JP2018538432A - ニッケル電極、自立ニッケル層、それを製造する方法およびその使用 - Google Patents
ニッケル電極、自立ニッケル層、それを製造する方法およびその使用 Download PDFInfo
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 341
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 158
- 238000004519 manufacturing process Methods 0.000 title claims description 19
- 239000002245 particle Substances 0.000 claims abstract description 74
- BFDHFSHZJLFAMC-UHFFFAOYSA-L nickel(ii) hydroxide Chemical compound [OH-].[OH-].[Ni+2] BFDHFSHZJLFAMC-UHFFFAOYSA-L 0.000 claims abstract description 21
- 238000005496 tempering Methods 0.000 claims abstract description 18
- 239000011230 binding agent Substances 0.000 claims abstract description 16
- 238000000034 method Methods 0.000 claims abstract description 16
- 239000000546 pharmaceutical excipient Substances 0.000 claims abstract description 9
- 238000005868 electrolysis reaction Methods 0.000 claims description 15
- 239000001257 hydrogen Substances 0.000 claims description 14
- 229910052739 hydrogen Inorganic materials 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 11
- 229910052751 metal Inorganic materials 0.000 claims description 11
- 239000002184 metal Substances 0.000 claims description 11
- 239000011888 foil Substances 0.000 claims description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 4
- 229910052799 carbon Inorganic materials 0.000 claims description 4
- 239000003054 catalyst Substances 0.000 claims description 3
- 229920000642 polymer Polymers 0.000 claims description 3
- 230000015572 biosynthetic process Effects 0.000 claims description 2
- 239000003990 capacitor Substances 0.000 claims description 2
- 239000000919 ceramic Substances 0.000 claims description 2
- 150000002429 hydrazines Chemical class 0.000 claims description 2
- 239000011261 inert gas Substances 0.000 claims description 2
- 239000006262 metallic foam Substances 0.000 claims description 2
- 229920005615 natural polymer Polymers 0.000 claims description 2
- 230000001699 photocatalysis Effects 0.000 claims description 2
- 238000003786 synthesis reaction Methods 0.000 claims description 2
- 229920001059 synthetic polymer Polymers 0.000 claims description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims 1
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 18
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 description 12
- 239000003792 electrolyte Substances 0.000 description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- 238000000576 coating method Methods 0.000 description 6
- 238000002484 cyclic voltammetry Methods 0.000 description 6
