TWI788452B - 基於氟化物之清洗組合物 - Google Patents
基於氟化物之清洗組合物 Download PDFInfo
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- TWI788452B TWI788452B TW107139429A TW107139429A TWI788452B TW I788452 B TWI788452 B TW I788452B TW 107139429 A TW107139429 A TW 107139429A TW 107139429 A TW107139429 A TW 107139429A TW I788452 B TWI788452 B TW I788452B
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- 239000003960 organic solvent Substances 0.000 claims abstract description 18
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Images
Classifications
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- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
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- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
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Abstract
本發明係關於一種清洗組合物,其包含a)占該組合物之總重量1至5重量%之氟化銨;b)占該組合物之總重量30至70重量%之水溶性有機溶劑;c)占該組合物之總重量1.5至20重量%之有機胺;及d)占該組合物之總重量31至60重量%之去離子水。本發明之清洗組合物提供良好的清洗功效,同時為溫和的清洗組合物且具有穩定的pH。
Description
本發明係關於適合於半導體晶圓清洗之基於氟化物之清洗組合物。
諸如積體電路及大型積體電路之半導體器件以及液晶面板裝置及其他顯示面板裝置之製造包含以下步驟:在金屬層或絕緣層上形成均一光阻塗層;執行所需曝露及顯影以形成光阻圖案;藉由化學氣相沈積使用光阻圖案作為光罩來(選擇性地)蝕刻具有金屬層或絕緣層之基板以形成微電路;及用液體汽提塔自基板移除不合需要之光阻層、蝕刻殘餘物、殘餘光阻及光阻副產物中之一或多者。各種有機液體光阻汽提溶液已用於自基板移除不合需要之光阻層、蝕刻殘餘物、殘餘光阻及光阻副產物。先前技術通常採用含氟化合物之組合物諸如含氫氟酸之光阻汽提溶液以用於移除不合需要之光阻層。
先前技術中所描述之一種光阻汽提溶液主要包含(a)具有不含金屬之基質之氫氟酸之鹽、(b)水溶性有機溶劑及(c)水,且具有5至8之pH。與此種溶液相關之問題通常關於氫氟酸之鹽之量,較低量導致差清洗有效性,而較高量導致溶解度問題。
另一種光阻汽提溶液包含鹼性物質以調節溶液之pH。此種組合物之實例包含(a)具有不含金屬離子之基質之氫氟酸之鹽;(b)水溶性有機溶劑;(c)鹼性物質;及(d)水。一般而言,此種溶液中之較佳pH值為8.5至10.0,且先前技術指示該pH值可藉由少量鹼性物質0.1-0.3 wt%來達成。此種溶液之潛在問題在於,藉由用水稀釋顯著地降低pH。此外,存在與由於水沖洗導致之鋁金屬腐蝕相關之問題。
先前技術亦揭示含有氫氟酸之鹽之緩衝清洗組合物。此等組合物之pH通常為7至11。此pH範圍由於對TEOS (藉由化學氣相沈積正矽酸四乙酯而製成之二氧化矽膜)之低損壞而為較佳的。緩衝系統有助於pH值之穩定性,然而,當用水稀釋清洗組合物時pH仍波動。
