CN114196986B - 一种BiVO4/CoF2光阳极的制备方法 - Google Patents
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Abstract
本发明涉及一种BiVO4/CoF2光阳极的制备方法。包括如下步骤:首先将制备好的CoF2分散于去离子水中,超声,直至固体颗粒完全溶解,形成均匀的悬浊液,然后将制备好的BiVO4浸入到悬浊液中,静置后取出,再用去离子水冲洗,最后用N2吹干,得到BiVO4/CoF2光阳极。本发明制备的BiVO4/CoF2光阳极,能够实现光生载流子的有效分离,提高光阳极的光电催化水氧化性能。
Description
技术领域
本发明属于光阳极制备领域,具体涉及一种BiVO4/CoF2光阳极的制备方法。
背景技术
由于化石能源的不断减少和环境污染问题的日益突出,太阳能作为一种绿色可持续的清洁能源,研究人员通过研究发现,可以通过参考自然界中的光合作用设计出一系列人工光合作用模型,通过光电化学的方法将水直接分解成氢气和氧气。BiVO4由于其合适的价带位置和优异的可见光吸收性能,是一种优秀的半导体材料。析氧反应是水分解过程中一个重要的半反应,而其复杂的多步骤过程和缓慢的动力学过程需要更多的光子和电驱动水分解的能量耗散。因此,如何制备高效稳定的光阳极是反应的关键所在。通过制备BiVO4/CoF2光阳极来催化水裂解,使其光电流密度与单独BiVO4相比显著提高。
发明内容
为解决上述问题,本发明采用的技术方案为:一种BiVO4/CoF2光阳极的制备方法,包括如下步骤:
1)将CoF2分散于去离子水中,超声3min,直至固体颗粒完全溶解,形成均匀的悬浊液;
2)将BiVO4浸入到步骤1)得到的悬浊液中,静置后取出,用去离子水冲洗,再用N2吹干,得到BiVO4/CoF2光阳极。
进一步的,一种BiVO4/CoF2光阳极的制备方法,步骤1)中,所述CoF2与去离子水的质量体积比为1mg:1mL。
进一步的,一种BiVO4/CoF2光阳极的制备方法,步骤2)中,所述静置时间为12小时。
进一步的,一种BiVO4/CoF2光阳极的制备方法,步骤1)中,所述CoF2的制备方法为:将Co(NO3)2·6H2O和尿素溶解于35mL去离子水中,然后置于反应釜中,在120℃下水热反应12小时,冷却至室温后,重复用去离子水和乙醇洗涤,得到前驱体Co(CO3)xOHy,将洗涤后的Co(CO3)xOHy和氟化氢铵(H5F2N)在N2保护下400℃加热反应1小时,得到CoF2。
更进一步的,上述CoF2的制备方法,所述Co(NO3)2·6H2O的添加量为1mmol/L。
更进一步的,上述CoF2的制备方法,所述尿素的添加量为5mmol/L。
更进一步的,上述CoF2的制备方法,所述Co(CO3)xOHy和H5F2N在加热反应中的质量比为1:3。
进一步的,一种BiVO4/CoF2光阳极的制备方法,步骤2)中,所述BiVO4的制备方法包括如下步骤:
1)将2.91g硝酸铋和9.96g碘化钾分散于硝酸溶液中,超声使其充分溶解,再加入60mL含有0.23mol/L的对苯醌乙醇溶液,充分搅拌,得到电沉积液;
2)取适量的步骤1)得到的电沉积液置于小烧杯中,以FTO作为工作电极,以铂丝为对电极,以Ag/AgCl为参比电极,采用三电极体系在外加偏压-0.1V vs.Ag/AgCl下沉积300秒,取出用去离子水冲洗,氮气吹干,在沉积层上滴加50μL的含有0.2mol/L乙酰丙酮氧矾的二甲基亚砜溶液,在空气中450℃下煅烧2小时,最后在1mol/L的氢氧化钠水溶液中浸渍30分钟,除去五氧化二钒,用去离子水冲洗,氮气吹干,得到BiVO4。
更进一步的,上述BiVO4的制备方法,步骤1)中,所述硝酸溶液的pH为1.7。
更进一步的,上述BiVO4的制备方法,步骤2)中,所述450℃是以2℃/min的升温速率升温至450℃。
本发明的有益效果为:
1、本发明的氟掺杂Co基催化剂的合成方法简单易行,且制备的电极活性和稳定性能较高,为合理设计光电极、以实现高效的水氧化过程奠定了基础。
2、针对现有的单独钒酸铋半导体的光生电荷分离效率低,水氧化动力学弱的问题,本发明制备的BiVO4/CoF2光阳极,能够实现光生载流子的有效分离,提高光阳极的光电催化水氧化性能,为今后制备并储存清洁能源提供了更多可能性。
附图说明
图1为BiVO4/CoF2光阳极的扫描电镜图。
图2为BiVO4/CoF2光阳极的X射线衍射(XRD)谱图。
图3为BiVO4光阳极和BiVO4/CoF2光阳极的线性扫描伏安曲线图。
图4为BiVO4光阳极和BiVO4/CoF2光阳极的ABPE图。
具体实施方式
实施例1一种BiVO4/CoF2光阳极的制备
1、CoF2的制备
将1mmol/L的Co(NO3)2·6H2O和5mmol/L的尿素溶解于35mL去离子水中,然后置于反应釜中,在120℃下水热反应12小时,冷却至室温后,重复用去离子水和乙醇洗涤,得到前驱体Co(CO3)xOHy,将洗涤后的Co(CO3)xOHy和3倍质量的H5F2N在N2保护下400℃加热反应1小时,得到CoF2。
