JP2005062259A - Resist-stripping liquid for substrate process in single-wafer processing cleaner, and stripping method using the same - Google Patents
Resist-stripping liquid for substrate process in single-wafer processing cleaner, and stripping method using the same Download PDFInfo
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Abstract
Description
【0001】
【発明の属する技術分野】
本発明は枚葉式洗浄装置の基板工程用レジスト剥離液及びそれを用いた剥離方法に関する。
【0002】
【従来の技術】
半導体製造工程で用いられるウェット洗浄装置は25〜50枚のウエハを一括処理するバッチ式とウエハを1枚ずつ処理する枚葉式に分類される。バッチ式は多くの洗浄溶液槽と純水リンス槽を装備する多槽式と1槽の中で種々の薬液洗浄と純水リンスを行う単槽式がある。従来、バッチ式の多槽式がマニュアル操作から全自動へと変遷しながら発展してきたが、近年、バッチ式の単槽式と枚葉式洗浄装置が特定の工程後の洗浄に用いられるようになってきた。今後は生産性向上のために大口径Siウエハ(径300mm又は450mm)が用いられていくためにウエハ面内での洗浄均一性が高く、また装置の設置面積が小さい枚葉式洗浄装置が主流になりつつある。
【0003】
従来、基板工程(Front End of Line 工程)におけるレジスト剥離は、従来はバッチ式洗浄装置において硫酸と過酸化水素水からなる混合溶液(SPM洗浄液)により行われてきた。典型的な使用条件としてはSPM洗浄液(硫酸:過酸化水素水=4:1)で10分間、100〜120℃で処理することにより行われる。
【0004】
しかしながら、枚葉式洗浄装置においては、装置的、コスト的な制限からSPM洗浄液のような濃厚で高温の溶液を用いることができなかった。また、装置的に引火点を有する薬液も望ましくなく、これまで、この洗浄装置に適した基板工程用のレジスト剥離液はなかった。
【0005】
【発明が解決しようとする課題】
本発明の目的は、高温で長時間剥離剤を使用できない装置、特に枚葉式洗浄装置で使用するのに好適なレジスト剥離液及びその使用方法を提供することである。すなわち、露出している多結晶Si(poly−Si)、Si酸化膜(SiO2)などにダメージを与えることなく、80℃以下の温度及び短時間(〜30秒)の条件下でレジスト及び反射防止膜を除去可能で、更に引火点を持たないレジスト剥離液を提供することにある。
【0006】
【課題を解決するための手段】
本発明者らは、枚葉式洗浄装置の基板工程用レジスト剥離液(以後レジスト剥離液)について鋭意検討した結果、シアノエチルエチレンジアミン、シアノエチルシクロヘキシルアミン、水、及び水酸化テトラメチルアンモニウム及び/又はアンモニアを含んでなる混合溶液がpoly−Si、SiO2などに与えるダメージが少なく、80℃以下の温度及び短時間(30秒以内、好ましくは〜15秒)の条件下でレジスト及び反射防止膜を除去することができ、更に引火点を持たないことを見出し、本発明を完成するに至った。
【0007】
すなわち、本発明は、シアノエチルエチレンジアミン、シアノエチルシクロヘキシルアミン、水、及び水酸化テトラメチルアンモニウム及び/又はアンモニアを必須成分とするレジスト剥離液及びそれを用いた剥離方法である。
【0008】
以下に本発明を詳細に説明する。
【0009】
本発明におけるレジスト剥離液は、低温短時間で剥離処理が必要な装置、特に枚葉式洗浄装置の基板工程において用いられる。ここで基板工程とは半導体製造工程の配線構造形成前までのいわゆるFEOL(Front End of Line)工程のことである。
【0010】
本発明において、剥離とは、フォトレジスト及び/又は反射防止膜を基板上に塗布した後、露光、現像し、エッチング、イオン注入などの処理を施し回路を形成した後、残ったレジスト及び/又は反射防止膜を除去することをいう。
【0011】
本発明のレジスト剥離液はフォトレジスト及び/又は反射防止膜を剥離するのに使用される。すなわち、フォトレジスト及び/又は反射防止膜を基板上に塗布した後、露光、現像し、エッチング、イオン注入などの処理を施し回路を形成した後、本発明のレジスト剥離液で剥離する。
【0012】
本発明のレジスト剥離液はシアノエチルエチレンジアミン、シアノエチルシクロヘキシルアミン、水、及び水酸化テトラメチルアンモニウム及び/又はアンモニアを含んでなる水溶液から成る。
【0013】
本発明のレジスト剥離液に使用するシアノエチルエチレンジアミン、シアノエチルシクロヘキシルアミンはレジスト及び/又は反射防止膜をウエハより剥離させ溶解させる作用がある。特に、シアノエチルシクロヘキシルアミンはレジスト、反射防止膜の溶解性に優れるが、水への溶解性が低いため、シアノエチルエチレンジアミンを添加することにより溶解度を高めることができる。
【0014】
