CN110678581A - 镍电极,制备镍电极的方法,及镍电极的用途 - Google Patents
镍电极,制备镍电极的方法,及镍电极的用途 Download PDFInfo
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- CN110678581A CN110678581A CN201880032415.3A CN201880032415A CN110678581A CN 110678581 A CN110678581 A CN 110678581A CN 201880032415 A CN201880032415 A CN 201880032415A CN 110678581 A CN110678581 A CN 110678581A
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- C25B11/073—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material
- C25B11/075—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of a single catalytic element or catalytic compound
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- C—CHEMISTRY; METALLURGY
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- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
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- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
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- C25B1/04—Hydrogen or oxygen by electrolysis of water
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- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
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- C25B1/34—Simultaneous production of alkali metal hydroxides and chlorine, oxyacids or salts of chlorine, e.g. by chlor-alkali electrolysis
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- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
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- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
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- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
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- Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)
- Battery Electrode And Active Subsutance (AREA)
- Electric Double-Layer Capacitors Or The Like (AREA)
Abstract
本发明涉及一种镍电极,包含具有镍丝或格子状的、包含网的镍扩张网的导电的镍网,以及具有互相黏附的球形的纳米多孔镍颗粒的镍层;的纳米多孔镍颗粒仅施加至镍网的丝或仅施加于镍扩张网的网,镍电极可通过包含以下步骤的方法获得:a)提供球形氢氧化镍颗粒;b)在还原气氛中,于270℃至330℃的温度下部分还原的球形氢氧化镍颗粒,以获得部分还原的球形Ni/NiO颗粒;c)由所获得的Ni/NiO颗粒、有机和/或无机粘合剂、表面活性剂,和可选的另外的佐剂制备糊剂;d)将糊剂以涂层的形式涂覆到导电的镍网或镍扩张网上;以及e)在还原气氛中,于500℃至800℃的温度下回火被涂覆的镍网或镍扩张网。本发明还涉及一种制造根据本发明的镍电极的方法及其用途,特别是其用作水电解的电极的用途。根据本发明的镍电极的特征在于高的机械稳定性和有利的电化学性能,特别是在水电解中增加的气体逸出。
Description
技术领域
本发明涉及具有球形的纳米多孔(nanoporous)的镍颗粒的高表面积镍层的镍电极,其制备方法及其用途,尤其是其作为水电解的电极的用途。
背景技术
一般而言,除非在高温下施加接触压力,否则难以生产能够牢固粘附于镍片上的镍颗粒层;所形成的镍颗粒层通常很容易从载体处再次分离。由于需要高温下的高接触压力,因此烧结工艺复杂而昂贵。自1928年以来,烧结镍电极一直尤其地被用于镍镉可充电电池(nickel-cadmium rechargeable batteries)中,其要求的烧结温度范围为800-1000℃(AK Shukla,B Hariprakash,SECONDARY BATTERIES–NICKEL SYSTEMS,Electrodes:Nickel.,第407页,Elsevier,2009)。
US4,605,484描述了一种用于产生氢气的电极,其包括导电基底,该导电基底上具有由铬组分和选自镍和钴中的至少一种金属的氧化物所组成的涂层。使用一种复杂的等离子喷涂工艺,通过熔融喷涂(melt spraying)生产该涂层。
EP0226291A1描述了延长用于产生氢气的电极的使用寿命的方法,该电极包括导电基底和金属氧化物涂层;在氢气生成过程中,将金属组分(例如钛或铌)添加到碱性电解质中。该电极表面的金属氧化物涂层可通过例如等离子喷涂或火焰喷涂(flame spraying)制备。
DE2002298描述了一种用于通过在金属基底上施加多孔镍层来制备用于电解工业用水的电极的方法;该多孔镍层在碱金属碳酸盐或碱金属碳酸氢盐的水溶液中被阳极氧化,由此形成的氧化产物随后被还原为精细分布的金属镍。通过将金属镍火焰喷涂或电弧喷涂(arc spraying)到粗糙化的金属基底上制成该多孔镍层。
可商业购得各种各样的镍电极。例如,已知具有棒状镍颗粒的镍烧结电极(参见Morioka Y.,Narukawa S.,Itou T.,Journal of Power Sources 100(2001):107-116中的图1)、具有蜂窝状结构的镍泡沫电极(见图2)或具有圆柱体镍纤维的镍纤维电极(参见OhmsD.,Kohlhase M.,Benczur-Urmossy G.,Schadlich G.,Journal of Power Sources 105(2002):127-133中的图3)。
上文提及的、可商业购得的镍电极被用作电池的电极,并被优化以接收活性物质。
US4,300,993描述了一种用于具有多孔表面的、用于碱性电解的镍电极的制造方法,其中将镍粉或含镍合金的粉和粘合剂的悬浮液施加到钢板载体上并干燥,随后在高温下烧结涂层,并在该烧结层上电解沉积镍/锌合金,然后通过浸入苛性溶液,从镍/锌合金中提取锌,从而在电沉积材料中产生孔隙。镍或铁的丝网(wire mesh)可以用作金属基底。
