SEM results were collected with a JEOL microscope (model JSM-6700F). TEM images were collected from a JEOL microscope (model JEM-1400). EDS results were also obtained from the same model JEOL microscope with SEM tests. XRD patterns were collected with a D8 focus diffractometer (Bruker AXS, Germany). FTIR tests were carried out on a PerkinElmer 580B spectrophotometer made in the United States. XPS data were obtained from an X-ray photoelectron spectroscope (ESCALAB 250, ThermoFisher Scientific). The electrochemical tests (EIS and i–t) were tested on a Zahner electrochemical workstation (model Zennium PP211) with a three-electrode system. ZSimpWin software was used to fit the parameters for EIS data. PL spectra were obtained from a LS-45/55 spectrometer (PerkinElmer). UV–vis experiments were performed on a Lambda 35 UV–vis spectrometer (PerkinElmer).
D8 focus diffractometer
Manufactured by Bruker
Sourced in Germany, United States
The D8 FOCUS is a versatile X-ray diffractometer designed for phase identification, quantitative analysis, and material characterization. It features a fixed-slit optical geometry and provides high-quality diffraction data with excellent angular resolution. The core function of the D8 FOCUS is to enable precise measurement and analysis of crystalline materials.
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Lab products found in correlation
S 4800, by Hitachi (5 mentions)
Tecnai g2 s twin, by Thermo Fisher Scientific (4 mentions)
F 7000 spectrophotometer, by Hitachi (4 mentions)
Lambda 35 uv vis spectrometer, by PerkinElmer (3 mentions)
Escalab 250, by Thermo Fisher Scientific (3 mentions)
Escalab 250 system, by Thermo Fisher Scientific (3 mentions)
Zennium pp211, by Zahner (2 mentions)
Asap 2020, by Micromeritics (2 mentions)
Ascend 400, by Bruker (2 mentions)
Tga q5000, by TA Instruments (2 mentions)
Vertex perkin elmer 580bir spectrophotometer, by Bruker (2 mentions)
Tristar 3000, by Micromeritics (2 mentions)
Tecnai f20, by Thermo Fisher Scientific (2 mentions)
Su8010, by Hitachi (2 mentions)
580b ir spectrophotometer, by PerkinElmer (2 mentions)
K alpha spectrometer, by Thermo Fisher Scientific (2 mentions)
Jem 1400, by JEOL (1 mentions)
Jsm 6700f, by JEOL (1 mentions)
Asap 2010, by Micrometrics (1 mentions)
Zetasizer nano zs90, by Malvern Panalytical (1 mentions)
58 protocols using d8 focus diffractometer
1
Comprehensive Materials Characterization Protocol
2
Synthesis and Characterization of MOFs
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The synthesis of MOF-5 followed previous work with some modifications3 . Likewise, nano-sized Eu-MOF was synthesized according to the procedure of Choi et al.51 (link), while the blue uniform crystals of the MOF-199 were synthesized by following the procedure of Millward et al.52 (link).
The synthesized MOF products were characterized and verified by using PXRD (Bruker D8 Focus diffractometer), SEM (Mini-SEMSNE-4000M), and Attenuated reflectance method (ATR)-FTIR spectroscopy (PerkinElmer L1600400–IR spectrometer). A diffraction analysis was performed on a standard glass slide for background correction. The data were recorded over a 2θ range of 5–35°. Specific surface area and pore parameters were estimated from N2 adsorption/desorption isotherms at 77 K using a Micrometrics ASAP 2010. Prior to experiments, MOF samples were heated at 423 K for 8 h under a reduced pressure of 133.3 Pa to remove adsorbed water and gases. A detailed description of the synthesis of the MOFs is provided in the supporting information.
