TW201510214A - 基板的洗淨劑組成物 - Google Patents

基板的洗淨劑組成物 Download PDF

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TW201510214A
TW201510214A TW103118812A TW103118812A TW201510214A TW 201510214 A TW201510214 A TW 201510214A TW 103118812 A TW103118812 A TW 103118812A TW 103118812 A TW103118812 A TW 103118812A TW 201510214 A TW201510214 A TW 201510214A
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detergent composition
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Masaya Ueno
Hideyoshi Yanagisawa
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Shinetsu Chemical Co
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Abstract

本發明之目地在於提供一種使用於被聚矽氧成分污染之水接觸角為100度以上之基板表面的洗淨之基板的洗淨劑組成物。 本發明之解決手段為基板的洗淨劑組成物，係使用於基板表面的洗淨之洗淨劑組成物，其特徵為：含有下述成分而成； (A)第四級銨鹽：0.1~2.0質量% (B)水：0.1~4.0質量% (C)有機溶媒：94.0~99.8質量%。

Description

基板的洗淨劑組成物
本發明係關於基板的洗淨組成物。
近年來，各種基板的微型化或高集積化發展，例如半導體安裝中，藉由進行3次元安裝，實現更加的高密度、大容量化。3次元半導體安裝技術意指使一個半導體芯片薄型化，進而藉由矽貫通電極(TSV；through silicon via)將此一邊做結線一邊做多層層合之半導體製作技術。
為了實現此，需要有藉由反面研削使形成有半導體電路的基板薄型化，進而在背面形成含TSV之電極等的電極形成步驟。
雖然提案有使薄型化之際，藉由在矽、玻璃等支撐基板介由接著劑接合形成有半導體電路的基板，而能夠耐住反面研削步驟、反面電極形成步驟等加工的系統，在該步驟後須要能夠容易地剝離支撐基板，支撐基板剝離後，去除殘餘在形成有半導體電路的基板表面之接著劑後，最後須要進行薄膜半導體基板表面的洗淨。
加工步驟中有成為150℃以上的高溫之情形，接著劑亦被要求耐熱性而使用聚矽氧系接著劑，基板表面洗淨時，在僅溶解接著劑之有機溶劑的洗淨，基板表面的水接觸角變成100度以上，難以充分地去除接著劑，而預測到後續的製造步驟中會發生密封材料之接著不良好等問題。
因而，期望不會腐蝕基板表面，並在短時間能夠充分地去除殘餘接著劑的洗淨劑組成物，無法發現在短時間能夠充分地洗淨藉由聚矽氧成分被污染之基板的表面之洗淨劑組成物(專利文獻1)。
〔先前技術文獻〕 〔專利文獻〕
[專利文獻1]特開2013-010888
本發明係鑑於上述問題所進行者，其目的在於提供使用於例如表面係藉由聚矽氧成分被污染的水接觸角為100度以上之矽半導體基板等基板表面的洗淨之基板的洗淨劑組成物。
為了解決上述課題，本發明提供基板的洗淨 劑組成物，係使用於基板表面的洗淨之洗淨劑組成物，其特徵為其含有下述成分而成；
