Readme.txt - Summary of data in repository for: Tuning room-temperature phosphorescence from carbon dots in inorganic crystalline nanocomposites Repository author: David C. Green, ORCID:0000-0002-0578-2369, email: chmdcg@leeds.ac.uk Compiled 31st May 2018 File name and contents: SEM_raw.zip - Scanning electron micrographs in tif format of crystals produced under the conditions described. pXRD_raw.zip - Powder X-ray diffractograms obtained by pXRD, data given in raw and excel-ready formats Confocal_raw.zip - Raw confocal fluorescence microscopy data, format usable in ImageJ or Fiji FLIMPLIM_raw.zip - All raw fluorescence and phosphorescence lifetime imaging data obtained from CLF at didcot under proposal 17330015. Data readable in FlimFIT Spectroscopy_raw.zip - Raw steady-state photoluminescence spectroscopy, phosphorescence spectroscopy and UV-Vis spectroscopy. Files can be opened in Origin. Contains raw and background deleted data sets. Videos_raw.zip - Videos obtained at 25 fps with an SLR Canon camera. Openable in VLC and extractable in VeeDub. Raman_raw.zip - Raw Raman spectroscopy data openable in excel and Renishaw's Wire software package. TRPM_raw.zip - All raw time-resolved phosphorescence micoscopy data obtained from CLF at didcot under proposal 17330015. Data readable in ImageJ. FTIR_raw.zip - raw fourier transform infra-red spectra of carbon dots and raw component molecules. *** Details: Raman microscopy Raman microscopy was conducted on calcite samples grown on glass substrates using a Renishaw inVia Raman Microscope (785 nm laser) with a 50x objective using MS20 encoded sample stage control through rollerball XYZ peripheral. Data acquisition was undertaken with Renishaw WiRE 3.4 with a laser intensity of 0.1% under 3 accumulated acquisitions (3 x scan time 30 s) between 1200 to 100 cm-1. All spectra saved as .txt files (x = wavelength in nm, Y = intensity in a.u.) as exported from Renishaw WiRE 3.4; importable into Microsoft Excel. Powder X-ray diffraction (XRD) Powder XRD was conducted on a Bruker D2 Phaser with a LYNXEYE detector for phase confirmation studies. Dry powdered samples were deposited onto a silicon substrate as dried powder or from ethanolic suspension. Data was obtained between 2? = 5 and 95° over 20 min, with the smallest possible step size, on spinning samples. All data acquisition, instrument control and data conversion was conducted in DIFFRAC.SUITE software package. Patterns saved as manufacturer-specific .brml and .raw files, openable in Bruker DIFFRAC.SUITE software; or .xy files (X = 2theta degrees, Y = intensity in counts per second cps); Importable into Microsoft Excel. Scanning electron microscopy (SEM) SEM was conducted on FEI NanoSEM Nova 450 from samples grown directly on clean glass substrates. Samples were mounted on aluminium stubs with double sided Cu tape, with tape folded to a portion of the top surface of the substrate to minimise charging. All samples were coated with 2 nm Ir conductive layer prior to analysis. Images saved in TIFF format; openable in a wide range of image viewing and editing software. Confocal fluorescence microscopy (CFM) CFM was conducted on Zeiss LSM510 Upright Confocal Microscope using samples grown directly on clean glass substrates under oil immersion where required. Laser and imaging settings were controlled with Zeiss ZEN software (excitation laser at 405 nm, emission low pass filter from 440 nm). Images saved as .czi; openable with Zeiss ZEN software or open-source Fiji (Fiji Is Just ImageJ) software with suitable plugin for compatability with .czi files. Image analysis For all confocal fluorescence and SEM micrographs, rendering and analysis was conducted in ImageJ or Fiji applet. For confocal fluorescence microscope z-stacks, optical images were taken from the central most plane. Fluorescence confocal micrographs were obtained by forming a z-projection for z-stacks. Surface images, as viewed from various angles, were obtained by rendering confocal fluorescence z-stacks into 3D, and rotating the rendered image manually. All plots are prepared in Windows Excel and Origin Pro, before being exported as .emf or wmf for use in figure design software such as Serif DrawPlus. These files can be found in various zip folders. Steady-state photoluminescence (SS-PL) spectroscopy Steady-state photoluminescence spectra (excitation and emission) were obtained from diluted CD solution and solid powders using a Jobin Yvon Horiba FluoroMax-3 fluorescence spectrometer operated by FluorEssence (v3.5) software. Powdered samples were prepared for fluorescence spectroscopy by mixing phosphorescent powders with grease and smearing onto a glass substrate. PL spectra of grease and glass slide were used as background signals. Background subtraction was essential due to high amounts of scattered light. CD solutions were diluted until optimal signal was obtained at emission maxima. Quartz fluorescence vials were used for obtaining data. Spectra saved in .opj format, openable in Origin or Origin Pro.