JP4296320B2 - Resist stripper composition and method of using the same - Google Patents

Resist stripper composition and method of using the same Download PDF

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Publication number
JP4296320B2
JP4296320B2 JP17345499A JP17345499A JP4296320B2 JP 4296320 B2 JP4296320 B2 JP 4296320B2 JP 17345499 A JP17345499 A JP 17345499A JP 17345499 A JP17345499 A JP 17345499A JP 4296320 B2 JP4296320 B2 JP 4296320B2
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resist
organic solvent
composition
water
wiring
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JP2001005200A (en
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容子 村田
瑞樹 武井
武 小谷
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Nagase Chemtex Corp
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Description

【0001】
【発明の属する技術分野】
本発明は、半導体集積回路、液晶パネルの半導体素子回路等の製造に用いられるフォトレジスト剥離剤組成物及びその使用方法、詳しくは、半導体基板上又は液晶用ガラス基板上に配線を形成するときに生成するレジスト残渣の除去性能と、基板のアルミニウム防食性との両方を向上させるフォトレジスト剥離剤組成物及びその使用方法に関するものである。
【0002】
【従来の技術】
剥離剤組成物は、半導体集積回路、液晶パネルの半導体素子回路等の製造に用いられるフォトレジストを剥離する際に用いられる。
半導体素子回路又は付随する電極部の製造は、以下のように行われる。まず、シリコン、ガラス等の基板上に金属膜をCVDやスパッタ等の方法で積層させる。その上面にフォトレジストを膜付けし、それを露光、現像等の処理でパターン形成する。パターン形成されたフォトレジストをマスクとして金属膜をエッチングする。その後、不要となったフォトレジストを剥離剤組成物を用いて剥離・除去した後、洗浄液で洗浄する。これらの操作を繰り返すことにより素子の形成が行われる。
【0003】
従来、剥離剤組成物としては、有機アルカリ、無機アルカリ、有機酸、無機酸、極性溶剤等の単一溶剤、これらの混合溶液、又はこれらの水溶液が用いられている。
また、半導体素子回路等の製造工程における配線形成時に生成するレジスト残渣を除去するために、アルキルアミン及びアルキルアンモニウム水酸化物の少なくともいずれかと、有機溶剤と、水とを主成分とするレジスト剥離剤組成物も良く知られている。
【0004】
さらに、フッ化水素酸と各種アミンとの混合物が半導体基板製造工程又は液晶用ガラス基板製造工程における配線形成時に生成するレジスト残渣除去に有効であることが知られている。
例えば、特開平8−202052号公報には、フッ化水素酸、フッ化アンモニウム、水溶性有機溶媒及び防食剤を含有するレジスト剥離液組成物が記載されている。
また、特開平9−197681号公報には、フッ化水素酸と金属を含まない塩基との塩、水溶性有機溶媒及び水を含有し、水素イオン濃度(pH)が5〜8であるレジスト用剥離液組成物が記載されている。
【0005】
また、特開平7−201794号公報には、半導体装置製造工程において生成する保護堆積膜を、第四級アンモニウム塩とフッ素化合物を含有する水溶液、又は第四級アンモニウム塩とフッ素化合物に、アミド類、ラクトン類、ニトリル類、アルコール類、エステル類から選ばれた有機溶媒を含有する水溶液からなる半導体装置洗浄剤を用いて剥離することが記載されている。