用于制造电极的金属网的常规金属涂覆工艺通常导致网孔(mesh openings)的不期望的填充或密封,尤其是在较小的丝间距(wire spacing)的情况下;这严重阻碍了气体的传输。另一方面,期望在镍电极中获得尽可能大的表面积以及良好的气体传输,以便在用于水解器(hydrolyzers)中时提高生产率。
发明内容
发明目的
本发明的目的是提供一种镍电极,该镍电极在导电的镍基底上具有牢固粘附的镍层,具有良好的机械稳定性,并具有最大可能的表面积,同时避免了现有技术的缺点。此外,该镍电极将具有有利的电化学性能,以能够增加氧气和氢气的释放以及提供良好的气体传输,特别是在水电解过程中。
此外,将提供一种用于制备上述镍电极的简单且成本有效的方法。
发明内容
上文列举的目的通过根据本发明权利要求1所述的镍电极、根据权利要求10所述的制备所述镍电极的方法,以及根据权利要求1所述的镍电极的用途实现。
在从属权利要求中描述了本申请的主题的优选或特别实用的实施例。
因此,本发明涉及一种镍电极,包含具有镍丝或格子状的镍扩张网(nickelexpanded metal)的导电的镍网,以及具有互相黏附的球形的纳米多孔镍颗粒的镍层;所述镍扩张网包含网;所述的纳米多孔镍颗粒仅施加至所述镍网的丝或仅施加于所述镍扩张网的所述网,所述的镍电极可通过包含以下步骤的方法获得:
a)提供球形氢氧化镍颗粒;
b)在还原气氛中,于270℃至330℃的温度下部分还原所述的球形氢氧化镍颗粒,以获得部分还原的球形Ni/NiO颗粒;
c)由所获得的Ni/NiO颗粒、有机和/或无机粘合剂、表面活性剂,和可选的另外的佐剂(adjuvants)制备糊剂;
d)将所述的糊剂以涂层的形式涂覆到所述导电的镍网或所述镍扩张网上;以及
e)在还原气氛中,于500℃至800℃的温度下回火被涂覆的所述镍网或所述镍扩张网。
本发明还涉及一种制备这种镍电极的方法,包括以下步骤:
a)提供球形氢氧化镍颗粒;
b)在还原气氛中,于270℃至330℃的温度下部分还原所述的球形氢氧化镍颗粒,以获得部分还原的球形Ni/NiO颗粒;
c)由所获得的Ni/NiO颗粒、有机和/或无机粘合剂、表面活性剂,和可选的另外的佐剂制备糊剂;
d)将所述的糊剂以涂层的形式涂覆到所述导电的镍网或所述镍扩张网上;以及
e)在还原气氛中,于500℃至800℃的温度下回火被涂覆的所述镍网或镍扩张网。
最后,本发明还涉及所述的镍电极的用途,尤其是其在水电解中或在碱性介质中的其它电化学反应中作为电极的用途。
发明具体描述
根据本发明所述的镍电极的特点在于一种镍层,该镍层由互相黏附的球形的纳米多孔镍颗粒所组成,其内表面积比迄今为止可商业购得的、用于电池的镍电极(例如泡沫、烧结,或纤维电极)的内表面积更大。
这些表面纳米结构的镍网或镍扩张网可用于碱性介质中的水电解。由于表面积大,因此与常规水解器相比可以实现更高的生产率。然而,该效果还可以用于减小安装空间,并同时通过水电解获得恒定的生产率。
本文使用的术语“纳米多孔(nanoporous)”或“纳米结构的(nanostructured)”是指孔开口的最大直径为约500nm(例如直径为100nm至500nm)的多孔结构。
在工业实践中,基于具有球形的纳米多孔镍颗粒的镍层的镍网或镍扩张网的镍电极是迄今未知的。我们惊讶地发现,根据本发明的镍电极可特别有利地用于在碱性介质中的水电解,并且在氧气生成和尤其是氢气生成的过程中能够显著产生更多的气体。显而易见地,能够产生更多气体的这一令人惊讶的效果可归因于镍层的内表面积大。由于较大的内表面积,电极与周围介质的接触电阻非常低;从而使水解过程中可以达到的电流密度增加(例如与未涂覆的镍表面相比)。
采用根据本发明所述的方法,可以通过简单的工艺步骤在镍丝上或在镍扩张网的网上获得牢固黏附的镍颗粒层;所述的简单的工艺步骤为例如:在室温下的无压涂覆(pressureless coating),随后对所涂覆的镍片进行回火。以这种方式生产的镍电极具有很高的机械稳定性;即使在镍基底的机械变形期间和之后,球形镍颗粒层仍保持黏附。在剥离测试(peel test)中,可以检测到高达350N的保持力(holding forces),而该保持力可通过改变工艺参数得到进一步的提高。
