TWI283705B - Lactam compositions for cleaning organic and plasma etched residues for semiconductor devices - Google Patents
Lactam compositions for cleaning organic and plasma etched residues for semiconductor devices Download PDFInfo
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- TWI283705B TWI283705B TW094103865A TW94103865A TWI283705B TW I283705 B TWI283705 B TW I283705B TW 094103865 A TW094103865 A TW 094103865A TW 94103865 A TW94103865 A TW 94103865A TW I283705 B TWI283705 B TW I283705B
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- 150000003951 lactams Chemical class 0.000 title abstract 2
- 238000004140 cleaning Methods 0.000 title description 63
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- 238000000034 method Methods 0.000 claims abstract description 32
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- -1 amine carboxylate Chemical class 0.000 claims description 20
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- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 235000010233 benzoic acid Nutrition 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- KDYFGRWQOYBRFD-NUQCWPJISA-N butanedioic acid Chemical compound O[14C](=O)CC[14C](O)=O KDYFGRWQOYBRFD-NUQCWPJISA-N 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 125000002091 cationic group Chemical group 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 159000000006 cesium salts Chemical class 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- OEYIOHPDSNJKLS-UHFFFAOYSA-N choline Chemical compound C[N+](C)(C)CCO OEYIOHPDSNJKLS-UHFFFAOYSA-N 0.000 description 1
- 229960001231 choline Drugs 0.000 description 1
- 235000015165 citric acid Nutrition 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 150000001924 cycloalkanes Chemical class 0.000 description 1
- 125000000113 cyclohexyl group Chemical group [H]C1([H])C([H])([H])C([H])([H])C([H])(*)C([H])([H])C1([H])[H] 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- VAYGXNSJCAHWJZ-UHFFFAOYSA-N dimethyl sulfate Chemical compound COS(=O)(=O)OC VAYGXNSJCAHWJZ-UHFFFAOYSA-N 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000002255 enzymatic effect Effects 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- FRUHKPFGFOXNQJ-UHFFFAOYSA-N ethyl 2-(3-ethoxy-6-oxoxanthen-9-yl)benzoate Chemical compound CCOC(=O)C1=CC=CC=C1C1=C2C=CC(=O)C=C2OC2=CC(OCC)=CC=C21 FRUHKPFGFOXNQJ-UHFFFAOYSA-N 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000013020 final formulation Substances 0.000 description 1
- 235000019253 formic acid Nutrition 0.000 description 1
- 230000006870 function Effects 0.000 description 1
