TWI362571B - Stripper composition for photoresist - Google Patents
Stripper composition for photoresist Download PDFInfo
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- TWI362571B TWI362571B TW96118832A TW96118832A TWI362571B TW I362571 B TWI362571 B TW I362571B TW 96118832 A TW96118832 A TW 96118832A TW 96118832 A TW96118832 A TW 96118832A TW I362571 B TWI362571 B TW I362571B
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- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03F—PHOTOMECHANICAL PRODUCTION OF TEXTURED OR PATTERNED SURFACES, e.g. FOR PRINTING, FOR PROCESSING OF SEMICONDUCTOR DEVICES; MATERIALS THEREFOR; ORIGINALS THEREFOR; APPARATUS SPECIALLY ADAPTED THEREFOR
- G03F7/00—Photomechanical, e.g. photolithographic, production of textured or patterned surfaces, e.g. printing surfaces; Materials therefor, e.g. comprising photoresists; Apparatus specially adapted therefor
- 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
Description
1362571 九、發明說明： 【發明所屬之技術領域】 本發明係有關於一種光阻脫除組成物。 本發明係主張韓國專利申請號Korean Patent 5 Application No. 10-2006-0047668國際優先權，係於2〇〇6年5 月26曰於韓國知識產權局（KIp〇)申請，本發明之揭露内容 係以其為依據。1362571 IX. Description of the Invention: [Technical Field to Which the Invention Is Ascribed] The present invention relates to a photoresist removal composition. The present invention claims the Korean Patent Application No. 10-2006-0047668 International Priority, which is filed on May 26, 2002 in the Korean Intellectual Property Office (KIp〇), the disclosure of the present invention. Based on it.
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20 【先前技術】 半導體積體電路或液晶顯示器之精細線路之製作方 法包括：均勻地將一光阻塗佈於一導電金屬膜上，其係由 鋁、-鋁合金、銅、或一銅合金、或一絕緣膜(如：形成於 一基板上之一氧化矽膜或一氮化矽膜）所製得；選擇性地將 光阻曝光及顯影形成一光阻圖案，以圖案化光阻膜作為光 罩’使該導電金屬膜或絕緣膜進行濕式㈣或乾式姓刻， 進而於光阻下層描繪出精細線路圖案；並使用_脫除劑將 不必要的光阻層移除。 g於製造半導體裝置及液晶顯示器製程中使用脫除 劑移除光阻時，需考量到以下的特性。 其光阻必須於低溫以及於一短期間内被脫除，且需要 徹底的脫除以防止光阻的殘留物於沖洗後滞留於基板上。 此外，必須具有低的腐錄以使得其光阻下層之金屬膜或 絕緣膜不被破壞。若組成脫除劑之溶劑之間發生交互作 用，則脫_之儲存穩定性可能下降，且其物理特性可能 5 1362571 隨著脫除劑生產期間混合步驟的順序而改變。因此，互相 混合之溶劑必須彼此之間不會產生反應，且必須確保即使 於高溫狀況下仍具有穩定性。再者，有關於毒性問題，係 為考量到廢棄物處理，脫除劑應對於操作員不具傷害性且 5應對環境無害。當於高溫下移除光阻時，若發生大量揮發， 組成比例將快速改變，進而降低脫除劑之穩定性以及操作 的再生能力。因此，脫除劑之揮發性應該被降至最小。此 外，許多基板需使用一小量的脫除劑作處理，而構成脫除 劑之組成物應以低成本簡單地製得，且過量的脫除劑應再 ίο 循環利用以符合經濟效益。 為了滿足上述之需求，而發展出各種類型之光阻的脫 除組成物，舉例如下。 最初被研發出的光阻脫除組成物的範例係揭露於曰 本專利JP-A-51-72503中，其脫除組成物包含：一具有1〇至 15 20個碳原子之烷基苯磺酸，以及沸點為150t或更高之非鹵 化芳烴。曰本專利JP-A-57-84456係揭露一脫除組成物，其 包含：二甲基亞砜（dimethyl sulfoxide)或二乙基亞礙（diethyl sulfoxide)，以及一有機颯化合物。此外，美國專利號u s pat No.4,256,294揭露一脫除組成物，其包括：一烷基芳基磺 2〇 酸、一具有6至9個碳原子之親水性芳香磺酸、以及沸點為 150°C或更高之非鹵化芳烴。然而，由於上述之組成物對 紹、銘合金、銅'或銅合金所製得之導電金屬膜具有高腐 鞋性、且其具強毒性並會造成環性污染，因而不適用。 爲了避免上述問題’日前亦已提出混合各種有機溶劑 6 1362571 之脫除組成物，其中有機溶劑係以水溶性烷醇胺 5[Prior Art] A method for fabricating a fine circuit of a semiconductor integrated circuit or a liquid crystal display includes uniformly applying a photoresist to a conductive metal film, which is made of aluminum, aluminum alloy, copper, or a copper alloy. Or an insulating film (for example, a tantalum oxide film or a tantalum nitride film formed on a substrate); selectively exposing and developing the photoresist to form a photoresist pattern to pattern the photoresist film As the reticle, the conductive metal film or the insulating film is wet-typed (four) or dry-type, and the fine line pattern is drawn under the photoresist; and the unnecessary photoresist layer is removed using the _ remover. g When using a remover to remove photoresist in the fabrication of semiconductor devices and liquid crystal displays, the following characteristics should be considered. The photoresist must be removed at low temperatures and for a short period of time and requires thorough removal to prevent residues of photoresist from remaining on the substrate after rinsing. In addition, it is necessary to have a low rot so that the metal film or the insulating film of the lower layer of the photoresist is not damaged. If the interaction between the solvents constituting the remover occurs, the storage stability of the detachment may be lowered, and the physical properties thereof may vary depending on the order of the mixing steps during the production of the remover. Therefore, the mutually mixed solvents must not react with each other and must ensure stability even under high temperature conditions. Furthermore, regarding toxicity, the disposal of waste should be considered. The remover should be non-harmful to the operator and 5 should be environmentally friendly. When the photoresist is removed at a high temperature, if a large amount of volatilization occurs, the composition ratio will change rapidly, thereby reducing the stability of the remover and the regenerative ability of the operation. Therefore, the volatility of the remover should be minimized. In addition, many substrates require a small amount of remover to be treated, and the composition constituting the remover should be simply produced at low cost, and the excess remover should be recycled to be economical. In order to satisfy the above needs, various types of photoresist removal compositions have been developed, as exemplified below. An example of a photoresist removal composition originally developed is disclosed in JP-A-51-72503, the removal composition comprising: an alkylbenzenesulfonate having from 1 to 15 20 carbon atoms. An acid, and a non-halogenated aromatic hydrocarbon having a boiling point of 150 t or more. JP-A-57-84456 discloses a removal composition comprising: dimethyl sulfoxide or diethyl sulfoxide, and an organic ruthenium compound. In addition, U.S. Patent No. 4,256,294 discloses a removal composition comprising: an alkylarylsulfonate, a hydrophilic aromatic sulfonic acid having 6 to 9 carbon atoms, and a boiling point of 150°. Non-halogenated aromatic hydrocarbons of C or higher. However, since the above-mentioned composition has high corrosion resistance to the conductive metal film produced by Shao, Ming alloy, copper 'or copper alloy, and it is highly toxic and causes ring pollution, it is not applicable. In order to avoid the above problems, a stripping composition of various organic solvents 6 1362571 has been proposed, in which the organic solvent is a water-soluble alkanolamine 5
