a plurality of times of cleaning (see Patent 5), and the method for cleaning the parts having a gap such as a fine bag-like hole is revealed. The pressure reduction and the normal pressure transformation (P-Swlng) washing method are repeatedly performed in the liquid tank (refer to Patent Document 6, etc.). In the washing method described in Patent Document 5, as the detergent composition, for example, a solvent petroleum brain-based washing liquid is used. In the cleaning method described in Patent Document 6, the dilution of the surfactant is used as the detergent composition, and after the pressure in the tank is reduced to the required pressure, the control valve is immediately switched to the normal pressure.门 阪 先前 先前 先前 先前 152 152 152 2011 2011 2011 2011 2011 2011 2011 2011 2011 2011 2011 2011 2011 2011 2011 2011 2011 2011 2011 2011 2011 2011 2011 2011 2011 2011 2011 2011 2011 2011 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 Japanese Patent Laid-Open Publication No. Hei. No. Hei. No. Hei. No. Hei. No. Hei. No. Hei. The problem to be solved by the invention is that in the manufacturing process of an electronic component such as a semiconductor device, when a component (for example, a semiconductor wafer, a chip capacitor, or another circuit substrate) is mounted on a circuit board, the circuit board may be formed on the circuit board. A space (gap) is formed between the parts. The solder used for mounting the above-mentioned components contains a flux. However, if the flux remains in the gap as a residue for a long period of time after soldering, migration or the like occurs, which causes a short circuit between the electrodes. With the miniaturization and high density of electronic components, a semiconductor wafer mounting method using solder bumps such as a flip chip method is often used, and the installation is prone to be more cumbersome. Therefore, the importance of cleaning the flux residue in the manufacture of electronic parts is further enhanced. However, with the miniaturization and high density of the electronic components, the above-mentioned gaps are difficult to remove the flux residue entering the narrow gap, and as a result, the productivity of the electronic components is degraded. Therefore, it is desired to develop a cleaning method in which the flux residue remaining in the gap is excellent in removability. 15250).doc 201134562 The present invention provides a kind of cleaning material which is not only for a narrow fishing net. The agent is "relative, and the washing power of the water is also good. The foaming method is used to clean the washed residue of the flux residue." and: Use: The manufacturing method of the electronic parts of the net method and use Technical Solution for Solving the Problem The cleaning method of the washed matter to which the flux is adhered in the present invention includes washing the step of washing the adhered material with the flux residue by using the detergent composition. The washing step includes: a step of impregnating the detergent composition to which the flux is adhered to the detergent composition contained in the cleaning tank of the adjustable pressure (first step); The dusting force in the washing tank is reduced to a pressure reducing step (second step) satisfying the pressure P1 (kPa) of the following formula (1); the above-mentioned washing in the depressurizing step is carried out under reduced pressure for 8 to 16 seconds. The pressure in the tank is maintained at the crucible (10)), and the above washing in the above-mentioned washing tank The temperature of the detergent composition is maintained at 50 to 7 (the pressure reduction holding step of TC (third step); and after the pressure reduction holding step, the pressure in the cleaning tank is such that the following formula (2) is satisfied. The pressure step (step 4) of the pressure pjkPa). The above second step to fourth step are carried out in 10 to 220 seconds. 2) (2) 0.1 (kPa)^P1^7 (kPa) 50 (kPa) $ P2$ 120 (kPa) The detergent composition contains 2% by weight or more of water (component A) of less than 9% by weight, 50% by weight or more and less than 97.75% by weight of the glycol ether (ingredient B) 'and 〇.〇 5 wt% or more and 5 wt%. /. The following amine compound (ingredient C). The above component B is represented by the following general formula (1). R]-0-(E0)m-R2 (1) 152501.doc 201134562 In the above formula (1), 'R1 is an alkyl group having a carbon number, and R2 is a hydrogen atom or a carbon number of 1 to 3, and EO is Oxygen-extended ethyl group, m represents the average addition molar number of EO', and the above-mentioned component C is represented by the following general formula (2). R3-n-(E〇)ph (UH (2) In the above formula (2), R3 represents a hydrogen atom or an alkyl group of carbon number 4, and E〇 is an oxygen-extension ethyl group 'p, q respectively The average addition molar number of E〇 satisfies 1 each p+q$ 4. The manufacturing method of the electronic component including the solder bump of the present invention comprises: forming a solder on the substrate of the electronic component using a solder flux containing a flux a step of bumping; and a step of cleaning the flux residue derived from the flux by the cleaning method of the above-mentioned washed object of the present invention. The cleaning device of the present invention is a washing of the washed object of the present invention. a cleaning device for a clean method; and a moisture control mechanism for causing the water (former A) of the detergent composition in the cleaning tank to have a content of 2% by weight or more and 5% by weight or less EFFECTS OF THE INVENTION In the present invention, a specific detergent composition is used, and a series of steps including a salt pressure step, a pressure reduction holding step, and a pressure increasing step are sequentially employed as a cycle because of a specific time. Performing this cycle, the physical force and cause due to pressure changes Detergent (4) step of the detergent composition 152501. (J〇q 201134562 / Fu Teng and the physical strength of the house to taste the role of the broken powder in the narrow gap of the material exists in the flux residue Therefore, ]t Υ /Γ仔 is not only in the supply of the flux residue in the narrow gap, but also has good cleanability, and the foaming is good The method of cleaning the cleaned material of the flux residue and the method of manufacturing the electronic component including the solder bump using the cleaning method is omitted. < · The rosin-based flux containing rosin or rosin derivative used in the case of q π, in the present invention, the welding method of the reflow method and the flow mode. In the present invention, the term "draining agent" refers to a mixture of a stilbant and a auxiliaries. The term "flux residue" refers to a source of self-retaining on a substrate after soldering using a flux or a tan flux. In the present invention, the scoop person contains the ship (Pb) solder and no external solder." 匕3, the term "physical due to the boiling of the detergent composition" means washing by The water contained in the detergent composition is stagnation and production: the so-called "frozenness of the detergent composition" means the boiling of the water of the detergent. Thereby, the more the amount of the detergent composition is, the larger the physical force is, and the smaller the detergent composition is, the smaller the physical force is. The cleaning method of the washed matter to which the flux residue is adhered according to the present invention is also referred to as "the cleaning method J", and the use of the specific glycol ether and the specific amine compound respectively in the specific water is used. The detergent composition having a content of 2% by weight or more and 10% by weight or less is subjected to a 152501.doc 201134562 sequence including a reduction step, a reduction column, a retention step, and a step of -1 step In the step, and even if the holding time of the reduction is short, a certain time is ensured, and it is unexpectedly found that the flux residue remaining in the flux is more excellent, the foaming is suppressed, and the washing of the water is not green. In the case where the above-mentioned series of steps are 1 circumstance, when the repetitive grading 1 is re-introduced into the 仃1 cycle, the cleaning property of the X.Vjfc flux residue which is present in the narrow gap is further improved. Therefore, if the cleaning method of the present invention is used in the manufacturing process of the electronic component including the solder bumps, it is expected to improve the productivity or reliability of the electronic component. [The method of cleaning the object to be washed] Cleaning method For example, the washing step is sequentially performed, the rinsing step of washing the washed matter using the rinsing agent composition, and the drying step. [Washed material] As the washing method of the present invention, the washed object is preferably used. A manufacturing intermediate including a circuit board or the like and a component soldered to a circuit board or the like is included, and the manufacturing inter-substance contains a flux residue in a gap between the circuit board and the component. The intermediate is a semiconductor package or a semiconductor device. The manufacturing intermediate in the manufacturing step of the electronic component includes, for example, a semiconductor wafer, a wafer type electric valley Is, and other circuit boards mounted on the circuit board by soldering using a flux. The gap is, for example, a space between a circuit board and the above-described components mounted on the circuit board by soldering, and the height (the shortest distance between the circuit board and the component) is, for example, 5 to 500 μm, 1 to 250 μm, Or a space of 2〇~100 μΠ1. The width and depth of the gap depend on the size or spacing of the electrodes (solder joints) on the mounted component or circuit board. Such as 152501.doc 201134562 is 130~20000 4 melon or 13〇~1〇〇〇〇μιη, the depth is 13〇~25〇〇〇Claw or 130~10000. [Washing step] Washing steps include: will attach The impregnation step of the flux residue impregnated with the adjustable pressure in the following detergent composition contained in the cleaning tank (the impregnation step is also referred to as "the third step"); a pressure reduction step in which the pressure in the washing tank is reduced to a specific value (the pressure reducing step is also referred to as "second step"); maintaining the pressure in the depressurized washing tank in the depressurizing step at a specific specific time for a specific period of time a pressure reduction holding step in which the temperature of the detergent composition in the washing tank is maintained within the temperature range (the pressure reduction holding step is also referred to as "third step"); After the step, the pressure in the wash = is boosted to a specific value step (this step is also referred to as the fourth step). The washing step may further include a post-boost pressure maintaining step (step 2) and/or a fifth step. The step 4a is carried out after the fourth step, and is carried out before the fifth step in the case where the washing includes the fifth step. In the step 4a, the pressure in == is maintained within a specific pressure range and is continuously maintained, and the fifth step is performed after the fourth step, and in the case where the washing step is blunt, the step is repeated in the fourth step - At least the steps of the second step of the above step are sequentially included. In the U4 step, one of the washing methods of the umbrella is praised, and the cleaning tank may be used for two or more washing tanks. For example, when the washing tank is subjected to the washing method of the present invention, No. 5: In the fifth step, I52501.doc 201134562 may be performed without repeating the i-th step. In the case of the human music 2 steps to the fourth step, the present invention is implemented in two or more washing tanks. The washing method β is repeated in the fifth step, and may also be in the case of the 铱c soil brother 1 dream step 4 step 15 step towel is the sputum, = step ~ 2 ^ V ; "x 1 °^2 2 °# # ^ ^ ^ ^ ^ 'P includes a series of steps from step 2 to step 4 above to improve the cleanliness of the flux residue present in the narrow gap and From the viewpoint of shortening the washing time, it is preferably carried out at 15 to H) for 0 seconds, more preferably for 15 to 50 seconds, and further preferably for a heart of (10) seconds. (Step 1) First, in the step, the detergent residue adhered to the detergent residue in the cleaning tank containing the detergent composition is first added to the detergent composition. The amount of the detergent composition to be washed is not particularly limited as long as the amount of the object to be washed is impregnated. The cleaning tank may be, for example, a heating mechanism. a pressure vessel such as an ultrasonic oscillator, etc. The cleaning tank is connected to an air pipe connected to a suction device such as a vacuum pump, and the air pipe includes a branch pipe that is not connected to the suction device. In the pipe, the opening and closing control of the switching control valve is performed, and the pressure in the cleaning tank is reduced to the required pressure or the pressure is raised to the required pressure. An example of the above-described cleaning tank is disclosed in Japanese Laid-Open Patent Publication No. Hei 6-29694 No. 152501. .doc -10- 201134562 In the first step, from the viewpoint of improving the detergency, the temperature of the detergent composition filled in the washing tank is preferably 50 to 70 C immediately before the pressure reduction is started. More preferably, it is 55 to 70. (:, and further preferably 60 to 70. (:. specifically, δ, which is adjusted to be 〇~4〇〇c, the detergent composition is filled into the above-mentioned washing tank) Heating is carried out to a temperature within the above preferred range. The heating of the compound may be carried out by using a heating mechanism provided in the washing tank. The temperature of the detergent composition is measured by a thermometer provided in the washing tank. (Second step) Next, the washing tank is cleaned. The pressure inside is depressurized to Pi (kPa). Ρι satisfies the relationship of 0.1 (kPa) $ p 丨彡 7 (kPa). In the second step, it improves the presence of the narrow gap in the washed object. From the viewpoint of the detergency of the flux residue and the shortening of the washing time, it is more preferable to depressurize the inside of the washing tank until it is preferably 〇1 to _ small, preferably 0.1 to 5 (kPa), and further Good for the pressure within the range of ~ (4)). In the second step, the detergent composition can be forcibly mixed in a narrower gap by decompression. Thus, the flux residue present in the narrow gap can be prevented from coming into contact with the detergent composition. The air is forced out from the gap, and the dissolved gas contained in the detergent composition can also be degassed. Therefore, the cleaning method of the present invention is suitable as a washing method for the residue of the aid agent which is mixed into a narrow gap. In the second step, the pressure in the clean tank of the cleaning I52501.doc 201134562 is P1 (the viewpoint of improving the detergency of the coal-carrying agent residue present in the narrow gap and shortening the washing time). kPa) required