また、特開平7−271056号公報には、有機カルボン酸アンモニウム塩又は有機カルボン酸アミン塩、及びフッ素化合物を含有する水溶液からなるフォトレジスト用剥離液が記載されている。
さらに、特開平9−62013号公報には、フッ素化合物及びベタイン化合物と、アミド類、ラクトン類、アルコール類から選ばれた一種以上の有機溶剤を含む半導体装置用洗浄剤が記載されている。
【0006】
【発明が解決しようとする課題】
レジスト剥離剤組成物は、レジスト残渣除去性に優れており、かつ、基板上に形成されたアルミニウム、アルミニウム合金等の導電性金属膜の腐食が良好に防止できることが要求される。
しかし、フッ化化合物を含有するレジスト剥離剤組成物において、上記公報に記憶されている組成を用いても、残渣除去性とアルミニウム防食性の両方を満足させることができない。
現在、半導体製造工程におけるAl配線上のレジスト残渣除去の際に、フッ化水素酸とアミンとの塩、水溶性有機溶媒及び水よりなるレジスト剥離剤組成物が使用されているが、必ずしもレジスト残渣の除去性及びアルミニウム防食性を両立させるものではない。
特に、Al配線上のレジストをアッシングすると、主にAl酸化物が残渣として残るが、これは両性酸化物であるため、剥離剤組成物をアルカリ性もしくは酸性に調整する方が残渣除去性は良くなる。
【0007】
そこで、本発明者は種々の実験を重ねた結果、フッ化アンモニウム、極性有機溶剤及び水からなる組成物にアスコルビン酸を添加することによって、組成物を酸性、具体的にはpHを5未満にすることでレジスト残渣の除去性が向上し、アルミニウム防食性を兼ね備えたレジスト剥離剤組成物となることを見出した。
加えて、この剥離剤組成物に含有させる極性有機溶剤に、N,N−ジメチルホルムアミド、N,N−ジメチルアセトアミド、ジメチルスルホキシド、エチレングリコール及びプロピレングリコールの少なくともいずれかを用いれば、レジスト残渣除去性において好ましいことを見出した。
本発明は、上記の知見に基づいてなされたもので、本発明の目的は、配線形成時に生成するレジスト残渣を高性能で除去すると同時に、基板上のアルミニウムの腐食を良好に防止することができるレジスト剥離剤組成物及びその使用方法を提供することにある。
【0008】
【課題を解決するための手段】
上記の目的を達成するために、本発明のレジスト剥離剤組成物は、フッ化アンモニウム、極性有機溶剤及び水を主成分とし、アスコルビン酸を添加し、かつ、水素イオン濃度(pH)が5.0未満であるように調製される。
このレジスト剥離剤組成物において、フッ化アンモニウムの添加量が0.1〜2重量%、望ましくは0.5〜1.5重量%、極性有機溶剤の含有量が20〜98.8重量%、望ましくは50〜80重量%、水の含有量が1〜79.8重量%、望ましくは5〜50重量%、アスコルビン酸の含有量が0.05〜1.9重量%、望ましくは0.1〜1.5重量%である。
【0009】
フッ化アンモニウムが上記の範囲未満の場合は、レジスト残渣の除去性が低下し、上記の範囲を超える場合は、アルミニウムやシリコン酸化膜に対する腐食が激しくなる。
また、極性有機溶剤の含有量が上記の範囲未満の場合は、レジスト残渣の除去性が低下し、上記の範囲を超える場合は、フッ化アンモニウムが析出する場合がある。
また、水の含有量が上記の範囲未満の場合は、レジスト残渣の除去性が低下し、かつフッ化アンモニウムが析出する場合がある。一方、上記の範囲を超える場合はアルミニウムが腐食しやすくなる。
また、アスコルビン酸の含有量が上記の範囲未満の場合は、期待したレジスト残渣の除去性が得られない。一方、上記の範囲を超えて含有させてもレジスト残渣の除去効果は同じで、経済性の面からも好ましくない。
【0010】
pHが5.0以上となる場合は、レジスト残渣除去性が低下する。なお、pH値はアスコルビン酸の添加により5.0未満になるように調整されるが、その添加量は残りの組成物の含有量との兼ね合いで決定される。
極性有機溶剤としては、N,N−ジメチルホルムアミド、N,N−ジメチルアセトアミド、ジメチルスルホキシド、エチレングリコール、プロピレングリコールの1種類又は混合物が用いられる。
また、本発明のレジスト剥離剤組成物の使用方法は、半導体基板上又は液晶用ガラス基板上に配線を形成する際に生成するレジスト残渣を、上記の本発明の剥離剤組成物を用いて剥離・除去して配線を形成することを特徴としている。
【0011】
【実施例】
以下に実施例及び比較例を示し、本発明の特徴とするところをより一層明確にする。
