TW416984B - Ethylenediaminetertraacetic acid or its ammonium salt semiconductor process residue removal composition and process - Google Patents

Ethylenediaminetertraacetic acid or its ammonium salt semiconductor process residue removal composition and process Download PDF

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Publication number
TW416984B
TW416984B TW087104387A TW87104387A TW416984B TW 416984 B TW416984 B TW 416984B TW 087104387 A TW087104387 A TW 087104387A TW 87104387 A TW87104387 A TW 87104387A TW 416984 B TW416984 B TW 416984B
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Taiwan
Prior art keywords
substrate
composition
patent application
residues
item
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TW087104387A
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English (en)
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Wai Mun Lee
Zhefei Jessie Chen
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Ekc Technology Inc
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    • B24B37/042—Lapping machines or devices; Accessories designed for working plane surfaces operating processes therefor
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Description

416984 經濟部中央標华跔負工消费合作社印製 A7 137 五、發明説明（1 ) 發明起源 本發明係爲1 9 9 6年4月1 7日申請之申請案第 0 8 / 6 2 8，0 6 0號之部分連續申請案，後者係爲 1 9 9 3年6月2 1曰申請之申請案第 08/07 8，6 5 7號之部分連續申請案，後者係爲 1 9 9 2年7月9曰申請之申請案第 07/9 1 1，1 0 2號—現在爲美國專利第 5，3 3 4，3 3 2號一之部分連續申請案，後者係爲 1990年11月5曰申請之申請案第 0 7/ 610，044號一現在爲美國專利第 5，2 7 9 ，7 7 1號—之部分連續申請案。此等申請案 :之揭示供作本發明之參考》
(I
I 發明背景 1 '發明範疇： 本發明大體上有關一種用以自基質上移除有機、有機 金屬 '及金屬氧化物殘留物之淸除組成物及方法。尤其有 關一種用以自半導體裝置基質移除半導體裝置製程殘留物 之組成物及方法，諸如於矽晶圓上製造積體電路及其他方 法之電漿蝕刻步驟後之蝕刻殘留物。特別有關一種可移除 此等物質，而實質避免攻擊積體電路上之金屬或絕緣層包 括駄層之組成物及方法。 2、先前技鷄描沭： 本紙張尺度適用1國國家標準（CNS〉Λ4规格（210x 297公聲) (請先閱讀背面之i±意事項再填巧本頁〕