シアノエチルエチレンジアミンは大過剰のエチレンジアミンにアクリロニトリルを反応させることにより容易に得ることができる。同様にシアノエチルシクロヘキシルアミンはシクロヘキシルアミンとアクリロニトリルを反応させることにより容易に得ることができる。原料となるエチレンジアミン、アクリロニトリル、シクロヘキシルアミンは一般的に市販されており容易に入手することができる。
【0015】
本発明のレジスト剥離液に使用する水酸化テトラメチルアンモニウム及び/又はアンモニアは、レジスト及び反射防止膜をウエハより剥離させる作用がある。水酸化テトラメチルアンモニウム又はアンモニアは水溶液として一般的に市販されており容易に入手することができるが、ウエハの清浄度を保つため、高純度品を使用するのが好ましい。
【0016】
本発明のレジスト剥離液のpHは10〜13であることが好ましく、特に好ましくは11〜13である。
【0017】
本発明の洗浄液の組成は必須成分であるシアノエチルエチレンジアミン、シアノエチルシクロヘキシルアミン、及び水酸化テトラメチルアンモニウム及び/又はアンモニアの組み合わせで調整するため、それぞれ使用する濃度により水への溶解度が変わり、2層分離したりするため、夫々の濃度を限定することは困難であるが、シアノエチルエチレンジアミンの含有量は0.1〜15重量%、特に、0.5〜10重量%が好ましい。この範囲を超えてシアノエチルエチレンジアミンの濃度を増加させても添加量に見合った効果が得られないだけでなく、poly−Si、SiO2にダメージを与えてしまう。濃度が少なすぎると短時間での剥離効果が不十分となるだけでなく、シアノエチルエチレンジアミンは水に難溶のシアノエチルシクロヘキシルアミンの相溶剤としても作用するためシアノエチルシクロヘキシルアミンの溶解度の低下を招く。
【0018】
シアノエチルシクロヘキシルアミンの含有量は0.1重量%〜5重量%、好ましくは1重量%〜5重量%である。この範囲を越えてシアノエチルシクロヘキシルアミンの濃度が増加すると、水に溶けず2層に分離し、少なすぎると剥離効果が小さくなる。
【0019】
水酸化テトラメチルアンモニウム及び/又はアンモニアの含有量は0.001〜0.1重量%、好ましくは0.005〜0.05重量%である。この範囲を超えて水酸化テトラメチルアンモニウム及び/又はアンモニアの濃度が増加すると剥離効果に優れるが、poly−Si、SiO2にダメージを与えてしまう。逆に少なすぎると短時間での剥離効果が不十分となる。
【0020】
本発明のレジスト剥離液は、レジストを剥離する際に各成分を添加して使用しても良いし、あらかじめ各成分を混合しておいてから使用しても良い。
【0021】
本発明のレジスト剥離液は、ネガ型、ポジ型を含めて、アルカリ性水溶液で現像できるi線用、KrFエキシマレーザー用等のレジストの剥離に利用できる。
【0022】
本発明のレジスト剥離液は、無機質基体上に塗布されたフォトレジスト膜、イオン注入などの処理をしたフォトレジスト層、反射防止膜を剥離する際に最も好適に用いられる。
【0023】
本発明のレジスト剥離液は枚葉式洗浄装置で使用され、洗浄時の温度は装置上の制限から20℃〜80℃が好ましい。また、洗浄時間は生産性の観点から30秒以内が好ましい。
【0024】
【実施例】
以下、本発明の方法を実施例により説明するが、本発明はこれらに限定されるものではない。
【0025】
実施例1〜4、比較例1〜7
KrFレジストウエハを表1に示す剥離液に80℃、15秒浸漬し、その後水洗いし、乾燥した。なお、シアノエチルエチレンジアミン及びシアノエチルシクロヘキシルアミンはそれぞれ、エチレンジアミンあるいはシクロヘキシルアミンとアクリロニトリルを反応させ蒸留により精製したものを用いた。水酸化テトラメチルアンモニウムは多摩化学工業(株)製(高純度グレード)、アンモニアはキシダ化学のものを使用した。
【0026】
洗浄後のウエハの表面を走査型電子顕微鏡で観察しレジストの剥離性を調べた。また、Siの侵食については、poly−Si膜ウエハ、SiO2膜ウエハを80℃、5分間浸漬し、表面観察から評価した。引火点はタグ密閉式およびクリーブランド開放式により測定を行った。なお、表1に剥離液組成を示すが、残部は水である。
KrFレジストの剥離性、Siの侵食性は以下のように評価した。
<i線用レジスト及び反射防止膜の剥離性>
○:完全剥離、△:一部残存、×:全面に残存
<Siの侵食性>
○:侵食なし、△:一部侵食有り、×:激しい侵食有り
【0027】
【表1】
【発明の効果】
本発明のレジスト剥離液は多結晶Si(poly−Si)、Si酸化膜(SiO2)などにダメージを与えることなく、80℃以下の温度及び短時間(〜15秒)の条件下でレジストを除去することができ、更に引火点を持たないため特に枚葉式洗浄装置の基板工程用レジスト剥離液として極めて有用である。[0001]
BACKGROUND OF THE INVENTION
The present invention relates to a resist stripping solution for a substrate process of a single wafer cleaning apparatus and a stripping method using the resist stripping solution.
[0002]
[Prior art]
