TWI243861B - Formulations including a 1,3-dicarbonyl compound chelating agent and copper corrosion inhibiting agents for stripping residues from semiconductor substrates containing copper structures - Google Patents

Formulations including a 1,3-dicarbonyl compound chelating agent and copper corrosion inhibiting agents for stripping residues from semiconductor substrates containing copper structures

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Publication number
TWI243861B
TWI243861B TW090130319A TW90130319A TWI243861B TW I243861 B TWI243861 B TW I243861B TW 090130319 A TW090130319 A TW 090130319A TW 90130319 A TW90130319 A TW 90130319A TW I243861 B TWI243861 B TW I243861B
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Taiwan
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TW090130319A
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William A Wojtczak
Fatima Ma Seijo
Long H Nguyen
David D Bernhard
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Advanced Tech Materials
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    • 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
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    • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
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    • C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
    • C23G5/00—Cleaning or de-greasing metallic material by other methods; Apparatus for cleaning or de-greasing metallic material with organic solvents
    • C23G5/02—Cleaning or de-greasing metallic material by other methods; Apparatus for cleaning or de-greasing metallic material with organic solvents using organic solvents
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    • G03F7/26—Processing photosensitive materials; Apparatus therefor
    • G03F7/42—Stripping or agents therefor
    • G03F7/422—Stripping or agents therefor using liquids only
    • G03F7/425—Stripping or agents therefor using liquids only containing mineral alkaline compounds; containing organic basic compounds, e.g. quaternary ammonium compounds; containing heterocyclic basic compounds containing nitrogen
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  • Chemical & Material Sciences (AREA)
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  • Metallurgy (AREA)
  • Cleaning Or Drying Semiconductors (AREA)
  • Detergent Compositions (AREA)
  • Photosensitive Polymer And Photoresist Processing (AREA)
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Description

1243861 五、發明說明（1) 相關申請案之交互參照 本申請案係1999年8月20曰提出申請之美國專 No· 0 9 / 3 3 1，5 3 7之部分延續，此美國專利申3請申請案 0 9/33 1，537係以1 9 97年12月23日接中φ嗜+二木N〇· VC T明 < 國東 案No· PCT/US9 7/23 9 1 7為主並主張其之優先^ τ寻利申請 指定為選定聲明。 *’及將美國 發明之背景 發明之領媸 本發明大致係關於用於半導體晶圓製造之與 尤其係關於被利用於在光阻劑電漿灰化步驟，配方，及 除殘渣之化學配方。更明確言之’本發^係^ =自晶圓移 細銅互連結構之半導體晶圓移除無機殘渣之主^自包含精 先前技藝之説明 π冷配方。 組成物。此種配方伴隨有包括金屬或 =合劑之 及促進期望金屬層’尤其係銅或鋼合金部ς =不期望 點。 77 <腐麵的 -些此等配方使用腐#抑制添 中之不期望的銅金屬腐蝕。然而， :j在清潔過鞋 典型上由於此等添加劑會盥殓、、杏丄 〈屬蝕抑制添加劑 潰於清潔流體中之溶解/而ί:ί:互作用’及抑制此種殘 L ^ 、 辟而對清潔過程具有不利的影響。 此外，習知之添加劑於清潔 /月/糸過程完成後並不易自銅表面沖 習慣上在光阻劑灰化㈣之後，使用 除殘渣及清潔晶圓。此等化學配方中之—此2子配方來移 或氫氧化四烷基銨、水及/或其他溶劑、ς匕括含鞍及/ 性 移除 缺 组成物。，t卜.錄Β?·古座陡士 a，』. 甜合劑< &
!243861 五、發明說明（2) 洗掉，且其之存在會造成積體電路 ^會使受污染區域之電阻不利地提 之不可預測的傳導故障。 因此，本發明之一目的為提供於 有效移除殘渣之化學配方。 另一目的為提供不會侵姓應使其 屬結構及使其潛在地降解之晶圓清 本發明之又另一目的為提供一種 板上之銅結構之改良腐蝕抑制劑的 抑制劑係於殘渣移除程序完成後易 洗掉，因而可降低晶圓基板上之積 成物形態。 本發明之其他目的及優點將可由 之申請專利範圍而完全明瞭。 之概述 本發明係關於具有，例如，在電 中用於清潔半導體晶圓之效用的半 在一態樣中，本發明係關於_種 灰化步驟之後自此種晶圓移除殘洁 與包括下列成份之清潔配方接觸^ (iii)含氮羧酸或亞胺，（iv) i 3一 (v)極性有機溶劑，及視需要包括 甜合劑。 之污染。積體電路之污 高，並造成電路系統内 光阻劑灰化步驟之後可 殘留於晶圓上之精細金 潔配方。 包括用於保護半導體基 晶圓清潔配方，此腐雀虫 被水或其他滌洗介質沖 體電路系統之污染的組 隨後之揭示内容及隨附 漿灰化後之半導體製造 導體晶圓清潔配方。 在晶圓上之光阻劑電漿 之方法，其包括使晶圓 (i)有機胺，（i i)水， 二幾基钳合化合物’ v i)至少一其他的金屬 本發明之另-態樣係關於—種晶圓清潔配方，其包括