(A)第四級銨鹽：0.1~2.0質量%
(B)水：0.1~4.0質量%
(C)有機溶媒：94.0~99.8質量%。
藉由用洗淨劑組成物洗淨基板，不會腐蝕基板並能夠高效率地洗淨基板。
又，前述經洗淨基板能夠作為具有100度以上，通常100~120度的水接觸角之矽半導體基板。
此係主要來自殘餘在基板表面的聚矽氧系接著劑組成物，使用X線電子光譜儀進行基板表面的元素分析時，來自聚矽氧接著劑的Si元素係通常對於洗淨前被檢測的全元素100質量%成為10質量%以上，特別是成為20質量%以上的含有率。
另外，在本案使用之矽基板係也能夠使用在薄型基板的加工步驟所用之使用於為了在形成有電路的矽基板進而進行金屬佈線等小型用組件。在通常的厚度之矽基板的支撐體上貼合已形成有高分子接著劑的層合體，利用切削並研磨矽基板背面而能夠進行薄型加工。
並且，使用於薄型加工的接著劑係薄型加工後不須要，所以用有機溶劑洗淨而去除，特別是聚矽氧系接著劑時變成難以去除，會成為在基板上殘留10質量%以上的基板。
如此，若本發明的洗淨劑組成物，則能夠以 短時間充分地洗淨表面為被聚矽氧成分污染的水接觸角係100度以上之矽半導體基板的表面，且也能夠將水接觸角設為未滿100度。具體而言，能夠獲得10~30度，佳為10~20度的接觸角為止使接觸角變小的基板即可。
藉由將接觸角設為未滿100度，而使用於半導體組件材等層合體的情形時，能夠獲得顯著更提高與密封材料的接著力等效果者。
又，前述第四級銨鹽為四烷基氫氧化銨，特別是四乙基氫氧化銨為佳。
如此，第四級銨鹽為第四級銨氫氧化物為佳。
又，前述有機溶媒在分子中含有至少1個以上的羥基之有機溶媒，含碳數1~8的飽和脂肪族醇，碳數2~16的乙二醇，及碳數4~20的乙二醇醚之中至少1種以上。
如此，本發明之基板的洗淨劑組成物，係作為有機溶媒能夠使用如上述者。
如以上說明，藉由使用本發明之基板的洗淨劑組成物進行矽半導體基板等基板的洗淨，以短時間能夠獲得良好清潔性，並不會腐蝕基板，且有以高效率洗淨矽半導體基板的可能性，作為薄型矽半導體基板能夠獲得不會腐蝕之有耐久性的基板，能夠有效地使用於半導體組件 用。
以下詳細地說明關於本發明。
如前述期望有以短時間能夠充分地洗淨矽半導體基板等基板的可能性，並有以高效率良好地洗淨基板的可能性之洗淨劑組成物的開發。
於是，本發明者們為了解決上述課題，進行致力研究的結果，發現若以所規定的比例含有第四級銨鹽、水、有機溶媒的洗淨劑組成物，則不會腐蝕基板並以高效率洗淨基板，而完成本發明。
雖以下詳細地說明關於本發明，但本發明並無限定於該等。
本發明之使用於基板表面的洗淨之洗淨劑組成物係含有下述成分而成：
(A)第四級銨鹽：0.1~2.0質量%
(B)水：0.1~4.0質量%
(C)有機溶媒：94.0~99.8質量%。
〔第四級銨鹽〕
達成本發明目的之第四級銨鹽，能夠列舉第四級銨氫氧化物、第四級銨氯化物等，作為該第四級銨氫氧化物能夠列舉具有碳數1~5的直鏈狀烷基之四烷基銨、具有碳數1~5的烷基及碳數1~5的羥基烷基之氫氧化三烷基羥 基烷基銨等，能夠列舉氫氧化四甲銨(TMAH)、氫氧化四乙銨(TEAH)、氫氧化四丙銨(TPAH)、氫氧化四丁銨(TBAH)、氫氧化三甲基(羥基乙基)銨(俗稱膽鹼)、氫氧化三乙基(羥基乙基)銨等。上述第四級銨鹽之中，就清潔性、清潔液的穩定性等理由而言，四烷基氫氧化銨、特別是四乙基氫氧化銨(TEAH)為佳。
〔有機溶媒〕
