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负载于热还原氧化石墨烯上的金属氟化物纳米颗粒的合成

Synthesis of metal-fluoride nanoparticles supported on thermally reduced graphite oxide.

作者信息

Schmitz Alexa, Schütte Kai, Ilievski Vesko, Barthel Juri, Burk Laura, Mülhaupt Rolf, Yue Junpei, Smarsly Bernd, Janiak Christoph

机构信息

Institut für Anorganische Chemie und Strukturchemie, Heinrich-Heine-Universität Düsseldorf, 40204 Düsseldorf, Germany.

Gemeinschaftslabor für Elektronenmikroskopie RWTH-Aachen, Ernst Ruska-Centrum für Mikroskopie und Spektroskopie mit Elektronen, D-52425 Jülich, Germany.

出版信息

Beilstein J Nanotechnol. 2017 Nov 22;8:2474-2483. doi: 10.3762/bjnano.8.247. eCollection 2017.

Abstract

Metal-fluoride nanoparticles, (MF -NPs) with M = Fe, Co, Pr, Eu, supported on different types of thermally reduced graphite oxide (TRGO) were obtained by microwave-assisted thermal decomposition of transition-metal amidinates, (M{MeC[N(iPr)]} ) or [M(AMD) ] with M = Fe(II), Co(II), Pr(III), and tris(2,2,6,6-tetramethyl-3,5-heptanedionato)europium, Eu(dpm), in the presence of TRGO in the ionic liquid (IL) 1-butyl-3-methylimidazolium tetrafluoroborate ([BMIm][BF]). The crystalline phases of the metal fluorides synthesized in [BMIm][BF] were identified by powder X-ray diffraction (PXRD) to be MF for M = Fe, Co and MF for M = Eu, Pr. The diameters and size distributions of MF @TRGO were from (6 ± 2) to (102 ± 41) nm. Energy-dispersive X-ray spectroscopy (EDX) and X-ray photoelectron spectroscopy (XPS) were used for further characterization of the MF -NPs. Electrochemical investigations of the FeF-NPs@TRGO as cathode material for lithium-ion batteries were evaluated by galvanostatic charge/discharge profiles. The results indicate that the FeF-NPs@TRGO as cathode material can present a specific capacity of 500 mAh/g at a current density of 50 mA/g, including a significant interfacial charge storage contribution. The obtained nanomaterials show a good rate capacity as well (220 mAh/g and 130 mAh/g) at a current density of 200 and 500 mA/g, respectively.

摘要

通过在离子液体1-丁基-3-甲基咪唑四氟硼酸盐([BMIm][BF₄])中,在热还原氧化石墨烯(TRGO)存在的情况下,对过渡金属脒基化合物(M{MeC[N(iPr)]₂} 或 [M(AMD)₃],其中M = Fe(II)、Co(II)、Pr(III))以及三(2,2,6,6-四甲基-3,5-庚二酮)铕(Eu(dpm))进行微波辅助热分解,获得了负载在不同类型热还原氧化石墨烯(TRGO)上的金属氟化物纳米颗粒(MFₓ-NPs,其中M = Fe、Co、Pr、Eu)。通过粉末X射线衍射(PXRD)确定在[BMIm][BF₄]中合成的金属氟化物的晶相,对于M = Fe、Co为MF₂,对于M = Eu、Pr为MF₃。MFₓ@TRGO的直径和尺寸分布为(6 ± 2)至(102 ± 41) nm。能量色散X射线光谱(EDX)和X射线光电子能谱(XPS)用于对MFₓ-NPs进行进一步表征。通过恒电流充放电曲线评估了FeF₂-NPs@TRGO作为锂离子电池阴极材料的电化学性能。结果表明,FeF₂-NPs@TRGO作为阴极材料在电流密度为50 mA/g时可呈现500 mAh/g的比容量,包括显著的界面电荷存储贡献。所获得的纳米材料在电流密度分别为200和500 mA/g时也显示出良好的倍率性能(分别为220 mAh/g和130 mAh/g)。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/1cba/5704767/7fde989968bc/Beilstein_J_Nanotechnol-08-2474-g006.jpg

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