Wet cleaning apparatuses used in semiconductor manufacturing processes are classified into a batch type that batch-processes 25 to 50 wafers and a single wafer type that processes wafers one by one. The batch type includes a multi-tank type equipped with many cleaning solution tanks and a pure water rinsing tank, and a single tank type for performing various chemical cleaning and pure water rinsing in one tank. In the past, batch-type multi-tank systems have evolved while shifting from manual operation to full-automatic operation, but in recent years, batch-type single tank systems and single wafer cleaning systems have been used for cleaning after specific processes. It has become. In the future, large-diameter Si wafers (diameter 300 mm or 450 mm) will be used to improve productivity, so single-wafer cleaning equipment with high cleaning uniformity within the wafer surface and small equipment installation area will be the mainstream. It is becoming.
[0003]
Conventionally, resist removal in a substrate process (Front End of Line process) has been conventionally performed with a mixed solution (SPM cleaning liquid) composed of sulfuric acid and hydrogen peroxide in a batch type cleaning apparatus. As typical use conditions, it is performed by treating at 100 to 120 ° C. for 10 minutes with an SPM cleaning solution (sulfuric acid: hydrogen peroxide solution = 4: 1).
[0004]
However, in a single wafer cleaning apparatus, a concentrated and high-temperature solution such as an SPM cleaning liquid cannot be used due to limitations in terms of apparatus and cost. Also, a chemical solution having a flash point is not desirable in terms of apparatus, and until now there has been no resist stripping solution for a substrate process suitable for this cleaning apparatus.
[0005]
[Problems to be solved by the invention]
An object of the present invention is to provide a resist stripper suitable for use in a device that cannot use a stripper at a high temperature for a long time, particularly a single wafer cleaning device, and a method for using the resist stripper. In other words, resist and reflection under conditions of a temperature of 80 ° C. or less and a short time (˜30 seconds) without damaging the exposed polycrystalline Si (poly-Si), Si oxide film (SiO 2 ), etc. An object of the present invention is to provide a resist stripping solution that can remove the prevention film and has no flash point.