decompression r 1 is more difficult, preferably more than 1 second or more after the start of decompression of the pressure in the washing tank, more preferably within 1 second to 60 seconds, and more preferably 】 Within seconds, further better than 1 second and 15 seconds. ~ In the second step, (4) to improve the cleaning property of the flux (4) present in the narrow gap and shorten the cleaning time, the pressure in the cleaning tank is Pl (kPa) The speed is preferably i5 to 3Q (kpa/s), more preferably 17 to 30 (kPa/s), and still more preferably 18 to 3 Å (kpa/s). From the viewpoint of improving the detergency of the cognac money present in the narrow gap, more specifically, obtaining a higher physical force and suppressing the detergent by boiling of the detergent composition The evaporation of water in the composition suppresses the decrease in water in the washing tank, and the detergent composition in the second step is suppressed from the viewpoint of suppressing the deterioration of the detergent property due to the composition fluctuation of the detergent composition. The temperature is the same as in the first step, preferably 5 〇 7 7 (rc, more preferably 55 to 70 ° C, still more preferably 6 〇 7 7 Torr). The heating of the detergent composition is required to be washed. Preferably, in the second step, the temperature of the detergent composition adjusted to the temperature within the preferred range in the first step is maintained in the second step. In the second step The above temperature of the detergent composition is an average value of the temperature measured per 1 second by a thermometer provided in the washing tank, and the average value may be based on the average temperature of the detergent composition in the third step described below. Calculated by the formula. (Step 3) Next, in the depressurization holding step, 'Continuous 8 The pressure in the above-mentioned depressurization step in the degassing washing tank was maintained at p>±〇4 kPaT for 16 seconds, and the temperature of the detergent composition in the 152501.doc 12 201134562 washing tank was maintained at 5 〇~70〇C. In the third step, from the viewpoint of maintaining a stable boiling state of the detergent composition, the pressure in the washing tank must be 〇, from the same viewpoint, the third step The fluctuation range of the pressure in the washing tank is preferably P1: t〇_3 (kPa), more preferably P1 ± 0 2 (kPa), and further preferably Pi ± 0.1 (kPa). The pressure in the washing tank in the holding step is preferably substantially constant, more preferably fixed. Further, the pressure in the washing tank is measured by a manometer. The boiling of the detergent composition is maintained. From the viewpoint of the state, the temperature of the detergent composition in the third step must be 5 Torr to 7 Torr when the pressure in the washing tank is PpO.VkPa). In other words, from the viewpoint of improving the detergency of the flux residue present in the gap by the physical force of boiling, when the pressure 匕 in the cleaning tank is 〇, it is preferably 50 to 70°. C. When the pressure in the washing tank exceeds 5 kPa and is 7 kpa or less, it is preferably 60 to 70. (: The temperature of the detergent composition in the third step may vary from 5 Torr to 7 Torr. The temperature range of 〇 varies, but the change is maintained from the viewpoint of maintaining a stable boiling state of the detergent composition. The amplitude is based on the average value of the temperature of the detergent composition in the third step, and the car is good as the illusion. (4), more preferably the gentry is less than or equal to ±0.2. That is, in the cleaning method of the present invention, the temperature of the detergent composition in the third step is preferably substantially fixed, and more preferably fixed. The temperature of the detergent composition in the third step is 0. The thermometer provided in the washing tank is measured, for example, every one second. The detergent combination in the third step 152501.doc 201134562 The average value Tx (time average holding temperature) of the material/dish can be determined.遴 而 时间 时间 时间 Σ Σ Σ Σ Σ Σ Σ Τ Τ Τ Τ Τ Τ Τ Τ Τ Τ Τ Τ Τ Τ Τ Τ Τ Τ Τ Τ Τ Τ Τ Τ Τ Τ Τ Τ 保持 保持 保持 保持 保持 保持 保持 保持 保持 保持 保持 保持In the view of improving the detergency of the flux residue in the narrower (four), the sea of the detergent composition The state must be 8 or more. In addition, at the same time, the maintenance of the depletion of the flux remaining in the gap and the shortening of the cleaning time are simultaneously achieved, and the decompression is maintained: (the time of the third step) It must be 16 seconds or less. Therefore, the dust holding time is 8 to 16 seconds from the viewpoint of improving the cleaning property of the flux residual edge and the cleaning time in the gap. The reason is 5, preferably 8 to 15 seconds, more preferably 9 to 13 seconds. The holding time of the grinding is in the second step (decreasing step), and the time when the I force in the self-cleaning sample reaches Pl The point starts to calculate. In the second step, when the repeated force in the washing tank is reduced to 5 (kPa), for example, the measurement starts at the time point when the pressure in the self-cleaning tank reaches 5 (kPa). Dust reduction retention = between. In the third step, even if the pressure in the washing tank rises or falls, the value within the range of P^G.VkPa) can also be used as the wish in the washing tank. The holding time of the reduced pressure is calculated while maintaining the reduced pressure state. Preferably, the ultrasonic vibration is applied to the detergent composition. Step 3. By the second step 'the air present in the gap is forced out from the gap ' thereby allowing the flux residue to be in good contact with the detergent composition' and if in the detergent composition After the degassing of the dissolved gas, ultrasonic vibration is applied to the I52501.doc 201134562 detergent composition, and the cleaning property of the flux residue is improved, so that it is excellent in m. Therefore, in terms of improving the damage to the washed matter existing in the gap, the third step: f = netness and suppression of the frequency of the ultrasonic wave and the super-wave complex, Η Λ super-wave Here, the density is preferably 20 to 400, (Μ~4.〇w/cm2 HZ, G.2 to 2.GW/cm2. The super-wave vibration is given by, for example, #南丨振堡器. Ultrasonic vibration is applied to the detergent composition by the ultrasonic cleaning method disposed in the cleaning tank = only during the third step. Ultrasonic vibration can be applied to the detergent composition at least at least one of the first step to the fifth step, and the process of "10" is carried out until a wide step. From the viewpoint of the net nature, it is preferred that the ultrasonic composition imparts ultrasonic vibration to all the steps from the first step to the fifth step. (Step 4) ^, the pressure in the washing tank is raised to (10) Satisfied with 5〇^P2S12〇(kPa) 〇: In the fourth step, 'the pressure in the cleaning tank is better than the viewpoint of improving the compatibility of the flux residue in the gap. The pressure in the range is better than the pressure in the range of 8〇~1〇2(4), and then the normal dust. In addition, the so-called normal pressure means the strength is not particularly reduced or the dust is usually 'atmospheric pressure'. Equivalent, approximately 41 air pressure (10)! Male (10). In the 4th step, the viewpoint is to improve the cleaning performance and shortening the cleaning time of the flux residue of I52501.doc • 15· 201134562 which exists in the narrow gap. In other words, the pressure increase time required to make the pressure in the cleaning tank P2 (kPa) is preferably in the cleaning tank. When the pressure rise starts, the ice is less than 60 seconds, more preferably less than the ice, and further preferably less than 10 seconds and less than 10 seconds. In terms of improving the cleanliness of the flux recorded in the narrow gap, The temperature of the detergent composition in the fourth step is preferably such that the temperature of the detergent composition in the third step of the tray is equal, specifically, preferably 50 to 7 (TC' more specifically. Preferably, the temperature is the same as the temperature maintained in the third step. The heating of the detergent composition may be carried out by using a heating means provided in the cleaning tank. The detergent composition in the fourth step The above temperature is an average value of the temperature measured by a thermometer provided in the cleaning tank, for example, the average value can be obtained from the above formula of the average temperature of the detergent composition in the third step. Step 4a) In terms of improving the detergency of the flux residue present in the narrow gap, the cleaning method of the present invention preferably further comprises the step of the step after the third step Post-press pressure holding step (this step It is called "Step 4a"), which is to keep the pressure p in the washing tank within the range of rhyme (4) and equal to or higher than P2 ± ( (4 kPa). The pressure lasts for 8 to 16 seconds. Especially in the case where ultrasonic vibration is applied to the detergent composition in the fourth step, the cleaning method of the present invention preferably includes the above from the viewpoint of improving the detergency. Step 43. For example, when the pressure P2 (kPa) in the washing tank in the fourth step is lower than that of the normal dust, the 'opening washing tank' causes the pressure in the washing tank to be I52501 outside the washing tank. Doc 201134562 Pressure balance, keep the balance between the pressure in the washing tank and the pressure outside the washing tank for a specific time. In the case where the pressure in the washing tank in the third step is p] ± 〇 4 (kpa), especially in the viewpoint of the efficiency at the time of the reverse washing, the washing tank in the second step The temperature of the detergent composition is preferably ~7 〇t:. The temperature of the detergent composition in the cleaning tank in the step 4a may be varied within the range of 50 to 70 t, more preferably the same temperature as the temperature of the detergent composition in the fourth step. The temperature of the detergent composition in the step 4a is determined by using a thermometer provided in the washing tank, for example, every! The average of the temperatures measured in seconds. The average value can be obtained from the above formula of the average temperature of the detergent composition in the third step. In the step 4a, the fooling force p3 in the washing tank is maintained at P2 ± 0.4 (kPa) from the viewpoint of simultaneously improving the cleaning property of the agent and the washing time which are present in the material gap. The time of the pressure higher than (4) tearing a) in the range of 50 to 12 〇 kpa is preferably 8 to _, more preferably 8 to 10, more preferably 9 to 16 seconds. When the method of cleaning the Niu Mingming includes the step #1, if a series of steps including the same step is used as one cycle, the netness is improved to improve the flux present in the narrow gap. The washing of the residual stains is carried out in the above-mentioned U Tanglu ± quanjia for 20 to 230 seconds (4), preferably 25 to UG seconds, more preferably 25 to 60 R, and more preferably 25 ~5〇 seconds to proceed. (Step 5) In order to improve the flux residue in the narrow gap, 152501.doc 17 201134562, the method of 'φ total na of the invention is preferably included to further repeat 5 times. Steps 2 to 4 of the fourth step are repeated (step 5). Steps 2 to 4 which are repeatedly performed in the fifth step are performed under the same conditions as the second to fourth steps before the fifth step. However, in the second step of repeating, in view of the fact that the cleaning time of the flux residue which is present by the π + water t is narrower, the washing time is shortened. Preferably, the grinding force in the washing tank is reduced to the range of (4), and the temperature between the reducing materials is preferably less than 1 second and 120 seconds after the start of the pressure reduction, and the temperature of the detergent composition is higher. Preferably, in the third step of repeating the same viewpoint, it is preferable to maintain the pressure in the washing tank at a pressure of P1±G.4 (kPa), and more preferably to wash. The force in the clean tank is maintained at P!±〇.i(kpa), and the temperature of the detergent composition in the washing tank is P1±G.4 (kPa). In the case of a shape, it is preferably 5 (four). c, the calorie of the detergent group is more preferably a solid, and the holding time of the reduced pressure is preferably 8 to 10. The same viewpoint is used to repeat the fourth In the step, the pressure reached by the pulverization is preferably normal pressure, and the temperature of the detergent composition is preferably 50 to 70 〇 C. Further, since the cleaning is performed every time the second to the *th steps are completed, the cleaning is performed. In the case of a groove, it is necessary to further carry out the step of immersing the object to be washed in the detergent composition (first step), and this will "further repeat 1 to 50 times to ^2 to 4th steps above. The "step" is replaced by "the step of repeating the above steps 1 to 4". Further, in the case where the cleaning method of the present invention includes the above-mentioned step 4a, it is preferable to carry out the fourth step after each of the fourth steps performed in the fifth step. When the fifth step includes the fourth step 152501.doc 201134562, the second to fourth steps to be repeated as the (10) ring are preferably at least one repeated cycle and then the fourth step is performed, and the improvement is simultaneously achieved. From the viewpoint of the detergency of flux remnant and the cleaning time in the narrow gap, it is more preferable to carry out step 4a after all the cycles in the fifth step, and in the fifth step, Preferably, the step of repeating (four) times includes at least the above-mentioned second step to the first step of the cycle, preferably repeating 1 to 50 times of the U shield ring including the first step to the first step, or preferably repeating The sub-step includes the above-mentioned second step to the first step of the first step. The number of cycles in the number of times of the repetition (4) is different depending on the shape of the gap of the object to be washed and the state of the flux residue, but the viewpoint of improving the detergency and productivity of the flux residue existing in the gap is improved. In general, it is preferably (four) times, more preferably 2 to 35 times, and still more preferably (four) times. By repeating the second step to the fourth step, the step - 4a step, or the second step to the 43rd step in a short time, the physical force due to the pressure change and the The physical force generated by the boiling of the detergent composition in the step of reducing the holding is repeatedly applied to the object to be washed. Therefore, the cleansing power of the flux present in the narrow gap is further improved. (Adjustment of water content) In the cleaning method of the present invention, it is also possible to wash a washed object, and to add it to the detergent composition in the washing tank in the middle of the washing step, in order to wash A plurality of washed objects and a continuous use