2、BiVO4的制备
1)将2.91g硝酸铋和9.96g碘化钾分散于pH为1.7的硝酸溶液中,超声使其充分溶解,再加入60mL含有0.23mol/L的对苯醌乙醇溶液,充分搅拌,得到电沉积液;
2)取适量的电沉积液置于小烧杯中,以FTO作为工作电极,以铂丝为对电极,以Ag/AgCl为参比电极,采用三电极体系在外加偏压-0.1V vs.Ag/AgCl下沉积300秒,取出用去离子水冲洗,氮气吹干,在沉积层上滴加50μL的含有0.2mol/L乙酰丙酮氧矾的二甲基亚砜溶液,在空气中450℃(以2℃/min的升温速率升温)下煅烧2小时,最后在1mol/L的氢氧化钠水溶液中浸渍30分钟,除去五氧化二钒,用去离子水冲洗,氮气吹干,得到BiVO4。
3、BiVO4/CoF2光阳极的制备
1)将10mg制备好的CoF2分散于10mL去离子水中,超声3min,直至固体颗粒完全溶解,形成均匀的悬浊液;
2)将制备好的BiVO4浸入到步骤1)得到的悬浊液中,静置12h后取出,用去离子水冲洗,再用N2吹干,得到BiVO4/CoF2光阳极。
4、电化学性能测试
采用方型电解池和三电极工作系统进行了电化学性能测试。以上述制备方法制备的BiVO4/CoF2光阳极为工作电极,铂丝为对电极,Ag/AgCl电极为参比电极,进行电化学性能分析。以pH为9.5的1.0M K3BO3溶液为电解液,氙灯的光功率密度为mW/cm2,光照射FTO背面,通过扫描速率为50mV/s的线性扫描伏安法获得电流密度与电压特性(J-V)曲线,所有的测量单位都转化成RHE(ERHE=EAg/AgCl+0.197V+0.059pH)。
使用下面等式从J-V曲线计算施加的偏置光子对电流效率(ABPE):
ABPE(%)=J×(1.23-Vbias)×100%÷Pin
其中J是光电流密度(mA/cm2),Vbias是外加偏压,Pin是测得的光功率密度(AM1.5G,100mW/cm2)。
图1为BiVO4/CoF2光阳极的扫描电镜图,从图1中可以看出蠕虫形状的BiVO4上面有物质聚集。
图2为BiVO4/CoF2光阳极的X射线衍射(XRD)谱图。
图3为BiVO4光阳极和BiVO4/CoF2光阳极的线性扫描伏安曲线图,如图3所示,通过对比可以发现,使用CoF2作为催化剂后光电流密度明显提升,达到4.8mA/cm2,说明BiVO4/CoF2光阳极可以有效提高水分解的效率。
图4为BiVO4光阳极和BiVO4/CoF2光阳极的ABPE图,从图4中可以看出,BiVO4/CoF2光阳极的ABPE值在0.72V时达到最大,为1.49%,是单独BiVO4(0.84V时为0.3%)的4.97倍。
Claims (8)
1.一种BiVO4/CoF2光阳极的制备方法,其特征在于,制备方法包括如下步骤:
1)将CoF2分散于去离子水中,超声3 min,直至固体颗粒完全溶解,形成均匀的悬浊液;
2)将BiVO4浸入到步骤1)得到的悬浊液中,静置后取出,用去离子水冲洗,再用N2吹干,得到BiVO4/CoF2光阳极;
步骤1)中,所述CoF2的制备方法为:将Co(NO3)2·6H2O和尿素溶解于35 mL去离子水中,然后置于反应釜中,在120 ℃下水热反应12小时,冷却至室温后,重复用去离子水和乙醇洗涤,得到前驱体Co(CO3)xOHy,将洗涤后的Co(CO3)xOHy和氟化氢铵在N2保护下400 ℃加热反应1 小时,得到CoF2;
步骤2)中,所述BiVO4的制备方法包括如下步骤:
2.1)将2.91 g硝酸铋和9.96 g碘化钾分散于硝酸溶液中,超声使其充分溶解,再加入60 mL含有 0.23 mol/L的对苯醌乙醇溶液,充分搅拌,得到电沉积液;
2.2)取适量的步骤2.1)得到的电沉积液置于小烧杯中,以FTO 作为工作电极,以铂丝为对电极,以Ag/AgCl为参比电极,采用三电极体系在外加偏压-0.1 V vs. Ag/AgCl下沉积300 秒,取出用去离子水冲洗,氮气吹干,在沉积层上滴加50μL的含有0.2 mol/L乙酰丙酮氧矾的二甲基亚砜溶液,在空气中450℃下煅烧2小时,最后在1 mol/L的氢氧化钠水溶液中浸渍30分钟,除去五氧化二钒,用去离子水冲洗,氮气吹干,得到BiVO4。
2.根据权利要求1所述的制备方法,其特征在于,所述Co(NO3)2·6H2O的添加量为1mmol/L。
3.根据权利要求1所述的制备方法,其特征在于,所述尿素的添加量为5mmol/L。
4.根据权利要求1所述的制备方法,其特征在于,所述Co(CO3)xOHy和氟化氢铵在加热反应中的质量比为1:3。
5. 根据权利要求1所述的制备方法,其特征在于,步骤1)中,所述CoF2与去离子水的质量体积比为1 mg:1 mL。
6.根据权利要求1所述的制备方法,其特征在于,步骤2.1)中,所述硝酸溶液的pH为1.7。
7.根据权利要求1所述的制备方法,其特征在于,步骤2.2)中,所述450℃是以2℃/min的升温速率升温至450℃。
8.根据权利要求1所述的制备方法,其特征在于,步骤2)中,所述静置时间为12小时。
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