- 238000002309 gasification Methods 0.000 description 1
- 229910052732 germanium Inorganic materials 0.000 description 1
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 description 1
- 239000000174 gluconic acid Substances 0.000 description 1
- 235000012208 gluconic acid Nutrition 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 150000004820 halides Chemical class 0.000 description 1
- 229910000040 hydrogen fluoride Inorganic materials 0.000 description 1
- 230000005661 hydrophobic surface Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 150000002484 inorganic compounds Chemical class 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 description 1
- 239000011976 maleic acid Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 229910001092 metal group alloy Inorganic materials 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 229910044991 metal oxide Chemical group 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 150000007522 mineralic acids Chemical class 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- HDZGCSFEDULWCS-UHFFFAOYSA-N monomethylhydrazine Chemical compound CNN HDZGCSFEDULWCS-UHFFFAOYSA-N 0.000 description 1
- 230000003472 neutralizing effect Effects 0.000 description 1
- 150000002823 nitrates Chemical class 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 125000002524 organometallic group Chemical group 0.000 description 1
- 235000006408 oxalic acid Nutrition 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 description 1
- 229940112042 peripherally acting choline derivative muscle relaxants Drugs 0.000 description 1
- 150000002989 phenols Chemical class 0.000 description 1
- DAVIFOGMMPLOJQ-UHFFFAOYSA-N piperidine-4,4-dithiol Chemical compound SC1(CCNCC1)S DAVIFOGMMPLOJQ-UHFFFAOYSA-N 0.000 description 1
- 238000001020 plasma etching Methods 0.000 description 1
- 239000003495 polar organic solvent Substances 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 229920000052 poly(p-xylylene) Polymers 0.000 description 1
- 229920001721 polyimide Polymers 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 239000005373 porous glass Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 235000019260 propionic acid Nutrition 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 125000001453 quaternary ammonium group Chemical group 0.000 description 1
- 150000003242 quaternary ammonium salts Chemical class 0.000 description 1
- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 description 1
- 150000003248 quinolines Chemical class 0.000 description 1