実施例1〜5、比較例1〜3
シリコン酸化膜上にTiN、その上にTi、さらにその上にAl−Cuを膜付けした基板を、パターニングされたレジストをマスクとしてCl2 とBCl3 を用いてドライエッチングし、続いて酸素と水とを用いてアッシングした時に配線側壁又は上部に生成するレジスト残渣を剥離対象物とした。
表1に示す剥離剤組成物の中に上述の対象物を24℃で3min.浸漬した後、24℃の純水中に1min.浸漬、さらに新たな24℃の純水中に1min.浸漬後、24℃の純水シャワーで1min.水洗し、最後に窒素ガスで乾燥させた。
走査電子顕微鏡(SEM)にて剥離性(残渣除去の程度)及びアルミニウム腐食の程度を観察し、比較を行った。結果は表1に示した。
表1の剥離性において、○は「残渣なし」、△は「処理前より残渣は除去できているが残渣が残っている」、×は「処理前の残渣の状態と同じ」を示す。
また、表1のアルミニウム防食性において、○は「腐食なし」、×は「配線が細る又は表面荒れがある」、NAは「残渣が多く判定不可能」を示す。
また、表1において、DMFはN,N−ジメチルホルムアミド、DMACはN,N−ジメチルアセトアミド、PGはプロピレングリコール、EGはエチレングリコール、DMSOはジメチルスルホキシド、MEAはモノエタノールアミンを表す。
【0012】
【表1】

Figure 0004296320
【0013】
表1より、アスコルビン酸を添加し、かつ、水素イオン濃度が5.0未満である剥離剤組成物は剥離性が良好であり、また、Al腐食も抑制されていることがわかる。
つぎに、本発明のレジスト剥離剤組成物の使用方法の一例について説明する。半導体基板上又は液晶用ガラス基板上に金属薄膜をCVDやスパッタ等により形成させる。その上面にフォトレジストを膜付けした後、露光、現像等の処理でパターン形成する。パターン形成されたフォトレジストをマスクとして金属薄膜をエッチングする。その後、アッシングによりレジストを灰化する。最後に灰化したレジスト残渣を本発明のレジスト剥離剤組成物を用いて剥離・除去して配線等が形成された半導体素子が製造される。
【0014】
【発明の効果】
本発明は上記のように構成されているので、つぎのような効果を奏する。
(1) フッ化アンモニウム、極性有機溶剤、水及びアスコルビン酸を含有し、かつ、pHが5.0未満の範囲にあるようにレジスト剥離剤組成物を調製することにより、半導体又は液晶用の素子回路等の製造工程における配線形成時に生成するレジスト残渣を高性能で除去することができるとともに、基板上のアルミニウム等の金属薄膜の腐食を良好に防止することができる。[0001]
BACKGROUND OF THE INVENTION
The present invention relates to a photoresist remover composition used in the manufacture of semiconductor integrated circuits, semiconductor element circuits of liquid crystal panels, and the use thereof, and more specifically, when wiring is formed on a semiconductor substrate or a glass substrate for liquid crystal. The present invention relates to a photoresist stripping composition that improves both the performance of removing the generated resist residue and the aluminum corrosion resistance of the substrate, and a method for using the same.
[0002]
[Prior art]
The stripping composition is used when stripping a photoresist used for manufacturing a semiconductor integrated circuit, a semiconductor element circuit of a liquid crystal panel, and the like.