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20 (alkanolamine)作為必要成分，其相關範例如下所述。 美國專利U.S. Pat. No. 4,617,251係揭露一包含兩組成 份之脫除組成物，其包括：一有機胺化合物（如：乙醇胺 (monoethanolamine, MEA)及 2-(2-氣基乙氧基）-1-乙醇 (2-(2-aminoethoxy)-1-ethanol, AEE)) > 以及一極性溶劑 (如：二曱基曱酿胺（dimethylformamide，DMF)、二曱基乙酿 胺（dimethylacetamide， DMAc)、N-曱基0tb 洛院酮 (N-methylpyrrolidinone，NMP)、二甲基亞礙（DMSO)、二乙 二醇乙醚乙酸脂（carbitol acetate)、以及丙二醇曱趟醋酸面旨 (PGMEA))。美國專利 U.S. Pat. No. 4,770,713 揭露一包含兩 組成份之脫除組成物，其包括：一有機胺化合物以及一氨基 溶劑（如：二甲基曱醯胺（DMF)、二曱基乙醯胺（DMAc)、N-甲基-N-乙基丙酰《胺（N-methyl-N-ethylpropionamide)、二乙 基乙醯胺（DEAc)、二丙基乙醯胺（DPAc)、Ν,Ν-二曱基丙醯 胺（Ν,Ν-dime.thylpropionamide)、以及 Ν，Ν-二甲基 丁醯胺 (Ν,Ν-dimethylbutylamide))。曰本專利 JP-A-62-49355係揭露 一包含亞烧基聚胺礙（alkylene polyamine sulfone)化合物之 脫除組成物，其中，環氧乙烧（ethylene oxide)被提供至烧醇 胺（alkanolamine)、乙二胺與乙二醇單烧基醚（glycol monoalkyl ether)中。日本專利 JP-A-63-208043係揭露一包含 一水溶性烷醇胺以及1,3-二甲基-2-咪唑啉酮 (l，3-dimethyl-2-imidazolidinone，DMI)之脫除組成物。日本 專利JP-A-63-231343揭露一正型光阻脫除組成物，其包括一 7 1362571 胺類化合物、一極性溶劑、及一界面活性劑。日本專利 JP-A-64-42653係揭露一脫除組成物，其包括50wt%或更多 之二曱基亞艰（DMSO)、1至50wt%之一或多種之溶劑、以及 一含氮之有機氫氧化物（如：單乙醇胺（monoethanolamine, 5 MEA)) ’其溶劑係選自由二乙二醇單烷基醚（diethylene glycol monoalkyl ether)、二乙二醇雙烷基醚（diethylene glycol dialkyl ether)、7 -丁内醋（gamma-butyrolactone)、以 及1，3-二曱基-2-咪唑啉酮所組成之群組。日本專利 JP-A-4-124668係揭露一脫除組成物，其包括20至90wt%之 10 有機胺、0.1至20wt%之磷酸酯類界面活性劑、〇.1至20wt% 之 2- 丁炔-1，4-二酵（2-butyne-l，4-diol)、二乙二醇二烧基 醚、以及非質子極性溶劑。其中，在不降低脫除特性之條 件下，添加2-丁炔-1,4-二醇及磷酸酯類界面活性劑可用以 防止金屬層被腐蝕。然而，由於用以脫除光阻之組成物對 15 鋁及鋁合金膜而言具有較低的防蝕能力，因此會於脫除步 驟中產生顯著的腐蝕現象以及於後製程之閘極絕緣膜沉澱 時形成缺陷碎片（defective fraction)。 此外，曰本專利JP-A-4-350660係揭露一脫除組成物其 包括1,3-二曱基-2-咪唑啉酮（DMI)、二曱基亞砜（DMSO)、 2〇 以及一水溶性有機胺；且日本專利JP-A-5-281753係揭露一 脫除組成物，其包括烷醇胺、一砜類化合物或一亞砜類化 合物、以及一（C6H6)n(OH)n(n係為1、2、或3之整數）之氫氧 化物。日本專利JP-A-8-87118係揭露一脫除組成物，其包括 50至 90wt%之N-烧基烧醇胺（N-alkylalkanolamine)以及 50至 8 1362571 10wt%之二甲基亞砜（DMSO)或二曱基甲醯胺（DMF)。然 而，近來生產液晶顯示器以及半導體裝置的過程中，由於 製程條件係非常極端（例如，玻璃基板以及矽晶圓基板須以 120°C或更高的溫度處理），光阻必須於後烤的高溫製程中 5 迅速投入。因此，顯著的固化問題使上述之脫除組成物無 法達到合意的移除結果。 包含水及/或一羥胺化合物之光阻脫除組成物可完全 移除高溫製程中固化之光阻。例如，日本專利JP-A-4-289866 揭露一脫除組成物，其包括羥胺、烷醇胺、以及水。曰本 10 專利JP-A-6-2661 19揭露一脫除組成物，其包括經胺、烧醇 胺、水、以及一腐蝕抑制劑。此外，日本專利JP-A-7-69618 更揭露一脫脫除組成物，其包括一極性非質子溶劑（如：7 -丁内酯（GBL)、二甲基甲醯胺（DMF)、二甲基乙醯胺 (DMAc)、以及N-曱基吡咯烷酮（NMP))、胺醇（包含2-甲氨基 15 乙醇（2-methylamino ethanol, N-MAE))、以及預設比例的 水。再者，日本專利JP-A-8-123043更揭露一脫除組成物， 其包括胺醇、水、以及乙二醇烧基醚（glycol alkyl ether，如： 二乙二醇單 丁基醚（diethylene glycol monobutyl ether, BDG))。日本專利JP-A-8-262746係揭露一脫除組成物，其 20 包括烧醇胺、烧氧基烧基胺、二醇烧基醚、一糖類化合物、 氫氧化敍（quaternary ammonium hydroxide)、以及水；且曰 本專利JP-A-9-152721係揭露一脫除組成物，其包括烷醇 胺、羥胺、二乙二醇單烷基醚、一糖類化合物（如：山梨糖 醇）作為一腐蝕抑制劑、以及水。曰本專利JP-A-9-9691 1係 9 1362571 揭露一脫除組成物，其包括羥胺、水、解離常數（pKa)介於 7.5至13之間的胺類、一水溶性極性有機溶劑、以及一腐蝕 抑制劑。然而，上述之脫除組成物會由於高溫製程、乾式 银刻、灰化（ashing)、以及離子注入製程而惡化。以移除交 5 聯型（crosslinked)光阻層能力、光阻姓刻殘餘物（钕刻過程 中與金屬性副產物反應形成）、以及鋁或鋁合金薄膜（為光阻 下之導電層）之防腐力來說，此脫除組成物並不理想。此 外，其另存有羥胺化合物於高溫中不穩定的問題，羥胺化 合物會隨時間分解掉。 10 上述之脫除組成物依據其組成份及組成比例而有明 顯之差異，組成份及組成比例與光阻之脫除特性、金屬腐 蝕特性、脫除後的沖洗性、操作的再生性、儲存特性、以 及經濟效益相關，而目前需開發一種可於不同製程中，低 成本條件下，具有最佳效能的脫除組成物。 15 同時，液晶顯示器的尺寸增加，且液晶顯示器被大量 的生產。據此，可藉由單一晶圓處理裝置進行光阻的脫除 步驟，其中，單一晶圓處理裝置一次僅處理單一晶圓，而 非以大量脫除劑的浸泡步驟進行，且其使用一可用於裝置 之脫除組成物。 2〇 例如，韓國專利早期公開號Korean Patent Laid-Open20 (alkanolamine) as an essential component, the relevant examples are as follows. US Pat. No. 4,617,251 discloses a removal composition comprising two components comprising: an organic amine compound (e.g., monoethanolamine (MEA) and 2-(2-carbethoxy)). 1-(2-aminoethoxy)-1-ethanol, AEE)) & a polar solvent (eg dimethylformamide (DMF), dimethylacetamide, DMAc) ), N-mercapto 0tb N-methylpyrrolidinone (NMP), dimethyl sulfoxide (DMSO), carbitol acetate, and propylene glycol hydrazine acetate (PGMEA) . A removal composition comprising two components comprising an organic amine compound and an amino solvent (eg, dimethyl decylamine (DMF), dimercaptoacetamide) is disclosed in US Pat. No. 4,770,713. (DMAc), N-methyl-N-ethylpropionamide, diethylacetamide (DEAc), dipropylacetamide (DPAc), hydrazine, hydrazine - Dimercaptopropionamide, and dimethyl-dimethylbutylamide. JP-A-62-49355 discloses a removal composition comprising an alkylene polyamine sulfone compound in which an ethylene oxide is supplied to an alkanolamine (alkanolamine). ), ethylene diamine and glycol monoalkyl ether. Japanese Patent JP-A-63-208043 discloses a removal composition comprising a water-soluble alkanolamine and 1,3-dimethyl-2-imidazolidinone (DMI). Things. A positive resist removal composition comprising a 7 1362571 amine compound, a polar solvent, and a surfactant is disclosed in Japanese Patent Publication No. JP-A-63-231343. Japanese Patent JP-A-64-42653 discloses a removal composition comprising 50% by weight or more of dimethyl sulfoxide (DMSO), 1 to 50% by weight of one or more solvents, and a nitrogen-containing one. An organic hydroxide (eg, monoethanolamine (5 MEA)) 'the solvent is selected from the group consisting of diethylene glycol monoalkyl ether, diethylene glycol dialkyl ether ), a group consisting of 7-butyrolactone and 1,3-didecyl-2-imidazolidinone. Japanese Patent JP-A-4-124668 discloses a removal composition comprising 20 to 90% by weight of 10 organic amines, 0.1 to 20% by weight of a phosphate ester surfactant, and 0.1 to 20% by weight of 2-butyl. Alkyne-1,4-dipropion (2-butyne-l, 4-diol), diethylene glycol dialkyl ether, and aprotic polar solvent. Among them, 2-butyne-1,4-diol and a phosphate ester surfactant can be added to prevent corrosion of the metal layer without lowering the removal characteristics. However, since the composition for removing the photoresist has a low corrosion resistance to the 15 aluminum and aluminum alloy film, significant corrosion occurs in the removal step and the gate insulating film precipitates in the post process. A defective fraction is formed. In addition, the present patent JP-A-4-350660 discloses a removal composition comprising 1,3-dimercapto-2-imidazolidinone (DMI), dimercaptosulfoxide (DMSO), 2〇, and A water-soluble organic amine; and Japanese Patent JP-A-5-281753 discloses a removal composition comprising an alkanolamine, a sulfone compound or a sulfoxide compound, and a (C6H6)n(OH) A hydroxide of n (n is an integer of 1, 2, or 3). Japanese Patent JP-A-8-87118 discloses a removal composition comprising 50 to 90% by weight of N-alkylalkanolamine and 50 to 8 1362571 10% by weight of dimethyl sulfoxide ( DMSO) or dimethylformamide (DMF). However, in the recent production of liquid crystal displays and semiconductor devices, since the process conditions are extremely extreme (for example, the glass substrate and the germanium wafer substrate must be treated at a temperature of 120 ° C or higher), the photoresist must be baked at a high temperature. 5 quickly invested in the process. Therefore, significant curing problems prevent the above-described removal of the composition from achieving a desired removal result. A photoresist removal composition comprising water and/or a hydroxylamine compound completely removes the cured photoresist in the high temperature process. For example, Japanese Patent JP-A-4-289866 discloses a removal composition comprising hydroxylamine, an alkanolamine, and water. A detachment composition comprising an amine, an alkaloid, water, and a corrosion inhibitor is disclosed in Japanese Patent Publication No. Hei. In addition, Japanese Patent JP-A-7-69618 discloses a release composition comprising a polar aprotic solvent (e.g., 7-butyrolactone (GBL), dimethylformamide (DMF), two Methylacetamide (DMAc), and N-mercaptopyrrolidone (NMP), amine alcohol (containing 2-methylamino ethanol (N-MAE)), and water in a predetermined ratio. Further, Japanese Patent JP-A-8-123043 discloses a removal composition comprising an amine alcohol, water, and a glycol alkyl ether such as diethylene glycol monobutyl ether ( Diethylene glycol monobutyl ether, BDG)). Japanese Patent No. JP-A-8-262746 discloses a removal composition comprising 20 an alkalamine, an alkoxyalkylamine, a glycol alkyl ether, a saccharide