CN111850613A - 一种PtIr纳米溶胶的制备方法 - Google Patents
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Abstract
本发明公开了一种PtIr纳米溶胶的制备方法,本发明采用方波电势法制备PtIr合金纳米粒子,该方法以大块PtIr合金丝为原材料,制备过程绿色、方便、经济,既不需要在溶液中引入金属盐和添加剂,也无需去模板的后处理。该方法为利用方波电势脉冲在NaOH溶液中电化学分散纯PtIr丝新方法,短时间内即可制备出PtIr合金纳米粒子。
Description
技术领域
本发明涉及材料技术领域,尤其涉及一种PtIr纳米溶胶的制备方法。
背景技术
氨氧化反应因其在直接氧化燃料电池或储氢化合物的潜在应用而受到科研工作者的极大关注。其中,PtIr合金纳米粒子是氨氧化反应的高效催化剂。通常情况下,制备PtIr合金纳米催化剂的方法有很多种,其中,大部分的方法是在保护剂以及其他有机溶剂存在的条件下,化学还原Pt和Ir的金属离子前驱体制备PtIr合金纳米粒子。本发明中,采用电化学方法一步制备PtIr合金纳米粒子。本制备方法在室温的条件下,将纯PtIr丝在NaOH溶液中进行温和的方波电势扰动即可制备PtIr纳米溶胶,制备方法简单、快速,无需任何金属离子前驱体、还原剂、保护剂以及有机溶剂的参与。对PtIr纳米溶胶进行了XRD、XPS和TEM等表征。和采用相同方法制备的单种Pt纳米粒子相比,PtIr纳米粒子在室温下对氨氧化反应具有较高的催化活性。
发明内容
本发明的目的在于为了解决上述问题而提供一种PtIr纳米溶胶的制备方法。
本发明通过以下技术方案来实现上述目的:
本发明包括以下步骤:
S1:将PtIr电极丝置于2M NaOH溶液中,采用三电极体系,在电化学工作站上采用方波电势法,设置高电势为0.2V,低电势为-5V,频率为100Hz,方波时间为300s;
S2:当电化学反应结束后,收集PtIr纳米溶胶并离心分离后,超纯水和乙醇交替清洗各5次;
S3:然后将PtIr纳米粒子通过超声波分散在乙醇中,负载在玻碳电极上,自然晾干,得到PtIr纳米粒子修饰的玻碳电极。
所述步骤S2中离心分离转速为12000r/min。
采用步骤S1和S2的方法能够制备Pt纳米溶胶。采用相同方法制备的Pt 纳米粒子用于和PtIr纳米粒子做比较,能更清晰的说明双金属PtIr纳米粒子在电催化活性方面的优越性。
采用步骤S1-S3的方法能够制备得到Pt纳米粒子修饰的玻碳电极。
PtIr纳米粒子修饰的玻碳电极和Pt纳米粒子修饰的玻碳电极的电催化活性测试是在0.5M NaOH+2M NH4OH溶液中进行的。
本发明的有益效果在于:
本发明是一种PtIr纳米溶胶的制备方法,与现有技术相比,本发明采用方波电势法制备PtIr合金纳米材料,该方法以大块PtIr合金为原材料,制备过程绿色、方便、经济,既不需要在溶液中引入金属盐和添加剂,也无需去模板的后处理。该方法为利用方波电势脉冲技术在NaOH溶液中电化学分散纯PtIr丝制备PtIr合金纳米粒子的新方法,短时间内即可制备出PtIr合金纳米粒子。与其它制备方法相比,具有如下优点:
(1)反应条件温和:一般在常温常压下进行。
(2)可控性好:可选择性的调节和控制外加电势、电流及波形,实现纳米材料的形状、大小可控。
(3)适用范围广:可制备多种纳米态单金属、合金、氧化物等材料。
(4)可与其它化学制备方法联用,来制备各种不同要求的纳米材料。