\\312\2d^code\91-03\90130319.ptd $ 6頁 !243861
有機胺，（ii)水，（iii)含氮羧酸或亞胺，（b) 1,3_ 二羰基鉗合化合物，（v)極性有機溶劑，及視需要包括 、v 1 )至少一其他的金屬鉗合劑。 在再-態樣巾’本發明係關於一種使用於電漿灰化後之 旦導體製造中之半導體晶圓清潔配方，其包括在所示之重 里百分比（以配方之總重量計）範圍内之下列成份： 有機胺 。。 本發明之配方於電漿灰化步驟 >查’尤其係金屬鹵化物及金屬氧 之使用過程中亦可顯著地降低不 圓上之銅金屬結構的移除。 水 1，3 ~二羰基化合物鉗合劑 額外的不同钳合劑 含氮羧酸或亞胺 塵性有爐溶劍__ 總計 0-50% 0 . 1 - 6 0 % 0-25% 0.5-40% 2-98°/〇 10 0% 之後可有效地移除無機殘 化物殘渣。此種配方在其 期望的腐蝕或在半導體晶
本發明之配方於殘渣移除程序之 良：產生之微電子裝置產品的品質。 本舍明之其他特辨Θ彳爲赴g交 附之申請專利範圍^。炎” ”明於隨後之揭示内容及隨 故j圭具體說明 本％明係關於適用於將由跟命 度電漿蝕刻所產生機B =用3虱电I灰化之咼密 王之無機日日a殘渣移除之配方。
1243861 五、發明說明（4) 化合物及/或其他金屬鉗 水或其他溶劑作為主成 此配方有利地包含1，3 -二鑛基 合劑、含氮羧酸或亞胺、胺、及 份。 較佳的配方包括在所示之重量百分比（以配方之總重量 計）範圍内之下列成份： 2-98% 0-50% 0. 1-60% 0-25% 0. 5-40% 2 - 9 8 % 有機胺 水 1，3 -二羰基化合物鉗合劑 額外的不同鉗合劑 含氮羧酸或亞胺 極性有機溶劑_ 100% 熟悉技藝人士所明瞭之任 成份之明確的說明性及較 的成份係以上述所指示之 的重量百分比濃度來表 5 - 9 5 % 5-95% 總計 如前所述之配方的成份可為如 何適當類型或種類。將配方之各 佳配方成份說明於下，其中明確 總重量計之，其以配方中之較佳 示。 較佳的胺包括： 五曱基二伸乙三胺（PMDETA) 三乙醇胺（TEA) 其他高度有利的胺包括： 單乙醇胺 二甘醇胺 二吖雙環（2 · 2 · 2 )辛烷
\\312\2d-code\91-03\90130319.ptd 第8頁 1243861 五、發明說明（5) 二伸乙三胺 3, 3’ -亞胺雙（N，N-二曱基丙胺） N-曱基咪唑 四伸乙五胺 三伸乙四胺 三甲氧乙氧乙胺 二乙醇胺 甲基二乙醇胺 四甲基己二胺 N，N-二乙基乙醇胺 化合物甜合劑包括： 2-90% 明確的較佳1，3 -二羰 2，4 _戊二酉同 2-90% 1 5 - 7 0 % 10-48.3% N，N -二甲基乙醯乙醯胺 乙醯乙酸曱酯 丙二酸二甲酯 其他高度有利的1，3-二羰基化合物包括 N -甲基乙醯乙醯胺 乙醯乙醯胺 丙二醢胺 較佳的含氮羧酸或亞胺包括： 0. 5-2. 5°/〇 0. 5-2. 5% 0. 5-2. 5°/〇 0. 5-2. 5°/〇 亞胺二乙酸 甘氨酸 氮基三乙酸 1，1，3，3 -四曱脈
\\312\2d-code\91-03\90130319.ptd 第9頁 1243861 五、發明說明（6) 其他高度有利的含氮羧酸或亞胺包括 CH3C( = NCH2CH20H)CH2C(0)N(CH3)2 CH3C(=NCH2CH20CH2CH20H)CH2C(0)N(CH3), CH3C(-NH)CH2C(0)CH3 (CH3CH2)2NC( = NH)N(CH3CH2)2 HOOCCH2N(CH3)2