因此,仍需要一種清洗組合物,其提供高清洗效率,同時在經水稀釋期間具有穩定的pH值,且為溫和的且不對諸如SiO2
之介電材料以及諸如鋁及鋁合金之金屬層造成損壞。
本發明係關於一種清洗組合物,其包含a)占該組合物之總重量1至5重量%之氟化銨;b)占該組合物之總重量30至70重量%之水溶性有機溶劑;c)占該組合物之總重量1.5至20重量%之有機胺;及d)占該組合物之總重量31至60重量%之去離子水。
本發明係關於本發明之組合物在半導體清洗中之用途。
本發明亦涵蓋自基板移除蝕刻殘餘物、殘餘光阻及光阻副產物中之一或多者之方法,其包含以下步驟:使上面存在蝕刻殘餘物、殘餘光阻及光阻副產物中之一或多者之基板與本發明的組合物接觸。
本發明更詳細地描述於以下段落中。除非相反地清楚指示,否則如此描述之各態樣可與任何其他一或多個態樣組合。詳言之,指示為較佳或有利之任何特點均可與指示為較佳或有利之任何其他一或多個特點組合。
在本發明之上下文中,除非上下文另外指出,否則根據以下定義解釋所使用之術語。
除非上下文另外清楚地指出,否則如本文所使用之單數形式「一(a/an)」及「該」包括單數個及複數個提及物。
如本文所使用之術語「包含(comprising/comprises)」及「由……構成(comprised of)」與「包括(including/includes)」或「含有(containing/contains)」同義,且為包括性或開放性的,且不排除額外的未敍述成員、元素或方法步驟。
數值端點之敍述包括包含於各別範圍內之所有數字及分數以及所敍述之端點。
除非另外指示,否則本文所提及之所有百分比、份數、比例及其類似者均以重量計。
當以範圍、較佳範圍或較佳上限值及較佳下限值之形式表達量、濃度或其他值或參數時,應理解在不考慮所獲得之範圍是否清楚地在上下文中清楚地提及之情況下,特定地揭示藉由組合任何上限值或較佳值與任何下限值或較佳值而獲得之任何範圍。
在本說明書中所引用之所有參考文獻均以全文引用之方式併入本文中。
除非另外定義,否則用於揭示本發明之所有術語包括技術及科學術語均具有如本發明所屬領域之一般熟習此項技術者通常所理解的意義。藉助於進一步導引,將術語定義包括在內以更好地瞭解本發明之教示內容。
本發明係關於一種清洗組合物,其包含a)占該組合物之總重量1至5重量%之氟化銨;b)占該組合物之總重量30至70重量%之水溶性有機溶劑;c)占該組合物之總重量1.5至20重量%之有機胺;及d)占該組合物之總重量31至60重量%之去離子水。
本發明之清洗組合物含有相對較高量之氟化銨以提供高清洗效率,然而儘管為高量,氟化銨仍保持可溶性。另外,本發明之清洗組合物在經水稀釋時具有穩定的pH值。此外,本發明之清洗組合物為溫和的清洗溶液,且不損壞諸如SiO2
之介電材料以及諸如鋁及鋁合金之金屬層。
根據本發明,組合物中之超過1%之氟化銨視為高量且組合物中之少於0.1%之氟化銨視為低量。一般而言,高氟化銨量有利於清洗,然而,高量可能造成溶解度問題且對金屬表面(Al、AlCu、Cu)及介電材料(SiO2
)造成損壞。一般而言,低氟化銨量不造成損壞,然而,清洗功效受到不利影響。
本發明之清洗組合物包含高量氟化銨。使用氟化銨係因為其有助於達成高濃度之氟陰離子,這引起高清洗有效性。儘管在組合物中具有高氟化銨量,其不對Al、AlCu、Cu及SiO2
(TEOS)表面造成損壞。
用於本發明之合適的市售氟化銨為例如但不限於來自Morita Chemical Industories CO., Ltd.之電子級氟化銨溶液40%及來自Kanto Chemical Co., Inc.之氟化銨(40%)。
本發明之清洗組合物包含占該組合物之總重量1至5重量%、較佳2至4重量%且更佳2.5至3.5重量%之氟化銨。