(5)耗能低、环境友好、设备简单、操作方便。
附图说明
图1是PtIr纳米粒子的扫描电镜(SEM)图;
图1中:(A,B)PtIr纳米粒子的SEM图,(C)PtIr纳米粒子的X-射线色散能量谱(EDS)图。图1A的插图是PtIr纳米溶胶的光学照片;
图2是PtIr纳米溶胶的透射电镜(TEM)图;
图2中:(A,B)PtIr溶胶的TEM表征图,(C)PtIr溶胶的高分辨透射电镜 (HR-TEM)表征图;
图3是方波法制备的PtIr纳米粒子和Pt纳米粒子的X射线衍射(XRD)图;
图4是Pt 4f和Ir4f高分辨X-射线光电子能谱(XPS)图;
图4中:(A)Pt4f、(B)Ir-4f;
图5是PtIr和Pt纳米粒子对氨(0.5M NaOH+2M NH4OH)的电催化氧化。
具体实施方式
下面结合附图对本发明作进一步说明:
循环伏安实验和方波电势实验在H型电解池和CHI660C电化学工作站(辰华仪器,中国上海)上进行。工作电极为多晶PtIr丝(直径1mm,纯度≥99.99%, Pt:Ir=80:20%),对电极为铂片(面积1cm2),参比电极为饱和硫酸亚汞电极 (SMSE)。工作电极在使用之前用2000#砂纸打磨抛光,超纯水超声清洗3次。
PtIr溶胶的制备是将PtIr电极丝置于2MNaOH溶液中,采用三电极体系,在电化学工作站上采用SWP法,0.2V,低电势为-5V,频率为100Hz,方波时间为300s。当电化学反应结束后,收集纳米溶胶并离心(12000r/min)分离,采用超纯水和乙醇交替清洗纳米粒子各5次。同时,采用同样的方法可制备Pt 纳米溶胶。然后将PtIr和Pt纳米粒子分散在乙醇中,负载在GC电极上,自然晾干,得到PtIr纳米粒子修饰的GC电极(PtIrNPs/GC)。采用同样的方法可制备Pt纳米粒子修饰的GC电极(PtNPs/GC)。
PtIrNPs/GC和PtNPs/GC的电催化活性测试是在0.5M NaOH+2M NH4OH 溶液中进行的。
PtIr纳米溶胶的表征:
图1A的插图显示了用方波电势法制备的PtIr纳米溶胶,从图片中可以看出, PtIr纳米溶胶呈黑色,能长时间稳定存在。图1A和B为PtIr纳米溶胶的扫描电镜图,从图中可以看出,PtIr纳米粒子团聚在一起呈多孔海绵结构。从图1B可以看出,PtIr纳米粒子的粒径不规则,粒子聚集在一起形成了不规则小孔,这可能与制备过程中H2的析出有关。通过EDS分析(如图1C所示),制备的PtIr 纳米粒子中Pt和Ir的元素组成分别为67.53和32.47at%。此外,Pt和Ir在光滑 PtIr丝中的元素组成分别为80.00和20.00at%。与本体金属相比,PtIr纳米粒子中的Ir含量有所增加,这可能是由于Ir比Pt更容易从大块金属中剥离。
图2A为PtIr纳米粒子的TEM图,由于制备过程中未加保护剂,纳米粒子呈团聚态,难以准确估计粒径分布。从图2B可以看出,PtIr纳米粒子交联在一起,粒径约10-20nm,为了获得单分散的PtIr合金纳米粒子,课题组将在下一步工作中进行探索。如图2C所示,PtIr纳米粒子的晶面间距为0.230nm,对应 PtIr合金的(111)面,因此,采用方波电势法制备的PtIr纳米粒子为合金态。
采用XRD来检测所制备的PtIr合金纳米粒子的物相,其结果如图3所示。为了更好的分析其合金峰的位置,图3以Pt(JCPDS编号04-0802)和Ir(JCPDS 编号06-0598)为参考。对单种Pt纳米粒子也进行了XRD表征。如图3所示, 39.8°、46.2°和67.8°处出现特征衍射峰为Pt的(111)、(200)和(220)晶面。 39.8°,46.2°和67.8°处出现特征衍射峰分别为PtIr的(111)、(200)和(220)晶面。PtIr 的衍射峰并未发生分离,证实了Pt与Ir形成了PtIr合金。
