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25 protocols using empyrean xrd

1

Characterization of MWCNT-LiFePO4 Sheets

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Scanning Electron Microscopy (Nova NanoSEM, FEI) was used to determine the morphology of MWCNT-LiFePO4 sheets. No coating of palladium/gold layer was applied to the samples. Energy-dispersive X-ray spectroscopy (EDS) mapping was performed using Quanta 250 ESEM at 20 kV accelerating voltage. Raman spectroscopy was performed using a Witec Alpha 300RAS with 532 nm excitation wavelength. X-ray diffraction was performed using XRD Empyrean from PANalytical XPert PRO using a powder method, with copper Kα1 of 1.540598 Å, 40 kV voltage, 40 mA current, step size of 0.02° and 2θ range from 10° to 80°. Particle sizes of as-received LiFePO4 powders and ball milled LiFePO4 powders were determined using HORIBA LA-950 Particle Size Analyzer. The samples were prepared for measurement of the particle size such that LiFePO4 powders were immersed in water followed by sonication using VCX 750 Ultrasonic Processor (Sonic, USA) for 10 minutes, then particle size measurements were immediately performed using HORIBA LA-950 Particle Size Analyzer.
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2

Crystallinity Analysis of Printed Samples

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An XRD Empyrean (Panalytical, Netherlands) was employed to examine the crystallinity of the bulk printed samples. Samples were scanned between 5 and 40 ° 2-theta values using a CuKα source with a voltage of 45 kV and a current of 20 mA, and a step size of 0.026, and 100 s per step.
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3

XRD Analysis of Ground Samples

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The samples were firstly prepared, as described in Section 2.2.2. After stopping hydration by isopropanol and vacuum drying, samples were ground and measured by XRD (XRD Empyrean, Malvern Panalytical, Malvern, UK) with CuKα (λ = 1.54 Å) for the 2θ range of 5° to 65° with a step width of 0.013°.
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4

Crystallinity Analysis of CNCs

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CNC were analyzed with Malvern Instruments XRD Empyrean (Malvern, UK) with Cu-Kα radiation at 45 kV and a current of 40 mA. The incidence angle was set to 5–70° (step size of 0.2°). The percentage of crystallinity was calculated according to the Rietveld method [40 ], and the obtained data was analyzed with the University of Trento MAUD 2.1 software (Trento, Italy).
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5

Comprehensive Characterization of FeOx Nanoparticles

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The prepared FeOx NP samples were characterized as follows: impurities in the FeOx (P2) sample were analyzed with an ICP Emission Spectrometer (iCAP 6000 Series, Thermo Scientific, Cambridge, UK). Crystal structures were analyzed by using a X-ray diffractometer (XRD, Empyrean, Malvern Panalytical B.V., Malvern, UK) with Cu K radiation over a range of 2θ angles from 20° to 80°. In addition, their surface areas were measured with Brunauer, Emmett, and Teller (BET) surface area analyzer (Tristar II 3020, Micromeritics, Norcross, GA, USA). Their particle size and morphology were observed by using by a high resolution transmission electron microscope (HRTEM, JEM-ARM200F, JEOL, Tokyo, Japan). Saturation magnetization of samples was measured by using a vibrating sample magnetometer (VersaLab VSM, Quantum Design, Inc., San Diego, CA, USA) under room temperature and applied magnetic fields of up to 30,000 Oe.
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6

Mineralogical Analysis of Opalinus Clay Facies

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The mineralogical composition was analyzed from eight samples each of the sandy and of the shaly OPA facies and from one sample of the PW formation. Samples of the sandy facies (BMA‐3) were obtained between 3.45 and 9.30 m from the gallery wall, while samples of the shaly facies (BMA‐4) were obtained between 3.97 and 9.13 m from the gallery. A PANalytical Empyrean XRD was used for the measurements, operating at 40 kV and 40 mA with Cu‐Kα radiation and a step size of 0.013°2θ from 4.6° to 85°. The mineralogy was first determined with the software EVA (version 11.0.0.3) by Bruker. Rietveld refinement for quantitative analysis was performed using the program BGMN and the graphical user interface Profex (version 3.10.2, Döbelin & Kleeberg, 2015 (link)). The error is expected to be in the range of 3 wt%.
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7

Biosynthesis and Characterization of Silver Nanoparticles

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The nanoparticles were biosynthesized by adding 6.0 ml of silver nitrate solution (1 M) with 40 ml of extract and 154 ml of deionized water. The reaction mixture was observed for color change depending on parameter studied such as time, silver nitrate, and extract concentration at 80°C. The resultant reddish brown-colored reaction mixture was then centrifuged at 12,000 rpm for 10 min (REMI, India). The pellet obtained was washed thrice with deionized water and finally with acetone. The resultant pellet was dried and stored for further characterizations. The preparation of silver nanoparticles was characterized by ultraviolet-visible (UV-Vis) spectrophotometer (Themoscientific SpectraScan) in the wavelength range of 340–900 nm. The surface morphology and particle size distribution of the S. podophyllum nanoparticles were examined using an atomic force microscope (AFM, NDMDT) with a conducting P (n)-doped silicon tip under normal atmospheric condition in semicontact mode. The X-ray diffraction (XRD) patterns of silver nanoparticles were obtained using X-ray diffractometer (PANalytical Empyrean XRD) with diffraction angle in the range of 20°–80°.
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8

Microstructure and Mineral Analysis of Broken Specimens

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The broken specimen pieces were collected and soaked in absolute alcohol for 24 h after testing. Then, they were dried in a 40 °C vacuum drying oven for 24 h to prepare them for microstructure characterization.
Quanta FEG 450 SEM/EDS (Thermo Fisher Scientific, Waltham, MA, USA) with 20 kV acceleration voltage and a 5.0 spot size was used to observe the microstructure. Empyrean XRD (PANalytical, Almelo, The Netherlands) was used to determine the mineral phases, and the spectra were analyzed in the range of 2θ 10°–90°.
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9

Characterizing Fiber Alignment in 3D Printed PLA/Lyocell Composites

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In order to investigate fibre alignment during printing, 3D printed PLA/lyocell composite samples were analysed through XRD analysis. The 3D printed discs were analysed in a Panalytical Empyrean XRD (Worcestershire, UK) in transmission mode using CuKα radiation (40 kV; 40 mA) and a PixCel linear detector. First, the samples were analysed in a continuous 2θ scan mode between 5–45° 2θ using a scanning step of 0.01° and equivalent exposure time of 40 s at φ angles (disc rotation axis) of 0° and 90°. Then, a scan through the φ axis (0–180°) was conducted at the 2θ angle (approximately 21.2°) determined in the first scan using a step size of 0.5° and exposure time of 10 s.
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10

Structural Analysis of Deposited Films

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The crystallinity and structural phase of deposited films were analyzed by grazing incidence X-ray diffraction (GIXRD) system equipped with a CuKα X-ray source (PANalytical Empyrean XRD, Netherlands) operating at beam intensity of 40 kV and 40 mA. The glancing angle X-ray was incident at an angle of 0.5°. Cross-sectional micro-structure of the fuel cell was characterized by field-emission scanning electron microscopy (FESEM, JSM-7600F, JEOL, Ltd., Japan) and transmission electron microscopy (TEM, JEM-2100, JEOL, Ltd., Japan).
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