416984 A7 Μ 五、發明説明（2 ) (請先閱讀背而之注意事項存填轉本萸) 積體電路製程日趨读雜，而於矽或其他半導體晶圓上 製造之電路元件愈來愈小，故用以移除此等材料所產生之 殘留物之技術需持續改善。製程完成時，經常使用氧電漿 氧化以移除使用後之光阻或其他聚合物材料。此等高能量 之方法一般使得在該製程所形成之結構之側壁上形成有機 金屬及其他殘留物。 積體電路製程通常使用各式各樣之金屬及其他料層， / 包括鋁、鋁/矽/銅、鈦、氮化鈦、鈦/鎢、鎢、氧化矽 、多矽晶體等。使用該等不同料層導致於高能量方法中形 成不同之有機金屬殘留物。除了可移除該殘留物外，淸除 組成物亦應不攻擊積體電路製程中所使用之不同金屬或絕 緣體= 經濟部中夹標準局爲工消费合作社印製 已發展出各種適於積體電路:製程之殘留物移除組成物 及方法，而甶本發明之所有權人一E K C Technology, inc. 市場化。某些此等組成物及方法可用以於積體電路製程中 自基質剝除光阻、聚醯胺或1 5種其他聚合物層，E K C 亦發展出各種於積體電路製程中自基質剝除該等聚合物層 之組成物及方法。該等組成物及方法係揭示於以下屬於相 同權人之專利中：L e e於1 9 9 6年1月9曰申請之美 國專利第5 ，482 ，566號；Lee於1995年3 月2 1曰申請之美國專利第5 ，3 9 9 ，4 6 4號；
Le e於1995年1月17日申請之美國專利第 5 ，381 ，807 號：Lee 於 1994 年 8 月 2 日申 請之美國專利第5，3 3 4，3 3 2號；L e e於 本紙張尺度適中國國家標準（CNS )如規格（21〇>< 297公犛）-5 - 經濟部中央標準局員工消贤合作社印製 416384 五、發明説明（3 ) 1 9 9 4年1月1 8日申請之美國專利第 5 ’ 279 ，771 號；Lee 於 1989 年 4 月 25 日 申請之美國尊利第4，824，763號及Le e於 1 9 8 3年7月2 6曰申請之美國專利第 4 ^ 3 9 5，3 4 8號。此等組成物實質上成功地應用於 擯體電路製程中。然而，積體電路及其製程之進一步發展 ^生了對殘留物移除組成物及方法進行改善之需求.。 積體電路工業諸如次微米尺寸裝置之製造中持續要求 縮小臨界尺寸，故蝕刻殘留物淸除及基質與潤溼處理所使 用之化學品之相容性，對於在極大型積合（V L S I )及 超大型積合（ULSI)過程中得到可接受之產量而言， 愈趨重要。該蝕刻殘留物之組成物通常係由經蝕刻之基質 '底層基質、光阻及蝕刻氣體所谢成。該晶圓之基質與潤 溼化學品之相容性與多矽之處理、多階互連介電層及晶圓 之薄膜沉積、蝕刻及後續蝕刻-此等製程經常彼此差異極 大-中之金屬化極具關連。前述組成物中有些於特定金屬 或絕綠體基質上產生腐蝕，諸如包括鈦金屬層。鈦已更廣 泛地使用於半導體製造過程中。其同時充作障壁層以1 0 防止特定原子之電滲移，及於其他金屬頂層上充作抗反射 層。 發明簡述 本發明之目的係提供一種用以淸除殘留物之改良組成 物，及符合現在半導體製造需求而使用該組成物之方法。 i紙ift尺度適刑中國國家標準（CNS ) 柏（210X 297公身)~7〇1 一 ‘ (锦先閱讀背而之注意事項#填转本頁)
416984 A7 B7 五、發明説明（4 ) 本發明另一個目的係提供一種適於自晶圓及其他基質 包括一或多層鈦金屬層淸除殘留物，而實質上不攻擊該鈦 ®之組成物及方法。 ·，. / 此等及相關目的可使用本發明所揭示之該殘留物淸除 組成物及方法達成。本發明之殘留物淸除組成物包含乙二 胺四乙酸或其單— ' 二-、三一或四—銨鹽，及水或極性 有機溶劑。本發明自基質淸除殘留物之方法包括使該基質 與含有乙二胺四乙酸或其單一、二一、三一或四一銨鹽之 組成物接觸，時間及溫度足以自該基質淸除殘留物。當使 用酸形式之乙二胺四乙酸時，可單獨用爲主要活性成份或 與氨結合而於原位形成銨鹽。 實際上，吾人發現使用乙二胺四乙酸或其單一、二— 、三-或四-銨鹽產生攻擊钛之;情況較先前組成物低例如 至少約3倍之殘留物淸除組成物》同時，含乙二胺四乙酸 或其單一、二三一或四—銨鹽之組成物產生殘留物淸 除性能至少等於先前技藝淸除組成物之殘留物清除組成物 0 熟習此技藝者參照附圖復閱以下本發明詳述後》可達 到前述及相關目的、優點及特色，其中： 發明詳述