The synthesized MOF products were characterized and verified by using PXRD (Bruker D8 Focus diffractometer), SEM (Mini-SEMSNE-4000M), and Attenuated reflectance method (ATR)-FTIR spectroscopy (PerkinElmer L1600400–IR spectrometer). A diffraction analysis was performed on a standard glass slide for background correction. The data were recorded over a 2θ range of 5–35°. Specific surface area and pore parameters were estimated from N2 adsorption/desorption isotherms at 77 K using a Micrometrics ASAP 2010. Prior to experiments, MOF samples were heated at 423 K for 8 h under a reduced pressure of 133.3 Pa to remove adsorbed water and gases. A detailed description of the synthesis of the MOFs is provided in the supporting information.
3
Comprehensive Characterization of Graphene Oxide
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AFM images were recorded on MultiMode 8 AFM (Bruker, Bremen, Germany) in the tapping mode using a silicon cantilever for the geometry of individual GO nanosheets deposited on mica. SEM images were obtained by using a field emission SEM (Hitachi S-4800, Tokyo, Japan) with an acceleration voltage of 10 kV. Contact angle measurement was carried out on an OCA25LHT (Dataphysics, Filderstadt, Germany) instrument at room temperature. XRD patterns were collected on a Bruker D8 Focus diffractometer using an incident wavelength of 1.5418 Å (Cu Kα radiation). The zeta potential of GO colloids (0.1 mg mL−1) was measured with a Malvern Zetasizer NanoZS90.
4
Characterization of Functional Materials
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The X-ray diffraction (XRD) measurements were performed on a D8 Focus diffractometer (Bruker) with Cu Kα radiation (λ = 0.15405 nm). Transmission electron microscopy (TEM) was performed using FEI Tecnai G2 S-Twin with a field emission gun operating at 200 kV. Thermogravimetric and differential scanning calorimetry (TG-DSC) data were recorded with a Netzsch Thermoanalyzer STA 409 with a heating rate of 10 °C min−1 in N2 environment. UV-vis absorption spectra were measured by Beijing Pushi General Instrument Tu-1901. The PL measurements were performed with a Hitachi F-7000 spectrophotometer equipped with a 150 W xenon lamp as the excitation source. The mechanical properties of the film are tested by Universal testing machine (UTM4104). The luminescence decay curves were obtained from a Lecroy Wave Runner 6100 digital oscilloscope (1 GHz) using a tunable laser (pulse width = 4 ns, gate = 50 ns) as the excitation source (Continuum Sunlite OPO). The thickness of gelatin films was measured by a step profiler (AMBIOS, XP-100). The Fourier transform infrared (FTIR) spectra were recorded on a Nicolet 6700 spectrophotometer (USA) in the range of 4000–400 cm−1.
5
Comprehensive Materials Characterization Protocol
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The morphology of the samples was examined by using scanning electron microscopy (SEM, Hitachi S4800) with an accelerating voltage of 10 kV. The transmission electron microscopy (TEM) images were recorded on a JEOL JEM-2010EX transmission electron microscope with an accelerating voltage of 200 kV. The Fourier transform infrared (FT-IR) spectra were collected within the 400–4000 cm−1 spectral range on a Thermo Fisher Nicolet-6700 spectrometer. The X-ray powder diffraction (XRD) patterns from 5° to 80° were taken on a D8 Focus diffractometer (Bruker) with Cu target (40 kV, 40 mA). The X-ray photoelectron spectra (XPS) were obtained on an AXIS Ultra instrument from Kratos Analytical. The nitrogen adsorption–desorption isotherms were collected using a Micromeritics ASAP 2020 instrument. The specific surface areas were calculated using the Brunauer–Emmett–Teller (BET) method, and the pore size distributions were evaluated using the Barrett–Joyner–Halenda (BJH) model. The thermogravimetric analyses (TGA) were carried out using a TG/SDTQ600 instrument in atmosphere within temperature range of 0–900 K. The ultraviolet-visible (UV-vis) spectroscopy measurements were carried out with a UV-3600 UV-vis spectrophotometer (Shimadzu).