能夠達成本發明之目的的有機溶媒，係無特別限定於該等，能夠列舉例如分子中含有至少1個以上的羥基、例如碳數1~8、佳為碳數2~7、更佳為碳數3~6的飽和脂肪族醇類、碳數2~16、佳為碳數3~14、佳為碳數5~12的二醇類、碳數4~20、碳數4~18、碳數4~15的二醇醚類等，能夠單獨1種、或將2種以上混合後使用。作為飽和脂肪族一元醇類，能夠列舉例如甲醇、乙醇、正-丙醇、異丙醇、1-丁醇、2-丁醇、異丁醇、第三-丁醇、1-戊醇、2-戊醇、3-戊醇、2-甲基-1-丁醇、異戊醇、第二-丁醇、第三-戊醇、3-甲基-2-丁醇、新戊醇、1-己醇、2-甲基-1-戊醇、4-甲基-2-戊醇、2-乙基-1-丁醇、1-庚醇、2-庚醇、3-庚醇、1-辛醇、2-辛醇、2-乙基-1-己醇、環己醇、1-甲基環己醇、2-甲基環己醇、3-甲基環己醇、4-甲基環己醇、2-乙基己醇等。作為二醇類，能夠列舉例如乙二醇、丙二醇、丁二醇、己二醇、二乙二醇、二丙二醇、三甲二醇、三乙二醇、四乙二醇、四乙二醇等。作為二醇 醚類，能夠列舉例如乙二醇單甲基醚、乙二醇單乙基醚、乙二醇單正-丙基醚、乙二醇單正-丁基醚、二乙二醇單甲基醚、二乙二醇單乙基醚、二乙二醇單丙基醚、二乙二醇單丁基醚、二乙二醇單己基醚、三乙二醇單甲基醚、三乙二醇單乙基醚、丙二醇單甲基醚、丙二醇單乙基醚、丙二醇單丙基醚、丙二醇單丁基醚、二丙二醇單甲基醚、二丙二醇單乙基醚、三丙二醇單甲基醚、3-甲氧基-3-甲基-1-丁醇等。
其中較佳使用碳數6~12的高級有機溶劑，特別是能夠更佳使用丙二醇單丁基醚。
要獲得本發明之基板的洗淨劑組成物時，並無特別限定，能夠混合洗淨劑組成物的構成成分。混合順序也是任意的，鹼性洗淨劑組成物的構成成分之中，能夠預先調配2成分或3成分以上，接著混合剩餘成分，也能夠一次混合全部成分。
製造本發明的洗淨劑組成物之際，不會發生沉澱產生或液分離等不利的範圍為佳。
具體而言，成分(A)：第四級銨鹽的濃度係相對組成物全量為0.1~2.0質量%，佳為0.2~1.5質量%、更佳為0.3~1.2質量%。成分(A)未滿0.1質量%時，有薄型半導體基板表面的洗淨性變為不充分之虞，超過2.0質量%時，不能夠得到洗淨效果，能夠預期矽半導體基板的腐蝕等。
成分(B)係水濃度為0.1~4.0質量%，佳為 0.1~3.0質量%，更佳為0.5~2.5質量%。成分(B)係未滿0.1質量%時，有薄型半導體基板表面的洗淨性變為不充分之虞，超過4.0質量%時，不能夠得到洗淨效果，能夠預期矽半導體基板的腐蝕等。
成分(C)係分子中具有至少1個以上的羥基之有機溶媒濃度為94.0~99.8質量%，佳為95.5~99.7質量%，更佳為96.3~99.6質量%。成分(C)係未滿94.0質量%時，不能夠溶解少量的接著劑成分而有清潔性不夠的可能性，超過99.8質量%時，不能夠得到效果。
如上述，能夠將各成分濃度成為最適宜的方式調整而製造，又，也能夠任意地添加其他成分。
本發明的洗淨劑組成物係未限定於矽半導體基板，也有能夠洗淨鍺基板、鎵-砷基板、鎵-磷基板、鎵-砷-鋁基板、鍍鋁矽基板、鍍銅矽基板、鍍銀矽基板、鍍金矽基板、鍍鈦矽基板、氮化矽膜形成矽基板、氧化矽膜形成矽基板、聚醯亞胺膜形成矽基板、玻璃基板、石英基板、液晶基板、有機EL基板等的可能性。
在本發明能夠洗淨通常厚度的基板，特別是對於經加工切削處理的薄型基板有效，作為厚度佳為20~100μm、更佳為20~70μm之基板的洗淨有效。
作為洗淨方法，有將殘留有聚矽氧樹脂等有機物的基板浸漬於本發明的洗淨劑組成物或藉由噴霧處理之洗淨的可能性，佳為30秒~30分鐘、更佳為1分鐘~10分鐘左右進行洗淨、水洗、乾燥處理。另外，就視情 況自洗淨劑之分散性的點而言加溫也無妨。
另外，如此所獲得不會腐蝕薄型基板係進而在該基板上進行電鍍、濺鍍處理等，有有效地使用於小型半導體組件的可能性。
〔實施例〕
以下，表示實施例及比較例更具體地說明本發明，但本發明並無特別限定該等。
〔基板的製造〕