此外,所使用的粘合剂和表面活性剂可以被蒸发而不留下任何残留物。因此,其不会在镍层表面留下麻烦的碳沉积物。
根据本发明所使用的、包含网的格子状的镍扩张网包含扩张镍网(expandednickel metal);其也可以被称为镍扩张网(nickel expanded metal mesh)。它们通常是通过在金属拉伸变形的同时进行不损失材料的交错切割制造的。由片(sheets)或条(strips)构成的格子状的材料的网并非编织的或焊接的。典型的网格形状是菱形网格、长节点(long-bond)网格、六边形网格、圆形网格,和方形网格。
根据本发明所使用的镍网同样可以具有不同的网形状。在由丝(wire)制成的镍网中,也可以在涂覆之前将镍网滚制(roll)。
所使用的3D镍结构(网或扩张网)的网眼尺寸优选在100μm至3000μm的范围内,更优选在100μm至1000μm的范围内。
本发明所使用的球形氢氧化镍颗粒可作为电池材料在市面上购得(例如购自比利时的Umicore公司和日本的Tanaka公司),并且其平均粒径优选为0.3μm-75μm,更优选为3μm-30μm,特别优选为9μm-12μm。最优选的是平均粒径为约10μm的颗粒。
本发明所述的方法中的步骤b)的部分还原优选地在270℃-330℃,更优选地在290-310℃的温度下进行。
所述的部分还原方便地在上述条件下进行3至5小时。
根据本发明的方法所述的步骤b)中的部分还原和步骤e)中的回火均在还原性气氛中进行,所述还原性气氛包含例如10%-100%,优选为10%-50%的氢气;当还原气氛不由100%的氢气组成时,所述的还原性气氛还包括可选的惰性气体,如氮气。
用于与通过部分还原而获得的Ni/NiO颗粒共同制造糊剂或悬浮液的合适的有机粘合剂尤其包括天然和/或合成聚合物或其衍生物。合适的例子为醇酸树脂、纤维素及其衍生物、环氧树脂、聚丙烯酸酯,如聚甲基丙烯酸甲酯(PMMA)和聚丙烯酸(PAA)、聚三氟氯乙烯(PCTFE)、聚六氟丙烯(PHFP)、聚酰亚胺(PI)及其衍生物、聚氨酯(PU)及其衍生物、聚四氟乙烯(PTFE)、聚三氟乙烯(PTrFE)、聚乙烯醇(PVA)、聚偏二氟乙烯(PVDF)、硅酮、淀粉及其衍生物、苯乙烯-丁二烯橡胶(SBR)以及前述这些材料的混合物。特别优选的有机粘合剂为聚乙烯醇。
基于糊剂或悬浮液的总重量,在步骤c)中用于制备糊剂或悬浮液的表面活性剂的量优选为0.1重量%至20重量%,更优选为2重量%至10重量%。表面活性剂合适地选自由非离子表面活性剂、离子表面活性剂,和两性表面活性剂组成的组。
尤其是以下类别的物质的表面活性剂可用作制备糊剂或悬浮液的表面活性剂:
-阴离子表面活性剂,例如烷基羧酸盐、烷基苯磺酸盐、仲烷基磺酸盐、脂肪醇硫酸盐、烷基醚硫酸盐、牛磺酸盐、烯烃/烷烃(paraffin)磺酸盐、磺基琥珀酸盐以及亚磷酸或膦酸酯及其盐;
-阳离子表面活性剂,例如来自烷基三甲基铵、二烷基二甲基铵、烷基苄基,和乙氧基化烷基铵氯化物和溴化物类物质的季铵化合物;
-非离子表面活性剂,例如醇乙氧基化物、油基鲸蜡醇乙氧基化物(oleyl cetylalcohol ethoxylates)、壬/十一醇(C9/C11)乙氧基化物、异癸醇(C10)乙氧基化物、月桂基-十四烷基(C12-C14)乙氧基化物、异十三烷基(C13)乙氧基化物、蓖麻油乙氧基化物,和其他醇类乙氧基化物;
-两性表面活性剂,例如来自以下类别物质的甜菜碱(betaines)和磺基甜菜碱(sultaines):羧基甘氨酸盐、亚氨基丙酸酯、亚氨基甘氨酸盐、脂肪酸酰胺基丙基甜菜碱,和脂肪酸酰胺丙基羟基磺基甜菜碱(fatty acid amidopropylhydroxysultaines);
-非离子两性表面活性剂,例如脂肪醇乙氧基化物EO/PO加合物、烷基葡糖苷、聚山梨酸酯、脂肪酸二乙醇酰胺,和氧化胺。
已发现特别合适的是例如具有亲水性聚环氧乙烷链和芳族烃基的非离子表面活性剂,其可以是亲脂性或疏水性的,例如聚乙二醇叔辛基苯基醚。