- 150000003254 radicals Chemical class 0.000 description 1
- FTIMWVSQXCWTAW-UHFFFAOYSA-N ruthenium Chemical compound [Ru].[Ru] FTIMWVSQXCWTAW-UHFFFAOYSA-N 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 235000002906 tartaric acid Nutrition 0.000 description 1
- 239000011975 tartaric acid Substances 0.000 description 1
- SITVSCPRJNYAGV-UHFFFAOYSA-L tellurite Chemical class [O-][Te]([O-])=O SITVSCPRJNYAGV-UHFFFAOYSA-L 0.000 description 1
- 150000005622 tetraalkylammonium hydroxides Chemical class 0.000 description 1
- 239000010891 toxic waste Substances 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- 238000002525 ultrasonication Methods 0.000 description 1
- 238000009834 vaporization Methods 0.000 description 1
- 230000008016 vaporization Effects 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/16—Organic compounds
- C11D3/26—Organic compounds containing nitrogen
- C11D3/33—Amino carboxylic acids
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02041—Cleaning
- H01L21/02057—Cleaning during device manufacture
- H01L21/02068—Cleaning during device manufacture during, before or after processing of conductive layers, e.g. polysilicon or amorphous silicon layers
- H01L21/02071—Cleaning during device manufacture during, before or after processing of conductive layers, e.g. polysilicon or amorphous silicon layers the processing being a delineation, e.g. RIE, of conductive layers
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
- C11D7/22—Organic compounds
- C11D7/26—Organic compounds containing oxygen
- C11D7/261—Alcohols; Phenols
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
- C11D7/22—Organic compounds
- C11D7/28—Organic compounds containing halogen
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
- C11D7/22—Organic compounds
- C11D7/32—Organic compounds containing nitrogen
- C11D7/3281—Heterocyclic compounds
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
- C11D7/22—Organic compounds
- C11D7/34—Organic compounds containing sulfur
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
- C11D7/50—Solvents
- C11D7/5004—Organic solvents
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D2111/00—Cleaning compositions characterised by the objects to be cleaned; Cleaning compositions characterised by non-standard cleaning or washing processes
- C11D2111/10—Objects to be cleaned
- C11D2111/14—Hard surfaces
- C11D2111/22—Electronic devices, e.g. PCBs or semiconductors
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Physics & Mathematics (AREA)
- Computer Hardware Design (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Health & Medical Sciences (AREA)
