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16 protocols using ultra dld

1

Characterization of CO₂-LiAlH₄-Graphite Products

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The products of CO2 reacting with LiAlH4 and graphite samples were characterized by XRD (X’Pert PRO), Raman spectroscopy (Renishaw Invia plus), field emission scanning electron microscopy (FESEM, NOVA NANOSEM 450) with EDS (Oxford X-Max 80 SDD), high-resolution transmission electron microscopy (HRTEM, FEI Tecnai G2 F30), ICP-MS (PerkinElmer Elan DRC-e), and XPS (Kratos Axis Ultra DLD) with monochromatized Al Kα excitation source. The XRD data were collected on an X’Pert PRO diffractometer with Cu Kα radiation at 40 kV and 40 mA in the 2θ range of 10‒80°. Raman spectra were obtained at the excitation wavelength of 532 nm. Nitrogen adsorption and desorption measured on a Micromeritics ASAP 2020 were used to determine the specific surface area and pore size distribution of graphite submicroflakes. TG analysis (Q5000IR) was carried out from room temperature to 700 °C at a heating rate of 5 °C min–1 in air. Gas composition was determined by gas chromatography-mass spectrometry and FTIR spectra (Thermo Nicolet 6700).
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2

Comprehensive Characterization of g-C3N4

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The phase composition of g-C3N4 was identified by XRD, recorded on a Rigaku D/max-3B X-ray diffractometer (Cu-Kα radiation, λ = 0.15418 nm) over the 2θ range of 10°-60° at 40 kV and 30mA. The chemical groups in g-C3N4 structure were confirmed by FT-IR, operated on a Nicolet Nexus infrared spectrometer after mixture of g-C3N4 sample with spectroscopic grade KBr (300 mg). The crystal morphology and microstructure of g-C3N4 were observed by SEM and TEM, realized on FEISirion200 scanning electron microscope and JEOL JEM-2010 transmission electron microscope, respectively. X-ray photoelectron spectroscopy (XPS) with Al Kα X-rays radiation (AXIS ULTRADLD, Kratos) was used to investigate the element compositions and surface properties of the samples. The binding energy was corrected using C1s (284.6 eV) as the internal standard. DRS spectra, recorded in the range of 400–800 nm, were implemented on an USB4000 UV-vis spectrometer (Ocean Optics) equipped with an integral sphere, using a standard template provided by South Africa Optics as the reference. The BET specific surface area of g-C3N4 was measured on a Sibata SA-1100 surface area analyzer, according to the nitrogen adsorption-desorption data at liquid nitrogen temperature. Surface Zeta potentials of g-C3N4 were examined by Zeta potential analyzer (Nano-ZS90) at different pH values.
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3

Characterization of HA-Tb Nanocrystals

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The morphology of the HA-Tb nanocrystals was observed using TEM on an FEI Tecnai G2 F20 instrument at 200 kV. The XRD patterns were acquired using a PANalytical Empyrean instrument in the 2θ range from 20° to 60° with Cu Kα radiation (λ = 1.5406 Å). The Fourier transform IR spectra were recorded in a transmission mode at a wave number range of 500 to 4000 cm−1 (PerkinElmer 6000). The elements were measured via both EDX mapping on TEM and XPS analyses (AXIS Ultra DLD, Kratos, UK). The photoluminescence was recorded using a Hitachi F-7000 fluorescence spectrophotometer. The HA-Tb nanocrystal powder implanted in the bone defects was scanned using micro-CT (vivaCT 80, SCANCO Medical AG, Switzerland) and a two-photon LSCM (LSM 780 NLO, ZEISS, Germany).
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4

Characterization of Novel Materials

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The samples were
characterized by X-ray diffraction (XRD) using a PANalytical X’pert
pro diffractometer (Cu Kα radiation, secondary graphite monochromator,
scanning rate of 1° 2θ/min). IR spectroscopic studies were
carried out in a PerkinElmer FTIR spectrophotometer (spectrum two)
in the range from 4000 to 550 cm–1 with a resolution
of 4 cm–1. X-ray photoelectron spectra (XPS) of
the samples were recorded using a Kratos axis Ultra DLD. Scanning
electron microscopy (SEM) images were recorded using a Zeiss, Ultra
55 field emission scanning electron microscope. A PerkinElmer LS 35
spectrometer was used to record the UV–visible spectra. The
catalytic oxidation of benzyl alcohol was monitored by HPLC (Jasco)
using a C18 column and a UV detector at 253 nm. A mixture of water
and acetonitrile in a 70:30 volume ratio and 0.2 M phosphoric acid
was used as the mobile phase. The mobile phase flow rate was maintained
at 0.8 mL min–1. The nitrogen sorption analysis
was performed in a BELsorp mini-II instrument at liquid nitrogen temperature.
The surface area of the material was determined by employing the Brunauer–Emmett–Teller
equation. The pore sizes and pore volumes of the materials were obtained
by the Barrett–Joyner–Halenda (BJH) method.
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5