若氟化銨之量少於1%,則清洗有效性降低,然而量超過5%,氟化銨不可溶於富含溶劑之溶液中。
本發明之清洗組合物包含水溶性有機溶劑。合適的水溶性有機溶劑促進其他成分在清洗組合物中之溶解度,且另外,其提供良好的清洗有效性。
用於本發明之合適的水溶性有機溶劑選自由以下組成之群:N-甲基吡咯啶酮(NMP)、二甲亞碸(DMSO)、甲基二甘醇(MDG)、丁基二甘醇(BDG)、N,N-二甲基甲醯胺、N,N-二甲基乙醯胺、γ-丁內酯、乙二醇、丙二醇及其混合物,該溶劑較佳選自N-甲基吡咯啶酮(NMP)、二甲亞碸(DMSO)及其混合物。
DMSO為較佳之水溶性有機溶劑,此係因為其促進氟化銨之極佳溶解度。DMSO亦促進待自表面移除之樹脂之溶解度。
在一個實施例中,本發明之清洗組合物包含一或多種水溶性有機溶劑與DMSO之混合物。額外的水溶性有機溶劑並未受到特定限制,只要其可與水及DMSO混溶即可。該等水溶性有機溶劑之實例包括不限於N-甲基吡咯啶酮(NMP)、甲基二甘醇(MDG)、丁基二甘醇(BDG)。N-甲基吡咯啶酮(NMP)較佳與DMSO組合使用,因為其提供良好的清洗有效性。
用於本發明之合適的市售水溶性有機溶劑為例如但不限於來自Toray Fine Chemical Co., Ltd.之DMSO、來自Mitsubishi Chemical Corporation之N-甲基-2-吡咯啶酮(NMP)及來自BASF SE之N-甲基-2-吡咯啶酮(dist.)。
本發明之清洗組合物包含占該組合物之總重量30至70重量%、較佳35至65重量%、更佳45至65重量%且甚至更佳50至61重量%之水溶性有機溶劑。
若有機溶劑量少於30%,則因此組合物富含水且對Al、Cu及AlCu表面造成損壞。然而,過高有機溶劑量超過70%,導致氟化銨之差溶解度。
當使用溶劑DMSO與NMP之組合時,DMSO:NMP之比率較佳為99:1至10:90,更佳50:50至20:80。
本發明之清洗組合物含有有機胺。當組合物經水稀釋時有機胺為其提供pH穩定性。降低pH值具有諸如鋁及鋁合金之金屬之腐蝕問題。有機胺促進降低對氧化矽之損壞。此外,有機胺促進氟化銨之溶解度。
用於本發明之合適的有機胺選自由以下組成之群:單乙醇胺、二乙醇胺、三乙醇胺、單異丙醇胺、2-(2-胺基乙胺基)乙醇、2-胺基-2-甲基-1-丙醇、N-甲基乙醇胺、2-(二甲胺基)乙醇、乙二胺、丙二胺及其混合物,該有機胺較佳為單乙醇胺、三乙醇胺。
三乙醇胺為較佳有機胺,此係因為其提供pH穩定性且其促進待自表面移除之樹脂之膨脹及溶解。
用於本發明之合適的市售有機胺為例如但不限於來自BASF SE之三乙醇胺(純)及單乙醇胺(純);來自the Dow Chemical Company之三乙醇胺DOW™及單乙醇胺DOW™。
本發明之清洗組合物包含占該組合物之總重量1.5至20重量%、較佳2至15重量%、更佳2.5至12.5重量%且甚至更佳3.5至5重量%之有機胺。
當有機胺量小於1.5%時,在用水稀釋組合物時pH波動,且TEOS受到損壞,而量高於20%,組合物對Al及AlCu表面造成損壞。
本發明之清洗組合物包含水。水促進氟化銨之溶解度及AlCu蝕刻速率。
用於本發明之組合物之水必須為去離子水,此係因為金屬離子污染對半導體器件之電性質提供負面影響。去離子水之純度之特徵在於電阻率。用於適用於本發明之去離子水之電阻率較佳超過15 MΩ/cm、更佳超過17 MΩ/cm且甚至更佳超過18 MΩ/cm。可藉由使用來自HORIBA Ltd.之HE-480R及來自Myron L® Company之Ultrameter II™量測電阻率。
本發明之清洗組合物包含占該組合物之總重量31至60重量%、較佳32至50重量%、更佳32至45重量%且甚至更佳32至40重量%之水。
若水量少於31%,則氟化銨之溶解度降低,然而若量超過60%,則組合物對Al、Cu及AlCu表面造成損壞。
