Highscore software

An X−ray diffractometer (Philips X’PERT MPD, Malvern Panalytical Inc., Westborough, MA, USA) was used to obtain wide−angle XRD patterns. The ground samples were exposed to the radiation of Co Kα (0.179 nm) on the XRD machine. Using the HighScore software (Malvern Panalytical Inc., Westborough, MA, USA), data were converted to Cu Kα radiation−based 2θ values between 2θ = 5° and 30°.

Scanning
electron microscopy (SEM) was performed by using a Zeiss Sigma microscope
with a coupled Oxford Instruments energy dispersive X-ray spectroscopy
(EDS) detector. EDS was conducted and analyzed using Aztec software.
X-ray diffraction (XRD) was conducted using an Aeris desktop machine
with data analysis performed by means of Highscore software (Malvern
Panalytical). To understand the electrochemical trend observed in
terms of electrode microstructures, we performed an X-ray computerized
tomography (XCT) analysis of CMF electrodes. The CMF sample was scanned
on a ZEISS Vectra 520 for determining the surface microstructures
of interest. The specimen was scanned at a voltage of 80 kV, a power
of 7 W, an exposure time of 20 s, and a minimum of 10× over 1601
projections as reported previously.^{16 (link)}

The crystallinity of the powder samples was determined with an X’Pert PRO MPD PW3040/60 X-ray diffractometer (Malvern Panalytical, Malvern, UK) equipped with Cu Kα radiation. An aluminum holder was used to analyze the samples over a 2θ range of 5–35° at a rate of 2°/min. The PANalytical High Score software was used to analyze the diffractogram.

The surface morphology and composition of Mg samples after 24-h immersion degradation under flow and static conditions were characterized using the scanning electron microscope (SEM, Nova NanoSEM 450, FEI Co., Hillsboro, OR, USA) with the attached detector for energy dispersive X-ray spectroscopy (EDS, Nova NanoSEM 450, FEI Co., Hillsboro, OR, USA, X-Max 450). The surface elemental composition and distribution were analysed using the EDS detector and the AZtecEnergy software (Oxford Instruments, Abingdon, Oxfordshire, UK). Elemental mapping combined with SEM was used for investigating the degradation products on Mg samples after 24-h immersion degradation under flow and static conditions while EDS point analysis was used for analysing specific features in the degradation layers. The SEM and EDS analyses were carried out at an accelerating voltage of 20 kV and the SEM images were obtained at an original magnification of 500 x and 5000x. The phases of Mg after 24-h immersion study under flow and static condition were analysed using X-ray diffraction (XRD; Empyrean, PANalytical) at 45 KV and 40 mA with 2θ angles from 10° to 80° at a step size of 0.002°. The diffraction peaks were identified based on the international center for diffraction data database using HighScore software (PANAlytical).

Powder diffraction data were collected in focusing mode on a Panalytical Empyrean X-ray diffractometer equipped with Bragg–Brentano HD optics, a sealed-tube copper X-ray source (λ = 1.54178 Å), Soller slits on both the incident and receiving optics sides, and a PixCel3D Medipix detector. Samples were hand ground for 20 minutes using an agate mortar and pestle and packed in metal sample cups with a sample area 16 mm wide and 2 mm deep. 1/4° anti-scatter slits and 1/16° divergence slits as well as a 4 mm mask were chosen based on sample area and starting θ angle. Data were collected between 5 and 90° in 2θ using Data Collector software (PANalytical, 2019 ▸ ). Rietveld refinements were performed against the models of the single-crystal-structure data sets using the HighScore software (PANalytical, 2018 ▸ ). Refinement of preferred orientation was included using a spherical harmonics model.
Differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA) data were measured using a TA Instruments Q20 DSC with heating rates of 5°C min⁻¹. The sample was run in an alumina open pan from 25 to 100°C. The DSC and TGA traces are given in the Supporting Information (Fig. S3).