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Inorganics 2017, 5, 25 Inorganics 2017, 5, 25 Inorganics 2017, 5, 25 8 of 17 8 of 17 8 of 17 Figure 8. (a) TEM image of a crystalline 6 μm-V2O5 prepared by solid state reaction; (b) needle-like Figure 8. (a) TEM image of a crystalline 6 μm-V2O5 prepared by solid state reaction; (b) needle-like α’-NayV2O5 synthesized via the hydrothermal route with ethanol as complexing reagent and (c) V2O5 α’-NayV2O5 synthesized via the hydrothermal route with ethanol as complexing reagent and (c) V2O5 film prepared by PLD technique with 80 nm grain size. film prepared by PLD technique with 80 nm grain size. Figure 9 shows the discharge curves of three LixV2O5//Li cells including the electrodes described Figure 8. (a) TEM image of a crystalline 6 μm-V2O5 prepared by solid state reaction; (b) needle-like above. The discharge profile of crystalline micron-sized LixV2O5 (1 μm-particle size) is rather Figure 9 shows the discharge curves of three LixV2O5//Li cells including the electrodes described α’-NayV2O5 synthesized via the hydrothermal route with ethanol as complexing reagent and (c) V2O5 complex, showing three plateaus due to the appearance of several structural phases: the α-phase is above. The discharge profile of crystalline micron-sized LixV2O5 (1 μm-particle size) is rather complex, film prepared by PLD technique with 80 nm grain size. formed at x < 0.01 followed by the ε-phase (0.35 < x < 0.7) and then the δ-phase. For further Li insertion, showing three plateaus due to the appearance of several structural phases: the α-phase is formed at x > 1, a permanent structural modification occurs leading to the γ-phase, which can be cycled in the Figure 9 shows the discharge curves of three LixV2O5//Li cells including the electrodes described x < 0.01 followed by the ε-phase (0.35 < x < 0.7) and then the δ-phase. For further Li insertion, x > 1, range 0 ≤ x ≤ 2 [28]. Bouhedja et al. [30] was the first group to show the reversible lithium intercalation above. The discharge profile of crystalline micron-sized LixV2O5 (1 μm-particle size) is rather a permanent structural modification occurs leading to the γ-phase, which can be cycled in the range within the α’-NayV2O5 nanoneedle structure. Similarly to V2O5, the quasi-1D, needle-like structure α’- complex, showing three plateaus due to the appearance of several structural phases: the α-phase is 0 ≤ x ≤ 2 [28]. Bouhedja et al. [30] was the first group to show the reversible lithium intercalation NayV2O5 exhibits a stepwise discharge behavior during the insertion of Li. Three well-defined regions formed at x < 0.01 followed by the ε-phase (0.35 < x < 0.7) and then the δ-phase. For further Li insertion, withintheα’-NaVO nanoneedlestructure.SimilarlytoVO,thequasi-1D,needle-likestructure are observed iyn t2he d5 ischarge curve of LixNaV2O5 in the range 02≤ x5≤ 2 (Figure 9). In this compositional x > 1, a permanent structural modification occurs leading to the γ-phase, which can be cycled in the α’-NadoVmaOin,tehxehdiibsicthsaargsetceuprwveisceordreiscphonardgsetobtehheavvoilotargdeuproinfigletcheariancsteritsitoicnooftfhLein.eTedhlree-leikwecerlyl-sdtaelfined y25 range 0 ≤ x ≤ 2 [28]. Bouhedja et al. [30] was the first group to show the reversible lithium intercalation associatedwiththeoccupationoftheoctahedralsitesbyLi.Thefirstregionextendsupto0.12e per regionsareobservedinthedischargecurveofLiNaVO intherange0≤x≤2(Figure9).Inthis within the α’-NayV2O5 nanoneedle structure. Similxarly to2V2O5 5, the quasi-1D, needle-like structure−α’- vanadium, the second one (with an S-shape behavior) up to 0.6 e− per vanadium, and the third one compoNsaiytVio2Ona5 el xdhoibmitsaians,tetphwe idseisdcihscahragregecbuerhvaevicoorrdruersipnognthdesintosetrhtioenvoflLtai.gTehrpereowfielell-cdhefairnaecdtreergisiotincs