利用XPS分析了PtIr纳米粒子的表面化学组成和价态。图4A和B给出了 Pt 4f和Ir4f的高分辨XPS图谱。图4A所示结合能的表明,~71.41和~74.48 eV处分别为Pt4f7/2和4f5/2峰,另一方面,在73.8和74.6eV处,没有出现Pt2+和Pt4+的能谱峰,说明Pt为0价金属状态。图4B所示,61.04eV和64.07eV对应于Ir 4f7/2和Ir 4f5/2峰,说明PtIr纳米粒子中的Ir为0价。此外,通过XPS表征,PtIr合金纳米粒子的Pt/Ir的表面原子比为68.16/31.84。根据XPS和EDS(图 1C)分析结果,Pt在PtIr合金粒子的表面富集。
PtIr纳米粒子的电催化活性:
PtIr-NPs/GC电极和Pt-NPs/GC电极对氨的电催化氧化活性研究是在0.5M NaOH+2M NH4OH溶液中进行的,扫描速率为50mV s-1。
如图5所示,在0.5M NaOH+2M NH4OH溶液中,以50mV s-1的扫速,研究了PtIr-NPs/GC电极和Pt-NPs/GC电极对氨的电催化氧化。在-0.66V时,与 Pt NP(0.18mA cm-2)比较,PtIrNP(0.38mA cm-2)的电流密度更高。基于上述结果,PtIr纳米粒子具有较高的电化学活性可能是源于Pt与Ir之间的双功能机理和电子效应。此外,与纯Pt纳米粒子相比,PtIr纳米粒子对氨的电催化氧化具有更低的氧化起始电势,双金属PtIr改善了氨的氧化动力学,因此具有更高的催化性能。
以上显示和描述了本发明的基本原理和主要特征及本发明的优点。本行业的技术人员应该了解,本发明不受上述实施例的限制,上述实施例和说明书中描述的只是说明本发明的原理,在不脱离本发明精神和范围的前提下,本发明还会有各种变化和改进,这些变化和改进都落入要求保护的本发明范围内。本发明要求保护范围由所附的权利要求书及其等效物界定。
Claims (5)
1.一种PtIr纳米溶胶的制备方法,其特征在于,包括以下步骤:
S1:将PtIr电极丝置于2M NaOH溶液中,采用三电极体系,在电化学工作站上采用方波电势法,设置高电势为0.2V,低电势为-5V,频率为100Hz,方波时间为300s;
S2:当电化学反应结束后,收集PtIr纳米溶胶并离心分离后,超纯水和乙醇交替清洗各5次;
S3:然后将PtIr纳米粒子通过超声波分散在乙醇中,负载在玻碳电极上,自然晾干,得到PtIr纳米粒子修饰的玻碳电极。
2.根据权利要求1所述的PtIr纳米溶胶的制备方法,其特征在于:所述步骤S2中离心分离转速为12000r/min。
3.根据权利要求1所述的PtIr纳米溶胶的制备方法,其特征在于:采用步骤S1和S2的方法能够制备Pt纳米溶胶。
4.根据权利要求1所述的PtIr纳米溶胶的制备方法,其特征在于:采用步骤S1-S3的方法能够制备得到Pt纳米粒子修饰的玻碳电极。
5.根据权利要求1或4所述的PtIr纳米溶胶的制备方法,其特征在于:PtIr纳米粒子修饰的玻碳电极和Pt纳米粒子修饰的玻碳电极的电催化活性测试是在0.5M NaOH+2M NH4OH溶液中进行的。
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