JP4170710B2 - Release agent composition - Google Patents
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Description
【０００１】
【発明の属する技術分野】
本発明は、シリコンウェハ等の半導体用基板上に半導体素子を形成する工程において使用したレジストをアッシングにより除去した後に残存するデポ（レジスト、絶縁膜及び金属材料由来の酸化生成物）の剥離に用いられる剥離剤組成物、並びにそれを用いる半導体用基板及び半導体素子の洗浄方法に関する。
【０００２】
【従来の技術】
半導体素子の製造において、スパッタリング等の方法で薄膜を形成し、リソグラフィーにより薄膜上に所定のパターンをレジストで形成する。これをエッチングレジストとして下層部の薄膜を選択的にエッチングで除去した後、アッシングにてレジストを除去する工程が取られる。この一連の工程が繰り返されて製品が製造される。
【０００３】
従来のアルミニウム配線を用いた半導体素子の剥離剤として様々な剥離剤組成物が提案されており、フッ素含化合物を用いた剥離剤やヒドロキシルアミンに代表されるアミンを用いた剥離剤が主に使用されている。
【０００４】
しかし、半導体素子の微細化にともない、アッシング後に生成されるデポの付着量が増大しており、フッ素含化合物系剥離剤を用いて剥離を行った場合、剥離不足や再付着（一度剥離したデポが剥離剤中に浮遊し、半導体素子上に再付着する）等の問題が発生する。また、アミン系剥離剤を用いて剥離を行った場合、高温（〜７０℃）での剥離が必要になるため、安全性や臭い等、作業環境性に問題が発生する。
【０００５】
そこで、上記の問題を解決すべく、本発明者らは多価カルボン酸及び/ 又はその塩と、水とを含有する剥離剤（特許文献１参照）を提案した。
【０００６】
【特許文献１】
特開2000-214599 号公報
【０００７】
【発明が解決しようとする課題】
しかしながら、更に研究を進めた結果、特定の組成の剥離剤組成物において、特に優れた性能を発揮することを見出し、本発明を完成するに至った。従って、本発明の目的は、アッシング後に発生するデポに対し優れた剥離性が得られると共にデポの再付着を防止でき、配線材料に対する腐食が少なく、低温保存時においても結晶化による沈殿生成や、それに起因する剥離性能の低下等がなく、安定な性状と剥離性が得られる剥離剤組成物、該剥離剤組成物を用いる半導体基板又は半導体素子の洗浄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】
即ち、本発明の要旨は、
〔１〕 多価カルボン酸塩0.5 〜5 重量% とグリコールエーテル1 〜18重量% 及び水77〜98.5重量% とを含有する剥離剤組成物、
〔２〕 多価カルボン酸塩0.5 〜5 重量% とグリコールエーテル1 〜18重量% 及び水77〜98.5重量% とを配合してなる剥離剤組成物、並びに
〔３〕 前記〔１〕又は〔２〕記載の剥離剤組成物を用いて半導体基板又は半導体素子を剥離洗浄する工程を有する半導体基板又は半導体素子の洗浄方法
に関する。
【０００９】
【発明の実施の形態】
１．剥離剤組成物
本発明の剥離剤組成物は、前記のように、多価カルボン酸塩0.5 〜5 重量% とグリコールエーテル1 〜18重量% 及び水77〜98.5重量% とを含有する又は配合してなる点に特徴があり、かかる剥離剤組成物を用いることにより、半導体素子形成時に発生するデポに対し、優れた剥離性が得られ、且つデポを溶解する機能を有するため、その再付着を防止することができ、また配線金属等の金属材料に対する腐食が少なく、低温保存時においても結晶化による沈殿生成や、それに起因する剥離性能の低下等がなく、低温でも安定な性状と剥離性が得られるという効果が発現される。
【００１０】
多価カルボン酸塩として具体的には、シュウ酸アンモニウム、フタル酸アンモニウム、マロン酸アンモニウム、コハク酸アンモニウム、アジピン酸アンモニウム、クエン酸アンモニウム等があげられる。これらは酸化した金属に対し、高い溶解性を保持しており、また酸化していない金属に対しては溶解性が極めて低く、デポと配線金属の選択性が非常に高い。すなわち、剥離により除去すべきデポに対しては高い溶解性を示し、保護すべき金属配線に対しては殆ど腐蝕しない。
