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1 Supporting Information Activating Room Temperature Long Afterglow of Carbon Dots via Covalent Fixation Kai Jiang,, Yuhui Wang, Congzhong Cai, and Hengwei Lin*, Key Laboratory of Graphene Technologies and Applications of Zhejiang Province, Ningbo Institute of Materials Technology & Engineering (NIMTE), Chinese Academy of Sciences, Ningbo 31521, China. State Key Laboratory of Coal Mine Disaster Dynamics and Control, Department of Applied Physics, Chongqing University, Chongqing 444, China. *Correspondence and requests for materials should be addressed to H.L. ( Experimental section Materials Reagent grade of m-phenylenediamines (mpd) was purchased from Aldrich. Colloidal nanosilica (i.e. nsio 2 ) (LUDOX TMA colloidal silica, 34 wt% suspension in H 2 O, ph=4~7) was provided from Sigma-Aldrich. Ethanol, methanol, methylene chloride, polyethylene glycol (PEG) (Mw=1) and poly(vinyl alcohol) (PVA) (Mw=175±5) were provided by Sinopharm Chemical Reagent Co., Ltd. (Shanghai, China). All chemicals were used as received without further purification unless otherwise specified. Deionized (DI) water was used throughout this study. 1 / 9
2 Equipments and characterization Transmission electron microscopy (TEM) observations were performed on a Tecnai F2 microscope. Fourier transform infrared (FT-IR) spectra were obtained on a Nicolet 67 FT-IR spectrometer. XPS were carried out with ESCALAB 25Xi (Thermo Scientific). Photoluminescence, afterglow emission and excitation spectra (phosphorescence mode) were measured on a Hitachi F-46 spectrophotometer at ambient conditions. For the temperature-dependent experiment, the sample was placed in a high temperature fluorescence attachment (Orient KOJI, TAP-2) with temperatures controlled between and K. The UV-vis absorption spectra were recorded on a PERSEE T1CS UV-Vis spectrophotometer. PL and afterglow lifetimes were measured using Fluorolog 3-11 (HORIBA Jobin Yvon). Photographs of PL, RTP and RTDF were taken using a Canon camera (EOS 55) under excitation by a hand-hold UV lamp (365 nm). Preparation of m-cds, m-cds@nsio 2 and corresponding inks Synthesis of m-cds: mpd (.9 g) was dissolved in 9 ml of ethanol, and then these solution was transferred into poly(tetrafluoroethylene)-lined autoclaves. After heating at 18 ºC in oven for 12 h and cooling down to room temperature naturally, gray suspension was obtained. The crude product was followed purification with a silica column chromatography using mixtures of methylene chloride and methanol as eluents. After removing solvents and further drying under vacuum, the purified m-cds could be finally obtained in 8-15 wt% yields. Preparation of m-cds@nsio 2 :.15 g (or.6,.3,.75, and 1.5 g) nsio 2 solution were firstly diluted with 9 ml DI water and mixed with 1. ml of m-cds solution (1. mg/ml in ethanol). The mixture was then transferred into poly(tetrafluoroethylene)-lined autoclaves. After heating at 18 ºC in oven for 12 h and cooling down to room temperature naturally, the resulting bluish green suspension was centrifuging at 2 rpm for 3 min to remove the solvent. The final products were collected after twice washing with ethanol to remove unreacted m-cds, and the precipitates were re-dissolved in water for further use. The m-cds@nsio 2 powders can be simply obtained through drying the ethanol-washed precipitates. Phosphorescence ink (a typical formulation): 2 µl of m-cds solution (5. mg/ml in ethanol) were firstly diluted with 3 µl DI water, and then mixed with 1.5 ml of PVA (Mw=175±5) 2 / 9
