Pt纳米绒球的控制合成及其电催化性能
|
摘要
以氯铂酸(H_2PtCl_6·6H_2O)为前驱体、三缩四乙二醇(TEG)为溶剂和还原剂、聚乙烯吡咯烷酮(PVP)为稳定剂,在160℃下油浴反应3 h,合成了Pt纳米颗粒,利用TEM、SEM、XRD和XPS等技术对Pt纳米颗粒的形貌和结构进行了表征,初步探索了其电催化性能。结果表明,所得Pt纳米颗粒为形貌单一、大小均匀、平均粒径约(60±5) nm的Pt纳米绒球,反应体系的最适宜H_2PtCl_6∶C_6H_5COOH∶PVP物质的量比为1∶15∶22.5;所得Pt纳米绒球的电催化活性相对于商业铂黑明显增强。
Using chloroplatinic acid(H_2PtCl_6·6 H_2O) as a precursor,tetraethylene glycol(TEG) as both a solvent and a reducing agent,and polyvinylpyrrolidone(PVP) as a stabilizer,we synthesized uniform and well-defined pompon-like Pt nano-pompons with an average diameter of(60±5) nm under 160 ℃ oil-bath for 3 h.Moreover,we characterized the morphology and structure of Pt nano-pompons by TEM,SEM,XRD,and XPS,and preliminarily investigated the electrocatalytic property.The optimum molar ratio of H_2PtCl_6,C_6H_5COOH,and PVP is 1∶15∶22.5 in the reaction system.The electrocatalytic property of the prepared Pt nano-pompons enhances obviously compared with that of commercial Pt black.
Using chloroplatinic acid(H_2PtCl_6·6 H_2O) as a precursor,tetraethylene glycol(TEG) as both a solvent and a reducing agent,and polyvinylpyrrolidone(PVP) as a stabilizer,we synthesized uniform and well-defined pompon-like Pt nano-pompons with an average diameter of(60±5) nm under 160 ℃ oil-bath for 3 h.Moreover,we characterized the morphology and structure of Pt nano-pompons by TEM,SEM,XRD,and XPS,and preliminarily investigated the electrocatalytic property.The optimum molar ratio of H_2PtCl_6,C_6H_5COOH,and PVP is 1∶15∶22.5 in the reaction system.The electrocatalytic property of the prepared Pt nano-pompons enhances obviously compared with that of commercial Pt black.
引文
[1] CHEN G X,XU C F,HUANG X Q,et al.Interfacial electronic effects control the reaction selectivity of platinum catalysts[J].Nat Mater,2016,15(5):564-569.
[2] FU X,WANG Y,WU N,et al.Preparation of colloidal solutions of thin platinum nanowires[J].J Mater Chem,2003,13(5):1192-1195.
[3] KIM S W,KIM M,LEE W Y,et al.Fabrication of hollow palladium spheres and their successful application as the recyclable heterogeneous catalyst for Suzuki coupling reactions[J].J Am Chem Soc,2002,124(26):7642-7643.
[4] SON S U,JANG Y,PARK J,et al.Designed synthesis of atom-economical Pd/Ni bimetallic nanoparticle-based catalysts for Sonogashira coupling reactions[J].J Am Chem Soc,2004,126(16):5026-5027.
[5] KANG Y J,PYO J B,YE X,et al.Shape-controlled synthesis of Pt nanocrystals:the role of metal carbonyls[J].ACS Nano,2012,7(1):645-653.
[6] ZHOU W,WU J,YANG H.Highly uniform platinum icosahedra made by hot injection-assisted grails method[J].Nano Lett,2013,13:2870-2874.
[7] TIAN N,ZHOU Z Y,SUN S G,et al.Synthesis of tetrahexahedral platinum nanocrystals with high-index facets and high electro-oxidation activity[J].Science,2007,316(5825):732-735.
