CN114122424A - 一种亲水碳基Ni纳米ORR电催化剂的制备方法 - Google Patents
一种亲水碳基Ni纳米ORR电催化剂的制备方法 Download PDFInfo
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Abstract
本发明公开了一种亲水碳基Ni纳米ORR电催化剂的制备方法,涉及ORR电催化剂技术领域,包括以下步骤:将四水合醋酸镍、聚乙烯吡咯烷酮加入到无水乙醇中,超声,加热反应,离心,得Ni棱晶前体沉淀,干燥;将Ni棱晶前体分散到DMF中,超声,加入含2,3,6,7,10,11‑六羟基三亚苯有机配体的DMF溶液,加热反应,离心,得Ni‑pre@MOF沉淀;将Ni‑pre@MOF沉淀于保护气氛下先进行预热解,然后再升温进行热解,获得蚕蛹状的亲水富氧碳壳负载Ni纳米粒子的O‑C@Ni。本发明制得的O‑C@Ni产品可用作燃料电池阴极ORR过程的电催化剂,该材料具有的良好亲水性,有利于反应过程中氧气分子的吸附,且高比表面积的Ni纳米粒子能大大促进催化剂的氧相关动力学,从而使其在催化ORR的过程中表现出高的催化活性。
Description
技术领域
本发明涉及ORR电催化剂技术领域,尤其涉及一种亲水碳基Ni纳米ORR电催化剂的制备方法。
背景技术
燃料电池是一种将存在于燃料与氧化剂中的化学能直接转化为电能的发电装置,通常由形成离子导电体的电解质板和其两侧配置的燃料极(阳极)和空气极(阴极)、及两侧气体流路构成。燃料电池作为新一代绿色能源技术,因其成本低、容量高、环境友好而所受到广泛关注。然而,受限于商用铂基催化剂稳定性差、成本高和储量低等缺点,燃料电池以及相关绿色能源技术的应用缓慢,因此,研发高效绿色的替代性氧气还原反应(ORR)电催化剂,是电催化领域的研究热点。
纳米镍由于尺寸小,比表面积大,表面原子数较多和表面原子的配位不饱和性导致其表面活性位点增多,具有很高的催化活性。将镍基催化剂负载于如无机或有机载体上,能有效地提高催化剂的活性和稳定性。
目前,现有技术中公开的碳基负载Ni纳米ORR催化剂,其通过简单的热解处理过程,所制备出的Ni纳米颗粒呈现出不规则的形态,大部分Ni位点深包裹在碳基材内部,无法提供足够的暴露活性位点;并且材料亲水性欠佳,这些都极大地阻碍了电催化ORR效率的提升。
发明内容
基于背景技术存在的技术问题,本发明提出了一种亲水碳基Ni纳米ORR电催化剂的制备方法,制备的材料具有高度暴露的表面活性中心和优良的亲水能力,从而使其在催化ORR的过程中表现出高的催化活性。
本发明提出的一种亲水碳基Ni纳米ORR电催化剂的制备方法,包括以下步骤:
S1、Ni棱晶前体的制备:将四水合醋酸镍、聚乙烯吡咯烷酮加入到无水乙醇中,超声分散,加热反应,冷却,离心收集沉淀,即得Ni棱晶前体沉淀,洗涤,干燥;
S2、Ni-pre@MOF的制备:将Ni棱晶前体分散到N,N-二甲基甲酰胺中,超声,然后加入含2,3,6,7,10,11-六羟基三亚苯有机配体的N,N-二甲基甲酰胺溶液,加热反应,冷却,离心收集沉淀,获得核壳结构的Ni-pre@MOF棱晶沉淀,洗涤;
S3、O-C@Ni的制备:将Ni-pre@MOF棱晶沉淀于保护气氛下先在300-400℃下进行预热解,然后再升温至600℃-800℃进行热解,获得蚕蛹状的亲水富氧碳壳负载Ni纳米粒子的O-C@Ni。
优选地,S1中,聚乙烯吡咯烷酮为PVP-K30;采用油浴90℃下加热反应10h。
优选地,S2中,Ni棱晶前体和2,3,6,7,10,11-六羟基三亚苯有机配体的质量比为20:29-35。