of the washing tank can also be used in the washing step for washing the washed objects and/or before the cleaning agent in the washing tank. Water is added to the composition. In the first method of the present invention, the detergent composition is boiled. Therefore, especially in the fifth step 152501.doc •19·201134562, the water content in the second step to the second composition is repeated. During the process, each component of the detergent composition used in the detergent composition maintains a similar change in the ratio of the deviation of the fish to the ratio of w ± 0, preferably in the first step. Pre- and/or t-way, in the step of washing in the washing tank, water is added to the first detergent composition to suppress the composition of the detergent composition. For example, water is used as a water sensor, and the water is concentrated in the detergent composition before and/or in the first step to the fifth step, and the water is supplied to the washing according to the measured value. The detergent composition in the clean tank can be used. In order to accurately measure the concentration of water in the detergent composition, it is preferred to measure the concentration of water in the state of (iv) _, circulation pump, ultrasonic __ detergent composition. The type of the detector for the moisture sensor is not particularly limited, and may be, for example, any of a near-infrared spectroscopy type, a capacitance conductivity type, and a conductivity type. The water supply to the detergent composition in the cleaning tank is performed by, for example, circulating a detergent composition in the sub tank and a detergent composition in the cleaning tank, and the sub tank is connected to the cleaning. The solenoid valve that opens and closes according to the measured value of the moisture sensor provided in the cleaning tank. In the case where the washing tank is continuously used for washing a plurality of objects to be washed, the replenishment of water is preferably, for example, during the period in which the liquid is lifted and removed from the washing tank in order to move the object to the washing tank, and It is carried out before putting other washed materials into the washing tank. Preferably, the moisture sensor is disposed not only in the cleaning tank but also in the sub tank. The adjustment of the water content in the above detergent composition can be carried out using, for example, the cleaning apparatus shown in Fig. 3. 152501.doc • 20-201134562 As shown in Fig. 3, the cleaning device includes a cleaning tank u containing a pressure adjusting unit (not shown) that can store the detergent composition inside and adjust the internal pressure. And a moisture meter 15 for the concentration of the water of the detergent plant accumulated in the interior of the washing tank η; a subtank 14 which can accumulate the detergent composition and a circulation line 18 which is provided The cleaning tank u is connected to the sub tank, and the valve of the flow path can be opened and closed according to the measured value of the moisture meter i 5 (for example, electromagnetic enthalpy); and the liquid supply unit (pump or the like, not shown) based on the moisture meter The measured value of ruthenium circulates the detergent composition in the cleaning tank 11 and the detergent composition in the sub tank 14 via the circulation line 18. In the cleaning apparatus, if the measured value of the moisture meter 15 is not a value within a specific range, the valve 17 can be opened, and the liquid supply unit can be operated, and the detergent composition and the cleaning liquid can be passed through the circulation line 18 14 . The inner washing composition is circulated until the concentration of water in the washing composition in the washing tank n becomes a value within a specific range. From the viewpoint of ensuring high detergency of the flux residue, the above-mentioned range must be 2% by weight or more and less than or equal to the amount of the amount, and is preferably 3 to 8% by weight, from the same viewpoint, It is preferably Η% by weight. Further, the value within the specific range is preferably the initial value of the concentration of water in the cleaning composition of the washing tank. In the cleaning apparatus shown in Fig. 3, the moisture control means includes a sub tank 14, a moisture meter 15, and a circulation line 18 having a valve 17. Preferably, not only the cleaning tank 11, but also the sub-tank 14 is provided with a moisture meter 16. Further, the cleaning device may further include: a first washing tank 12 for pre-rinsing the washed matter in the washing tank U through the washing step, and a second washing tank 13 for performing the flushing. Thus, if the detergent composition for washing the washed matter is replenished, 152501.doc •21 · 201134562 can also be used to wash the detergent composition for other washed materials, which is economical. . (Preparation for washing) In the cleaning method of the present invention, the washing step may further include washing before being subjected to the correcting step, for example, in a washing tank different from the washing tank for performing the second step to the fifth step. The step of immersing the detergent in the detergent composition for a certain period of time. The detergent composition may be the same as the following detergent composition used in the seventh step of the second step, or may be a previously known flux to be washed and adhered to the flux residue other than the following detergent composition. A detergent composition for the laundry. The impregnation time for the detergent composition is, for example, preferably from 1 to 10 minutes. [Rinsing Step] The rinsing step is a step of adhering the detergent to the detergent composition on the object to be washed, residual flux residue/inspection, or re-attaching flux residue, etc. When the net method does not include the fourth step and the fifth step, it is performed after the fourth step. When the cleaning method of the present invention includes the step 4a but does not include the fifth step, it is tied to the third step. After the step, when the cleaning method of the present invention includes the fifth step, it is carried out after the fifth step. The rinsing step can be carried out using one rinsing tank or by using more than two rinsing tanks. The rinsing step is carried out by, for example, replacing the detergent composition with the rinsing composition, and the other steps are carried out by the same conditions as the second to fourth steps in the above-described washing step. That is, in one example of the rinsing step, after the rinsing agent in the washing step is immersed in the 152501.doc •22-201134562 rinsing agent composition contained in the rinsing tank, the steps including the decompression step are sequentially performed. And the steps of the boost step - series. The series of steps may include the step of the fourth step (the rising seat holding step) of the above washing step relative to the library. In addition to replacing the detergent composition with the rinse composition in the third step of the rinsing step, X is also prepared under the same conditions as step 4a of the washing step, preferably during the rinsing step. The detergent composition used in the step is replaced with a rinsing agent composition, and the salt pressure step, the pressure reduction holding step, and the pressure increasing step are repeatedly performed - the series of cattle: the step is more preferably repeated, including a pressure reduction step, A series of steps of the pressure reduction holding step and the pressure increasing step after pressure boosting. The conditions such as the degree = degree, star force, time, number of cycles, "time taken by the shield ring, and the imparting of the ultra-chopping vibration' may be the same as in the washing step. The number of times of the second to fourth steps in the rinsing step or the number of times from the second to the fourth step 4 to the number of times of the smear can be determined according to the degree of the above-mentioned dirt, and the two can be cleaned and the productivity is improved. W. More preferably, it is 2 3 §, preferably 1 to 5 times. In the case of using a plurality of rinsing tanks; ~: human, and more preferably 3 to 30, in the case of sucking double 1u sweat washing tanks, the total number of washings may be the above-mentioned number of times. s 仃 冲 The above rinsing composition is usually water or the like. Depending on the degree of soiling, it is preferred to use the ion-exchanged water, preferably ion-exchanged water, to form the composition and the diluent. The use of the diluent as a washing step: the rinsing step of the composition includes a rinsing step using a diluent < In the shape of a moon, the ion-exchanged water is used as the flushing brake composition of the flushing brake composition, and the washing step is used. In order to distinguish the I5250i.doc • 23· 201134562, the diluent is used. The rinsing step is called a pre-flushing step. The pre-rinsing step and the completion rinsing step are performed, for example, using the same washing tank as the washing tank used in the washing step as the rinsing tank. If the soil and/or detergent composition does not remain in the object after the completion of the rinsing step, the active ingredient other than the water of the detergent composition in the rinsing composition used in the pre-rinsing step The content is not particularly limited, and is preferably 0.0001 to 10 parts by weight. /〇, more preferably 〇1~8 wt%, and then 轼 preferably 0.0001~5 weight 0/〇. The rinse composition used in the pre-rinsing step may contain a previously known detergent composition for washing the deposited residue to which the flux residue is attached, other than the following detergent composition. When any of the following detergent compositions or the above-described known detergent compositions are included in the rinse composition,

提高殘留之助焊劑殘渣、或再附著之助焊劑殘潰等污垢L 洗滌性之觀點而言,沖洗劑組合物中之水之含量較佳 90〜99.9999重量更佳為92〜99.9999重量%,進而較佳為 95~99.9999重量 %。 马 就提高洗雜之觀點而言,沖洗劑組合物之溫度較佳為 5 0 〜7 0 〇C 〇 就提高洗務性之觀點而言,較佳為於沖洗步驟中亦對沖 洗劑組合物賦予超音波振動。若於沖洗步驟之第3步驟對 沖洗劑組合物施加超音波振動, u &過第2步驟而將存在 於間隙中之空氣自間隙迫出,故 1之上边巧垢與沖洗劑, :物:好地接觸,且由於對進行了溶存氣體之脫氣的沖洗 劑組&物施加超音波振動,故㈣巾所存在之污垢之除去 I5250l.doc -24- 201134562 :生提高。因此’若於沖洗步驟之第3步驟中對 物施加超音波振動,則可期待沖洗時間之縮短化,因此: 佳·。超音波之頻率及超音波之能量密度可與第3步驟^ 予洗淨劑組合物者相同。 [乾燥步驟] 於沖洗步驟之後所進行之乾燥步驟中,例如藉由對 洗劑組合物中取出之被洗淨物吹送溫風,而除去附著於表 面之沖洗劑組合物後’搬送至真空乾燥容器内。真空乾燥 容器内之溫度例如設定成50〜1〇〇t,將真空乾燥容器:減 壓至〇·卜5(kPa)。利用真空乾燥容器所進行之乾燥進行例 如1〜30分鐘即可。 再者’就提高生產性之觀點而言,本發明之洗淨方法使 用包含-個以上可調整愿力之洗淨槽、兩個以上可調整麼 t洗槽及真空乾燥容器的設備進行以依序連續進 行洗淨步驟、例如包括預沖洗步驟與完工沖洗步驟之沖洗 步驟、乾燥步驟。上述設備之—例例如揭示於日本專利特 開平6-296940號公報中。 [洗淨劑組合物] 其次,對本發明之洗淨方法用之洗淨劑組合物進行說 明。 本發明之洗淨劑組合物含有水(成分A)、特定乙二醇醚 (成分B)、及特定胺化合物(成分c)。 (成分A) 成刀A含有热餾水、離子交換水、或超純水等水。The content of water in the rinsing agent composition is preferably from 90 to 99.9999 by weight, more preferably from 92 to 99.9999% by weight, from the viewpoint of improving the residual flux residue or the flux of the re-adhesive flux. It is preferably 95 to 99.999% by weight. The rinsing agent composition preferably has a temperature of from 50 to 70 〇C 观点 from the viewpoint of improving the washing, and is preferably a rinsing agent in the rinsing step from the viewpoint of improving the washing property. Give ultrasonic vibration. If ultrasonic vibration is applied to the rinsing agent composition in the third step of the rinsing step, u & after the second step, the air existing in the gap is forced out of the gap, so that the upper side is finely smeared with the rinsing agent, : Good contact, and due to the ultrasonic vibration applied to the rinsing agent group & the degassing of the dissolved gas, the dirt of the (4) towel is removed. I5250l.doc -24- 201134562: Health is improved. Therefore, if ultrasonic vibration is applied to the object in the third step of the rinsing step, the rinsing time can be expected to be shortened. Therefore, it is preferable. The frequency of the ultrasonic waves and the energy density of the ultrasonic waves can be the same as those in the third step of the detergent composition. [Drying step] In the drying step performed after the rinsing step, for example, by blowing warm air to the washed material taken out of the lotion composition, the rinsing composition attached to the surface is removed, and then transferred to vacuum drying. Inside the container. The temperature in the vacuum drying vessel is set, for example, to 50 to 1 Torr, and the vacuum drying vessel is depressurized to 〇·b 5 (kPa). The drying by vacuum drying of the container can be carried out, for example, for 1 to 30 minutes. Furthermore, from the viewpoint of improving productivity, the cleaning method of the present invention uses a device including more than one cleaning tank capable of adjusting the wish force, two or more adjustable t-wash tanks, and a vacuum drying container. The washing step is continuously performed, for example, a rinsing step including a pre-rinsing step and a finishing rinsing step, and a drying step. An example of the above-mentioned apparatus is disclosed in Japanese Laid-Open Patent Publication No. Hei 6-296940. [Detergent composition] Next, the detergent composition for the cleaning method of the present invention will be described. The detergent composition of the present invention contains water (ingredient A), a specific glycol ether (ingredient B), and a specific amine compound (ingredient c). (Component A) The forming blade A contains water such as hot distilled water, ion exchanged water, or ultrapure water.

S 152501.doc •25- 201134562 就確保對於助焊劑殘渣之高洗淨性之觀點而言,洗淨劑 組合物中之水含量必須為2重量%以上1〇重量%以下就相 同之觀點而言,較佳為3~8重量%,進而較佳為4〜7重量 %。本發明之一個特徵在於:於進行減壓、減壓狀態之保 持、及升壓之洗淨方法中,較佳為反覆進行減壓、減壓狀 態之保持、及升壓之洗淨方法中所使用的洗淨劑組合物中 之水含量為2重量❹/。以上1〇量%以下之特定範圍。本發明 中’可藉由因減壓及升壓之壓力變化而產生之物理力與因 減壓保持步驟中之洗淨劑組合物之沸騰而產生之物理力, 而戲劇性地除去先前難以除去之較窄間隙的助焊劑殘渣。 著眼於因洗淨劑組合物之沸騰而產生之物理力而決定洗淨 劑組合物中之水含量◊若水含量未達2重量%則沸騰之物 理力不足,若超過1 〇重量%,則助焊劑殘渣之溶解性較 差’因此無論那種情況均無法獲得充分之洗淨性。 (成分B) 成分B含有下述通式(1)所示之乙二醇醚。S 152501.doc •25- 201134562 The water content in the detergent composition must be 2% by weight or more and 1% by weight or less from the viewpoint of ensuring high detergency of the flux residue. It is preferably from 3 to 8% by weight, and more preferably from 4 to 7% by weight. One of the features of the present invention is that in the method of performing the pressure reduction, the pressure reduction state, and the pressure increase, it is preferable to carry out the method of repeatedly performing the pressure reduction, the pressure reduction state, and the pressure increase cleaning method. The water content of the detergent composition used was 2% by weight. The above range is less than or equal to the specific range of %. In the present invention, the physical force generated by the pressure change due to the pressure reduction and the pressure increase and the physical force generated by the boiling of the detergent composition in the pressure reduction holding step can be dramatically removed. A narrower gap of flux residue. Focusing on the physical strength of the detergent composition due to the physical force generated by the boiling of the detergent composition, if the water content is less than 2% by weight, the physical strength of boiling is insufficient, and if it exceeds 1% by weight, it is helpful. The flux residue has poor solubility. Therefore, sufficient detergency cannot be obtained in either case. (Component B) Component B contains a glycol ether represented by the following formula (1).

