TWI239435B - Method and composition for removing sodium-containing material from microcircuit substrates - Google Patents

Method and composition for removing sodium-containing material from microcircuit substrates Download PDF

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TWI239435B
TWI239435B TW090103920A TW90103920A TWI239435B TW I239435 B TWI239435 B TW I239435B TW 090103920 A TW090103920 A TW 090103920A TW 90103920 A TW90103920 A TW 90103920A TW I239435 B TWI239435 B TW I239435B
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stripping
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George Schwartzkopf
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    • G03F7/00Photomechanical, e.g. photolithographic, production of textured or patterned surfaces, e.g. printing surfaces; Materials therefor, e.g. comprising photoresists; Apparatus specially adapted therefor
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    • C11D7/00Compositions of detergents based essentially on non-surface-active compounds
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    • GPHYSICS
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    • G03FPHOTOMECHANICAL PRODUCTION OF TEXTURED OR PATTERNED SURFACES, e.g. FOR PRINTING, FOR PROCESSING OF SEMICONDUCTOR DEVICES; MATERIALS THEREFOR; ORIGINALS THEREFOR; APPARATUS SPECIALLY ADAPTED THEREFOR
    • G03F7/00Photomechanical, e.g. photolithographic, production of textured or patterned surfaces, e.g. printing surfaces; Materials therefor, e.g. comprising photoresists; Apparatus specially adapted therefor
    • G03F7/26Processing photosensitive materials; Apparatus therefor
    • G03F7/42Stripping or agents therefor
    • G03F7/422Stripping or agents therefor using liquids only
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    • GPHYSICS
    • G03PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
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    • G03F7/00Photomechanical, e.g. photolithographic, production of textured or patterned surfaces, e.g. printing surfaces; Materials therefor, e.g. comprising photoresists; Apparatus specially adapted therefor
