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Elucidating the Impact of Cobalt Doping on the Lithium

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Elucidating the Impact of Cobalt Doping on the Lithium DOI:10.1002/celc.201600179 Articles Elucidating the Impact of Cobalt Doping on the Lithium Storage Mechanism in Conversion/Alloying-Type Zinc Oxide Anodes Franziska Mueller,[a, b, c] Dorin Geiger,[d] UteKaiser,[d] Stefano Passerini,*[a, b] and Dominic Bresser*[a, b, e] Herein, an in-depthinvestigation of the influence of transition- in situ electrochemical XRD analysisofthe first de-/lithiation of metal doping on the structural and electrochemical character- ZnO and Zn0.9Co0.1Orevealed the highly beneficial impact of istics of ahybrid conversion/alloying-typelithium-ionanode the transition-metal dopant on the reversible degradation of materialispresented. Therefore, pure zinc oxide (ZnO) and lithium oxide (Li2O) and suppression of zinc crystallite growth cobalt-doped ZnO (Zn0.9Co0.1O) were investigated comparative- upon lithiation;both effects are essential for greatlyimproved ly.Characterization by using X-ray diffraction (XRD), scanning electrochemical performance. As aresult, Co doping leads to 1 electron microscopy (SEM), and transmission electron micros- asubstantially increasedspecific capacityfrom 326 mAhgÀ 1 copy (TEM) confirmedthe successful incorporation of the for pure ZnO to 789 mAhgÀ for Zn0.9Co0.1Oafter 75 full cobalt (Co) dopant into the wurtzite ZnO structure, which led charge–discharge cycles. to adecreased particlesize for the doped compound. The 1. Introduction Despite great technological interestinnanostructured zinc this inferiorelectrochemical performance of ZnO-based electro- oxide (ZnO) for alarge variety of applications, such as light- des, Pelliccione and co-workers[6] very recently performed an emitting diodes,[1] gas sensors,[2] or dye-sensitized solar cells,[3] in situ X-ray absorption fine structure (XAFS) spectroscopy their investigation as lithium-ion anode materials has been re- study.Itwas found that this substantial capacity decay mainly ported rather scarcely to date. In fact, although atheoretical originates from the formation of relatively large metallic zinc 1 specific capacity of about 988 mAhgÀ (if the reaction ZnO+ particles upon continuous de-/lithiation. Once the size of these + 3Li +3eÀ LiZn+ Li Oisconsidered to be fully reversible) particles exceeds acertain limit, the formation of ZnO accom- $ 2 certainly arouses interest, apart from afew outstanding excep- paniedbythe degradationofLi2O, that is, the conversion reac- tions[4] most electrochemical studies revealed poor per- tion, shows no further reversibility and only the alloying reac- formance and rapid capacity fading.[5] To explain the origin of tion of zinc with lithium takes place reversibly, which, in turn, is associated with the characteristic issues of alloyingmateri- als.[5f] [a] F. Mueller,Prof. Dr.S.Passerini, Dr.D.Bresser Helmholtz Institute Ulm (HIU) In addition, the large volume changes upon alloying–deal- Helmholtzstrasse 11,89081, Ulm (Germany) loying lead to pulverization of the active material, ongoing E-mail:[email protected] electrolyte decomposition, and finally the loss of electrical con- [email protected] tact within the composite electrode.[5f] Additionally,the de- [b] F. Mueller,Prof. Dr.S.Passerini, Dr.D.Bresser crease in electronic conductivity within the electrode owing to Karlsruher Institute of Technology(KIT) P.O. Box 3640, 76021Karlsruhe (Germany) the insulating nature of Li2Opresumably contributes to the ob- [6] [c] F. Mueller served rapid capacity fading. We have recently reported that Institute of Physical Chemistry these challenges and, in particular,the reversibility of the con- University of Muenster version reactioncan be substantially enhanced by introducing Corrensstrasse 28/30, 48149 Muenster (Germany) atransition-metaldopant into the metal oxide structure.[7] This [d] Dr.D.Geiger, Prof. Dr.U.Kaiser new conceptfollowsthe general approach of introducing CentralFacility for Electron Microscopy Group of Electron Microscopy of Materials Science ametallic element that does not alloy with lithium once re- [8] University of Ulm duced to the metallicstate, whichthusensuresasufficient 89081 Ulm (Germany) electron supply throughout the initial particles to enable the [e] Dr.D.Bresser degradation of Li2O. However,little is knownsofar about the DRF/INAC/SYMMES/PCI detailedreaction mechanism of this new class of conversion/al- CEA, UMR-5819, CEA-CNRS-UJF 17 Rue des Martyrs, 38054 Grenoble (France) loying materials. The ORCID identification number(s) for the author(s) of this article can Herein, we present an in-depth structuraland electrochemi- be found under http://dx.doi.org/10.1002/celc.201600179. cal characterization of pure ZnO and Co-doped ZnO nanoparti- ChemElectroChem 2016, 3,1311–1319 1311 