出乎意料的是,向糊剂或悬浮液中添加表面活性剂防止了镍网或镍扩张网的开口的关闭:在随后将糊剂作为涂层涂覆到导电的镍网或镍扩张网上的过程中,糊剂或浆料沿镍网的金属丝或沿镍扩张网的网明显收缩。
可根据需要添加其他常用的佐剂以制备糊剂,所述的佐剂为,例如,有机或无机溶剂或分散剂。
水性介质中的铵盐或肼盐特别适合用作无机粘合剂。
被涂覆的镍网或镍扩张网的最终回火优选在500℃-800℃,更优选在600℃-700℃的温度下进行。最终回火通常需要3到5个小时。最终回火的目的在于完全还原Ni/NiO颗粒,以获得具有互相牢固黏附的球形的纳米多孔镍颗粒组成的镍层。此外,应确保所使用的粘合剂、表面活性剂,和(如果适用的)佐剂被完全除去和/或蒸发,没有残留物。
根据本发明所述的镍电极的镍层的厚度优选为1μm-1000μm,更优选为10μm-900μm,并且特别优选为20μm-200μm。
球形的纳米多孔镍颗粒的平均粒径优选为0.1μm-25μm,更优选为1μm-10μm,进一步优选为2μm-6μm,特别优选为3μm-4μm。
根据本发明,可以掺杂具有多孔镍颗粒的镍层。在回火之前、之中或之后,可使用外来离子掺杂这些颗粒。
根据本发明所述的的镍电极特别适合用作标准电池、可再充电电池、对称和非对称双层电容器、传感器的工作电极;也适合用作催化剂载体以及电化学合成过程中或光电和光催化装置中的电极,尤其适合用作碱性介质中的水电解的电极。
还特别包括在电解中的应用,如在氯碱电解(chlorine-alkali electrolysis)、催化、光伏涂层和光伏氢生成(photovoltaic hydrogen generation)中的应用。
由于表面纳米结构,根据本发明使用的镍网或镍扩张网具有增加的表面积,因此有利于在镍网/电解质或镍扩张网/电解质界面处进行更简单的电荷和质量传递。通过将纳米结构的镍颗粒仅施加到镍网的丝上或仅施加到镍扩张网的网上,就可以实现网或扩张网的纳米结构。至关重要的是仅仅丝或网被一层镍颗粒所覆盖,以保持网孔或扩张网的开口敞开。
附图说明
图1示出了商购烧结镍电极表面放大1000倍的SEM(scanning electronmicroscope,扫描电子显微镜)图像(来自Morioka Y.,Narukawa S.,Itou T.,Journal ofPower Sources100(2001):107–116);
图2示出了具有蜂窝结构的商购镍泡沫电极表面放大150倍的SEM图像;
图3示出了商购镍纤维电极表面放大500倍的SEM图像(来自Ohms D.,KohlhaseM.,Benczur-Urmossy G.,Schadlich G.,Journal of Power Sources 105(2002):127–133);
图4示出了如下文的制造例中所描述的、根据本发明所述的镍电极的表面的光学显微总图(light microscopic overview image),该镍电极的形式为镍网(丝间距1.2mm,丝厚度150μm),在15倍放大下具有约60μm厚的纳米结构的镍颗粒(粒径3μm至4μm)的均匀涂层;
图5示出了图4所示的本发明的镍电极的表面的放大55倍的显微照片。
图6示出了下文的比较例中描述的镍电极的表面的放大40倍的光学显微总图。
具体实施方式
制备根据本发明所述的镍电极
将50g的球形β-Ni(OH)2颗粒在温度为300℃、含50体积%氢气的氮气气氛的退火炉中还原4小时,保持约10μm的平均粒径。这些部分还原的、球形的Ni/NiO颗粒已经具有内部纳米多孔结构。
用10g的所述部分还原的球形Ni/NiO颗粒与6mL的、7.5重量%的聚乙烯醇和10%Triton X-100(非离子表面活性剂)的水溶液共同制备糊剂。通过浸涂(dipping)将该糊剂施加到镍网上。所使用的方形镍网的丝径(wire diameter)为150μm,网径(mesh size)为1200μm。由于它们减小的表面张力,因此糊剂在镍丝的表面上收缩并释放出镍网的网眼。
在退火炉中的最终回火阶段在620℃的温度下和含50体积%氢气的氮气的还原气氛中进行;在该回火阶段结束后,可直接使用所形成的电极。涂覆到镍网上的球形镍颗粒的平均直径为3.4μm,并具有内部纳米多孔结构。
