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Silicon Nanopillar Anodes for Lithium-Ion Batteries Using Nanoimprint Lithography with Flexible Molds Eric Mills, John Cannarella, Qi Zhang, Shoham Bhadra, Craig B

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Silicon Nanopillar Anodes for Lithium-Ion Batteries Using Nanoimprint Lithography with Flexible Molds Eric Mills, John Cannarella, Qi Zhang, Shoham Bhadra, Craig B Silicon nanopillar anodes for lithium-ion batteries using nanoimprint lithography with flexible molds Eric Mills, John Cannarella, Qi Zhang, Shoham Bhadra, Craig B. Arnold, and Stephen Y. Chou Citation: Journal of Vacuum Science & Technology B 32, 06FG10 (2014); doi: 10.1116/1.4901878 View online: http://dx.doi.org/10.1116/1.4901878 View Table of Contents: http://scitation.aip.org/content/avs/journal/jvstb/32/6?ver=pdfcov Published by the AVS: Science & Technology of Materials, Interfaces, and Processing Articles you may be interested in In situ cycling and mechanical testing of silicon nanowire anodes for lithium-ion battery applications Appl. Phys. Lett. 100, 243901 (2012); 10.1063/1.4729145 Fabrication of silicon template with smooth tapered sidewall for nanoimprint lithography J. Vac. Sci. Technol. B 29, 06FC16 (2011); 10.1116/1.3662094 High aspect ratio fine pattern transfer using a novel mold by nanoimprint lithography J. Vac. Sci. Technol. B 29, 06FC15 (2011); 10.1116/1.3662080 Sub- 200 nm gap electrodes by soft UV nanoimprint lithography using polydimethylsiloxane mold without external pressure J. Vac. Sci. Technol. B 28, 82 (2010); 10.1116/1.3273535 Silicon nanowires for rechargeable lithium-ion battery anodes Appl. Phys. Lett. 93, 033105 (2008); 10.1063/1.2929373 Redistribution subject to AVS license or copyright; see http://scitation.aip.org/termsconditions. Download to IP: 128.112.142.131 On: Tue, 30 Dec 2014 22:19:15 Silicon nanopillar anodes for lithium-ion batteries using nanoimprint lithography with flexible molds Eric Mills NanoStructure Laboratory, Department of Electrical Engineering, Princeton University, Princeton, New Jersey 08544 John Cannarella Department of Mechanical and Aerospace Engineering, Princeton University, Princeton, New Jersey 08544 Qi Zhang NanoStructure Laboratory, Department of Electrical Engineering, Princeton University, Princeton, New Jersey 08544 Shoham Bhadra and Craig B. Arnold Department of Mechanical and Aerospace Engineering, Princeton University, Princeton, New Jersey 08544 Stephen Y. Choua) NanoStructure Laboratory, Department of Electrical Engineering, Princeton University, Princeton, New Jersey 08544 (Received 5 September 2014; accepted 4 November 2014; published 19 November 2014) The lithium ion battery, a preferred energy storage technology, is limited by its volumetric and gravimetric energy densities, as well as its capacity retention with prolonged cycling. In this work, the authors exploited the extremely high lithium storage capacity of Si as an anode material and tackled the issue of lithium-induced volume expansion by patterning the Si into a nanopillar array using nanoimprint lithography and reactive-ion etching. Arrays of 200 nm-pitch Si pillars of 50–70 nm diameter and 200–500 nm height were fabricated on stainless steel substrates, assembled into coin cells, and tested against lithium counter electrodes. Initial charge capacities in excess of 3000 mAh/g, and a low rate-dependence, were obtained with these Si pillar anodes. This represents an improvement over previously reported nanoimprint-patterned Si anodes. Though this initial capacity is roughly equivalent to previously reported values for bulk Si anodes, our nanopillar ano- des exhibit far superior capacity retention with subsequent charge–discharge cycles. VC 2014 American Vacuum Society.[http://dx.doi.org/10.1116/1.4901878] I. INTRODUCTION integrity is compromised during battery cycling. For the pop- ular Si nanowire-based anode, first demonstrated by Cui The lithium ion battery has become the energy storage me- 9 dium of choice for almost all applications requiring recharge- et al. in 2008, this critical radius has been shown to be on the order of 300 nm for initially crystalline Si.8 Randomly able batteries, due to its favorable performance characteristics relative to other rechargeable battery chemistries.1,2 However, packed nanowire systems are also popular because they do for applications with size and weight constraints, such as elec- not require binders or conductive additives (which reduce energy density), and they have intrinsic free space to accom- tric vehicles, it is still necessary to achieve significant increases in energy density. Consequently, the development of modate volumetric expansion of the Si electrode material battery electrode materials with higher lithium storage capaci- during lithiation. The accommodation of volumetric expan- sion is critical for reducing mechanical stress in the individ- ties has remained an area of intense research. One promising anode material is silicon, which shows theoretical Li-storage ual structures as well as stress within the cell as a whole, which can lead to overall cell degradation.10 A number of specific charge capacities of 3600 mAh/g (Ref. 3)atroom deposition-based methods have been used to create viable temperature, nearly 10Â that of current commercial anodes, 11 which are typically graphite (372 mAh/g).4 Si anodes made Si Nanowire (NW) anodes, including thin film deposition, creation of random wire networks,12 and coating existing from 45 lm-sized powders have shown initial capacities of 13 5 fibers with Si via chemical vapor deposition (CVD). nearly 4000 mAh/g, though anodes made from such “bulk” 6 Etching-based fabrication techniques, involving chemical Si typically lose 80%–90% of their capacities with 5 cycles. 