3 solution (1. g in 15 ml water). Such obtained PVA solutions are employed as luminescent inks to prepare PVA films or write on filter paper directly. Delayed fluorescence ink: 2 µl of m-cds@nsio 2 solution (5 mg/ml in ethanol) were firstly diluted with 3 µl DI water, and the following process was the same as the preparation of phosphorescence emissive inks. Fluorescence ink: 2 µl of m-cds solution (5. mg/ml in ethanol) were firstly diluted with 3 µl DI water, and then mixed with 1.5 ml of PEG (Mw=3) solution (1. g in 5 ml water). Such obtained PEG solutions are employed as PL inks to write on filter paper directly. Supporting Figures and Tables a) PL PHs m-cds@nsio 2-1:2 m-cds@nsio 2-1:5 m-cds@nsio 2-1:1 m-cds@nsio 2-1:25 m-cds@nsio 2-1: m-cds@nsio 2-1:2 m-cds@nsio 2-1:5 m-cds@nsio 2-1:1 m-cds@nsio 2-1:25 m-cds@nsio 2-1: Figure S1. The PL a) and afterglow emission spectra of m-cds@nsio 2 prepared with different ratios of m-cds to nsio 2 by weight (i.e. 1:2, 1:5, 1:1, 1:25, 1:5, respectively) with the excitation of 365 nm. 3 / 9
4 5 nm Figure S2. TEM image of the nsio 2. a) m-cds C1s Raw data Fitted line Background ev C-C/C=C ev C-N/C=N ev C-O m-cds N1s Raw data Fitted line Background ev pyridinic N 399. ev amino N 4.2 ev pyrrolic N c) Binding Energy (ev) m-cds@nsio 2 C1s Raw data Peak Background ev C-Si ev C-C/C=C ev C-N/C=N ev C-O d) m-cds@nsio 2 N1s Binding Energy (ev) Raw data Peak Background ev N-Si ev pyridinic N ev amino N 4.8 ev pyrrolic N Binding Energy (ev) Binding Energy (ev) Figure S3. The high resolution XPS spectra of C1s and N1s of m-cds (a, and m-cds@nsio 2 (c,d), respectively. 4 / 9
5 PL Figure S4. PL emission spectra of m-cds@nsio 2 in water dispersions under air (black line) and argon (red line) conditions (excitation of 365 nm). Air Ar PL IRF m-cds@nsio 2 Fitted Line Time (ns) τ avg = 7.56 ns Figure S5. PL decay spectrum and fitting curves of the m-cds@nsio 2 in water dispersion. 5 / 9
6 K K K K K K K K Time (s) Figure S6. Afterglow decay profiles of the m-cds@nsio 2 (powder) at K. Table S1. Afterglow lifetimes of the m-cds@nsio 2 (powder) at different temperatures. T [K] τ 1 [ms] B 1 [%] τ 2 [ms] B 2 [%] τ 3 [ms] B 3 [%] τ avg [ms] ϕ Nor. Em Intensity nm 58 nm Phos (77K) FL (77K) Figure S7. The low temperature (77K) fluorescence (red curve) and phosphorescence (black curve) spectra of m-cds@nsio 2 under excitation at 365 nm. 6 / 9
7 a) 12 TADF K nm 519 nm TADF K nm 515 nm c) d) e) g) 6 TADF K nm 518 nm TADF K nm 519 nm f) 2 TADF K 462 nm 514 nm TADF K nm 516 nm TADF K nm 518 nm Figure S8. The afterglow emission spectra of m-cds@nsio 2 (powder) at different temperatures and the Gaussian fitted by two emission peaks. Table S2. The relative contents of the two peaks for the m-cds@nsio 2. T [K] λ em [nm] B 1 [%] λ' em [nm] B 2 [%] / 9
8 a) Decay Fit Decay Fit Time (s) Time (s) Figure S9. The afterglow emission decay spectra and fitting curves of m-cds@sio 2 at 461 nm (a) and 518 nm ( under excitation at 365 nm. Table S3. Fitting results of the afterglow lifetimes of the m-cds@nsio 2 at 461 nm and 518 nm under 365 nm excitation. Emission (nm) τ 1 (ms) B 1 (%) τ 2 (ms) B 2 (%) τ 3 (ms) B 3 (%) τ avg (ms) ϕ Abs (a.u) Abs of m-cds Abs of m-cds@nsio 2 RTDF Ex Figure S1. Absorption spectra of m-cds (black line), m-cds@nsio 2 (red line) dispersed in ethanol, and RTDF excitation spectrum of m-cds@nsio 2 (blue line) dispersed in ethanol. 8 / 9
9 Absorbtion m-cds-t m-cds Wavenumber (cm -1 ) Figure S11. FT-IR spectra of m-cds, and m-cds after a treatment with light irradiation (365 nm) during air bubbling for 6 hours (named m-cds-t). a) Dry wet Dry wet Figure S12. RTP and RTDF spectra of (a) m-cds-pva and ( m-cds@sio 2 -PVA films before and after damped by water vapours; all measurement was carried out on phosphorescence mode. 9 / 9
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