The mechanism of the mechanically assisted mineral carbonation of commercial olivine under the flow of a carbon dioxide (CO2)/nitrogen (N2) mixture has been elucidated by ex situ powder X-ray diffraction and Fourier-transform infrared spectroscopy. The overall CO2 conversion depends on the rotational frequency of the mill’s engine, and it reaches 85% within 90 min of mechanical treatment at a flow rate of 2.5 L min−1. By tuning the frequency of rotation, the kinetics of CO2 conversion unveil a complex reaction pathway involving subsequent steps. Structural analyses suggest that clinochlore, a magnesium (Mg-)- and iron (Fe-)-containing aluminosilicate gathered among the components of olivine, is formed and consumed in different stages, thus promoting the CO2 sequestration that eventually results in the formation of hydrated and anhydrous Mg-based carbonates.
A 3D-printable, ARDUINO-based multipurpose X-ray stage of compact dimensions enabling in situ electric field and temperature-dependent measurements is put into practice and tested here. It can be routinely applied in combination with a technique of structural characterization of materials. Using high-performance X-ray laboratory equipment, two investigations were conducted to illustrate the device’s performance. The lattice characteristics and microstructure evolution of piezoelectric ceramics of barium titanate, BaTiO3 (BT), and barium calcium zirconate titanate, with compositions of (Ba0.92Ca0.08) (Ti0.95Zr0.05)O3 (BC8TZ5), were studied as a function of the applied electric field and temperature. The X-ray stage is amenable as an off-the-shelf device for a diffraction line in a synchrotron. It provides valuable information for poling piezoceramics and subsequent optimization of their performance.
Replacement of the ubiquitous lead titanate zirconate piezoceramics is still a challenge involving sustainable materials and processes. An extended effort has been paid for the optimization of the properties of (K 0.5 Na 0.5 )NbO 3 (KNN) lead‐free piezoceramics at the expenses of high‐energetic budget. A sustainable solid‐state processing with potential for industrial scaling (knowledge‐based, sustainable, reproducible, and cost‐effective) is still lacking. In this work, an efficient solution is proposed using the well‐known and noncontaminant attrition‐ball‐milling of the mixture of reagents for only 3 h, prior to the synthesis tests at increasing temperatures. After calcination at only 450 °C/2 h, 60 wt% KNN is achieved. Moreover, after 850 °C/2 h the calcined powder becomes a pure KNN. A second ball‐milling of powder calcined at 700850 °C gives place to populations of nanostructured particles (380–40 nm, respectively). The milled powder calcined at 700 °C is pressureless sintered in air for 2 h at 1050 and 1100 °C, leading to coarse grained ceramics. Milled powder calcined at 750 and 850 °C, sintered at the same conditions, produces fine grain homogeneous microstructures. Ceramics show an orthorhombic Amm2 pure KNN perovskite phase, as seen by x‐ray diffraction and Rietveld analysis. The piezoelectric values ( d33 = 115 pC/N, d31 = − 22 pC/N, kp = 20%, kt = 40%) are exceptional when derived from such a straightforward solid‐state route.
A single (Ba0.85Ca0.15)(Zr0.10Ti0.90)O3 phase material with a tetragonal structure is processed and synthesized with a modified Pechini method using ethylenediaminetetraacetic acid and glycerol as chelating and esterifying agents, respectively. The complete chemical transformation to the desired phase is achieved at 900 °C, which is 300 °C lower than conventional synthesis methods. Its consolidation, reaching up to 91% relative density, is carried out at 1400 °C. It is clearly demonstrated that the use of ethylenediaminetetraacetic acid and glycerol reagents is particularly beneficial for inducing a homogeneous grain size distribution (10 μm), which leads to very promising electromechanical properties (d33 = 451 pC/N; d31 = 160 pC/N; kp = 0.40; = 4790 and Qm = 358) of the densified system.
The mechanism of the mechanically assisted mineral carbonation of commercial olivine under flow of CO2/N2 mixture has been elucidated by ex situ powder X-ray diffraction and Fourier-transform infrared spectroscopy. The overall CO2 conversion depends to the rotation frequency of the mill’s engine, and reached 85% within 90 minutes of mechanical treatment, at a flow rate of 2.5 l min-1. By tuning the frequency rotation, the kinetics of CO2 conversion changed from a sigmoid behaviour into a more complex reaction pathway, involving subsequent steps. The structural analyses suggest the clinochlore, a Mg- and Fe- containing aluminosilicate gathered among the components of olivine, is formed and consumed in different stages, thus promoting the CO2 sequestration that eventually results into the formation of hydrated and anhydrous Mg-based carbonates.