compound, a quaternary ammonium hydroxide, And water; and the present patent JP-A-9-152721 discloses a removal composition comprising an alkanolamine, a hydroxylamine, a diethylene glycol monoalkyl ether, a monosaccharide compound (eg, sorbitol) as A corrosion inhibitor, and water. JP-A-9-9691 1 Series 9 1362571 discloses a removal composition comprising hydroxylamine, water, an amine having a dissociation constant (pKa) of between 7.5 and 13, a water-soluble polar organic solvent, And a corrosion inhibitor. However, the above-described removal composition is deteriorated by a high temperature process, dry silver etching, ashing, and ion implantation process. To remove the crosslinked photoresist layer, photoresist residue (formed by reaction with metallic by-products during engraving), and aluminum or aluminum alloy film (for conductive layer under photoresist) In terms of corrosion resistance, this removal of the composition is not ideal. In addition, there is a problem that the hydroxylamine compound is unstable at high temperatures, and the hydroxylamine compound decomposes over time. 10 The above-mentioned removal composition has obvious differences depending on its composition and composition ratio, composition and composition ratio and photoresist removal characteristics, metal corrosion characteristics, rinseability after removal, reproducibility of operation, and storage. The characteristics and economic benefits are related, and it is currently necessary to develop a removal composition that has the best performance in different processes and at low cost. 15 At the same time, the size of liquid crystal displays has increased, and liquid crystal displays have been produced in large quantities. Accordingly, the step of removing the photoresist can be performed by a single wafer processing apparatus, wherein the single wafer processing apparatus processes only a single wafer at a time instead of the soaking step of a large amount of the removing agent, and one of the available ones is available. The composition is removed from the device. 2〇 For example, Korean Patent Early Publication No. Korean Patent Laid-Open
Publication No. 2000-8103係揭露一脫除組成物，其包括5 至15wt%之烷醇胺、35至55wt%之亞砜或颯類化合物、以及 35至55wt%之二醇醚。韓國專利早期公開號Korean Patent Laid-Open Publication No. 2000-8553係揭露一脫除組成物 ίο 1362571 其，包括10至30wt%之水溶性胺類化合物以及7〇至9〇wt%之 二乙二醇單烷基醚以及N—烷基吡咯烷酮或羥烷基吡咯烷 _。然而，上述之組成物雖然對金屬的腐蝕力小，但卻有 低溫下脫除能力不佳的缺點。 5 並且，於一剝離製程（lift_off Process)中，在光阻塗佈 至整個表面並圖案化之後，一金屬膜或一絕緣膜（如：氧化 矽膜或氮化矽膜）將沉澱於其上，並將其光阻移除。因此， 好處為可省去將薄膜圖案化之姓刻步驟。然而，由於光阻 • 纟非整面接受曝光，因此需花費長時間進行光阻的脫除步 10 驟。 此外，上述所有組成物具有剝離製程中光阻脫除的時 . 間需要10分鐘或更久，且鋁或銅線（組成物塗佈於其上）會受 腐钱之缺點。 15 【發明内容】 (技術問題） 鲁 本案發明人對於光阻脫除組成物具有相當的研究，其 可於短時間内脫除光阻，並於剝離製程（光阻脫除步驟）中具 有對金屬膜或絕緣膜之低腐姓性，據此發現一光阻脫除組 20成物，其包含-水溶性有機胺化合物以及一預定比例之腐 蝕抑制劑。於剝離製程中，Λ光阻脫除組成物可於低溫且 短時間内完全脫除因過度光微影製程（ph〇t〇mh〇graphy process)而變質之光阻層；且即使僅使用水（而非異丙醇（中 間物沖洗溶液）)作沖洗’仍不會傷到光阻下部位的導電層以 25及絕緣膜；且對於光阻下部位的導電金屬膜以及絕緣膜具Publication No. 2000-8103 discloses a removal composition comprising 5 to 15% by weight of an alkanolamine, 35 to 55% by weight of a sulfoxide or an anthraquinone compound, and 35 to 55% by weight of a glycol ether. Korean Patent Laid-Open Publication No. 2000-8553 discloses a removal composition ίο 1362571 which comprises 10 to 30% by weight of a water-soluble amine compound and 7 to 9% by weight of diethyl 2 Alcohol monoalkyl ethers and N-alkylpyrrolidone or hydroxyalkylpyrrolidine. However, although the above composition has a small corrosive force to metal, it has a disadvantage of poor removal ability at a low temperature. 5 Also, in a lift_off process, after the photoresist is applied to the entire surface and patterned, a metal film or an insulating film (such as a hafnium oxide film or a tantalum nitride film) will be deposited thereon. And remove its photoresist. Therefore, the advantage is that the step of patterning the film can be omitted. However, since the photoresist is not exposed to the entire surface, it takes a long time to perform the photoresist removal step. Further, all of the above compositions have a photoresist removal time in the stripping process of 10 minutes or more, and aluminum or copper wires (on which the composition is applied) may suffer from the disadvantages of the money. 15 [Summary of the Invention] (Technical Problem) The inventor of the Luben case has a considerable research on the photoresist removal composition, which can remove the photoresist in a short time and has a pair in the stripping process (resistance removal step) The low-corrosion property of the metal film or the insulating film is based on the discovery that a photoresist removal group 20 is composed of a water-soluble organic amine compound and a predetermined ratio of a corrosion inhibitor. In the stripping process, the photoresist removal composition can completely remove the photoresist layer which is deteriorated by the ph〇t〇mh〇graphy process at a low temperature and in a short time; and even if only water is used (not isopropyl alcohol (intermediate rinsing solution)) for rinsing 'will still not damage the conductive layer under the photoresist to 25 and the insulating film; and for the conductive metal film under the photoresist and the insulating film
10 1510 15
有優異太的翁抑制能力，因而實現本發明之目的。 此本發明之一目的係在於提供一種光阻脫除組成 物’ f具有優秀的光阻脫除能力，並對導電層以及絕緣膜 具有高的損壞或腐蝕抑制能力。 本發月之另一目的係在於提供一種使用一光阻脫除 組成物以脫除光阻之方法。 本發明之又一目的係在於提供一種製造液晶顯示器 或半導體裝置之方法，其包括此脫除光阻方法。 (技術上解決方法） 本發明係將一光阻脫除組成物應用於含鋁、銅、或鋁 及銅之基板》其光阻脫除組成物包括：丨）一腐蝕抑制劑， 其包含至少一化合物，其係選自由式丨、2、以及3所組成之 群組，2)—水溶性有機胺化合物，其使用量為2至5〇倍重量 之腐蝕抑制劑的重量；以及3)—極性溶劑； [式1]There is an excellent ability to suppress the worms, thereby achieving the object of the present invention. SUMMARY OF THE INVENTION An object of the present invention is to provide a photoresist removal composition 'f which has excellent photoresist removal ability and which has high damage or corrosion inhibiting ability to a conductive layer and an insulating film. Another object of this month is to provide a method of removing the photoresist using a photoresist to remove the photoresist. It is still another object of the present invention to provide a method of fabricating a liquid crystal display or semiconductor device including the method of removing photoresist. (Technical Solution) The present invention relates to a photoresist removal composition applied to a substrate containing aluminum, copper, or aluminum and copper. The photoresist removal composition includes: a corrosion inhibitor comprising at least a compound selected from the group consisting of hydrazines, 2, and 3, 2) a water-soluble organic amine compound in an amount of 2 to 5 times the weight of the corrosion inhibitor; and 3) Polar solvent; [Formula 1]