本發明之組合物可進一步包含酸。用於本發明之合適的酸可為有機酸或無機酸,較佳為有機酸。
可將有機物添加至本發明之組合物以調節pH,以充當pH緩衝液、腐蝕抑制劑或螯合劑。
用於本發明之合適的有機酸可選自由以下組成之群:甲酸、乙酸、丙酸、丁酸、異丁酸、草酸、丙二酸、丁二酸、戊二酸、順丁烯二酸、反丁烯二酸、苯甲酸、鄰苯二甲酸、1,2,3-苯三甲酸、乙醇酸、乳酸、蘋果酸、檸檬酸、酒石酸及其混合物。
本發明之組合物可包含占該組合物之總重量0.1至10.0重量%、較佳0.5至5.0重量%且更佳1.0至3.0重量%之有機酸。
用於本發明之合適的市售有機酸為例如但不限於來自Showa Kako Corporation之單水合檸檬酸及無水檸檬酸。
本發明之清洗組合物可進一步包含選自以下之一或多種額外的組分:界面活性劑,其選自陰離子界面活性劑、非離子界面活性劑及其混合物;腐蝕抑制劑,其選自唑化合物、硫醇化合物、諸如木糖醇及山梨醇之糖醇;及螯合劑。
本發明之清洗組合物係藉由在摻合槽中摻合原料來製成。優選控制溫度低於40℃,同時進行摻合以避免不合需要之副反應及任何原料之蒸發。封閉系統較佳用於摻合以避免任何原料之蒸發。
本發明之組合物之pH為8.0至11.0、較佳8.5至10.5。pH係藉由使用玻璃電極法(Glass-Electrode Method)由10%水溶液及未經稀釋溶液在室溫下量測。pH係藉由使用由Horiba, Ltd.製造之pH計(型號:F-51)來量測。
8.0至11.0之pH為較佳的,此係因為其提供清洗效率與對金屬表面(Al、AlCu、Cu)及介電材料(SiO2
)之損壞之間的平衡。若組合物之pH大於11.0,則清洗效率降低且對金屬表面造成損壞。在另一方面,若組合物之pH低於8.0,則其對介電材料(SiO2
)造成損壞。
本發明之組合物可用於半導體清洗,較佳用於半導體分批清洗、半導體分批噴霧清洗,用於半導體毛刷清洗及用於半導體單晶圓清洗,更佳用於半導體單晶圓清洗。
本發明係關於自基板移除蝕刻殘餘物、殘餘光阻及光阻副產物中之一或多者之方法,其包含以下步驟:使上面存在蝕刻殘餘物、殘餘光阻及光阻副產物中之一或多者之基板與本發明的組合物接觸。實例
pH係藉由使用玻璃電極法由10%水溶液及未經稀釋溶液在室溫下量測。pH係藉由使用由Horiba, Ltd.製造之pH計(型號:F-51)來量測。
AlCu蝕刻速率(ER)由加工時間及形成於矽晶圓上之AlCu膜之厚度損失確定。AlCu膜之厚度係藉由使用由Napson Corporation製造之RT-70四點探針來量測。在測定初始AlCu厚度之後,在25℃下將測試晶圓浸入測試溶液中。在30分鐘之後,將測試晶圓自測試溶液中移除,用去離子水沖洗三分鐘且在氮氣下完全乾燥。隨後,量測AlCu厚度以確定由浸入測試溶液中而導致之厚度損失。
TEOS蝕刻速率(ER)由加工時間及形成於矽晶圓上之TEOS膜之厚度損失確定。TEOA膜之厚度係藉由使用由Otsuka electronics co. Ltd.製造之光學厚度監視器(型號:FE-3000)來量測。在測定初始TEOS厚度之後,在25℃下將測試晶圓浸入測試溶液中。在30分鐘之後,將測試晶圓自測試溶液中移除,用去離子水沖洗三分鐘且在氮氣下完全乾燥。隨後,量測TEOS厚度以確定由浸入測試溶液中而導致之厚度損失。
經AlCu塗佈之晶圓:用市售氣相沈積之AlCu合金(Al:99.5%,Cu:0.5%)膜塗佈晶圓300 nm。
經TEOS塗佈之晶圓:用藉由化學氣相沈積市售正矽酸四乙酯而製成之二氧化矽膜塗佈晶圓100 nm。
將經塗佈之晶圓切割成2.5 cm×2.5 cm片件且在25℃下浸入測試溶液中。
表1舉例說明實例1-8中之本發明之清洗組合物。所有此等實例均具有高濃度氟化銨及穩定的pH值,另外組合物中無一者對TEOS及AlCu表面造成損壞。
圖1說明水與AlCu蝕刻速率(ER)之間的關係。圖1含有比較實例14及實例1至5之組合物之AlCu ER資料。