【００１１】
これらの中で、剥離性とデポ溶解性の観点から、第一解離定数ｐＫａ１が3.6 以下の多価カルボン酸塩である、シュウ酸アンモニウム、フタル酸アンモニウム、マロン酸アンモニウムが好ましく、シュウ酸アンモニウムがより好ましい。
【００１２】
剥離剤組成物中の多価カルボン酸塩含有量としては、充分な剥離性と配線金属の防食性発現の観点から0.5 〜5 重量％であり、1 〜4 重量％が好ましい。
【００１３】
グリコールエーテルとして具体的には、エチレングリコールモノメチルエーテル、エチレングリコールモノエチルエーテル、エチレングリコールモノブチルエーテル、ジエチレングリコールモノメチルエーテル、ジエチレングリコールモノエチルエーテル、ジエチレングリコールモノブチルエーテル、ジエチレングルコールジメチルエーテル、ジエチレングリコールジエチルエーテル、エチレングリコールモノフェニルエーテル、ジエチレングリコールモノフェニルエーテル、トリエチレングリコールモノフェニルエーテル、エチレングリコールモノベンジルエーテル、ジエチレングリコールモノベンジルエーテル等があげられる。
【００１４】
これらの中で、充分な剥離性が必要な観点から、デポへの浸透力が高い化合物が好ましく、さらに水との混和性の観点から、ジエチレングリコールモノブチルエーテル、トリエチレングリコールモノフェニルエーテルが好ましい。
【００１５】
剥離剤組成物中のグリコールエーテル含有量としては、充分なデポ浸透性と低温安定性発現の観点から1 〜18重量％であり、5 〜16重量％が好ましい。
【００１６】
多価カルボン酸塩、グリコールエーテルを均一に溶解させる溶媒としては、水が好ましく用いられる。
【００１７】
水は本発明の剥離剤組成物の目的を阻害しない物であれば特に限定されるものではない。水としては超純水、純水、イオン交換水、蒸留水等があげられる。
【００１８】
剥離剤組成物中の水含有量としては、低温安定性発現の観点から77〜98.5重量％であり、80〜95重量％が好ましい。
【００１９】
剥離剤組成物のｐＨとしては、配線金属等の防食性と安全性、作業環境の観点から、6 〜8 が好ましい。なお、ｐＨの調整は、酢酸、アンモニア水等を用いてすることができる。
【００２０】
本発明の剥離剤組成物には、配線金属の腐食をさらに抑制するために、各種腐食抑制剤を添加することが出来る。腐食抑制剤としては、本発明の剥離剤組成物の目的を阻害しないものであれば特に限定されるものではない。
【００２１】
本発明の剥離剤組成物は、半導体素子や半導体基板の製造工程のいずれの工程で使用しても良い。具体的には、半導体素子製造工程、例えば、レジスト現像後、ドライエッチング後、ウェットエッチング後、アッシング後等の工程で使用することができる。特に、デポの剥離性の観点から、ドライアッシング後の剥離工程に用いることが好ましい。
【００２２】
２．洗浄方法
本発明の洗浄方法は、本発明の剥離剤組成物を用いて、半導体基板又は半導体素子を剥離洗浄する方法である。
【００２３】
本発明に用いることのできる剥離洗浄手段としては、特に限定されないが、浸漬剥離洗浄、揺動剥離洗浄が好ましい。その他の剥離洗浄方法としては枚葉剥離洗浄、スピナーのような回転を利用した剥離洗浄、パドル洗浄、気中又は液中スプレーによる剥離洗浄及び超音波を用いた剥離洗浄等があげられる。
【００２４】
洗浄時の剥離剤組成物の温度は特に限定されるものではないが、デポ剥離性、デポの溶解性、金属配線の腐食抑制、安全性、操業性の観点から２０〜６０℃の範囲が好ましい。
【００２５】
上記の様にして得られる半導体基板及び半導体素子は、デポの残留がなく、配線材料に対して腐蝕が少ないものであり、ＬＣＤ、メモリ、ＣＰＵ等の電子部品の製造に好適に使用することができるという効果が発現される。
【００２６】
なお、本発明は、アルミニウム、銅、タングステン等の金属を含む配線を有する半導体基板及び半導体素子を対象とするものであり、中でもアルミニウム由来のデポに対する剥離性に優れる観点から、配線金属としてアルミニウムを含有する半導体基板及び半導体素子が好ましい。
【００２７】
【実施例】
