CN107243356A - 一种具有镍钴氮化物三维结构的电催化剂及其应用 - Google Patents
一种具有镍钴氮化物三维结构的电催化剂及其应用 Download PDFInfo
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- 239000003054 catalyst Substances 0.000 title claims abstract description 37
- -1 nickel cobalt nitride Chemical class 0.000 title claims abstract description 19
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 40
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- 229910021529 ammonia Inorganic materials 0.000 claims abstract description 12
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 claims abstract description 12
- YTBWYQYUOZHUKJ-UHFFFAOYSA-N oxocobalt;oxonickel Chemical compound [Co]=O.[Ni]=O YTBWYQYUOZHUKJ-UHFFFAOYSA-N 0.000 claims abstract description 12
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910001981 cobalt nitrate Inorganic materials 0.000 claims abstract description 11
- 239000008151 electrolyte solution Substances 0.000 claims abstract description 9
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 8
- 229910052709 silver Inorganic materials 0.000 claims abstract description 8
- 239000004332 silver Substances 0.000 claims abstract description 8
- SDLBJIZEEMKQKY-UHFFFAOYSA-M silver chlorate Chemical compound [Ag+].[O-]Cl(=O)=O SDLBJIZEEMKQKY-UHFFFAOYSA-M 0.000 claims abstract description 8
- 239000007864 aqueous solution Substances 0.000 claims abstract description 5
- QXZUUHYBWMWJHK-UHFFFAOYSA-N [Co].[Ni] Chemical compound [Co].[Ni] QXZUUHYBWMWJHK-UHFFFAOYSA-N 0.000 claims description 4
- 238000004062 sedimentation Methods 0.000 claims description 4
- 238000000034 method Methods 0.000 claims description 3
- 150000004767 nitrides Chemical class 0.000 claims description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims 2
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- 239000004575 stone Substances 0.000 claims 1