Multimodal Characterization of NTO Powders and Coatings

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Microstructural
and phase analyses of the NTO powders and the coatings were carried
out using X-ray diffraction (XRD: Panalytical X’Pert Pro) and
Raman spectroscopy (Renishaw inVia, using a 633 nm laser source).
The morphology and composition of the processed surfaces were characterized
using scanning electron microscopy (SEM, FEI NOVA 230) coupled with
an energy dispersive X-ray emission spectrometer (EDS, Thermo Scientific
UltraDry). Finally, both elemental compositions and valence states
were examined by X-ray photoelectron spectroscopy (XPS, Kratos Ultra
DLD) using monochromated Al Kα radiation (15 kV, 10 mA), with
a pass energy of 20 eV for high-resolution surveys. It should be noted
that, prior to the XPS analysis, the sample surfaces were cleaned
by Ar+ sputtering for 3 min to remove any surface impurities.
Following XPS analysis, quantitative analysis of the spectra was carried
out using the CasaXPS software.31
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6

Graphene Crystallinity Analysis via LEED

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LEED embodied in Kratos Ultra DLD was used for tracking the crystallinity of the samples. The distortion of the image, clearly seen from the imperfection of the hexagons formed in the diffraction pattern of the graphene, is caused by the form of the lens, non‐flat samples’ surface and edge effects of the signal capturing camera.
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7

Ultraviolet Photoelectron Spectroscopy Technique

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UPS spectra were obtained from an AXIS ULTRA DLD (Kratos) with He I (21.22 eV) excitation lines and a sample bias of –9 V under a vacuum of 3.0 × 10–8 Torr. Radiation damage from the light source on the organic films was carefully examined and no damage was detected. All measurements were carried out in the dark.
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8

Comprehensive Materials Characterization Protocol

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XRD patterns were supplied by Bruker D8 Advance. TEM image and EDS images were captured by Tecnai G2 F20 with EDS Inca X–Max (Oxford). Scanning electron microscopy (SEM) images were given by Gemini SEM 300. In-situ XPS measurement was operated on a Kratos-Axis Ultra DLD instrument using a xenon lamp as the light source. The binding energy of C1s at 284.8 eV was used for energy calibration. VB XPS spectra and UPS of the samples were collected by Escalab Xi+ (Thermo Scientific), and UV–vis DRS was determined by the UV-2600 system (Shimadzu). The content of K and Li was obtained from ICP-OES (PE Avio 200) and the content of H was obtained from O, N, and H co-meter (LECO ONH836). AFM images and KPFM images were captured by Bruker MultiMode 8, and the probe used was a silicon probe. During the measurement, a xenon lamp was used as the light source, and the light irradiation time was 15 min. In this case, the powder sample was dispersed in an ethanol solution and then dropped onto the silicon wafer to form a uniform film for testing.
In-situ DRIFTS characterization was operated on a Nicolet iS50 FTIR spectrometer. 13C isotope tracing experiment was performed by mass spectrometry (Finnigan MAT 271). The O2 generated during the CO2 photoreduction process was detected by a gas chromatograph (GC14C, Shimadzu) with a TCD detector.
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9

Surface Characterization and Mg Release

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SEM (S-3400, HITACHI, Japan) was used to examine the surface morphologies of the four groups. The surface chemical composition was examined with XPS (AXIS UltraDLD, Kratos, Japan). The release kinetics of Mg were evaluated by using a previously described method17 (link). In brief, the samples (2 cm squares) were immersed in 10 mL phosphate buffer solution (PBS) for various durations at 37 °C without agitation. The resultant solutions were analysed by using ICP-AES. The surface wettability of the samples was evaluated on the basis of contact angle measurements (Automatic Contact Angle Meter Model SL200B, Solon, China). Data were collected after a 2 μL deionized water droplet was dropped onto the sample surface and stabilized at room temperature. Three samples in each group were tested for statistical analysis.
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10

Comprehensive Material Characterization

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The crystalline structure of the samples was determined using a powder X-ray diffractometer (XRD, Rigaku SmartLab SE) at a scan step of 2°·min−1 with Cu Kα radiation. SEM (HITACHI SU8100) and transmission electron microscopy (TEM, TF20) were used to examine the morphology and microstructure of the samples. X-ray photoelectron spectroscopy (XPS, KRATOS, Axis UltraDLD) was performed, and the content of Ag+ in the solution was determined using an inductively coupled plasma optical emission spectrometer (ICP-OES, SPECTRO BLUE). TG curves were measured using a thermogravimetric analyzer (PerkinElmer TL8000). The element content was measured and calculated by ICP-MS (Agilent 7800).
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