CN113755888B - 一种新型Co@CoP2/CF全解水电催化剂 - Google Patents
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Abstract
本发明公开了一种新型Co@CoP2/CF高效电催化剂,属于半导体电催化技术领域。先将洁净的泡沫铜(CF)片及浓度分别为0.1mol L‑1的Co(NO3)2·6H2O、0.5mol L‑1的NH4F、0.5mol L‑1的CH4N2O和0.01~0.025mol·L‑1的植酸的水溶液置于反应釜中,在120℃下水热反应8h,制得原位生长在泡沫铜(CF)上的中间产物;再将所得中间产物在Ar/H2气氛下280℃煅烧2h,得到花状微球形貌的具有肖特基异质结构的Co@CoP2/CF高效电催化剂。该电催化剂在1mol·L‑1KOH溶液中达到10mA cm‑2的电流密度时的催化HER和OER过电位分别仅为55~70mV和210~244mV,且Co@CoP2/CF||Co@CoP2/CF的全解水系统仅需1.54~1.56V的电压即可达到10mAcm‑2的电流密度。
Description
技术领域
本发明属于半导体电催化技术领域,具体涉及一种新型Co@CoP2/CF全解水电催化剂。
背景技术
人口激增和经济快速发展导致全球能源危机和环境污染,因此开发清洁的可再生能源具有重要意义。与风能、太阳能等典型的可再生、间歇性能源相比,电催化全解水技术是最有前景的可持续能源生产技术之一。然而,阴极析氢反应(HER)和阳极析氧反应(OER)的高过电位以及迟缓动力学限制了电催化全解水技术的的进一步发展,这使新型高效电催化剂的开发受到人们的广泛关注。
作为基准电催化剂,贵金属Pt和贵金属氧化物RuO2分别表现出优异的HER和OER活性。然而,高成本和储量稀缺性极大地限制了其实际应用。因此,开发可替代贵金属的价格低廉、储量丰富、活性优越的非贵金属电催化剂成为当前的研究热点。在非贵金属基电催化材料中,过渡金属化合物因其成本低、储量丰富、毒性低、氧化还原化学丰富而备受瞩目,尤其钴基磷化物,如Co2P,CoP,CoP2和MCoP(M=Cu,Ni,Fe)等,由于在碱性溶液中具有高的耐腐蚀性和丰富的可变价态,表现出良好的HER活性。但是,这些磷化物的OER活性不佳,很少有钴基磷化物电催化剂能够在同一体系中同时高效催化HER和OER。
增加磷含量、进行元素掺杂、表面修饰和复合等是目前普遍采用的提高磷化钴基电催化活性的手段。其中,Co和P在Co-P基电催化剂中分别作为氢化物受体和质子受体中心,同时P可以促进Co-氢化物的形成,进而通过电化学脱附析氢加速电催化反应的进行。而目前关于上述因素协同效应共同促进电催化剂HER和OER性能的报道较少。因此,如何同时利用高磷含量及肖特基效应的协同作用来构建具有高效HER和OER双功能的电催化剂仍是一个巨大的挑战。基于此,本发明采用水热-煅烧法制备出一种新型肖特基Co@CoP2/CF全解水电催化剂,该电催化剂能高效地催化析氢和析氧,具有广阔的实际应用前景。
发明内容
本发明的目的在于提供一种新型高效的全解水电催化剂。本发明所制备的Co@CoP2/CF 电催化剂具有优异的HER、OER和全解水性能,且原料储量丰富易得,环境友好,制备方法简单,易于操作,便于大量制备,应用前景广阔。具体发明内容为:
1.在采用水热-煅烧法制备的Co@CoP2/CF全解水电催化剂中,由纳米片插接而成的微米花球状Co@CoP2原位生长在泡沫铜上(CF),且金属Co与半导体CoP2形成肖特基异质结,其具有优异的HER、OER和全解水性能,在1mol·L-1的KOH溶液中10mAcm-2的电流密度时的催化HER和OER过电位分别仅为55~70mV和210~244mV,且 Co@CoP2/CF||Co@CoP2/CF的全解水系统仅需1.54~1.56V的电压即可达到10mAcm-2的电流密度。