OH 其中，R1及R2互為相同或不同，且分別獨立為氫或羥 基，且 R3為氫、叔丁基、羧酸基（-COOH)、曱酯基 20 (-COOCH3)、乙醋基（-C00C2H5)、或丙酯基（-CO〇C3H7)， [式2] 12 5 【實施方式】 本發明光阻脫除組成物之組成份將詳述如下。 於本發明之光阻脫除組成物中，較佳為，使用不會 ，下部位的導電金屬膜或絕緣膜造成傷害的化合物作為 ▲钱抑制齊J纟發明之該腐姓抑制劑，即使以水而非 Π内醇（中間物沖洗溶液）作沖洗，仍可防止—導電層 (:鋁或鋁合金膜）或絕緣膜被腐蝕。 10 15 :般而言’當僅以水而不使用異丙醇卜#間物沖洗溶 洗時，脫除射之胺類化合物將與水^合產生驗性 :有強腐蝕特性)之氫氧根離子’如此則引起金屬的腐蝕。 ’’、、而於本發财，該腐射卩制劑即使於驗性狀態下，亦 可與鋁形成-複合物’並吸附於鋁表面 膜，進而防止氣氧根離子之腐飯作用發生。/成保 相較於廣泛使用作為銅膜腐蝕抑制劑之苯并三唑 _ # 13Ζ〇10及甲苯并二唾⑽yltriaz〇le)，本發明光阻脫 …及、物中之式卜2、或3腐姓抑制劑苯并三唾苯并三峻且 有顯著更好的腐姓抑制特性。據此，即使僅添加少量的腐 20 餘抑制劑，光阻下部位的導電層（如：銅或銅合金膜）亦不會 被腐餘’且該腐钱抑制劑非常適用於移除硬化光阻 物質》 -式1、2、或3腐蝕抑制劑之防腐機制如下所述。於式^ 所不之腐飯抑制劑令，直接接至於苯環上之氫氧基係吸附 於紐上以控制驗溶液對金屬的腐餃作用^於式2、或3所示 之腐敍抑制劑中’二氮唾環⑻咖⑷中充足的氮原子之未 14 25 1362571 共用電子將與銅電性鍵結（electronically bonded)，以控制金 屬的腐触作用。 於本發明之光阻脫除組成物中，其腐蝕抑制劑可為式1 化合物與式2或3化合物所組成之混合物。 5 於本發明之光阻脫除組成物中，以組成物之總重量為 基準’其腐蝕抑制劑之含量較佳為〇.〇1至5wt%，且更佳為， 0.1至lwt%。若該腐蝕抑制劑之含量少於0 01wt%，則當使 預備進行脫除程序之基板與脫除劑接觸一段長時間後，其 φ 金屬線可能會部分遭到腐蝕。當該腐蝕抑制劑之含量多於 10 5wt%時’黏性會增加而造成脫除能力減低，且由於組成份 的價格提1¾ ’因而無法符合經濟效益。 • 於本發明之光阻脫除組成物中，較佳為，2)水溶性有 機胺化合物係至少一選自由一級氨基醇化合物、二級氨基 醇化合物、以及三級氨基醇化合物所組成之群組。 15 該氨基醇化合物較佳係至少一選自由乙醇胺（MEA)、 1-氨基異丙醇（AIP)、2-氨基-1-丙醇、N-曱氨基乙醇 • (N-methylaminoethanol，N-MAE)、3-氨基-1-丙醇、4-氨基 -1-丁醇、2-(2-氨基乙氧基）-1-乙醇（AEE)、2-(2-氨基乙氨 基）-1-乙醇（2-(2-aminoethylamino)-l-ethanol)、二乙醇胺 2〇 (diethanolamine，DEA)、三乙醇胺（triethanolamine，TEA)、 以及羥乙基哌°桊（hydroxyethylpiperazine，HEP)所組成之群 組。以脫除特性、腐蝕抑制特性、以及經濟效應而言，更 佳係，使用2-(2-氨基乙氧基）-1-乙醇（AEE) » 該水溶性有機胺類化合物之含量可為腐蝕抑制劑之2 15 1362571 至50倍，且較佳係，以組成物之總重量為基準，為1至 60wt%，且更佳為3至30wt%。若該水溶性有機胺類化合物 .之含量少於lwt%，則脫除變質光阻之能力不理想。若該水 溶性有機胺類化合物之含量多於60wt%，由於剝離製程期間 5 黏稠度增加，而造成光阻塗佈的分散性降低，進而增加脫 除的時間。再者，不預期的光阻下層導電金屬膜的腐蝕則 會增加。 於本發明之光阻脫除組成物中，當1)腐蝕抑制劑為二 或二種以上組成份之混合時，2)水溶性有機胺化合物較佳 10 係為一級氨基醇化合物，且更佳為2-(2-氨基乙氧基）-1-乙醇 (AEE)。 於本發明之光阻脫除組成物中，3)極性溶劑與水及有 機化合物共溶性極佳，以作為溶解光阻之溶劑。此外，其 極性溶劑會降低脫除劑之表面張力，以增脫除劑對光阻層 15 之潤濕能力。 較佳為，極性溶劑具有lcP或更低的黏度，以及150°C 或更高的沸點。其極性溶劑之特殊範例包括：N-甲基吡咯 烷酮（NMP)、1,3-二曱基-2-咪唑啉酮（DMI)、二曱基亞砜 (DMSO)、二曱基乙醯胺（DMAc)、二甲基曱醯胺（DMF)、 2〇 N-曱基曱醯胺（N-methylformamide，NMF)、環丁颯 (tetramethylenesulfone)、或其混合物。 以組成物之總重量為基準，該極性溶劑之含量，較佳 為1至95wt%，更佳為35至95wt%，而最佳係為50至95wt%。 若該極性溶劑之含量為lwt%或更少，該脫除劑之黏性則會 16 1362571 增加，因而降低了脫除劑的脫除能力。因此，較佳為，使 其重量增加越多越好。 此外，本發明之其光阻脫除組成物更可包括一水溶性 非離子性之界面活性劑。 5 再者’本發明之該光阻脫除組成物更可包括一非極性 溶劑。 非極性溶劑之相關範例可包括：BDG (二乙二醇單丁基 峻）、EDG (乙基二乙二醇 ’ ethyl diglycol)、MDG (曱基二 # 乙二醇，methy1 diglycol)、TEG (三甘醇，triethylene 10 giycol)、以及 DEM (二乙二酵乙醚，diethyleneglycol monoethyl ether) ° - 以組成物之總重重為基準，該非極性溶劑之含量，較 佳為，〇至40wt%。該非極性溶劑之含量較佳是越低越好。 當非極性溶劑之含量增加時，其脫除能力會降低而產生不 15純物，且會由於使用的光阻量增加而造成良率的降低。 本發明之光阻脫除組成物不會對光阻下部位的導電層 • &絕緣膜造成傷害’且對光阻下部位的導電金屬膜及絕緣 膜具有優異的腐蝕抑制特性。 該導電金屬膜或絕緣膜可為單層或含紹、銅或其合金 20之二或多層之多層膜，或可為單層或含铭、銅或其合金、 以及敍、钥或其合金之二或多層之多層膜。 -般而言’於半導體褒置及液晶顯示器的製造過程 中’須進行-或多種之光阻製程。此外，塗佈於基板上之 導電金屬膜或絕緣膜可為單層膜或具有二或多層包含紹及 1362571 /或銅之多層膜。於相關技術中，不同的光阻脫除劑於光阻 步驟—被使用於-上方形成含鋁之導電金屬膜或絕緣膜之 基板’以及被使用於-上方形成含銅之導電金屬膜或絕緣 膜之基板。 5 然而，本發明之光阻脫除組成物對於基板（包含鋁、 銅、或鋁與銅之導電金屬膜，或絕緣膜係形成於其上）具有 優秀的脫除力以及腐蝕力。也就是，本發明之一般用途之 光阻脫除組成物包括一預定比例之水溶性有機胺化合物以 • 及腐蝕抑制劑，而可應用於任何含鋁及/或銅之基板上。 10 此外，本發明係提供一種將光阻由一包含鋁、銅、或 在呂與銅之基板上方脫除之方法。該方法包括：1}將光阻塗 ' 佈於一上方具有導電金屬膜或絕緣膜形成之基板上；2)圖 • 案化形成於該基板上之該光阻；3)以圖案化光阻膜作為一 光罩刻導電金屬膜或絕緣膜；以及4)使用本發明之光 15 阻脫除組成物將光阻層脫除。 再者，本發明係提供一種將光阻由一包含鋁、銅、或 Φ *呂與銅之基板上方脫除之方法。該方法包括：1)將光阻塗 佈於基板整面；2)圖案化於基板上之該光阻；3)沉積一導電 金屬膜或一絕緣膜於形成有圖案化光阻之基板上丨以及4) 20 使用本發明之光阻脫除組成物將光阻脫除。 於脫除光阻之方法中，其導電金屬膜或絕緣膜可為單 層或含铭、銅或其合金之二或多層之多層膜，或可為單層 ，含銘、銅或其合金、以及斂、翻或其合金之二或多層之 多層膜。尤其，較佳係為一 A1_Nd/M〇雙層膜或Cu/M〇x。 18 1362571 以本發明之光阻脫除組成物，將光阻由基板上方脫除 之方法中（基板上方具有精細線路圖案），可進行浸泡步驟 (其中待進行脫除程序之基板係同時浸泡於一大量的脫除 劑中）及單一晶圓處理步驟（其中脫除劑係一個接著一個噴 麗於基板上方，以移除光阻）達成。OH wherein R1 and R2 are the same or different from each other, and are independently hydrogen or hydroxy, and R3 is hydrogen, tert-butyl, carboxylic acid (-COOH), oxime 20 (-COOCH3), ethyl acetate ( -C00C2H5), or a propyl ester group (-CO〇C3H7), [Formula 2] 12 5 [Embodiment] The components of the photoresist removal composition of the present invention will be described in detail below. In the photoresist removal composition of the present invention, it is preferred that the compound which does not cause damage to the conductive metal film or the insulating film in the lower portion is used as the inhibitor of the stagnation of the invention, even if Water, rather than sputum alcohol (intermediate rinsing solution) for rinsing, prevents the conductive layer (: aluminum or aluminum alloy film) or insulating film from being corroded. 10 15 : Generally speaking, when the water is washed by water instead of isopropyl alcohol, the amine compound which is removed from the shot will be combined with water to produce hydrogen chloride which has strong corrosive properties. The root ion 'so causes corrosion of the metal. The sputum sputum preparation can form a complex with aluminum and adsorb it on the aluminum surface film even in the presence of the present invention, thereby preventing the action of the gas oxygen ion. Compared with benzotriazole _ #13Ζ〇10 and toluene (10) yltriaz〇le which are widely used as copper film corrosion inhibitors, the photoresist of the present invention is in the form of 3 The rot-inhibitor benzotris-tris-benzotrim has a significantly better inhibition property of rot. Accordingly, even if only a small amount of rotant is added, the conductive layer under the photoresist (such as copper or copper alloy film) will not be spoiled' and the rot is very suitable for removing hardened light. The anti-corrosion mechanism of the corrosion inhibitor of Formula 1, 2, or 3 is as follows. In the formula, the fermented rice inhibitor is directly attached to the benzene ring, and the hydroxyl group is adsorbed on the ruthenium to control the effect of the test solution on the rot of the metal. The inhibition of the rot is shown in Formula 2 or 3. In the agent, the diazoxide ring (8) coffee (4) has sufficient nitrogen atoms. 14 25 1362571 The shared electrons will be electronically bonded to the copper to control the corrosion of the metal. In the photoresist removal composition of the present invention, the corrosion inhibitor may be a mixture of the compound of the formula 1 and the compound of the formula 2 or 3. 5 In the photoresist removal composition of the present invention, the content of the corrosion inhibitor is preferably from 〇1 to 5 wt%, and more preferably from 0.1 to 1 wt%, based on the total weight of the composition. If the content of the corrosion inhibitor is less than 0.01% by weight, the φ metal wire may be partially corroded when the substrate to be subjected to the removal process is brought into contact with the remover for a long period of time. When the content of the corrosion inhibitor is more than 10 5 wt%, the viscosity is increased to cause a decrease in the removal ability, and the price of the component is increased by 13⁄4 ′. In the photoresist removal composition of the present invention, preferably, 2) the water-soluble organic amine compound is at least one selected from the group consisting of a primary amino alcohol compound, a secondary amino alcohol compound, and a tertiary amino alcohol compound. group. 