(X = wavelength, Y = intensity) Phosphorescence spectroscopy Phosphorescence (dark-state) spectra were obtained using Ocean Optics 2000+ interfacing fibre optic signal inlet to a Sony ILX511B CCD detector with Overture (v1.0.1) software control. Powdered samples were prepared as above, and excited with an Applied Photophysics 150 W shuttered xenon arc lamp. Excitation light (360 nm) was filtered with a Comar Optics 360-50 band pass filter (band width between 300 and 400 nm, asymmetric transmittance peak centred on 360 nm). Data was transferred directly into Windows Excel and saved as .xslx (X = wavelength, Y = intensity) UV-Vis Absorbance spectroscopy Absorption spectra of aqueous CD solutions were obtained on a Perkin-Elmer Lambda 35 spectrometer in a quartz cuvette, against a water blank. Spectra were obtained between 200 and 700 nm at 240 nm/min, with 1 nm intervals. Data acquisition, instrument control and automatic background deletion was handled by the UV WinLab software. Data was saved as instrument-specific .sp files, and converted to Excel-importable .csv files (X = wavelength (nm), Y = intensity. Fourier transform infra-red spectroscopy (FTIR) FTIR spectra were obtained with Perkin-Elmer Spectrum 100 with ATR accessory and sample mounting. Spectra were obtained across 650 to 4000 cm-1 at 1 cm-1 intervals, accumulated over 4 runs. Data acquisition, instrument control and automatic background deletion was handled by the Spectrum software. Data was saved as instrument-specific .sp files, and converted to Excel-importable .csv files (X = wavelength (nm), Y = transmission (%)). Video stroboscopy Videos of RTP composites were obtained with Canon EOS 7D SLR camera in video mode (25 fps) with manual focus and manual exposure settings; with a Canon EF 100mm f/2.8 Macro USM lens. Photoluminescence was stimulated with a Spectroline UV lamp (6 W. longwave 365 nm), and shuttered manually. Video processing was conducted in VirtualDub 1.10.4 (64-bit) for frame isolation and image sequence generation, followed by image analysis and recomposition in ImageJ 1.46r. These videos were used for low resolution stroboscopy. Stroboscopic data was obtained by plotting mean grey values against time with a 0.04 s interval, with lifetimes (t) obtained using Origin Pro 8. Time-resolved phosphorescence microscopy (TRPM) High resolution stroboscopic studies, at a time interval of 5 ms, were conducted using a Nikon Eclipse Ti optical microscope (40x quartz objective) with a sCMOS (Hamamatsu ORCA-Flash4.0) controlled by the MicroManager 1.4 software suite. Powders for afterglow nanocomposites were deposited onto a glass coverslip, and illuminated with an LED (40 µW illumination at sample, 340 nm LED with condenser from ThorLabs, powered by either ThorLabs LED driver LEDd1b, set at 0.7 A maximum for continuous illumination; or Thandar TG501 function generator set with a 0.5 or 0.25 Hz squarewave for light/dark measurements). Image analysis was conducted in ImageJ, where stroboscopic data was extracted from individual images as absolute intensity values. Lifetimes and pre-exponential factors (a) were obtained using Origin Pro 8. Pre-exponential factors indicate the proportion of the decay curve which is calculated to have the corresponding lifetime in a multiexponential plot, and are expressed as a percentage. Here, it is referred to as “x% of the decay signal” or “proportion of the decay curve”. Data was saved as .tiff stacked images, openable in ImageJ. Plot values for intensity vs time were exported as .xls Microsoft Excel files. Fluorescence and Phosphorescence Lifetime Imaging Microscopy (FLIM/PLIM) FLIM/PLIM was performed using a Nikon Eclipse Ti optical microscope with a Becker and Hickl DSC-120 dual channel confocal scanning head and an SPC-150 time correlated-single photon counting controller, using Becker and Hickl in-house software (v 9.77 in 64-bit). All data was obtained in Fifo mode, with both picosecond and microsecond decay traces per pixel. Afterglow nanocomposites were grown directly onto glass slides from conditions as stated above, and imaged with a 60x water immersion objective. Nanocomposites were excited with a two-photon process via a Coherent Mira 700F, (pumped by a 10 W Verdi CW laser at 532 nm) at 730 nm with variable power and monitored using a Thorlabs silica diode power meter. A Tektronix TDS 3052B Oscilloscope was used to monitor the output of the Ti:Sapphire laser. All data was analysed using a Becker and Hickl image analysis software suite, SPCimage, version 6, or using FlimFit 5.0.3. All lifetime and pre-exponential factors values were taken from the brightest regions of each crystal. All files were saved as instrument-specific .sdt files, openable in B&H Spsm64 software. Each file was uncompressed in B&H software to larger .sdt files, openable in open-source FlimFIT software package.