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Production of Uniformly Sized Gallium-Based Liquid Alloy Nanodroplets Via Ultrasonic Method and Their Li-Ion Storage

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Production of Uniformly Sized Gallium-Based Liquid Alloy Nanodroplets Via Ultrasonic Method and Their Li-Ion Storage materials Article Production of Uniformly Sized Gallium-Based Liquid Alloy Nanodroplets via Ultrasonic Method and Their Li-Ion Storage Chenghao Huang 1 , Junjie Zong 1, Xiaodong Wang 1, Qingpin Cao 1, Dongxian Zhang 1,2 and Jian-Zhong Jiang 1,* 1 International Center for New-Structured Materials (ICNSM), Laboratory of New-Structured Materials, State Key Laboratory of Silicon Materials, School of Materials Science and Engineering, Zhejiang University, Hangzhou 310027, China; [email protected] (C.H.); [email protected] (J.Z.); [email protected] (X.W.); [email protected] (Q.C.); [email protected] (D.Z.) 2 State Key Laboratory of Modern Optical Instrumentation, Zhejiang University, Hangzhou 310027, China * Correspondence: [email protected] Abstract: Gallium-based liquid alloys are attractive due to their unique properties, and they can potentially be applied in the field of flexible electronics as coolant materials for nuclear and liquid batteries, due to the high thermal conductivity and excellent fluid properties of liquid metals. However, it is still challenging to fabricate gallium-based liquid alloy nanodroplets with uniform and small size. Here, we performed a systematical study on the influence of various factors affecting the size of nanodroplets. Liquid metal nanodroplets with an average size of 74 nm and narrow size distribution were successfully fabricated. Li-ion half-cells were assembled with eutectic GaIn (eGaIn) nanodroplets as anode active materials, which showed higher specific capacity than the bulk eGaIn alloy under the same testing conditions. Keywords: Ga-based liquid alloys; nanodroplets; ultrasonic technique; surfactant; centrifugation; Citation: Huang, C.; Zong, J.; Wang, X.; Cao, Q.; Zhang, D.; Jiang, J.Z. Li-ion battery Production of Uniformly Sized Gallium-Based Liquid Alloy Nanodroplets via Ultrasonic Method and Their Li-Ion Storage. Materials 1. Introduction 2021, 14, 1759. https://doi.org/ The concept of liquid alloys has a long history [1]. Generally speaking, in the periodic 10.3390/ma14071759 table of elements, post-transition elements, zinc group elements and their alloys, and Group IA elements and their alloys belong to this kind of emerging materials, such as Ga, Academic Editor: Masato Sone GaIn, Hg, NaK, etc. They have both metallic and liquid properties, such as fluidity, high conductivity, and high thermal conductivity. Compared with amalgam [2] and alkali metal Received: 28 February 2021 elements, gallium-based alloys have attracted much attention due to their low toxicity, low Accepted: 31 March 2021 volatility, and biocompatibility. At present, nanostructured gallium-based liquid alloys, Published: 2 April 2021 e.g., nanodroplets, have many applications in the fields of reconfigurable electronics, soft robotics, and conformable medical devices [3–5]. For example, it has been proved that Publisher’s Note: MDPI stays neutral adriamycin (DOX)-treated ultrasonic gallium-based alloy nanodroplets can be used for with regard to jurisdictional claims in tumor-targeted therapy and enhance the chemotherapy efficacy of tumor-bearing mice [6]. published maps and institutional affil- iations. In addition to biomedical applications, nanodroplets of gallium and its alloys are often used in sensor devices to increase the surface to volume ratio for significant improvement of the sensitivity [7]. Although gallium-based alloy nanodroplets have many applications, the issue of how to prepare these nanodroplets or even high-quality nanodroplets (uniform narrow Copyright: © 2021 by the authors. size distribution and small average size below 100 nm) is still challenging. Microfluidics Licensee MDPI, Basel, Switzerland. produced uniform liquid alloy microdroplets [8–11], but with limited effects on the size This article is an open access article of liquid alloy droplets [12]. Physical vapor deposition was also used to prepare liquid distributed under the terms and conditions of the Creative Commons alloy nanodroplets on various substrates. The most common strategy is to disperse bulk Attribution (CC BY) license (https:// liquid alloys to micro or nano scale by an ultrasonic technique in an appropriate solvent creativecommons.org/licenses/by/ with surfactants. Hohman et al. found that ultrasound treatment could effectively emulsify 4.0/). liquid metal, and assist the formation of liquid metal nanodroplets through sulfhydryl Materials 2021, 14, 1759. https://doi.org/10.3390/ma14071759 https://www.mdpi.com/journal/materials Materials 2021, 14, x FOR PEER REVIEW 2 of 11 Materials 2021, 14, 1759 2 of 11 emulsify liquid metal, and assist the formation of liquid metal