JP4762822B2 - 薬液混合方法および薬液混合装置 - Google Patents
薬液混合方法および薬液混合装置 Download PDFInfo
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- 239000007788 liquid Substances 0.000 title claims description 132
- 238000002156 mixing Methods 0.000 title claims description 92
- 239000000126 substance Substances 0.000 title claims description 77
- 238000000034 method Methods 0.000 title claims description 37
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 358
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 181
- QOSATHPSBFQAML-UHFFFAOYSA-N hydrogen peroxide;hydrate Chemical compound O.OO QOSATHPSBFQAML-UHFFFAOYSA-N 0.000 claims description 32
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 235000012431 wafers Nutrition 0.000 description 39
- 239000002253 acid Substances 0.000 description 35
- 238000003860 storage Methods 0.000 description 19
- 239000000243 solution Substances 0.000 description 17
- 238000004140 cleaning Methods 0.000 description 13
- 239000011259 mixed solution Substances 0.000 description 13
- 239000008155 medical solution Substances 0.000 description 11
- 230000000052 comparative effect Effects 0.000 description 8
- 238000010586 diagram Methods 0.000 description 8
- 238000004519 manufacturing process Methods 0.000 description 8
- 239000000758 substrate Substances 0.000 description 7
- 238000006243 chemical reaction Methods 0.000 description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- MHSVJXJTONHWLL-VEDIPHOLSA-N (3e,5r)-5-methyl-3-(oxolan-2-ylidene)oxolane-2,4-dione Chemical compound O=C1[C@@H](C)OC(=O)\C1=C/1OCCC\1 MHSVJXJTONHWLL-VEDIPHOLSA-N 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 239000000203 mixture Substances 0.000 description 2
- 239000007800 oxidant agent Substances 0.000 description 2
- 230000001502 supplementing effect Effects 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
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Description
ここで、硫酸と過酸化水素水との混合には二種類のパターンがある。
まず、一つ目のパターンとしては、以下の化学反応が挙げられる。
H2SO4+H2O2→H2SO4+H2O+O※・・・式(1)
式(1)による反応により、活性酸素(O※)が生成される。この活性酸素は強い酸化剤である。
H2SO4+H2O2→H2SO5+H2O・・・式(2)
式(2)による反応により、カロ酸(ペルオキソ酸ともいう、H2SO5)が生成される。このカロ酸も活性酸素と同様に強い酸化剤であるが、ウエハに付着するレジストのような有機物を分解するには、カロ酸の方が活性酸素よりも効果が大きい。すなわち、硫酸と過酸化水素水を混合させ、カロ酸を生成させることにより、ウエハに付着するレジストを十分に剥離することができるようになる。
図8の薬液混合過程に使用される薬液混合装置は、過酸化水素水が内槽ではなく外槽に供給されるようになっている点以外は図6に示す薬液混合装置と同様のものである。
まず、図8(b)に示すように、硫酸供給バルブが開とされ、内槽が満杯となるよう硫酸が内槽に供給される。次に、図8(c)に示すように、硫酸供給バルブが閉とされるとともに過酸化水素水供給バルブが開とされ、外槽に過酸化水素水が供給される。その後、図8(d)に示すように、過酸化水素水供給バルブが閉とされるとともに硫酸供給バルブが再び開とされ、内槽に硫酸が更に供給される。ここで、内槽は既に硫酸が満杯となっているので、硫酸が外槽にあふれ、この外槽内において硫酸と過酸化水素水が混合される。
しかも、過酸化水素水の補充を行う際に供給される過酸化水素水は直接的に戻し管に送られることとなる。このため、戻し管内において補充された過酸化水素水と硫酸とのいわゆる攪拌が行われ、この際に過酸化水素水の量は相対的に少ないので、戻し管内でカロ酸が十分に生成されることとなる。このため、過酸化水素水の補充により生成されるカロ酸の量の割合が大きくなり、混合液におけるレジストの剥離性能を維持することができる。
また、本発明の薬液混合装置においては、前記戻し管にはヒータが介設されており、前記制御装置は、前記戻しポンプが作動されてから予め設定された時間が経過した後にこのヒータを作動させるよう当該ヒータの制御をも行うことが好ましい。
ここで、硫酸と過酸化水素水を混合させてカロ酸を生成するにあたり、混合前の液体の温度が高すぎる場合にはカロ酸を十分に生成することができないが、戻しポンプを作動させるがヒータは作動させないという時間帯を十分に確保することにより、液体の循環のみを行う時間が得られ、このときにカロ酸を十分に生成することができるようになる。
このうち、図1は、本実施の形態における薬液混合装置の構成を示す概略構成図であり、図2は、図1の薬液混合装置における内槽および外槽の上面図である。また、図3(a)〜(f)は、図1の薬液混合装置を用いた薬液混合過程を順次示す図である。
なお、図1乃至図3を参照するにあたり、図6に示した一般的な薬液混合装置と同一部材には同一符号を付して説明する。