优选地,S2中,采用油浴115-125℃下加热反应5-7h。
优选地,S3中,先在300-400℃进行预热解40-70min,然后再升温至600-800℃进行热解1.5-2.5h。
有益效果:本发明提出了一种亲水碳基Ni纳米ORR电催化剂的制备方法,是先通过在棱晶状的Ni前体上生长一层有机金属框架MOF,形成核壳结构的Ni-pre@MOF棱晶沉淀,然后再通过两步热解反应,形成最终的蚕蛹状富氧碳壳支撑的金属镍纳米颗粒,所制得的产品具有高度暴露的表面活性中心;此外,采用富含羟基的2,3,6,7,10,11-六羟基三亚苯作为有机配体来制备金属有机框架,所得表面富含大量氧元素的亲水性碳壳,从而赋予产品优良的亲水能力。所制得亲水富氧碳壳负载Ni纳米粒子的O-C@Ni产品可用作燃料电池阴极ORR过程的活性电化学催化剂,一方面该材料具有的良好亲水性,有利于反应过程中氧气分子的吸附,另一方面高比表面积的Ni纳米粒子能大大促进催化剂的氧相关动力学,从而使其在催化ORR的过程中表现出高的催化活性,实现高效的ORR催化过程,提高ORR效率。
附图说明
图1为本发明实施例1中制备的样品的SEM图;其中,a-c依次为Ni-pre、Ni-pre@MOF、O-C@Ni的FEI图,d-f依次为Ni-pre、Ni-pre@MOF、O-C@Ni的TEM图;
图2为本发明实施例1制备的Ni-pre、Ni-pre@MOF、O-C@Ni的XRD图;
图3为本发明实施例1制备的O-C@Ni、对比例1制备的Ni-pre(A)、对比例2制备的NiMOF(A)、石墨Graphite的接触角测试数据。
图4为本发明实施例1制备的O-C@Ni、对比例1制备的Ni-pre(A)、对比例2制备的NiMOF(A)的XPS谱图;
图5为本发明实施例1制备的O-C@Ni(d)、对比例1制备的Ni-pre(A)(b)、对比例2制备的Ni MOF(A)(c)、商业Pt/C催化剂(a)的LSV曲线。
具体实施方式
下面,通过具体实施例对本发明的技术方案进行详细说明。
实施例1
一种亲水碳基Ni纳米ORR电催化剂的制备方法,包括以下步骤:
S1、Ni棱晶前体的制备:将160mg四水合醋酸镍和375mg聚乙烯吡咯烷酮(PVP-K30)加入到25mL无水乙醇中,超声分散30min使其充分混合,然后将溶液转移到100mL三颈瓶中,在90℃下的油浴中保持10h,自然冷却至室温后,离心收集沉淀,即得Ni棱晶前体沉淀,用乙醇洗涤3-4次,烘干备用;
S2、Ni-pre@MOF的制备:将20mg Ni棱晶前体分散到32mL N,N-二甲基甲酰胺中,超声,然后加入8mL含有32mg的2,3,6,7,10,11-六羟基三亚苯有机配体配体的N,N-二甲基甲酰胺溶液中,搅拌10min后,在120℃下油浴中保持6h,然后通过搅拌使其冷却至室温,离心收集沉淀,获得核壳结构的Ni-pre@MOF棱晶沉淀,用乙醇洗涤3-4次;
S3、O-C@Ni的制备:采用两步热解法对Ni-pre@MOF进行热解处理,具体是先将Ni-pre@MOF棱晶沉淀转移至管式炉中,于N2气氛下先以2℃/min的速率升温至300℃,保持1h进行预热解,然后再以1℃/min的速率升温至600℃,保持2h进行热解,自然冷却至室温后获得蚕蛹状的亲水富氧碳壳负载Ni纳米粒子的O-C@Ni样品。
对比例1
与实施例1相比,区别在于:不含有S2步骤,是采用两步热解法直接对S1中的Ni棱晶前体进行热解处理;所得产品记作Ni-pre(A)。
对比例2