Manufacture of a semiconductor element circuit or an accompanying electrode part is performed as follows. First, a metal film is laminated on a substrate such as silicon or glass by a method such as CVD or sputtering. A photoresist is formed on the upper surface, and a pattern is formed by processing such as exposure and development. The metal film is etched using the patterned photoresist as a mask. Thereafter, the unnecessary photoresist is stripped and removed using a stripper composition, and then washed with a cleaning liquid. Elements are formed by repeating these operations.
[0003]
Conventionally, as a release agent composition, a single solvent such as an organic alkali, an inorganic alkali, an organic acid, an inorganic acid, or a polar solvent, a mixed solution thereof, or an aqueous solution thereof is used.
In addition, in order to remove a resist residue generated at the time of forming a wiring in a manufacturing process of a semiconductor element circuit or the like, a resist stripper mainly composed of at least one of alkylamine and alkylammonium hydroxide, an organic solvent, and water Compositions are also well known.
[0004]
Furthermore, it is known that a mixture of hydrofluoric acid and various amines is effective for removing resist residues generated during wiring formation in a semiconductor substrate manufacturing process or a liquid crystal glass substrate manufacturing process.
For example, JP-A-8-202052 describes a resist stripping solution composition containing hydrofluoric acid, ammonium fluoride, a water-soluble organic solvent, and an anticorrosive agent.
Japanese Patent Application Laid-Open No. 9-197681 discloses a resist containing a salt of hydrofluoric acid and a base containing no metal, a water-soluble organic solvent and water and having a hydrogen ion concentration (pH) of 5 to 8. A stripping composition is described.
[0005]
Japanese Patent Application Laid-Open No. 7-201794 discloses a protective deposition film formed in a semiconductor device manufacturing process as an aqueous solution containing a quaternary ammonium salt and a fluorine compound, or a quaternary ammonium salt and a fluorine compound. And peeling using a semiconductor device cleaning agent comprising an aqueous solution containing an organic solvent selected from lactones, nitriles, alcohols and esters.
JP-A-7-271056 discloses a photoresist stripping solution comprising an aqueous solution containing an organic carboxylic acid ammonium salt or organic carboxylic acid amine salt and a fluorine compound.
Further, JP-A-9-62013 discloses a cleaning agent for a semiconductor device containing a fluorine compound and a betaine compound and one or more organic solvents selected from amides, lactones and alcohols.
[0006]
[Problems to be solved by the invention]
The resist remover composition is required to have excellent resist residue removability and to be able to satisfactorily prevent corrosion of conductive metal films such as aluminum and aluminum alloys formed on the substrate.
However, in the resist stripper composition containing a fluorinated compound, even if the composition memorized in the above publication is used, both the residue removal property and the aluminum anticorrosion property cannot be satisfied.
Currently, a resist remover composition comprising a salt of hydrofluoric acid and an amine, a water-soluble organic solvent, and water is used for removing a resist residue on an Al wiring in a semiconductor manufacturing process. It is not intended to achieve both the removability of aluminum and the corrosion resistance of aluminum.
In particular, when the resist on the Al wiring is ashed, mainly Al oxide remains as a residue. However, since this is an amphoteric oxide, the residue removability is improved by adjusting the stripping composition to alkaline or acidic. .
[0007]
Therefore, as a result of repeating various experiments, the inventor made the composition acidic by adding ascorbic acid to a composition comprising ammonium fluoride, a polar organic solvent, and water, specifically, the pH was set to less than 5. Thus, it was found that the resist residue removability was improved and a resist stripping composition having aluminum corrosion resistance was obtained.
In addition, if at least one of N, N-dimethylformamide, N, N-dimethylacetamide, dimethyl sulfoxide, ethylene glycol, and propylene glycol is used as the polar organic solvent to be contained in the release agent composition, resist residue removability Was found to be preferable.
The present invention has been made on the basis of the above knowledge, and an object of the present invention is to remove resist residues generated at the time of wiring formation with high performance, and at the same time, well prevent corrosion of aluminum on the substrate. It is in providing a resist remover composition and a method of using the same.