Ri-CKEO^R2 (1) 其中’於上述通式(1)中’ R1為碳數1〜6之烷基,R2為氮 原子或碳數1〜3之烷基’ EO為氧伸乙基,m表示EO之平均 加成莫耳數,滿足2SmS3。 就確保對於助焊劑殘渣之高洗淨性與高安全性之觀點而 言’ R1之碳數較佳為2〜4 ’更佳為3〜4。 作為上述通式(1)所示成分B之具體例,就提高助焊劑殘 渣對於洗淨劑組合物之溶解性之觀點而言,較佳為e〇2 152501.doc -26· 201134562 平均加成莫耳數m為2之單烷基型乙二醇醚、£〇之平均加 成莫耳數m為3之單烷基型乙二醇醚、E〇之平均加成莫耳 數m為2之二烷基型乙二醇醚、E〇之平均加成莫耳數爪為] 之二烧基型乙二醇醚等。該等乙二醇醚可僅使用1種亦可 併用2種以上。 作為之平均加成莫耳數m為2之單院基型乙二醇趟, 可歹丨舉.一乙—醇單甲鱗、二乙二醇單乙喊、二乙二醇單 異丙鱗、二乙二醇單丁醚、二乙二醇單異丁謎、二乙二醇 單己峻等。 4為EO之平均加成莫耳數爪為3之單烷基型乙二醇醚, 可列舉.S乙二醇單甲縫、三乙二醇單乙_、三乙二醇單 異丙醚、三乙二醇單丁醚等。 作為EO之平均加成莫耳數瓜為2之二烷基型乙二醇醚, 可列舉.—乙二醇二甲醚、二乙二醇甲基乙醚、二乙二醇 甲土丙醚—乙—醇二乙醚、二乙二醇甲基丁醚、二乙二 醇丁基甲醚、^乙二醇甲基異丁醚等。 作為EO之平均加成莫耳數_ 3之二燒基型乙二醇謎, 可列舉:三乙二醇二甲醚等。 該等乙二醇謎之中,就提高安全性,呈現高水溶性,及 提高二焊劑殘渣之溶解性之觀點而言,較佳為選自由二乙 一醇平曱鱗、二乙二睦留 抑 一私早乙醚、二乙二醇單丁醚、二乙二 醇早異丁醚、〔乙二醇單己驗、三乙二醇單甲醚、三乙二 醇單乙⑽、三乙二醇單異丙醚、三乙二醇單丁_、二乙二 醇丁基甲謎、—乙二醇甲基異丁趟、及三乙二醇二甲驗所 組成之群中之至少1種。 152501.doc -27- 201134562 就提高對於較窄間隙中所殘留之助焊劑殘渣之洗淨性之 觀點而言,洗淨劑組合物中之成分B的含量必須為5〇重量 %以上未達97·75重量%’就相同之觀點而言,較佳為的以 上未達97.75重量% ’更佳為8〇〜97.25重量〇/〇。 (成分C) 成分C含有下述通式(2)所示胺化合物。 [化2] R3 —Ν—(ΕΟ)ρ —Η (E〇)q-H (2) 上述通式⑺中’以示氫原子或碳數卜4之烧基,E〇表 不氧伸乙基,p、#別表示Ε〇之平均加成莫耳數,滿足 1 Sp+q各 4。 就提高對於㈣中所殘留之助焊_渣之洗淨性及洗條 性之觀點而言,R3之碳數較佳為1〜3。心為滿足如⑼ 者,就提高對於間隙中所殘留之助焊劑殘渣之洗淨性之觀 點而言’更佳為滿足l$p+q$3。 作為上述通式⑺所示成分C之具體例,就提高洗務性及 提南對於間隙中所殘留之助焊劑殘清之洗淨性之觀點而 言’較佳為單乙醇胺、r乙醇胺、曱基二乙醇胺、甲基單 乙醇胺、乙基單乙醇胺等烷基醇胺類。 就提高洗祕及提高對於_:中所殘留之助焊劑殘邊之 洗淨性之觀點而言’洗淨劑組合物中之成分c之含量必須 為〇.〇5重量%以上5重量%以下,較佳為0.5M.5重量%。 就提高對於間隙中所殘留之助焊劑殘渣之洗淨性之觀點 152501.doc -28 · 201134562 而言,成分B與成分C之重量比(成分b/成分〇較 20〜",更佳為94〜98,進而較佳為95〜97。 ' 就提高對於間隙中所殘留之助焊劑殘渣之洗淨性之觀點 而言’成分B與成分A之重量比(成分b/成分A) 20〜",更佳為20〜50,進而較佳為30〜50。 . 就提高對於間隙中所殘留之助谭劑殘渣之洗淨性之觀點 而言,成分B之重量與成分A和成分c之總計重量的重量比 {成分Μ成分A+成分C]}較佳為1〇〜5(),更佳為15〜35 ,進 而較佳為23〜33。 洗淨劑組合物亦可含有下述界面活性劑(成分D)。 ,抑制起泡性之觀點而言,洗淨劑組合物中之成分D之 含讀佳為未達0.01重量%,就相同之觀點而言,較佳為 0.005重量。/。以下,更佳為膏 I佳為T質不含有成分D,X更佳為不 含有成分D。 作為成分D之具體例,可列舉:聚氧乙稀烧基驗、聚氧 :烯聚氧峨基醚、聚氧乙輪醋、聚氧乙烯聚氧丙 =酸酉旨、聚氧乙稀聚氧丙烯共聚物等非離子性界面活性 [其他任意成分] =劑组合物在無損於使用洗淨劑組合物而洗淨被洗淨 劑殘渣之高洗淨性、良好之中所存在之助焊 mκ之洗滌性、及低起泡性之範 作為成分c以外之胺化人物令 物’亦可含有味你、乙基 末琳專味妹類:㈣、三乙基二胺、五甲基二乙三胺、四 152501 .doc •29- 201134562 甲基丙二胺等。 作為洗淨劑組合物中之另外的其他成分,亦可視需要含 有通常洗淨劑組合物中所使用之選自由螯合劑、防腐劑、 防銹劑、殺菌劑、抗菌劑、抗氧化劑、酯、及甘油或聚乙 一醇專醇類專所組成之群中的至少一種。 就提高對於間隙中所殘留之助焊劑殘渣之洗淨性之觀點 而言,洗淨劑組合物中之上述其他任意成分之總計含量較 佳為45重量%以下,更佳為2()重量%以下,進而較佳為〇」 重量°/〇以下,進而更佳為0 〇5重量。以下。 [洗淨劑組合物之製備方法] 洗淨劑組合物之製備方法並無任何限制,可藉由將成分 A、成分B、及成分C加以混合,視需要進而混合成分d及/ 或其他任意成分而製備。 。。再者,作為用以混合各成分之容器,可使用sus製容 杰、GS(玻璃襯裏)製容器作為溶液授拌機構,可使用 螺旋紫葉片、折葉槳(pitched paddle)、等撥掉翼 或磁力攪拌器等。 攪拌中之混合液之溫度較佳為1〇〜4〇t:,更佳為 Μ〜3〇°C。上述攪拌翼之週速通常較佳為卜3…秒。又, 較佳為將所有成分加人容器中後,將混合液混㈣分鐘以 上’更佳為混合20分鐘以上。 [洗淨劑組合物之pH值] 洗淨劑組合物之pH值根據被洗淨物之種類或洗淨後之被 洗淨物的要求品質等而適當決定即可,就抑制被洗淨物之Ri-CKEO^R2 (1) wherein 'in the above formula (1), 'R1 is an alkyl group having 1 to 6 carbon atoms, and R2 is a nitrogen atom or an alkyl group having 1 to 3 carbon atoms. EO is an oxygen-extended ethyl group. , m represents the average addition mole of EO, which satisfies 2SmS3. From the viewpoint of ensuring high detergency and high safety of the flux residue, the carbon number of R1 is preferably 2 to 4', more preferably 3 to 4. As a specific example of the component B represented by the above formula (1), from the viewpoint of improving the solubility of the flux residue to the detergent composition, it is preferably e〇2 152501.doc -26· 201134562 average addition. The monoalkyl type glycol ether having a molar number m of 2, the average addition molar number m of the monoalkyl type glycol ether of 3, and the average addition molar number of the E m m is 2 The dialkyl type glycol ether and the average addition molar number of the E 〇 are the dialkyl type glycol ethers. These glycol ethers may be used alone or in combination of two or more. As a single-added base type ethylene glycol oxime with an average addition molar number m of 2, it can be used. One-ethyl alcohol monomethyl scale, diethylene glycol single-ethyl shunt, diethylene glycol single isopropyl scale , diethylene glycol monobutyl ether, diethylene glycol monoisobutyl mystery, diethylene glycol single self and so on. 4 is an average addition of EO, and the monoalkyl type glycol ether having a molar number of 3 is exemplified by .S ethylene glycol monomethyl sequestration, triethylene glycol monoethyl _, triethylene glycol monoisopropyl ether. , triethylene glycol monobutyl ether and the like. As the average addition molar amount of EO, the melon number is a dialkyl glycol ether of 2, which may be exemplified by - ethylene glycol dimethyl ether, diethylene glycol methyl ether, diethylene glycol methyl propyl ether. Ethyl alcohol diethyl ether, diethylene glycol methyl butyl ether, diethylene glycol butyl methyl ether, ethylene glycol methyl isobutyl ether and the like. As the average addition molar amount of EO _ 3 bis-based ethylene glycol mystery, triethylene glycol dimethyl ether or the like can be mentioned. Among these ethylene glycol mysteries, from the viewpoint of improving safety, exhibiting high water solubility, and improving the solubility of the residue of the second flux, it is preferably selected from the group consisting of diacetyl alcohol squama and diterpene retention. A private early ether, diethylene glycol monobutyl ether, diethylene glycol early isobutyl ether, [ethylene glycol single test, triethylene glycol monomethyl ether, triethylene glycol monoethyl (10), triethylene glycol At least one of a group consisting of monoisopropyl ether, triethylene glycol monobutylene, diethylene glycol butyl mystery, ethylene glycol methyl isobutyl hydrazine, and triethylene glycol dimethyl test. 152501.doc -27- 201134562 From the viewpoint of improving the detergency of the flux residue remaining in the narrow gap, the content of the component B in the detergent composition must be 5% by weight or more and less than 97%. From the viewpoint of the same, from the viewpoint of the same, it is preferably less than 97.75% by weight 'more preferably 8 〇 to 97.25 〇/〇. (Component C) Component C contains an amine compound represented by the following formula (2). R3 —Ν—(ΕΟ)ρ—Η (E〇)qH (2) In the above formula (7), 'is a hydrogen atom or a carbon number of 4, and E is an oxygen-free ethyl group. p, # don't indicate the average addition of the number of moles, satisfying 1 Sp+q each. The carbon number of R3 is preferably from 1 to 3 from the viewpoint of improving the detergency and the washing property of the flux-residue remaining in (4). In order to satisfy the viewpoint of improving the detergency of the flux residue remaining in the gap, the heart satisfies, for example, l$p+q$3. Specific examples of the component C represented by the above formula (7) are preferably monoethanolamine, rethanolamine, and hydrazine from the viewpoint of improving the detergency and the cleaning property of the flux residue remaining in the gap. Alkyl alcohol amines such as diethanolamine, methyl monoethanolamine, and ethyl monoethanolamine. The content of the component c in the detergent composition must be 〇.5% by weight or more and 5% by weight or less from the viewpoint of improving the cleansing property and improving the cleanability of the flux residue remaining in the _: Preferably, it is 0.5 M.5% by weight. From the viewpoint of improving the detergency of the flux residue remaining in the gap 152501.doc -28 · 201134562, the weight ratio of component B to component C (component b/component 〇 is 20~", more preferably 94 to 98, further preferably 95 to 97. 'The weight ratio of the component B to the component A from the viewpoint of improving the detergency of the flux residue remaining in the gap (component b/component A) 20~ " More preferably, it is 20 to 50, and further preferably 30 to 50. The weight of the component B and the component A and the component c are from the viewpoint of improving the detergency of the residue of the aiding agent remaining in the gap. The weight ratio of the total weight (component A component A + component C]} is preferably from 1 〇 to 5 (), more preferably from 15 to 35, still more preferably from 23 to 33. The detergent composition may also contain the following The surfactant (component D). The content of the component D in the detergent composition is preferably less than 0.01% by weight from the viewpoint of suppressing foaming property, and is preferably 0.005 by weight from the same viewpoint. In the following, it is more preferable that the paste I is T-free and does not contain the component D, and X is more preferably the component D. The specific example of the component D is as follows: Non-ionic interfacial activity such as polyoxyethylene bromide test, polyoxygen: olefin polyoxyalkyl ether, polyoxyethylene vinegar, polyoxyethylene polyoxypropylene = acid, polyoxyethylene polyoxypropylene copolymer [ Other optional ingredients] The agent composition washes away the detergent residue with high washability without detrimental to the use of the detergent composition, good cleaning of the flux mκ, and low foaming property. Fan as an aminized character of the component c' can also contain the taste of you, Ethyllinium exclusive taste: (4), triethyldiamine, pentamethyldiethylenetriamine, four 152501.doc •29- 201134562 Methyl propylene diamine, etc. As other additional components in the detergent composition, it may optionally be selected from the group consisting of a chelating agent, a preservative, a rust inhibitor, a bactericide, and the like, which are used in a usual detergent composition. At least one of a group consisting of an antibacterial agent, an antioxidant, an ester, and a glycerin or a polyhydric alcohol-specific alcohol. The detergent is improved from the viewpoint of improving the detergency of the flux residue remaining in the gap. The total content of the above other optional components in the composition is preferably 45% by weight. More preferably, it is 2 (% by weight or less), further preferably 〇" by weight / 〇 or less, more preferably 0 〇 5 by weight. Hereinafter. [Preparation method of detergent composition] detergent composition The preparation method is not limited, and may be prepared by mixing the component A, the component B, and the component C, and further mixing the component d and/or any other component as needed. Further, as a component for mixing the components As the container, a container made of SUS, GS (glass lining) can be used as a solution mixing mechanism, and a spiral purple blade, a pitched paddle, a paddle or a magnetic stirrer can be used. The temperature of the mixture in the stirring is preferably 1 Torr to 4 Torr: and more preferably Μ 3 〇 °C. The peripheral speed of the agitating blades described above is usually preferably 3 seconds. Further, it is preferred that after all the components are added to the container, the mixed solution is mixed for (four) minutes or more, more preferably for 20 minutes or more. [pH of the detergent composition] The pH of the detergent composition is appropriately determined depending on the type of the object to be washed or the required quality of the object to be washed after washing, and the object to be washed is suppressed. It