15 Preferably, the amino alcohol compound is at least one selected from the group consisting of ethanolamine (MEA), 1-aminoisopropanol (AIP), 2-amino-1-propanol, and N-methylaminoethanol (N-MAE). ), 3-amino-1-propanol, 4-amino-1-butanol, 2-(2-aminoethoxy)-1-ethanol (AEE), 2-(2-aminoethylamino)-1- Group of 2-(2-aminoethylamino)-l-ethanol, diethanolamine (DEA), triethanolamine (TEA), and hydroxyethylpiperazine (HEP) . In terms of removal characteristics, corrosion inhibition characteristics, and economic effects, it is more preferable to use 2-(2-aminoethoxy)-1-ethanol (AEE) » The content of the water-soluble organic amine compound can be corroded The inhibitor is 2 15 1362571 to 50 times, and more preferably 1 to 60% by weight, and more preferably 3 to 30% by weight based on the total weight of the composition. If the content of the water-soluble organic amine compound is less than 1% by weight, the ability to remove the deteriorated photoresist is not satisfactory. If the content of the water-soluble organic amine compound is more than 60% by weight, the viscosity of the photoresist coating is lowered due to an increase in the viscosity during the peeling process, thereby increasing the removal time. Furthermore, the corrosion of the underlying conductive metal film of the photoresist is increased as expected. In the photoresist removal composition of the present invention, when 1) the corrosion inhibitor is a mixture of two or more components, 2) the water-soluble organic amine compound is preferably a primary amino alcohol compound, and more preferably Is 2-(2-aminoethoxy)-1-ethanol (AEE). In the photoresist removal composition of the present invention, 3) the polar solvent is excellent in compatibility with water and an organic compound as a solvent for dissolving the photoresist. In addition, its polar solvent reduces the surface tension of the remover to increase the wetting ability of the remover to the photoresist layer 15. Preferably, the polar solvent has a viscosity of lcP or lower, and a boiling point of 150 ° C or higher. Specific examples of polar solvents include: N-methylpyrrolidone (NMP), 1,3-dimercapto-2-imidazolidinone (DMI), dimercaptosulfoxide (DMSO), dimercaptoacetamide ( DMAc), dimethyl decylamine (DMF), 2 N-methylformamide (NMF), tetramethylenesulfone, or a mixture thereof. The content of the polar solvent is preferably from 1 to 95% by weight, more preferably from 35 to 95% by weight, based on the total weight of the composition, and most preferably from 50 to 95% by weight. If the content of the polar solvent is 1% by weight or less, the viscosity of the remover is increased by 16 1362571, thereby reducing the removal ability of the remover. Therefore, it is preferable to increase the weight as much as possible. Further, the photoresist removal composition of the present invention may further comprise a water-soluble nonionic surfactant. Further, the photoresist removal composition of the present invention may further comprise a non-polar solvent. Examples of non-polar solvents may include: BDG (diethylene glycol monobutyl sulphate), EDG (ethyl diethylene glycol 'ethyl diglycol), MDG (mercapto-diethylene glycol, methy1 diglycol), TEG (three-glycan) Alcohol, triethylene 10 giycol), and DEM (diethyleneglycol monoethyl ether) ° - The content of the non-polar solvent is preferably from 40% by weight based on the total weight of the composition. The content of the non-polar solvent is preferably as low as possible. When the content of the non-polar solvent is increased, the removal ability is lowered to produce a purity of 15 and the yield is lowered due to an increase in the amount of photoresist used. The photoresist removal composition of the present invention does not cause damage to the conductive layer and the insulating film at the lower portion of the photoresist, and has excellent corrosion-suppressing properties to the conductive metal film and the insulating film at the lower portion of the photoresist. The conductive metal film or the insulating film may be a single layer or a multilayer film containing two or more layers of copper, copper or alloys thereof, or may be a single layer or containing an inscription, copper or an alloy thereof, and a syllabary or a key thereof. Two or more multilayer films. Generally speaking, in the manufacturing process of semiconductor devices and liquid crystal displays, it is necessary to perform - or a plurality of photoresist processes. Further, the conductive metal film or the insulating film coated on the substrate may be a single layer film or have two or more layers including a multilayer film of 1362571 / or copper. In the related art, different photoresist removal agents are used in the photoresist step—the substrate on which the aluminum-containing conductive metal film or the insulating film is formed—and used to form a copper-containing conductive metal film or insulation. The substrate of the film. 5 However, the photoresist removal composition of the present invention has excellent release force and corrosive force for a substrate (a conductive metal film containing aluminum, copper, or aluminum and copper, or an insulating film formed thereon). That is, the general-purpose photoresist removal composition of the present invention comprises a predetermined proportion of a water-soluble organic amine compound and a corrosion inhibitor, and can be applied to any substrate containing aluminum and/or copper. Further, the present invention provides a method of removing photoresist from a substrate comprising aluminum, copper, or a substrate of argon and copper. The method comprises: 1} coating a photoresist on a substrate formed with a conductive metal film or an insulating film; 2) patterning the photoresist formed on the substrate; 3) patterning the photoresist The film is used as a reticle to engrave a conductive metal film or an insulating film; and 4) the photoresist 15 is removed using the light 15 of the present invention to remove the composition. Furthermore, the present invention provides a method of removing photoresist from a substrate comprising aluminum, copper, or Φ*Lu and copper. The method comprises: 1) applying a photoresist to the entire surface of the substrate; 2) patterning the photoresist on the substrate; 3) depositing a conductive metal film or an insulating film on the substrate on which the patterned photoresist is formed. And 4) 20 removing the photoresist using the photoresist removal composition of the present invention. In the method for removing photoresist, the conductive metal film or the insulating film may be a single layer or a multilayer film containing two or more layers of indium, copper or an alloy thereof, or may be a single layer containing an inscription, copper or an alloy thereof. And a multilayer film of two or more layers of agglomerates, turns or alloys thereof. In particular, it is preferably an A1_Nd/M〇 bilayer film or Cu/M〇x. 18 1362571 The method for removing the photoresist of the present invention and removing the photoresist from the upper side of the substrate (with a fine line pattern above the substrate) can be subjected to a soaking step (where the substrate to be subjected to the removal process is simultaneously immersed in A large amount of the removal agent) and a single wafer processing step (where the removal agent is sprayed one over the other to remove the photoresist).
