JPWO2018034317A1 - 炭酸水素水及びこれを使用する洗浄方法 - Google Patents
炭酸水素水及びこれを使用する洗浄方法 Download PDFInfo
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- JPWO2018034317A1 JPWO2018034317A1 JP2018534420A JP2018534420A JPWO2018034317A1 JP WO2018034317 A1 JPWO2018034317 A1 JP WO2018034317A1 JP 2018534420 A JP2018534420 A JP 2018534420A JP 2018534420 A JP2018534420 A JP 2018534420A JP WO2018034317 A1 JPWO2018034317 A1 JP WO2018034317A1
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- water
- hydrogen
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- hydrogen carbonate
- cleaning
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- 238000004140 cleaning Methods 0.000 title claims abstract description 59
- JYYOBHFYCIDXHH-UHFFFAOYSA-N carbonic acid;hydrate Chemical compound O.OC(O)=O JYYOBHFYCIDXHH-UHFFFAOYSA-N 0.000 title claims abstract description 53
- 238000000034 method Methods 0.000 title claims abstract description 40
- 239000000758 substrate Substances 0.000 claims abstract description 74
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 66
- 229910001868 water Inorganic materials 0.000 claims abstract description 59
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 58
- 239000001257 hydrogen Substances 0.000 claims abstract description 58
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 58
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims abstract description 39
- 239000001569 carbon dioxide Substances 0.000 claims abstract description 19
- 229910002092 carbon dioxide Inorganic materials 0.000 claims abstract description 19
- BVKZGUZCCUSVTD-UHFFFAOYSA-M Bicarbonate Chemical compound OC([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-M 0.000 claims abstract description 17
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 10
- 239000012498 ultrapure water Substances 0.000 claims description 10
- 230000033116 oxidation-reduction process Effects 0.000 claims description 7
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims description 4
- 238000005507 spraying Methods 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- 239000000243 solution Substances 0.000 description 19
- 239000000126 substance Substances 0.000 description 17
- 239000007788 liquid Substances 0.000 description 8
- 238000004519 manufacturing process Methods 0.000 description 8
- 230000000694 effects Effects 0.000 description 7
- 239000008213 purified water Substances 0.000 description 6
- 239000004065 semiconductor Substances 0.000 description 6
- 235000012431 wafers Nutrition 0.000 description 6
- 230000015572 biosynthetic process Effects 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- 238000002347 injection Methods 0.000 description 4
- 239000007924 injection Substances 0.000 description 4
