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1 Electronic Supplementary Information 5 An alternative hydrolytic synthesis route for uniform metal selenide nanoparticles Sandip Kumar Pahari, Provas Pal, Arka Saha, Sourindra Mahanty,* and Asit Baran Panda* 10 Experimental Materials: Zinc nitrate [Zn(NO 3 ) 2 6H 2 O], Cadmium nitrate [Cd(NO 3 ) 2 ], Indium nitrate [In(NO 3 ) 3,xH 2 O], Lead 15 nitrate [Pb(NO 3 ) 2 ], Copper nitrate [Cu(NO 3 ) 2 ], Decanoic acid [C 9 H 19 CO 2 H],Sodium borohydride [NaBH 4 ], metalic selenium powder [Se], methanol and deionized water. All the chemicals, were purchased from s.d. fine Chem., India and/or Sigma Aldrich, USA, and were used without further purification. 20 Synthesis: (a) Preparation of ZnSe: In a typical synthetic procedure, aqueous solution of 1.68 mmol (0.5 g) of zinc nitrate was added dropwiseto an aqueous saturated ammonium carbonate solution to make a clear solution of 10 ml zinc ammonium carbonate complex. Then, in a hot (~60 C) biphasic mixture of water (20ml) and decanoic 25 acid (33.48 mmol, 5.76 g to 11.6 mmol, 2 g), the prepared 10 ml zinc ammonium carbonate complex solution was added dropwise with constant stirring and a homogeneous and transparent solution resulted with the effervescence of carbon dioxide and ammonia (Solution-A) In a 50 ml beaker 1.68 mmol Selenium powder (0.31 g) was dispersed in 10ml deionised water and cooled in an ice bath mmol sodium borohydride was dissolved in 10 ml deionised water and 30 cooled in ice bath separately. Then, the sodium borohydride solution was added drop wise to the selenium dispersion and the mixture was kept in an ice bath. Gradually, the solution became clear with the formation of NaHSe (Solution -B). Next, solution-b was added drop wise to solution-a and quickly the mixture was transformed to a teflon lined 40 ml capacity autoclave and placed at a preheated oven at 150 C for 15 min to 4 hrs. 35 After the reaction, the autoclave was naturally cooled to ambient temperature. The final product was collected and washed with methanol for several time. (b) Preparation of CdSe: For the synthesis of CdSe, water solution of cadmium nitrate (1.88 mmol, 0.5gm) was added to a 40 concentrated solution of ammonium hydroxide to make a clear solution. After that, all the procedures are identical as detailed for the synthesis of ZnSe nanoparticle. (c) Preparation of In 2 Se 3 : In case of InSe, indium nitrate was added drop wise to an aqueous saturated ammonium carbonate 45 solution to make a clear solution. Then, a similar procedure to that for ZnSe was followed. However, in this case, the autoclave was heated at 180 C for 2 hrs.

2 (d) Preparation of CuSe: In a typical synthesis of CuSe, an aqueous solution of 1.68 mmol (0.5 g) of cooper nitrate was added drop wise to an aqueous saturated ammonium carbonate solution to make a clear solution. Then, a 5 similar procedure to that for ZnSe was followed. However, in this case, the autoclave was heated at 110 C for 1 hr. (e) Preparation of PbSe: In case of PbSe, lead nitrate was added drop wise to an aqueous sodium hydroxide solution to make a 10 clear solution. Then, a similar procedure to that for ZnSe was followed. However, in this case, the autoclave was heated at 140 C for 1hr. Formation mechanism: 15 Decanoic acid is not soluble in cold water (A). On heating (100 C), very little amount is soluble 20 in water (B). Addition of aqueous solution of metal nitrate salt to the aqueous solution of ammonium hydroxide or ammonium carbonate resulted in a basic clear solution by forming aqueous soluble metal ammonium or ammonium carbonate solution. After addition of the basic metal ammonium (Cd, Pb)/

