Juan Carlos Rendon-Angeles

The sol–gel coprecipitation method is highly efficient for synthesising a wide range of binary perovskite solid solutions (SSs), which have been under exhaustive study due to their semiconductor and catalytic properties. Therefore, we conducted a systematic study to extend the chemical stability of the cubic structure in Zr⁴⁺-rich SS in the system SrTiO₃–SrZrO₃. The proposed new approach involves in situ gel coprecipitation and simultaneous hydrothermal processing, which was conducted at standard conditions (200 °C for 6 h) in a KOH (5 M) solution under stirring at 130 rpm. The formation of the cubic perovskite-structured SS occurred in the compositional range from 10.0 to 100.0 mol% Ti⁴⁺. The particle crystallisation was achieved via the dissolution-crystallisation mechanism, which proceeded rapidly, aided by preliminary gel dehydration and vigorous stirring. The prepared particles, either orthorhombic or cubic, have a unique morphology, resembling a pseudocuboidal shape with rounded edges. The particle size decreases as the Ti⁴⁺ content in the SSs increases, due to improved gel solubility. The band gap of the cubic intermediate SSs is sharp, ranging from 3.12 to 3.57 eV; thus, these perovskites can be applied in the development of semiconductor devices and in catalysis. These powders can also be employed as cool pigments due to their high NIR solar irradiance of 80.22%.

Recently, the development of nanoparticle pigments has attracted interest in chemical preparation due to their potential functional properties, such as phosphate-based pigments. The present research focuses on the feasibility of synthesising the BaCr₂(P₂O₇)₂ pigment under hydrothermal conditions. The effect of the microstructural features of ceramic pigments (the crystalline structure, morphology, and particle size) on their optical properties (colour and reflectance) was also studied. The BaCr₂(P₂O₇)₂ compound was prepared in different fluid media, including water and NaOH solutions (0.5–1.0 M), at several reaction temperatures (170–240 °C) and intervals (6–48 h). The single-phase BaCr₂(P₂O₇)₂ did not crystallise without by-products (BaCr₂O₁₀, BaCr₂(PO₇)₂) in water and the alkaline solutions, even at 240 °C for 48 h; in these fluids, the ionic Cr³⁺ species oxidised to Cr⁶⁺. In contrast, the BaCr₂(P₂O₇)₂ single-phase crystallisation was favoured by adding urea as a reductant agent (25.0–300.0 mmol). Monodispersed BaCr₂(P₂O₇)₂ fine particles with a mean size of 44.0 nm were synthesised at a low temperature of 170 °C for 6 h with 0.5 M NaOH solution in the presence of 50.0 mmol urea. The phosphate pigment particle grew to approximately 62.0 nm by increasing the treatment temperature to 240 °C. A secondary dissolution–recrystallisation achieved after 24 h triggered a change in the particle morphology coupled with the incrementation of the concentration of NaOH in the solution. The pyrophosphate BaCr₂(P₂O₇)₂ pigments prepared in this study belong to the green colour spectral space according to the CIELab coordinates measurement, and exhibit 67.5% high near-infrared (NIR) solar reflectance.

In recent decades, perovskite-type compounds (ABB′O₃) have been exhaustively studied due to their unique ferroelectric properties. In this work, a systematic study aiming to prepare fine particles in the binary system SrZrO₃–SrTiO₃ was conducted under hydrothermal conditions in a KOH (5 M) solution at 200 °C for 4 h under a constant stirring speed of 130 rpm. The precursors employed were SrSO₄ powder ( x > 100.0 mol% Ti⁴⁺. The XRD results revealed the formation of two crystalline phases rich in Zr⁴⁺, an orthorhombic structured SrZr_0.93Ti_0.07O₃ and a cubic structured SrZr_0.75Ti_0.25O₃ within the compositional range of 0.1–0.5 mol of Ti⁴⁺. A cubic perovskite structured solid solution, SrTi_1-xZr_xO₃, was preferentially formed within the compositional range of 0.5 > x > 0.1 mol% Ti⁴⁺. The SrZrO₃ and SrZr_0.93Ti_0.07O₃-rich phases had particle sizes averaging 3 μm with a cubic morphology. However, a remarkable reduction in the particle size occurred on solid solutions prepared with hydrous Ti-gel over contents of 15 mol% Ti⁴⁺ in the reaction media, resulting in the formation of nanosized particle agglomerates with a cuboidal shape self-assembled via a 3D hierarchical architecture, and the sizes of these particles varied in the range between 141.0 and 175.5 nm. The limited coarsening of the particles is discussed based on the Zr-gel and Ti-gel dehydration capability differences that occurred under hydrothermal processing.