HOOCCH2N(CH3)CH2COOH 較佳的溶劑包括： 0-50% 0-74% 0 - 4 9 % 0-10% 水 乙二醇 N -甲基p比洛咬酮（Ν Μ P ) 四氫嚷吩石風 或可 視需要可利用於本發明之一些配方中之教佳的第 選擇的鉗合劑包括： 咄咯啶二硫基胺基甲酸銨 0-25% 胺基甲酸銨 0-15% 草酸鈹 0-15% 硫鼠酸錢 0-15% 硫代硫酸敍 0-15% 三氟乙酸 0-12% 利用包含1，3 -二羰基化合物及/或其他金屬鉗合劑與胺 及溶劑結合之配方可達成技藝的獨特改良。本發明之配方 提供較習知之包含兒茶酚、胺、及溶劑之晶圓移除配方佳 的移除性能及低的腐#性。
\\312\2d-code\91-03\90130319.ptd 第10頁 1243861 五、發明說明（7) 缓：或亞胺係本發明之另—有二一' 示，在殘ΐ ΐ含特別吸引游離銅原子的官-二改良。含氮 制移除過程中與銅表面接觸如圖1所 清潔心附著至鋼表面’並形成保護屑，而鋼特異之腐蝕抑 =劑Α4Χ-腐钱。此外，如圖隻層，而防止銅表面被 Ρ制劑C可容易地被去離 他’、此種對鋼特異之腐 因此，其於清潔操作完成後，在铜#他條洗介質沖洗掉， 除了明確舉出者外，本發明之配上留下極少污染。 :其有機㉟、甜合劑、及含氮竣酸：：：括種類繁多的溶 =基化合物及適當特性之相關化人.胺。特殊的1，3-二 合物： 〇物包括如下化學式之化 X-CHR-γ 其中R為氫原子或脂族基團， 烯基等等，X及Υ係彼此相同或不D，’ C^C8烷基、芳基、 之包含多重鍵結基團的官能基，二，且為具有拉電子性質 ⑽R，R，、CN、N〇2、s〇R，、或s〇 ^如，C〇NH2、C0NHR，、 不同，且代表。，。烷基，及z代2夺a其中R’及R”係相同或 如，氫、_基或Ci - c8院基。原子或基團，例 具有廣泛實行本發明之效用之 化學式之化合物： 其他的含氮羧酸包括如下 COOH - CH2-NRR， 酸其中各R及R’係分別選自包括氫、烧基、芳基、及叛 可將除明確說明於上之外的胺基甲酸鹽及二硫基胺基甲 \\312\2d-code\91-03\90130319.ptd $ 11頁 1243861 五、發明說明（8) 酸二烷酯使 可使用各 合使用。 本發明之 定最終應用 劑、腐蝕抑 本發明之 再經氧電漿 型上包含金 不造成有效 本發明之 地展示。 實施例1 於具有以 測試包括含 表1 用作為廣泛實行本發 種其他的極性有機溶 配方視需要亦可包括 或此最終應用所期望 制劑、缓衝劑、及共 配方特別有利於經含 灰化之晶圓。由此類 屬氧化物。通常很難 装置性能所需之金屬 特徵及優點由以下之 下成份及特性之兩不 氮緩酸或亞胺之對銅 配方 WT2
Wmz.mzmm 胺、及水 化銨、三乙醇胺1 甲蕋二伸乙三胺、及水 70 40 利用標準的四點探針技術測定 示，加入根據本發明之腐蝕抑制 率’並有效地防止在清潔過程中
\\312\2d-code\91-03\90130319.ptd 明之鉗合劑。 劑’例如’單獨或與水混 有利於本發明之配方之預 之諸如表面活性劑、安定 溶劑之成份。 氣或含氟電漿蝕刻，隨後 型之處理所產生之殘渣典 將此等殘渣完全溶解，而 部份的腐蝕。 非限制性實施例作更完全 同類型的鹼性清潔配方中 特異之腐蝕抑制劑。 銅蝕刻速率 (埃/分鐘） 鋼蝕刻速率。如由下表戶j 劑可顯著地減緩銅餘刻 之不期望的腐餘：
第12頁 1243861 五、發明說明（9) 腐蝕抑制劑 溫度 (°C) 使 用 配 方 濃度 (%) 溶液 之 pH 銅蝕刻 速率 (埃/分 鐘） 蝕刻速率 之降低 (%) 亞胺二乙酸 40 2 1.5 8.0 1-2 -73.3 〜86· 7 甘氨酸 40 2 1.5 9.2 3.6 -52.0 氮基三乙酸 40 2 1.5 8.2 3.6 -52.0 1，1，3,3-四甲胍 40 2 1.5 8.7 3.4 -54.7 CH3C(=NCH2CH2〇H)CH2 C(0)N(CH3)2 70 1 24 10.9 6.2 -64.4 CH3C(=NCH2CH2OCH2CH2OH) ch2c(o)n(ch3)2 70 1 36 10.7 0.32 -98.2 CH3C(=NH)CH2C(0)CH3 40 2 13.68 7.9 4.4 -41.3 表2 實施例2 於包含亞胺二乙酸抑制劑之配方2上進行污染試驗。待 清潔之半導體晶圓包含銅及矽薄膜。於清潔操作完成後， 以2 5 °C之去離子水滌洗晶圓約1 5分鐘。測得的第二離子質 量光譜術數據（S I M S )如下：