3 ammonium carbonate(zn, In, Cu)complex solution to the bi-phasic aqueous decanoic acid solution in hot condition (B), decanoic acid solublized in the water through the formation of decanoate salt (C) with liberated ammoniaformed by decomposition of the complex in hot condition. The addition of reactive sodium hydrogen selenide (NaHSe) in that solution (C), metal selenide nanoparticles were 5 formed (D). The newly formed nanoparticles were stabilized by the water solubilized decanoate ion through the bi-dented coordination of carboxylate group of the acid with the metal ion of metal selenide. The formed decanoic acid stabilized metal selenide nanoparticles are hydrophobic, as layer of hydrophobic aliphatic chains are present in the outer surface of the particles. Thus, the nano particles are insoluble in water and separate out form the solution (D), and gave a perfect colloidal solution in 10 non polar solvent like toluene. Procedure for electrochemical measurements: 15 (a) Coin Cell Fabrication Electrochemical properties of the nano crystalline CuSe were evaluated in 2032 coin cells vs Li/Li +. A typical electrode was prepared from a slurry of CuSe powder (70wt%), acetylene black (20wt%) and PVDF binder (10 wt%) in n-methyl pyrrolidinone (NMP) solvent. The slurry was coated onto a 15 µm thick copper foil (current collector) and dried at 110 o C in an oven for 12 h. After 20 pressing the coated foil at 4.0 ton inch -2, circular disks of 16.3 mm in diameter were cut and used as electrode. Typical weight of the active material (excluding acetylene black and PVDF) was 5-6 mg type coin cells were assembled with these electrodes using Li metal as counter as well as reference electrode, LiPF 6 in EC: DMC (1:2 vol%) as electrolyte and Celgard 2300 as separator within an argon filled glove box (M BRAUN, Germany) where the moisture and oxygen levels were both 25 kept below 1.0 ppm. (b) Cyclic Voltammetry&Galvanostatic Charge-discharge Cyclic voltammetry of the cells was carried out by a galvanostat-potentiostat (Model: PGSTAT 30, Autolab, the Netherlands) between 0.01 and 3.0 V at a scanning rate of 0.1 mvs -1. Gavanostatic 30 charge-discharge measurements were carried out using an automatic battery tester (Model: BT2000, Arbin, USA) in the potential window of V with a constant current density of 50 mahg -1. Throughout the measurements, same current density was used for both charge and discharge. Specific capacities were defined as the values per unit weight of active material (excluding acetyl black and PVDF); discharge refers to the lithiation process of CuSe and charge refers to the corresponding de- 35 lithiation process

4 Supporting Figures: 5 Fig. S1: Histogram of particle size distribution of the 5 nm CdSe particle. 10 Fig S2 : Energy-dispersive X-ray spectroscopy (EDX) spectrum of CdSe. The spectrum shows that the compositional ratio of Cd and Se of synthesized particles is ~ 1 : 1.

5 Fig S3: FTIR spectrum of pure decanoic acid (a) and synthesized CdSe nano-particles in the presence of decanoic acid. 5 The spectra represent the coordination of decanoic acid with the surface of CdSe nanoparticle through a bi-dented coordination. In both the spectra, the bands due to C-H and C-C bond vibration of aliphatic chains of decanoic acid are identical. IR absorption band in the region originating from carboxyl group changes significantly in both the cases.. The sharp band as singlet at 1712 cm -1 of localized carbonyl group of 10 pure decanoic acid was replaced by the symmetric and asymmetric stretching vibrations of the carboxylate group (COO ) at 1533 and 1408, giving a splitting of γ = γ as γ s = 125 cm -1, in the decanoic acid modified CdSe nanoparticles. In case of mono-dentate coordination for carboxyl group, the ν as (COO )will be shifted to higher frequencies whereas ν s (COO ) will be shifted to lower frequencies. When the carboxylate group 15 (COO ) coordinate in a bi-dentate fashion, both the ν as (COO ) and ν s (COO ) frequencies will change in the same direction [1]. Because, in the latter case bond orders of both C=O bonds would change by the same amount. According to the obtained results, we can say that carboxylate group coordinate in a bi-dentate fashion with Cd of CdSe nanoparticles.

6 Fig S4: Combined UV-Vis absorption and corresponding PL spectra of CdSe nanoparticles synthesized by hydrothermal treatment for 1h (a), 2h (b), 4h (c), 6h (d).the photograph of the colloidal 5 solution in toluene of CdSe synthesized under varying hydrothermal treatment time is shoen in (e). Fig S5: XRD of synthesized CdSe nanoparticle at 150 C with different time interval.

7 Fig S6: TEM images of CdSe nanoparticles at 150 C at a) 30 min, b) 2hrs c) 8 hrs 5 Fig S7 : XRD ofznse (JCPDS ),CdSe (JCPDS ), InSe(JCPDS ), CuSe (JCPDS ) PbSe (JCPDS ) nanoparticles. 10 Fig S8: UV-Visabsorption spectra of ZnSe nanoparticle with increasing time.

8 Fig S9:Galvanostatic charge-discharge profiles for CuSe//LiPF6 in EC-DMC (1:2)//Li coin cell for the 5 first two cycles at a current density of 50 mahg -1. References: [1] McCarthy, K. Nakamato, P. J. McCarthy, Spectroscopy and Structure of Metal Chelate Compounds.New York, NY, USA: John Wiley & Sons; 1968.]

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