In recent decades, perovskite-type compounds (ABB′O3) have been exhaustively studied due to their unique ferroelectric properties. In this work, a systematic study aiming to prepare fine particles in the binary system SrZrO₃–SrTiO₃ was conducted under hydrothermal conditions in a KOH (5 M) solution at 200 °C for 4 h under a constant stirring speed of 130 rpm. The precursors employed were SrSO₄ powder (< 38 μm size) and coprecipitated hydrous gels of Zr(OH)₄•9.64 H₂O (Zr-gel) and Ti(OH)₄•4.5H₂O (Ti-gel), which were mixed according to the stoichiometry of the SrZr_1-xTixO₃ in the compositional range of 0.0>x>100.0 mol% Ti⁴⁺. The XRD results revealed the formation of two crystalline phases rich in Zr⁴⁺, an orthorhombic structured SrZr0.93Ti0.07O3 and a cubic structured SrZr0.75Ti0.25O3 within the compositional range of 0.1–0.5 mol of Ti4+. A cubic perovskite-structured solid solution, SrTi1-xZrxO3, was preferentially formed within the compositional range of 0.5>x>0.1 mol% Ti⁴⁺. The SrZrO₃ and SrZr_0.93Ti_0.07O₃-rich phases had particle sizes averaging 3 m with a cubic morphology. However, a remarkable reduction in the particle size occurred on solid solutions prepared with hydrous Ti-gel over contents of 15 mol% Ti⁴⁺ in the reaction media, resulting in the formation of nanosized particles agglomerates with cuboidal shape self-assembled via a 3D hierarchical architecture, the sizes of these particles varied in the range between 141.0–175.5 nm. The limited coarsening of the particles is discussed based on the Zr-gel and Ti-gel dehydration capability differences that occurred under hydrothermal processing.

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Oxide dispersion strengthened (ODS) ferritic alloys are structural materials used in nuclear fusion reactors, which exhibit enhanced mechanical properties, as well as corrosion and irradiation resistance. In the present work, ODS ferritic alloys with composition Fe-14Cr-1.5W-0.4Ti-(0, 0.4, 0.8) Y2O3 (in wt.%) were prepared employing high energy milling (HEM) followed by Spark Plasma Sintering (SPS). The particle size distribution (PSD) of the milled powders was characterized by laser diffraction. These powders and the sintered materials produced were characterized using X-ray diffraction (XRD), and scanning electron microscopy (SEM). The sintered materials were also characterized by dilatometry, diametral compression, Vickers microhardness, and corrosion rate tests. The largest Young’s modulus, microhardness, and dimensional shrinkage/expansion were obtained for the 0.8 wt.% Y2O3 alloy. However, this alloy was the least ductile. Furthermore, the 0.8 wt.% Y2O3 alloy was the one with the least dimensional change. According to the potentiodynamic polarization studies, it was found that the protective layer of Cr2O3 formed on the surface of the three alloys studied was less effective for the yttria-free alloy, since in this case the rupture of such protective layer occurred earlier than for the case of the yttria-containing alloys. Based on these results, it is suggested that the 0.8 wt.% Y2O3 alloy having fine microstructure could constitute a potential alternative as a structural material for Gen IV-type reactors.

The synthesis of partially substituted silicon hydroxyapatite (Si-HAp) nanopowders was systematically investigated via the microwave-assisted hydrothermal process. The experiments were conducted at 150 °C for 1 h using TMAS (C₄H₁₃NO₅Si₂) as a Si⁴⁺ precursor. To improve the Si⁴⁺ uptake in the hexagonal structure, the Si precursor was supplied above the stoichiometric molar ratio (0.2 M). The concentration of the TMAS aqueous solutions used varied between 0.3 and 1.8 M, corresponding to saturation levels of 1.5–9.0-fold. Rietveld refinement analyses indicated that Si incorporation occurred in the HAp lattice by replacing phosphate groups (PO₄³⁻) with the silicate (SiO₄⁻) group. FT-IR and XPS analyses also confirmed the gradual uptake of SiO₄⁻ units in the HAp, as the saturation of Si⁴⁺ reached 1.8 M. TEM observations confirmed that Si-HAp agglomerates had a high crystallinity and are constituted by tiny rod-shaped particles with single-crystal habit. Furthermore, a reduction in the particle growth process took place by increasing the Si⁴⁺ excess content up to 1.8 M, and the excess of Si⁴⁺ triggered the fine rod-shaped particles self-assembly to form agglomerates. The agglomerate size that occurred with intermediate (0.99 mol%) and large (12.16 mol%) Si contents varied between 233.1 and 315.1 nm, respectively. The excess of Si in the hydrothermal medium might trigger the formation of the Si-HAp agglomerates prepared under fast kinetic reaction conditions assisted by the microwave heating. Consequently, the use of microwave heating-assisted hydrothermal conditions has delivered high processing efficiency to crystallize Si-HAp with a broad content of Si⁴⁺.

One-pot hydrothermal preparation of Ca₃Cr₂Si₃O₁₂ uvarovite nanoparticles under alkaline conditions was investigated for the first time. The experimental parameters selected for the study considered the concentration of the KOH solvent solution (0.01 to 5.0 M), the agitation of the autoclave (50 rpm), and the nominal content of Si⁴⁺ (2.2–3.0 mole). Fine uvarovite particles were synthesised at 200 °C after a 3 h interval in a highly concentrated 5.0 M KOH solution. The crystallisation of single-phase Ca₃Cr₂Si₃O₁₂ particles proceeded free of by-products via a one-pot process involving a single-step reaction. KOH solutions below 2.5 M and water hindered the crystallisation of the Ca₃Cr₂Si₃O₁₂ particles. The hydrothermal treatments carried out with stirring (50 rpm) and non-stirring triggered the crystallisation of irregular anhedral particles with average sizes of 8.05 and 12.25 nm, respectively. These particles spontaneously assembled into popcorn-shaped agglomerates with sizes varying from 66 to 156 nm. All the powders prepared by the present method exhibited CIE-L*a*b* values that correspond to the Victoria green colour spectral space and have a high near infrared reflectance property. The particle size and structural crystallinity are factors affecting the Victoria pigment optical properties, such as CIE-L*a*b* values, green tonality, and near-infrared reflectance.