実施例１〜８（但し、実施例６、７は参考例である）、比較例１〜７
以下の条件でアルミニウム（Ａｌ）配線パターンの剥離性、アルミニウム（Ａｌ）配線腐食抑制及び低温安定性の評価を行った。結果を表１、２に示す。
【００２８】
１．評価用ウェハ
以下の構造を有するアルミニウム配線（配線幅：１ミクロン）を用いたパターン付きウェハを１ｃｍ角に分割し、これを使用した。
（アルミニウム配線の構造）
TiN ／Al-Si ／TiN ／Ti／SiO2／下地
【００２９】
２．剥離剤組成物の調製
表１、表２に示す組成（数値は重量％）の剥離剤組成物を調製した。
【００３０】
３．剥離性評価
剥離方法：３０ｍｌの剥離剤組成物に４０℃で１５分間、評価用ウェハを浸漬し、剥離した。
すすぎ方法：３０ｍｌの超純水に２５℃で１分間、評価用ウェハを浸漬し、これを２回繰り返してすすぎとした。
評価方法：すすぎを終えた評価用ウェハの乾燥後、FE-SEM（電子走査型顕微鏡）を用いて50000 倍の倍率下で以下のようにアルミニウム配線（Al配線）パターンの剥離性の評価を行った。Al配線の腐食抑制についても同様に以下のように評価を行った。
【００３１】
（Al配線パターン剥離性）
◎：デポの残存が全く確認されない
○：デポが一部残存している
△：デポが大部分残存している
×：デポ除去できず
【００３２】
（Al配線腐食抑制）
◎：アルミニウム配線の腐食は全く確認されない
○：アルミニウム配線に孔蝕が一部発生している
△：アルミニウム配線に孔蝕が大部分発生している
×：アルミニウム配線全体に腐食が発生している
なお、合格品はAl配線パターン剥離性が○又は◎、且つAl配線腐食抑制が○又は◎であるもの。
【００３３】
４．低温安定性評価
表１、表２に示す組成（数値は重量％）の剥離剤組成物を低温（1 ℃）恒温倉庫にて6 ヶ月間、静置保管し、剥離剤組成物の安定性を以下のように評価を行った。
◎：剥離剤組成物に全く異常なし。
×：結晶析出、沈殿物等の異常発生あり。
なお、合格品は◎であるもの。
【００３４】
【表１】
【表２】
表１及び２の結果より、本発明の剥離剤組成物（実施例１〜８）は、デポに対しての剥離性に優れ、Ａｌ配線の腐食抑制に優れ、且つ低温安定性に優れたものであった。一方、多価カルボン酸以外のカルボン酸を用いた組成や多価カルボン酸の含有量が少ない、あるいは多い組成（比較例１〜３）においては剥離性が得られなかったり、充分な腐食抑制が得られなかった。また、グリコールエーテルを含まない組成（比較例４、５）においても、充分な剥離性が得られず、グリコールエーテルの含有量が多い組成（比較例６、７）では低温で良好な安定性が得られなかった。
【００３７】
【発明の効果】
本発明の剥離剤組成物は、半導体素子形成時に発生するデポに対し、優れた剥離性を有し、且つデポを溶解する機能を有するため、デポの再付着防止に優れる。また配線金属等の金属材料に対する防食性に優れ、低温安定性にも優れるので剥離性能の低下がなく、安定な性状と剥離性が得られる。したがって、本発明の剥離剤組成物を用いることで、品質の優れたＬＣＤ、メモリ、ＣＰＵ等の電子部品を製造することができるという効果が発現される。[0001]
BACKGROUND OF THE INVENTION
The present invention is used to remove a deposit (resist, insulating film, and oxidation product derived from a metal material) remaining after removing a resist used in a process of forming a semiconductor element on a semiconductor substrate such as a silicon wafer by ashing. The present invention relates to a release agent composition, a semiconductor substrate using the same, and a method for cleaning a semiconductor element.