使用聚矽氧樹脂壬烷溶液接著劑，在直徑8英寸矽半導體基板(直徑200mm、厚度725μm)上用旋轉塗佈器以10μm的膜厚形成接著層。將8英寸玻璃基板(玻璃晶圓)作為支撐基板，在真空接合裝置內將此支撐基板與具有接著層的矽半導體基板以200℃接合，製作由晶圓、接著層、及支撐基板所成層合體。之後使用研磨機進行矽半導體基板的背面研削。最後基板厚度成為50μm為止的方式進行研磨。接著層合基板之中水平地固定矽半導體基板，剝離支撐基板後，6分鐘浸漬於壬烷，去除接著層後使乾燥，製作洗淨試驗用矽半導體基板。此時，基板表面的水接觸角為108℃，以X線電子光譜儀進行基板表面的元素分析結果，Si含有率為23%。另外，Si含有率為來自矽基板的Si除外。
(實施例1)
在組裝有攪拌裝置、冷卻裝置、溫度計的500ml燒瓶添加TMAH五水和物4g、水1g、1-丁氧基-2-丙醇95g，在室溫下攪拌，使TMAH五水和物溶解，獲得洗淨劑組成物A。
(實施例2)
在組裝有攪拌裝置、冷卻裝置、溫度計的500ml燒瓶添加25% TPAH水溶液4g、1-丁氧基-2-丙醇96g，在室溫下攪拌至均勻為止，獲得洗淨劑組成物B。
(實施例3)
在組裝有攪拌裝置、冷卻裝置、溫度計的500ml燒瓶添加37% TBAH甲醇溶液2.7g、水0.3g、1-丁醇97g，在室溫下攪拌至均勻為止，獲得洗淨劑組成物C。
(實施例4)
在組裝有攪拌裝置、冷卻裝置、溫度計的500ml燒瓶添加35% TEAH水溶液1.5g、1-丁氧基-2-丙醇98.5g，在室溫下攪拌至均勻為止，獲得洗淨劑組成物D。
(實施例5)
在組裝有攪拌裝置、冷卻裝置、溫度計的500ml燒瓶添加35% TEAH水溶液1.5g、水0.5g、1-己醇49g、1-丁 氧基-2-丙醇49g，在室溫下攪拌至均勻為止，獲得洗淨劑組成物E。
(實施例6)
在組裝有攪拌裝置、冷卻裝置、溫度計的500ml燒瓶添加35% TEAH水溶液2.86g、水0.14g、二丙二醇48.5g、1-丁氧基-2-丙醇48.5g，在室溫下攪拌至均勻為止，獲得洗淨劑組成物F。
(實施例7)
在組裝有攪拌裝置、冷卻裝置、溫度計的500ml燒瓶添加35% TEAH水溶液5.71g、水0.09g、甲醇47.15g、1-丙氧基-2-丙醇47.15g、在室溫下攪拌至均勻為止，獲得洗淨劑組成物G。
(比較例1)
在組裝有攪拌裝置、冷卻裝置、溫度計的500ml燒瓶添加35% TEAH水溶液0.14g、水0.86g、1-丁氧基-2-丙醇99g，在室溫下攪拌，獲得洗淨劑組成物H。
(比較例2)
在組裝有攪拌裝置、冷卻裝置、溫度計的500ml燒瓶添加TMAH五水和物6g、水2g、1-丁氧基-2-丙醇92g，在室溫下攪拌，使TMAH五水和物溶解而獲得洗淨劑組 成物I，但水層分離，不能夠獲得良好洗淨劑組成物。
(比較例3)
在組裝有攪拌裝置、冷卻裝置、溫度計的500ml燒瓶添加水3g、1-丙氧基-2-丙醇97g、在室溫下攪拌至均勻為止，獲得洗淨劑組成物J。
(比較例4)
在組裝有攪拌裝置、冷卻裝置、溫度計的500ml燒瓶添加10% TEAH丙二醇溶液5g、1-丁氧基-2-丙醇95g，在室溫下攪拌至均勻為止，獲得洗淨劑組成物K。
(實施例1~7、比較例1~4)
藉由使用洗淨劑組成物A~K浸漬前述矽半導體基板進行6分鐘洗淨。作為洗淨劑組成物的評價進行下述評價。各組成物的組成比及結果表示於表1。
〔外觀〕
以目視確認洗淨劑組成物的外觀。也確認沈澱物的析出或水層分離等不利，不能夠確認到異常時表示為○，確認到異常時表示為×。
〔基板表面清潔性評價〕