[8] XIA B Y,WU H B,WANG X,et al.Highly concave platinum nanoframes with high-index facets and enhanced electrocatalytic properties[J].Angew Chem Int Ed,2013,52(47):12337-12340.
[9] ZHANG Z,HUI J,LIU Z C,et al.Glycine-mediated syntheses of Pt concave nanocubes with high-index(hk0) facets and their enhanced electrocatalytic activities[J].Langmuir,2012,28(42):14845-14848.
[10] HUANG X Q,ZHAO Z,FAN J,et al.Amine-assisted synthesis of concave polyhedral platinum nanocrystals having(411) high-index facets[J].J Am Chem Soc,2011,133(13):4718-4721.
[11] DAI L,CHI Q,ZHAO Y,et al.Controlled synthesis of novel octapod platinum nanocrystals under microwave irradiation[J].Mater Res Bull,2014,49(1):413-419.
[12] ZHANG L,CHEN D,JIANG Z,et al.Facile syntheses and enhanced electrocatalytic activities of Pt nanocrystals with(hkk) high-index surfaces[J].Nano Res,2012,5(3):181-189.
[13] WAGNER C D,RIGGS W M,DAVIS L E,et al.Handbook of X-ray Photoelectron Spectroscopy[M].Perkin-Elmer,Physical Electronics Division,Eden Prairie,1979.
[2] FU X,WANG Y,WU N,et al.Preparation of colloidal solutions of thin platinum nanowires[J].J Mater Chem,2003,13(5):1192-1195.
[3] KIM S W,KIM M,LEE W Y,et al.Fabrication of hollow palladium spheres and their successful application as the recyclable heterogeneous catalyst for Suzuki coupling reactions[J].J Am Chem Soc,2002,124(26):7642-7643.
[4] SON S U,JANG Y,PARK J,et al.Designed synthesis of atom-economical Pd/Ni bimetallic nanoparticle-based catalysts for Sonogashira coupling reactions[J].J Am Chem Soc,2004,126(16):5026-5027.
[5] KANG Y J,PYO J B,YE X,et al.Shape-controlled synthesis of Pt nanocrystals:the role of metal carbonyls[J].ACS Nano,2012,7(1):645-653.
[6] ZHOU W,WU J,YANG H.Highly uniform platinum icosahedra made by hot injection-assisted grails method[J].Nano Lett,2013,13:2870-2874.
[7] TIAN N,ZHOU Z Y,SUN S G,et al.Synthesis of tetrahexahedral platinum nanocrystals with high-index facets and high electro-oxidation activity[J].Science,2007,316(5825):732-735.
[8] XIA B Y,WU H B,WANG X,et al.Highly concave platinum nanoframes with high-index facets and enhanced electrocatalytic properties[J].Angew Chem Int Ed,2013,52(47):12337-12340.
[9] ZHANG Z,HUI J,LIU Z C,et al.Glycine-mediated syntheses of Pt concave nanocubes with high-index(hk0) facets and their enhanced electrocatalytic activities[J].Langmuir,2012,28(42):14845-14848.
[10] HUANG X Q,ZHAO Z,FAN J,et al.Amine-assisted synthesis of concave polyhedral platinum nanocrystals having(411) high-index facets[J].J Am Chem Soc,2011,133(13):4718-4721.
[11] DAI L,CHI Q,ZHAO Y,et al.Controlled synthesis of novel octapod platinum nanocrystals under microwave irradiation[J].Mater Res Bull,2014,49(1):413-419.
[12] ZHANG L,CHEN D,JIANG Z,et al.Facile syntheses and enhanced electrocatalytic activities of Pt nanocrystals with(hkk) high-index surfaces[J].Nano Res,2012,5(3):181-189.
[13] WAGNER C D,RIGGS W M,DAVIS L E,et al.Handbook of X-ray Photoelectron Spectroscopy[M].Perkin-Elmer,Physical Electronics Division,Eden Prairie,1979.