- Emergency Medicine (AREA)
- Detergent Compositions (AREA)
- Cleaning Or Drying Semiconductors (AREA)
- Drying Of Semiconductors (AREA)
- Exposure Of Semiconductors, Excluding Electron Or Ion Beam Exposure (AREA)
Description
1283705 九、發明說明: 【發明所屬之技術領域】
本發明係關於對於清洗半導體機材之有機及無機化合物 或聚合物(後#刻殘留物)特別有用之半水性清洗組合物。至 於此處所用之”半水性”一詞係指晶圓極有機溶劑之混合 物。本發明亦包含使用該組合物清洗半導體機材之殘留物 之方法。更特別的是,本發明敘述半水性清洗組合物及其 用法。溶液為部含或含it化物化合物、水及可視情況含腐 I虫抑制劑、螯合劑、界面活性劑、酸及驗之溶劑之有機錄 化合物或胺羧酸酯化合物。 【先前技術】 半導體工業中使用含氟化物之化學品清洗原始矽晶圓 (尚未經離子植入或設備建構之晶圓)已數年。通常氟化物化 學品(經常為稀釋之氫氟酸)係用作後續稱之為’’RCA洗滌” 中之最終製程步驟中。基材通常受先前製程中單層量之金 屬、因離子及/或有機污染物或表面殘留物(顆粒)之污染。 此等污染物已顯示對簡單試驗設備構造之電整合性會有明 顯的衝擊,且因此需在部損及其整合性之下有效的清洗。 此清洗方法可包含技術文獻,例如1991 _ Int. Conf. On Solid State Devices.and Materials,第 484-486頁,或 1996·之Kujime Τ·等人之 Semi.Pure Water and Chemicals,第 245-256頁,及 1995年 8月 Singer,Ρ·之 Semi. International,第 88 頁中討論 之技術。 教示以低pH值溶液清洗基礎晶圓之方法之專利包含美國 O:\99\99339.DOC -6- 1283705 專利第 5,560,857 及 5,645,737 ; 5,181,985 ; 5,603,849 ; 5,705,089 〇
用於最終RCA清洗步驟中之氟化物化學品(經常為HF)會 造成撥水疏水態(表面以Si-H基覆蓋)之石夕晶圓表面。該清洗 步驟過程中,會使某些比例之晶圓表面溶解(移除)。除非小 心地偵測清洗條件(時間、溫度、溶液組合物),否則可能會 傷及基材,如 1997. Rafols,C·等人在 J· Elec troanalytic C hem-433 , 第 77-83頁中 所述。 許多組合物均 結合水及有機 溶劑。 此等HF溶液中之水濃度非常的有限。如1998.8/5-7,史丹佛 大學 NSF/SRC Eng. Res. Center,Environmentally Benign Semiconductor Manufacturing,中之紀錄,氧化石夕氧化物在 HF/水中蝕刻速率為21埃/分鐘(@25°C ),但在異丁醇中之速 率降至2.14埃/分鐘,且在丙酮(aprotic solvent)最低,其速 率僅0.12埃/分鐘。 流線前端(FEOL)清洗製程之後,晶圓進行半導體設備之 一般流線後端(BEOL)之製造製程,其中之設備可為動態無 規存取記憶體(DRAMs),靜態無規存取記憶體(SRAMs), 僅可邏輯電可程式讀取之記憶體(EPROMs),矽上之補償金 屬(CMOS),等。使用化學反應之蝕刻製造技術(液體或電 漿)均曾用作在該半導體基材上形成價現構造之方法。 將光組劑薄膜沉積在晶圓上形成光罩,接著使基材設計 在薄膜層上呈像、烘烤,且以光組劑清洗劑移除未顯像之 圖像。留下之圖像再以以電漿能量提昇之反應性蝕刻氣體 轉移到底層材料(電介質或金屬)上。蝕科技氣體選擇性的侵 O:\99\99339.DOC -7- 1283705 • 餘基材之未經保護區。液態#刻化學品(經常含氟化物之化 學品)已經廣泛的使用於蝕刻金屬(A1)及電介質數年。氣化 物化學品極強烈,且會導致is〇tr〇piC姓刻(所有方向均同等 的餘刻)。對於今曰嚴密之尺寸控制需求,並無法忍受 Isotropic蝕刻之影響,雖然已經經由統計學上之製程控制技 術¥咸的控制isotropic姓刻,如Taylor,D”於1998年7月 Solid State Technology,第 119頁中所述。 g 常用之電漿蝕刻製程包含各相異性(單向)蝕刻,同時副 產物(包含光組劑、蝕刻氣體以及蝕刻之材料)以殘留物沉積 在蝕刻開口之側壁上。 該保護性侧壁沉積物形成之缺點微在蝕刻步驟後要移除 . 沉積物相當的困難。若此等沉積物中之成分以某些方式移 除或中和’則殘留物將會吸收水氣,且性成會腐餘金屬構 造之酸性物質。所得之酸腐蝕架線材料,且產生副作用, 如增加電阻抗及亂之中斷。此問題經常會發生,尤其是一 鲁純用紹及銘合金當作架線材料時。若未控制,則晶圓基 材與酸性材料接觸可能破壞金屬結構。 依據蝕刻操作’光組光罩需自經保護之表面移除,以完 成操作。期望上能發展一種改良之氮係組合物,以便在不 使金屬電路受損、溶解或光澤消失下或化學性的改變晶圓 基材下’自經塗覆之無機基材上移除有機聚合物物質。 . 用於移除尚未灰化之光阻劑塗料或其他基材之清洗組合 ,物大部份均為高度可燃,且對人類及環境通常有害,且包 括呈現不期望之毒性之反應性溶劑混合物。再者,此等清