152501.dQC •30· 201134562 腐蝕之觀點而言,較佳為8〜u,更佳為9〜η。 洗淨劑組合物之ΡΗ值可視需要藉由適當調配所需量之硝 酸、硫酸等無機酸,氧羧酸、多元羧酸、胺基聚羧酸、胺 基酸等有機酸,及該等之金屬鹽核鹽、氨、氫氧化納、 氫氧化鉀、胺等驗性物質而調整。 [電子零件之製造方法] 本發明之電子零件之製造方法為包含焊料凸塊之電子零 件之製造方法,且包括:使用焊料助焊劑於電子零件之基 板上形成焊料凸塊之步驟;以及利用本發明之洗淨方法洗 淨源自焊料助焊劑之助焊劑殘渣之步驟。即,本發明之電 子零件之製造方法包括:使用焊料助焊劑將零件焊接於基 板上,繼而進行回流,獲得經由焊料凸塊而於上述基板上 搭載有上述零件之製造中間物(被洗淨物)的步驟;以及利 用本發明之洗淨方法洗淨上述基板與上述零件之間隙中所 存在的源自焊料助焊劑之助焊劑殘渣。焊料凸塊例如可藉 由如下先前公知的使用助焊劑之焊料凸塊之形成方法而形 成:將膏狀焊料助焊劑印刷塗佈於基板上,隨後進行加熱 (回流)而形成焊料凸塊之印刷法;或對基板上所形成之阻 焊劑層的開口部進行焊料電鑛,隨後進行加熱(回流)而形 成焊料凸塊之電鍍法;向形成於基板上之阻焊劑層的開口 部填充膏狀焊料助焊劑,隨後進行加熱(回流)而形成焊料 凸塊之方法等。 此處,所謂電子零件之「基板」,除了電路基板、封裝 基板(插入式基板)等,亦包含形成有焊料凸塊之半導體^ 152501.doc -31 - 201134562 片等,作為電子零件,可列舉含有上述基板之半導體裝置 等。作為「零件」,可列舉半導m晶片型電容器、 與用作「基板」之電路基板不同的電路基板等。於利用任 -方法形成焊料凸塊時,均可藉由於回流步驟後利用本發 明之洗淨方法洗淨基板等,而高效率地洗淨上述基板與上 述零件之間的空間(間隙)之助焊劑殘渣。若採用本發明之 洗淨方法,則亦可容易地除去例如高度(基板與零件之上 下方向之最短距释)5〜5〇〇 μιη、寬度13〇〜2〇〇〇〇 、深度 130〜25000 μπΐ2較窄間隙中所進入之助焊劑殘渣。 實施例 藉由以成為表1、表3、表5、及表6中記載之組成之方式 調配及混合各成分,而獲得實施例丨〜丨了及比較例^。之洗 淨劑組合物。攪拌中之混合液之溫度設為25°C,混合液之 攪拌係使用磁力攪拌器(80 mm轉子)。磁力攪拌器之轉速 设為200 rpm,將所有成分加入容器中後之攪拌時間設為 30分鐘。該等洗淨劑組合物之pH值為1 〇〜11。各洗淨劑組 合物之pH值係使用pH計(東亞電波工業公司製造, 3〇G)測定之25°C下之值。 使用所獲得之洗淨劑組合物,進行下述試驗(1)〜(6)。將 所獲得之洗淨劑組合物填充至洗淨槽(容積:25 L)中,加 溫至6 0 °G。 <助焊劑殘渣之製備> 將膏狀焊料(Tamura化研製造之UFSOLDER LF_204-11) 塗佈於銅板後,對該等於氮氣環境下進行熱處理(25〇。〇, 152501.doc •32- 201134562 製備助焊劑m藉由上述熱處理使f狀焊料中之助 焊劑熔融而自料金屬浮起,分μ料金屬與助焊劑殘 〉查。助㈣㈣於銅板上可以茶褐色膜之類的污垢而觀察 到。 <測試件之製作> processing 上,以其 ’於1對鋁 如圖1Α及圖1Β所示,於市售之Mpu(micr〇 unit,微處理單元)之PKG基板1的其中之一主面 間隔W4為3 mm之方式相互平行地配置】對紹板2 板2上配置蓋玻璃5。蓋玻璃5與]?尺(}基板丨之間的空間之高 度W3為50㈣。使用環氧樹脂化將】對鋁板2固定於ρκ = 板1上,及將蓋玻璃5固定於丨對鋁板2上,形成由PKG基板 1、1對鋁板2、蓋玻璃5圍成之間隙17。 自銅板取下於上述 <助焊劑殘渣之製備>中製備之助焊劑 殘渣,將其0.05 g放置於上述間隙17之其中之一端附近 後,將該等放入15(TC高溫槽内。如此,藉由毛細管現象 而使助焊劑殘渔侵入間隙17内。繼而,藉由環氧樹脂补密 封上述間隙1 7之其_之一端,獲得測試件。再者,藉由毛 細管現象而使填充至區域4内之助焊劑殘渣的長度方向之 長度為5 mm,藉由助焊劑殘渣而覆蓋包圍區域4之整個 面。於圖1A中,W丨及W2之長度均為5 mm,構件編號6係 指空氣積存而形成之積存空氣。由PKG基板1、1對銘板 2、蓋玻璃5、及環氧樹脂3b包圍之空間(間隙} 7)的高度為 50 μιη,寬度為3 mm,深度為1〇 mm。 (1)間隙洗淨性試驗1 152501.doc •33- 201134562 其人將測"式件设置於夾具上後,積存空氣6以較區域4 位於更下方之方式浸潰於洗淨槽(容積:25 l)内之洗淨劑 組合物(6(TC ’ 5 。繼而,經過使洗淨槽内之愿力例如 以19 kPa/s(實施例丨之情形)之速度減壓達到表工、表3、表 5及表6所不壓力Pi為止之減壓步驟後,將該經減壓之壓 力保持表1、表3、表5、友表6所示時間(參照「減壓保持 時間」),繼而,將洗淨槽内之壓力例如以19 kPa/s(實施 例1之情形)之速度升壓直至達到表丨、表3、表5、及表6所 示壓力p2。於壓力1>2與常壓⑽3(kPa))相等之情形時,其 後,將洗淨槽内之壓力以表i、表3、表5、及表6中記載之 時間(參照「升壓後壓力保持時間」)保持在常壓。於壓力 P2低於常壓之情形時,將該洗淨槽内之壓力保持μ、表 3、表5、及表6中記載之時間(參照「升壓後壓力保持時 間」)。包括減壓步驟、減壓保持步驟、升壓步驟、及升 壓後壓力保持步驟之一系列步驟進行表丨、表3、表5、及 表6中記載之次數(參照「循環數」)。然而,比較例】中未 進行減壓或升壓。又,實施例16〜17、比較例2、2〇〜23中 未進行升壓後壓力保持步驟。比較例13中未進行減壓保持 步驟及升壓後壓力保持步驟。 減壓速度及升壓速度分別係藉由各步驟中之初始壓力斑 下-步驟中之初始麼力(特定壓力)的壓力差除以成為該特 定壓力所需之時間而求出。例如,於實施例i中自常壓 (101.3 kPa)以5秒減壓至40 kPa,因此減壓速度為 kPa/s(= (1〇ΐ·3-4·0)/5)。 I5250I.doc -34. 201134562 減歷保持步驟、升壓步驟 减壓步驟 持步驟中之洗淨槽内之壓力係利用測壓計(柴田科學公司 製造之DM-10S)而測定。於各步驟中連續地監視洗淨槽内 之壓力。又,進行減壓保持步驟、升壓後壓力保持步驟之 實施例及比較例之任一者中,減壓保持步驟中之洗淨槽内 之壓力均控制在卩1±〇.4(卯勾之範圍内,升壓後壓力保持步 驟t之洗淨槽内之壓力控制在p2±〇 4(kPa)之範圍内。 減塵步驟、減壓保持步驟、升壓步驟、及升壓後壓力保 持步驟中之洗淨槽内之洗淨劑組合物的溫度,及下述沖洗 月J ”且〇物之’篮度係利用附設於洗淨槽中之溫度計而測定。 減壓步驟' 減壓保持步驟、升壓步驟、及升壓後壓力保持 步驟中之洗淨劑組合物之溫度係各步驟中每1秒測量而進 行監視,但任-實施例、及比較财,均控制在洗淨劑組 合物之溫度的平均值士 〇彳152501.dQC • 30· 201134562 From the viewpoint of corrosion, it is preferably 8 to u, more preferably 9 to η. The enthalpy value of the detergent composition may be appropriately adjusted by using a desired amount of an inorganic acid such as nitric acid or sulfuric acid, an organic acid such as an oxycarboxylic acid, a polycarboxylic acid, an amine polycarboxylic acid or an amino acid, and the like. The metal salt is adjusted with a mineral salt such as a salt, ammonia, sodium hydroxide, potassium hydroxide or an amine. [Manufacturing Method of Electronic Component] The manufacturing method of the electronic component of the present invention is a method of manufacturing an electronic component including solder bumps, and includes the steps of: forming a solder bump on a substrate of the electronic component using a solder flux; The cleaning method of the invention cleans the flux residue derived from the solder flux. That is, the method of manufacturing an electronic component according to the present invention includes: soldering a component to a substrate using a solder flux, and then performing reflow to obtain a manufacturing intermediate (washed material) on which the component is mounted on the substrate via a solder bump And the step of cleaning the flux residue derived from the solder flux present in the gap between the substrate and the component by the cleaning method of the present invention. The solder bumps can be formed, for example, by a previously known method of forming a solder bump using a flux: a paste solder flux is printed on a substrate, followed by heating (reflow) to form a solder bump. Or a plating method in which a solder paste is applied to an opening portion of a solder resist layer formed on a substrate, followed by heating (reflow) to form a solder bump; and an opening portion of the solder resist layer formed on the substrate is filled with a paste A solder flux, followed by heating (reflow) to form a solder bump, and the like. Here, the "substrate" of the electronic component includes a semiconductor chip 152501.doc -31 - 201134562 in which a solder bump is formed, in addition to a circuit board, a package substrate (inserted substrate), and the like. A semiconductor device or the like including the above substrate. Examples of the "parts" include a semi-conductive m-chip type capacitor and a circuit board different from the circuit board used as the "substrate". When the solder bump is formed by any of the methods, the space (gap) between the substrate and the component can be efficiently cleaned by washing the substrate or the like by the cleaning method of the present invention after the reflow step. Flux residue. According to the cleaning method of the present invention, for example, the height (the shortest distance between the upper and lower sides of the substrate and the part) can be easily removed, 5 to 5 μm, width 13 〇 2 〇〇〇〇, depth 130 to 25000 Ϊ́πΐ2 flux residue entering in a narrow gap. EXAMPLES Examples were prepared and mixed in such a manner as to have the compositions described in Tables 1, 3, 5, and 6, to obtain Examples and Comparative Examples. The detergent composition. The temperature of the mixture in the stirring was set to 25 ° C, and the stirring of the mixture was carried out using a magnetic stirrer (80 mm rotor). The speed of the magnetic stirrer was set to 200 rpm, and the stirring time after all the ingredients were added to the container was set to 30 minutes. The pH of the detergent compositions is from 1 〇 to 11 . The pH of each of the detergent compositions was measured at 25 ° C using a pH meter (manufactured by Toago Corporation, 3 〇 G). Using the obtained detergent composition, the following tests (1) to (6) were carried out. The obtained detergent composition was filled in a washing tank (volume: 25 L) and heated to 60 °G. <Preparation of Flux Residue> After applying a cream solder (UFSOLDER LF_204-11 manufactured by Tamura Chemical Co., Ltd.) to a copper plate, heat treatment was performed under the nitrogen atmosphere (25 〇. 〇, 152501.doc • 32- 201134562 Preparation of flux m by the above-mentioned heat treatment to melt the flux in the f-shaped solder and float the metal from the material, and to separate the metal and the flux residue. Help (4) (4) Observe the stain on the copper plate such as a brown film. <Production of test piece> Processing, in which one pair of aluminum is shown in Fig. 1A and Fig. 1A, which are commercially available as Mpu (micr〇unit, micro processing unit) PKG substrate 1 A main surface interval W4 is arranged in parallel with each other in a manner of 3 mm. The cover glass 5 is disposed on the plate 2 of the plate 2. The height W3 of the space between the cover glass 5 and the substrate is 50 (four). Oxygenation will be performed by fixing the aluminum plate 2 to the ρκ = plate 1 and fixing the cover glass 5 to the iridium pair aluminum plate 2 to form a gap 17 surrounded by the PKG substrate 1, 1 for the aluminum plate 2 and the cover glass 5. The copper plate is removed from the flux residue prepared in the above <Preparation of flux residue> After placing 0.05 g near one of the ends of the gap 17, the sheet is placed in a 15 (TC high temperature bath. Thus, the flux is invaded into the gap 17 by capillary action. Then, by epoxy resin The test piece is obtained by sealing one of the ends of the gaps 17. The length of the flux residue filled in the region 4 is 5 mm in length by the capillary phenomenon, and is covered by the flux residue. The entire surface of the region 4 is surrounded. In Fig. 1A, the lengths of W丨 and W2 are both 5 mm, and the component number 6 refers to the accumulated air formed by the accumulation of air. The PKG substrate 1, 1 pairs of the nameplate 2, the cover glass 5, And the space surrounded by epoxy resin 3b (gap} 7) has a height of 50 μηη, a width of 3 mm, and a depth of 1〇mm. (1) Gap washability test 1 152501.doc •33- 201134562 After the formula is placed on the jig, the accumulated air 6 is immersed in the detergent composition (6 (TC ' 5 ) in a washing tank (volume: 25 l) in a manner lower than the area 4 (then, TC ' 5 . The speed of the cleaning tank is, for example, at a speed of 19 kPa/s (in the case of the embodiment) After the pressure reaches the decompression step until the pressure Pi of Table 3, Table 3, Table 5 and Table 6, the pressure of the decompression is maintained in Table 1, Table 3, Table 5, and Friends Table 6 (refer to " The pressure is maintained for a time"), and then the pressure in the washing tank is increased, for example, at a rate of 19 kPa/s (in the case of Example 1) until the pressures shown in Table 丨, Table 3, Table 5, and Table 6 are reached. P2. When the pressure 1 > 2 is equal to the normal pressure (10) 3 (kPa), the pressure in the washing tank is thereafter the time shown in Table i, Table 3, Table 5, and Table 6 (refer to " The pressure holding time after boosting is maintained at normal pressure. When the pressure P2 is lower than the normal pressure, the pressure in the cleaning tank is maintained at μ, and the times described in Tables 3, 5, and 6 (refer to "pressure-holding time after pressurization"). The series of steps including the pressure reduction step, the pressure reduction holding step, the pressure increasing step, and the pressure holding step after the pressure increase are performed in the table, Table 3, Table 5, and Table 6 (refer to "cycle number"). However, in the comparative example, no pressure reduction or pressure increase was performed. Further, in Examples 16 to 17, and Comparative Examples 2 and 2A to 23, the post-boost pressure holding step was not performed. In Comparative Example 13, the pressure reduction holding step and the pressure increasing pressure holding step were not performed. The decompression speed and the pressure increase rate are respectively obtained by dividing the pressure difference of the initial force (specific pressure) in the initial pressure spot-step in each step by the time required to become the specific pressure. For example, in Example i, the pressure was reduced from normal pressure (101.3 kPa) to 40 kPa in 5 seconds, so the pressure reduction rate was kPa/s (= (1〇ΐ·3-4·0)/5). I5250I.doc -34. 201134562 Reduction and retention steps, pressure-up steps Pressure-reduction step The pressure in the cleaning tank in the step is measured using a manometer (DM-10S manufactured by Shibata Scientific Co., Ltd.). The pressure in the washing tank was continuously monitored in each step. Further, in any of the examples of the pressure reduction holding step and the pressure maintaining step after pressure increase, the pressure in the washing tank in the pressure reducing holding step is controlled at 卩1±〇.4 (卯Within the range, the pressure in the cleaning tank after the boosting pressure maintaining step t is controlled within the range of p2 ± 〇 4 (kPa). The dust reduction step, the pressure reduction holding step, the pressure increasing step, and the pressure maintaining after the pressure increase The temperature of the detergent composition in the washing tank in the step, and the following rinsing month J" and the basket of the sputum are measured by a thermometer attached to the washing tank. The temperature of the detergent composition in the step, the step of increasing the pressure, and the pressure-retaining step after the step-up is monitored every 1 second in each step of the step, but the examples are controlled in the detergent. The average temperature of the composition