of the up to 1.0 e− per vanadium. Above x = 0.4 in LixNaV2O5, the voltage decreases smoothly down to 1.5 V are observed in the discharge curve of LixNaV2O5 in the range 0 ≤ x ≤ 2 (Figure 9). In this compositional needle-like crystal associated with the occupation of the octahedral sites by Li. The first region extends with a slope of 0.52 V·mol−1. From the electro-neutrality point of view, the intercalation of Li+ ions in domain−, the discharge curve corresponds to the voltage profile characteristic of the needle−-like crystal up to 0.12 e per vanadium, the second one (with an S-shape behavior) up to 0.6 e per vanadium, the LixNaV2O5 lattice should lead to the quantitative reduction of VV into VIV and VIII valence −states associatedwiththeoccupationoftheoctahedralsitesbyLi.Thefirstregionextendsupto0.12e per and the third one up to 1.0 e− per vanadium. Above x = 0.4 in LixNaV2O5, the voltage decreases giving the vanadium bronze Li2NaV2O5 [30]. From the structural− point of view, it may be inferred vanadium, the second one (with an S-shape behavior) up to 0.6 e per vanadium, and the third one smoothly down to 1.5 V with a slope of 0.52 V·mol−1. From the electro-neutrality point of view, that the fib−rous morphology of NaV2O5 needles allows fast Li+ ion diffusion in the solid phase. The upto1.0e pervanadium.Abovex=0.4inLixNaV2O5,thevoltagedecreasessmoothlydownto1.5V theintercalationofLi+ionsintheLiNaVO latticeshouldleadtothequantitativereductionofVV ewffeitcht aofsltohpeenoafn0o.s5t2ruVc·tmuorel−1i.sFcrloemarltxyheveliedc2etnroc5-endeuintrtahlietydpisocihnatrogfevciuewrv,ethoef iPnLteDrcVal2aOti5ofnilomf Leil+eciotrnosdiens. intoVIVandVIIIvalencestatesgivingthevanadiumbronzeLiNVaVOIV[30].IFIIromthestructural FtohresLmixaNllapVa2rOti5claetsticze,sthhoeufldreeleGadibtbostehneeqrugaynotiftVat2iOve5 nreadnuocstirounctoufrVe2dignrtaoi2nVs5isarnedmVarkvabaleynmceosdtiaftiesd; pointthgouifvsvi,nitgehwethm,eiotvdmainfaiaeydibuGemibinbfsreoernrzeerdgLytih2pNaluatVsth2tOhee5fip[b3r0re]os.euFnsrcomemoftrhapmehsotrlpuohcgtoyurosaflgprNaoiainVtboOuf nvdineaewrei,edistlepmsroavylildboewaisnsffmearsoretodLthi+ ion ++ dtihscahtathrgeefipbrofuislemfrormph3o.l5ogtoy0o.f5NVavVs2.OL5in/Leei°dlienstahlelowhsoflaestLLixiV2iOon5 cdoifmfupsoiosnitiionnth(0e≤soxli≤d2p)haasseth.eThcell diffusion in the solid phase. The effect of the nanostructure is clearly evidenced in the discharge curve peoftfenctioafl Vth(ex)niasntohsetrduecrtiuvraetiivsecl∂ea(rΔlGy )e/v∂idx.enced in the discharge curve of PLD V2O5 film electrodes. of PLD V2O5 film electrodes. For small particle size, the free Gibbs energy of V2O5 nanostructured For small particle size, the free Gibbs energy of V2O5 nanostructured grains is remarkably modified; grains is remarkably modified; thus, the modified Gibbs energy plus the presence of amorphous grain thus, the modified Gibbs energy plus the presence of amorphous grain boundaries provide a smooth boundaries provide a smooth discharge profile from 3.5 to 0.5 V vs. Li+/Li◦ in the whole LixV2O5 discharge profile from 3.5 to 0.5 V vs. Li+/Li° in the whole LixV2O5 composition (0 ≤ x ≤ 2) as the cell composition (0 ≤ x ≤ 2) as the cell potential V(x) is the derivative ∂(∆G)/∂x. potentialV(x)isthederivative ∂(ΔG)/∂x. 25 Figure 9. Discharge profiles of LixV2O5 electrodes recorded at room temperature at C/48 rate in Li cells with 1 mol·L−1 LiClO4 in PC as electrolyte. Figure 9. Discharge profiles of LixV2O5 electrodes recorded at room temperature at C/48 rate in Li cells Figure 9. Discharge profiles of LixV2O5 electrodes recorded at room temperature at C/48 rate in Li with 1 mol·L−1 LiClO4 in PC as electrolyte. cells with 1 mol·L−1 LiClO4 in PC as electrolyte.PDF Image | Nanotechnology of Positive Electrodes for Li-Ion Batteries
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