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- 238000004519 manufacturing process Methods 0.000 description 6
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- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 4
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Abstract
本发明公开了一种具有镍钴氮化物三维结构的电催化剂，由如下方法制得：以硝酸镍和硝酸钴的水溶液为电解质溶液，以石墨纤维作为工作电极，铂片电极作为对电极，银/氯化银作为参比电极，恒电压沉积在石墨纤维上，然后对沉积在石墨纤维上的镍钴氧化物在氨气气氛下灼烧氮化，得到的纳米片/纳米球多级结构的镍钴氮化物三维结构即为电催化剂。本发明的电催化剂具有较低的过电势和优异的电催化性能，在电催化分解水领域具有广泛的应用。
Description
技术领域
本发明涉及一种三维结构的电催化剂及其应用，尤其涉及一种以石墨纤维为衬底的具有镍钴氮化物三维结构的电催化剂及其应用。
背景技术
随着全球不可再生能源的消耗，化石燃料的短缺和伴随的环境问题成为了广大研究学者关注的焦点。这就促使科研工作者开展大量的工作探索和利用各种各样廉价、绿色的可再生能源转化和存储技术。在这其中，电催化分解水被广泛地认为是一种有前景的生产持续、安全、绿色的氢能。电催化分解水可被分为两个半反应：阴极的析氢反应和阳极的析氧反应。两个半反应的效率是决定电催化分解水的关键因素，然而，析氧反应因为较低的动力学参数而使其具有高的过电势极大地影响了分解水的过程。这就需要一种合适的电催化剂来降低过电势从而促进另一端的析氢反应。
目前，一些贵金属及其氧化物例如Pt基和Ir基的复合纳米材料被认为是较好的析氧反应的电催化剂。虽然如此，但是由于其地球中含量较少和价格昂贵阻碍了其广泛地应用。最近有研究学者报道了利用地球中含量较丰富的材料作为电催化剂，例如磷化钴、钙钛矿氧化物和过渡金属氧化物及过氧化物作为析氧反应电催化剂，过渡金属硫化物和钼镍合金作为析氢反应的电催化。然而其难以在一个综合统一的电解池中进行电催化分解水。鉴于此，制备一种能够在同一种电解质溶液中同时进行析氢和析氧反应的电催化剂成为了当今的挑战性课题。目前有学者提出了用MoO2，CoP，NiP等作为具有析氢和析氧反应双重催化性能的电催化剂，但经检索未见利用双金属氮化物作为具有析氢和析氧反应双重催化性能的电催化剂的报道。
发明内容
针对现有技术的不足，本发明要解决的问题是提供一种具有析氢和析氧反应双重催化性能的具有镍钴氮化物三维结构的电催化剂及其应用。
本发明的技术方案是：选取具有优良导电性能的石墨纤维作为集流体，通过电沉积的方法在石墨纤维上沉积镍钴的氧化物，然后在氨气气氛下对氧化物进行灼烧氮化，制得具有纳米片/纳米球多级结构的、形貌良好、具有较低的过电势催化性能突出的三维结构的电催化剂。
本发明所述的具有镍钴氮化物三维结构的电催化剂，其特征在于，所述电催化剂由如下方法制得：以硝酸镍和硝酸钴的水溶液为电解质溶液，以石墨纤维作为工作电极，铂片电极作为对电极，银/氯化银作为参比电极，-1V～-10V恒电压沉积在石墨纤维上，然后对沉积在石墨纤维上的镍钴氧化物在氨气气氛下灼烧氮化，得到的纳米片/纳米球多级结构的镍钴氮化物三维结构即为电催化剂；其中：所述硝酸镍的浓度为2～50mM，硝酸钴的浓度为4～100mM，石墨纤维直径为7～20微米；所述恒电压沉积时间为10～15min；所述在氨气气氛下灼烧氮化的温度为400～800℃；所述纳米片厚度为2～10nm，所述纳米球的直径为10～50nm。
上述具有镍钴氮化物三维结构的电催化剂优选由如下方法制得：以硝酸镍和硝酸钴的水溶液为电解质溶液，以石墨纤维作为工作电极，铂片电极作为对电极，银/氯化银作为参比电极，-5V恒电压沉积在石墨纤维上，然后对沉积在石墨纤维上的镍钴氧化物在氨气气氛下灼烧氮化，得到的纳米片/纳米球多级结构的镍钴氮化物三维结构即为电催化剂；其中：所述硝酸镍的浓度为24mM，硝酸钴的浓度为48mM，石墨纤维直径为10～20微米；所述恒电压沉积时间为10min；所述在氨气气氛下灼烧氮化的温度为600℃，升温速度为1℃/min，保温2h；所述纳米片厚度为2～8nm，所述纳米球的直径为10～40nm。
本发明所述具有镍钴氮化物三维结构的电催化剂在电催化分解水中的应用。
