The purpose of the observation of the microstructure was a qualitative identification of the crystalline and amorphous phases, their morphology and elemental composition. Like before, examinations were performed for 12 brick samples with defined forms of damage. The samples were in the form of irregular chunks with a volume of approx. 1 cm3. The specimens were glued onto stubs with silver glue. Due to the lack of sputtering (none coating), the examination was carried out in variable vacuum, in the pressure range of 80–120 Pa and at constant accelerating voltage EHT 20 kV. The microstructural observations were made in a scanning electron microscope EVO MA10 from Zeiss, equipped with VPSE, SE and BSD detectors and an X Flash 6/30 (EDS) detector from Bruker (Hamburg, Germany).
Xflash 6 30
Manufactured by Bruker
Sourced in Germany
The XFlash 6/30 is an energy-dispersive X-ray (EDX) detector designed for elemental analysis in scanning electron microscopes (SEMs). It provides fast, accurate, and reliable detection of elements from beryllium (Be) to uranium (U) with a 30 mm2 active area.
Automatically generated - may contain errors
Lab products found in correlation
Supra 40, by Zeiss (2 mentions)
K alpha, by Thermo Fisher Scientific (2 mentions)
Sigma 300, by Zeiss (2 mentions)
Evo ma10, by Zeiss (1 mentions)
Feg 450, by Thermo Fisher Scientific (1 mentions)
X pert pro mpd, by Malvern Panalytical (1 mentions)
Geminisem 300, by Zeiss (1 mentions)
Em scd 500, by Leica (1 mentions)
Merlin vp compact, by Zeiss (1 mentions)
Evo18, by Bruker (1 mentions)
Dimension icon, by Bruker (1 mentions)
D2 phaser x ray, by Bruker (1 mentions)
Uv vis spectroscopy, by PerkinElmer (1 mentions)
Mira3, by TESCAN (1 mentions)
Icap q, by Thermo Fisher Scientific (1 mentions)
Uv 1600pc uv vis spectrometer, by Avantor (1 mentions)
10 protocols using xflash 6 30
1
Microstructural Analysis of Damaged Bricks
2
Characterization of Copper Oxide Catalysts
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The morphological properties of the copper oxide catalysts were characterized using a scanning electron microscope (FEI FEG 450) coupled to an EDX spectrum (BRUKER XFlash 6/30). An IRAffinity-1S SHIMADZU Fourier transform infrared (FTIR) spectrophotometer was equipped with a Golden Gate single reflection attenuated total reflectance (ATR) accessory. FTIR spectra were recorded in the range of 500–4000 cm−1 at a resolution of 16 cm−1 and were used to determine the structural properties of the catalysts. A PANalytical X-ray diffractometer (XRD) X'PERT PRO MPD, with Cu Kα = 1.540598 Å and operating at 45 kV and 30 mA, was used on the prepared electrode to determine the crystalline phase of Cu(OH)2–Cu2O supported on PPy/F-MWCNTs/CPE.
3
Surface Morphology Analysis of 3Y-TZP Ceramics
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The surface morphology of 3Y-TZP, 3Y-TZP with APA, 3Y-TZP with GCSD and LDGC before and after HF etching (n = 3) was investigated with scanning electron microscopy (SEM, GeminiSEM 300, Carl Zeiss Microscopy GmbH, Germany). The elemental compositions were examined with energy dispersive X-ray analysis (EDX, XFlash 6-30, Bruker, USA).
4
FE-SEM and EDX Protocol for Elemental Analysis
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Samples were analyzed by a field emission scanning electron microscope (FE-SEM, Merlin® VP Compact, Zeiss, Oberkochen, Germany) equipped with an energy dispersive X-ray (EDX) detector (XFlash 6/30, Bruker, Berlin, Germany). The samples were coated with carbon under vacuum (EM SCD 500, Leica, Bensheim, Germany). Representative areas of the samples were analyzed and mapped for elemental distribution on the basis of the EDX-spectra data by QUANTAX ESPRIT microanalysis software (Version 2.0, Bruker, Billerica, MA, USA). EDX mappings were taken from the selected regions operated with 10 kV accelerating voltage and 500 times magnification.
5
Soil Microstructure Analysis with SEM and EDS
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SEM has been used to study the microstructures of soil aggregates. The operating principle of SEM is that a narrow electron beam rasters over the object's surface and secondary electrons are generated from each point of sample surface. The detector captures the secondary electrons to generate an electronic signal that provides a visual image. Soil powder was mounted in a conductive adhesive and sprayed with gold powder by an ion sputtering instrument for testing in the SEM (Zeiss Evo18).
An EDS instrument (Bruker Nano Berlin, Germany, XFlash 6|30) with an acceleration voltage of 10 kV was used. The main elements represented by this detector include O, Si, Al, Fe, Ca, Na, K, Mg and P. For the XRD analyses, the operating conditions were an electron beam acceleration voltage of 10 kV, beam current of 0.2 nA, working distance of 80 mm and X-ray angle of emergence of 35°. The signal was recorded in channel 4096 for a counting time of 40 seconds and detection thickness of 0.45 mm. To calibrate the EDS results, we used standardless quantification method. This method relied on peak-to-background ZAF evaluation (P/B-ZAF) and provided reliable quantification results.
An EDS instrument (Bruker Nano Berlin, Germany, XFlash 6|30) with an acceleration voltage of 10 kV was used. The main elements represented by this detector include O, Si, Al, Fe, Ca, Na, K, Mg and P. For the XRD analyses, the operating conditions were an electron beam acceleration voltage of 10 kV, beam current of 0.2 nA, working distance of 80 mm and X-ray angle of emergence of 35°. The signal was recorded in channel 4096 for a counting time of 40 seconds and detection thickness of 0.45 mm. To calibrate the EDS results, we used standardless quantification method. This method relied on peak-to-background ZAF evaluation (P/B-ZAF) and provided reliable quantification results.
