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9 protocols using jem 2010 high resolution transmission electron microscope

1

Characterization of Material Properties

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The Fourier transform infrared (FTIR) spectra were recorded in the range of 4000–400 cm−1 on a NEXUS FTIR spectrometer (Nicolet, Madison, WI, USA) using the KBr pellets. Thermal gravimetric analysis (TGA) was tested from 35 to 900 °C on a Diamond TG-DTA 6300 thermal analyzer (PerKinElmer, Waltham, MA, USA) at the heating rate of 10 °C min−1 under an oxygen atmosphere. The specific surface area, pore volume and pore size distribution of the samples were measured on an Accelerated Surface Area and Porosimetry System (Micromeritics, ASAP2020, Atlanta, GA, USA) using N2 as an adsorbate at 77 K. The TEM images were taken using a JEM-2010 high resolution transmission electron microscope (HRTEM) (JEOL, Tokyo, Japan) at an acceleration voltage of 200 kV, and the sample was ultrasonically dispersed in anhydrous ethanol and dropped onto a grid before observation. The microscopic morphology was observed on a scanning electronic microscope (SEM, JSM-6701F, JEOL, Ltd., Tokyo, Japan) after the samples were fixed on copper sheets and coated with a gold film.
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2

Fabrication and Characterization of Magnetic Nano-Carbon Composites

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IOP (Ultravist ® 370) and Glucose (used as electron donor) were purchased from Bayer Schering Pharma and Aldrich, respectively. Basal medium solution was composed of several mineral salts (K2HPO4, NaHCO3, MgSO4, NH4Cl and CaCl2) and trace elements dissolved in distilled water as described in previous works (Cervantes et al. 2000 (link); Amezquita-Garcia et al. 2013 ; Toral-Sánchez et al. 2016 ).
The fabrication of MNS was performed using an aerosol-phase methodology previously proposed (Chen et al. 2012 (link); Chen et al. 2013 (link); Lv et al. 2016 (link)) using a colloidal suspension of GO (0.5 mg/mL) and magnetite NP (1mg/mL). In order to demonstrate the assembly of magnetic NP in the MNS, micrographs of these nano-carbon composites were performed using a JEOL JEM-2010 High Resolution Transmission Electron Microscope (HRTEM).
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3

Comprehensive Characterization of Nanoparticles

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Characterization by Fourier transform infrared (FT-IR) spectroscopy was performed with an FT-IR 8400S spectrometer (Shimadzu, Japan). Spectra were recorded over the range of 4000–400 cm−1 in transmission mode, and 32 scans were accumulated at a resolution of 4 cm−1. Magnetic properties were determined with a 7410 vibrating sample magnetometer (VSM, Lake Shore Cryotronics, Inc., Ohio, USA). Morphological observations of the nanoparticles were carried out with a JEM-2010 high-resolution transmission electron microscope (JEOL, Tokyo, Japan). Thermogravimetric analysis (TGA) was conducted using a Mettler Toledo TGA2 analyzer (Switzerland) from 30 to 750 °C at a heating rate of 10 °C min−1. X-ray diffraction (XRD) patterns were recorded in the range of 2θ = 20–80° by step scanning using a Rigaku D/Max-2500 diffractometer (Japan) with Cu Kα radiation. 1H NMR and 13C NMR spectra were recorded with a Bruker AV-400 spectrometer with chemical shifts reported as ppm (in CDCl3 and DMSO-d6 with TMS as an internal standard). Mass spectrometric analysis was carried out using an LCQ Fleet mass spectrometer (Thermo Fisher). An ICP-OES system (715-ES, Varian Medical Systems, USA) was used for the determination of REEs.
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4

Comprehensive Catalyst Characterization

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X-ray diffraction (XRD) experiments were carried out with Bruker D8 Advance diffractometer. The elemental content was determined by Shimadzu ICPS-7500 equipment. The morphology and structure of catalysts were studied on JEOL JEM-2010 high-resolution transmission electron microscope. AC-HAADF-STEM images and EDS mapping data were performed on JEOL JEM-ARM200F. The CO pulses chemisorption experiments were conducted on Micromeritics Autochem II 2920. Quasi in situ XPS measurements were recorded on Kratos Axis Ultra DLD Instrument. The pre-treated sample was placed in a glove box and transferred into a sample rod in a N2 atmosphere. In situ/Operando XAFS at Ir L3-edge and Ce L3-edge measurements were recorded at the beamline BL11B of the Shanghai Synchrotron Radiation Facility (SSRF), Shanghai Institute of Applied Physics, Chinese Academy of Sciences (CAS). In situ/operando DRIFTS were studied on a Bruker TENSOR II infrared spectrometer with a MCT detector. The detailed experimental methods are present in the Supplementary Information.
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5

