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Materials 2022, 15, x FOR PEER REVIEW 8 of 15 Materials 2022, 15, 6231 Materials 2022, 15, x FOR PEER REVIENWa2Te peaks remained. The NaGa4 phase partly disappeared when the electrod8e owf a1s5 the electrode was fully discharged (D: 5 mV), NaGa4 peaks were observed and Na2Te The reaction mechanism during the first sodiation/desodiation process of the Ga2Te3– TiO2–C(10%) electrode was investigated using ex situ XRD (Figure 4a,b). Peaks The reaction mechanism during the first sodiation/desodiation process of the Ga2Te3– corresponding to Na2Te and Ga were observed at a discharge voltage of 1.37 V (D: 1.37 TiO2–C(10%) electrode was investigated using ex situ XRD (Figure 4a,b). Peaks correspond- V). When the electrode was fully discharged (D: 5 mV), NaGa4 peaks were observed and ing to Na2Te and Ga were observed at a discharge voltage of 1.37 V (D: 1.37 V). When charged to 0.92 V (C: 0.92V). In a charging state of 1.72 V, the Na2Te phase partly peaks remained. The NaGa4 phase partly disappeared when the electrode was charged 7 of 15 disappeared, Ga was observed, and NaGa4 completely disappeared. Only the peaks to 0.92 V (C: 0.92 V). In a charging state of 1.72 V, the Na2Te phase partly disappeared, cGoarrwesapsoonbdsinergvteodG, an2Tde3NwaeGrea obcosemrvpeledtealgyaidniswaphpeneatrhede.leOctnrloydtehwe apsefauklslyccohrarergspedontodi2n.g5 4 The reaction mechanism during the first sodiation/desodiation process of the Ga2Te3– VtoG(aC:Te2.w5ereVo).bseGrav2eTde3agauindwerhgeonetshetehlectrfodlleowiansgfulslytruchctaurrgaeldtcoh2a.n5gVes(C:d2u.5rinVg). 23 TiO2–C(10%) electrode was investigated using ex situ XRD (Figure 4a,b). Peaks sGoadiTaetiounn/desrogdoieastitohne:following structural changes during sodiation/desodiation: 23 corresponding to Na2Te and Ga were observed at a discharge voltage of 1.37 V (D: 1.37 V). W1hsstetndiitshcehaearlregcetrode was fully discharged (D: 5 mV), NaGa4 peaks were observed and Na2Te peaks remained. The NaGa4 phase partly disappeared when the electrode was • Intercalation stage • Intercalation stage +− charged to 0.92 V (C: 0.92V). In a charging state of 1.72 V, the Na2Te phase partly Ga2Te3 + xNa + xe → NaxGa2Te3 (2.5−1.37 V). (i) Ga2Te3 + xNa+ + xe− → NaxGa2Te3 (2.5−1.37 V). (i) disappeared, Ga was observed, and NaGa4 completely disappeared. Only the peaks • Conversion stage −+−− correspondNiangGtao GTea2T+e3(6we)rNe oabs+er(v6edx)aegai→n w3NheanTthee+e2leGcatr(o1d.3e7w−a0s.5f2ulVly).cha(rigi)ed to 2.5 • C o n vx e r s 2i o n 3 s t a g e 2 V (C•: 2A.5lloyV)s.tagGe a2Te3 undergoes the following structural changes during NaxGa2Te3 + (6−) Na+ + (6−x)e− → 3Na2Te + 2Ga (1.37−0.52 V). (ii) +− sodiation/d4Gesao+diNataion+: e → NaGa4 (0.52−0.005 V). (iii) • Alloy stage 1ssttdcihsacrhgaerge +− 4•Ga +DNea-al+loey s→tagNe aGa4 (0.52−0.005 V). (iii) • Intercalation stage + - NaGa → 4Ga + Na + e (0.005−0.92 