2.新型Co@CoP2/CF全解水电催化剂具体是通过以下步骤制备的:
(1)将面积为1×1cm2泡沫铜(CF)片置于3mol·L-1的HCl溶液中超声20min,再依次用去离子水和无水乙醇超声清洗并干燥,备用;
(2)将Co(NO3)2·6H2O、NH4F、CH4N2O和植酸溶于去离子水中,制得Co(NO3)2·6H2O、NH4F、CH4N2O和植酸的浓度分别为0.1mol L-1、0.5mol L-1、0.5mol L-1和0.01~0.025mol·L-1的水溶液;
(3)将经过步骤(1)预处理后的CF及步骤(2)制得的溶液20mL转移至反应釜中, 于120℃下水热反应8h,自然冷却至室温后离心分离并依次用去离子水和无水乙醇洗涤、真空干燥所得沉淀;
(4)用瓷舟盛放步骤(3)所得沉淀物并将其置于管式炉中,在Ar/H2气氛下,以5℃·min-1的升温速率升温至280℃,保温2h,自然冷却至室温,即得目标催化剂。
附图说明
图1为实施例1中所制备的Co@CoP2/CF电催化剂的扫描电镜照片;
图2为实施例1中所制备的Co@CoP2/CF电催化剂的透射电镜以及高分辨透射电镜照片;
图3为实施例1中所制备的Co@CoP2/CF电催化剂在1M KOH溶液中电催化析氢(a)、析氧(b)和全解水(c)性能图;
图4为实施例2中所制备的Co@CoP2/CF电催化剂在1M KOH溶液中电催化析氢(a)、析氧(b)和全解水(c)性能图;
图5为实施例3中所制备的Co@CoP2/CF电催化剂在1M KOH溶液中电催化析氢(a)、析氧(b)全解水(c)性能图;
具体实施方式
以下,结合附图及具体实施例对本发明作进详细说明,但附图及具体实施例仅作为示例,不以任何方式限制本发明的范围。
实施例1
(1)将面积为1×1cm2泡沫铜(CF)片置于3mol·L-1的HCl溶液中超声20min,再依次用去离子水和无水乙醇超声清洗并干燥;
(2)取2mmol Co(NO3)2·6H2O、10mmol NH4F、10mmol CH4N2O及0.33mmol植酸,用去离子水溶解,制得20mL混合溶液;
(3)将经过步骤(1)预处理后的CF及步骤(2)制得的混合溶液转移至反应釜中,于120℃下水热反应8h,待其自然冷却至室温后离心分离并依次用去离子水和无水乙醇洗涤、真空干燥所得沉淀;
(4)用瓷舟盛放步骤(3)所得沉淀物,并将其置于管式炉中,在Ar/H2气氛下,以 5℃·min-1的升温速率升温至280℃,保温2h,自然冷却至室温,即得目标催化剂。其扫描电镜照片见附图1。从附图1可以看出,Co@CoP2呈现微米花球形貌,花球直径为0.8-1μm。其透射电镜及高分辨透射电镜照片见附图2。从透射电镜照片附图2(a)可以清楚地看到 Co@CoP2的花状微球形貌,且金属Co为直径5nm的颗粒,其生长在CoP2纳米片上;高分辨透射电镜照片附图2(b)证实具有肖特基异质结构的Co@CoP2/CF电催化剂被成功制备。
(5)分别以Hg/HgO、铂丝和所制备的Co@CoP2/CF电极为参比电极、对电极和工作电极,在1mol·L-1的KOH电解质中测定所制备试样的HER、OER和全解水性能,结果见附图 3(a~c)。附图3(a)和(b)显示,在1mol·L-1KOH溶液中10mAcm-2的电流密度时Co@CoP2/CF 催化HER和OER过电位分别为55mV和210mV。附图(c)显示,Co@CoP2/CF||Co@CoP2/CF 的全解水系统仅需1.54V的电压下电流密度即可达到10mAcm-2。
实施例2
(1)按照实施例1中步骤(1)方法预处理CF;