[0006]
[Means for Solving the Problems]
As a result of intensive studies on a resist stripping solution for substrate process (hereinafter referred to as resist stripping solution) of a single wafer cleaning apparatus, the present inventors have found that cyanoethylethylenediamine, cyanoethylcyclohexylamine, water, and tetramethylammonium hydroxide and / or ammonia are added. The resist solution and the antireflection film are removed under conditions of a temperature of 80 ° C. or less and a short time (within 30 seconds, preferably ˜15 seconds) with little damage to the mixed solution containing poly-Si, SiO 2 and the like. And found that it has no flash point, and has completed the present invention.
[0007]
That is, the present invention is a resist stripping solution containing cyanoethylethylenediamine, cyanoethylcyclohexylamine, water, tetramethylammonium hydroxide and / or ammonia as essential components, and a stripping method using the resist stripping solution.
[0008]
The present invention is described in detail below.
[0009]
The resist stripping solution in the present invention is used in a substrate process of an apparatus that requires a stripping process at a low temperature in a short time, particularly a single wafer cleaning apparatus. Here, the substrate process is a so-called FEOL (Front End of Line) process before the formation of the wiring structure in the semiconductor manufacturing process.
[0010]
In the present invention, peeling refers to the application of a photoresist and / or antireflection film on a substrate, exposure, development, etching, ion implantation, and the like to form a circuit, and then the remaining resist and / or It means removing the antireflection film.
[0011]
The resist stripping solution of the present invention is used for stripping a photoresist and / or an antireflection film. That is, after a photoresist and / or antireflection film is applied on a substrate, exposure, development, etching, ion implantation, and other processes are performed to form a circuit, and then the resist is stripped with the resist stripping solution of the present invention.
[0012]
The resist stripping solution of the present invention comprises an aqueous solution containing cyanoethylethylenediamine, cyanoethylcyclohexylamine, water, and tetramethylammonium hydroxide and / or ammonia.
[0013]
Cyanoethylethylenediamine and cyanoethylcyclohexylamine used in the resist stripping solution of the present invention have an action of stripping and dissolving the resist and / or antireflection film from the wafer. In particular, cyanoethylcyclohexylamine is excellent in the solubility of the resist and the antireflection film, but since the solubility in water is low, the solubility can be increased by adding cyanoethylethylenediamine.
[0014]
Cyanoethylethylenediamine can be easily obtained by reacting acrylonitrile with a large excess of ethylenediamine. Similarly, cyanoethylcyclohexylamine can be easily obtained by reacting cyclohexylamine with acrylonitrile. Ethylenediamine, acrylonitrile, and cyclohexylamine as raw materials are generally commercially available and can be easily obtained.
[0015]
The tetramethylammonium hydroxide and / or ammonia used in the resist stripping solution of the present invention has the action of stripping the resist and the antireflection film from the wafer. Tetramethylammonium hydroxide or ammonia is generally commercially available as an aqueous solution and can be easily obtained. However, in order to maintain the cleanliness of the wafer, it is preferable to use a high purity product.
[0016]
The pH of the resist stripping solution of the present invention is preferably 10-13, particularly preferably 11-13.
[0017]
The composition of the cleaning liquid of the present invention is adjusted with a combination of essential components cyanoethylethylenediamine, cyanoethylcyclohexylamine, and tetramethylammonium hydroxide and / or ammonia, so the solubility in water varies depending on the concentration used, and two-layer separation However, it is difficult to limit the concentration of each, but the content of cyanoethylethylenediamine is preferably 0.1 to 15% by weight, particularly preferably 0.5 to 10% by weight. Even if the concentration of cyanoethylethylenediamine is increased beyond this range, not only an effect commensurate with the amount added is obtained, but also poly-Si and SiO 2 are damaged. If the concentration is too low, not only the peeling effect in a short time becomes insufficient, but also cyanoethylethylenediamine acts as a compatibilizer of cyanoethylcyclohexylamine which is hardly soluble in water, so that the solubility of cyanoethylcyclohexylamine is reduced.