Characterization of Nitrogen-Doped Carbon Aerogel

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The morphology of the nitrogen-doped carbon aerogel was measured using an FEI-Inspect F field emission scanning electron microscope and JEOL JEM-2010 high resolution transmission electron microscope. The surface area and pore sizes for the nitrogen-doped carbon aerogel were determined with Brunauer-Emmett-Teller (BET) theory and Density Functional Theory (NLDFT), respectively, using Nitrogen absorption and desorption isotherms obtained at 77 K with a Quantachrome Nova 4200e. The J-V curves of the devices were measured with a Keithley 2400 Source Meter under simulated AM 1.5 G solar light irradiation from a Solar Simulator from Newport class ABB and in the dark. The intensity of the solar light illumination was measured using a standard silicon cell. The electrochemical impedance spectra (EIS) of symmetrical cells made by sandwiching together two counter electrodes and filling with electrolyte were measured using a Gamry Instrument Interface 1000 in a frequency range from 0.01 Hz to 100 kHz, with 10 mV amplitude, in the dark.
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6

Hepatoma Cell Culture and Characterization

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SMMC-7721 human hepatoma cells were purchased from the Shanghai Institute of Biology
and Cell Biochemistry, Chinese Academy of Science. RPMI 1640 culture medium was
purchased from Gibco-BRL (USA). Trypsin (0.25%) was purchased from AMRESCO (USA). MTT
and diethyl bicarbonate (DEPC) were purchased from Sigma (USA). Giemsa dye was
purchased from Chroma (USA). AMV reverse transcriptase, dNTP, Oligo(dT)18, Taq DNA
polymerase, 100 bp DNA ladder, RNasin (40 U/L), and RNase-free DNase I were all
purchased from Takara Co. (China). The immunocytochemical reagents,
streptavidin-peroxidase (SP) staining kit and liquid aminoethyl carbazole (AEC)
enzyme substrate visualization kit were purchased from Beijing Zhongshan
Biotechnology Co., Ltd., China. All biochemical reagents used in this study were of
analytical grade.
A PTC-100 thermal cycler, Multiskan MK3-353 enzyme linked immunosorbent assay (ELISA)
reader and Vantage SE fluorescence-activated cell sorting (FACS) system (USA) were
used. An inverted microscope and JEM-2010 high-resolution transmission electron
microscope (JEOL, Japan) were used. An SP-04C high-frequency induction heater
(Shenzhen Shuangping High-Frequency Heater Factory, China) was used with the
following operating parameters: frequency=200 kHz; power=4 kW; output alternating
heating current=100-350 A.
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7

Detailed Characterization of MrGO-N and rGO-N

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Morphological characterization of MrGO-N and rGO-N was performed on a LEO 1530 VP Scanning Electron Microscope (SEM) and JEOL JEM-2010 High Resolution Transmission Electron Microscope (HRTEM). Samples were suspended in ethanol and then sonicated for 30 min. After that, the samples were mounted in a Cu TEM grid. Raman spectroscopy was performed on a WITEC-A300M+ Confocal Raman Microscope with laser frequency of 514 nm as excitation source trough a 50× objective. Zeta potential measurements of the samples were measured in DI water using a Malvern Nano-ZS dynamic light scattering equipment. X-ray diffraction (XRD) patterns were obtained in a Bruker D8 Advanced diffractometer using CuKα radiation. Infrared spectra were recorded by Fourier transform-infrared (FT-IR) spectroscopy using a Jasco FTIR-4100 Instrument in ATR mode. Finally, oxygenated groups were quantified by Boehm titrations with an automatic titrator Mettler-Toledo T70. Details of experimental conditions and procedures are described in previous work [26 (link)].
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8

Nanoporous Silica Characterization Techniques

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The FTIR spectra of the samples were
taken with a Bruker TENSOR equipped with a Platinum ATR from 4000
to 400 cm–1, with a resolution of 2 cm–1. Nitrogen and water vapor adsorption–desorption experiments
were performed with an ASAP 2020 surface area and porosity analyzer
from Micromeritics. Nanoporous silica samples were degassed under
vacuum at 90 °C for 24 h. Nitrogen adsorption isotherms were
taken at 77 K and the water vapor adsorption isotherms at 298.15 K.
Thermogravimetric analyses were performed with a Q50 thermonuclear
from TA Instruments under a controlled nitrogen gas flow from ambient
temperature to 850 °C with a temperature ramp of 10 °C/min.
Small-angle X-ray scattering patterns were collected using a Xeuss
2.0 HR SAXS/WAXS instrument from Xenocs with a Cu Kα (5 kV,
0.6 A). TEM images were taken with a JEOL JEM-2010 high-resolution
transmission electron microscope operating at 200 kV.
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9

Characterization of Drug-Loaded Nanocarriers

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The size and the morphology of the m-HAP, 6-Gin-m-HAP, Dox-m-HAP and 6-Gin + Dox-m-HAP were acquired using a transmission electron microscope (TEM, JEOL JEM-2010 High resolution transmission electron microscope, Japan) operating at 80 kV. The different functional groups of the carrier and the drug-carrier molecules were identified using Fourier transform infra-red (FT-IR) spectroscopy (Bruker Vertex 80, Germany) via the diffuse reflectance mode, within the spectral range 400–4000 cm−1. Further, the interaction of the drug molecules with the carrier was studied using X-ray photoelectron spectroscopic (XPS) analysis (a K-alpha instrument, Thermo Scientific, East Grinsted, UK, equipped with a monochromated Al Kα X-ray source was used with a pass energy of 40 eV and step size of 0.1 eV). Spectra were processed using the CasaXPS software (Casa Software Ltd., Teignmouth, UK).
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