- WFDIJRYMOXRFFG-UHFFFAOYSA-N Acetic anhydride Chemical compound CC(=O)OC(C)=O WFDIJRYMOXRFFG-UHFFFAOYSA-N 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 230000002378 acidificating effect Effects 0.000 description 3
- 150000001412 amines Chemical class 0.000 description 3
- 239000013043 chemical agent Substances 0.000 description 3
- 239000000356 contaminant Substances 0.000 description 3
- 238000011109 contamination Methods 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- -1 carboxylic acid compound Chemical class 0.000 description 2
- 238000005341 cation exchange Methods 0.000 description 2
- 238000005108 dry cleaning Methods 0.000 description 2
- 238000005868 electrolysis reaction Methods 0.000 description 2
- 238000011086 high cleaning Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 2
- 229910000679 solder Inorganic materials 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- GETQZCLCWQTVFV-UHFFFAOYSA-N trimethylamine Chemical compound CN(C)C GETQZCLCWQTVFV-UHFFFAOYSA-N 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- BTXXTMOWISPQSJ-UHFFFAOYSA-N 4,4,4-trifluorobutan-2-one Chemical compound CC(=O)CC(F)(F)F BTXXTMOWISPQSJ-UHFFFAOYSA-N 0.000 description 1
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 1
- BQACOLQNOUYJCE-FYZZASKESA-N Abietic acid Natural products CC(C)C1=CC2=CC[C@]3(C)[C@](C)(CCC[C@@]3(C)C(=O)O)[C@H]2CC1 BQACOLQNOUYJCE-FYZZASKESA-N 0.000 description 1
- RSWGJHLUYNHPMX-UHFFFAOYSA-N Abietic-Saeure Natural products C12CCC(C(C)C)=CC2=CCC2C1(C)CCCC2(C)C(O)=O RSWGJHLUYNHPMX-UHFFFAOYSA-N 0.000 description 1
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- KGMSWPSAVZAMKR-UHFFFAOYSA-N Me ester-3, 22-Dihydroxy-29-hopanoic acid Natural products C1CCC(C(O)=O)(C)C2C1(C)C1CCC(=C(C)C)C=C1CC2 KGMSWPSAVZAMKR-UHFFFAOYSA-N 0.000 description 1
- KGMSWPSAVZAMKR-ONCXSQPRSA-N Neoabietic acid Chemical compound [C@H]1([C@](CCC2)(C)C(O)=O)[C@@]2(C)[C@H]2CCC(=C(C)C)C=C2CC1 KGMSWPSAVZAMKR-ONCXSQPRSA-N 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 239000000443 aerosol Substances 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- 235000011089 carbon dioxide Nutrition 0.000 description 1
- VZCFVXZALPZXDN-UHFFFAOYSA-N carbonic acid;dihydrate Chemical compound [OH3+].[OH3+].[O-]C([O-])=O VZCFVXZALPZXDN-UHFFFAOYSA-N 0.000 description 1
- 150000001244 carboxylic acid anhydrides Chemical class 0.000 description 1
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 150000001991 dicarboxylic acids Chemical class 0.000 description 1
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 235000019253 formic acid Nutrition 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000001678 irradiating effect Effects 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000002923 metal particle Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- DUCKXCGALKOSJF-UHFFFAOYSA-N pentanoyl pentanoate Chemical compound CCCCC(=O)OC(=O)CCCC DUCKXCGALKOSJF-UHFFFAOYSA-N 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 150000003335 secondary amines Chemical class 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 150000003512 tertiary amines Chemical class 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