    • G03F7/26Processing photosensitive materials; Apparatus therefor
    • G03F7/42Stripping or agents therefor
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    • C11D2111/00Cleaning compositions characterised by the objects to be cleaned; Cleaning compositions characterised by non-standard cleaning or washing processes
    • C11D2111/10Objects to be cleaned
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/04Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
    • H01L21/18Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
    • H01L21/30Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
    • H01L21/31Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to form insulating layers thereon, e.g. for masking or by using photolithographic techniques; After treatment of these layers; Selection of materials for these layers
    • H01L21/3105After-treatment
    • H01L21/311Etching the insulating layers by chemical or physical means
    • H01L21/31127Etching organic layers
    • H01L21/31133Etching organic layers by chemical means

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Description

1239435 A7 B7 五、發明説明 lJU力領域 本發明係在製造積體電路中自微電路基材移除光阻與其 他材料之領域内。 复·量技術之說明 微電子製作的整體部分係使用光阻自護罩或網上轉移影 像土所需電路層。完成必要影像轉移後剝除光阻而後進行 其次某些程序步騾。 文活動離子特別經鈉離子沾污、尤其在高溫作業期間斜 向預燒試驗中為積體電路許多不合格之起因。積體電路製 作期間可於多項階段内引進活動離子污染。 有關積體電路技藝的發展不斷尋求減少活動離子污染之 材料與技術。美國專利5,417,802號中用冠狀醚類以多價螯 合於有機溶劑内供移除光阻用之I族及11族離子。 發明之概要 根據本發明提供剝除含鈉物質如光阻的方法及組成物。 剥除組成物包括在有機溶劑内之丨,2 _二胺基環己烷四羧酸 (C YDTA )。本發明方法包括用該剥除組成物接觸該基 材。 發明的詳細說明 光阻移除及金屬蝕刻後清潔用有機溶劑為活動離子污染 《普通來源。典型溶劑包含伯胺、仲胺與其他溶劑諸如二 甲亞颯及二甲基乙醯胺的摻混物。此等溶劑常貯在塑膠(例 如高密度聚丙缔)容器中ϋ此等塑膠容器涉及使用其
1239435 A7 B7 五、發明説明(2 ) 中可能含鈉的無機觸媒。因此當溶劑儲於此等塑膠容器内 時納能浸提入溶劑。溶劑中鋼濃度隨接觸塑膠期間增加。 頃發現1,2 -二胺基環己烷四羧酸(CYDTA )與鈉離子適當 螯合,抑制鈉吸附於積體電路表面。在移除光阻或金屬蝕 刻後清潔習用之有機溶劑内添加1,2 -二胺基環己烷四羧酸 經發現所得潔淨後積體電路表面上測出的鈉濃度大為減 少 〇 用氮化鈦沈積於矽基底上並以輔助的離子質譜術(SIMS ) 檢查之實驗指出添加1,2 -二胺基環己烷四羧酸於習用的有 機溶劑配方諸如 NJ,Phillipsburg,Mallinckrodt Baker Incorporated之註冊商標ALEG-3 10®等,大幅降低此等基材 的表面鈉濃度。與前述冠狀醚類平行處理之直接比較證明 本發明在所得潔淨表面上結果鈉濃度低得多。 於一典型應用中,可使用經1,2 -二胺基環己烷四羧酸改 良之有機溶劑自蝕刻之氧化物、金屬或半導體基材圖樣中 移除有花樣的光阻,藉以減低所得積體電路之鈉污染程 度。或者,光阻可藉曝露於氧電漿部分移除光阻,再用本 發明移除所得不必要之餘留物。 一具體例利用一剥除溶劑、一親質子性胺、一不含氮的 弱酸,其量足以部分中和此親質子性胺俾此剝除組成物當 以約1 0份水稀釋時有約9.6至約10.9之水液pH,該弱酸的 水溶液有2.0或較高p K值及低於140之當量及1,2-二胺基環 己烷四羧酸,因而該剝除組合物能在極少增加洗淨積體電 路的表面鈉濃度下剥除無用之光阻或光阻殘餘物。 -5- 本紙張尺度適用中國國家標準(CNS) A4規格(210X297公釐) 1239435 A7 ____ B7 五、發明説明( ) 3 本發明中可用的不含氮弱酸包括有機酸如羧酸類或紛類 及無機酸如碳酸或氫氟酸之鹽類。 所謂弱酸係指水溶液内離解常數具有強度以” p K ”表示 至少2.0以上,較佳2.5或更高。特別適用pK > 2.0之弱 紅’宜有當量小於約140。可提及作為本發明中可用的不 含氮弱酸實例如羧酸類諸如醋酸、酞酸、苯氧基醋酸及其 類似物,有機酸類諸如2 -巯基苯甲酸、2 -巯基乙醇及其類 似物,一般pK在9-10範圍中之酚類如苯酚、1,3,5-三經基 苯、連苯三酚、間苯二酚、4 -特丁基苯鄰二酚及其類似 物’及無機酸類如碳酸、氫氟酸及其類似物。本發明剥除 組成物中弱酸用量為該組成物重量之約0.05%至約2 5 %, 含量將中和剥除組成物内所存約1 9 %至約7 5 %重量的胺, 因而得該剝除組成物之含水沖洗pH自約9.6至約10.9。 本發明中可用的鹼性剥除組成物亦涵蓋廣範圍結構型。 其離析常數仍以pK值表示,範圍自β -氧或-氮代胺類之約 9至1 1以迄仲胺、嗎啉與羥胺類的8 · 3及某些更低ρ κ值之 羥胺衍生物。可提及之可用的鹼性組份有親核胺類,較佳 例如1-胺基-2-丙醇,2-(2 -胺乙氧)基乙醇,2 -胺基乙 醇’ 2-(2 -胺基乙胺基)乙醇,2-(2 -胺乙基胺基)乙胺及其 類似物。比胺之實際p K值更重要者為其親質子性應高。 本發明剝除組成物中胺組份用量為該組成物重量的約1 % 至約5 0 %。 相信此等鹼性剥除組份與本發明所用弱酸範圍之相互作 用基本上係可逆的: -6- 1239435 A7 B7 五、發明説明(4 ) 驗性組份+酸=鹽狀之複合物。 由於此反應的可逆性、縱使自化學計算觀點言多量鹼性 、’且伤已、,二中和、剥除程序期間仍保留實質濃度之驗性組 份。如此可證即使有此等酸類存在亦察見剝除速度奇快。 本發明的光阻剥除組成物含一有機溶劑系統。此有機溶 劑系統具有溶解度參數自約8至約15,得自三項Hansen溶 解度參數(分散的、極性與氫鍵)平方總和之平方根。此溶 劑系統可由任何多數單獨溶劑或幾種不同溶劑的混合物組 合。可提述之此項溶劑實例有多種吡咯烷酮化合物諸如2_ 吡各烷酮,1 -甲· 2 -吡咯烷酮,丨·乙_ 2 _吡咯烷酮,卜丙_ 2-吡咯烷酮,丨_羥乙基-2-吡咯烷酮,丨_羥丙基比咯烷 酮及其類似物;二甘醇-烷基醚諸如具h〇CH2CH2_〇_ CH2CHr 0-R式其中R係一 1-4碳原子的烷基團者,含二氧 化硫之化合物諸如 〇
II
Rl—S—R2 » 〇 式的二烷基亞颯(DMSO),其中r% R2係丨·4碳原子之烷 基;
〇 本紙張尺度適用中國國家標準(CNS) Α4規格(210 X 297公釐) A7 B7 1239435 五、發明説明(c ) 5 式的四氫喧吩-1,1-二氧化物,其中R3係氫,甲基或乙基, ‘者如一氧p塞吩、甲基一氧喧吩及乙基二氧ϊτ塞吩,與聚乙二 醇一甲基乙醯胺或一甲基甲酿胺。本發明剝除組合物之 溶劑系統部分通常佔組成物重量約5 〇 %至約9 8 %,較佳約 重量8 5 %至約9 8 %。 較佳▲劑為N-燒基-2 -外1^各垸酮,諸如n -甲基·,n、乙 基-,N-丙基.與N-(2_羥乙基卜,二甲亞砜,二甲基乙醯 胺及二甲基甲醯胺。 特佳4劑為N -甲基-2 - p比嘻垸酮與四氫喧吩_ 1,1 _二氧化 物。 實例 种量1 0 0 〇公克的剥除溶劑入一氟聚合物杯,含約5 〇份 N-曱基-2-吡咯烷酮,約10份四氫噻吩·丨,^二氧化物, 約2 5份2 -胺基乙醇,約5份丨,2 _二羥苯與約丨〇份水。秤出 添加劑1,2 -二胺基環己烷四羧酸或1 8 •冠狀醚_ 6,視需要 /谷於刎除落劑。升高溶液至所須溫度,放置一氮化鈦(丁iN) 包覆的晶片於溶液中歷2〇分鐘,取出以Di水沖洗並用 SIMS分析。全部實驗在一丨〇 〇級潔淨室内完成,特別慎防 晶片之鋼污染。 三塊晶片接受水沖洗與乾燥步驟僅為建立底線鈉值而不 作任何釗除溶劑處理。在6 5 t與8 5 °C測試未修飾之剝除 幺片]歷20刀鐘以決定此法在丁 iN表面上餘留的相對納量。 結果表現於表i。第二組實驗内加〇1重量%之水合丨,八二 胺基環己燒四羧酸(CYDTA)於剥除溶劑。第三組實驗中
1239435 A7 B7 五、發明説明(Λ ) 6 水合1,2 -二胺基環己烷四羧酸重量%增至0 · 5 %。第四組 實驗内提高水合1,2 -二胺基環己烷四羧酸的重量百分比至 0.9%。第五組中加0.1重量%之1 8 -冠狀醚-6於剝除溶劑, 在4 5 °C,6 5 °C及8 5 °C下試驗。 此等數據(表1 )顯然證明添加1,2 -二胺基環己烷四羧酸 於剝除溶劑結果表面納濃度比未修飾的溶劑内降低很多。 添加冠狀醚效果無益。 表1 製程 虛理溫/ire) 相對表面鈉濃/ti用SIMS) 水漂與乾燥 (未處理) 0.0052, 0.0046, 0.0051 僅剥除溶劑 65〇C 0.16 85〇C 0.25 溶劑+0.1%CYDTA 65t 0.04 85〇C 0.07 溶劑 + 0.5% CYDTA 65〇C 0.02 85〇C 0.05 溶劑 + 0.9% CYDTA 65〇C 0.03 85〇C 0.04 溶劑+ 0.1% 18-冠狀醚-6 45〇C 0.33 65〇C 0.41 85〇C 0.45 本紙張尺度適用中國國家標準(CNS) A4規格(210 X 297公釐)