值ο.1 C以内。例如,表1中之實施例J 之洗淨劑組合物的溫度「60t」意指於減壓步驟(第2步 驟)、減壓保持步驟(第3步驟)、升壓步驟(第4步驟)、及升 =力保持步驟(第4a步驟)中,洗淨劑組合物 ::值於任—步驟中均在机。再者,減壓步驟、減㈣ 持乂驟、升壓步驟、及 合物的溫度之控制係利用設置於::::中之洗淨劑" 置,秒監控溫度而控制為::::槽中之溫度控制裝 完進行一次預沖洗步驟、完工沖洗步驟,使 預沖洗步驟、及— 乾燥。洗淨步驟、 及凡工沖洗步驟分別於不同之槽内進行。 152501.doc •35· 201134562 於預沖洗步驟中,除了使用各實施例、比較例中均使用 之洗淨劑組合物的5%稀釋液作為沖洗劑組合物以外,以 與洗淨步驟相同之條件依序進行減壓步驟、減壓保持步 驟、升壓步驟、及升壓後壓力保持步驟。關於循環數,亦 與相對應之洗淨步驟之循環數相同。 除了於完工沖洗步驟中使用水作為沖洗劑組合物以外, 以與相對應之洗淨步驟相同之條件,依序進行減壓步驟、 減壓保持步驟、升壓步驟、及升壓後壓力保持步驟。關於 循環數’亦與相對應之洗淨步驟之循環數相同。 於預沖洗步驟及完工沖洗步驟中,比較例1中均未進行 減壓及升壓。又,中實施例16〜17、比較例2、20〜23中未 進行升壓後壓力保持步驟。比較例丨3中未進行減壓保持步 驟及升壓後壓力保持步驟。 經過洗淨步驟及沖洗步驟之測試件之乾燥係藉由如下方 式進行:藉由對測試件吹送溫風(25。〇,而除去附著於表 面之冲洗劑組合物後,將測試件於設定為80亡之真空乾燥 谷裔内放置5分鐘。真空乾燥容器内之壓力為l.O(kPa)。 於間隙洗淨性試驗〗中,於測試件浸潰於實施例卜13、 16、17之洗淨劑組合物及比較例卜13、2〇〜23之洗淨劑組 。物期間’對洗淨劑组合物繼續施加超音波振動⑽ kHz,1.0 w/cm2)。 (2)間隙洗淨性試驗2 除了施加至洗淨劑組合物之超音波振動之能量密度為 〇.5 W/em2以外,進行與間隙洗淨性試驗1㈣之試驗。再 152501.doc • 36 - 201134562 2 =洗淨性試驗2⑷係針對實施例1〜13之洗淨劑組合 較例1〜丨3之洗淨劑組合物而進行。 (3)間隙洗淨性試驗2(b) 除了洗淨步驟中之循環數為間隙洗淨性試驗2⑷中之循 環數之2倍以外,進行與間隙洗淨性試驗2⑷相同之試驗。 再者’間隙洗淨性試驗2_針對實施例卜此洗淨劑組 合物及比較例卜13之洗淨劑組合物而進行。 、使用光予顯微鏡(倍率5〇倍)觀察分別俯視各間隙洗淨性 式驗則後_之’則试件時所觀察到之區域4中的助谭劑殘潰殘 留之區域的面積。I出該區域4之面積中之除去助焊劑殘 渣的°卩分之面積相對於分別俯視測試件時所觀察到之區域 4的面積之比例作為洗淨率(百分率),以下述判定基準評價 洗淨劑組合物對於助焊劑殘渣之洗淨性。 (4)間隙洗淨性試驗3 除了未對實施例14〜15之洗淨劑組合物及比較例14〜19之 洗淨劑組合物賦予超音波振動以外’以與間隙洗淨性試驗 1相同之方式進行試驗。其中’比較例14中未進行減壓或 升壓。又’實施例14、15、比較例15〜19中未進行升壓後 壓力保持步驟。 (5)間隙洗淨性試驗4(實施例18 :調整洗淨劑組合物中 之水之濃度之情形) 如圖3所示’該試驗使用包含進行洗淨步驟之洗淨槽 Π、進行預沖洗之第i洗滌槽12、及進行完工沖洗步驟之 第2洗滌槽13的洗淨裝置。又,準備20個以上述 <測試件之 152501.doc •37- 201134562 製作 >相同之方法製作的測試件。 將上述測試件20個中之一個設置於夾具上後,以積存空 氣6(參照圖1A)較區域4位於更下方之方式將該測試件浸潰 於洗淨槽11内之洗淨劑組合物(,⑺中。洗淨劑組合物係 使用實施例1之洗淨劑組合物。 以與上述(1)間隙洗淨性試驗丨相同之條件,依序進行減 壓步驟、減壓保持步驟、升壓步驟、及升壓後壓力保持步 驟。即,將洗淨槽内減壓至4 kPa,將該減壓狀態保持1〇 秒鐘,繼而將洗淨槽内之壓力升壓至常壓(1〇1 3以幻後, 將^壓狀態保持1 〇秒鐘。反覆進行丨〇次包括該減壓步驟、 減壓保持步驟、升壓步驟、升壓後壓力保持步驟之一系列 步驟洗淨步驟開始前之洗淨槽内的洗淨劑組合物之量為 以3 0秒進行包括減壓步驟、減壓保持步驟、及升壓 v驟及升壓後壓力保持步驟之丨循環。洗淨時間為秒。 於測試件浸潰於洗淨劑組合物期間,繼續對洗淨劑組合 物施加超音波振動(40 kHz、1.0 W/cm2)。 反覆進行10次包括減壓步驟、減壓保持步驟、升壓步 驟及升壓後壓力保持步驟之一系列步驟後,自洗淨槽中 取出測試件^與上述⑴間隙洗淨性試Μ相同之條件, 、’〜則忒件依序各進行一次預沖洗、完工沖洗經過完工 中先^驟後,使經洗淨之測試件乾燥。預沖洗步驟及完工 先步驟刀別進行300秒。於預沖洗步驟中,使用實施例1 之洗淨劑組合物之5%稀釋液作為沖洗劑組合物,於完工 沖洗步驟中’使用水作為沖洗劑組合物。 152501.doc •38- 201134562 其人在將與上述測試件不同之測 ,淨槽之前,使洗—組 之洗淨劑組合物循環,將洗淨槽u内之洗淨劑“:内 水含量調整為與初始值相等之濃度(5.0重量%)。…中之 洗淨槽u内之洗淨劑組合物之水含f及副槽14内之 ’組合物中之水含量係同時使用電容型水分計(機 工她刪恤公司製造,EM⑽邮、16而測定。預= 步驟、完工沖洗步驟係於每次一片測試件沖洗έ士…先 別換成未使用之沖洗劑組合物而進行。以相同方式進二 驗直至第2〇片測試件。對各測試件之洗淨的:; -•人,對總计20片測試件之總循環數為2〇〇次。 整、dr二作為參考例’除了於上述洗淨性試驗中未調 續組合物中之水含量以外,以與實施例18相同之方 =對20片測拭件進行相同之洗淨性試驗。該洗淨性試驗之 、.、〇果不於表7。 如表7可知,若洗淨劑組合物中之水含量為2〜ι〇 %,則獲得高洗淨性…於反覆使用洗淨劑組合物之情 形時,補充隨著使用而蒸發之水分m淨劑組合物中 之水的含量維持在2〜1G重量%,則亦可維持高洗淨性。 (6)洗淨性之評價 <助焊劑殘渣之洗淨性之判定基準> A :洗淨率為9〇%以上 B :洗淨率為80%以上未達90% C:洗淨率為70%以上未達80% 152501.doc -39- 201134562 D :洗淨率為60%以上未達70 % E:洗淨率為50%以上未達60% F :洗淨率未達50% (7)洗滌性試驗 於洗滌性試驗中,對利用水能夠多大程度地洗滌上述測 試件中之1對玻璃板間之間隙17中所進入之洗淨劑組合物 進行測試。其中,關於該試驗中所使用之測試件,上述間 隙17中並未填充助焊劑殘渣。 準備上述間隙1 7由水溶性染料亞甲基藍(試劑;Sigma_ Aldrich公司製造)而著色之洗淨劑組合物填滿之試件。以^ 對玻璃板中之長度方向兩端部中之遠離環氧樹脂儿的端部 側位於下方之方式將測試件設置於夾具上後,以該姿勢將 測試件浸潰於沖洗劑組合物(水,6〇。〇中。於水洗滌性試 驗中’將洗淨劑組合物換成水,以與間隙洗淨試驗卜戈3中 之洗淨步驟(第1〜第5步驟)相同之條件進行洗滌。 使用光學顯微鏡(倍率50倍)觀察分別俯視洗務性試驗名 =測試件之間隙17時所觀察到的染料殘留之區域之面積^ 算出俯視測試件之間隙17時所觀察到之平面中之除去上由 染料的區域之面積相對於俯視測試件之間隙㈣觀察到^ 平面的面積之比例(百分率)作為洗隸,根據下述基 價洗淨劑組合物之洗滌性。 <洗淨劑組合物之水之洗滌性之判定基準> A :洗滌性為90°/。以上 B :洗滌性為70°/。以上未達9〇〇/0 152501.doc •40- 201134562 C ··洗滌性為50%以上未達70% D :洗滌性未達5〇°/。 (8)超音波真空脈衝洗淨時之起泡性試驗 (a)於圖2所示容器7内放入2升洗淨劑組合物,目視觀察 使谷器7内減壓(5 kPa)時之泡之高度,(b)於圖2所示容器7 内放入2升之利用水稀釋洗淨劑組合物以使洗淨劑組合物 之濃度成為10重量%而獲得之稀釋液(相當於預沖洗步驟用 之沖洗劑組合物),目視觀察使容器7内減壓(5 kPa)時之泡 之向度。 再者,於圖2中,構件編號8係指減壓開放閥,構件編號 1 〇係指進打與真空泵連接之配管的開閉控制之閥,構件編 號9係指排液閥。 <超音波真空脈衝洗淨時之起泡性之判定基準> A :泡高度未達10 cm B.泡鬲度為10 cm以上未達2〇 cm C ·泡高度為20 cm以上 表1表6所示,使用作為洗淨劑組合物之水含量少如 2〜10重量%之特定組成者,減壓步驟中所達到之洗淨槽内 力為0.1〜7 kPa之範圍的pi(kpa),連續8〜16秒鐘將減 壓保持步驟中之洗淨槽内之壓力保持在Pi±G4(kpa),且將 洗淨劑組合物之溫度保持在5〇〜7(TC,升壓步驟中所達到 先淨槽内 < 壓力為5〇〜12〇 kpa之範圍的p2(kpa),以 1〇〜220秒鐘進行減壓步驟至升壓步驟,實施例W7之洗淨 “勿對於寬度較窄之間隙17中所殘留之助焊劑殘渣之 152501.doc 201134562 洗淨性較比較例1 ~23高,且水之洗務性亦較為良好。又, 實施例1〜1 7之洗淨劑組合物中,成分B及成分C以外之界 面活性劑之含量為〇.〇〇8重量%以下,由於實質上不含成八 B及成分C以外之界面活性劑,因此起泡獲得抑制。 刀 152501.doc 42· 20 45 3 鬥I <】 6: ss 2丄 1 〇 〇 I 101.3 1 〇 300 | 10(9) i i 1 1 1 i 1 1 1 1 1 I 卜 jj 1 S I 〇 1 〇 〇 I 300 I 宕 1〇⑼ i 1 1 1 1 1 1 1 1 1 I l 私 1 § i 寸 〇 1 〇 1 300 I 1 10(9) I i 1 1 1 1 1 1 1 i 1 1 I v〇 aJ 1 〇 1 寸 〇 1 1 101.3 〇 300 沄 | ίο⑼ | 1 1 1 1 1 i 1 1 1 I I I 对 I 1 I 寸 〇 I | 101.3 | *Τ) (HI 1 m m S i 1 1 1 1 1 1 1 1 I I I 1 1 1 〇 1 1 101.3 | ! 300 (N 1 12(11) ! I 1 1 1 1 I 1 1 I I l I -Ο 1 I 1 对 I (loi^l ο | 320 | 〇 m ο 00 I I 1 1 1 1 1 1 1 i Ϊ 1 <N I I 寸 1 | 101.3] ο Γ315Π <Ν m 0? GN l 1 1 1 1 1 1 1 1 I Ϊ I 对 uJ m ※ 1 1 I 1 | 101.3 1 ο 1 300 ] in <N 丨 12(11)] I 1 1 1 1 1 1 1 1 1 l i 駟 反覆常壓 與減壓 (有沸騰) 1 1 〇 I | 101.3 I ο 〇 m 10(9) 1 I 1 I t 1 1 1 1 1 1 1 m -£ 反覆常壓 與減壓(無 沸騰) 1 1 〇 m 〇 1 ί 101.3 ο 300 10⑼ 1 1 1 1 • 1 1 1 I I i 1 CN 減壓洗淨 (有沸騰) 1 m 寸 290 m 101.3 1 300 300 300 1 1 1 1 1 1 t 1 1 1 1 I _〇 常壓洗淨 1_ § 1 1 1 1 | 101.3 I 1 300 1 1 1 o 94.0 1 1 1 q 1 1 100.0 as 第2步驟~第43步驟 第2步驟 第3步驟 第4步驟 第4a步驟 所有洗淨步驟 第2步驟~第4步驟 第2步驟~第43步驟 成分A 成分B 成分c 成分D 洗淨方法之概要 洗淨劑組合物之溫度(°c) 達到壓力P丨之時間(sec) 壓力P/kPa) 減壓保持時間(sec) 達到壓力P2之時間(sec) 壓力 P2(kPa) 升壓後壓力保持時間[sec] 洗淨時間(sec) 1 Φ: S 獎 ίΝ 餘! ^ S» 埤拿: 循環數(次)※4 <洗淨劑組合物> 水(離子交換水) 二乙二醇單丁醚 三乙二醇單丁醚 二乙二醇單己醚 三乙二醇二甲醚 曱基二乙醇胺 二乙醇胺 SccCi2-14~〇-(E〇)7H 總計 重量比(成分B/成分C) 重量比(成分B/成分A) + 省— Μ υ >W <r •5适駟-炽「扣」*52--炽「-J W 备^-※ •«蛘筠>4>琀^5!*^蚱4》?:^龙('1茶 •肊羿萆^硃羿柏-^丨」^·^^-※ 琀屯'雎^蝴~蜊*丨耸淑蝴古丨结轵-雄阐皙丨运淑哟喊卩锌筠一-※ 152501.doc •43- 20 45 3 0 u Q u CQ < < 卜 jj Q ω Q < < < 扭 < CD < < < < VD iJ ω lx PJ < < < < DQ < < < < m ίΚ < OQ < < < < u-> u Q U < < < (N < OQ < < < < 寸 £ u Q u < < < %κ < CQ < < < < m i? u Q u CQ < < (N -O ω [JU ω 0Q < < [Xl PL, [X. Q < < 超音波 物理力(40 kHz,1.0 WVcm2) 超音波 物理力(40 kHz,0·5 W/cm2) iTi 〇 N 3 o 逛 w <N 超音波 物理力(40 kHz,1.0 W/cm2) 間隙洗淨性試驗1 間隙洗淨性試驗2(a) 間隙洗淨性試驗2(b) 水洗條性 起泡性(a) 起泡性(b) 152501.doc •44· 201134562The value is less than ο.1 C. For example, the temperature "60t" of the detergent composition of Example J in Table 1 means a pressure reduction step (second step), a pressure reduction holding step (third step), and a pressure increasing step (fourth step). And the liter=force holding step (step 4a), the detergent composition:: value is in the machine-by-step. Furthermore, the control steps of the depressurization step, the subtraction (4) holding step, the step of increasing the pressure, and the temperature of the compound are controlled by using the detergent set in ::::, and the temperature is controlled as follows::: : The temperature control in the tank is completed by performing a pre-flushing step, a finishing rinsing step, a pre-flushing step, and - drying. The washing step and the rinsing step are carried out in different tanks. 152501.doc •35· 201134562 In the pre-rinsing step, the same conditions as the washing step were carried out except that 5% of the detergent composition used in each of the examples and the comparative examples was used as the rinsing composition. The pressure reduction step, the pressure reduction holding step, the pressure increasing step, and the post-boost pressure maintaining step are sequentially performed. Regarding the number of cycles, it is also the same as the number of cycles of the corresponding washing step. The pressure reduction step, the pressure reduction holding step, the pressure increasing step, and the post-boost pressure maintaining step are sequentially performed under the same conditions as the corresponding washing step except that water is used as the rinsing agent composition in the finishing rinsing step. . The number of cycles 'is also the same as the number of cycles of the corresponding washing step. In the pre-rinsing step and the completion rinsing step, no pressure reduction and pressure increase were performed in Comparative Example 1. Further, in the above Examples 16 to 17, and Comparative Examples 2 and 20 to 23, the pressure-retaining pressure holding step was not performed. In Comparative Example 3, the pressure reduction holding step and the pressure after pressure step were not performed. The drying of the test piece after the washing step and the rinsing step is performed by blowing a warm air (25 〇 to the test piece and removing the rinsing agent composition attached to the surface, and setting the test piece to 80 dead vacuum dry grain placed in the grain for 5 minutes. The pressure in the vacuum drying container is lO (kPa). In the gap washability test, the test piece is dipped in the cleaning of the examples, 13, 16, and 17. The composition of the agent and the detergent group of Comparative Example 13, 2〇~23. During the period of the article, 'ultrasonic vibration (10) kHz, 1.0 w/cm 2 was continuously applied to the detergent composition. (2) Gap Detergency Test 2 The test was carried out in the same manner as the gap detergency test 1 (4) except that the energy density of the ultrasonic vibration applied to the detergent composition was 〇.5 W/cm2. Further, 152501.doc • 36 - 201134562 2 = detergency test 2 (4) was carried out for the detergent compositions of Examples 1 to 13 as compared with the detergent compositions of Examples 1 to 3. (3) Gap Detergency Test 2 (b) The same test as the gap detergency test 2 (4) was carried out except that the number of cycles in the washing step was twice the number of cycles in the gap detergency test 2 (4). Further, the "gap detergent test 2" was carried out for the detergent compositions of Comparative Examples and Comparative Examples. Using a light microscope (magnification: 5 times), the area of the area where the helper agent was left in the area 4 observed in the sample after the test piece was examined in a plan view. I take the ratio of the area of the flux-removing residue in the area of the region 4 to the area of the region 4 observed when the test piece is viewed from above, as the washing rate (percentage), and evaluate the washing with the following criteria. The detergency of the detergent composition for the flux residue. (4) Gap Washability Test 3 The same as the gap cleansing test 1 except that the ultrasonic wave vibration was not applied to the detergent compositions of Examples 14 to 15 and the detergent compositions of Comparative Examples 14 to 19. The way to conduct the test. In the comparative example 14, no pressure reduction or pressure increase was performed. Further, in Examples 14 and 15, and Comparative Examples 15 to 19, the pressure-retaining step was not performed. (5) Gap Detergency Test 4 (Example 18: Adjustment of the concentration of water in the detergent composition) As shown in Fig. 3, the test uses a washing tank containing a washing step to carry out the pretreatment. The i-th washing tank 12 for rinsing and the washing device for the second washing tank 13 for performing the finishing rinsing step. Further, 20 test pieces prepared in the same manner as the above <test piece 152501.doc •37-201134562 > After the one of the test pieces 20 is placed on the jig, the test piece is immersed in the detergent tank 11 so that the accumulated air 6 (refer to FIG. 1A) is located below the area 4 (7) In the detergent composition, the detergent composition of Example 1 was used. The pressure reduction step and the pressure reduction retention step were sequentially performed under the same conditions as in the above (1) gap cleaning property test. The step of boosting and the step of maintaining the pressure after boosting, that is, reducing the pressure in the washing tank to 4 kPa, maintaining the reduced pressure state for 1 second, and then boosting the pressure in the washing tank to normal pressure ( After 1 〇 1 3 is illusory, the pressure state is maintained for 1 〇 seconds. Repeatedly, the pressure reduction step, the pressure reduction holding step, the pressure increasing step, and the pressure maintaining step after pressure step are washed. The amount of the detergent composition in the washing tank before the start of the step is a cycle of performing the pressure reduction step, the pressure reduction holding step, and the pressure increasing step and the pressure increasing step after the pressure increase in 30 seconds. The time is in seconds. Continue to the detergent combination during the impregnation of the test piece with the detergent composition. Ultrasonic vibration (40 kHz, 1.0 W/cm2) is applied to the device. After repeated steps of 10 steps including decompression step, depressurization holding step, step-up step and post-boost pressure holding step, self-cleaning tank The test piece is taken out and the same condition as the above (1) gap cleaning test, and '~ the piece is pre-rinsed in sequence, and the finished rinsing is completed after the completion, and the washed test piece is dried. The pre-rinsing step and the finishing step are performed for 300 seconds. In the pre-rinsing step, a 5% dilution of the detergent composition of Example 1 is used as a rinsing composition, and water is used as a rinsing step in the finishing rinsing step. Agent composition. 