supplementary materia data.docx
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Powder X-ray diffraction (XRD) data were collected in the 3-70° range by the D8 Advance diffractometer (Bruker., Germany) with Cu Kα radiation at 0.02°step size and 5°/min scanning rate. Single crystal was extracted from the precipitates of MOF 1 and MOF 2, respectively. Single crystal XRD data were recorded using D8 Quest diffractometer (Bruker., Germany) at 273 K. Data collection was carried out using the BluIce software suite with processing undertaken in XDS program. Analysis and refinements of the crystal structures were carried out using direct method with the help of SHELXTL software. All non-hydrogen atoms were resolved using anisotropic correction. Fourier transform infrared (FTIR) spectrometer (Nicolet 6700, USA) was used to record FTIR spectrum of samples. An appropriate amount of ground MOF samples was placed in the photoacoustic cup (5 mm high and 10 mm in diameter) for direct determination of itsinfrared photoacoustic spectrum. Prior to the measurements, the cup was flushed with helium for 20s to reduce interference of carbon dioxide and water vapor in the air. Scans were conducted in the 4000-500 cm-1range with the 0.32 cm s-1mirror speed and 4 cm-1 resolution. Each spectrum was scanned 32 consecutive times. A 4300 handheld FTIRspectrometer (Agilent Technologies, Inc, USA) was used to analyzed the samples. Each spectrum was collectedin the spectral region of 600–4000 cm−1 at a 4 cm−1 resolution by the default Microlab Mobile version 5.3 software equipped with theinstrument and reported as an average of 24 spectra. Before eachscan, the background spectrum was also collected to avoid the interference of any impurities on the sensor area, which could impede the scanning process of the sample spectra. laser-induced breakdown spectroscopy (LIBS) was used to analyze the elemental composition of the synthesized samples. A MobiLIBS system (IVEA, France) was used for LIBS. The system consisted of a fourth-harmonic Nd:YAG laser (Quantel, France) driving 5-ns pulses. The frequency, delivery energy and wavelength of the pulsed laser were 20 Hz,16 mJ and 266 nm, respectively.An intensified charge-coupled device camera (iStar, Andor Technology, Northern Ireland) was used to collect the diffracted light in the 200–1000 nm spectral range. The X-ray Photoelectron Spectroscopy (XPS) analysis of the samples was conducted (Escalab 250xi, Thermo Fisher Scientific, UK) using monochromatized Al-KD radiation (1486.6 eV, energy step size 0.050 eV). The binding energy scale was calibrated with respect to the C1s signal at 284.8 eV. The detailed information for microstructure, morphology and surface topologyof the synthesized sampleswere observed using scanning electron microscopy (SEM)(ZEISS Merlin 132 Compact, Germany)on 10 kV accelerating voltage (AV).The surface elemental compositions and distribution were analyzed using an energy dispersive X-ray spectroscopy (EDX) detector attached to the SEM. The Fe and P contents in the solutions after hydrothermal reaction were determined using an iCAP 7000 inductively coupled plasma optical emission spectrometer (ICP-OES) (Thermo Fisher Scientific, Waltham, MA USA) under the following operation condition: RF power 1150 W, coolant gas flow 12 L min-1, atomizer gas flow 0.5 L min-1, auxiliary gas flow 0.5 Lmin-1, pump speed 45 rpm, and exposure time 10 s. Spectral intensities are the average of 3 replicate readings per sample. C, O and N contents of samples were measured by a CHN/O/S elemental analyzer CE-440 (Exeter Analytical, Inc. USA).
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figshare
创建时间:
2022-06-01