O:\99\99339.DOC 1283705 洗組合物不僅有毒,而且由於需當作有毒廢棄物處理,因 此處理費用高。另彳,此等組合㈣其❹時間—般有嚴 格之限制’ 大部份均無法再回收或再利用。 侧壁殘留物以酸性有機溶劑或驗性有機溶劑移除。酸性 溶::般包含酚化合物或氯溶劑,及/或芳香系烴,及/或烷 基本石買酸。此等之調配物一般需在溫度達到或超過⑺代下 使用。此等化學品一般需以異丙醇洗滌。 稀釋之氫氟酸溶液可在特定之條件下,藉由強烈的侵蝕 電介質之側壁,移除側壁之聚合物,因此會改變裝置之尺 寸(如 Ireland,P.,在 Thin Solid Films,3〇4, pp M2 (1997)中 所教示者),且可能改變介電常數。先前含1^、硝酸、水及 羥基胺之化學品夠強至足以蝕刻矽,如授與A· 之美 國專利第3,592,773號中教示者。最近之資料亦顯示烯册溶 液對於清洗較新之CFx蝕刻殘留物可能無效,如K· Uen〇等 人在以稀釋氫氟酸溶液清洗CHF3電漿姓刻之Si〇2/siN/Cu 構造”J· Electrochem· Soc·,ν〇1· 144,(7) 1997 中之教示。開 在TiSi2上之接觸孔亦不容易以hf溶液清洗,因為其明顯的 在 TiSi2 層之下。如 Baklanov,M.R.等人在 Proc_ Electrochem Soc·,1998, 97-3 5, ρρ· 602-609.中之教示,化學品在狹窄親 水性接觸孔中大量的輸送可能亦相當困難。 一般層間之電介質、TEOS(四乙基原矽酸鹽)及磷矽酸硼 玻璃(BPSG)(其一般係用於步驟涵蓋之較佳順服性用之超 大型機體(ULSI)構造)之接觸孔四週之光阻劑通常係以hf 溶液移除。HF亦侵蝕電介質材料通常並不尋常。該侵蝕並 O:\99\99339.DOC -9- 1283705 • 非期望者(見 Lee,C.及 Lee,S,Solid State Electronics,4, PP, 921-923 (1997)) 〇 後14刻殘留物移除用之鹼性有機溶劑可包含胺及/或烷 醇胺及/或中和之有機溶劑。此等調配物通常需在溫度超過 . i〇0°c下使用。最近已使用一種新形後蝕刻殘留物清洗化學 品以移除此等基材。此等化學品包含羥基胺、胺、烷醇胺、 及腐蝕抑制劑,且一般係在比溫度低2〇至3〇度下操作。 % 最近,在有限之情況中已使用以氟為主之化學品,以移 除後蝕刻殘留物,且程度有限的在BE〇L(Back End 〇f Une) 製程過程中,自積體電路基材上移除光阻劑殘留物。許多 晶圓清洗組合物含氟化物成分,尤其是氟化氫。除此等組 • 合物可能含強的鹼性化學品(膽鹼衍生物,四烷基氫氧化 銨,氫氧化銨),如美國專利第5,129,955、5,563,119、或 5,571,447號中之揭示,或可使用兩相溶劑系統,其含有具 氫氟酸及水之相,且第二相含非極性有機溶劑(酮、醚、烷 • 或烯)(美國專利第5,603,849號)。其他調配物包含羥基胺及 氟化銨(授與Ward之美國專利第5,709,756)。其他實例包含 季銨鹽及以氟化物為主之組合物,如公開之歐洲申請 0662705號中揭*,及有機緩酸錄鹽或緩酸胺及以氣化物為 主之組合物,如美國專利第5,63〇,9〇4號中揭示。 部分化學品亦包含螯合劑,以便自晶圓表面移除離子性 或非離子性污物(PCT US98/02794),但螯合劑如檸檬酸、 鎵酸、及苯鄰二酚對涵蓋鋁金屬線之氧化鋁為強烈者。 . 0hman及Sjoberg之研究顯示檸檬酸離子之強的錯合化能力
O:\99\99339.DOC -10- 1283705 可增加氧化鋁之溶解度,且因此在PH5至6下,以166至468 之因子’使金屬曝露而進一步腐蚀(見〇hman等人之j. chem.
Soe,Dalton Trans. (1983),ρ·2513)。 清洗晶圓上之金屬及金屬氧化物殘留物之其他方法包含 將水蒸氣喷佈入電漿灰化室中,接著導入含氟之氣體(氫氟 酸)(美國專利第5,181,985號),或含氫氟酸、氟化銨、及水, 且pH值在1.5至低於7之間之液體。
在BEOL製程過程中亦需自晶圓表面移除粒狀殘留物。通 常大部分之製程均在超音波或megasonic清洗下,依賴異丙 醇及/或DI水潤濕清洗。對於氧化物晶圓表面之化學機械拋 光(CMP)清洗,一般僅使用01水,但對於鎢晶圓,經常需 要結合稀NH4OH及稀HF。 自晶圓表面移除雜質(顆粒或離子)之機構有五項: 1 ·以溶劑物理性的解吸附,其包含以大積之弱吸收溶劑 取代小量之強吸收顆粒(改變表面電荷之作用); 2·以酸或鹼改變表面電荷,及Si_〇H基可以以酸變成正電 或質子化,或藉由移除質子,以鹼變成負極; 3.藉由添鎵酸移除吸收之金屬離子使離子錯合化,· 4·雜質氧化或分解(包含使金屬、有機材料漿料顆粒之表 面氧化)會使雜質與基材表面間之化學力改變。化學反應可 為氧化還原或游離基; 5 ·钱刻氧化物表面,其會釋出雜質同時使一定厚度之美 材鰾面溶解。 一般所用以氟為主之化學品可以以第2項及第5項協助, O:\99\99339.DOC -11 - 1283705 但需謹慎控制其清洗條件。需多情況下,清洗組合物之成 分為相對較毒之反應性溶劑混合物,且因此使用者需在嚴 格之使用條件下使用,且須毒害化學處理步驟,及穿戴安 全衣物,以避免與清洗組合物接觸。另外,由於該清洗組 合物之許多毒性成分揮發性高,且具有高的蒸發速率,因 此在組合物儲存及使用過程中,需要特殊之人與環境安全 之預警。 據此,需要發展經改善之清洗組合物,以有效的清洗各 種基材上之各種沉積物。特別是在積體電路製造之領域 上,應了解針對改善清洗效能且避免侵蝕欲清洗之基材之 要求持續的增加。此意指適用於清洗較不複雜基電路基材 之組合物對於在製造製程中含更先進積體電路之基材可能 無法產生滿意之結果。 此等組合物亦應經濟、對環境無害且容易使用。 本發明教示此種新穎且經改善之清洗組合物,以及其使 用方法。該組合物為水性、溶解有機及無機基材,且當用 於製程中時,可清洗各種基材。該組合物提供更有效之基 材清洗’意指可更有效的移除殘留物,另外意指猶豫清洗 之基材可得到更高之製造產率。 【發明内容】 發明之簡單敘述 本發明之新穎清洗組合物在低溫下呈現使用單一成分, 或與其他清洗成分結合之成分,或與其他清洗成分結合之 成分’如乙氧基乙醇胺或院基醯胺不可能達到之協同提昇
O:\99\99339.DOC -12- 1283705 之清洗作用。 本發明之-t目的係提供一種在低溫下有效之半導體基 材清洗組合物。 /本發明之另—目的係提供—種可抑制金屬離子再沉殿之 後钱刻殘留物清洗組合物。 本發明之另一目的係性成不燃之此種清洗溶液。 本發明之另一目的係提供一種具有對氧化矽低蝕刻速率