適用於本發明之乙二胺四乙酸（EDTA)或其單一 '二-、三-或四-銨鹽以具有相對高之分解溫度爲佳。 該E D T A鹽之較佳較高分解溫度特例包括二銨E D T A ^1張尺^用中國國家榇率（CNS ) Λ小規輅（210 X 297公J： ) - 7 - — V I - (#先間讀背而之注意事項本頁) 象 i i rn * 訂 經濟部中央#準扃另工消费合作社印製 416984 A7 ____B7 五、發明説明（5 ) 及四銨E D Τ A。 組成物期望含有至少約1至5 ◦重量百分比之至少一 種乙二胺四乙酸或其單一、二一、三—或四—銨鹽；選擇 性之由約2 5至約7 5重量百分比之一或多種胺或錠醇胺 ;選擇性之由約2 5至約7 5重量百分比之有機極性溶劑 ;選擇性之由約0 . 1 5至約1 〇重量百分比之有機或無 機銨鹽；選擇性之由約5至約2 5重量百分比之其他鉗合 劑，諸如苯鄰二酚或桔酸；及由約2 5至約7 5重量百分 比之水（例如乙二胺四乙酸或其銨鹽之一部分）。使用酸 彫式之乙二胺四乙酸時，該組成物可選擇性地含有由約1 至約1 0重量百分比之氨。 " 乙二胺四乙酸（EDTA)係爲世界上最廣泛使用之 鉗合劑。其銨鹽可溶於水及大部〈分有機溶劑，因有額外之 銨鉗合部位故應爲較E D Τ A強之鉗合劑。此等有機銨鹽 係爲供以銨爲主之積體電路淸除調配物使用之良好起始化 學品。 . 適於該組成物之胺包括乙二胺、二（伸乙基）三胺、 2 -亞甲基胺基伸丙二胺等。 適於該組成物之烷醇胺實例包括單乙醇胺、二乙醇胺 、三乙醇胺、第三丁基二乙醇胺、異丙基丙醇胺、二異丙 基丙醇胺（2 —胺基一 1 —丙醇、1 _胺基一 2 -丙醇） 、三異丙基丙醇胺、3 -胺基_ 1 _丙醇、異丁醇胺、2 一（2 —胺鉴乙氧基）乙醇（二甘醇胺）、2 -胺基—2 一乙氧基丙醇、甲基乙醇胺、N，N _二（伸乙基）羥胺 本紙張尺度適用中國國家標準（CNS ) Λ4規S ( 2丨0X 297公，攀) (請先閱讀背而之注意事項再填艿本茛) ;裝· 、·ιτ 經濟部中央棕準局貝工消费合作社印製 經濟部中央標"-局負工消货合作社印製 416984 A二 137 _____ 五、發明説明（6 ) 等。 除水以外之適用於組成物之極性溶劑的實例包括二甲 基亞砸、乙二醇、乙二醇烷醚 '二（乙二醇）烷醚 '三（ 乙二醇）烷醚、丙二醇、丙二醇烷醚、N —經取代批咯啉 酮、磺雜環戊烷（sulfolane )、二甲基乙醯胺等。本發明組 成物亦可使用其他技藝界已知之極性溶劑s 適用於該組成物之敍鹽實例除E D T A外另外包括有 機銨鹽、諸如酒石酸銨、檸檬酸銨、甲酸銨、葡糖酸銨； 無機銨鹽，諸如氟化銨、硝酸銨、硫代硫酸銨、過硫酸銨 、碳酸氫銨、磷酸銨等。 本發明組成物之殘留物淸除組成物可自各種積體電路 矽晶圓基質淸除有機金屬及金屬氧化物殘留物，該基質包 括金屬層諸如鋁或鈦，氧化物層:u，諸如矽氧化物，氮化物 層，諸如氮化矽等。本發明淸除組成物亦可在積體電路製 程中移除於所用蝕刻裝置之基質上所產生之有機金屬及金 屬氧化物殘留物。市售蝕刻裝置之實例包括Lam Research， legal, Electrotech, Applied Material, Tokyo Electron, Hitachi等 ° 使用本發明淸除組成物淸除基質之方法包括使其上層 具有有機金屬及金屬氧化物殘留物之基質與本發明之剝除 及淸除組成物接觸，時間及溫度係足以移除該殘留物。該 基質通常浸漬於該剝除及淸除組成物中。時間及溫度係根 據欲自基質移除之特定材料決定。溫度通常係介於約室溫 至約1 2 0 °C之範圍內，而接觸時間係由約2至6 〇分鐘 — _. . ____ 本紙張尺度適用中國國家標準（CNS ) Λ4规格（210Χ2<Γ/公# ) - 9 - ' ^ - - - — (請先閱讀背面之注意事項再填寫本頁)