- 239000011248 coating agent Substances 0.000 description 5
- 239000003822 epoxy resin Substances 0.000 description 5
- -1 hydrogen salt Chemical class 0.000 description 5
- 229920000647 polyepoxide Polymers 0.000 description 5
- 239000004372 Polyvinyl alcohol Substances 0.000 description 4
- 239000003513 alkali Substances 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 238000010292 electrical insulation Methods 0.000 description 4
- 239000000835 fiber Substances 0.000 description 4
- 239000006260 foam Substances 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 229920002451 polyvinyl alcohol Polymers 0.000 description 4
- 239000000758 substrate Substances 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 230000007062 hydrolysis Effects 0.000 description 3
- 238000006460 hydrolysis reaction Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 2
- 239000004642 Polyimide Substances 0.000 description 2
- 238000000137 annealing Methods 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000010285 flame spraying Methods 0.000 description 2
- 150000002431 hydrogen Chemical class 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 239000002609 medium Substances 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- 238000007750 plasma spraying Methods 0.000 description 2
- 229920002493 poly(chlorotrifluoroethylene) Polymers 0.000 description 2
- 229920003229 poly(methyl methacrylate) Polymers 0.000 description 2
- 239000005023 polychlorotrifluoroethylene (PCTFE) polymer Substances 0.000 description 2
- 229920001721 polyimide Polymers 0.000 description 2
- 239000004926 polymethyl methacrylate Substances 0.000 description 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 2
- 239000004810 polytetrafluoroethylene Substances 0.000 description 2
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 238000005507 spraying Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- 229920002125 Sokalan® Polymers 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 229920000180 alkyd Polymers 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 150000003863 ammonium salts Chemical class 0.000 description 1
- 230000003321 amplification Effects 0.000 description 1
- 238000002048 anodisation reaction Methods 0.000 description 1
- 239000012736 aqueous medium Substances 0.000 description 1
- OJIJEKBXJYRIBZ-UHFFFAOYSA-N cadmium nickel Chemical compound [Ni].[Cd] OJIJEKBXJYRIBZ-UHFFFAOYSA-N 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- LNEPOXFFQSENCJ-UHFFFAOYSA-N haloperidol Chemical compound C1CC(O)(C=2C=CC(Cl)=CC=2)CCN1CCCC(=O)C1=CC=C(F)C=C1 LNEPOXFFQSENCJ-UHFFFAOYSA-N 0.000 description 1