ίο 15 20 25 本發明光阻脫除組成物可脫除之光阻相關範例係包 括：一正型光阻、一負型光阻、以及一正/負雙型光阻。可 使用之光阻之相關範例，其組成份並無限制，可包括：包 含光反應化合物（具有熱塑性酚醛樹脂型之酚醛樹脂以及 重敗萘醌（diazonaphthoquinone))之光阻。 此外，本發明係提供一製造液晶顯示器或半導體裝置 之方法。該方法包括光阻脫除之方法。 使用本發明之方法製造出之液晶顯示器或半導體裝 置，其基板上之精細圖案不會於光阻脫除期間被腐蝕或破 壞’且殘餘之光阻量很少。 本發明係提供-光阻脫除組成物，其可於高溫及低溫 且於-短期間内輕易地移除光微影製程中變質之光阻層， 並且’即使僅使用水而非異丙醇（_中間㈣洗溶液）進^冲 ^ ’亦不會使光阻下部位之銘、紹合金、銅、或銅合金作 成之導電層以及絕緣膜受腐蝕。 尤其，於本發明令，該由於過度光微影製程而變質之 =阻層可於-短期間内低溫下（於剝離製料光阻脫除期 間）元全被脫除。 【實施方式】 1362571 在以下文字中將以實施例詳細描述本發明。然而該實 施例僅為說明用，並不會對發明權力之範圍有所限制。於 以下實施例以及比較例中’其各個組成的比例除非有特別 標示，皆為重量比。 5 <實施例1至33> 所使用之組成物以及組成比例係如下表1所示，於室溫 下攪拌2小時，而產物係為經由過濾得到具有〇.1μιη尺寸之 顆粒。如此則可得到一脫除劑溶液。Ίο 15 20 25 Examples of photoresists that can be removed by the photoresist removal composition of the present invention include: a positive photoresist, a negative photoresist, and a positive/negative dual photoresist. Examples of the photoresist that can be used are not limited in terms of composition, and may include: a photoresist containing a photoreactive compound (a phenolic resin having a thermoplastic phenol resin type and a diazonaphthoquinone). Further, the present invention provides a method of manufacturing a liquid crystal display or a semiconductor device. The method includes a method of photoresist removal. A liquid crystal display or semiconductor device fabricated by the method of the present invention has a fine pattern on the substrate which is not corroded or broken during photoresist removal' and the residual photoresist is small. The present invention provides a photoresist removal composition which can easily remove a deteriorated photoresist layer in a photolithography process at high temperature and low temperature and for a short period of time, and 'even if only water is used instead of isopropanol (_Intermediate (four) washing solution) into the ^ ^ ^ will not make the conductive layer under the photoresist, the alloy, copper, or copper alloy made of conductive layer and insulating film corrosion. In particular, in the present invention, the resist layer which is deteriorated due to the excessive photolithography process can be completely removed at a low temperature (during the stripping photoresist removal period) during a short period of time. [Embodiment] 1362571 In the following text, the present invention will be described in detail by way of examples. However, the examples are for illustrative purposes only and do not limit the scope of the invention. In the following examples and comparative examples, the ratios of the respective compositions are weight ratios unless otherwise specified. 5 <Examples 1 to 33> The compositions and composition ratios used were as shown in Table 1 below, and stirred at room temperature for 2 hours, and the product was obtained by filtration to obtain particles having a size of 0.1 μm. Thus, a remover solution can be obtained.
1010
<比較例1至6> 使用同實施例1相同步驟以及下表1之組成物以及組 成比例製得一脫除劑溶液。 【表1】 項目 組成份（重量份） 水溶性有機胺化合物 溶劑 腐餘抑制劑 Type 份量 Type 份量 Cl C2 實施例1 AEE 5 NMF 94.2 0.5 0.3 NMF 30 實施例2 AEE 7 NMP 12.5 0.5 0.3 DMAc 49.7 NMF 30 實施例3 AEE 7 0.5 〇 Ί. DMAc 62.2 NMF 30 實施例4 AEE 7 NMP 5 0.5 0.3 DMAc 57.2 ***_ 1362571<Comparative Examples 1 to 6> A remover solution was prepared using the same procedure as in Example 1 and the composition of Table 1 below and the composition. [Table 1] Item Composition (parts by weight) Water Soluble Organic Amine Compound Solvent Corrosion Inhibitor Type Part Size Type Partition Cl C2 Example 1 AEE 5 NMF 94.2 0.5 0.3 NMF 30 Example 2 AEE 7 NMP 12.5 0.5 0.3 DMAc 49.7 NMF 30 Example 3 AEE 7 0.5 〇Ί. DMAc 62.2 NMF 30 Example 4 AEE 7 NMP 5 0.5 0.3 DMAc 57.2 ***_ 1362571
NMF 30 實施例5 AEE 5 NMP 12.5 0.5 0.3 DMAc 51.7 NMF 10 實施例6 AEE 5 NMP 12.5 0.5 0.3 DMAc 71.7 實施例7 AEE 5 DMAc 94.2 0.5 0.3 實施例8 AEE 5 NMP 94.2 0.5 0.3 NMF 10 實施例9 AEE 7 NMP 12.5 0.5 0.3 DMAc 69.7 實施例10 AEE 7 NMF 92.2 0.5 0.3 NMF 10 實施例11 AEE 3 NMP 12.5 0.5 0.3 DMAc 73.7 NMF 30 實施例12 AEE 3 NMP 12.5 0.5 0.3 DMAc 53.7 實施例13 AEE 3 NMF DMAc 30 66.2 0.5 0.3 實施例14 AEE 3 NMP 96.2 0.5 0.3 實施例15 AEE 3 NMF 96.2 0.5 0.3 NMF 10 實施例16 AEE 10 NMP 12.5 0.5 0.3 DMAc 66.7 21 1362571NMF 30 Example 5 AEE 5 NMP 12.5 0.5 0.3 DMAc 51.7 NMF 10 Example 6 AEE 5 NMP 12.5 0.5 0.3 DMAc 71.7 Example 7 AEE 5 DMAc 94.2 0.5 0.3 Example 8 AEE 5 NMP 94.2 0.5 0.3 NMF 10 Example 9 AEE 7 NMP 12.5 0.5 0.3 DMAc 69.7 Example 10 AEE 7 NMF 92.2 0.5 0.3 NMF 10 Example 11 AEE 3 NMP 12.5 0.5 0.3 DMAc 73.7 NMF 30 Example 12 AEE 3 NMP 12.5 0.5 0.3 DMAc 53.7 Example 13 AEE 3 NMF DMAc 30 66.2 0.5 0.3 Example 14 AEE 3 NMP 96.2 0.5 0.3 Example 15 AEE 3 NMF 96.2 0.5 0.3 NMF 10 Example 16 AEE 10 NMP 12.5 0.5 0.3 DMAc 66.7 21 1362571