經濟部中央標率局員工消费合作社印製 416984 B7 ___ 五、發明説明（7 ) 〇 該基質可使用極性溶劑諸如異丙醇淋洗’之後以去離 子水淋洗。該基質經機械乾燥，諸如旋轉乾燥器’或吹氮 乾燥。 . 下文係爲非限制實施例，進一步描述本發明。 下表I列出適於自基質移除抗蝕劑或其他有機殘留物之本 發明淸除組成物的實例。 (諸先閱讀背而之注意事項再填^本頁)
適 度 尺 張 纸 本 率 標 家
一.S 今 416984 A7 B7 五、發明説明（8 ) _表 1_ 淸除 EDTA或鹽 其他成份 烷醇胺 溶劑 組成物 Wi·% Wt.% Wt.% Wt.% A 17.5% ΤΑΕ 5%苯鄰二酚 60% DGA 17.5% 水 B 5% DAE 5% 12.5% HAD; 72·5% 水 5% MEA C '5% DAE 17.5% HAD; 17.5% 水 60% DGA; D 5% EDTA 15% HAD; 15% 水， 10% DHA 55% DMSO E 5% DAE 15% HAD; 15% 水， f ! i 10% DHA 55% DMSO F : 5% DAE 20% HAD; 20% 水， 55% DMSO G 5% TAE 20% HAD; 20% 水； 55% DMAC Η 13% EDTA 5%苯鄰二酚 60% DGA 19% 水 (請先閱讀背而之注意事項#填耗本頁) 經濟部中央標準局負工消费合作社印裂 3% NH3 (28-30%水溶液） 縮寫：
E D 丁 A =乙二胺四乙酸 D A E = —鏡 EDTA TAE =四銨 EDTA 本紙張尺度適用中國國家標準（CNS ) Λ4規梠（210 X 297公# ) -11- 經濟部中央標準局貝工消费合作社印製 416984 五、發明説明（9 ) DGA=二甘醇胺 H D A =羥基胺 Μ E A =單乙醇胺 D I MS〇=二甲基亞砸 DMA C =二甲基乙醯胺 DHA = N，N —二（伸乙基）羥胺 前述組成物使用以下實驗方法。視該化學品爲標準物 質。於室溫下攪拌該混合物直至得到澄淸溶液以製備該溶 液。某些情況需加熱以加速固體成份之溶劑化。 具有 T i N/A 1 — C u/T i /T i N/T i 或 T i N/A 1 _Cu — S i/T i堆疊物之灰化通孔、未 灰化晶圓及金屬晶圓於4 5 °C、广5 5 °C及6 5 °C下於此等 所製備之淸除溶液中處理3 0分鐘，視調配物之性質而定 。該晶圓於此等不同淸除溶液中處理之前及之後製成碎片 ，之後於FE Hitachi 4500掃描式電子顯微鏡觀察於通孔中 之後續灰分殘留物移除及於金屬堆疊物上之基質相容性。 實施例1 二氧化矽介電層中1 . 2微米之通孔使用標準二氧化 矽電漿蝕刻法經由光阻圖型開口蝕刻。氧電漿灰化移除光 阻。圖1 A係爲此實施例所用之代表性基質之掃描式電子 顯微鏡（S E Μ )影像之顯微相片，顯示殘留於基質表面 上之濃厚有機金屬蝕刻殘留物，尤其是通孔開口周圍。該 本紙张尺度適闱中國國家標举（CNS ) 現格（210X297公身）-12 - (讀先閲讀背而之注意事項两填寫本頁)
經濟部t央標準局κ Η消费合作社印製 416984 : 五、發明説明（10 ) 基質於5 5 °C下於組成物A中處理3 0分鐘。圖1 B —形 成之S E Μ相片-顯示組成物A移除所有有機金屬殘留物 〇 實施例2 此實施例顯示組成物A不攻擊鈦金屬部分。具有 丁 i N/A 1 -C u/T i/T i N/T i 金屬部分之夾 層金屬薄膜基質形成圖型，於電漿金屬蝕刻器中蝕刻。圖 2 A顯示在以氧電漿灰化移除光阻後，金屬線路表面留有 有機金屬殘留物。該晶圓於5 5 °C下曝於組成物A歷經 3 ◦分鐘，實質上完全移除有機金屬殘留物而不攻擊鈦金 屬部分，如圖2 B所示。 lr
