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Cu&Si Core–Shell Nanowire Thin Film As High-Performance Anode applied sciences Article Cu&Si Core–Shell Nanowire Thin Film as High-Performance Anode Materials for Lithium Ion Batteries Lifeng Zhang 1, Linchao Zhang 1,*, Zhuoming Xie 1 and Junfeng Yang 1,2,* 1 Key Laboratory of Materials Physics, Institute of Solid State Physics, Hefei Institute of Physical Science, Chinese Academy of Sciences, Hefei 230032, China; [email protected] (L.Z.); [email protected] (Z.X.) 2 Lu’an Branch, Anhui Institute of Innovation for Industrial Technology, Lu’an 237100, China * Correspondence: [email protected] (L.Z.); [email protected] (J.Y.) Abstract: Cu@Si core–shell nanowire thin films with a Cu3Si interface between the Cu and Si were synthesized by slurry casting and subsequent magnetron sputtering and investigated as anode materials for lithium ion batteries. In this constructed core–shell architecture, the Cu nanowires were connected to each other or to the Cu foil, forming a three-dimensional electron-conductive network and as mechanical support for the Si during cycling. Meanwhile, the Cu3Si layer can enhance the interface adhesion strength of the Cu core and Si shell; a large amount of void spaces between the Cu@Si nanowires could accommodate the lithiation-induced volume expansion and facilitate electrolyte impregnation. As a consequence, this electrode exhibits impressive electrochemical properties: the initial discharge capacity and initial coulombic efficiency is 3193 mAh/g and 87%, respectively. After 500 cycles, the discharge capacity is about 948 mAh/g, three times that of graphite, corresponding to an average capacity fading rate of 0.2% per cycle. Keywords: lithium ion battery; anode; silicon; core–shell structure; magnetron sputtering Citation: Zhang, L.; Zhang, L.; Xie, Z.; Yang, J. Cu&Si Core–Shell Nanowire Thin Film as High-Performance Anode Materials 1. Introduction for Lithium Ion Batteries. Appl. Sci. Silicon (Si) has the highest known theoretical capacity of 4200 mAh/g, almost ten 2021, 11, 4521. https://doi.org/ times that of the currently used graphite anode, and is therefore being considered as the 10.3390/app11104521 most promising anode material for high-energy-density lithium ion batteries (LIBs) [1,2]. Unfortunately, Si suffers from as high as 300% volume change upon full (de)lithiation, Academic Editor: Francesco Enrichi inducing pulverization of the silicon particles and therefore losing electrical connectivity from the current collector and the thickening of the solid electrolyte interface (SEI) layer Received: 28 April 2021 upon cycling; these eventually hinder the practical application of Si-based anode materials Accepted: 10 May 2021 Published: 15 May 2021 in LIBs [3,4]. To tackle these issues, enormous attention has been directed towards the develop- Publisher’s Note: MDPI stays neutral ment of Si nanostructured materials [5], of which Si nanowires (SiNWs) have attracted with regard to jurisdictional claims in considerable interest owing to its small lithium diffusion length and facile strain relaxation published maps and institutional affil- during (de)lithiation [6,7]. However, the complete lithiation of Si nanowire impedes charge iations. transport in the longitudinal direction, limiting its rate performance [8]. Cui et al. success- fully synthesized a core–shell structured Si nanowire with a crystallite Si (c-Si) core and amorphous Si (a-Si) shell, in which the a-Si shell can be cycled alone as lithium ion storage whereas the c-Si core remains intact as mechanical sturdy support and efficient electron transport pathways by setting an appropriate cut-off potential owing to the higher lithiation Copyright: © 2021 by the authors. ∼ ∼ Licensee MDPI, Basel, Switzerland. potential of a-Si than c-Si ( 220 mV vs. 120 mV, respectively), resulting in significant This article is an open access article improvement in electrochemical performance over traditional Si nanowires, such as a high distributed under the terms and charge capacity of 1000 mAh/g and a capacity retention of 90% over 100 cycles [9]. On conditions of the Creative Commons the heels of this work, a series of core–shell nanowires with Si as the core and electron Attribution (CC BY) license (https:// conductive material as shell [10,11], or with Si as the shell and other electron conductive creativecommons.org/licenses/by/ materials as the core [12,13], also have been fabricated, contributing to great achievement 4.0/). in Si nanowire-based anodes. However, they not only involved high temperature, complex Appl. Sci. 2021, 11, 4521. https://doi.org/10.3390/app11104521 https://www.mdpi.com/journal/applsci Appl. Sci. 2021, 11, x FOR PEER REVIEW 2 of 10 Appl. Sci. 2021, 11, 4521 achievement in Si nanowire-based anodes. However, they not only involved high temper-2 of 9 ature, complex steps and the use of catalysts during preparation, but also have a low tap density when applied as an anode. Therefore, the Si core–shell nanowire-based anodes are relatively expensive to produce and hard to