nanodroplets through sulfhydryl self-assembly [13]. Finkenauer et al. studied the effects of solvents and self-assemblysurfactants on [ 13the]. Finkenauerformation and et al. stability studied theof gallium effects of-based solvents alloy and nanodroplets surfactants onin thean formationultrasonic andmethod, stability and offound gallium-based that ethanol alloy and nanodroplets octadecanethiol in an were ultrasonic better method,choices [14]. and foundHowever, that ethanolthe nanodroplets and octadecanethiol obtained by were these better methods choices are [14 still]. However, large in thesize, nanodroplets and highly obtaineduneven with by thesea wide methods size distribution. are still large in size, and highly uneven with a wide size distribution.In this work, the effects of various factors on the preparation of gallium-based alloy nanodropletsIn this work, by an the ultrasonic effects of various method factors will be on systematically the preparation investigated, of gallium-based especially alloy nanodropletsultrasonic amplitude, by an ultrasonic time, and method surfactant will be systematicallyconcentration, investigated,among other especially factors. ul-In trasonicaddition, amplitude, eutectic GaIn time, (eGaIn) and surfactant nanodroplets concentration, can be applied among as other active factors. electrode In addition,material eutecticfor Li-ion GaIn batteries (eGaIn) owing nanodroplets to their high can theoretical be applied capacity as active and electrode self-healing material properties for Li-ion as batteriescompared owing with to bul theirk higheGaIn theoretical liquid. capacityThus, a andhalf self-healing-cell Li-ion properties battery using as compared eGaIn withnanodroplets bulk eGaIn prepared liquid. here Thus, was a half-cell assembled, Li-ion which battery shows using average eGaIn nanodropletsdischarge specific pre- pared here was assembled, which shows average discharge specific capacity of 582.6 and capacity of 582.6 and 379.6 mAh g−1 at a current density of 0.1 and 3.0 A g−1, respectively, 379.6 mAh g−1 at a current density of 0.1 and 3.0 A g−1, respectively, which is much better which is much better than bulk eGaIn. than bulk eGaIn. 2. Materials and Methods 2.1. Synthesis of Eutectic GaIn Nanodroplets For the preparation of a eutectic GaIn alloy (eGaIn, 85.8 at.% Ga and 14.2 at.% In), purepure galliumgallium andand indiumindium withwith puritypurity higherhigher thanthan 99.9999.99 at.%at.% werewere used.used. TheThe mixturesmixtures ofof purepure galliumgallium andand indiumindium were were sealed sealed in in quartz quartz tubes tubes under under a vacuuma vacuum of of ~5 ~5× ×10 10−−44 Pa andand heated at 250 ◦°CC for aa fewfew hourshours untiluntil completecomplete meltingmelting inin aa thermostaticthermostatic oiloil bath.bath. AfterAfter melting, thethe alloys alloys were were cooled cooled to roomto room temperature temperature and and transferred transferred into sealedinto seal vialsed using vials ausing plastic a transferplastic transfer pipette forpipette further for use. further The second use. The step second is to prepare step is eGaIn to prepare nanodroplets. eGaIn Innanodroplets. this process, 0.2In gthis of eGaIn process alloy, 0.2 and g 20 of mL eGaIn surfactant alloy solution and 20 (octadecanethiol mL surfactant dissolved solution into(octadecanethiol ethanol) are droppeddissolved into into a ethanol) 25 mL beaker. are dropped Nitrogen into gas a was25 mL used beaker. to remove Nitro oxygengen gas forwas 5 used min to remove improve oxygen combined for 5 efficiency min to improve between combined ligand andefficiency liquid between alloy. Then, ligand eGaIn and alloyliquid was alloy. synthesized Then, eGaIn into nanoparticlesalloy was synthesized by performing into ultrasonication nanoparticles withby performing the Sonics Vibra-Cellultrasonication Ultrasonic with Processor the Sonics VCX 750Vibra (Sonics&Materials-Cell Ultrasonic Inc, Newton,Processor MA, VCX USA) 750 for different(Sonics&Materials times (1, 2,Inc 4,, 6,Newton and 12, MA, h). Ultrasonication USA) for different processor times was (1, operated2, 4, 6, and at 75012 W,h). 20Ultrasonication kHz, and different processor amplitudes was operated (30%, 40%,at 750 and W, 50%20 kHz, of the and maximum). different amplitudes In the ultrasonic (30%, process,40%, and an 50% ice of bath the wasmaximum). used to In mitigate the ultrasonic the temperature process, an fluctuation. ice bath was The used final to solutionmitigate wasthe temperature centrifuged tofluctuation. remove the The surfactant final solution and dropped was centrifuged onto a silicon to remove wafer. Thethe surfactant synthesis processand dropped of eGaIn on nanodropletsto a silicon bywafer. sonicating The synthesis the bulkeGaIn process alloy of precursor eGaIn nanodroplets is schematically by illustratedsonicating inthe Figure bulk 1eGaIn. alloy precursor is schematically illustrated
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