152501.doc •38- 201134562 The person will circulate the wash-group detergent composition before the net test, which will be different from the test piece above, and clean the detergent in the tank. The internal water content is adjusted to a concentration equal to the initial value (5.0% by weight). The water content of the detergent composition in the cleaning tank u is f and the water content in the composition in the sub tank 14 is At the same time, a capacitive moisture meter is used (the mechanic is made by her company). , EM (10) mail, 16 and measured. Pre-step, finishing rinsing step is to wash the gentleman each time a piece of test piece... do not change to the unused rinsing agent composition. In the same way, enter the second test until the second 〇 Piece test piece. For the cleaning of each test piece: - - person, the total number of cycles for a total of 20 test pieces is 2 times. The whole, dr two as a reference example 'except for the above-mentioned detergency test In the same manner as in Example 18 except for the water content in the unregulated composition, the same detergency test was carried out on 20 test pieces. The results of the detergency test were not shown in Table 7. As can be seen from Table 7, if the water content in the detergent composition is 2 to 〇%, high detergency is obtained. When the detergent composition is used repeatedly, the water evaporated by use is replenished. When the content of water in the m-cleaning composition is maintained at 2 to 1 G% by weight, high detergency can be maintained. (6) Evaluation of detergency <Criteria for determination of detergency of flux residue> A: Washing rate is 9〇% or more B: Washing rate is 80% or more and less than 90% C: Washing rate 70% or more is less than 80% 152501.doc -39- 201134562 D : Washing rate is 60% or more and less than 70% E: Washing rate is 50% or more and less than 60% F: Washing rate is less than 50% (7) Washability test In the washability test, the detergent composition which was entered in the gap 17 between the glass sheets in the test piece by the water can be washed to a large extent. Among them, regarding the test piece used in the test, the flux residue was not filled in the gap 17. A test piece in which the above-mentioned gap 17 was filled with a water-soluble dye methylene blue (reagent; Sigma Aldrich) and the colored detergent composition was prepared. After the test piece is placed on the jig in such a manner that the end side away from the epoxy resin in the longitudinal direction of the glass plate is located below, the test piece is immersed in the rinsing composition in this posture ( Water, 6 〇. 〇中. In the water washing test, 'replace the detergent composition with water, in the same conditions as the washing step (1st to 5th steps) in the gap washing test Bugo 3 The area of the dye residue observed when the washability test name = the gap 17 of the test piece was observed by an optical microscope (magnification: 50 times) ^ The plane observed when the gap 17 of the test piece was viewed from above was calculated. The ratio (percentage) of the area of the area of the dye-removed area relative to the gap (4) of the top view test piece was taken as a wash, according to the washing property of the base detergent composition described below. A criterion for determining the washing property of water of the detergent composition > A: the washing property is 90°/. The above B: the washing property is 70°/. The above is less than 9〇〇/0 152501.doc • 40- 201134562 C · · Washability is 50% or more and less than 70% D: Washability is not up to 5 〇 ° / (8) Foaming test at the time of ultrasonic pulse cleaning (a) 2 liters of the detergent composition was placed in the container 7 shown in Fig. 2, and the inside of the granulator 7 was decompressed visually. (b) the height of the bubble at (5 kPa), (b) 2 liters of the detergent composition diluted with water in the container 7 shown in Fig. 2 to obtain a concentration of the detergent composition of 10% by weight. The diluent (corresponding to the rinsing composition for the pre-rinsing step) was visually observed for the degree of bubble when the inside of the container 7 was depressurized (5 kPa). Further, in Fig. 2, the member number 8 means decompression. Open valve, member No. 1 〇 refers to the valve for opening and closing control of the pipe connected to the vacuum pump, and the component number 9 is the drain valve. <Criteria for determining the foaming property of ultrasonic pulse cleaning; > A : The bubble height is less than 10 cm B. The bubble degree is 10 cm or more and less than 2 cm C. The bubble height is 20 cm or more. Table 6 is shown in Table 1, and the water content used as the detergent composition is as low as 2~ 10% by weight of the specific composition, the internal pressure of the cleaning tank reached in the decompression step is pi (kpa) in the range of 0.1 to 7 kPa, and the pressure is maintained for 8 to 16 seconds in a row. The pressure in the cleaning tank is maintained at Pi±G4 (kpa), and the temperature of the detergent composition is maintained at 5 〇 7 (TC, in the first clean tank reached in the step of pressure < pressure is 5 P2 (kpa) in the range of 〇~12〇kpa, the depressurization step to the step of boosting in 1 〇 to 220 seconds, and the cleaning of the embodiment W7 "Do not leave the flux remaining in the gap 17 having a narrow width Residue 152501.doc 201134562 The detergency was higher than that of Comparative Examples 1 to 23, and the water washability was also good. Further, in the detergent compositions of Examples 1 to 17, the components B and C were not. The content of the surfactant is 8% by weight or less, and since the surfactant other than the component BB and the component C is substantially not contained, foaming is suppressed. Knife 152501.doc 42· 20 45 3 Bucket I <] 6: ss 2丄1 〇〇I 101.3 1 〇300 | 10(9) ii 1 1 1 i 1 1 1 1 1 I 卜jj 1 SI 〇1 〇 〇I 300 I 宕1〇(9) i 1 1 1 1 1 1 1 1 1 I l Private 1 § i inch 〇 1 〇 1 300 I 1 10(9) I i 1 1 1 1 1 1 1 i 1 1 I v HIaJ 1 〇1 inch 〇1 1 101.3 〇300 沄| ίο(9) | 1 1 1 1 1 i 1 1 1 III to I 1 I inch 〇I | 101.3 | *Τ) (HI 1 mm S i 1 1 1 1 1 1 1 1 III 1 1 1 〇1 1 101.3 | ! 300 (N 1 12(11) ! I 1 1 1 1 I 1 1 II l I -Ο 1 I 1 Pair I (loi^l ο | 320 | 〇m ο 00 II 1 1 1 1 1 1 1 i Ϊ 1 <NII inch 1 | 101.3] ο Γ315Π <Ν m 0? GN l 1 1 1 1 1 1 1 1 I Ϊ I to uJ m * 1 1 I 1 101.3 1 ο 1 300 ] in <N 丨12(11)] I 1 1 1 1 1 1 1 1 1 1 li 驷Reverse pressure and decompression (with boiling) 1 1 〇I | 101.3 I ο 〇m 10 (9) 1 I 1 I t 1 1 1 1 1 1 1 m -£ Overpressure and decompression (no boiling) 1 1 〇m 〇1 ί 101.3 ο 300 10(9) 1 1 1 1 • 1 1 1 II i 1 CN Decompression wash (with boiling) 1 m inch 290 m 101.3 1 300 300 300 1 1 1 1 1 1 t 1 1 1 1 I _〇 Normal pressure washing 1_ § 1 1 1 1 | 101.3 I 1 300 1 1 1 o 94.0 1 1 1 q 1 1 100.0 as Step 2 ~Step 43 2nd Step 3rd Step 4th Step 4a Step All Cleaning Steps 2nd Step - 4th Step 2nd Step - 43rd Step Component A Component B Component c Component D Summary of Cleaning Method Detergent Composition temperature (°c) Time to pressure P丨 (sec) Pressure P/kPa) Pressure reduction time (sec) Time to reach pressure P2 (sec) Pressure P2 (kPa) Pressure hold time after boost [sec] ] Washing time (sec) 1 Φ: S Prize Ν Ν !! ^ S» :: Cycle number (times) ※4 <Detergent composition> Water (ion exchange water) Diethylene glycol monobutyl ether Triethylene glycol monobutyl ether Diethylene glycol monohexyl ether Ethylene glycol dimethyl ether decyl diethanolamine diethanolamine SccCi2-14~〇-(E〇)7H Total weight ratio (component B / component C) Weight ratio (component B / component A) + province - Μ υ >W <r •5 驷 驷 炽 炽 炽 * 52 52 52 - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - -肊羿萆^朱羿柏-^丨"^·^^-※ 琀屯'雎^蝶~蜊*丨 淑淑蝶古丨结轵-雄皙丨皙丨皙丨淑哟哟哟卩筠-※ 152501 .doc •43- 20 45 3 0 u Q u CQ << 卜jj Q ω Q <<<< CD <<<<< VD iJ ω lx PJ <<<;< DQ <<<< m ίΚ < OQ <<<<u-> u QU <<<< (N < OQ <<<<寸 £ u Q u <<< %κ < CQ <<<< mi? u Q u CQ << (N -O ω [JU ω 0Q << [Xl PL , [X. 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(u'-g^w'^'-^stifH (°¾)25哲w swim 窟卜詩isuloo 窗h°4-»-r-»0-r(u'-g^w'^'-^stifH (°3⁄4)25哲w swim 卜卜诗isuloo window h°4-»-r-»0-r

菡to蚪»-rtoM菡to蚪»-rtoM

nB--ra^rtoT 5B*tou 砩Β- 0s,n Η 卜(03)-0k.2uu3s ϋφ^/βφ^)^ϊ 锏 (νφ^/ραφ^)^«Η« {υφ 噠+νφ噠】/Ηφ^}玉 一-侧 3OP.I0s(N51 152501.doc -50- 201134562 , 比23 < U U 比22 1 1 1 :比21 < < < 比20 < < < 實17 < < < 實16 < < < 超音波 物理力(40 kHz,1.0 W/cm2) 水洗蘇性 起泡性(a) 起泡性(b) 152501.doc 。ί4邊駟羿艄「駟」<f4«qi If塒「壬」※ 。鵷蛘ww-e-鎵^s«r嫦;t^w Μ湞类(寸※ 。匣巽萆^遽^·^·^^,—」“·!!-^?^※ 餘电埭难V嘞麵趔古Τ餘电哟ΦΓ丨錄-ί农维蜊囑Τ餘私哟囑=ti釋一 (⑸※ .ις,uop.losfNsl •51 · 201134562 [表7]nB--ra^rtoT 5B*tou 砩Β- 0s,n Η 卜(03)-0k.2uu3s ϋφ^/βφ^)^ϊ 锏(νφ^/ραφ^)^«Η« {υφ 哒+νφ哒】 / Η φ ^ } jade one - side 3OP.I0s (N51 152501.doc -50- 201134562, than 23 < UU than 22 1 1 1 : than 21 <<< than 20 <<< 17 <<< Real 16 <<< Ultrasonic physical force (40 kHz, 1.0 W/cm2) Washed Susceptibility (a) Foaming (b) 152501.doc .羿艄 "驷" <f4«qi If埘"壬" ※.鹓蛘ww-e-GaN^s«r嫦;t^w Μ浈 (inch ※.匣巽萆^遽^·^·^ ^,—""·!!-^?^※ 埭 埭 嘞 嘞 嘞 嘞 趔 - - - - - - - - - - - - - - - - - - ί ti ti ti ti ti ti ti ti ti ti ti ti ti ti ti ti ti uop.losfNsl •51 · 201134562 [Table 7]

及表6中之各成分之詳細内容如 [成分B] 二乙二醇單丁醚(日本乳化劑公司製造) 三乙二醇單丁醚(日本乳化劑公司製造) 二乙一醇單己趟(日本乳化劑公司製造) 二乙一醇一甲轉(日本乳化劑公司製造) [成分C] 二乙醇胺(和光純藥工業公司製造) 甲基二乙醇胺(和光純藥工業公司製造) [成分D]And the details of the components in Table 6 are as follows [Component B] Diethylene glycol monobutyl ether (manufactured by Nippon Emulsifier Co., Ltd.) Triethylene glycol monobutyl ether (manufactured by Nippon Emulsifier Co., Ltd.) Diethyl alcohol monohexanide ( Made by Japan Emulsifier Co., Ltd.) Ethyl alcohol-to-one (manufactured by Nippon Emulsifier Co., Ltd.) [Component C] Diethanolamine (manufactured by Wako Pure Chemical Industries, Ltd.) Methyldiethanolamine (manufactured by Wako Pure Chemical Industries, Ltd.) [Ingredient D]

SecCi2_M_〇-(EO)7H(非離子性界面活性劑,日本觸媒公司 製造)SecCi2_M_〇-(EO)7H (nonionic surfactant, manufactured by Nippon Shokubai Co., Ltd.)