- 229910001867 inorganic solvent Inorganic materials 0.000 description 1
- 239000003049 inorganic solvent Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910052758 niobium Inorganic materials 0.000 description 1
- 239000010955 niobium Substances 0.000 description 1
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229920000058 polyacrylate Polymers 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 229920003048 styrene butadiene rubber Polymers 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
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- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/74—Iron group metals
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Abstract
Description
a)球状の水酸化ニッケル粒子を提供するステップと、
b)高温にて還元雰囲気中で前記球状の水酸化ニッケル粒子を部分的に還元して、部分的に還元した球状のNi/NiO粒子を得るステップと、
c)得られたNi/NiO粒子ならびに有機および/または無機結合剤ならびに必要に応じてさらなる賦形剤からペーストを調製するステップと、
d)層の前記ペーストを、前記導電性ニッケルシートの片側または両側に塗布するステップと、
e)高温にて還元雰囲気中で、コーティングした前記ニッケルシートを焼き戻すステップと
を含む方法によって得られる、ニッケル電極である。
a)球状の水酸化ニッケル粒子を提供するステップと、
b)高温にて還元雰囲気中で前記球状の水酸化ニッケル粒子を部分的に還元して、部分的に還元した球状のNi/NiO粒子を得るステップと、
c)得られたNi/NiO粒子ならびに有機および/または無機結合剤ならびに必要に応じてさらなる賦形剤からペーストを調製するステップと、
d)層の前記ペーストを担体に塗布するステップと、
e)高温にて還元雰囲気中で、コーティングした前記担体を焼き戻すステップと、
f)前記担体を分離して、自立多孔質ニッケル層を得るステップと
を含む方法によって得られる、自立ニッケル層である。
a)球状の水酸化ニッケル粒子を提供するステップと、
b)高温にて還元雰囲気中で前記球状の水酸化ニッケル粒子を部分的に還元して、部分的に還元した球状のNi/NiO粒子を得るステップと、
c)得られたNi/NiO粒子ならびに有機および/または無機結合剤ならびに必要に応じてさらなる賦形剤からペーストを調製するステップと、
d)層の前記ペーストを、前記導電性ニッケルシートの片側または両側に塗布するステップと、
e)高温にて還元雰囲気中で、コーティングした前記ニッケルシートを焼き戻すステップと
を含む、方法である。
a)球状の水酸化ニッケル粒子を提供するステップと、
b)高温にて還元雰囲気中で前記球状の水酸化ニッケル粒子を部分的に還元して、部分的に還元した球状のNi/NiO粒子を得るステップと、
c)得られたNi/NiO粒子ならびに有機および/または無機結合剤ならびに必要に応じてさらなる賦形剤からペーストを調製するステップと、
d)層の前記ペーストを担体に塗布するステップと、
e)高温にて還元雰囲気中で、コーティングした前記担体を焼き戻すステップと、
f)前記担体を分離して、自立多孔質ニッケル層を得るステップと
を含む、方法である。
50gの球状β−Ni(OH)2粒子を、焼きなまし炉において窒素中の50vol%水素の雰囲気中で300℃の温度にて4時間部分的に還元し、約10μmの平均粒径を保存した。それらは部分的に還元すると、球状Ni/NiO粒子は既に内部多孔質構造を有する。5gの部分的に還元した球状Ni/NiO粒子を、3mlの7.5wt%ポリビニルアルコール水溶液でペーストに変換し、次いでそのペーストを125μm厚のニッケルシートの片側に塗布する。
その大きな内部表面積のために、本発明による電極と周囲媒体との間の境界抵抗は非常に低く、このことは、例えば、加水分解の間に達成され得る電流密度は、コーティングされていないニッケルシートによって提供されるものより大きいことを意味する。コーティングされていないニッケルシートにおいて、Hg/HgO参照電極に対して0.819Vの電圧で144mA/cm2の範囲の電流密度、ならびに5.5M KOH、2.5M NaOHおよび0.5M LiOHからなる電解質において50〜100μVの範囲の電圧変化が得られる。低電圧変化は準静的測定とみなされ得る。Hg/HgO参照に対する0.819Vの選択された電位は酸素発生のみに起因する。本発明による方法により製造された大きな表面積を有するニッケル電極により、218〜232mA/cm2の電流密度が同じ条件下で見出される。これは約1.5倍の電流密度の平均増加に対応する(表2を参照のこと)。対応するサイクリックボルタモグラムを図6a〜dに示す。