I 實施例3 使用組成物B重複實施例1及2之方法’但淸除溫度 係爲4 5°C 圖3A及3 B顯示所得結果。由圖3A之目 測法得到灰化通孔晶圓約有9 0 %淸除度。此情況不腐蝕 金屬，或僅開始攻擊底層鋁金屬部分。圖3 B顯示完全淸 除 T i N/A 1 — Cu/T i/T i N/T i 堆疊物晶圓 ’而實質上不腐蝕金屬，或僅開始攻擊堆疊金屬中之鋁層 實施例4 使用組成物C重複實施例3之方法’淸除溫度亦爲 本紙张尺度適用中國國家標準（CNS > Μ規格（UO X 297公身.）-1 3 - (請先閱讀背而之注意事項#填寫本頁)
經濟部+央標準局負工消费合作社印製 416984 A7 _B7 __ 五、發明説明（11 ) 4 5 t：。圖4 A及4 B顯示所得結果。由圖4 A之目測法 發現灰化通孔晶圓完全淸除。此情況完全控制金屬腐蝕。 圖4B顯示完全淸除T i N/A 1 — Cu/T i/T i N / T i堆疊物晶圓，如頂層T i N層之淸潔外觀所示，而 不腐蝕金屬。 實施例5 使用組成物D重複實施例3之方法，但淸除溫度係爲 65°C。圖5A、5B及5C顯示所得結果。由圖5A之 目測法得到灰化通孔晶圓約有9 0 %淸除度。此情況不腐 蝕金屬。圖5 B顯示幾乎完全淸除未灰化通孔晶圓之殘留 物，僅於通孔底部留有某些殘留物。圖5 C顯示完全淸除 TiN/Al-Cu/Ti / TVi N/Ti 堆疊物晶圓， 而實質上不腐蝕金屬。 實施例6 使用組成物E重複實施例5之方法。圖6A、6B及 6 C顯示所得結果。由圖6 A之目測法顯示完全淸除灰化 通孔晶圓之表面及側壁，僅於通孔底部留有某些殘留物。 此情況不腐蝕金屬。圖6 B顯示完全淸除未灰化晶圓之通 孔之表面及側壁之殘留物，僅於通孔底部留有某些殘留物 ，而不腐蝕金屬。圖6 C顯示完全淸除T i N/A 1 -C u — S i / T i堆疊物晶圓。 本紙張尺度適用中國國家標準（CNS ) Λ4規柏（210X297公專）_ 14 - (請先閱^背面^注意事項#填寫本頁)
A7 137 經 濟 部 中 央 標 消 合 社 印 % 416984 五、發明説明（12 ) 實施例7 使用組成物F重複實施例5之方法。圖7 A、7 B及 7 C顯示所得結果。由圖7 A之目測法顯示未完全淸除灰 化通孔晶圓之通孔側壁及底部。此情況不腐蝕金屬。圖 7 B顯示完全淸除未灰化晶圓上之2 5殘留物，僅有少許 鋁被切除。圖7C顯示完全淸除T i N/A 1 — Cu/ T i/T i Ν/Τ ί堆疊物晶圓，而不腐蝕金屬。 實施例8 使用組成物G重複實施例5之方法。圖8 A、8 Β及 8 C顯示所得結果。由圖8 A之目測法顯示完全淸除灰化 通孔晶圓之表面及側壁，僅於通孔底部留有某些殘留物。 此情況不腐蝕金屬。圖8 B顯示!:完全淸除未灰化晶圓之通 孔之表面及側壁之殘留物，僅於通孔底部留有某些殘留物 ，而不腐蝕金屬。圖8 c顯示完全淸除T i N/A i — C u/T i /T i N/T i堆疊物晶圓而實質上不腐蝕金 屬，或僅開始腐蝕鈦。 實施例9 使用組成物Η於三種不同晶圓上重複實施例1之方法 。混合組成物Η時，產生大量1 0熱量，顯示根據下式於 原位形成四銨E D T A : EDTA + 4NH3 · H2〇-> (NH3) 4EDTA + 4 Η 2 Ο 本紙張尺度適用中國國家標準（cns ) Λ4規格（210Χ 297公，.祭）-15 - ’•.1 (請先閱1S'·背面之注意事項再填葙本頁)
I 416334 A7 B7 五、發明説明（13 ) 圖9 A、9 B及9 C顯示所得結果。由圖9 A之目測法顯 示灰化通孔晶圓僅有約8 0%之淸除度。圖9 B顯示完全 淸除 T i N + /A 1 — C u/T i/T i N/T i 堆疊物晶 圓，而實質不腐蝕鋁或鈦層。圖9 C顯示完全清除T i /
A 1 - C u - S T〖N堆疊物而實質上不腐蝕鋁或鈦 熟習此技藝者現在應已努瞭可達成本發明所提及之目 的之新穎組成物及方法。本發明以乙二胺四乙酸或其單一 、二一 ' 三一 ' 或四銨鹽爲主之改良組成物及使用該組成 物之方法可符合目前半導體製程之要求。該組成物及方法 適於自晶圓及其他基質包括一或多層金屬層移除光砠殘留 物及其他殘留物 > 而實質上不攻擊該鈦層^ 熟習此技藝夸應進一步明瞭〈可針對本發明之形式及細 節進行各種改變。而此等改變應包括於本發明之精神及範 圍中。 ’ (請先閲請背而之注意事項#填tir本頁) 丁 •=9 經濟部令央標準局員工消资合作社印^ 附^簡述 圖1 A至係爲掃描式電子顯微鏡（s EM)相片 ，顯示使用本發明組成物及方法所達成之對照結果❶ iri 本紙掁尺度適用中國國家梯準（CNS ) Λ4現核（2IOX 297公蝮）-16 - ’:.1,

