JP5480542B2 - 導電性ダイヤモンド電極並びに導電性ダイヤモンド電極を用いたオゾン生成装置 - Google Patents
導電性ダイヤモンド電極並びに導電性ダイヤモンド電極を用いたオゾン生成装置 Download PDFInfo
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- JP5480542B2 JP5480542B2 JP2009148342A JP2009148342A JP5480542B2 JP 5480542 B2 JP5480542 B2 JP 5480542B2 JP 2009148342 A JP2009148342 A JP 2009148342A JP 2009148342 A JP2009148342 A JP 2009148342A JP 5480542 B2 JP5480542 B2 JP 5480542B2
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- 229910003460 diamond Inorganic materials 0.000 title claims description 108
- 239000010432 diamond Substances 0.000 title claims description 108
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 title claims description 71
- 238000005868 electrolysis reaction Methods 0.000 claims description 67
- 239000000758 substrate Substances 0.000 claims description 67
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 56
- 239000012528 membrane Substances 0.000 claims description 50
- UQSQSQZYBQSBJZ-UHFFFAOYSA-N fluorosulfonic acid Chemical compound OS(F)(=O)=O UQSQSQZYBQSBJZ-UHFFFAOYSA-N 0.000 claims description 37
- 238000005341 cation exchange Methods 0.000 claims description 35
- 239000007787 solid Substances 0.000 claims description 18
- 239000005518 polymer electrolyte Substances 0.000 claims description 13
- 230000003746 surface roughness Effects 0.000 claims description 10
- 238000000034 method Methods 0.000 description 32
- 239000007789 gas Substances 0.000 description 26
- YADSGOSSYOOKMP-UHFFFAOYSA-N dioxolead Chemical compound O=[Pb]=O YADSGOSSYOOKMP-UHFFFAOYSA-N 0.000 description 24
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 23
- 229910052710 silicon Inorganic materials 0.000 description 23
- 239000010703 silicon Substances 0.000 description 23
- 239000012071 phase Substances 0.000 description 19
- 239000003014 ion exchange membrane Substances 0.000 description 16
- 239000000463 material Substances 0.000 description 13
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 10
- 229910052799 carbon Inorganic materials 0.000 description 10
- 238000006243 chemical reaction Methods 0.000 description 10
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 9
- 239000003054 catalyst Substances 0.000 description 9
- 238000010586 diagram Methods 0.000 description 9
- 239000001257 hydrogen Substances 0.000 description 9
- 229910052739 hydrogen Inorganic materials 0.000 description 9
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 8
- 238000004519 manufacturing process Methods 0.000 description 8
- 238000003825 pressing Methods 0.000 description 8
- 238000005268 plasma chemical vapour deposition Methods 0.000 description 7
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 6
- 239000003792 electrolyte Substances 0.000 description 6
- 239000008151 electrolyte solution Substances 0.000 description 6
- 239000000835 fiber Substances 0.000 description 6
- 239000007788 liquid Substances 0.000 description 6
- 230000007246 mechanism Effects 0.000 description 6
- 229910052751 metal Inorganic materials 0.000 description 6
- 239000002184 metal Substances 0.000 description 6
- 239000001301 oxygen Substances 0.000 description 6
- 229910052760 oxygen Inorganic materials 0.000 description 6
- 229920000642 polymer Polymers 0.000 description 6
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 5
- 230000015572 biosynthetic process Effects 0.000 description 5
- 229910052796 boron Inorganic materials 0.000 description 5
- 230000007423 decrease Effects 0.000 description 5
- 238000002156 mixing Methods 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 229910021642 ultra pure water Inorganic materials 0.000 description 5
- 239000012498 ultrapure water Substances 0.000 description 5
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 4
