CN111508716B - Ni3Bi2S2/N-C电催化材料的制备方法 - Google Patents
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Abstract
本发明提供一种Ni3Bi2S2/N‑C电催化材料的制备方法。首先将一定量的六水合硝酸镍(Ni(NO3)2·6H2O)、五水合硝酸铋(Bi(NO3)3·5H2O)和硫脲(Tu)依次溶于一定体积的二甲基甲酰胺(DMF)中,持续搅拌得到Ni‑Bi‑Tu前驱体溶液。然后加入苯二甲酸和三乙烯二胺,搅拌,最后加入C3N4,搅拌至均匀分散。将得到的分散液中的溶剂蒸发,得到的产物在高纯Ar气氛中退火,得到Ni3Bi2S2/N‑C电催化剂。与现有技术相比,本发明所涉及的制备Ni3Bi2S2工艺无需真空条件,且材料来源更为普遍,简单易操作。新型Ni3Bi2S2与N‑C复合,首次应用于染料敏化太阳能电池和电催化氧还原反应,具有较好的活性。
Description
技术领域
本发明涉及一种新型Ni3Bi2S2/N-C电催化材料的制备方法,属于电催化领域。
背景技术
近年来,电催化材料在新型能源转化领域显示了重要的应用前景。贵金属Pt以其独特的表面结构和电子构型,在众多电催化反应体系(I3 -离子还原、氧还原反应等)中备受青睐。但由于Pt是稀有金属,储量低且价格高昂,极大地限制了其大规模工业化生产与应用,使得贵金属Pt替代材料研究成为电催化领域的重要方向之一。与此同时,寻求价格低廉、储量丰富且电催化性能优越的Pt对电极替代材料也成为未来染料敏化太阳能电池(简称DSSC)发展的重要方向。
近年来,无机金属化合物,包括金属碳化物、氮化物、氧化物、硫化物和硒化物等对电极材料的研究尤为活跃。其中,金属硫化物由于具有储量丰富、电催化性能高和导电性好等优势而备受关注。我们前期的研究表明,金属铋的硫化物在对电极材料领域表现出了一定的电催化性能,但是薄膜的导电性能较差限制了其催化性能的发挥,进而限制了其大规模的生产和应用。一般地,三元金属硫化物相对二元金属硫化物显示出更优异的导电性和稳定性。作为一种超导化合物,三元铋基硫化物Ni3Bi2S2具有着特殊的层状结构,研究表明,其具备金属特性,导电性很好,而目前为止,Ni3Bi2S2的制备工艺和电催化性能研究少有报道。基于以上背景,本专利发明一种Ni3Bi2S2/N-C电催化材料及其制备方法,以其作为氧还原和染料敏化太阳能电池电催化剂,显示出优异的电催化性能。
发明目的
本发明的目的是提供一种新型的Ni3Bi2S2/N-C电催化材料及其制备方法,不仅可以作为染料敏化太阳能电池对电极材料,还可作为氧还原电催化材料。
本发明的技术方案包括以下步骤:
(1)将Ni(NO3)2·6H2O、Bi(NO3)3·5H2O、Tu(Tu即为硫脲)依次溶于DMF,持续搅拌得到Ni-Bi-Tu前驱体溶液;
(2)在步骤(1)得到的Ni-Bi-Tu前驱体溶液中加入苯二甲酸和三乙烯二胺,搅拌,然后再加入C3N4,搅拌12-24h至均匀分散;
(3)将步骤(2)得到的分散液蒸发溶剂,然后将产物在高纯Ar或氮气气氛中,退火温度为850-1000℃,退火时间为0.5-2h即可制备得到黑色粉末Ni3Bi2S2/N-C。
Ni(NO3)2·6H2O、Bi(NO3)3·5H2O、Tu、苯二甲酸、三乙烯二胺、C3N4的质量比为1:0.9-1.5:0.1-0.5:1.5-3:2-4:0.3-7。