[0002]
[Prior art]
In manufacturing a semiconductor element, a thin film is formed by a method such as sputtering, and a predetermined pattern is formed with a resist on the thin film by lithography. Using this as an etching resist, the lower layer thin film is selectively removed by etching, and then the resist is removed by ashing. This series of steps is repeated to produce a product.
[0003]
Various stripping agent compositions have been proposed as stripping agents for semiconductor devices using conventional aluminum wiring, and stripping agents using fluorine-containing compounds and stripping agents using amines typified by hydroxylamine are mainly used. Has been.
[0004]
However, as semiconductor elements are miniaturized, the amount of deposits generated after ashing has increased. When stripping is performed using a fluorine-containing compound-based stripping agent, stripping is insufficient or re-deposited (deposited once deposited). Floating in the release agent and reattaching on the semiconductor element). Moreover, when peeling is performed using an amine-based release agent, peeling at a high temperature (up to 70 ° C.) is required, which causes a problem in work environment such as safety and odor.
[0005]
Therefore, in order to solve the above problems, the present inventors have proposed a release agent containing polyvalent carboxylic acid and / or a salt thereof and water (see Patent Document 1).
[0006]
[Patent Document 1]
Japanese Patent Laid-Open No. 2000-214599
[Problems to be solved by the invention]
However, as a result of further research, it was found that a particularly excellent performance was exhibited in a release agent composition having a specific composition, and the present invention was completed. Therefore, the object of the present invention is to obtain excellent releasability with respect to the deposit generated after ashing and prevent re-deposition of the deposit, less corrosion on the wiring material, precipitation generation by crystallization even during low temperature storage, An object of the present invention is to provide a release agent composition capable of obtaining stable properties and releasability without degradation of the release performance due to the above, and a method for cleaning a semiconductor substrate or a semiconductor element using the release agent composition.
[0008]
[Means for Solving the Problems]
That is, the gist of the present invention is as follows.
[1] A release agent composition containing 0.5 to 5% by weight of a polyvalent carboxylate salt, 1 to 18% by weight of glycol ether and 77 to 98.5% by weight of water,
[2] A release agent composition comprising 0.5 to 5% by weight of a polyvalent carboxylate, 1 to 18% by weight of glycol ether and 77 to 98.5% by weight of water, and [3] the above [1] or [2 ] It is related with the cleaning method of a semiconductor substrate or a semiconductor element which has the process of peeling and cleaning a semiconductor substrate or a semiconductor element using the peeling agent composition of description.
[0009]
DETAILED DESCRIPTION OF THE INVENTION
1. Release Agent Composition The release agent composition of the present invention contains or contains 0.5 to 5% by weight of a polyvalent carboxylate salt, 1 to 18% by weight of glycol ether and 77 to 98.5% by weight of water as described above. By using such a release agent composition, an excellent release property can be obtained with respect to a deposit generated at the time of forming a semiconductor element, and it has a function of dissolving the deposit. In addition, there is little corrosion on metal materials such as wiring metal, and there is no precipitation due to crystallization even during storage at low temperatures, and there is no deterioration in peeling performance due to it, and stable properties and peelability even at low temperatures. The effect of being obtained is expressed.
[0010]
Specific examples of the polyvalent carboxylate include ammonium oxalate, ammonium phthalate, ammonium malonate, ammonium succinate, ammonium adipate, and ammonium citrate. These retain high solubility with respect to oxidized metal, and have extremely low solubility with respect to non-oxidized metal, and the selectivity between the deposit and the wiring metal is very high. That is, it shows high solubility for the deposit to be removed by peeling and hardly corrodes the metal wiring to be protected.
[0011]
Among these, from the viewpoints of releasability and depot solubility, ammonium oxalate, ammonium phthalate, and ammonium malonate, which are polyvalent carboxylates having a first dissociation constant pKa1 of 3.6 or less, are preferred, and ammonium oxalate is preferred. More preferred.