Cu(原子/cm2) F(原子/cm2) C源子/cm2) CuxO(埃） 未淸潔晶圓 1.6x1 Ο10 3.3χ]Ο13 7.5xl013 42 經淸潔晶圓 8.5x1 Ο9 5.1 χ 1 0 13 ].5x1 Ο13 15 前述之結果顯示氧化銅C ux 0已被清潔方法有效地移除
\\312\2d-code\91-03\90130319.ptd 第13頁 1243861 五 發明說明α〇) 主要由清潔配方中之有機腐蝕 、、^、 大大地降低。 劑所造成之咬、'一 明 明 =:f發明已經參照特定的特徵、 木則 =二：應明瞭本發明並不因此及具體例而說 可以各式各樣的組成物、相對的成份=1此，本發 而相應地具體實現。因此，應明瞭本發明〜二及最終用途 出專利申請之本發明之精神及範圍内2 =盍在如後文提 改及替代的具體例。 R有此等變化、修
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\\312\2d-code\91-03\90130319.ptd 1243861 圖式簡單說明 圖1係有用於概括實行本發明之對銅特異之腐蝕抑制劑 的概略圖式，此腐^虫抑制劑在銅金屬上形成保護層而防止 腐蚀。 圖2係被去離子水自銅表面沖洗掉之對銅特異之腐蝕抑 制劑的概略圖式。
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Claims (1)

1243861 六、申請專利範圍 丨 1. 一種半導體晶圓之清潔配方，係使用於電漿灰化後之 半導體製造中，其包括在所示之重量百分比（以配方之總 重量計）範圍内之下列成份： 有機胺 水 1，3-額外 含氮 極性 二幾基化合物钳合劑 的不同鉗合劑 羧酸或亞胺 有機溶劑_ 2-98% 0 - 5 0 % 0.1-60% 0-25% 0. 5-40% 2-98% 總計 2.如 包括選 五甲 三乙 3 ·如 羰基化 2, 4-N，N- 乙醯 丙二 4 ·如 或亞胺 亞胺 甘氨 100% ° 申請專利範圍第1項之清潔配方，其中，該有機胺 自包括下列之化合物： 基二伸乙三胺（PMDETA) 5-95% 醇胺（TEA) 5-95%。 申請專利範圍第1項之清潔配方，其中，該1，3 -二 合物鉗合劑包括選自包括下列之化合物： 戊二酮 2-90% 二曱基乙醯乙醯胺 2-90% 乙酸甲酯 15-70% 酸二甲酯 10-48.3% 。 其中該含氮羧酸 0. 5-2. 5% 0.5-2.5% 申請專利範圍第1項之清潔配方 包括選自包括下列之化合物： 二乙酸（IDA) 酸
\\312\2d-code\91-03\90130319.ptd 第16頁 1243861 六、申請專利範圍 氮 基 二 乙 酸 (NTA) 0· 5 - 2 · 5°/〇 1， 1， 3, 3- 四 曱 胍（TMG) 0· 5-2. 5% ° 5. 如 中 請 專 利 範 圍第1項之清潔配方， 其中 ，該 極性 有 機溶 劑 包 括 選 包 括下列之溶劑種類： 乙 二 醇 0- 74% N - 甲 基 口比 咯 啶 酉同 (NMP) 0- 49% 四 氫 噻 吩 砜 0- 10% 〇 6. 如 中 請 專 利 範 圍第1項之清潔配方， 其中 ，該 額外 的 不同 鉗 合 劑 包 括 選 自包括下列之種類： 吼 咯 啶 二 疏 基 胺 基甲酸銨 0- 25% 胺 基 甲 酸 锻 0- 15% 草 酸 銨 0- 15% 硫 氰 酸 鈹 0 - 15% 硫 代 硫 酸 銨 0- 15% 二 氟 乙 酸 0 - 12% ( 3 7. 如 中 請 專 利 範 圍第1項之清潔配方， 其中 ，該 有機 胺 包括選自包括下列之種類： 單乙醇胺 二甘醇胺 五曱基二伸乙三胺（PMDETA) 三乙醇胺（TEA) 二吖雙環（2· 2· 2)辛烷 二伸乙三胺 3, 3’ -亞胺雙（N，N-二甲基丙胺）
