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Materials 2022, 15, 2946 6 of 20 behavior was conducted by confirming whether the agglomerated masses that were found were impurities in the sand or something else that was formed during the cyclic heating. Energy-dispersive X-ray analysis (Jeol Limited, Akishima, Tokyo, EDX), together with a scanning electron microscope (Jeol Limited, Akishima, Tokyo, SEM) both by Jeol Limited (Akishima, Tokyo), were used to identify the elemental composition of the particulate materials. Qualitative and quantitative analyses were conducted to identify the types of elements that were present, as well as the percentage of each element’s concentration within the sample. Furthermore, an X-ray diffractogram (Billerica, Massachusetts, MA, USA, XRD) analysis was done using a Bruker D8 Discover multipurpose X-ray diffractometer (Billerica, Massachusetts, MA, USA) with CuKα source radiation to determine the crystallographic structure of the materials, as well as to determine the physical mechanisms responsible for the optical properties (color change) of the particles after exposure to heating. Bruker EVATM (Billerica, Massachusetts, MA, USA) was used for the matching and analyzing and interpretation of the XRD results. These tests and analyses were conducted on candi- date particulate materials “as received,” and on each heated sample (to 800 ◦C, 1000 ◦C, 1200 ◦C—6 h, and 1200 ◦C—500 h). The XRD patterns were obtained at room temperature. 3.3. Optical Properties The reflectivities of the candidate materials were measured using the ASD FieldSpe3 Portable Spectroradiometer device (Malvern Panalytical company, Cambridge, United Kingdom) shown in Figure 2 in the 350–2500 nm wavelength range. The instrument was calibrated with a certified reflectance standard provided by the Labsphere company. The tests were performed in a dark area to prevent the effects of reflection or diffusion of ambient light on the measurements. A sufficient thickness of each tested particulate material was placed on the sample stand to make sure that the stand was completely covered with particulates and light reflected to the sensor was only from the sample and not from the base of the stand. This procedure was performed to make sure that the light transmission was equal to zero. All of the reflectivity measurements for each sample were repeated following this protocol seven times. All of the particulate reflectance measurements were conducted at ambient temperature. Equation (1) was used to calculate the absorbance: Rλ + Tλ + Aλ = 1 (1) where R, T, and A indicate the reflectance, transmittance, and absorptance, respectively; while λ indicates the wavelength at which the measurement was performed. Considering a transmittance equal to zero, the absorptance was found using Equation (2): Aλ = 1 − Rλ (2) To find the weighted solar absorptance of the candidate particulate materials, the ab- sorptance values were weighted with respect to the values of the solar spectrum according to ASTM G173-03 and the air mass of AM1.5, as shown in Equation (3) [25]: Aweighted = AM1.5 (W/ m2nm )· Ameasured (3) Finally, a trapezoidal integration was executed under the curve to calculate the total absorptance of the material: where Ai is the first low range value, Ai+1 is the higher range value, and N is the number of values. N A1+Ai+1 Total Absorptance = ∑ 2 (4) i=1 N−1PDF Image | Low-Cost Particulates Used as Energy Storage and Heat-Transfer Medium
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