[0012]
The content of the polyvalent carboxylate in the release agent composition is 0.5 to 5% by weight, preferably 1 to 4% by weight, from the viewpoint of sufficient peelability and corrosion resistance of the wiring metal.
[0013]
Specific examples of glycol ethers include ethylene glycol monomethyl ether, ethylene glycol monoethyl ether, ethylene glycol monobutyl ether, diethylene glycol monomethyl ether, diethylene glycol monoethyl ether, diethylene glycol monobutyl ether, diethylene glycol dimethyl ether, diethylene glycol diethyl ether, and ethylene glycol monophenyl. Examples include ether, diethylene glycol monophenyl ether, triethylene glycol monophenyl ether, ethylene glycol monobenzyl ether, and diethylene glycol monobenzyl ether.
[0014]
Among these, a compound having a high permeability to a deposit is preferable from the viewpoint of sufficient peelability, and diethylene glycol monobutyl ether and triethylene glycol monophenyl ether are preferable from the viewpoint of miscibility with water.
[0015]
The glycol ether content in the release agent composition is 1 to 18% by weight, preferably 5 to 16% by weight, from the viewpoint of sufficient depot permeability and low temperature stability.
[0016]
Water is preferably used as the solvent for uniformly dissolving the polyvalent carboxylate and glycol ether.
[0017]
Water is not particularly limited as long as it does not interfere with the purpose of the release agent composition of the present invention. Examples of water include ultrapure water, pure water, ion exchange water, and distilled water.
[0018]
The water content in the release agent composition is 77 to 98.5% by weight, preferably 80 to 95% by weight, from the viewpoint of low temperature stability.
[0019]
The pH of the release agent composition is preferably 6 to 8 from the viewpoints of corrosion resistance and safety of wiring metal and the like, and the working environment. The pH can be adjusted using acetic acid, aqueous ammonia or the like.
[0020]
In order to further suppress the corrosion of the wiring metal, various corrosion inhibitors can be added to the release agent composition of the present invention. The corrosion inhibitor is not particularly limited as long as it does not hinder the purpose of the release agent composition of the present invention.
[0021]
The release agent composition of the present invention may be used in any process of manufacturing a semiconductor element or a semiconductor substrate. Specifically, it can be used in a semiconductor element manufacturing process, for example, a process after resist development, dry etching, wet etching, ashing, or the like. In particular, it is preferable to use it in the peeling process after dry ashing from the viewpoint of peelability of the deposit.
[0022]
2. Cleaning Method The cleaning method of the present invention is a method of peeling and cleaning a semiconductor substrate or a semiconductor element using the release agent composition of the present invention.
[0023]
The peeling cleaning means that can be used in the present invention is not particularly limited, but immersion peeling cleaning and rocking peeling cleaning are preferable. Other peeling cleaning methods include single wafer peeling cleaning, peeling cleaning using rotation such as a spinner, paddle cleaning, peeling cleaning by air or liquid spray, and peeling cleaning using ultrasonic waves.
[0024]
The temperature of the release agent composition at the time of cleaning is not particularly limited, but is preferably in the range of 20 to 60 ° C. from the viewpoints of deposit removability, deposit solubility, corrosion inhibition of metal wiring, safety, and operability. .
[0025]
The semiconductor substrate and the semiconductor element obtained as described above have no deposits and have little corrosion on the wiring material, and can be suitably used for manufacturing electronic components such as LCDs, memories, and CPUs. The effect that it is possible is expressed.
[0026]
The present invention is intended for a semiconductor substrate and a semiconductor element having a wiring containing a metal such as aluminum, copper, tungsten, etc. Among them, aluminum is used as a wiring metal from the viewpoint of excellent releasability from aluminum-derived deposits. The semiconductor substrate and semiconductor element to be contained are preferable.
[0027]
【Example】
Examples 1-8 (however, Examples 6 and 7 are reference examples) , Comparative Examples 1-7
Evaluation of peelability of aluminum (Al) wiring pattern, corrosion inhibition of aluminum (Al) wiring, and low-temperature stability was performed under the following conditions. The results are shown in Tables 1 and 2.