Claims (1)

  1. AS B8 C8 1239435 申請專利範圍 •二,在以含有機溶劑之組成物行光阻移除或金屬蝕刻後 清潔期間抑制鈉吸附至積體電路表面之方法,其包括使 琢表面與含有機溶劑之組成物接觸,該組成物包括: a)丨,2 -二胺基環己院四酷酸(CYDTA), b )親質子性胺,其以組成物重量計約丨至約5 q %之 存在, c )不含氮的弱酸,其量足以部分中和此親質子性胺俾此 剝除組成物當以約1 0份水稀釋時有約9 · 6至約 1 〇 · 9之水性p Η,該弱酸在水溶液内有2 〇或更高 的Ρ Κ值及小於1 4 0之當量值,及 ^ d)落劑,其係一剥除溶劑系統,其具有自約8至約^ $ 的落解度參數,含量為以組成物重量計自約5 〇 %至 約9 8% 2·,據=請專利範圍第丨項之方法,其中剝除組成物内弱 酸含量為以該剥除组成物重量計的約〇 〇5%至約2 5 %。 3·根據申請專利範圍第2項之方法’其中弱酸有2.5或更高 的PK。 4. 根據申請專利範圍第3項之方法,其中弱酸2 冬。 5. 根據中請專利範圍第4項之方法,#中親質子性胺為2_ 胺基乙醇。 6·根據申請專利範圍第5項之方法,其中溶劑系統包括為 Ν-甲基-2-吡咯烷酮與四氫嘍吩—^-二氧化物,可視情 况多達約1 〇 %的水。 7.根據申請專利範圍第i項之方法,其以重量基計包括: 自約50%至約98%的心甲基·2κ坡酮,自約1%至 -10-
    1239435 C8
    约2 0。/〇之四氫喧吩-i,i ·二氧化物,自約1 %至約2 〇。/〇的 水’自約1 %至約5 0 %之2 -胺基乙醇,自約0.05 %至約 25°/〇之1,2-二羥苯’及約〇·〇1%至二胺基環己 烷四幾酸。 8 · 一種在以含有機溶劑之組成物行光阻移除或金屬蝕刻後 清潔期間抑制鈉吸附至積體電路表面之組成物,該含有 機溶劑之組成物包括: a) 1,2-二胺基環己燒四醋酸(cydtA), b )親質子性胺,其以組成物重量計約1至約5 〇 %之量 存在, c )不含氮的弱酸,其量足以部分中和此親質子性胺俾此 剥除組成物當以約1 〇份水稀釋時有約9.6至約 1 〇 · 9之水性p Η ’該弱酸在水溶液内有2 · 〇或更高 的Ρ Κ值及小於1 4 0之當量值,及 d)洛劑,其係一剝除溶劑系統,其具有自約8至約1 5 的i解度參數,含量為以組成物重量計自約5 0 %至 約9 8% 9·根據申請專利範圍第8項之組成物,其中剥除組成物内 Θ故含I為以該剥除組成物重量計的約0.05%至約 2 5〇/〇。 * .根據申凊專利範圍第9項之組成物,其中弱酸有2 · 5或更 高的ρ K。 U·根據申請專利範圍第1 〇項之組成物,其中弱酸係1,2 -二 羥苯。 ’ 12·根據申請專利範圍第1 1項之組成物,其中親質子性胺為 -11 - 8 8 8 8 A BCD 1239435 ~—·~____ 六、申請專利範圍 胺基乙醇。 13.根據中請專利範圍第12項之組成物,其中溶劑系統包括 為N_曱基_2_吡咯烷酮與四氫。塞吩“,丨-二氧化物,可視 情沉多達約1 〇 %的水。 κ根據申請專利範圍第8項之組成物,其以重量基計包 括.自約5 0 %至約9 8 %的N -甲基-2 - p比咯燒酮,自約 1 %至約2 0 %之四氫嘍吩-丨,丨_二氧化物,自約1 %至約 2 0 0/〇的水,自約1 %至約5 〇 %之2 -胺基乙醇,自約 0.05%至約25%之1,2_二羥苯,及約0.01%至5%之1,2-二胺基環己烷四羧酸。 -12- i纸張尺度適用中國國家標準(CNS) A4規格(210X297公釐) 12394% . 申請曰期 9 〇、叫 十 —--— 案 號 090103920 類 別 ^〇yfY^( €ί^Υτ〇 C4 煩 請 委 員 明 f|專利説明書 -、雲!名稱 中 文 用於自微電路基材移除含鋼物質之方法及組成物 英 文 ME 1 HOD AND COMPusn iON FOR REMOVING SODIUM-CONTAINING MATERIAL FROM MICROCIRCUIT SUBSTRATES" 公修正後是否!.!♦;質内容< 姓 名 國 籍 喬治史瓦姿庫夫 GEORGE SCHWARTZKOPF 美國 發明 創作> 住、居所 姓 义(名稱) 國 籍 美國紐澤西州華盛頓市富蘭克林鎮比寇路97號 美商瑪琳I特公司 MALLINCKRODT INC. 美國 裝 線 三、申請人 f事務ία 名 美國密蘇里州聖路易市麥克當勞大道675號 傑佛瑞S.波恩 JEFFREY S. BOONE
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