之此種清洗溶液。 本發明之另一目的係提供此種清洗溶液以及移除後蝕刻 殘留物為主之金屬構造之方法。 本發明之另一目的係提供此種清洗溶液以及自vias移除 後鍅刻殘留物之方法。 本發明之另一目的係提供此種清洗溶液以及自低k之電 介質移除後|虫刻殘留物之方法。 此荨集相關之目的係藉由使用次處揭示之組合物及方法 達成。 依據本發明之組合物係用於清洗基材之殘留物,且不含 有機銨及胺羧酸酯。其包括約0.01重量%至約1〇重量%之一 種或多種氟化物化合物,自約20重量%至約50重量❶/。之水, 自約20重量%至約80重量。/()之内醯胺溶劑,及自約〇至約5〇 重里%之有機亞楓或二醇溶劑。該組合物之pH值在約6至約 1 〇之間。另外,該組合物可視情況含腐姓抑制劑、螯合劑、 界面活性劑、酸及鹼。 依據本發明自基材清洗殘留物之方法包括使基材與包括 O:\99\99339.DOC -13 - 1283705 一種或多種氟化物化合物、水及内醯胺溶劑之不含有機銨及 胺窥酸酯组合物,在溫度及時間均足以清洗基材之下接觸。 發明之詳細欽述 本發明之清洗組合物為不含有機銨及胺羧酸酯。藉由自 組合物去除有機銨及醯胺羧酸酯化合物達到許多優點。去 除此等化合物可降低產品之成本。有機銨及胺羧酸酯化合 物亦為一種稱之為相轉移觸媒之化合物。此等化合物在特 定溶劑條件下可不期望之副反性加速,亦即氫氧化物或鹵 化物反應之活化(其會腐蝕金屬之表面),如”工業上之相轉 移觸媒,,(實務指導及手冊,Mar· 1991,PTC Inteirface,Inc. Marietta,GA·)中所述。化學品中存在此等化合物亦會導入 額外之陽離子與陰離子污染物當作主材料源。 清洗組合物含一種或多種氟化物化合物。適當之氟化物 化合物為氟化銨,雙氟化銨及氫氟酸。較佳之氟化物化合 物為敦化銨及雙氟化銨。弱使用氫氟酸,可能需緩衝液將 其P Η值調整在約6至約丨〇之間。氟化物化合物期望之含量約 〇·〇1重里%至約1〇重量%。較好至約重量%至約5重量% 之間。通常,組合物中之氟化物化合物之濃度愈低,則使 用時所需之溫度愈高。 清洗組合物含一種或多種内醯胺溶劑。適當之内醯胺溶 劑包含具有4至7員環之内醯胺,包含1至5個碳原子烷基及 烷氧基取代之内醯胺,及5至7員環烷取代之内醯胺。内醯 胺溶劑適用之特殊實例包含哌啶酮,如1至5個碳原子烧 基、二烷基及烷氧基,二烷氧基哌啶酮,包含义甲基哌啶
O:\99\99339.DOC -14 - 1283705 酮、二甲基哌啶酮、N-曱氧基哌啶酮、二曱氧基哌啶酮、
N乙基略!1疋_、二乙基威σ定酮、二乙氧基略唆_等;此等 峰°疋_之環己基類似物,如Ν-曱基峨π各烧_、Ν-2-_美乙 基-2-吡咯烷酮、ν-2-(環己基)-2-吡咯烷酮。較佳之内醯胺 溶劑為N-曱基哌啶酮、二曱基哌啶_、及n_甲基吡咯烷酮。 二曱基哌啶酮為市售之主要為1,3_二甲基哌啶_及次要量 之1,5-二曱基喊咬酮之混合物。此内醯胺混合物可單獨或以 混合物使用。組合物可視情況含烷基亞砜,如二甲基亞諷 及/或^一酵’如丙二醇。 清洗組合物含水。一般係使用高純度去離子水。 組合物可視情況含腐蝕抑制劑。適當之腐蝕抑制劑包含 無基硝酸鹽,如硝酸銨、鉀、納及釕鹽。硝酸鋁及硝酸鋅。 組合物可視情況含螯合劑。適當之螯合劑為1997年9月3〇 曰授與Lee之美國專利第5,672,577號中敘述者,該專利在此 提出供參考。較佳之螯合劑包含兒茶酚、乙二銨四乙酸、 檸檬酸、戊二酮及戊二酮二 。 組合物可視情況含界面活性劑。適當之界面活性劑包含 聚(乙烯基醇)、聚(乙亞銨)及分類成陰離子性、陽離子性、 非離子性、兩性、及乙係為主之界面活性劑組合物。 成分之某些組合需要添加酸及/或鹼,將pH值調整至可接 受之值。本發明適用之酸為有機或無機酸。酸可包含硝酸、 硫酸、磷酸、鹽酸(雖然鹽酸會腐餘金屬),及有機酸、甲酸、 乙酸、丙酸、正-丁酸、異丁酸、苯甲酸、抗壞血酸、葡酸、 馬來酸、丙二酸、草酸、丁二酸、酒石酸、檸檬酸、鎵酸。 O:\99\99339.DOC -15- 1283705 隶後五種有機酸為螯合劑之實例 有機酸之一般構造 Ο
R—C—C-.OH
X
X=-OH,-NHR,-H,--素,-C02H,及-CH2C02H,-CHOH-C02H R=—般之脂肪系,η或芳香系 酸之濃度可在約1至約25重量%間變化。重要之因子為酸 及鹼性產物與水溶液中之任一種其他劑類之溶解度。 適用於調整清洗溶液之?11值之鹼性成分可由任一種一般 之鹼組成’即氫氧化納、鉀、鎂等。主要之問題為此等鹼 會將移動之離子導入最終之調配物中。移動之離子可能會 損壞今日半導體工業中欲製造之電腦晶片。其他之鹼可包 含膽鹼(季銨)或氫氧化銨。 操作: 使用本發明之清洗組合物清洗基材之方法包含使其上有 殘留物(特別是有機金屬或金屬氧化物殘留物)之基材與本 舍明之清洗組合物在足以移除殘留物之溫度下接觸一段時 間。可視情況使用技藝中已知之攪拌、循環、超音波或其 他技術。基材通常浸入清洗組合物中。時間及溫度之決定 係依據欲自基材上移除之特殊材料為基準。通常,溫度係 在常溫或是溫至約10(TC之間,且接觸時間係自約3〇秒至約 60分鐘之間。本發明所用之較佳溫度及接觸時間為在2〇至 O:\99\99339.DOC -16 - 1283705 45 °C下2至60分鐘。通常基材在使用此組合物之後會經洗 務。較佳之洗滌溶液為異丙醇及DI水。 本發明之組合物對於自金屬移除殘留物特別有用。