2016 Wiley-VCH Verlag GmbH &Co. KGaA, Weinheim Articles cles by using XRD, SEM,TEM, cyclic voltammetry (CV), and gal- (Rockwood Lithium, battery grade) as the counter and reference vanostatic cycling techniques. Moreover,weperformed acom- electrodes. The electrodes were separated by astack of polypropy- parativeinsitu XRD analysis of Co-doped and pure ZnO nano- lene fleeces (Freudenberg FS 2190), drenched with a1m solution particles. The obtained results, which are also discussed with of LiPF6 in amixture of ethylene carbonate/diethyl carbonate (UBE; 3:7wt/wt). Because metallic lithium foil was used as the counter respecttoour previousfindings for Fe-doped ZnO,[7a] provide and reference electrodes, all potential values given herein refer to an enhanced understanding of the advantageous impact of the Li/Li + redox couple. Cyclic voltammetry and galvanostatic cy- the transition-metal dopant on the reversibility of the de-/lith- cling were performed by using aVMP3 potentiostat (BioLogic) and iation mechanism in generaland the conversion reaction in aMaccor Battery Tester 4300, respectively.All electrochemical stud- particular. In fact, doping ZnO with cobalt resultsinasubstan- ies were conducted at (20 2)8Cinapotential range of 0.01–3.0 V. Æ tially enhanced specific capacity and cycling stabilityofnano- particulate ZnO-based lithium-ion anodes. In situ XRD Analysis In situ XRD analysis of Co-doped and pure ZnO nanoparticles upon Experimental Section galvanostatic de-/lithiation was conducted by using aself-designed two-electrode in situ cell.[9] Electrodes were prepared analogously Materials Synthesis to those used for the electrochemical characterization, with an For the synthesis of Co-doped ZnO nanoparticles, stoichiometric overall composition of 65 wt%active material, 25 wt%conductive amounts of zinc(II) gluconate hydrate and cobalt(II) gluconate hy- carbon, and 10 wt%CMC. The resulting mixture was dispersed by drate (both from ABCR) were dissolved in deionized water.The re- planetary ball-milling and cast onto aberyllium (Be) disk (thickness: sulting solution, with atotal metal ion concentration of 0.2m,was 250 mm, Brush Wellman) that served concurrently as the current added dropwise under vigorous stirring to aqueous sucrose (1.2m; collector and “window” for the X-ray beam. The coated Be disk ACROS ORGANICS). After continuous stirring for an additional was dried for 30 min at 80 8Cunder ambient atmosphere and sub- 15 min at RT,the solution was heated to about 1608Ctoremove sequently at 408Cunder vacuum overnight. Metallic lithium foil the water.Concurrently,the sucrose started to become thermally served as the counter electrode. Twosheets of Whatman glass decomposed. The remaining solid precursor was further dried at fiber drenched with asolution of LiPF6 (1m,500 mL) in ethylene around 3008C, then ground and calcined for 4h under air at carbonate/diethyl carbonate (UBE;3:7 wt/wt) were used as separa- 1 tor.The assembled cell was allowed to rest for 10 hprior to the 4008C(heating rate:38CminÀ ). Pure ZnO nanoparticles were pre- pared by following an analogous synthesis protocol in the absence in situ XRD measurements. Simultaneous galvanostatic cycling was of the Co precursor and using an annealing temperature of 450 C. performed by using aVSP potentiostat/galvanostat (BioLogic) and 8 1 applying aspecific current of 55 (Zn Co O) or 60 mAgÀ (ZnO) 0.9 0.1 and setting the cut-off potentials to 0.01 or 3.0 V. The XRD analysis Morphological and Structural Characterization was carried out in a2q range of 25–808 with astep size of 0.027588 and atime per step of 0.65 s. Consequently,every scan Powder X-ray diffraction (XRD) patterns were recorded by using lasted exactly 30 min, which included an initial rest step of 419 s. aBRUKER D8 Advance with CuKa1 radiation (l=154 pm) and astep size of 0.00928.Scanning electron microscopy (SEM) was carried out by using aZEISS LEO 1550VP field emission electron micro- 2. Results and Discussion scope. All samples were sputtered with platinum to prevent charg- 2.1. Structural and Morphological Characterization ing effects. High-resolution transmission electron microscopy (HRTEM)was performed by using aPhilips CM 20 at 200 kV for The X-ray diffractionpatterns of pure ZnO and Zn0.9Co0.1O, pre- Zn0.9Co0.1Onanoparticles samples deposited on acopper grid sented in Figure 1, show the characteristic pattern of hexago- coated with aholey carbon film. nal-wurtzite-structuredZnO with the P63mc space group (JCPDS file card no. 01-071-6424), which indicates thesynthesis Electrochemical Characterization of phase-pure materials and the successful doping of ZnO with cobalt.The additional low-intensity reflectionsatabout 28.7, Electrodes were prepared by dissolving sodium carboxymethyl cel- 31.1, and 32.78 (marked by *) originate from the diffractionof lulose (CMC, WALOCELTM
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