図1に示すような薬液混合装置を準備した。この薬液混合装置は、ウエハWが収容されるべき内槽10と、内槽10の周囲に設けられこの内槽10からあふれた液体が流入する外槽12とを備えている。また、外槽12内の液体を内槽10へ戻すための戻し管14が設置されている。この戻し管14には、外槽12内の液体を内槽10へ送る戻しポンプ16、戻し管14自体の振動等を軽減させるためのダンパ18、戻し管14内を通過する液体の加熱を行うヒータ20、および戻し管14内を通過する液体の濾過を行うフィルター22がそれぞれ直列状態で介設されている。
比較例においても図1に示すような薬液混合装置を準備した。この薬液混合装置における内槽10および外槽の容積、戻し管14および戻しポンプ16の態様、ならびに硫酸供給手段および過酸化水素水供給手段の態様は、それぞれ前述の本実施例のものと同様であったが、制御装置40による制御内容は図3に示すような本実施例のものと異なっており、比較例における制御内容は図8に示す通りであった。この制御内容の詳細については以下に説明する。
前述のように、硫酸と過酸化水素水とを混合させるとカロ酸が生成されるが、このカロ酸の量を直接的に測定する方法は現在では確立されていない。したがって、レジストが付着したウエハを、カロ酸を含む硫酸と過酸化水素水との混合液に浸し、このレジストの剥離の度合いによりカロ酸の相対的な量を推定する方法が一般に用いられている。
10a ウエハ保持具
12 外槽
14 戻し管
14a 取水口
16 戻しポンプ
18 ダンパ
20 ヒータ
22 フィルター
24 硫酸貯留槽
26 硫酸供給バルブ
28 硫酸供給管
28a 硫酸供給口
30 過酸化水素水貯留槽
32 過酸化水素水供給バルブ
34 過酸化水素水供給管
34a 過酸化水素水供給口
36 過酸化水素水補充管
38 過酸化水素水補充バルブ
40 制御装置
Claims (4)
- 硫酸と過酸化水素水とを混合させる薬液混合方法であって、
内槽、この内槽の周囲に設けられ内槽からあふれた液体が流入する外槽、外槽内の液体を内槽へ戻すための戻し管、および戻し管に介設され外槽内の液体を内槽へ送る戻しポンプをそれぞれ準備する工程と、
内槽に硫酸を供給する硫酸供給工程であって、この内槽を硫酸で満杯にするとともに内槽からあふれた硫酸が外槽にも流入するようにする硫酸供給工程と、
前記硫酸供給工程の後に内槽または外槽に過酸化水素水を供給する過酸化水素水供給工程であって、外槽に過酸化水素水を流入させこの外槽内に過酸化水素水および硫酸の2種類の液体を貯留させる過酸化水素水供給工程と、
前記過酸化水素水供給工程の開始と同時に前記戻しポンプを作動させ、外槽内の過酸化水素水および硫酸の2種類の液体を同時に内槽へ送りこの際に過酸化水素水と硫酸とを混合させる戻しポンプ作動工程と、
を備え、
過酸化水素水補充管により過酸化水素水の補充を行う過酸化水素水補充工程が更に設けられており、この過酸化水素水補充管は前記戻し管に連通していることを特徴とする薬液混合方法。 - 前記戻し管にはヒータが介設されており、
前記戻しポンプ作動工程が開始されてから予め設定された時間が経過した後に、前記ヒータを作動させるヒータ作動工程を行うことを特徴とする請求項1記載の薬液混合方法。 - 硫酸と過酸化水素水とを混合させる薬液混合装置であって、
内槽と、
この内槽の周囲に設けられ内槽からあふれた液体が流入する外槽と、
外槽内の液体を内槽へ戻すための戻し管と、
戻し管に介設され外槽内の液体を内槽へ送る戻しポンプと、
内槽に硫酸を供給する硫酸供給手段と、
内槽または外槽に過酸化水素水を供給する過酸化水素水供給手段と、
前記硫酸供給手段、前記過酸化水素水供給手段および前記戻しポンプを制御する制御装置であって、まず硫酸供給手段により内槽を硫酸で満杯にするとともに外槽にも内槽からあふれた硫酸が流入するようにし、次に過酸化水素水供給手段により内槽または外槽に過酸化水素水を供給して外槽に過酸化水素水を流入させてこの外槽内に過酸化水素水および硫酸の2種類の液体を貯留させ、この過酸化水素水供給手段の動作の開始と同時に戻しポンプを作動させるよう各々の制御を行う制御装置と、
を備え、
過酸化水素水の補充を行うための過酸化水素水補充管を、前記戻し管に連通するよう設置したことを特徴とする薬液混合装置。 - 前記戻し管にはヒータが介設されており、
前記制御装置は、前記戻しポンプが作動されてから予め設定された時間が経過した後にこのヒータを作動させるよう当該ヒータの制御をも行うことを特徴とする請求項3記載の薬液混合装置。
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SG200705612-0A SG139708A1 (en) | 2006-08-03 | 2007-08-01 | Chemical-liquid mixing method and chemical-liquid mixing apparatus |
US11/882,402 US9099502B2 (en) | 2006-08-03 | 2007-08-01 | Chemical-liquid mixing method and chemical-liquid mixing apparatus |
TW096128447A TWI402901B (zh) | 2006-08-03 | 2007-08-02 | Liquid mixture method and liquid medicine mixing device |
EP07015193A EP1884280B1 (en) | 2006-08-03 | 2007-08-02 | Chemical-liquid mixing method and apparatus for the cleaning of substrates such as semiconductor wafers |
KR1020070077698A KR101061949B1 (ko) | 2006-08-03 | 2007-08-02 | 약액 혼합 방법 및 약액 혼합 장치 |
CN2007101399220A CN101143713B (zh) | 2006-08-03 | 2007-08-03 | 药液混合方法和药液混合装置 |
US14/750,319 US9339775B2 (en) | 2006-08-03 | 2015-06-25 | Chemical-liquid mixing method and chemical-liquid mixing apparatus |
US15/130,282 US9415356B1 (en) | 2006-08-03 | 2016-04-15 | Chemical-liquid mixing method and chemical-liquid mixing apparatus |
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EP1884280B1 (en) | 2011-10-12 |
KR101061949B1 (ko) | 2011-09-05 |
US9099502B2 (en) | 2015-08-04 |
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TW200814169A (en) | 2008-03-16 |
US9415356B1 (en) | 2016-08-16 |
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US20150290599A1 (en) | 2015-10-15 |
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