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- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
- C11D7/02—Inorganic compounds
- C11D7/04—Water-soluble compounds
- C11D7/08—Acids
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- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02041—Cleaning
- H01L21/02043—Cleaning before device manufacture, i.e. Begin-Of-Line process
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- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
- H01L21/302—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to change their surface-physical characteristics or shape, e.g. etching, polishing, cutting
- H01L21/304—Mechanical treatment, e.g. grinding, polishing, cutting
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- B01F2101/00—Mixing characterised by the nature of the mixed materials or by the application field
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01F23/20—Mixing gases with liquids
- B01F23/23—Mixing gases with liquids by introducing gases into liquid media, e.g. for producing aerated liquids
- B01F23/237—Mixing gases with liquids by introducing gases into liquid media, e.g. for producing aerated liquids characterised by the physical or chemical properties of gases or vapours introduced in the liquid media
- B01F23/2376—Mixing gases with liquids by introducing gases into liquid media, e.g. for producing aerated liquids characterised by the physical or chemical properties of gases or vapours introduced in the liquid media characterised by the gas being introduced
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Abstract
Description
(1)化学薬品は、汚染物質除去には効果があるが、基板に形成したパターン等を一緒に削除したり、毀損するおそれがあり、化学薬品を使用した後、水等を利用して基板から化学薬品をきれいに除去しなければならない。
(2)また、化学薬品を除去するために使用した排水は、毒性を有するので、人体に害を及ぼすおそれがあるだけでなく、廃水処理にも気を使わなければならない。
(3)さらに、化学薬品を使用した後、基板に残った化学薬品を除去するために多くの水が必要である。
これらの問題を解決するための一つの方法として、化学薬品を使用せずに、不純物を除去することができる新しい洗浄技術が求められている。
(1)溶存水素濃度が0.1ppm〜2.0ppmである水素水に二酸化炭素を溶解したことを特徴とする炭酸水素水。
(2)水素水が、pHが5.5〜6.8であり、酸化還元電位が−200mV〜−700mVであり、溶存水素濃度が0.1ppm〜2.0ppmであることを特徴とする上記(1)記載の炭酸水素水。
(3)水素水が、純水若しくは超純水に水素ガスを溶解した水素水、又は純水若しくは超純水を電気分解した水素水であることを特徴とする上記(1)又は(2)記載の炭酸水素水。
(4)pHが4.0〜6.8であり、酸化還元電位が−50mV〜−650mVであり、電気伝導度が0.072μS/cm〜80μS/cmであることを特徴とする炭酸水素水。
(5)pHが4.0〜6.8であり、酸化還元電位が−50mV〜−650mVであり、電気伝導度が0.072μS/cm〜80μS/cmであることを特徴とする上記(1)〜(3)のいずれかに記載の炭酸水素水。
(6)基板を上記(1)〜(5)のいずれかに記載の炭酸水素水に浸漬する、又は基板に上記(1)〜(5)のいずれかに記載の炭酸水素水を噴射することにより、基板を洗浄することを特徴とする洗浄方法。
(7)基板を80〜300rpmで回転させ、炭酸水素水に1〜3MHzのメガソニックを印加しながら、前記炭酸水素水を5〜10分間基板に噴射して基板を洗浄することを特徴とする上記(6)記載の洗浄方法。