使用洗淨劑組成物A~H、J及K將所製造矽半導體基 板進行洗淨。具體而言任意時間浸漬於洗淨液組成物A~H、J及K後，以純水沖洗1分鐘，確認經乾燥之矽半導體基板表面的水接觸角。洗淨前的水接觸角為108°、接觸角變成未滿30°為止所花費的時間未滿6分鐘時表示為◎，6分鐘以上未滿10分鐘時表示為○，10分鐘以上時表示為×。
測定裝置：協和界面科學股份有限公司製接觸角計DM-301
〔基板表面洗淨後水接觸角〕
使用洗淨劑組成物A~H、J及K將所製造矽半導體基板進行洗淨。具體而言6分鐘浸漬於洗淨液組成物A~H、J及K後，以純水沖洗1分鐘，使用上述裝置確認經乾燥之矽半導體基板表面的水接觸角。
〔洗淨後基板表面分析〕
使用洗淨劑組成物A~H、J及K將所製造矽半導體基板進行洗淨。具體而言6分鐘浸漬於洗淨液組成物A~H、J及K後，以純水沖洗1分鐘，使用X線電子光譜儀將經乾燥矽半導體基板表面進行洗淨後之基板表面的元素分析，分析Si含有率。
測定裝置：KRATOS製AXIS-ULTRA DLD
根據表1的結果，滿足本發明之基板的洗淨劑組成物之構成要件的實施例1~實施例7中，能夠以短時間獲得良好清潔性，不會觀察到基板的腐蝕。
另一方面，不滿足本發明之基板的洗淨劑組成物之構成要件的比較例1~比較例4中，不能夠獲得良好清潔性，又，發生了基板的腐蝕。
藉此，確認了若本發明之基板的洗淨劑組成物，則即使薄型基板能夠以短時間獲得良好清潔性，並基板不會腐蝕且有以高效率矽半導體基板之洗淨的可能性。
另外，本發明並無特別限定於上述實施形 態。上述實施形態係例示，與記載在本發明之申請專利範圍之技術思想具有實質上相同構成，展現同樣作用效果者係即使如何者皆包含在本發明的技術範圍。

Claims (8)

  1. 一種基板的洗淨劑組成物，係使用於基板表面的洗淨之洗淨劑組成物，其特徵為：含有下述成分而成；(A)第四級銨鹽：0.1~2.0質量%(B)水：0.1~4.0質量%(C)有機溶媒：94.0~99.8質量%。
  2. 如申請專利範圍第1項之基板的洗淨劑組成物，其中前述經洗淨之基板為具有100度以上的水接觸角之矽半導體基板。
  3. 如申請專利範圍第1或2項之基板的洗淨劑組成物，前述第四級銨鹽為四烷基氫氧化銨。
  4. 如申請專利範圍第3項之基板的洗淨劑組成物，其中前述四烷基氫氧化銨為四乙基氫氧化銨。
  5. 如申請專利範圍第1或2項之基板的洗淨劑組成物，其中前述有機溶媒為在分子中含有至少1個以上的羥基之有機溶媒，含碳數1~8的飽和脂肪族醇，碳數2~16的乙二醇，及碳數4~20的乙二醇醚之中至少1種以上。
  6. 如申請專利範圍第1或2項之基板的洗淨劑組成物，其中前述經洗淨之基板係厚度20~100μm的薄型基板。
  7. 一種基板的薄型加工方法，其係於支持基盤介由接著劑接合形成有半導體電路之基板，予以背面加工處理，將支持基盤與接著劑一起剝離後，使用如申請專利範圍第 1項的洗淨劑組成物去除殘餘接著劑。
  8. 如申請專利範圍第7項之基板的薄型加工方法，其中接著劑為聚矽氧系接著劑。
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US10260027B2 (en) 2019-04-16
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US20170130174A1 (en) 2017-05-11
US20140357052A1 (en) 2014-12-04
TWI601815B (zh) 2017-10-11
JP6165665B2 (ja) 2017-07-19
KR101968780B1 (ko) 2019-04-12

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