[0008]
[Means for Solving the Problems]
In order to achieve the above object, the resist remover composition of the present invention comprises ammonium fluoride, a polar organic solvent and water as main components, ascorbic acid added, and a hydrogen ion concentration (pH) of 5. Prepared to be less than zero.
In this resist stripper composition, the amount of ammonium fluoride added is 0.1 to 2% by weight, desirably 0.5 to 1.5% by weight, the content of the polar organic solvent is 20 to 98.8% by weight, Desirably 50 to 80 wt%, water content 1 to 79.8 wt%, desirably 5 to 50 wt%, ascorbic acid content 0.05 to 1.9 wt%, desirably 0.1 ~ 1.5 wt%.
[0009]
When the ammonium fluoride is less than the above range, the resist residue removability is lowered, and when it exceeds the above range, the aluminum and the silicon oxide film are severely corroded.
Further, when the content of the polar organic solvent is less than the above range, the removability of the resist residue is lowered, and when it exceeds the above range, ammonium fluoride may be precipitated.
Further, when the water content is less than the above range, the removability of the resist residue is lowered and ammonium fluoride may be precipitated. On the other hand, when it exceeds the above range, aluminum tends to corrode.
Further, when the ascorbic acid content is less than the above range, the expected resist residue removability cannot be obtained. On the other hand, even if the content exceeds the above range, the removal effect of the resist residue is the same, which is not preferable from the viewpoint of economy.
[0010]
When the pH is 5.0 or more, the resist residue removability decreases. In addition, although pH value is adjusted so that it may become less than 5.0 by addition of ascorbic acid, the addition amount is determined by balance with content of the remaining composition.
As the polar organic solvent, one or a mixture of N, N-dimethylformamide, N, N-dimethylacetamide, dimethyl sulfoxide, ethylene glycol and propylene glycol is used.
In addition, the method of using the resist stripper composition of the present invention is to strip the resist residue generated when wiring is formed on a semiconductor substrate or a glass substrate for liquid crystal using the above stripper composition of the present invention. -It is characterized by removing and forming wiring.
[0011]
【Example】
Examples and Comparative Examples are shown below to further clarify the features of the present invention.
Examples 1-5, Comparative Examples 1-3
A substrate on which a TiN film is formed on a silicon oxide film, a Ti film thereon, and an Al-Cu film thereon is dry-etched using Cl 2 and BCl 3 using a patterned resist as a mask, followed by oxygen and water. The resist residue generated on the side wall or the upper part of the wiring when ashing was used as an object to be peeled.
After immersing the above-mentioned object in the release agent composition shown in Table 1 for 3 min. At 24 ° C., after 1 min. Immersion in pure water at 24 ° C., and further for 1 min. In new pure water at 24 ° C. The sample was washed with pure water at 24 ° C. for 1 min. And finally dried with nitrogen gas.
The peelability (degree of residue removal) and the degree of aluminum corrosion were observed and compared with a scanning electron microscope (SEM). The results are shown in Table 1.
In the peelability of Table 1, ◯ indicates “no residue”, Δ indicates “residue can be removed from before treatment but residue remains”, and x indicates “the same as the state of residue before treatment”.
Moreover, in the aluminum anticorrosive property of Table 1, “◯” indicates “no corrosion”, “×” indicates “wiring is thin or surface is rough”, and NA indicates “there are many residues and cannot be determined”.
In Table 1, DMF represents N, N-dimethylformamide, DMAC represents N, N-dimethylacetamide, PG represents propylene glycol, EG represents ethylene glycol, DMSO represents dimethyl sulfoxide, and MEA represents monoethanolamine.
[0012]
[Table 1]
Figure 0004296320
[0013]
From Table 1, it can be seen that the release agent composition to which ascorbic acid is added and the hydrogen ion concentration is less than 5.0 has good peelability, and Al corrosion is also suppressed.