V). (iv) 1st charge 4 Ga2Te3 + xNa+ + xe− → NaxGa2Te3 (2.5−1.37 V). (i) • De-conversion stage • De-alloy stage − + 3Na Te+2Ga→Li Ga Te +(6 x)Na +(6 x)e (0.92−1.72V). • Conv2ersion stage x 2 3 • De-intercalation+ sta-ge − − (v) NaGa4 → 4Ga + Na + e (0.005−0.92 V). (iv) NaxGa2Te3 + (6−) Na+ + (6−x)e− → 3Na2Te + 2Ga (1.37−0.52 V). (ii) NaxGa2Te3 → Ga2Te3 + xNa+ +xe− (1.72−2.5 V). (vi) • De-conversion stage • Alloy stage ◦ It is noteworthy that, after the first cycle, the Ga Te phase (major peaks at 53.8 , −+−−23 3Na2Te + 2Ga → LixGa2Te3 + (6 x) Na + (6 x)e (0.92−1.72 V). (v) +− ◦4Ga + Na ◦+ e → NaGa4 (0.52−0.005 V). (iii) 69.4 , and 71.5 ) was completely recovered without any impurity peaks, showing a highly • De-intercalation stage rever1ssitbclehainrgteraction of Ga2Te3 with Na ions. The alloying/dealloying and conversion mechanismoftheGaTeelectrod+edu−ringcharge/dischargeisshownbytheexsituXRD NaxGa2Te3 → G2a2T3e3 + xNa +xe (1.72−2.5 V). (vi) • De-alloy stage results, as schematically depicted in Figure 4c. It is noteworthy that, after the first cycle, the Ga2Te3 phase (major peaks at 53.8°, 69.4°, NaGa4 → 4Ga + Na+ + e- (0.005−0.92 V). (iv) For the first, fifth, and 20th cycles, the EIS profiles of the Ga2Te3–TiO2–C(10%), Ga2Te3– and 71.5°) was completely recovered without any impurity peaks, showing a highly TiO –C(20%), and Ga Te –TiO –C(30%) electrodes were obtained (Figure 5). The simplified 2232 • De-conversion stage reversible interaction of Ga2Te3 with Na ions. The alloying/dealloying and conversion equivalent circuit shown in Figure 5d includes the electrolyte resistance (Rb), charge- mechanism of the Ga2Te3 electrode d−uring+char−ge/d−ischarge is shown by the ex situ XRD 3Na2Te + 2Ga → LixGa2Te3 + (6 x) Na + (6 x)e (0.92−1.72 V). (v) transfer resistance (Rct), SEI layer resistance (RSEI), interfacial double-layer capacitance results, as schematically depicted in Figure 4c. (C ), Warburg impedance (Z ), and constant phase element (C ). The R at the electrode– dl w PEct • De-intercalation stage electrolyte interface is denoted by compressed semicircles in the mid-frequency region NaxGa2Te3 → Ga2Te3 + xNa+ +xe− (1.72−2.5 V). (vi) of the Nyquist plot. For all the electrodes, Rct gradually decreased as the cycle number increIatsiesdnfortoemwo1rttoh2y0t.hGata, aTfete–rTthiOe f–irCs(t1c0y%cl)ee,xtheibGitae2dTteh3eplhoawses(tmvajlourepoefaRks atft5e3r.82°0,c6y9c.4le°s, 23 2 ct a(Tnadbl7e1S.58°)), dweamsocnosmtraptlienteglytheremcoovsetrfeadcilwe iNthaoiuotnatnraynsimpoprutarittiyonp, ewahkisc,hshleodwtiontghea hhigighhelsyt rNevaesrtsoirbalgeeinpteerrfaocrtmioancoef. Ga2Te3 with Na ions. The alloying/dealloying and conversion mechanism of the Ga2Te3 electrode during charge/discharge is shown by the ex situ XRD results, as schematically depicted in Figure 4c.PDF Image | Ga2Te3-Based Anodes for Sodium-Ion Batteries
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