(2)取2mmol Co(NO3)2·6H2O,10mmol NH4F,10mmol CH4N2O,及0.5mmol植酸,用去离子水溶解,制得20mL混合溶液;
(3)按照实施例1步骤(3)操作;
(4)按照实施例1步骤(4)操作,制得目标催化剂;
(5)分别以Hg/HgO、铂丝和所制备的Co@CoP2/CF电极为参比电极、对电极和工作电极,在1mol·L-1的KOH电解质中测试所制备试样的HER、OER和全解水性能,结果见附图 4(a~c)。附图4(a)和(b)显示,在1mol L-1KOH溶液中10mAcm-2的电流密度时Co@CoP2/CF 催化HER和OER过电位分别为65mV和226mV。附图(c)显示,Co@CoP2/CF||Co@CoP2/CF 的全解水系统仅需1.55V的电压下电流密度即可达到10mAcm-2。
实施例3
(1)按照实施例1中步骤(1)方法预处理CF;
(2)取2mmol Co(NO3)2·6H2O,10mmol NH4F,10mmol CH4N2O,及0.2mmol植酸,用去离子水溶解,制得20mL混合溶液;
(3)按照实施例1步骤(3)操作;
(4)按照实施例1步骤(4)操作,制得目标催化剂;
(5)分别以Hg/HgO、铂丝和所制备的Co@CoP2/CF电极为参比电极、对电极和工作电极,在1mol·L-1的KOH电解质中测试所制备试样的HER、OER和全解水性能,结果见附图 5(a~c)。附图5(a)和(b)显示,在1mol·L-1KOH溶液中10mAcm-2的电流密度时Co@CoP2/CF 催化HER和OER过电位分别为70mV和244mV。附图(c)显示,Co@CoP2/CF||Co@CoP2/CF 的全解水系统仅需1.56V的电压下电流密度即可达到10mAcm-2。
上述实验结果证实通过水热-煅烧法成功制备出新型Co@CoP2/CF电催化剂,且该电催化剂表现出优异的电催化HER、OER和全解水性能。
Claims (3)
1.一种Co@CoP2/CF全解水电催化剂,其特征在于,由纳米片插接而成的微米花球状Co@CoP2原位生长在CF上,其中CF表示泡沫铜,且金属Co与半导体CoP2形成肖特基异质结,其通过以下步骤制备:
(1)将面积为1×1cm2CF片置于3mol·L-1的HCl溶液中超声20min,再依次用去离子水和无水乙醇超声清洗并干燥,备用;
(2)将Co(NO3)2·6H2O、NH4F、CH4N2O和植酸溶于去离子水中,制得含植酸的Co(NO3)2·6H2O、NH4F、CH4N2O的浓度分别为0.1mol·L-1、0.5mol·L-1、0.5mol·L-1的水溶液;
(3)将经过步骤(1)预处理后的CF及步骤(2)制得的溶液20mL转移至反应釜中,于120℃下水热反应8h,自然冷却至室温后离心分离并依次用去离子水和无水乙醇洗涤、真空干燥所得沉淀;
(4)用瓷舟盛放步骤(3)所得沉淀物并将其置于管式炉中,在Ar/H2气氛下,以5℃·min-1的升温速率升温至280℃,保温2h,自然冷却至室温,即得目标催化剂。
2.如权利要求1中所述的一种Co@CoP2/CF全解水电催化剂,其特征在于,步骤(2)中植酸的浓度为0.01~0.025mol·L-1。
3.如权利要求1所述的一种Co@CoP2/CF全解水电催化剂,其特征在于,该催化剂具有优异电催化HER、OER和全解水性能,在1mol·L-1的KOH溶液中,10mAcm-2的电流密度时的电催化HER和OER的过电位分别仅为55~70mV和210~244mV,且Co@CoP2/CF||Co@CoP2/CF的全解水系统仅需1.54~1.56V的电压即可达到10mAcm-2的电流密度。
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