6
Powder X-ray Diffraction Analysis
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Powder X-ray diffraction data were collected on a Bruker D8 Focus diffractometer using a Cu X-ray source (Kα = 8.04 keV, 1.5406 Å). The step size for a 5–60°, 4 min scan is 0.018585749° using a LynxEye detector. The exact scan time is 4 min and 10 s, using 2961 steps at 0.08 s/step. Measurements were performed at room temperature. The simulated pXRD patterns shown in Fig. 3 and Fig. S5 (blue trace) were calculated using the Mercury 3.10 powder calculation function. The simulated wavelength was set to 1.54056 Å and the peak shape was calculated for a FWHM (2θ) equal to 0.1.
7
Structural Characterization by X-ray Diffraction
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The reaction progress was monitored using laboratory X-ray powder diffraction data collected at room temperature on a Bruker D8 FOCUS diffractometer (Cu Kα) over a 2θ range between 5° and 70°. Once the reactions were deemed finished, laboratory XRD data with much better statistical significance, covering a 2θ range between 5° and 110°, were collected from each sample to establish the sample purity. The high-resolution SXRD data were acquired at Beamline 11-BM at the Advanced Photon Source at Argonne National Laboratory at a wavelength of ~ 0.4590 Å. Detailed structural refinements were performed by the Rietveld method (35 ) using the GSAS-II program, with crystal structures visualized by the VESTA program.
8
Characterization of Metal-Organic Framework
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NMR spectra were recorded using a Bruker Ascend 400 (400.13 MHz for 1H) spectrometer. The proton chemical shifts of the samples were calibrated with respect to the reference proton resonance signals occurring from the protic residues of the deuterated solvents. The elemental composition of the MOF sample was analyzed at the Organic Chemistry Research Center (Seoul, Republic of Korea). Thermogravimetric analysis was carried out using a TGA Q5000 (TA Instruments, New Castle, DE, USA) under a nitrogen atmosphere (ramping rate = 15 °C min−1). PXRD spectra were recorded on a Bruker D8 Focus diffractometer (40 kV, 30 mA, step size = 0.02°). UV-Vis spectra were collected by a Scinco S-3100 spectrophotometer. Solid-state fluorescence spectra were collected using a Hitachi F-4500 fluorescence spectrophotometer. Gas chromatographic analysis was performed using a HP-5890 Series II gas chromatograph equipped with a flame ionization detector (FID) and a capillary column (Supelco SPB-1; L × I.D. 30 m × 0.25 mm, df 1.00 μm). The retention times of the desired products of transesterification were determined by using commercially available authentic samples, and n-nonane was used as an internal standard for quantification.
9
X-Ray Diffraction Characterization of Crystalline Phases
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The crystallographic phase was checked by performing X-ray diffraction experiments at room temperature on a Bruker D-8 Focus diffractometer (Lynseye 1D detector) with Ni-filtered CuKα1 radiation in the range from 30° to 60° (0.02° increments) in θ–2θ configuration.
10
Characterization of Graphene-Ethyl Cellulose Composite
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UV-Vis spectrophotometer (Evolution-300, Thermo Scientific) was used to measure the localized surface plasmon resonance (LSPR) absorption band of Gr-EC. The crystalline structure of Gr was measured by the Bruker D8-Focus diffractometer in the 2θ range of 10°–80° at a sweep rate of 0.5° min−1. The functional group of Gr with EC was investigated by Fourier transform-infrared (FT-IR) Type ALPHA II, Bruker. The stability of Gr-EC was estimated by thermal gravimetric analysis (TGA, 8000, PerkinElmer) in the range of 25–600 °C. The morphology of Gr-EC was characterized by transmission electron microscopy (TEM Tecnai G2S-Twin, Philips) and field emission scanning electron microscopy (FE-SEM, JSM-7000F). The elemental constitution was confirmed by X-ray photoelectron spectroscopy (XPS) Type (PHI 5000 Versa Probe III, Physical Electronics). The average height and average roughness of the Gr nanosheets were calculated by scanning probe microscope including atomic force microscopy (AFM, NT-MDT-INTEGRA). Laser micro Raman analysis was studied with Jobin Yvon Labram-010, in the 632.8 nm wavelength with a 1 μm2 spot size.
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