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Inorganics 2017, 5, 25 9 of 17 3.2.2. Manganese Dioxide Inorganics 2017, 5, 25 9 of 17 Cryptomelane α-MnO2 polymorph is an attractive electrode material for lithium batteries due toits3.2lo.2w.Mcaonstg,aennesveirDoinomxidenetalfriendlinessandnaturalabundancebutsuffersfromlowelectronic conductivity [31,32]. Nanotechnology has recently been employed as another route to enhance the Cryptomelane α-MnO2 polymorph is an attractive electrode material for lithium batteries due to electrochemical properties of MnO2 cathode materials for rechargeable batteries [33–35], so that its low cost, environmental friendliness and natural abundance but suffers from low electronic capacities of ca. 250 mAh·g−1 can be reached [36]. Nanostructured LixMnO2 with with 2 × 2 tunnels conductivity [31,32]. Nanotechnology has recently been employed as another route to enhance the isastablematerialoverawiderangeoflithiationconcentration.α-MnO canbeusedasacathode electrochemical properties of MnO2 cathode materials for rechargeable b2atteries [33–35], so that +0 or ancaopdaecitnietshoefpcao.t2e5n0timalArha·nggeca3n.5b–e1.r5eaVchaendd[316.5].–N0aVnovsst.ruLcitu/reLdi L,irxeMspnOec2twiviethlyw. Sitehv2er×a2l tsutundneielsigsave −1 evidaenstcaebloefmthaeteirmiapl ovrtearnacweiodfeinrasnegrteeodfcliathtiioantisonfocronencehnatnractinong.sαtr-MucntOur2aclanstabbeiulisteydoafsαa-McatnhOode[3o7r,38]. 2 Theasntroudcetuinretshteabpiolitzenatiaolnrbanygtehe3.c5h–1e.m5iVcaalninds1e.r5t–io0nVovfst.wLoiL/Lii-i,ornespecrtiuvneliyt.cSeellv,etrhaulstiumdpiersovgainvgethe +0 evidence of the importance of inserted cations for enhancing structural stability of α-MnO2 [37,38]. initial discharge capacity, has been demonstrated by Kijima et al. [37] during cycling. Stable cycling The structure stabilization by the chemical insertion of two Li-ions per unit cell, thus improving the performance of α-MnO2 has also been reported for samples prepared by hydrothermal–electrochemical initial discharge capacity, has been demonstrated by Kijima et al. [37] during cycling. Stable cycling synthesis [39]. Due to the renewed interest of α-MnO2, we investigated the structural stability of its performance of α-MnO2 has also been reported for samples prepared by hydrothermal– lithiated phase in the potential range 3.5–1.5 V vs. Li+/Li0, when prepared as nanoneedles after the electrochemical synthesis [39]. Due to the renewed interest of α-MnO2, we investigated the structural reduction of KMnO4 by the ascorbic acid (AA) route, and nanowires prepared by the mixed chelator stability of its lithiated phase in the potential range 3.5–1.5 V vs. Li+/Li0, when prepared as (MC). Detailed XRD patterns are reported in Figure 4. nanoneedles after the reduction of KMnO4 by the ascorbic acid (AA) route, and nanowires prepared The galvanostatic discharge–charge profiles of Li//α-MnO2 cells are characterized by the by the mixed chelator (MC). Detailed XRD patterns are reported in Figure 4. following features: (i) the first cycle is dominated by a distinct irreversible capacity loss The galvanostatic discharge–charge profiles of Li//α-MnO2 cells are characterized by the C ≈35mAh·g−1 for both materials; (ii) the degree of crystallinity affects the shap−e1 of lossfollowing features: (i) the first cycle is dominated by a distinct irreversible capacity loss Closs ≈ 35 mAh·g dischfoarrgboet–hchmaartgeeriaplsr;o(fiiil)etsh;e(idiie)grteheodficsrcyhsatarlglieniatyndaffcehctasrgtheepshlatpeeauofsdairsechcalregaer–lcyhaorbgseeprvroefdileisn;(hiiig)hly crystahlelidziesdchMarCge-MandOchasragmeplea,tewauhsilaertehceledairslychoabrsgeerv–ecdhainrgheigchulryvcersysAtaAll-iMzendOMCd-MispnlOay2 samraptlhee,rwSh-islheape 22 the discharge–charge curves AA-MnO2 display a rather S-shape characteristic of a disordered characteristic of a disordered material. The initial discharge capacity of AA-MnO2 sample is materia−l.1The initial discharge capacity of AA-MnO2 sample−i1s 245 mAh·g−1, larger than that of the 245 mAh·g , larger than that of the MC-MnO2 (214 mAh·g ). This can be attributed to the smaller MC-MnO2 (214 mAh·g−1). This can be attributed to the smaller size of the particles of the AA-MnO2 size of the particles of the AA-MnO2 that results in an increased effective interface between the that results in an increased effective interface between the material and the electrolyte, but as soon as material and the electrolyte, but as soon as the second cycle is finished, the situation is reverse. the second cycle is finished, the situation is reverse. Figure 10 presents the Peukert plots of Figure 10 presents the Peukert plots of nanostructured α-MnO2 electrodes, i.e., the specific capacity as nanostructured α-MnO2 electrodes, i.e., the specific capacity as a function of the rate capability for −1 a function of the rate capability for discharge–charge current density in the range from 10 to 400 mA·g discharge–charge current density in the range from 10 to 400 mA·g−1 (1C = 260 mA·g−1). These results (1C = 260 mA·g−1). These results shows the better electrochemical performance of MC-MnO2 that shows the better electrochemical performance of MC-MnO2 that provides evidence of the importance provides evidence of the importance of its synthesis recipe. of its synthesis recipe. Figure 10. Peukert plots of the nanostructured α-MnO2 electrodes prepared by different wet-chemical Figure 10. Peukert plots of the nanostructured α-MnO2 electrodes prepared by different wet-chemical methods: single and mixed chelators. 3.3. Olivine-Like Materials LiMPO4 (M = Fe, Mn) olivine materials used as electrodes of high-power sources (in hybrid electric vehicles, for instance) request an increase of rate capability that could be achieved by reducing methods: single and mixed chelators.PDF Image | Nanotechnology of Positive Electrodes for Li-Ion Batteries
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