Eds system

The bioactivity assay was performed following “Implants for surgery—In vitro evaluation for apatite-forming ability of implant materials” (ISO 23317:2014) and as stablished by Kokubo et al. [39 (link)]. Pellets with 7 mm of diameter were immersed in simulated body fluid (SBF), an ionic solution with composition similar to the human plasma (Table 3), for 12 h, 24 h, 48 h, 96 h, 336 h and 672 h. The volume of SBF ( $V_s)$ , in mm³, placed in contact with the pellets considering their apparent surface area as indicated in the following equation: $$V_s=100· S_a$$
where $S_a$ is the superficial area of the sample. All pellets after immersion were washed with ultrapure water. The sample’s surface was analyzed before and after immersion times with SEM-EDS from TESCAN VEGA 3 (TESCAN, Brno, Czech Republic). A semi-quantitative study of the atomic elements percentage on the surface’s samples was made using the Bruker EDS system coupled to the microscope. In addition, the pH of the SBF medium for the all samples was measured at the end of the immersion times, as previously described [40 (link)]. The assay was performed in duplicate.

The morphology of the sample’s surface was evaluated using a SEM microscope from TESCAN (model Vega 3). A semi-quantitative examination of the chemical composition of the samples was made using the Bruker EDS system coupled to the microscope. Some regions of each sample were analysed using a square scanning area of 100 µm × 100 µm. Prior to the visualization, the sample’s surface was coated with carbon, reducing the surface electron resistivity.
The particle size and distribution were measured by the HORIBA Scientific LA-960V2 wet circulation system. The analysis was based on the principle of laser diffraction, and the particle size calculation was based on the Fraunhofer and Mie models. The measurements were assessed with the samples (Base and Zn2 powder) dispersed in distilled water.

Energy dispersive X-ray spectroscopy (EDS) was conducted in a Zeiss MERLIN Scanning Electron Microscope (SEM) equipped with a Bruker EDS system. For the EDS measurements, a map acquisition of the He⁺ irradiated WSe₂ film was taken over a ~6 × 8 μm area with a 15 min collection time. A beam energy of 4 keV and beam current of 0.7 nA were used to excite the sample and generate the X-ray spectra.

Thin sections of subglacial calcites were observed by optical and epifluorescence microscopy. One millimetre thick wafers of age-equivalent subglacial crusts were polished and ultrasonically cleaned. Imaging at nm-scale resolution on uncoated surfaces was carried out by field emission scanning electron microscopy with a ZEISS Sigma Variable Pressure field emission scanning electron microscopy equipped with Bruker EDS system in backscattered electron mode at the Electron Microscope and X-ray unit of the University of Newcastle, Australia. Semi-quantitative chemical microanalyses were carried out in situ on spot areas of ca. 500 nm diameter and the normalized weight % calculated with the Quantax software (Bruker nano). Epifluorescence was excited by light at 250–350 nm wavelength and the most common emission band was in the 450–550 nm.
Powder X-ray diffraction on clean calcite and Dm was carried out on a PANalytical h-h diffractometer equipped with a Cu X-ray tube operating at 40 kV and 40 mA. Scans were performed over the range 3–80° with an integrated step size of 0.017° and a counting time of 100 s per step. Identification of minerals, and cell parameter determination were performed using High Score Plus and the ICSD database (PANalytical).

SEM images were obtained using a Hitachi SU8220 device. The SEM elemental mapping analysis was conducted using an EDX (Oxford EDS, with INCA software). TEM images were obtained using a JEOL JEM-2100F microscope with an acceleration voltage of 200 kV. Elemental mapping in TEM was conducted using the Bruker EDS System. The XRD analysis was carried out using a Bruker D8 Advance with filtered Cu-Kα radiation (40 kV and 40 mA, λ = 0.154 nm); the step scan was 0.02°, the 2θ range was 2–10° or 2–70°, and the step time was 2 s. FTIR was conducted by Bruker VERTEX 33 units in the wavenumber range of 400–4000 cm⁻¹. The XPS analysis was performed using an ESCALAB 250 spectrometer (Thermo Fisher Scientific) with monochromated Al-Kα radiation (1486.6 eV) under a pressure of 2 × 10⁻⁹ Torr. The AFM images were obtained using a Bruker Multi Mode 8 scanning probe microscope (SPM, VEECO) in tapping mode. The TG measurement was analyzed on a Netzsch STA 449F3 instrument under the flow of N₂. The adsorption isotherms of H₂, CO₂, N₂, and CH₄ on the MXene membranes were measured using a Micromeritics (ASAP 2460) instrument. The mechanical tests were performed using an Instron-5565 universal testing machine (USA).