应用上述制备的电催化剂在1M KOH溶液中实施电催化分解水，产氢和产氧的过电势分别为60mV～100mV和150mV～230mV。
本发明公开的具有镍钴氮化物三维结构的电催化剂首次以石墨纤维作为集流体，原位生成双金属氧化物之后进行氮化，得到双金属氮化物，并且形成三维结构，具有较低的过电势和优异的电催化性能，在电催化分解水领域具有广泛的应用。
附图说明
图1为本发明所述石墨纤维的扫描电镜照片图。
图2为石墨纤维负载了镍钴氧化物的扫描电镜照片。
图3为本发明所述石墨纤维负载了镍钴氮化物的扫描电镜照片。
图4为本发明所述电催化剂析氢析氧的线性伏安曲线。
具体实施方式
下面结合实施例及附图，对本发明的保护内容做进一步阐述。
实施例1
本发明所述三维电催化剂的制备
①配制含有4mM硝酸钴和2mM硝酸镍的电解质溶液，以石墨纤维为工作电极，铂片电极为对电极，银/氯化银为参比电极，-1V恒压沉积10min。得到以石墨纤维为衬底的镍钴氧化物。将沉积在石墨纤维上的镍钴氧化物在60℃烘箱中烘干。
②将沉积在石墨纤维上的镍钴氧化物，在氨气气氛下800℃灼烧，升温速度为1℃/min，保温2h。得到的纳米片/纳米球多级结构的镍钴氮化物三维结构即为电催化剂；其中：所述石墨纤维直径为7～20微米；所述纳米片厚度为2～10nm，所述纳米球的直径为10～50nm。
用上述制备的电催化剂在1M KOH溶液中作为电催化分解水，产氢和产氧的过电势分别为70mV和200mV。
实施例2
①配制含有48mM硝酸钴和24mM硝酸镍的电解质溶液，以石墨纤维为工作电极，铂片电极为对电极，银/氯化银为参比电极，-5V恒压沉积10min。得到以石墨纤维为衬底的镍钴氧化物。将沉积在石墨纤维上的镍钴氧化物在60℃烘箱中烘干。
②将沉积在石墨纤维上的镍钴氧化物，在氨气气氛下600℃灼烧，升温速度为1℃/min，保温2h。得到的纳米片/纳米球多级结构的镍钴氮化物三维结构即为电催化剂；其中：所述石墨纤维直径为10～20微米；所述纳米片厚度为2～8nm，所述纳米球的直径为10～40nm。
用上述制备的电催化剂在1M KOH溶液中作为电催化分解水，产氢和产氧的过电势分别为60mV和150mV。
实施例3
①配制含有100mM硝酸钴和24mM硝酸镍的电解质溶液，以石墨纤维为工作电极，铂片电极为对电极，银/氯化银为参比电极，-10V恒压沉积10min。得到以石墨纤维为衬底的镍钴氧化物。将沉积在石墨纤维上的镍钴氧化物在60℃烘箱中烘干。
②将沉积在石墨纤维上的镍钴氧化物，在氨气气氛下600℃灼烧，升温速度为1℃/min，保温2h。其中：所述石墨纤维直径为10～20微米；所述纳米片厚度为5～10nm，所述纳米球的直径为30～50nm。
用上述制备的电催化剂在1M KOH溶液中作为电催化分解水，产氢和产氧的过电势分别为100mV和230mV。
Claims (3)
1.一种具有镍钴氮化物三维结构的电催化剂，其特征在于，所述电催化剂由如下方法制得：以硝酸镍和硝酸钴的水溶液为电解质溶液，以石墨纤维作为工作电极，铂片电极作为对电极，银/氯化银作为参比电极，-1V～-10V恒电压沉积在石墨纤维上，然后对沉积在石墨纤维上的镍钴氧化物在氨气气氛下灼烧氮化，得到的纳米片/纳米球多级结构的镍钴氮化物三维结构即为电催化剂；其中：所述硝酸镍的浓度为2～50mM，硝酸钴的浓度为4～100mM，石墨纤维直径为7～20微米；所述恒电压沉积时间为10～15min；所述在氨气气氛下灼烧氮化的温度为400～800℃；所述纳米片厚度为2～10nm，所述纳米球的直径为10～50nm。
2.如权利要求1所述具有镍钴氮化物三维结构的电催化剂，其特征在于，所述电催化剂由如下方法制得：以硝酸镍和硝酸钴的水溶液为电解质溶液，以石墨纤维作为工作电极，铂片电极作为对电极，银/氯化银作为参比电极，-5V恒电压沉积在石墨纤维上，然后对沉积在石墨纤维上的镍钴氧化物在氨气气氛下灼烧氮化，得到的纳米片/纳米球多级结构的镍钴氮化物三维结构即为电催化剂；其中：所述硝酸镍的浓度为24mM，硝酸钴的浓度为48mM，石墨纤维直径为10～20微米；所述恒电压沉积时间为10min；所述在氨气气氛下灼烧氮化的温度为600℃，升温速度为1℃/min，保温2h；所述纳米片厚度为2～8nm，所述纳米球的直径为10～40nm。
3.权利要求1所述具有镍钴氮化物三维结构的电催化剂在电催化分解水中的应用。
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