JP5520280B2 - 電解用陽極を使用するフッ素含有物質の電解合成方法 - Google Patents
電解用陽極を使用するフッ素含有物質の電解合成方法 Download PDFInfo
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- 238000005868 electrolysis reaction Methods 0.000 title claims description 59
- 238000000034 method Methods 0.000 title claims description 24
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 title claims description 22
- 239000011737 fluorine Substances 0.000 title claims description 22
- 229910052731 fluorine Inorganic materials 0.000 title claims description 22
- 230000015572 biosynthetic process Effects 0.000 title description 11
- 238000003786 synthesis reaction Methods 0.000 title description 10
- 239000000463 material Substances 0.000 title description 7
- 229910003460 diamond Inorganic materials 0.000 claims description 46
- 239000010432 diamond Substances 0.000 claims description 46
- 239000000758 substrate Substances 0.000 claims description 35
- 229910021397 glassy carbon Inorganic materials 0.000 claims description 12
- 150000001875 compounds Chemical class 0.000 claims description 5
- 150000002222 fluorine compounds Chemical class 0.000 claims description 5
- 230000002194 synthesizing effect Effects 0.000 claims description 5
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 4
- 239000004020 conductor Substances 0.000 claims description 4
- 230000035699 permeability Effects 0.000 claims description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 36
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 28
- 229910052759 nickel Inorganic materials 0.000 description 18
- 239000007789 gas Substances 0.000 description 17
- 230000000694 effects Effects 0.000 description 16
- 229910052799 carbon Inorganic materials 0.000 description 13
- 229910002804 graphite Inorganic materials 0.000 description 12
- 239000010439 graphite Substances 0.000 description 12
- 238000000576 coating method Methods 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 8
- QLOAVXSYZAJECW-UHFFFAOYSA-N methane;molecular fluorine Chemical compound C.FF QLOAVXSYZAJECW-UHFFFAOYSA-N 0.000 description 8
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 7
- 239000002585 base Substances 0.000 description 7
- 238000006243 chemical reaction Methods 0.000 description 7
- 239000011248 coating agent Substances 0.000 description 7
- 229910052710 silicon Inorganic materials 0.000 description 7
- 239000010703 silicon Substances 0.000 description 7
- 239000000126 substance Substances 0.000 description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- 238000004050 hot filament vapor deposition Methods 0.000 description 5
- 238000005259 measurement Methods 0.000 description 5
- 150000004812 organic fluorine compounds Chemical class 0.000 description 5
- 239000002245 particle Substances 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 4
- GQPLMRYTRLFLPF-UHFFFAOYSA-N Nitrous Oxide Chemical compound [O-][N+]#N GQPLMRYTRLFLPF-UHFFFAOYSA-N 0.000 description 4
- 239000003575 carbonaceous material Substances 0.000 description 4
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 4
- 238000001069 Raman spectroscopy Methods 0.000 description 3
- 238000005229 chemical vapour deposition Methods 0.000 description 3
- 238000005260 corrosion Methods 0.000 description 3
- 230000007797 corrosion Effects 0.000 description 3
- 239000002019 doping agent Substances 0.000 description 3
- 150000002894 organic compounds Chemical class 0.000 description 3
- 230000035515 penetration Effects 0.000 description 3
- -1 perfluoro compound Chemical class 0.000 description 3
- 239000011347 resin Substances 0.000 description 3
- 229920005989 resin Polymers 0.000 description 3
- YPJHKJFGSWJFTM-UHFFFAOYSA-N 1,1,1-trifluoro-n,n-bis(trifluoromethyl)methanamine Chemical compound FC(F)(F)N(C(F)(F)F)C(F)(F)F YPJHKJFGSWJFTM-UHFFFAOYSA-N 0.000 description 2
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 229910018499 Ni—F Inorganic materials 0.000 description 2
- 229910021529 ammonia Inorganic materials 0.000 description 2
- 229910003481 amorphous carbon Inorganic materials 0.000 description 2
- 239000010405 anode material Substances 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 239000007888 film coating Substances 0.000 description 2
- 238000009501 film coating Methods 0.000 description 2
- 229910000040 hydrogen fluoride Inorganic materials 0.000 description 2
- 150000002484 inorganic compounds Chemical class 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 229960001730 nitrous oxide Drugs 0.000 description 2
- 235000013842 nitrous oxide Nutrition 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 238000005240 physical vapour deposition Methods 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 239000011698 potassium fluoride Substances 0.000 description 2