14 15 This rapid degradation is due to the 310% volume expansion7 etching or deep reactive ion etching, have also been implemented, often in combination with self-assembled col- that occurs during lithiation, resulting in rapid capacity losses 14 due to mechanical pulverization of the electrode. loidal monolayers to create patterns. Random nanowire net- To prevent Si pulverization, it has been widely accepted works, such as those grown by CVD, typically show NWs growing in many directions12,16 and are thus extremely ineffi- that Si electrodes must be nanostructured, as Si systems ex- hibit a critical “cracking radius,”8 above which structural cient at filling volume. To efficiently fill volume, NWs with well-defined diameter, pitch, and orientation are required. Nanoimprint lithography (NIL), in combination with a)Electronic mail: [email protected] appropriate deposition and etching techniques, is an ideal 06FG10-1 J. Vac. Sci. Technol. B 32(6), Nov/Dec 2014 2166-2746/2014/32(6)/06FG10/5/$30.00 VC 2014 American Vacuum Society 06FG10-1 Redistribution subject to AVS license or copyright; see http://scitation.aip.org/termsconditions. Download to IP: 128.112.142.131 On: Tue, 30 Dec 2014 22:19:15 06FG10-2 Mills et al.: Silicon nanopillar anodes for lithium-ion batteries 06FG10-2 way to generate precisely ordered arrays of wires with mini- Inc.) PFPE was chosen due to its low surface energy, high mal defects.17 In addition, soft-mold NIL’s compatibility elastic modulus, and impressive solvent resistance.22 Ather- with roll-to-roll processes,18 and ability to produce patterns mal nanoimprint was conducted at <80 C and 200 psi using on substrates too rough for standard “hard-mold” NIL, make a Nanonex, NX-2500 nanoimprinter. it the perfect candidate for creating such patterns on rela- In step (3), the trilayer was etched using reactive ion etch- 19 tively “rough” metal substrates. To our knowledge, only ing (RIE) (PlasmaTherm, 720 SLR), with O2 (10 sccm, two previous attempts to apply NIL to the realm of nanopat- 3 mTorr, 50 W) for the residual imprint resist, CF4/H2 19,20 terned Si Li-ion battery anodes have been published. In (33/7 sccm, 50 mTorr, 300 W) for the SiO2 layer, and O2 this paper, we aimed to improve the specific charge capacity (10 sccm, 3 mTorr, 100 W) for the XHRiC polymer layer. of nanostructured Si electrodes fabricated via NIL by apply- E-beam evaporation of 25 nm Cr was then performed, fol- ing High-Fidelity Flexible Mold (HiF2M) NIL technology to lowed by liftoff of the trilayer in RCA1 (5:1:1 DI H2O:29% the production of Si nanopillars. Nanopillar structures are NH4OH:30% H2O2) solution. Si etching was accomplished preferable to those previously fabricated by NIL (nanobars with a pseudo-Bosch process (PlasmaTherm, 720 SLR), and nanoporous Si) due to their smaller size and greater sur- using an SF6/O2/H2/Ar recipe adapted from Mohajerzadeh face area, and are expected to exhibit excellent performance et al.,23 (17/2.5/7.5/0.5 sccm, 10 mTorr, 200 W, 9 s) with a at high cycling rates, as well as good tolerance of the CHF3 passivation step (20 sccm, 100 mTorr, 90 W, 15 s). A mechanical stresses imposed by lithiation.21 minimum 25% overetch was used, as residual Si would arti- ficially inflate capacity results. To obtain accurate values for Si loading, some samples were soaked in chromium-etchant II. EXPERIMENT (Cyantek, CR7), which dissolves enough underlying Cr in A. Fabrication of Si nanopillar anodes the substrate to knock over wires without damaging them. The fabrication has three key steps: (1) Si film deposition, These wires were examined via scanning electron micro- (2) nanoimprint lithography and metal liftoff, and (3) Si pillar scope (SEM) (Zeiss, Leo 1550), and the images were ana- etching (Fig. 1). In step (1), 1.5 in. diameter #8 polished stain- lyzed using ImageJ software. The examinations show that less steel disks (Stainless Supply) were cleaned ultrasonically fabricated pillars have heights between 200 and 500 nm, and in toluene, rinsed with isopropanol, dried with N2,andfinally widths between 30 and 75 nm. Pillars show a slight undercut cleaned in O2 plasma to remove any residual organics and from etching, which was accounted for during pillar volume enhance adhesion. E-beam evaporation of Si was then per- calculations. formed at <1 Â 10À5 Torr, at a rate of 6nm/min. In step (2), a trilayer of nanoimprint resist, consisting of B. Assembly of anodes 150 nm thermally cross-linking polymer (XHRiC 16, The cell preparation and assembly process has four key Brewer Sciences), 10 nm e-beam evaporated SiO2 (99.99%, steps: (1) transfer to an Ar-filled glovebox, (2) Li-disk prepa- Kamis Inc.), and 130 nm thermal imprint resist (NXR-1025, ration, (3) separator preparation, and (4) final assembly.
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