SecC12.14-〇_(E〇)7H 為 SecC12-0-(E0)7H 與 SecC14-0-(E0)7H 之混合物。 [任意成分] 甘油(花王公司製造) [其他] 152501.doc -52· 201134562 溶劑石油腦(和光純藥工業公司製造) 界面活性劑10%水溶液:BASF公司之Lutensol XL-70(非離 子界面活性劑之10重量%水溶液) 產業上之可利用性 本發明之洗淨劑組合物可較好地用於較窄間隙中所殘留 之助谭劑殘潰之洗淨。 【圖式簡單說明】 之評價中 圖1A係洗淨劑組合物對於助焊劑殘渣之洗淨性 所使用的測試件之概念平面圖; 圖1B係圖1A所示測試件之概念側視圖; 用之可調整壓 圖2係洗淨劑組合物之起泡性試驗中所使 力的洗淨槽之概略圖;及 圖3係實施例中所使狀洗淨裝置之概念圖 【主要元件符號說明】 1 PKG基板 2 鋁板 3a、3b 環氧樹脂 4 區域 5 蓋玻璃 6 積存空氣 7 容器 8 減壓開放閥 9 排液閥 10 配管開閉控制閥 152501.doc -53- 201134562 11 洗淨槽 12 第1洗滌槽 13 第2洗滌槽 14 副槽 15、16 水分計 17 閥 18 循環管路 152501.doc •54SecC12.14-〇_(E〇)7H is a mixture of SecC12-0-(E0)7H and SecC14-0-(E0)7H. [Independent ingredients] Glycerin (manufactured by Kao Corporation) [Others] 152501.doc -52· 201134562 Solvent petroleum brain (manufactured by Wako Pure Chemical Industries, Ltd.) Surfactant 10% aqueous solution: Lutensol XL-70 from BASF Corporation (nonionic interfacial activity) 10% by weight aqueous solution of the agent) Industrial Applicability The detergent composition of the present invention can be preferably used for washing of the residual agent which remains in a narrow gap. BRIEF DESCRIPTION OF THE DRAWINGS FIG. 1A is a conceptual plan view of a test piece used for the detergent residue of the detergent composition; FIG. 1B is a conceptual side view of the test piece shown in FIG. 1A; A schematic view of the cleaning tank for the force in the foaming test of the pressure-sensitive composition 2; and FIG. 3 is a conceptual diagram of the cleaning device in the embodiment [Description of the main components] 1 PKG substrate 2 Aluminum plate 3a, 3b Epoxy resin 4 Area 5 Cover glass 6 Accumulated air 7 Container 8 Decompression open valve 9 Discharge valve 10 Piping opening and closing control valve 152501.doc -53- 201134562 11 Washing tank 12 1st washing Tank 13 2nd washing tank 14 Sub tank 15, 16 Moisture meter 17 Valve 18 Circulation line 152501.doc •54

Claims (1)

201134562 七、申請專利範圍: 1·:種被洗淨物之洗淨方法’其包括使用洗淨劑組合物洗 淨附著有助·焊劑殘逢之被洗淨物之洗淨步驟; 上述洗淨步驟包括: 將附著有助焊劑殘渣之被洗淨物浸潰於收容於可調整 壓力之洗淨槽内的上述洗淨劑組合物中之浸潰步驟(第丄 步驟); 將上述洗淨槽内之壓力減壓至滿足下述式(丨)之壓力 PKkPa)之減壓步驟(第2步驟); 0.1(kPa)^P,^7(kPa) (1) 連續8〜16秒鐘將上述減壓步驟中經減壓之上述洗淨槽 内之壓力保持在?]±〇.4(1^?&),且將上述洗淨槽内之上述 洗淨劑組合物之溫度保持在5 〇〜70 °C之減壓保持步驟(第3 步驟);以及 經過上述減壓保持步驟後,使上述洗淨槽内之壓力為 滿足下述式(2)之壓力PJkPa)之升壓步驟(第4步驟); 50(kPa)^P2^120(kPa) (2) 以10〜220秒鐘進行上述第2步驟〜第4步驟, 上述洗淨劑組合物含有 2重量%以上1 〇重量%以下之水(成分a), 5〇重量%以上未達97.75重量%之乙二醇醚(成分0),以及 0.05重量%以上5重量%以下之胺化合物(成分c), 上述成分B係由下述通式(1)表示: R'-O^EO)™^2 (1) 152501.doc 201134562 [上述通式(1)中,Rl為碳數1〜6之烷基,R2為氫原子或 碳數1〜3之烷基,E〇為氧伸乙基,爪表示E〇之平均加成 莫耳數’滿足2^m^3], 上述成分C係由下述通式(2)表示: [化1] R3-N-(EO)p-H (ΕΟ), -Η (2) [上述通式(2)中’ r3表示氫原子或碳數1〜4之烷基,ΕΟ 為氧伸乙基,p、q分別表示E〇之平均加成莫耳數,滿足 1 ^ p+q ^ 4] 〇 2. 如明求項1之被洗淨物之洗淨方法,其更包括進而反覆 1〜50次至少上述第2步驟〜上述第4步驟之反覆步驟(第5步 驟), 分別以10〜220秒鐘進行上述第5步驟中反覆進行之上 述第2步驟〜上述第4步驟。 3. 如請求項1或2之被洗淨物之洗淨方法,其更包括升壓後 壓力保持步驟(第4a步驟),該步驟係於上述第4步驟之 後’將上述洗淨槽内之壓力保持在5〇〜12〇 kPa之範圍 内、且等於P2土〇.4(kPa)或高於P2±〇.4(kPa)之壓力8〜16秒 鐘。 4. 如請求項丨至3中任一項之被洗淨物之洗淨方法,其更包 括利用含有90〜99.9999重量%之水之沖洗劑組合物沖洗 上述被洗淨物之沖洗步驟。 5. 如清求項4之被洗淨物之洗淨方法,其中上述沖洗步驟 152501.doc 201134562 2將第5步驟中之第2步驟〜4步驟所使用之上述洗淨劑組 合物替換為上述沖洗劑組合物 而進行。 6·如β求項1至5中任一項之被洗淨物之洗淨方法,其中一 邊對上述洗淨劑組合物施加超音波振動,一邊進行上述 洗淨步驟之上述第3步驟。 7.如請求項5之被洗淨物之洗淨方法,其中一 洗劑組合物施加超音波振動,-邊進行上述沖洗步驟之 第3步驟。 8. -種包含焊料凸塊之電子零件之製造方法,其包括: 使用含有助焊劑之焊料助焊劑於電子零件之基板上 成焊料凸塊之步驟;以及 利用如清求項1至7中任一項之上述被洗淨物之洗淨方 9. 法,洗淨源自上述助焊劑之上述助谭劑殘潰之步驟。 -種洗淨裝置,其係如請求項⑴令任一項之被洗淨物 之洗淨方法中所使用者,且 具備用以使上述洗淨槽内之上述洗淨劑組合物之上 水(成分Α)的含量為2重量%以上1〇重量%以下 制機構。 & 152501.doc201134562 VII. Patent application scope: 1·: A method for cleaning a washed object', which comprises washing a cleaning agent with a cleaning agent and a flux residue by using a detergent composition; The step includes: immersing the object to which the flux residue is attached, the impregnation step in the detergent composition contained in the cleaning tank of the adjustable pressure (step )); The pressure inside is reduced to a pressure reduction step (second step) satisfying the pressure (PKkPa) of the following formula (丨); 0.1 (kPa)^P, ^7 (kPa) (1) for 8 to 16 seconds in succession During the depressurization step, the pressure in the above-mentioned washing tank under reduced pressure is maintained? And 〇.4 (1^?&), and maintaining the temperature of the detergent composition in the above-mentioned cleaning tank at a pressure reduction step of 5 〇 to 70 ° C (step 3); After the pressure reduction holding step, the pressure in the washing tank is a pressure increasing step (fourth step) satisfying the pressure (JJ) of the following formula (2); 50 (kPa)^P2^120 (kPa) (2) The second step to the fourth step are carried out in 10 to 220 seconds, and the detergent composition contains 2% by weight or more and 1% by weight or less of water (ingredient a), and 5% by weight or more and less than 97.75% by weight. A glycol ether (ingredient 0) and an amine compound (component c) of 0.05% by weight or more and 5% by weight or less, and the above component B is represented by the following formula (1): R'-O^EO)TM^ 2 (1) 152501.doc 201134562 [In the above formula (1), R1 is an alkyl group having 1 to 6 carbon atoms, R2 is a hydrogen atom or an alkyl group having 1 to 3 carbon atoms, and E is an oxygen-extended ethyl group. The claws indicate that the average addition molar number of E〇 satisfies 2^m^3], and the above component C is represented by the following general formula (2): [Chemical Formula 1] R3-N-(EO)pH (ΕΟ), -Η (2) [In the above formula (2), 'r3 represents a hydrogen atom or Alkyl groups of 1 to 4, ΕΟ is an oxygen-extended ethyl group, and p and q respectively represent the average addition molar number of E〇, satisfying 1^p+q^4] 〇2. The cleaning method of the net material further comprises the step of repeating at least the second step to the fourth step (the fifth step), and repeating the fifth step in the fifth step, respectively, in 10 to 220 seconds. The second step to the fourth step described above. 3. The method of cleaning the washed matter of claim 1 or 2, further comprising a pressure maintaining step after pressure increase (step 4a), wherein the step is after the fourth step, 'the inside of the cleaning tank is The pressure is maintained in the range of 5 Torr to 12 kPa, and is equal to the pressure of P2 soil. 4 (kPa) or higher than P2 ± 〇. 4 (kPa) for 8 to 16 seconds. 4. The method of cleaning a washed article according to any one of claims 3 to 3, which further comprises the step of rinsing said washed matter with a rinsing composition containing 90 to 99.9999% by weight of water. 5. The method of cleaning the washed matter according to claim 4, wherein the rinsing step 152501.doc 201134562 2 replaces the detergent composition used in the second step to the fourth step of the fifth step with the above The rinse composition is carried out. The method of cleaning the washed matter according to any one of the items 1 to 5, wherein the third step of the washing step is performed while applying ultrasonic vibration to the detergent composition. 7. The method of cleaning a washed article according to claim 5, wherein a detergent composition is subjected to ultrasonic vibration, and the third step of said rinsing step is carried out. 8. A method of manufacturing an electronic component including a solder bump, comprising: a step of forming a solder bump on a substrate of an electronic component using a solder flux containing a flux; and utilizing any of the items 1 to 7 A method of washing the above-mentioned washed matter by a method of washing the above-mentioned flux-removing agent. A cleaning device for use in a method of cleaning a washed article according to any one of claims 1 to 3, further comprising: said water-repellent composition in said cleaning tank; The content of (component Α) is 2% by weight or more and 1% by weight or less. & 152501.doc
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