scale up. steps and the use of catalysts during preparation, but also have a low tap density when Alternatively, Si film anodes have also been studied since they are binder and con- applied as an anode. Therefore, the Si core–shell nanowire-based anodes are relatively ductive additive free. Ab-initio calculations suggested that the critical thickness of the sil- expensive to produce and hard to scale up. icon film to avoid crack is about 100 nm, beyond which the silicon film would fracture Alternatively, Si film anodes have also been studied since they are binder and conduc- and lead to rapid capacity fading [14]. Such a thin Si-film is not able to provide sufficient tive additive free. Ab-initio calculations suggested that the critical thickness of the silicon Si loading density for practical application [15]. By using a Si-based multilayer thin film, film to avoid crack is about 100 nm, beyond which the silicon film would fracture and with alternating layers of inactive materials as a buffer layer [16,17], its loading density lead to rapid capacity fading [14]. Such a thin Si-film is not able to provide sufficient Si can be increased but only to a very limited extent. loading density for practical application [15]. By using a Si-based multilayer thin film, with alternatingIn this study, layers to of combine inactive materialsthe advantage as a buffer of both layer a Si [ 16thin,17 film], its and loading core–shell density Si can nan- be owire,increased Cu@Si but core–shell only to a verynanowire limited thin extent. film (Cu&Si CSNWF) electrodes were fabricated throughIn thisslurry study, casting, to combine heat thetreatment, advantage and of magnetron both a Si thin sputtering. film and core–shell Subsequently, Si nanowire, their electrochemicalCu@Si core–shell properties nanowire were thin investigated film (Cu&Si in CSNWF) detail. In electrodes comparison were with fabricated other core through ma- terials,slurry the casting, Cu nanowire heat treatment, core has and obvious magnetron advantage sputtering. such Subsequently,as (1) higher electrical their electrochem- conduc- tivityical properties and fracture were toughness investigated [18]; (2) in detail.it is inactive In comparison to lithium withand thus other experiences core materials, no vol- the umeCu nanowirechange during core hasthe obviouslithiation/delithiation advantage such of Si; as and (1) higher(3) the Cu electrical nanowires conductivity we used andare commerciallyfracture toughness available [18]; and (2) itvery is inactive cheap in to price, lithium and and easy thus to experiencesbe scale up in no practical volume changeappli- cation.during the lithiation/delithiation of Si; and (3) the Cu nanowires we used are commercially available and very cheap in price, and easy to be scale up in practical application. 2. Materials and Methods 2.1.2. MaterialsCu@Si Core–Shell and Methods Nanowire Thin Film (CSNWF) Preparation 2.1. Cu@Si Core–Shell Nanowire Thin Film (CSNWF) Preparation Cu nanowires were purchased from Hongwu Nanometer Material CO., LTD.,Xu- zhou China.Cu nanowires Cu&Si CSNWFs were purchased were prepared from Hongwu by three Nanometer steps as schematically Material CO., illustrated LTD.,Xuzhou in FigureChina. 1. Cu&SiFirstly, CSNWFs2 mg Cu werenanowires prepared (CuNWs), by three as stepsreceived as schematicallywithout any pretreatment, illustrated in wereFigure uniformly1 . Firstly, dispersed 2 mg Cu nanowiresinto 10 mL (CuNWs), isopropa asnol received (IPA), and without then anythe pretreatment,slurry was casted were ontouniformly 50 μm-thick dispersed Cu foil, into followed 10 mL isopropanol by heating at (IPA), 280 °C and for then 2 h under the slurry the reductive was casted atmos- onto ◦ phere50 µm-thick of 5 v% Cu H2 foil, + 95 followed v% Ar to by evaporate heating at IPA 280 andC forreduce 2 h under the oxide the reductiveon the surface atmosphere of the CuNWs.of 5 v% H2As +a 95result, v% Arthe to Cu evaporate foil was IPAcoated and with reduce a layer the oxide of cross-linked on the surface CuNW of the sediment. CuNWs. Finally,As a result, the Si the layer Cu foilwas was deposited coated withonto athem layer without of cross-linked intentional CuNW heating sediment. or cooling Finally, to obtainthe Si Cu@Si layer wascore–shell deposited nanowire onto thin them films without by direct intentional current heatingmagnetron or coolingsputtering to obtainof the SiCu@Si target. core–shell The sputtering nanowire power thin is about films by120 direct W, the current distance magnetron of the target sputtering to the substrate of the Si istarget. about The50 mm sputtering and the power work pressure is about 120is about W, the 0.4 distance Pa. For ofcomparison, the target topure the Si substrate film was is about 50 mm and the work pressure is about 0.4 Pa. For comparison, pure Si film was simultaneously deposited on Cu foil and glass substrate, respectively, under the same simultaneously deposited on Cu foil and glass substrate, respectively, under the same sputtering parameter.
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