Next, an example of a method for using the resist remover composition of the present invention will be described. A metal thin film is formed on a semiconductor substrate or a glass substrate for liquid crystal by CVD or sputtering. After a photoresist film is formed on the upper surface, a pattern is formed by processing such as exposure and development. The metal thin film is etched using the patterned photoresist as a mask. Thereafter, the resist is ashed by ashing. Finally, the ashed resist residue is stripped and removed using the resist stripper composition of the present invention to produce a semiconductor element in which wirings and the like are formed.
[0014]
【The invention's effect】
Since this invention is comprised as mentioned above, there exist the following effects.
(1) A semiconductor or liquid crystal device by preparing a resist remover composition so as to contain ammonium fluoride, a polar organic solvent, water and ascorbic acid, and have a pH in the range of less than 5.0. Resist residues generated at the time of wiring formation in a manufacturing process such as a circuit can be removed with high performance, and corrosion of a metal thin film such as aluminum on the substrate can be well prevented.

Claims (4)

フッ化アンモニウム、極性有機溶剤、水及びアスコルビン酸を含有し、かつ、水素イオン濃度(pH)が5.0未満であることを特徴とするレジスト剥離剤組成物。A resist remover composition comprising ammonium fluoride, a polar organic solvent, water and ascorbic acid, and having a hydrogen ion concentration (pH) of less than 5.0. フッ化アンモニウムの添加量が0.1〜2重量%、極性有機溶剤の含有量が20〜98.8重量%、水の含有量が1〜79.8重量%、アスコルビン酸の含有量が0.05〜1.9重量%である請求項1記載のレジスト剥離剤組成物。The addition amount of ammonium fluoride is 0.1 to 2% by weight, the content of polar organic solvent is 20 to 98.8% by weight, the content of water is 1 to 79.8% by weight, and the content of ascorbic acid is 0. The resist remover composition according to claim 1, which is 0.05 to 1.9% by weight. 極性有機溶剤がN,N−ジメチルホルムアミド、N,N−ジメチルアセトアミド、ジメチルスルホキシド、エチレングリコール及びプロピレングリコールの少なくともいずれかである請求項1又は2記載のレジスト剥離剤組成物。The resist remover composition according to claim 1 or 2, wherein the polar organic solvent is at least one of N, N-dimethylformamide, N, N-dimethylacetamide, dimethyl sulfoxide, ethylene glycol and propylene glycol. 半導体基板上又は液晶用ガラス基板上に配線を形成する際に生成するレジスト残渣を、請求項1、2又は3記載の剥離剤組成物を用いて剥離・除去して配線を形成することを特徴とするレジスト剥離剤組成物の使用方法。A resist residue generated when a wiring is formed on a semiconductor substrate or a glass substrate for liquid crystal is stripped and removed using the release agent composition according to claim 1, 2 or 3, thereby forming a wiring. A method for using a resist remover composition.
JP17345499A 1999-06-21 1999-06-21 Resist stripper composition and method of using the same Expired - Fee Related JP4296320B2 (en)

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JP3403187B2 (en) * 2001-08-03 2003-05-06 東京応化工業株式会社 Stripping solution for photoresist
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US7166419B2 (en) 2002-09-26 2007-01-23 Air Products And Chemicals, Inc. Compositions substrate for removing etching residue and use thereof
WO2006129538A1 (en) * 2005-06-01 2006-12-07 Nissan Chemical Industries, Ltd. Semiconductor wafer cleaning composition containing phosphonic acid and method of cleaning
JP4642001B2 (en) 2006-10-24 2011-03-02 関東化学株式会社 Composition for removing photoresist residue and polymer residue
JP2011503899A (en) * 2007-11-16 2011-01-27 イー.ケー.シー.テクノロジー.インコーポレーテッド Composition for removing metal hard mask etching residue from a semiconductor substrate
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