- 238000004042 decolorization Methods 0.000 description 4
- 239000006185 dispersion Substances 0.000 description 4
- 239000002019 doping agent Substances 0.000 description 4
- 239000004810 polytetrafluoroethylene Substances 0.000 description 4
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 238000004659 sterilization and disinfection Methods 0.000 description 4
- 229910052719 titanium Inorganic materials 0.000 description 4
- 239000010936 titanium Substances 0.000 description 4
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 229910001882 dioxygen Inorganic materials 0.000 description 3
- 238000001312 dry etching Methods 0.000 description 3
- 238000001459 lithography Methods 0.000 description 3
- 229910052758 niobium Inorganic materials 0.000 description 3
- 239000010955 niobium Substances 0.000 description 3
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 3
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 3
- 229910010271 silicon carbide Inorganic materials 0.000 description 3
- 230000001954 sterilising effect Effects 0.000 description 3
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 description 2
- 229920000557 Nafion® Polymers 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- UORVGPXVDQYIDP-UHFFFAOYSA-N borane Chemical compound B UORVGPXVDQYIDP-UHFFFAOYSA-N 0.000 description 2
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 239000004020 conductor Substances 0.000 description 2
- 239000000470 constituent Substances 0.000 description 2
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- 230000000694 effects Effects 0.000 description 2
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- 238000004050 hot filament vapor deposition Methods 0.000 description 2
- 238000007731 hot pressing Methods 0.000 description 2
- -1 hydrogen ions Chemical class 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229910017604 nitric acid Inorganic materials 0.000 description 2
- 238000010899 nucleation Methods 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 239000012466 permeate Substances 0.000 description 2
- 238000005240 physical vapour deposition Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 230000001681 protective effect Effects 0.000 description 2
- 239000003566 sealing material Substances 0.000 description 2
- 239000010865 sewage Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- 235000012431 wafers Nutrition 0.000 description 2
- 238000009736 wetting Methods 0.000 description 2
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 206010042674 Swelling Diseases 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 239000008346 aqueous phase Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 229910000085 borane Inorganic materials 0.000 description 1
- 229910052810 boron oxide Inorganic materials 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 230000008602 contraction Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000004332 deodorization Methods 0.000 description 1
- 230000001877 deodorizing effect Effects 0.000 description 1
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 238000009713 electroplating Methods 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 239000000383 hazardous chemical Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229920000554 ionomer Polymers 0.000 description 1
- 238000005304 joining Methods 0.000 description 1
- HTUMBQDCCIXGCV-UHFFFAOYSA-N lead oxide Chemical compound [O-2].[Pb+2] HTUMBQDCCIXGCV-UHFFFAOYSA-N 0.000 description 1
- 229910021514 lead(II) hydroxide Inorganic materials 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- YEXPOXQUZXUXJW-UHFFFAOYSA-N oxolead Chemical compound [Pb]=O YEXPOXQUZXUXJW-UHFFFAOYSA-N 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000007261 regionalization Effects 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 1