Claims (1)

  1. 3公告 ί Αδ ί Β8 i C8 D8 416084 —-一··—、 二----—ί 六、申請專利範圍 附件一： 第87 1043 87號專利申請案 y 中文申請專利範圍修正本 民國88年12月修正 1·一種自基質淸除光阻或其他聚合物材料或殘留物 之組成物，其包含至少1至5 0重量百分比之至少一種乙 二胺四乙酸或其單_、二~、三一或四銨鹽與水或極性有 機溶劑。 2 ·如申請專利範圍第1項之自基質淸除光阻或其他 聚合物材料或殘留物之組成物，其另外包含由2 5至7 5 重量百分比之胺或烷醇胺。 3 ·如申請專利範圍第1項之自基質淸除光阻或其他 聚合物材料或殘留物之組成物，其另外包含由〇 . 1 5至 1 0重量百分比之有機或無機銨鹽。 4·如申請專利範圍第1項之自基質淸除光阻或其他 聚合物材料或殘留物之組成物，其中該銨鹽係於組成物中 由氨與乙二胺四乙酸形成。 經濟部智慧財產局M3：工消费合作社印製 (請先閱讀背面之注意事項再填寫本頁) 線3- 5 _如申請專利範圍第1項之自基質淸除光阻或其他 聚合物材料或殘留物之組成物，其另外包含由5至2 5重 量百分比之其他鉗合劑。 6 .如申請專利範圍第5項之自基質淸除光阻或其他 聚合物材料或殘留物之組成物，其中該鉗合劑係爲苯鄰二 酚或掊酸。 7.—種自基質淸除光阻或其他聚合物材料或殘留物 本纸張叉度適用中國國家標準（CNS)A4规格（210 X 297公笼） 震D8 4169S4- 六、申請專利範圍 之方法’其包括使該基質與至少一種乙二胺四乙酸或其單 —、二_、三—或四銨鹽接觸，時間及溫度係足以自該基 質淸除該光阻、其他聚合物材料或殘留物。 8 _如申請專利範圍第7項之方法，其中該時間係由 2分鐘至6 0分鐘，而溫度係爲2 0至1 1 0攝氏度數。 9 ·如申請專利範圍第7項之方法，其另外包括同時 使該基質與胺或烷醇胺接觸。 1 0 ·如申請專利範圍第7項之方法，其另外包括同 時使該基質與有機或無機銨鹽接觸。 1 1 ·如申請專利範圍第7項之方法，其中該銨鹽係 由乙二胺四乙酸與氨形成。 1 2 .如申請專利範圍第7項之方法，其另外包括同 時使該基質與其他鉗合劑接觸。 13 .如申請專利範圍第12項之方法，其中該鉗合 劑係爲苯鄰二酚或掊酸。 1 4 .如申請專利範圍第7項之方法，其中該基質包 括鈦。 1 5 .如申請專利範圍第1 4項之方法，其中該鈦基 質包括積體電路之鈦層。 — — — — — — · - I ® (請先閱讀背面之注音W事項再填寫本頁) 訂---..------線· 經濟邹智慧財產局員工消费合作枝印製 本纸張义度適用中國國家標準（CNS)A‘l規格（210 x 297公釐） -2-
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US6492311B2 (en) 2002-12-10
WO1998045399A1 (en) 1998-10-15
US20010006936A1 (en) 2001-07-05
KR20010006024A (ko) 2001-01-15
JP2001526836A (ja) 2001-12-18
ATE340243T1 (de) 2006-10-15
EP0975731A4 (en) 2001-02-07
SG120055A1 (en) 2006-03-28
EP0975731A1 (en) 2000-02-02
JP4138891B2 (ja) 2008-08-27
EP0975731B1 (en) 2006-09-20
US6367486B1 (en) 2002-04-09

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