NMF 30 實施例17 AEE 10 NMP 12.5 0.5 0.3 DMAc 46.7 實施例18 AEE 10 NMF DMAc 30 59.2 0.5 0.3 實施例19 AEE 10 NMF 89.2 0.5 0.3 實施例20 AEE 20 NMF 79.2 0.5 0.3 實施例21 AEE 30 NMF 69.2 0.5 0.3 NMF 30 實施例22 AEE 5 BDG 30 0.5 0.3 DMAc 34.2 NMF 30 實施例23 AEE 5 MDG 30 0.5 0.3 DMAc 34.2 NMF 30 實施例24 AEE 5 EDG 30 0.5 0.3 DMAc 34.2 NMF 30 實施例25 AEE 10 BDG 30 0.5 0.3 DMAc 29.2 NMF 30 實施例26 AEE 10 MDG 30 0.5 0.3 DMAc 29.2 NMF 30 實施例27 AEE 10 EDG 30 0.5 0.3 DMAc 29.2 22 1362571NMF 30 Example 17 AEE 10 NMP 12.5 0.5 0.3 DMAc 46.7 Example 18 AEE 10 NMF DMAc 30 59.2 0.5 0.3 Example 19 AEE 10 NMF 89.2 0.5 0.3 Example 20 AEE 20 NMF 79.2 0.5 0.3 Example 21 AEE 30 NMF 69.2 0.5 0.3 NMF 30 Example 22 AEE 5 BDG 30 0.5 0.3 DMAc 34.2 NMF 30 Example 23 AEE 5 MDG 30 0.5 0.3 DMAc 34.2 NMF 30 Example 24 AEE 5 EDG 30 0.5 0.3 DMAc 34.2 NMF 30 Example 25 AEE 10 BDG 30 0.5 0.3 DMAc 29.2 NMF 30 Example 26 AEE 10 MDG 30 0.5 0.3 DMAc 29.2 NMF 30 Example 27 AEE 10 EDG 30 0.5 0.3 DMAc 29.2 22 1362571
實施例28 AEE 5 NMF BDG DMAc 30 15 49.2 0.5 0.3 NMF 30 實施例29 AEE 5 MDG 15 0.5 0.3 DMAc 49.2 NMF 30 實施例30 AEE 5 EDG 15 0.5 0.3 DMAc 49.2 NMF 30 實施例31 AEE 10 BDG 15 0.5 0.3 DMAc 44.2 NMF 30 實施例32 AEE 10 MDG 15 0.5 0.3 DMAc 44.2 NMF 30 實施例33 AEE 10 EDG 15 0.5 0.3 DMAc 44.2 比較例1 AEE 5 BDG 94.2 0.5 0.3 比較例2 AEE 5 EDG 94.2 0.5 0.3 比較例3 AEE 5 MDG 94.2 0.5 0.3 比較例4 AEE 10 BDG 89.2 0.5 0.3 比較例5 MEA 10 BDG 89.2 0.5 0.3 比較例6 NMAE 10 EDG 89.2 0.5 0.3 ※AEE :2-(2-氨基乙氧基）-1-乙醇， 23 1362571 NMF : N-曱基曱醯胺， NMP : N-曱基吡咯烷酮， DMAc :二曱基乙醯胺， MEA :乙醇胺， NMAE : N-曱氨基乙醇， BDG:二乙二醇單丁基醚， EDG :二乙二醇單乙基驗（diethylene glycol monoethyl ether)， MDG :二乙二醇甲醚（methyl diglycol)， 10 Cl :下述式5之化合物， [式5]Example 28 AEE 5 NMF BDG DMAc 30 15 49.2 0.5 0.3 NMF 30 Example 29 AEE 5 MDG 15 0.5 0.3 DMAc 49.2 NMF 30 Example 30 AEE 5 EDG 15 0.5 0.3 DMAc 49.2 NMF 30 Example 31 AEE 10 BDG 15 0.5 0.3 DMAc 44.2 NMF 30 Example 32 AEE 10 MDG 15 0.5 0.3 DMAc 44.2 NMF 30 Example 33 AEE 10 EDG 15 0.5 0.3 DMAc 44.2 Comparative Example 1 AEE 5 BDG 94.2 0.5 0.3 Comparative Example 2 AEE 5 EDG 94.2 0.5 0.3 Comparative Example 3 AEE 5 MDG 94.2 0.5 0.3 Comparative Example 4 AEE 10 BDG 89.2 0.5 0.3 Comparative Example 5 MEA 10 BDG 89.2 0.5 0.3 Comparative Example 6 NMAE 10 EDG 89.2 0.5 0.3 *AEE : 2-(2-aminoethoxy)-1-ethanol, 23 1362571 NMF : N-mercaptoamine, NMP : N-decylpyrrolidone, DMAc : dimercaptoacetamide, MEA : ethanolamine, NMAE : N-nonylaminoethanol, BDG: diethylene glycol monobutyl Ether, EDG: diethylene glycol monoethyl ether, MDG: methyl diglycol, 10 Cl : a compound of the following formula 5, [Formula 5]
OHOH
HO C2 :下述式6之化合物 15 [式 6]HO C2 : a compound of the following formula 6 [Formula 6]
<實驗例 >剝離之脫除能力以及腐蝕特性之評估 24 1362571 該實施例1至33以及比較例1至6之脫除組成物之脫除 能力以及腐蝕特性係經由以下方法作測試。 用以作測試之樣本，將取以下兩種樣本作測試。以剝 離製程製備之一晝素層玻璃基板，其2,000埃之Al-Nd層係 5 製作於玻璃上並接著進行閘極製程，將200埃之Mo層形成 於其上（於LCD之TFT線路製作過程中），使用包含酚醛樹脂 (novolac resin)以及PAC之正型光阻並乾燥，並經由光微影 製程形成圖案，以及使用濕式蝕刻製備一樣本。將300埃之 鉬合金形成於玻璃基板之後，接著進行閘極製程以形成 10 2,000埃之銅層於其上，使用包含酚醛樹脂以及PAC之正型 光阻並乾燥，並經由光微影製程形成圖案，以及使用濕式 蝕刻製備另一樣本。 1.脫除能力之測試 15 將樣本浸泡於脫除劑溶液中，並維持於70°C及50°C之 溫度1分鐘，使用去離子水沖洗30秒，並使用氮氣乾燥。完 全乾燥後，將樣本以一光學式顯微鏡放大1，〇〇〇倍以及電子 顯微鏡（FE-SEM)放大5,000至10,000倍觀察其光阻之脫除情 形。其脫除成效係以以下方式做標示。 20 ※ ◎ :優異的脫除效率， 〇 :可接受的脫除效率， Δ :不可接受的脫除效率， X ； :低下的脫除脫除效率。 25 2. —次腐钱之觀察 25 1362571 關於一次腐蝕之評估係為脫除步驟後以去離子水作 沖洗時進行腐蝕之情形的觀察。將樣本浸泡於丙酮中並維 持在40°C的溫度10分鐘，接著以異丙醇沖洗30秒以及去離 子水30秒，並待測。將待測樣本浸泡於常溫下含50g之脫除 5 劑溶液以及950g之水之混合溶液3分鐘，接著以去離子水沖 洗30秒，並以氮氣乾燥之。其樣本之表面、側面、以及切 塊係使用一電子顯微鏡（？丑-3£1^[)於50,000至100,000之倍率 下觀察其腐蝕情形。 其腐蝕情形係以以下方式做標示。 10 ※◎: Al-Nd以及Mo線路之表面及側面沒有被腐蝕， 〇：Al-Nd以及Mo線路之表面及側面有輕微的腐蝕， △ : Al-Nd以及Mo線路之表面及側面有部分被腐蝕， X : Al-Nd以及Mo線路之表面及側面嚴重地被腐蝕。 15 3.二次腐蝕之觀察 將樣本浸泡於脫除劑中並維持在70 °C的溫度10分 鐘，接著以去離子水沖洗30秒，並以氮氣乾燥之。重複該 脫除測試三次，接著以電子顯微鏡（FE-SEM)於50,000至 100,000之倍率下觀察其樣本之表面、側面、以及切塊腐蝕 20 情形。其腐蝕情形係以以下方式做標示。 ※ ◎:銅金屬線之表面以及側面沒有被腐蝕， 〇：銅金屬線之表面以及側面有輕微的腐蝕， △:銅金屬線之表面以及側面有部分被腐蝕， X :銅金屬線之表面以及側面嚴重地被腐蝕。 25 脫除能力以及腐蝕性之測量結果係如表2所示。 26 1362571<Experimental Example > Evaluation of peeling removal ability and corrosion characteristics 24 1362571 The removal ability and corrosion characteristics of the removal compositions of Examples 1 to 33 and Comparative Examples 1 to 6 were tested by the following methods. For the sample used for testing, the following two samples will be tested. A bismuth layer glass substrate was prepared by a stripping process, and a 2,000 angstrom Al-Nd layer system 5 was formed on the glass and then subjected to a gate process, and a 200 angstrom Mo layer was formed thereon (made on the TFT circuit of the LCD). In the process, a positive photoresist comprising a novolac resin and a PAC is used and dried, and a pattern is formed via a photolithography process, and the same is prepared using wet etching. After forming a 300 angstrom molybdenum alloy on the glass substrate, a gate process is then performed to form a 10 2,000 angstrom copper layer thereon, and a positive photoresist comprising a phenol resin and a PAC is used and dried, and formed by a photolithography process. Pattern, and another sample was prepared using wet etching. 1. Test for removal ability 15 The sample was immersed in the remover solution and maintained at 70 ° C and 50 ° C for 1 minute, rinsed with deionized water for 30 seconds, and dried with nitrogen. After complete drying, the sample was magnified by an optical microscope, 〇〇〇 and electron microscopy (FE-SEM) were magnified 5,000 to 10,000 times to observe the removal of the photoresist. The effectiveness of the removal is marked in the following manner. 