下文的表1总结了所使用的氢氧化镍颗粒、部分还原的Ni/NiO颗粒和镍层的球形多孔镍颗粒的平均粒径。
表1
样品 | 平均粒径(μm) |
β-Ni(OH)<sub>2</sub> | 10.1 |
部分还原的Ni/NiO | 10.3 |
涂覆在镍网上的镍颗粒 | 3.4 |
图4示出了以这种方式生产的镍电极的表面的光学显微图,图5示出了该镍电极的表面的细节的光学显微图。从这些显微图中可见,镍网的网孔保持打开,并且由纳米多孔镍颗粒组成的涂层仅位于镍网的丝上。
比较的镍电极的制备
使用类似于上述根据本发明所述的制备例来制备镍电极,唯一的例外是在制备糊剂期间不添加表面活性剂。
以这种方式制备的电极的光学显微总图如图6所示。由该图可见,镍网的网孔或多或少地被镍颗粒的涂层完全封闭了,其伴随着对气体传输的明显阻碍。
Claims (11)
1.一种镍电极,包含具有镍丝或格子状的镍扩张网的导电的镍网,以及具有互相黏附的球形的纳米多孔镍颗粒的镍层;所述镍扩张网包含网;所述的纳米多孔镍颗粒仅施加至所述镍网的丝或仅施加于所述镍扩张网的所述网,所述的镍电极可通过包含以下步骤的方法获得:
a)提供球形氢氧化镍颗粒;
b)在还原气氛中,于270℃至330℃的温度下部分还原所述的球形氢氧化镍颗粒,以获得部分还原的球形Ni/NiO颗粒;
c)由所获得的Ni/NiO颗粒、有机和/或无机粘合剂、表面活性剂,和可选的另外的佐剂制备糊剂;
d)将所述的糊剂以涂层的形式涂覆到所述导电的镍网或镍扩张网上;以及
e)在还原气氛中,于500℃至800℃的温度下回火被涂覆的所述镍网或所述镍扩张网。
2.根据权利要求1所述的镍电极,其中步骤a)中所提供的所述球形氢氧化镍颗粒的平均粒径为0.3μm至75μm,优选为3μm至30μm,更优选为9μm至12μm,特别优选为约10μm。
3.根据权利要求1和/或2所述的镍电极,其中步骤b)中所述的部分还原在290℃至310℃的温度下进行。
4.根据前述权利要求中至少一项所述的镍电极,其中步骤b)中所述的部分还原和步骤e)中所述的回火均在还原性气氛中进行,所述还原性气氛包含10%-100%的氢气和可选的惰性气体。
5.根据前述权利要求中至少一项所述的镍电极,其中在步骤c)中,天然和/或合成聚合物或其衍生物被用作有机粘合剂;且铵盐或肼盐被用作无机粘合剂。
6.根据前述权利要求中至少一项所述的镍电极,其中在步骤c)中,所述表面活性剂的量为相对于所述糊剂的总重量的0.1重量%至20重量%。
7.根据前述权利要求中至少一项所述的镍电极,其中在步骤c)中,用于制备所述糊剂的所述表面活性剂选自由非离子表面活性剂、离子表面活性剂,和两性表面活性剂组成的组。
8.根据前述权利要求中至少一项所述的镍电极,其中所述镍电极的所述镍层的厚度为1-1000μm,优选为10-900μm,更优选为20-200μm。
9.根据前述权利要求中至少一项所述的镍电极,其中所述球形的纳米多孔镍颗粒的平均粒径为0.1μm至25μm,优选为1μm至10μm,更优选为2μm至6μm,特别优选为3μm至4μm。
10.一种制备根据权利要求1-9中的至少一项所述的镍电极的方法,包括以下步骤:
a)提供球形氢氧化镍颗粒;
b)在还原气氛中,于270℃至330℃的温度下部分还原所述的球形氢氧化镍颗粒,以获得部分还原的球形Ni/NiO颗粒;
c)由所获得的Ni/NiO颗粒、有机和/或无机粘合剂、表面活性剂,和可选的另外的佐剂制备糊剂;
d)将所述的糊剂以涂层的形式涂覆到所述导电的镍网或镍扩张网上;以及
e)在还原气氛中,于500℃至800℃的温度下回火被涂覆的所述镍网或镍扩张网。
11.根据权利要求1至9中至少一项所述的镍电极在标准电池、可再充电电池、对称和非对称双层电容器、传感器中作为工作电极的用途;所述的镍电极作为催化剂载体的用途;所述的镍电极在电化学合成过程中或光电和光催化装置作为电极的用途,尤其是在碱性介质中的水电解中作为电极的用途。
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