本发明所得到的Ni3Bi2S2/N-C具有以下几个显著的特点:
相比于传统的以Ni、Bi、S单质为源真空合成Ni3Bi2S2的方法,本发明材料
来源更为普遍,且方法简单,易于操作;
Ni3Bi2S2/N-C具有多功能性,不仅可以作为染料敏化太阳能电池对电极,还可以电催化氧还原反应。
附图说明
图1为所制备的样品的XRD图谱,左图a曲线为实例1样品,b曲线为实例2样品,c曲线为实例3样品;右图为10-40o放大谱图。
图2为所制备的样品的SEM图,a实例1样品的低倍SEM图(20000倍);b为实例1样品的高倍SEM图(100000倍);c实例3样品的低倍SEM图(20000倍);d为实例3样品的高倍SEM图(100000倍)。
图3为实例2所制备的样品的TEM图,a为TEM形貌图,b为石墨化碳高分辨图,c为Ni3Bi2S2颗粒高分辨图。
图4为实例2所制备的样品的ORR LSV曲线。
图5为实例3所制备的样品的阻抗谱图。
图6为实例3所制备的样品作为对电极测试得到的器件的输出特性曲线。
具体实施方式:
实施例1
Ni3Bi2S2/N-C的具体制备步骤为:
(1)将0.291g Ni(NO3)2·6H2O、0.3254g Bi(NO3)3·5H2O、0.076g Tu依次溶于40mLDMF,持续搅拌得到Ni-Bi-Tu前驱体溶液;
(2)在步骤(1)得到的溶液中加入0.544g 苯二甲酸和0.86g 三乙烯二胺,搅拌,然后再加入0.7g C3N4,搅拌12h至均匀分散;
(3)将步骤(2)得到的分散液在70oC下蒸发溶剂,然后将产物在高纯Ar气氛中,900 oC退火1h,得到黑色粉末Ni3Bi2S2/N-C。
图1左a曲线为该实例下制备的样品的XRD图,图中衍射峰均能对应于Ni3Bi2S2。此外,如右图所示,将10-40o处放大,还可以观测到25o附近有一个宽衍射峰,对应于石墨化碳的(002)峰。证明样品为Ni3Bi2S2和石墨化碳的复合物。图2a-b为所得到的样品的SEM图谱,如图2a所示,经分析,样品主要由片状石墨组成,其中包覆了Ni3Bi2S2颗粒,尺寸大约为几百纳米(如圆圈中所示)。图2b为放大的SEM图,放大后发现石墨化碳表面较为平整,并和Ni3Bi2S2颗粒较好地复合在一起,使得片状结构较厚,大约在10-50nm。
实施例2
Ni3Bi2S2/N-C的具体制备步骤为:
(1)将0.291g Ni(NO3)2·6H2O、0.3254g Bi(NO3)3·5H2O、0.076g Tu依次溶于40mLDMF,持续搅拌得到Ni-Bi-Tu前驱体溶液;
(2)在步骤(1)得到的溶液中加入0.544g 苯二甲酸和0.86g 三乙烯二胺,搅拌,然后再加入1.5g C3N4,搅拌12h至均匀分散;
(3)将步骤(2)得到的分散液在70oC下蒸发溶剂,然后将产物在高纯Ar气氛中,900 oC退火1h,得到黑色粉末Ni3Bi2S2/N-C。
图1左b曲线为该实例下制备的样品的XRD图,与实例1相同,样品的XRD衍射峰均能对应于Ni3Bi2S2和石墨化碳。但是,由于C3N4的量相比于实例1高,因此对应石墨化碳的衍射峰较强,说明复合物中碳含量稍高。图3为该实例下制备的样品的TEM图谱,如图3a所示,样品由片状结构和Ni3Bi2S2微纳米级颗粒(红圈内所示)组成,颗粒尺寸为0.1-0.4 μm,比实例1得到的样品颗粒尺寸小。将片状区域放大之后可以观测到石墨化碳的晶格条纹(图3b),将颗粒进一步放大可以发现Ni3Bi2S2颗粒表面是被石墨碳层包覆的(图3c)。