6
Characterization of Nanoporous Gold Supports
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For determination of the pore and ligament sizes of the npAu supports as well as the zinc distribution the samples were transferred onto a microscope sample holder with a conductive carbon tape. Micrographs of the samples morphology were acquired with a Supra 40 (Zeiss, Germany) scanning electron microscope operated at 10.0 kV acceleration voltage, 300 pA probe current and 4 mm working distance. The pore and ligament sizes were determined by measuring the diameter of at least 250 pores or ligaments in the obtained SEM images using the program ImageJ. The specific surface area S was calculated from the ligament diameter d according to S = (C/ρd) where C is the porosity factor for npAu with 3.7 and ρ is the gold bulk density of 19.8 g cm−3 according to literature.40,41 (link) This method was shown to give values that are in good agreement with both, data from gas adsorption experiments (BET) as well as electrochemical methods (CV).40,41 (link) The amount of immobilized ZnPc as well as the zinc distribution on the surface were determined by energy dispersive X-ray spectroscopy (EDX, Bruker XFlash 6/30).
7
Comprehensive Physicochemical Characterization
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The physicochemical properties of the samples were characterized, as mentioned previously [25 (link),26 (link)]. The surface topography was analyzed by field-emission scanning electron microscopy (FE-SEM; Sigma 300, Zeiss, Oberkochen, Germany). The surface roughness was assessed by atomic force microscopy (AFM; Bruker dimension icon, Bruker, Karlsruhe, Germany). The surface chemistry of the samples was investigated by energy-dispersive X-ray spectroscopy (EDS, XFlash 6|30, Bruker, Karlsruhe, Germany) and X-ray photoelectron spectroscopy (XPS; K-Alpha, Thermo Fisher Scientific, Waltham, MA, USA). Wettability was measured by static water contact angles (WCA) on the sessile-drop method measuring device (DSA XROLL, Betops, Guangzhou, China).
8
Characterization of Synthesized Materials
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The structure and phase purity of the synthesized materials were characterized using a Bruker D2 Phaser X-ray diffractometer with a Å copper tube. Using the DIFRACC.EVA V4.3.1.2 software, a semi-quantitative analysis of the diffraction pattern was performed to identify secondary phases. The morphological analysis of the sample was performed using scanning electron microscopy and energy-dispersive X-ray spectroscopy. A field emission electron microscope MIRA 3, TESCAN equipped with a Bruker X-Flash 6–30 detector with a resolution of 123 eV in Mn K was used. The diffuse reflectance spectrum was measured by UV-Vis spectroscopy (Perkin Elmer, Waltham, MA, USA) with 200–1000 nm with an integrating sphere. These spectra were transformed by a Kubelka–Munk model in order to estimate the band gap value.
9
Characterization of ZnPc-Immobilized Nanoporous Gold
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The quantity of immobilized ZnPc on npAu was determined by inductively coupled-plasma mass spectrometry (ICP-MS, iCAP Q, Thermo Fisher Scientific GmbH) after dissolving 10 mg of the as prepared hybrid sample in ultrapure aqua regia (2 mL).
The pore size of the npAu support was determined acquiring micrographs of the samples on a scanning electron microscope (SEM, Supra 40, Zeiss, Germany) operated at 15.0 kV acceleration voltage, 300 pA probe current and 10 mm working distance. Characterization was performed by measuring the diameter of at least 250 pores in the obtained SEM images using the program ImageJ.
The zinc distribution on the surface was determined by energy dispersive X-ray spectroscopy (EDX, Bruker XFlash 6/30).
All UV-Vis spectra were recorded using a UV-1600PC UV-Vis spectrometer from VWR.
The pore size of the npAu support was determined acquiring micrographs of the samples on a scanning electron microscope (SEM, Supra 40, Zeiss, Germany) operated at 15.0 kV acceleration voltage, 300 pA probe current and 10 mm working distance. Characterization was performed by measuring the diameter of at least 250 pores in the obtained SEM images using the program ImageJ.
The zinc distribution on the surface was determined by energy dispersive X-ray spectroscopy (EDX, Bruker XFlash 6/30).
All UV-Vis spectra were recorded using a UV-1600PC UV-Vis spectrometer from VWR.
10
Biochar Surface Morphology Analysis
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An Environmental Scanning Electron Microscope ESEM FEG2500 FEI (FEI Europe, Eindhoven, Netherlands) with energy dispersive X-ray spectroscopy (EDX) was used to investigate the surface morphology: all the macro, micro, and nano pores of biochar structures. Samples of biochar of about 1cm 2 were positioned on a microscope stub attached with double adhesive tape. No preparation of the sample was necessary for the analyses. Analysis during acquisition were in point analysis mode. The working parameters were as follows: the working distance was approximately 10 mm, and the scanning time 1-3 μs, environmental low-vacuum (60 Pa) with a large field detector to allowed optimal secondary electron (SE) imaging, performed at 5 kV and 10 kV with a beam size of 2.5 μm and 20 kV with beam size of 4 μm for the EDX analysis. (Marmiroli et al., 2018) (link). EDX analysis was carried out with a Bruker XFlash®6 | 30 X-ray detector, the acquired spectra (for Mg, Ca, K, P, Mn, Si, Ti, Al, Fe, Cu, Zn, Co, Cd) were fully deconvoluted and standard-less quantification was performed using the P/B-ZAF (Peak/ Background evaluation matrix with atomic number (Z), absorption (A), and secondary fluorescence (F) correction) interactive method supported by Esprit 1.9 "Quantify Method Editor" option software.
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