[0018]
The content of cyanoethylcyclohexylamine is 0.1 wt% to 5 wt%, preferably 1 wt% to 5 wt%. When the concentration of cyanoethylcyclohexylamine increases beyond this range, it does not dissolve in water and separates into two layers, and if it is too small, the peeling effect decreases.
[0019]
The content of tetramethylammonium hydroxide and / or ammonia is 0.001 to 0.1% by weight, preferably 0.005 to 0.05% by weight. If the concentration of tetramethylammonium hydroxide and / or ammonia is increased beyond this range, the peeling effect is excellent, but poly-Si and SiO 2 are damaged. Conversely, if the amount is too small, the peeling effect in a short time becomes insufficient.
[0020]
The resist stripping solution of the present invention may be used by adding each component when stripping the resist, or may be used after mixing each component in advance.
[0021]
The resist stripping solution of the present invention can be used for stripping resists for i-line and KrF excimer laser that can be developed with an alkaline aqueous solution, including negative and positive types.
[0022]
The resist stripping solution of the present invention is most preferably used when stripping a photoresist film coated on an inorganic substrate, a photoresist layer treated with ion implantation, or an antireflection film.
[0023]
The resist stripping solution of the present invention is used in a single wafer cleaning apparatus, and the temperature during cleaning is preferably 20 ° C. to 80 ° C. due to limitations on the apparatus. Further, the washing time is preferably within 30 seconds from the viewpoint of productivity.
[0024]
【Example】
Hereinafter, the method of the present invention will be described with reference to examples, but the present invention is not limited thereto.
[0025]
Examples 1-4, Comparative Examples 1-7
The KrF resist wafer was immersed in a stripping solution shown in Table 1 at 80 ° C. for 15 seconds, then washed with water and dried. Cyanoethylethylenediamine and cyanoethylcyclohexylamine were each purified by distillation after reacting ethylenediamine or cyclohexylamine with acrylonitrile. Tetramethylammonium hydroxide was manufactured by Tama Chemical Industry Co., Ltd. (high purity grade), and ammonia was Kishida Chemical.
[0026]
The surface of the cleaned wafer was observed with a scanning electron microscope, and the resist peelability was examined. Also, the erosion of Si, poly-Si film wafer, 80 ° C. The SiO 2 film wafer was immersed for 5 minutes and evaluated the surface observation. The flash point was measured by a closed tag type and a Cleveland open type. In addition, although stripping liquid composition is shown in Table 1, the remainder is water.
The peelability of KrF resist and the erosion property of Si were evaluated as follows.
<Peelability of i-line resist and antireflection film>
○: Completely peeled, Δ: Partially retained, ×: Residual on the entire surface <Si erosion>
○: No erosion, △: Partial erosion, ×: Heavy erosion [0027]
[Table 1]
【The invention's effect】
The resist stripping solution of the present invention does not damage the polycrystalline Si (poly-Si), Si oxide film (SiO 2 ), etc., and resists under a temperature of 80 ° C. or lower and for a short time (˜15 seconds). Since it can be removed and has no flash point, it is extremely useful as a resist stripping solution for a substrate process of a single wafer cleaning apparatus.
Claims (6)
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2008023614A1 (en) * | 2006-08-21 | 2008-02-28 | Tosoh Corporation | Composition for removal of resist comprising poly(cyanoalkyl)ethyleneamine and method for removal of resist using the composition |
JP2008191631A (en) * | 2006-08-21 | 2008-08-21 | Tosoh Corp | Composition for removing resist |
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2008023614A1 (en) * | 2006-08-21 | 2008-02-28 | Tosoh Corporation | Composition for removal of resist comprising poly(cyanoalkyl)ethyleneamine and method for removal of resist using the composition |
JP2008191631A (en) * | 2006-08-21 | 2008-08-21 | Tosoh Corp | Composition for removing resist |
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