(8)炭酸水素水を40℃〜85℃で予熱することを特徴とする上記(6)又は(7)記載の洗浄方法。
(1)水素水に二酸化炭素(CO2)を溶解するため、酸でありながら、酸化還元電位が還元力を持ち、特に電気伝導度が高い炭酸水素水となるので、化学薬品を使用しなくても洗浄力の高い洗浄液を得ることができる。
(2)還元力が高い炭酸水素水は、基板洗浄するときに微粒子除去率を高めることができ、しかも還元力が高く、基板に形成したパターンへの酸化膜の形成を抑制し、洗浄効果をさらに高めることができる。
(3)基板を洗浄するときに、炭酸水素水に1〜3MHzのメガソニックを印加した場合、メガソニックエネルギーが基板全体に均一に伝達されるようにして、微粒子除去効率をさらに高めることができる。
(4)特に、炭酸水素水温度を予め設定した温度、例えば、50℃〜85℃で予熱して使用した場合、酸性度と還元力と電気伝導度をさらに高めて酸化膜形成の抑制に加え、微粒子除去を通じて洗浄効果をより一層高めることができる。
したがって、本願明細書に記載された実施例と図面に図示された構成は、本発明の最も望ましい一実施例に過ぎないだけで、本発明の技術的思想をすべて代弁することではないので、本出願の時点からこれらを代替できる多様な均等物と変形例があり得ることを理解しなければならない。
(1)pHと酸化還元電位(ORP):TOA DKK社HM−31P
(2)電気伝導度:TOA社 CM−21PW
(3)二酸化炭素濃度:TSI社 7515
(4)溶存水素濃度:TOA DKK社 DH−35A
本発明の炭酸水素水は水素水に二酸化炭素(CO2)を溶解して得ることができる。このとき、水素水は、純水、超純水のような電気伝導度が50μS/cm以下の精製水に水素ガスを溶解したり、前記精製水を電気分解して得られた水素水を好適に使用できる。このような水素水としては、溶存水素濃度が0.1ppm〜2.0ppmである水素水が好ましい。さらに、本発明における水素水は、純水、超純水のような電気伝導度が50μS/cm以下の精製水を電気分解して得られた水素水が好ましい。特に、本発明の好ましい実施形態では、このようにして得られた水素水は、pHが5.5〜6.8であり、酸化還元電位(ORP)が−200mV〜−700mVであり、溶存水素濃度が0.1ppm〜2.0ppmであることが好ましい。また、このような水素水に二酸化炭素(CO2)を溶解した炭酸水素水は、pHが4.0〜6.8であり、酸化還元電位が−50mV〜−650mVであり、電気伝導度が0.072μS/cm〜80μS/cmであるものが好ましく使用できる。炭酸水素水における二酸化炭素(CO2)の濃度は、0.1ppm〜2.0ppmが好ましく、0.5ppm〜2.0ppmがより好ましい。
本発明の炭酸水素水を使用した基板洗浄プロセスの一実施形態は、以下の通りである。まず、基板を所定の回転速度で回転しながら洗浄するスピン洗浄方法で洗浄する。このとき、基板は、好ましくは80〜300rpmの速度で回転させる。一方で、本発明の炭酸水素水は、このように回転する基板に対して、ノズル等を用いて基板表面に噴射される。このとき、炭酸水素水に、1〜3MHzのメガソニックを印加して、高周波エネルギーを持たせることにより、高周波振動などのエネルギーを利用しながら、このエネルギーにより基板全体をまんべんなく洗浄することができる。これらの炭酸水素水の噴射は、5〜10分間続けて行われる。また、他の実施形態として、本発明の炭酸水素水を満たした容器中に基板を浸漬させる方法や、この際、容器中の炭酸水素水に1〜3MHzのメガソニックを印加する方法も挙げられる。
まず、超純水を電気分解して水素水を得た。この時の水素水は、pHが6.5であり、酸化還元電位が−683mVであった。続いて、この水素水を密閉容器に入れて、二酸化炭素(CO2)を2ppm溶解して炭酸水素水を得た。この時の炭酸水素水は、pHが4.6であり、酸化還元電位(ORP)が−470mVであり、電気伝導度が43.2μS/cmであった。
このようにして得られた水素水、及び炭酸水素水の二酸化炭素(CO2)の濃度に基づいたpHおよび酸化還元電位(ORP)と電気伝導度の変化を比較した結果は表1の通りである。表1から、二酸化炭素の濃度が高くなることによって、より強い酸性を示し、酸化還元電位は多少落ちるが還元力を持つことができる範囲であり、電気伝導度は急激に高まったことが分かる。
オゾン水で酸化したシリコンウエハにAl2O3、CMPスラリーを一つのウエハに5,000個を汚染させた後、基板を80rpmで回転させながら、その表面に実施例1と同様の方法で得られた常温の炭酸水素水(pH4.9、ORP−500mV、電気伝導度18μS/cm)をスプレーノズル方式で噴射した。このとき、炭酸水素水には、2MHzのメガソニックを印加し、噴射時間は8分間続けた。その結果、汚染物質(0.07μm<)は除去率80%以上で除去された。
Claims (8)
- 溶存水素濃度が0.1ppm〜2.0ppmである水素水に二酸化炭素を溶解したことを特徴とする炭酸水素水。
- 水素水が、pHが5.5〜6.8であり、酸化還元電位が−200mV〜−700mVであり、溶存水素濃度が0.1ppm〜2.0ppmであることを特徴とする請求項1記載の炭酸水素水。
- 水素水が、純水若しくは超純水に水素ガスを溶解した水素水、又は純水若しくは超純水を電気分解した水素水であることを特徴とする請求項1又は2記載の炭酸水素水。
- pHが4.0〜6.8であり、酸化還元電位が−50mV〜−650mVであり、電気伝導度が0.072μS/cm〜80μS/cmであることを特徴とする炭酸水素水。
- pHが4.0〜6.8であり、酸化還元電位が−50mV〜−650mVであり、電気伝導度が0.072μS/cm〜80μS/cmであることを特徴とする請求項1〜3のいずれかに記載の炭酸水素水。
- 基板を請求項1〜5のいずれかに記載の炭酸水素水に浸漬する、又は基板に請求項1〜5のいずれかに記載の炭酸水素水を噴射することにより、基板を洗浄することを特徴とする洗浄方法。
- 基板を80〜300rpmで回転させ、炭酸水素水に1〜3MHzのメガソニックを印加しながら、前記炭酸水素水を5〜10分間基板に噴射して基板を洗浄することを特徴とする請求項6記載の洗浄方法。
- 炭酸水素水を40℃〜85℃で予熱することを特徴とする請求項6又は7記載の洗浄方法。
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