与实施例1相比,区别在于:不含有S1步骤,是将20mg四水合醋酸镍直接与32mg的2,3,6,7,10,11-六羟基三亚苯(HHTP)有机配体在DMF溶剂中混合,油浴反应,离心收集沉淀,洗涤,再采用两步热解法进行热解处理;所得产品记作Ni MOF(A)。
对本发明实施例1和对比例1-2中制备的材料进行表征和测试。
图1为SEM图,从图中可以看出,a、d中的Ni-pre为棱晶状的,在其上生长一层有机金属框架MOF,形成核壳结构的Ni-pre@MOF棱晶(b、e),再通过热解反应,得到蚕蛹状富氧碳壳支撑的金属镍纳米颗粒,其具有高度暴露的表面活性中心(c、f)。
图2为XRD图,从图中可以看出,O-C@Ni样品只有44.6°、51.9°、76.5°的衍射峰,分别对应于金属镍的(111)、(200)和(220)平面,说明O-C@Ni样品表面所形成的是金属Ni纳米颗粒。
图3为接触角测试数据,从图中可以看出,本发明中制备的O-C@Ni样品具有极强的亲水特性。
图4为XPS谱图,通过对比Ni MOF(A)和O-C@Ni样品的O1s谱峰,可发现O的含量在热解处理后仍较高,即在最终的O-C@Ni样品中存在稳固的C-O健,其表面富氧。
对本发明制备的材料进行电化学性能测试。图5为线性扫描电压LSV曲线,从图中可以看出,O-C@Ni催化剂表现出了优异的ORR性能,与可逆氢电极(vs.RHE)相比具有0.96V的较小的起始电位和0.83V较佳的半波电位,远优于0.70V的Ni-pre(A)和0.73V的Ni MOF(A),与商业Pt/C催化剂相当(0.86V vs.RHE)。此外,O-C@Ni催化剂实现了约5.0mA/cm2的相对较高的极限电流密度,接近商业Pt/C催化剂的极限电流密度(约5.2mA/cm2)。
以上所述,仅为本发明较佳的具体实施方式,但本发明的保护范围并不局限于此,任何熟悉本技术领域的技术人员在本发明揭露的技术范围内,根据本发明的技术方案及其发明构思加以等同替换或改变,都应涵盖在本发明的保护范围之内。
Claims (5)
1.一种亲水碳基Ni纳米ORR电催化剂的制备方法,其特征在于,包括以下步骤:
S1、Ni棱晶前体的制备:将四水合醋酸镍、聚乙烯吡咯烷酮加入到无水乙醇中,超声分散,加热反应,冷却,离心收集沉淀,即得Ni棱晶前体沉淀,洗涤,干燥;
S2、Ni-pre@MOF的制备:将Ni棱晶前体分散到N,N-二甲基甲酰胺中,超声,然后加入含2,3,6,7,10,11-六羟基三亚苯有机配体的N,N-二甲基甲酰胺溶液,加热反应,冷却,离心收集沉淀,获得核壳结构的Ni-pre@MOF棱晶沉淀,洗涤;
S3、O-C@Ni的制备:将Ni-pre@MOF棱晶沉淀于保护气氛下先在300-400℃下进行预热解,然后再升温至600℃-800℃进行热解,获得蚕蛹状的亲水富氧碳壳负载Ni纳米粒子的O-C@Ni。
2.根据权利要求1所述的亲水碳基Ni纳米ORR电催化剂的制备方法,其特征在于,S1中,聚乙烯吡咯烷酮为PVP-K30;采用油浴90℃下加热反应10h。
3.根据权利要求1所述的亲水碳基Ni纳米ORR电催化剂的制备方法,其特征在于,S2中,Ni棱晶前体和2,3,6,7,10,11-六羟基三亚苯有机配体的质量比为20:29-35。
4.根据权利要求1所述的亲水碳基Ni纳米ORR电催化剂的制备方法,其特征在于,S2中,采用油浴115-125℃下加热反应5-7h。
5.根据权利要求1所述的亲水碳基Ni纳米ORR电催化剂的制备方法,其特征在于,S3中,先在300-400℃进行预热解40-70min,然后再升温至600-800℃进行热解1.5-2.5h。
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