20 ※ ◎ : Excellent removal efficiency, 〇 : Acceptable removal efficiency, Δ : Unacceptable removal efficiency, X ; : Low removal efficiency. 25 2. Observation of Sub-corruption 25 1362571 The evaluation of primary corrosion is the observation of corrosion when it is rinsed with deionized water after the removal step. The sample was immersed in acetone and maintained at a temperature of 40 ° C for 10 minutes, followed by rinsing with isopropanol for 30 seconds and deionized water for 30 seconds, and was tested. The sample to be tested was immersed in a mixed solution containing 50 g of a 5 dose solution and 950 g of water at normal temperature for 3 minutes, followed by washing with deionized water for 30 seconds, and dried with nitrogen. The surface, side, and dicing of the sample were observed for corrosion using an electron microscope (? ug - 3 £ 1 ^ [) at a magnification of 50,000 to 100,000. The corrosion situation is marked in the following manner. 10 ※◎: The surface and side of the Al-Nd and Mo lines are not corroded. 〇: The surface and side of the Al-Nd and Mo lines are slightly corroded. △: Al-Nd and the surface and side of the Mo line are partially Corrosion, X: Al-Nd and the surface and side of the Mo line are severely corroded. 15 3. Observation of secondary corrosion The sample was immersed in the remover and maintained at a temperature of 70 ° C for 10 minutes, followed by rinsing with deionized water for 30 seconds, and dried with nitrogen. This removal test was repeated three times, and then the surface, side, and dicing corrosion of the sample were observed by electron microscopy (FE-SEM) at a magnification of 50,000 to 100,000. The corrosion situation is marked in the following manner. ※ ◎: The surface and side of the copper wire are not corroded. 〇: The surface and side of the copper wire are slightly corroded. △: The surface and side of the copper wire are partially corroded, X: the surface of the copper wire and The sides are severely corroded. 25 The measurement results of the removal ability and corrosivity are shown in Table 2. 26 1362571
【表2】 項目 脫除能力 腐蝕性 70°C 50°C Al-Nd Cu Mo 實施例1 ◎ ◎ ◎ ◎ ◎ 實施例2 ◎ ◎ ◎ ◎ ◎ 實施例3 ◎ ◎ ◎. ◎ ◎ 實施例4 ◎ ◎ ◎ ◎ ◎ 實施例5 ◎ ◎ ◎ ◎ ◎ 實施例6 ◎ ◎ ◎ ◎ ◎ 實施例7 〇 〇 ◎ ◎ ◎ 實施例8 〇 Δ ◎ ◎ ◎ 實施例9 ◎ ◎ ◎ ◎ ◎ 實施例10 ◎ ◎ ◎ ◎ ◎ 實施例11 ◎ ◎ ◎ ◎ ◎ 實施例12 ◎ ◎ ◎ ◎ ◎ 實施例13 ◎ ◎ ◎ ◎ ◎ 實施例14 〇 Δ ◎ ◎ ◎ 實施例15 ◎ ◎ ◎ ◎ 實施例16 ◎ ◎ ◎ ◎ ◎ 實施例17 ◎ ◎ ◎ ◎ ◎ 實施例18 ◎ ◎ ◎ ◎ ◎ 實施例19 ◎ ◎ ◎ ◎ ◎ 實施例20 ◎ ◎ ◎ ◎ ◎ 27 1362571[Table 2] Item removal ability Corrosivity 70 ° C 50 ° C Al-Nd Cu Mo Example 1 ◎ ◎ ◎ ◎ Example 2 ◎ ◎ ◎ ◎ ◎ Example 3 ◎ ◎ ◎. ◎ ◎ Example 4 ◎ ◎ ◎ ◎ Example 5 ◎ ◎ ◎ ◎ Example 6 ◎ ◎ ◎ ◎ ◎ Example 7 〇〇 ◎ ◎ ◎ Example 8 〇 Δ ◎ ◎ ◎ Example 9 ◎ ◎ ◎ ◎ ◎ Example 10 ◎ ◎ ◎ ◎ 实施 实施 实施 实施 实施 实施 实施 实施 实施 实施 实施 实施 实施 实施 实施 实施 实施 实施 实施 实施 实施 实施 实施 实施 实施 实施 实施 实施 实施 实施 实施 实施 实施 实施 实施 实施 实施 实施 实施 实施 实施 实施 实施 实施 实施 实施 实施 实施 实施 实施 实施 实施 实施 实施 实施 实施 实施 实施 实施 实施 实施 实施 实施 实施 实施 实施 实施 实施 实施 实施 实施 实施 实施 实施 实施 实施 实施 实施 实施 实施 实施 实施 实施 实施 实施Example 17 ◎ ◎ ◎ ◎ Example 18 ◎ ◎ ◎ ◎ Example 19 ◎ ◎ ◎ ◎ ◎ Example 20 ◎ ◎ ◎ ◎ ◎ 27 1362571
實施例21 ◎ ◎ ◎ ◎ ◎ 實施例22 〇 △ ◎ 〇 ◎ 實施例23 〇 Δ ◎ 〇 ◎ 實施例24 〇 △ ◎ 〇 ◎ 實施例25 〇 〇 〇 Δ ◎ 實施例26 〇 〇 〇 Δ ◎ 實施例27 〇 〇 〇 Δ ◎ 實施例28 〇 Δ ◎ 〇 ◎ 實施例29 〇 Δ ◎ 〇 ◎ 實施例30 〇 Δ ◎ 〇 ◎ 實施例31 〇 〇 〇 Δ ◎ 實施例32 〇 〇 〇 Δ ◎ 實施例33 〇 〇 〇 Δ ◎ t匕較例1 △ X 〇 〇 〇 比較例2 △ X 〇 〇 〇 比較例3 △ X 〇 〇 〇 比較例4 △ X Δ Δ Δ 比較例5 X X X X X 比較例6 X X X X XExample 21 ◎ ◎ ◎ ◎ Example 22 〇 △ ◎ 〇 ◎ Example 23 〇 Δ ◎ 〇 ◎ Example 24 〇 △ ◎ 〇 ◎ Example 25 〇〇〇 Δ ◎ Example 26 〇〇〇 Δ ◎ Example 27 〇〇〇Δ ◎ Example 28 〇Δ ◎ 〇 ◎ Example 29 〇Δ ◎ 〇 ◎ Example 30 〇Δ ◎ 〇 ◎ Example 31 〇〇〇Δ ◎ Example 32 〇〇〇Δ ◎ Example 33 〇 〇〇Δ ◎ t匕 Comparative Example 1 △ X 〇〇〇 Comparative Example 2 Δ X 〇〇〇 Comparative Example 3 Δ X 〇〇〇 Comparative Example 4 Δ X Δ Δ Δ Comparative Example 5 XXXXX Comparative Example 6 XXXXX
如表2所示，本發明之所有的脫除組成物皆具有優異.的 脫除能力以及腐蝕特性。 【圖式簡單說明】 28 1362571 圖1係為一液晶顯示器之光阻脫除步驟示意圖。 圖2係為以剝離製程進行光阻脫除步驟示意圖。 【主要元件符號說明】 5 無As shown in Table 2, all of the removal compositions of the present invention have excellent removability and corrosion characteristics. [Simple description of the diagram] 28 1362571 Figure 1 is a schematic diagram of the photoresist removal step of a liquid crystal display. FIG. 2 is a schematic view showing the step of removing the photoresist by a stripping process. [Main component symbol description] 5 None
2929
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| Publication number | Publication date |
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| KR100913048B1 (en) | 2009-08-25 |
| KR20070114038A (en) | 2007-11-29 |
| WO2007139315A1 (en) | 2007-12-06 |
| JP4773562B2 (en) | 2011-09-14 |
| TW200801855A (en) | 2008-01-01 |
| JP2009538456A (en) | 2009-11-05 |
| CN101454872A (en) | 2009-06-10 |
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| CN101454872B (en) | 2011-04-06 |
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