- 239000013076 target substance Substances 0.000 description 1
- TXEYQDLBPFQVAA-UHFFFAOYSA-N tetrafluoromethane Chemical compound FC(F)(F)F TXEYQDLBPFQVAA-UHFFFAOYSA-N 0.000 description 1
- DLYUQMMRRRQYAE-UHFFFAOYSA-N tetraphosphorus decaoxide Chemical compound O1P(O2)(=O)OP3(=O)OP1(=O)OP2(=O)O3 DLYUQMMRRRQYAE-UHFFFAOYSA-N 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- UONOETXJSWQNOL-UHFFFAOYSA-N tungsten carbide Chemical compound [W+]#[C-] UONOETXJSWQNOL-UHFFFAOYSA-N 0.000 description 1
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- C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
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- C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
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- C25B9/00—Cells or assemblies of cells; Constructional parts of cells; Assemblies of constructional parts, e.g. electrode-diaphragm assemblies; Process-related cell features
- C25B9/17—Cells comprising dimensionally-stable non-movable electrodes; Assemblies of constructional parts thereof
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Description
長期的に安定して電解を行うためには、電極触媒/イオン交換膜の接触部に水が常に供給され、安定な三相界面が形成されることが必要である。
の面圧であった。
シリコン板を水洗し、乾燥した後、前処理としてダイヤモンドパウダーをイソプロピルアルコール内に入れ、基板を入れて超音波を印加することで種付け処理を行った。成膜方法としては2.45GHzでのマイクロ波プラズマCVD法を用いた。ガスとしてH2、CH4、B2H6を用い、それぞれの流量を800sccm、20sccm、0.2sccm導入し、ガス圧力を3.2kPaとした。マイクロ波プラズマCVDによりドーパントとしてホウ素を含む導電性ダイヤモンド膜10を成膜して作製した。尚、実電解面積となる凸部頂部の総面積は6.25cm2である。
一方、凸部25の幅が2mm以上になると、凸部25がパーフルオロスルホン酸陽イオン交換膜9に接触しているにもかかわらず、凸部25の中間部に、常に水が入らず電解できない部分23が形成されてしまう。このように、凸部25の中間部に形成された、常に水が入らず電解できない部分23は、電解開始後には、図8(a)から図8(b)に示すように、気泡が導電性ダイヤモンド膜10の全面を覆うようになり、三相界面30の部分が殆どなくなり、電解ができない状態になってしまう。
尚、多数の帯状の基板29に換えて、角状、円状、その他の形状で突起物状に縦横に林立する基板を用いても良い。
尚、電極とイオン交換膜との良好な接触を得るには、予め電極表面にイオン交換膜と同様の組成のアイオノマーを電極表面に塗布し、ホットプレス法などの手法により接合して良好な接触を得ることが出来るが、電解時においては、電解液温度やジュール熱による発熱等の温度条件による材料の熱膨張や、イオン交換膜の含水状態による伸縮により容易に剥離するため、ある程度の押圧で接触を保持し続けることが、電解場を経時的に安定して保持するために必要である。
この他に超高圧で製造される合成ダイヤモンド粉末を樹脂等の結着剤を用いて基体に担持したダイヤモンド電極も使用可能である。
また、厚さ2.5mmのステンレス繊維焼結体(東京製綱(株))を陰極集電体とした。
パーフルオロスルホン酸陽イオン交換膜として、市販のパーフルオロスルホン酸型陽イオン交換膜(商品名:ナフィオン117、デュポン社製、カタログ厚さ183μm)を使用し、煮沸純水に30分間浸漬し、含水による膨潤処理を行った。
次に、ダイヤモンドソーを使ってダイシングにより表面に凸凹を多数作製した。尚、各試料の作製に用いたダイヤモンドソーの厚さは20μmである。
試料1〜7の凸部幅、凸部長さ、凹部幅、凹部深さは、表1に示した。実電解面積となる凸部の総面積は、試料1〜6が6.25cm2、試料7が15cm2であった。
また、厚さ2.5mmのステンレス繊維焼結体(東京製綱(株))を陰極集電体とした
2:陰極室排出口
3:陽極室
4:陰極室
5:陽極給電端子
6:陰極給電端子
7:陽極室供給口
8:陰極室供給口
9:パーフルオロスロホン酸陽イオン交換膜よりなる固体高分子電解室隔膜
10:導電性ダイヤモンド膜
11:基板
12:貫通孔
13:陰極
14:陰極集電体
15:シール材
16:締付ボルト
17:ナット
18:プレス板
19:陽極側気液分離器
20:陰極側気液分離器
21:電解用直流電源
22:陽極
23:常に水が入らず電解のできない部分
24:電解セル
25:凸部
26:凹部
27:隙間
28:給電体
29:帯状の基板
30:三相界面
Claims (5)
- 導電性ダイヤモンド電極の表面の全体に亘り、多数の凸凹部を有する基板と該基板の表面に被覆されたダイヤモンド膜よりなり、前記凸凹部の各凸部の形状が正方形状であり、かつ、前記凸凹部の各凸部の各辺の長さが0.2mm以上、1mm以下であることを特徴とする導電性ダイヤモンド電極。
- 前記基板に貫通孔を設けたことを特徴とする請求項1に記載の導電性ダイヤモンド電極。
- 前記凸凹部の各凸部の表面粗さRaが、0.2〜0.5μmであることを特徴とする請求項1又は2に記載の導電性ダイヤモンド電極。
- 固体高分子電解質隔膜の両側面に陽極及び陰極を密着させ、固体高分子電解質隔膜としてパーフルオロスルホン酸陽イオン交換膜を使用し、陽極として前記導電性ダイヤモンドを表面に有する電極を使用し、陽極室に純水を供給し、陽陰極間に直流電流を供給することによって、水を電気分解して、陽極室よりオゾンを生成させるオゾン生成装置において、請求項1〜3の何れか一つに記載の導電性ダイヤモンド電極を用いたことを特徴とするオゾン生成装置。
- 固体高分子電解質隔膜の両側面に陽極及び陰極を密着させ、固体高分子電解質隔膜としてパーフルオロスルホン酸陽イオン交換膜を使用し、陽極として前記導電性ダイヤモンドを表面に有する電極を使用し、陽極室に純水を供給し、陽陰極間に直流電流を供給することによって、水を電気分解して、陽極室よりオゾンを生成させるオゾン生成装置において、請求項1〜3の何れか一つに記載の導電性ダイヤモンド電極を用い、前記導電性ダイヤモンドを前記パーフルオロスルホン酸陽イオン交換膜の片面に、20kgf/cm2以上の面圧で押し付けて陽極とし、前記パーフルオロスルホン酸陽イオン交換膜の他方の面には陰極を押し付けた構造として、陽極側に水を供給しつつ、直流電流を供給して電解を行うことでオゾンを発生させることを特徴とするオゾン生成装置。
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US12/803,101 US8277623B2 (en) | 2009-06-23 | 2010-06-18 | Conductive diamond electrode and ozone generator using the same |
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