本發明之組合物對於低k之電介質特別有用。低k之電介 質為技藝中已知,且包含氟化之矽酸鹽玻璃(FSG),雜有機 矽氧烷聚合物(HOSP),多孔氧化矽(多孔玻璃)(LOSP),氫 矽半氧烷(HSQ),甲基矽半氧烷(MSQ),二乙烯基矽氧烷雙 (苯并環丁烯)(BCB),氧化矽低-k(SiLK),聚(芳烯基醚) (PAE,Flare,Parylene),及氟化聚亞醯胺(FPI)。 適於自基材移除光阻劑光罩或殘留物之本發明清洗組合 物或製成之實例列於下列實例中。 【實施方式】 實例1. 一組含氟化銨,水以及二曱基哌啶酮、乙腈、及 經基胺之一之清洗化學品以金屬晶圓作試驗,該金屬晶圓 為TEOS/Ti/TiN/AlCu/TiN(由下至上)之堆積,且以市售AMT DPS蝕刻器,以Cl1/BCli電漿蝕刻。所得具殘留物之金屬晶 圓切割成小樣品片,接著將該樣品片浸入表1中之化學溶液 中,且在室溫下清洗5分鐘。取出該樣品片,以去離子水洗 條,且以Νι流烘乾。以Hitachi 4500 FE-SEM進行SEM,以 評估其清洗及腐蝕作用。以目視比較分析金屬堆積上之殘 留物移除及腐蝕作用,且分成1至1 〇等。表1中之調配物係 以重量百分比表示。 O:\99\99339.DOC -17-
1283705 表1 時間 金屬線 配方 NH4F DI水 ACN DMP HDA (分) 清洗 A1 T1 TiN 氧化物 A 1 35 64 5 10 7 10 10 10 B 1 35 64 5 10 8 10 10 10 C 1 35 64 5 8 10 10 10 10 反應溫度:室溫 金屬線之金屬駐留 DI水:去離子水 金屬管:1-不良10-完全 ACN ··乙腈 A1旋轉:10-未改變,1-金屬切割 DMP : 1,3-二甲基哌啶酮 Ti維持:10-未改變,<5-發現腐蝕 HAD :羥基胺 TiN維持:10-未改變,<5-發現腐蝕 氧化物維持:10-未改變,<5-發現 腐蝕 結果發現含DMP之調配物可提供在鋁上稍微腐蝕形式之 最佳清洗效能與腐蝕之結合。依此基準,選擇DMP進一步 研究以提供提昇之效能。 實例2.以實例1之結果為準,評估具低氟化銻濃度之調配 物,以測定聚氟化銻與水及DMP之清洗調配物中氟化銻之 底限。以C12/BC13電漿配合市售LAM TCP9600蝕刻器蝕刻 氧化物/Ti/TiN/AlCu/TiN(由下至上)堆積金屬晶圓。所得具 殘留物之金屬晶圓切割成小樣品片,接著將該樣品片浸入 表2中之化學溶液中,且在室溫下清洗5分鐘。取出該樣品 片,以去離子水洗滌,且以N2流烘乾。以Hitachi 4500 FE-SEM進行SEM,以評估其清洗及腐蝕作用。以目視比較 分析金屬堆積上之殘留物移除及腐蝕作用,且分成1至1 〇 等。表2中之調配物係以重量百分比表示。 O:\99\99339.DOC -18- 1283705
反應溫度:室溫 金屬飨' • 1線之金屬駐留 DI水·去離子水 金θ . 戈屬官:1-不良10_穿令 DMP: U-二甲基哌啶酮A1 疋王 % 疋轉· 10-未改變,1-金屬切割 維持· 10-未改變,<5_發現腐蝕 灿維持·· 1G-未改變,<5_發現腐钱 氧化物維持未改變,<5_發現 腐名虫 此等結果顯示以含低至約〇 旦 •重里氟化録之組合物可得 到明顯的清洗結果,且沒有腐 β碼触。且以調配物中具有0.2重 量%之氟化錄濃度可得到較短之處理時間。 實例3.重複實例2之步驟,但使用含3重量%或1〇重量% I化銻’且添加丙二醇當作額外溶劑之調配物。結果示於 表3及4中。 表3 '〜— 以wt%計之調配物 配方 nh4f DI水 DMP in 時間 —*«-— 金屬線 LL 0.3 49.7 10 清洗 A1 T1 TiN 氧化物 ΜΜ 0.3 59.7 20 ~ 5 8 6 10 10 10 ΝΝ 0.3 49.7 40~ 9.5 5 10 10 10 00 0.3 79.7 10 5 8.5 4 10 10 10 ΡΡ 0.3 797 30 ιυ 48 5 1—-- 5 5 9 7 —10 10 10 QQ ΌΌ 0.3 39.7 24— 8 1 A 10 1 f\ 10 ' 10 10 10 10 10 i\Jtv SS TT 0.3 0.3 27.7 27.7 67 57 5 —H 5 5 IU 10 1 A IU 10 1 A —10 —10 10 10 1 \J 10 1Π 1 I UU 0.3 0.3 27.7 29.7 0 45~ -^. 5 lu 1 10 10 1 \J 10 10 1U 10 VV WW 0.3 0.3 29.7 29.7 25 69 A 7 7 10 10 10 10 10 10 10 10 XX 0.3 30.7 35 υ 5 —5 1 7 10 10 10 10 10 10 10 10
O:\99\99339.DOC -19- 1283705 反應溫度:室溫 DI水·去離子水 DMP · 1,3_一甲基喊唆轉 PG :丙二醇 金屬線之金屬駐留 /月洗官:10-完全1-幾乎未清洗 A1方疋轉:1〇_未改變,1-去掉A1層
Tl維持:1〇_未改變,1-去掉Ti層
TlN維持:!〇•未改變,1-去掉TiN層 氧化物維持:10-未改變,1-去掉氧 化物層
以wt%計之調配物
反應溫度:室溫 DI水:去離子水 金屬線之金屬駐留 清洗管:10-完全^幾乎未清洗 10-未改變,1-去掉A1層 10-未改變,1-去掉Ti層
DMP 1,3-二甲基喊咬_ PG :丙二醇 A1旋轉 Ti維持
TlN維持:10-未改變,1-去掉TiN層 氧化物維持:1〇-未改變,丨―去掉氧 細=了解表3及4中所示調配物所得之結果,以圖卜4之四 -仆物:圖描繪出數據,以分別顯示殘留物清洗效能與低 氣化物‘度及高氣化物濃度中水、崎㈣濃度之函數關
O:\99\99339.DOC -20- 1283705 係’圖5顯示表3中之pH與溶液中水、DMP及PG濃度之函數 關係。圖5中紀錄之pH值係以具有玻璃pH電極之〇ri〇n SA520計測量。圖1與圖2之比較顯示有時需較高之氟化物濃 度’以得到以高的水及高的DMP濃度之滿意清洗結果。圖3 及4顯示相對於水,以高濃度之dMp可得到最小之腐蝕。圖 5與圖1-4之結合顯示需以適當之pH值以避免鋁實質上之腐 姓以及得到最適之清洗結果。