\\312\2d-code\91-03\90130319.ptd 第17頁 1243861 六、申請專利範圍 N -曱基咪嗤 四伸乙五胺 三伸乙四胺 三曱氧乙氧乙胺 二乙醇胺 曱基二乙醇胺 四甲基己二胺 N，N -二乙基乙醇胺。 8.如申請專利範圍第1項之清潔配方，其中，該1，3 羰基化合物鉗合劑包括選自包括下列之化合物： 酮 4-戊 乙醯乙酸甲酯 丙二酸二曱酯 N -甲基乙醯乙醯胺 N，N -二曱基乙醯乙醯胺 乙醯乙醯胺 丙二醯胺。 其中，該含氮羧 9.如申請專利範圍第1項之清潔配方 酸或亞胺係選自包括： 亞胺二乙酸（IDA) 甘氨酸 氮基三乙酸（NTA) 1，1，3, 3-四甲胍（TMG) CH3C(=NCH2CH20H)CH2C(0)N(CH3)2
\\312\2d-code\91-03\90130319.ptd 第18頁 1243861 六、申請專利範圍 CH3C(-NCH2CH20CH2CH20H)CH2C(0)N(CH3)2 CH3C(=NH)CH2C(0)CH3 (CH3CH2)2NC( = NH)N(CH3CH2)2 HOOCCH2N(CH3)2 hoocch2n(ch3)ch2cooh。 1 0 .如申請專利範圍第1項之清潔配方，其中，該有機胺 包括選自包括下列之化合物： 五甲基二伸乙三胺（PMDETA) 5-95% 三乙醇胺（TEA) 5-95% 該1，3 -二羰基化合物鉗合劑包括選自包括下列之化合物： 2-90% 2-90% 15-70% 10-48. 3% 2，4 -戊二酮 N，N -二甲基乙醯乙醯胺 乙醯乙酸曱酯 丙二酸二曱酯 該含氮羧酸或亞胺包括選自包括下列之化合物 0· 0· 0· 0. -2. 5°/〇 -2. 5% -2· 5% -2. 5°/〇 亞胺二乙酸（IDA) 甘氨酸 氮基三乙酸（NTA) 1，1，3, 3-四甲胍（TMG) 及該極性有機溶劑包括選自包括下列之溶劑種類： 0-74% 0-49% 0-10% 乙二醇 N-曱基咄咯啶酮（NMP) 四氫p塞吩硬 1 1.如申請專利範圍第1項之清潔配方，其包括化學式如
\\312\2d-code\91-03\90130319.ptd 第19頁 1243861 六、申請專利範圍 下之鉗合劑： X-CHR-Y ，其中 R為鼠或脂族基團’及 X及Y為具有拉電子性質之包含多重鍵結基團的官能基。 1 2.如申請專利範圍第11項之清潔配方，其中，各X及Y 係分別選自，CONH2、CONHR’、CONR’ R”、CN、N02、SOR’、及 S02Z，其中R’及1^’為烷基，及Z為氫、鹵基、或烷基。 1 3.如申請專利範圍第1項之清潔配方，其中，該含氮羧 酸具有以下之化學式： COOH-CH2-NRR， 其中，各R及R’係分別選自包括氫、烷基、芳基、及羧 酸。 1 4. 一種半導體晶圓之製造方法，包括下列之步驟： 自晶圓之表面電漿I虫刻金屬化層； 自晶圓之表面將光阻劑電漿灰化； 利用包括在所示之重量百分比（以配方之總重量計）範圍 内之下列成份的半導體晶圓清潔配方來清潔晶圓· 2-98% 0-50% 0 · 1 - 6 0 % 0-25% 0. 5-40% 2-98% 100% 有機胺 水 1，3 -二幾基化合物甜合劑 額外的不同鉗合劑 含氮羧酸或亞胺 極性有機溶劑_ 總計
\\312\2d-code\91-03\90130319.ptd 第20頁 1243861 六、申請專利範圍 1 5.如申請專利範圍第1 4項之製造方法，其中，該有機 胺包括選自包括下列之化合物： 五曱基二伸乙三胺（PMDETA) 5-95% 三乙醇胺（TEA) 5-95%。 1 6.如申請專利範圍第1 4項之製造方法，其中，該1，3 -二羰基化合物鉗合劑包括選自包括下列之化合物： 2-90% 2-90% 15-70% 10-48.3% 2，4 -戊二酮 N，N -二曱基乙醯乙醯胺 乙醯乙酸甲酯 丙二酸二甲酯 1 7.