- NROKBHXJSPEDAR-UHFFFAOYSA-M potassium fluoride Chemical compound [F-].[K+] NROKBHXJSPEDAR-UHFFFAOYSA-M 0.000 description 2
- 239000002243 precursor Substances 0.000 description 2
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 description 2
- 238000004611 spectroscopical analysis Methods 0.000 description 2
- 230000003746 surface roughness Effects 0.000 description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical group [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- 229910016509 CuF 2 Inorganic materials 0.000 description 1
- 229910001209 Low-carbon steel Inorganic materials 0.000 description 1
- 229910017855 NH 4 F Inorganic materials 0.000 description 1
- 229910000990 Ni alloy Inorganic materials 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 208000034809 Product contamination Diseases 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 229910001515 alkali metal fluoride Inorganic materials 0.000 description 1
- 229910001618 alkaline earth metal fluoride Inorganic materials 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 238000010000 carbonizing Methods 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 239000012461 cellulose resin Substances 0.000 description 1
- 238000004769 chrono-potentiometry Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000007323 disproportionation reaction Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000003411 electrode reaction Methods 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 239000012025 fluorinating agent Substances 0.000 description 1
- 238000003682 fluorination reaction Methods 0.000 description 1
- 239000007849 furan resin Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- QKCGXXHCELUCKW-UHFFFAOYSA-N n-[4-[4-(dinaphthalen-2-ylamino)phenyl]phenyl]-n-naphthalen-2-ylnaphthalen-2-amine Chemical compound C1=CC=CC2=CC(N(C=3C=CC(=CC=3)C=3C=CC(=CC=3)N(C=3C=C4C=CC=CC4=CC=3)C=3C=C4C=CC=CC4=CC=3)C3=CC4=CC=CC=C4C=C3)=CC=C21 QKCGXXHCELUCKW-UHFFFAOYSA-N 0.000 description 1
- 238000005192 partition Methods 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 238000005268 plasma chemical vapour deposition Methods 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000010802 sludge Substances 0.000 description 1
- 235000013024 sodium fluoride Nutrition 0.000 description 1
- 239000011775 sodium fluoride Substances 0.000 description 1
- AKHNMLFCWUSKQB-UHFFFAOYSA-L sodium thiosulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=S AKHNMLFCWUSKQB-UHFFFAOYSA-L 0.000 description 1
- 235000019345 sodium thiosulphate Nutrition 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 238000007751 thermal spraying Methods 0.000 description 1
- 229920001187 thermosetting polymer Polymers 0.000 description 1
- WXRGABKACDFXMG-UHFFFAOYSA-N trimethylborane Chemical compound CB(C)C WXRGABKACDFXMG-UHFFFAOYSA-N 0.000 description 1
Description
本発明者らは、鋭意検討した結果、グラッシーカーボンから成る導電性基体の少なくとも一部を導電性ダイヤモンド膜で被覆した電解用電極は、無水HFを含有する電解浴での電解に於いて、電解浴中の無水HF濃度が高い場合であっても、陽極効果、電極の消耗、電極の崩壊が発生せず、長期の電解継続が可能な電極であることを発見した。
本発明からなる電極の導電性基体は、グラッシーカーボンから成り、その形状は特に限定されず、板状、棒状、パイプ状、或いは球状などが使用できる。グラッシーカーボンの気体透過度は、10-7cm2/sec以下であることが好ましく、更に好ましくは10-10cm2/sec以下である。
炭素源となるメタン、アルコール、アセトンなどの有機化合物とドーパントを水素ガスなどと共にフィラメントに供給する。フィラメントを水素ラジカルなどが発生する温度1800−2800℃に加熱し、この雰囲気内にダイヤモンドが析出する温度領域(750〜950℃)になるように導電性基体を配置する。混合ガスの供給速度は反応容器のサイズに依るが、圧力は15〜760Torrであることが好ましい。
導電性基体としてグラッシーカーボン板を使用し、熱フィラメントCVD装置を用いて、以下の条件で導電性ダイヤモンド電極を作成した。
陽極にグラファイト板を用いた以外は実施例1と同様の電解条件で、0℃に保持した無水HF浴中で電流−電位曲線の測定を実施した。
陽極にニッケル板を用いた以外は実施例1と同様の電解条件で、0℃に保持した無水HF浴中で電流−電位曲線の測定を実施した。
導電性基体としてシリコン板を使用した以外は実施例1と同様の手順で導電性ダイヤモンド電極を作製した。
導電性基体としてグラフィイト板を使用した以外は実施例1と同様の手順で導電性ダイヤモンド電極を作製した。
導電性基体としてグラッシーカーボン板を使用し、熱フィラメントCVD装置を用いて、実施例1と同様の方法で導電性ダイヤモンド電極を作成した。
陽極にグラファイト板を用いた以外は実施例2と同様の方法で、建浴直後の(CH3)4NF・5HF電解浴中で電解を実施した。
陽極にニッケル板を用いた以外は実施例2と同様の方法で、建浴直後の(CH3)4NF・5HF電解浴中で電解を実施した。
導電性基体としてシリコン板を使用した以外は実施例1と同様の手順で導電性ダイヤモンド電極を作製した。
導電性基体としてグラファイト板を使用した以外は実施例1と同様の手順で導電性ダイヤモンド電極を作製した。
Claims (1)
- 導電性材料を基体とし、その基体の少なくとも一部を導電性ダイヤモンド膜で被覆した電解用陽極を用いて、無水フッ化水素酸、またはこれに被フッ素化物を添加した電解浴を電解してフッ素又はフッ素含有化合物を電解合成する方法において、
1)前記基体がグラッシーカーボンよりなり、
2)該基体の気体透過度が10 -7 cm 2 /sec以下であることを特徴とする電解用陽極を使用するフッ素又はフッ素含有化合物を電解合成する方法。
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JP5520280B2 true JP5520280B2 (ja) | 2014-06-11 |
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CN109715858B (zh) * | 2016-11-22 | 2021-09-24 | 住友电气工业株式会社 | 碳材料及制造碳材料的方法 |
CN114196985B (zh) * | 2022-01-19 | 2023-11-10 | 辽宁大学 | 一种BiVO4/NiF2光阳极在光催化水裂解方面的应用 |
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JP4535822B2 (ja) * | 2004-09-28 | 2010-09-01 | ペルメレック電極株式会社 | 導電性ダイヤモンド電極及びその製造方法 |
JP3893397B2 (ja) * | 2005-03-14 | 2007-03-14 | ペルメレック電極株式会社 | 電解用陽極および該電解用陽極を使用するフッ素含有物質の電解合成方法 |
WO2007083740A1 (ja) * | 2006-01-20 | 2007-07-26 | Toyo Tanso Co., Ltd. | フッ素又は三フッ化窒素を製造するための電解装置 |
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