實例4.如實驗操作之結果,測定之最佳組合物為〇·75%含 40重量%濃度氟化鋁之水,17重量%2DMSO(二甲基亞 職),57.25重量%2DMP(二甲基哌啶酮)及25重量%之D I.。 依據貫例2之另一試驗對於表3及4中所列之所有基材均可 提供10之腐蝕數及10之清洗數。 其他氟化物化合物、内醯胺溶劑、有機亞砜、及其他二 醇之取代物均可得到類似有利之結果。 熟習本技藝者由前述之實例將會了解到依據製造製程中 之不同條件,可進行前述清洗溶液之改良及改變。上述之 具體例係以實例說明。例如,電介質維護之特定討論係以 提出之清洗溶液及方法保護之其他金屬、金屬合金及聚矽 基材構造之指標。教示之實例並不限於以下列巾請專利範 圍界定之本發明。 本說明書中提出之所有公告及專财請案均在此處提出 供參考。 本發明已充分的說明,熟f本技藝者須了解許多的改變 及改值均不離本發明之精神或範圍。
O:\99\99339.DOC -21 -
Claims (1)
- 公告本 * I28y?⑽薦號專利申請案 中文申請專利範圍替換本(96年2月) 96. 2. 27 十、申請專利範圍·· 1 · 一種自基材上移除光阻及蝕刻殘留物及抑制金屬離子之 再澱積之不含有機銨及胺羧酸酯之水性組合物,其包含 佔該組合物重量之0.01重量%至10重量%之一或多種氟化 物化合物,佔該組合物重量之20重量%至80重量%之一不 為哌啶酮之内醯胺溶劑,佔該組合物重量之2〇重量%至50 重量%之水,及一螯合劑,其中該組合物係具介於6及10 之間之pH值。 2·根據申請專利範圍第1項之組合物,其中該光阻及蝕刻殘 留物係自含低K介電物質之基材上移除。 3·根據申請專利範圍第1或2項之組合物,其中該一或多種 氟化物化合物係佔該組合物重量之〇 〇5重量%至5重量〇/〇。 4.根據申請專利範圍第3項之組合物,其進一步包含額外溶 劑’選自有機亞砜及二醇所組成之群組。 5 ·根據申請專利範圍第3項之組合物,其中該内醯胺溶劑具 • 有4至7員環。 6_根據申請專利範圍第4項之組合物,其中該額外溶劑係有 機亞砜。 7·根據申請專利範圍第4項之組合物,其中該額外溶劑係二 醇。 8_根據申請專利範圍第3項之組合物,其中該氟化物化合物 係氟化銨或雙氟化銨。 9·根據申巧專利範圍第3項之組合物,其中該内醯胺為吡咯 1283705 炫酮。 I 〇·根據申睛專利範圍第9項之組合物,其中該吡咯烷g同為 N-2-(經基乙基)_2-吡咯烷酮或N_2(環己基)-2_吡咯烷酮。 II ·根據申睛專利範圍第9項之組合物,其中該氟化物化合物 係氟化錢、雙氟化銨或氫氟酸。 12·根據申請專利範圍第3項之組合物,其進一步包含腐蝕抑 制劑。 13 ·根據申請專利範圍第3項之組合物,其進一步包含界面活 | 性劑。 14·根據申請專利範圍第7項之組合物,其中該二醇係丙二 醇。 1 5 ·根據申請專利範圍第3項之組合物,其中該組合物不含相 轉移觸媒。 16. —種自基材上移除光阻及腐餘殘留物及抑制金屬離子之 再澱積之方法,其包含使該基材與一不含有機銨及胺羧 酸醋之水性組合物接觸,該組合物係包含佔該組合物重 験 量之0.01重量%至10重量%之一或多種氟化物化合物,佔 該組合物重量之20重量%至80重量%之一不為哌啶酮之 内醯胺溶劑,佔該組合物重量之2〇重量%至5〇重量%之 水’及一螯合劑,其中該組合物係具介於6及10之間之pH 值。 17·根據申請專利範圍第16項之方法,其中該基材有緊密澱 積於其上之低K介電材料,及該光阻及腐餘殘留物係藉由 使該低K介電材料與包含一或多種氟化物化合物、不為哌 99339-960227.doc -2- .1283705 錢之内酿胺溶劑及整合劑之不含有機敍及胺叛酸醋之 ' 水性組合物接觸而移除。 18·根據申請專利範圍第16或17項之方法,其中該一或多種 氟化物化合物係佔該組合物重量之〇 · 〇 $重量%至5重量%。 19·根據申請專利範園第18項之方法,其中該内醯胺為吡咯 烷酮。 20·根據申請專利範圍第18項之方法,其進一步包含額外溶 劑’選自有機亞風及二醇所組成之群組。 參 21·根據申請專利範圍第2〇項之方法,其中該額外溶劑係二 醇。 22.根據申請專利範圍第21項之方法,其中該二醆及 ^ 吁1糸丙二醇。99339-960227.doc ,12 g3^0^65號專利申請案 中文圖式替換頁(96年2月) 十二、圖式>6 2,27DMF050 {sse000 12 號專利申請案 中文圖式替換頁(96年2月) 96; 2/2712 號專利申請案 中文圖式替換f(%年g月) S OJDMPf—冷 蕭骑 100
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- 2000-07-17 JP JP2001519124A patent/JP2003507901A/ja active Pending
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- 2000-07-17 WO PCT/US2000/019333 patent/WO2001005524A1/en active Application Filing
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US6235693B1 (en) | 2001-05-22 |
DE60041497D1 (de) | 2009-03-19 |
EP1212150B1 (en) | 2009-01-28 |
WO2001005524A1 (en) | 2001-01-25 |
ATE421905T1 (de) | 2009-02-15 |
AU6348600A (en) | 2001-02-05 |
JP2003507901A (ja) | 2003-02-25 |
HK1047063A1 (zh) | 2003-02-07 |
KR20020031159A (ko) | 2002-04-26 |
TWI233942B (en) | 2005-06-11 |
EP1212150A4 (en) | 2003-04-02 |
TW200521222A (en) | 2005-07-01 |
EP1212150A1 (en) | 2002-06-12 |
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