本発明による大きな表面積を有するニッケル電極に起因した顕著に多い気体生成増幅効果が水素発生について観察され得る。コーティングされていないニッケルシートにおいて、Hg/HgO参照電極に対して−1.231Vの電圧で5mA/cm2の範囲の電流密度ならびに5.5M KOH、2.5M NaOHおよび0.5M LiOHの電解質において50〜100μV/sの電圧変化を得た。低電圧変化は準静的測定とみなされ得る。Hg/HgO参照に対して−1.231Vの選択した電位は水素発生のみに起因する。本発明による方法により製造された大きな表面積を有するニッケル電極により、86〜91mA/cm2の電流密度が同じ条件下で見出される。これは約17倍の電流密度の平均増加に対応する(表3を参照のこと)。対応するサイクリックボルタモグラムを図6a〜dに示す。
Claims (13)
- 導電性ニッケルシートと、前記導電性ニッケルシートに堆積する、互いに接着する球状で多孔質のニッケル粒子からなるニッケル層とを含む、ニッケル電極であって、以下のステップ:
a)球状の水酸化ニッケル粒子を提供するステップと、
b)高温にて還元雰囲気中で前記球状の水酸化ニッケル粒子を部分的に還元して、部分的に還元した球状のNi/NiO粒子を得るステップと、
c)得られたNi/NiO粒子ならびに有機および/または無機結合剤ならびに必要に応じてさらなる賦形剤からペーストを調製するステップと、
d)層の前記ペーストを、前記導電性ニッケルシートの片側または両側に塗布するステップと、
e)高温にて還元雰囲気中で、コーティングした前記ニッケルシートを焼き戻すステップと
を含む方法によって得られる、ニッケル電極。 - 互いに接着する球状で多孔質のニッケル粒子からなる自立ニッケル層であって、以下のステップ:
a)球状の水酸化ニッケル粒子を提供するステップと、
b)高温にて還元雰囲気中で前記球状の水酸化ニッケル粒子を部分的に還元して、部分的に還元した球状のNi/NiO粒子を得るステップと、
c)得られたNi/NiO粒子ならびに有機および/または無機結合剤ならびに必要に応じてさらなる賦形剤からペーストを調製するステップと、
d)層の前記ペーストを担体に塗布するステップと、
e)高温にて還元雰囲気中で、コーティングした前記担体を焼き戻すステップと、
f)前記担体を分離して、自立多孔質ニッケル層を得るステップと
を含む方法によって得られる、自立ニッケル層。 - ステップa)において提供される球状の水酸化ニッケル粒子が、0.3〜75μm、好ましくは3〜30μm、より好ましくは9〜12μm、特に好ましくは約10μmの平均粒径を有する、請求項1または2に記載のニッケル電極または自立ニッケル層。
- ステップb)における部分的還元が、270〜330℃、好ましくは290〜310℃の温度にて実施される、請求項1〜3のいずれか一項に記載のニッケル電極または自立ニッケル層。
- ステップb)における部分的還元およびステップc)における焼き戻しが、10〜100%の水素および任意に不活性ガスを含有する還元雰囲気中で実施される、請求項1〜4のいずれか一項に記載のニッケル電極または自立ニッケル層。
- ステップc)において、有機結合剤として天然および/もしくは合成ポリマーまたはその誘導体が使用され、無機結合剤としてアンモニウム塩またはヒドラジン塩が使用される、請求項1〜5のいずれか一項に記載のニッケル電極または自立ニッケル層。
- 前記ニッケル電極または前記自立ニッケル層の前記ニッケル層が、1〜1,000μm、好ましくは10〜900μm、より好ましくは20〜200μmの範囲の厚さを有する、請求項1〜6のいずれか一項に記載のニッケル電極または自立ニッケル層。
- 前記球状で多孔質のニッケル粒子が、0.1〜25μm、好ましくは1〜10μm、より好ましくは2〜6μm、特に好ましくは3〜4μmの平均粒径を有する、請求項1〜7のいずれか一項に記載のニッケル電極または自立ニッケル層。
- ステップd)における担体として、金属フォイル、金属フォーム、金属メッシュ、エキスパンドメタル、炭素フォイル、炭素フォーム、ポリマーフォイルまたはセラミック担体が使用される、請求項2〜8のいずれか一項に記載の自立ニッケル層。
- 請求項1〜8のいずれか一項に記載のニッケル電極を製造する方法であって、以下のステップ:
a)球状の水酸化ニッケル粒子を提供するステップと、
b)高温にて還元雰囲気中で前記球状の水酸化ニッケル粒子を部分的に還元して、部分的に還元した球状のNi/NiO粒子を得るステップと、
c)得られたNi/NiO粒子ならびに有機および/または無機結合剤ならびに必要に応じてさらなる賦形剤からペーストを調製するステップと、
d)層の前記ペーストを、前記導電性ニッケルシートの片側または両側に塗布するステップと、
e)高温にて還元雰囲気中で、コーティングした前記ニッケルシートを焼き戻すステップと
を含む、方法。 - 請求項2〜9のいずれか一項に記載の自立ニッケル層を製造する方法であって、以下のステップ:
a)球状の水酸化ニッケル粒子を提供するステップと、
b)高温にて還元雰囲気中で前記球状の水酸化ニッケル粒子を部分的に還元して、部分的に還元した球状のNi/NiO粒子を得るステップと、
c)得られたNi/NiO粒子ならびに有機および/または無機結合剤ならびに必要に応じてさらなる賦形剤からペーストを調製するステップと、
d)層の前記ペーストを担体に塗布するステップと、
e)高温にて還元雰囲気中で、コーティングした前記担体を焼き戻すステップと、
f)前記担体を分離して、自立多孔質ニッケル層を得るステップと
を含む、方法。 - 特にアルカリ媒体における水電解のための、バッテリー、充電式バッテリー、対称および非対称二重層コンデンサ、センサにおける作用電極として、触媒担体として、電気化学合成におけるまたは光電デバイスおよび光触媒デバイスにおける電極としての請求項1〜8のいずれか一項に記載のニッケル電極の使用。
- 水電解のための電極としての請求項2〜9のいずれか一項に記載の自立ニッケル層の使用。
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