The crystal structure of the MnO2/BC hybrids was characterized by powder X-ray diffraction (XRD, X’pert PRO, PANalytical B. V, Holand) employing monochromatized Cu Kα incident radiation. The morphology and microstructure of the materials were investigated by field emission scanning electron microscopy (FESEM, Nova 600i, FEI, Hillsboro, OR, USA) equipped with energy dispersive X-ray spectroscopy (EDS) analysis operated at 15 kV and transmission electron microscopy (TEM, FEI-2100 Plus, JEOL, Japan). The surface chemical composition and oxidation state of the MnO2/BC hybrids were determined using X-ray photoelectron spectroscopy (XPS, Kratos Analytical Ltd., Manchester, UK). The nitrogen adsorption/desorption isotherms were carried out at 77 K using a Quantachrome Autosorb-1 instrument (Quantachrome Corporation, Florida, USA). The specific surface area and pore size distribution were calculated by the Brunauer-Emmett-Teller (BET) and density functional theory (DFT) methods, respectively.
Nova 600i
Manufactured by Thermo Fisher Scientific
Sourced in United States
The Nova 600i is a laboratory equipment designed for analytical measurements. It provides accurate and reliable results for various applications. The core function of the Nova 600i is to perform precise analytical tasks required in research and industrial settings.
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4 protocols using nova 600i
1
Characterization of MnO2/BC Hybrids
2
Fluorescently-labeled Silica Nanoparticle Synthesis
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Tetraethyl orthosilicate (TEOS 98%), 3-aminopropyl triethoxysilane (APTES), 5(6)-carboxyfluorescein (FCOOH), dicyclohexylcarbodiimide (DCC), 4-(N,N-dimethylamino)-pyridine (DMAP), and ammonia solution (25 or 30% aqueous) were purchased from Sigma Aldrich.
Acetone, ethanol (EtOH), dimethyl sulfoxide (DMSO), ethyl acetate (EtOAc), and tetrahydrofuran (THF) were used without further purification.
SEM measurements were performed with a TESCAN Vega TS 5130 LM working at 30 kV. High-performance FESEM investigations were conducted on a dual-beam FEI Nova 600i instrument, with a semi-in-lens cold cathode field emission scanning electron microscope source. The micrographs were taken at 5-kV accelerating voltage, using in-lens detector in pure secondary electron signal mode. In all cases, a thin layer of gold was sputtered onto samples.
Atomic force microscopy (AFM) maps were produced using a NT-MDT Ntegra instrument in a semi-contact mode with gold-coated Si cantilevers Etalon or NSG01, 03, 10, 30 types. A typical measure scans a 75 × 75 to 5 × 5 μm2 area, with a scanning frequency between 0.2 and 0.5 Hz, depending on the surface.
DLS measurements were performed with a Malvern Instruments Zetasizer.
Acetone, ethanol (EtOH), dimethyl sulfoxide (DMSO), ethyl acetate (EtOAc), and tetrahydrofuran (THF) were used without further purification.
SEM measurements were performed with a TESCAN Vega TS 5130 LM working at 30 kV. High-performance FESEM investigations were conducted on a dual-beam FEI Nova 600i instrument, with a semi-in-lens cold cathode field emission scanning electron microscope source. The micrographs were taken at 5-kV accelerating voltage, using in-lens detector in pure secondary electron signal mode. In all cases, a thin layer of gold was sputtered onto samples.
Atomic force microscopy (AFM) maps were produced using a NT-MDT Ntegra instrument in a semi-contact mode with gold-coated Si cantilevers Etalon or NSG01, 03, 10, 30 types. A typical measure scans a 75 × 75 to 5 × 5 μm2 area, with a scanning frequency between 0.2 and 0.5 Hz, depending on the surface.
DLS measurements were performed with a Malvern Instruments Zetasizer.
3
Micromechanical Characterization of Pillars
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Bulk single crystals were first oriented in [001] direction. The top surface was then carefully polished and machined into pillar by Focused Ion Beam milling system (FEI Nova 600i Nanolab). Low milling currents with amplitude ranging from 0.1 to 3 nA were applied in sequence to minimize the effects of Ga+ source on the pillars. The obtained pillars have a cylindrical shape with dimensions of ~ 1 µm × 5 µm (radius × height). The micro-compression tests were conducted on an in-situ nanoindenter (Hysitron PI 85) equipped with a flat diamond tip (2.5 µm in radius). Compressive loads were applied at a constant loading rate of 5 µN/s until samples failed. At the start of the test, the transducer of the nanoindenter was calibrated to ensure the accuracy of the measurements.
4
In-situ TEM Lamella Preparation and Characterization
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Cross-sectional transmission electron microscopy (TEM) specimens were prepared via an in situ lift-out procedure in a dual-beam instrument (FEI Nova 600i) that incorporated a focused ion beam microscope and scanning electron microscope in the same chamber. Both 5 and 2 kV ions were used to polish the TEM lamella to a thickness of 50 nm, and remove side damage. High-resolution scanning transmission electron microscopy (STEM) was performed using a probe-side aberration-corrected FEI Titan G2, operated at 80–200 kV with a high-brightness field-emission gun (X-FEG). Bright-field STEM imaging was performed using a probe convergence angle of 21 mrad and a probe current of ∼90 pA. In bright-field images, identification of each atomic layer was achieved by elemental analysis using energy dispersive X-ray (EDX) and electron energy loss spectroscopy (EELS). EDX images were obtained using a Super-X four silicon drift EDX detector system with a total-collection solid angle of 0.7 sr. EELS images were obtained using a Gatan Imaging Filter (GIF) Quantum ER system, with an entrance aperture of 5 mm. The lamella was oriented by using the Kikuchi bands to direct the electron beam down the zone axis of PMN-PT.
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