将样品分散到溶剂中,然后滴于旋转圆盘电极上,在氧饱和的0.1M KOH溶液中测试其ORR性能。图4为样品的LSV图谱,从图中可以看出,在1600rpm下,其起始电位为0.91Vvs. RHE,半波电位为0.81V vs. RHE,极限电流密度为5.72 mA cm-2,显示出较好的ORR性能。
实施例3
Ni3Bi2S2/N-C的具体制备步骤为:
(1)将0.291g Ni(NO3)2·6H2O、0.3254g Bi(NO3)3·5H2O、0.076g Tu依次溶于40mLDMF,持续搅拌得到Ni-Bi-Tu前驱体溶液;
(2)在步骤(1)得到的溶液中加入0.544g 苯二甲酸和0.86g 三乙烯二胺,搅拌,然后再加入0.3g C3N4,搅拌12h至均匀分散;
(3)将步骤(2)得到的分散液在70oC下蒸发溶剂,然后将产物在高纯Ar气氛中,900 oC退火1h,得到黑色粉末Ni3Bi2S2/N-C。
图1左c曲线为该实例下制备的样品的XRD图,与实例1相同,样品的XRD衍射峰也均能对应于Ni3Bi2S2和石墨化碳。但是,由于C3N4的量相比于实例1低,因此对应石墨化碳的衍射峰较弱,说明复合物中碳含量稍低。图2c-d为该实例下样品的SEM图谱,相比于实例1,可以看到Ni3Bi2S2颗粒增多(如圆圈区域所示),石墨化碳的片层厚度也增大,大于50nm。将该样品分散在溶剂中,然后刮涂于FTO导电面并50℃烘干,然后在管式炉中Ar气氛下400oC退火0.5h。图5为该实例下制备的样品的阻抗图谱,相比于Pt(电荷转移电阻Rct=1.40 Ω·cm2),Ni3Bi2S2/N-C具有更小的Rct,仅0.55 Ω·cm2,说明Ni3Bi2S2/N-C具有优异的电催化活性。将样品作为对电极组装染料敏化太阳能电池测试其输出特性(图6),经计算,器件的光电转换效率为6.41%,与Pt对电极器件的光电转换效率相当(6.14%),有望取代Pt作为新型高效的染料敏化太阳能电池对电极材料。
Claims (4)
1.一种Ni3Bi2S2/N-C电催化材料的制备方法,该Ni3Bi2S2/N-C电催化材料中Ni3Bi2S2负载在N-C上,其特征在于,具体步骤如下:
(1)将Ni(NO3)2·6H2O、Bi(NO3)3·5H2O、硫脲依次溶于DMF,持续搅拌得到Ni-Bi-硫脲前驱体溶液;
(2)在步骤(1)得到的Ni-Bi-硫脲前驱体溶液中加入苯二甲酸和三乙烯二胺,搅拌,然后再加入C3N4,搅拌至均匀分散;
(3)将步骤(2)得到的分散液蒸发溶剂,退火处理即可制备得到黑色粉末Ni3Bi2S2/N-C。
2.根据权利要求1所述的Ni3Bi2S2/N-C电催化材料的制备方法,其特征在于,Ni(NO3)2·6H2O、Bi(NO3)3·5H2O、硫脲、苯二甲酸、三乙烯二胺、C3N4的质量比为1:0.9-1.5:0.1-0.5:1.5-3:2-4:0.3-7。
3.根据权利要求1所述的Ni3Bi2S2/N-C电催化材料的制备方法,其特征在于,步骤(3)中蒸发溶剂过程中的温度为50-80℃。
4.根据权利要求1所述的Ni3Bi2S2/N-C电催化材料的制备方法,其特征在于,步骤(3)中退火气氛包括Ar、N2;退火温度为850-1000℃,退火时间为0.5-2h。
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