圖1說明水與AlCu蝕刻速率(ER)之間的關係。
Claims (5)
- 一種清洗組合物,其包含a)占該組合物之總重量2.5至3.5重量%之氟化銨;b)占該組合物之總重量50至61重量%之水溶性有機溶劑,其中該水溶性有機溶劑係N-甲基吡咯啶酮與二甲亞碸之混合物;c)占該組合物之總重量3.5至5重量%之有機胺,其中該有機胺係三乙醇胺;及d)占該組合物之總重量32至40重量%之去離子水,其中該組合物具有8.0至11.0之pH。
- 如請求項1之組合物,其進一步包含選自由以下組成之群之有機酸:甲酸、乙酸、丙酸、丁酸、異丁酸、草酸、丙二酸、丁二酸、戊二酸、順丁烯二酸、反丁烯二酸、苯甲酸、鄰苯二甲酸、1,2,3-苯三甲酸、乙醇酸、乳酸、蘋果酸、檸檬酸、酒石酸、葡萄糖酸、乙醛酸、五倍子酸及其混合物。
- 如請求項1或2之組合物,其pH為8.5至10.5。
- 一種如請求項1至3中任一項之組合物在半導體清洗中之用途。
- 一種自基板移除蝕刻殘餘物、殘餘光阻及光阻副產物中之一或多者之方法,其包含以下步驟: 使上面存在蝕刻殘餘物、殘餘光阻及光阻副產物中之一或多者之基板與如請求項1至3中任一項的組合物接觸。
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TW200702942A (en) * | 2005-05-06 | 2007-01-16 | Mallinckrodt Baker Inc | Compositions for the removal of post-etch and ashed photoresist residues and bulk photoresist |
TW201416436A (zh) * | 2012-10-23 | 2014-05-01 | Air Prod & Chem | 清潔配方 |
TW201725262A (zh) * | 2016-01-05 | 2017-07-16 | 富士軟片股份有限公司 | 處理液、基板的洗淨方法以及半導體裝置的製造方法 |
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US8030263B2 (en) | 2004-07-01 | 2011-10-04 | Air Products And Chemicals, Inc. | Composition for stripping and cleaning and use thereof |
TWI339780B (en) | 2005-07-28 | 2011-04-01 | Rohm & Haas Elect Mat | Stripper |
JP2007200944A (ja) | 2006-01-23 | 2007-08-09 | Tokuyama Corp | 基板洗浄液 |
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TW200702942A (en) * | 2005-05-06 | 2007-01-16 | Mallinckrodt Baker Inc | Compositions for the removal of post-etch and ashed photoresist residues and bulk photoresist |
TW201416436A (zh) * | 2012-10-23 | 2014-05-01 | Air Prod & Chem | 清潔配方 |
TW201725262A (zh) * | 2016-01-05 | 2017-07-16 | 富士軟片股份有限公司 | 處理液、基板的洗淨方法以及半導體裝置的製造方法 |
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