[0028]
1. A wafer with a pattern using aluminum wiring (wiring width: 1 micron) having the structure below the wafer for evaluation was divided into 1 cm squares and used.
(Aluminum wiring structure)
TiN / Al-Si / TiN / Ti / SiO 2 / Underground [0029]
2. Preparation of release agent composition Release agent compositions having the compositions shown in Tables 1 and 2 (numerical values are% by weight) were prepared.
[0030]
3. Peelability evaluation peeling method: A wafer for evaluation was immersed in 30 ml of a release agent composition at 40 ° C. for 15 minutes and peeled off.
Rinsing method: The wafer for evaluation was immersed in 30 ml of ultrapure water at 25 ° C. for 1 minute, and this was repeated twice.
Evaluation method: After the rinsed evaluation wafer is dried, the peelability of the aluminum wiring (Al wiring) pattern is evaluated using a FE-SEM (electronic scanning microscope) at a magnification of 50000 times as follows. It was. The corrosion inhibition of Al wiring was similarly evaluated as follows.
[0031]
(Al wiring pattern peelability)
◎: No depot remains. ○: Some depots remain. △: Most depots remain. ×: Depots cannot be removed.
(Al wiring corrosion suppression)
◎: Corrosion of aluminum wiring is not confirmed at all ○: Pitting corrosion is partly generated in aluminum wiring △: Pitting corrosion is mostly generated in aluminum wiring ×: Corrosion has occurred in the entire aluminum wiring In addition, an acceptable product is one in which the Al wiring pattern peelability is ○ or ◎ and Al wiring corrosion inhibition is ○ or ◎.
[0033]
4). Low temperature stability evaluation The release agent composition with the composition shown in Tables 1 and 2 (numerical value is% by weight) is stored in a low temperature (1 ° C) constant temperature warehouse for 6 months to improve the stability of the release agent composition. Evaluation was performed as follows.
A: No abnormality in the release agent composition.
X: Abnormal occurrence of crystal precipitation, precipitate, etc.
Passed products are ◎.
[0034]
[Table 1]
[Table 2]
From the results shown in Tables 1 and 2, the release agent compositions of the present invention (Examples 1 to 8) are excellent in releasability against deposits, excellent in suppressing corrosion of Al wiring, and excellent in low-temperature stability. Met. On the other hand, in a composition using a carboxylic acid other than the polyvalent carboxylic acid or a composition having a small or large content of the polyvalent carboxylic acid (Comparative Examples 1 to 3), no releasability is obtained or sufficient corrosion inhibition is achieved. It was not obtained. In addition, even in the composition containing no glycol ether (Comparative Examples 4 and 5), sufficient peelability was not obtained, and in the composition having a large content of glycol ether (Comparative Examples 6 and 7), good stability was obtained at low temperatures. It was not obtained.
[0037]
【The invention's effect】
The release agent composition of the present invention has an excellent releasability with respect to a deposit generated during the formation of a semiconductor element and has a function of dissolving the deposit, and thus is excellent in preventing re-deposition of the deposit. Moreover, since it is excellent in corrosion resistance to metal materials such as wiring metal and excellent in low-temperature stability, there is no deterioration in peeling performance, and stable properties and peelability can be obtained. Therefore, by using the release agent composition of the present invention, an effect that an electronic component such as an LCD, a memory, or a CPU having excellent quality can be produced is exhibited.
Claims (7)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2002256772A JP4170710B2 (en) | 2002-09-02 | 2002-09-02 | Release agent composition |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2002256772A JP4170710B2 (en) | 2002-09-02 | 2002-09-02 | Release agent composition |
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| JP2004094034A JP2004094034A (en) | 2004-03-25 |
| JP4170710B2 true JP4170710B2 (en) | 2008-10-22 |
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| JP2002256772A Expired - Lifetime JP4170710B2 (en) | 2002-09-02 | 2002-09-02 | Release agent composition |
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| JP4375991B2 (en) | 2003-04-09 | 2009-12-02 | 関東化学株式会社 | Semiconductor substrate cleaning liquid composition |
| JP6501492B2 (en) | 2014-10-31 | 2019-04-17 | 関東化學株式会社 | Composition for removing photoresist residue and / or polymer residue |
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