如申請專利範圍第1 4項之製造方法，其中，該含氮 羧酸或亞胺包括選自包括下列之化合物： 0· 0· 0· 0· -2. 5°/〇 -2. 5°/〇 -2. 5% -2. 5% 亞胺二乙酸（IDA) 甘氨酸 氮基三乙酸（NTA) 1，1，3, 3-四曱胍（TMG) 1 8.如申請專利範圍第1 4項之製造方法，其中，該極性 有機溶劑包括選自包括下列之溶劑種類： 乙二醇 0-74% N-甲基咄咯啶酮（NMP) 0-49% 四氮^塞吩石風 0-10%。 1 9.如申請專利範圍第1 4項之製造方法，其中，該額外 的不同鉗合劑包括選自包括下列之化合物： 25% 咄咯啶二硫基胺基甲酸銨
\\312\2d-code\91-03\90130319.ptd 第21頁 1243861 六、申請專利範圍 胺基甲酸銨 0-15% 草酸錢 0-15% 硫氰酸銨 0-15% 硫代硫酸銨 0-15% 三氟乙酸 0 - 1 2 %。 2 0.如申請專利範圍第1 4項之製造方法，其中，該有機 胺包括選自包括下列之化合物： 五曱基二伸乙三胺（PMDETA) 單乙醇胺 二甘醇胺 三乙醇胺（TEA) 二吖雙環（2 · 2 · 2 )辛烷 二伸乙三胺 3, 3’ -亞胺雙（N，N-二曱基丙胺） N -曱基117米峻 四伸乙五胺 三伸乙四胺 三甲氧乙氧乙胺 二乙醇胺 曱基二乙醇胺 四曱基己二胺 N，N -二乙基乙醇胺。 2 1.如申請專利範圍第1 4項之製造方法，其中，該1，3-二羰基化合物鉗合劑包括選自包括下列之化合物：
\\312\2d-code\91-03\90130319.ptd 第22頁 1243861 六、申請專利範圍 2，4 -戊二酮 N，N -二甲基乙醯乙醯胺 乙醯乙酸甲酯 丙二酸二曱酯 N -甲基乙醯乙醯胺 乙醢乙隨胺 丙二醯胺。 其中，該含氮 2 2.如申請專利範圍第1 4項之製造方法 羧酸或亞胺包括選自包括下列之化合物： 亞胺二乙酸（IDA) 甘氨酸 氮基三乙酸（NTA) 1，1，3, 3-四甲胍（TMG) CH3C(=NCH2CH20H)CH2C(0)N(CH3)2 CH3C(=NCH2CH20CH2CH20H)CH2C(0)N(CH3)2 CH3C(=NH)CH2C(0)CH3 (CH3CH2)2NC( = NH)N(CH3CH2)2 HOOCCH2N(CH3)2 _cch2n(ch3)ch2cooh。 2 3.如申請專利範圍第1 4項之製造方法，其中，該有機 胺包括選自包括下列之化合物： 五甲基二伸乙三胺（PMDETA) 5-95% 三乙醇胺（TEA) 5-95% 該1，3 -二裁基化合物钳合劑包括選自包括下列之化合物：
\\312\2d-code\91-03\90130319.ptd 第23頁 1243861 六、申請專利範圍 2, 4-戊二 2-90% 2 - 9 0 % 15-70% 10-48.3% 酮 N，N -二曱基乙醯乙醯胺 乙醯乙酸甲酯 丙二酸二甲酯 該含氮羧酸或亞胺包括選自包括下列之化合物： 0. 5-2. 5% 0. 5-2. 5% 0. 5-2. 5°/〇 0. 5-2. 5% 亞胺二乙酸（IDA) 甘氨酸 氮基三乙酸（NTA) 1，1，3, 3-四甲胍（TMG) 及該極性有機溶劑包括選自包括下列之化合物： 0-74% 0-49% 0-10% 乙二醇 N-曱基咄咯啶酮（NMP) 四氫11塞吩石風 2 4.如申請專利範圍第1 4項之製造方法，其中，該配方 包括化學式如下之鉗合劑： X-CHR-Y ，其中 R為氫或脂族基團，及 X及Y為具有拉電子性質之包含多重鍵結基團的官能基。 2 5.如申請專利範圍第24項之方法，其中，各X及Y係分 另丨J 選自 C0NH2、CONHR’、CONR’ Rn、CN、N02、SOR’、及 S02Z，其中R’及!^為烷基，及Z為氫、鹵基、或烷基。 2 6.如申請專利範圍第1 4項之製造方法，其包括化學式 如下之含氮羧酸： C00H - CH9-NRR，
\\312\2d-code\91-03\90130319.ptd 第24頁
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