Search Results (12)

The recent upgrading of synchrotron radiation (SR) sources has favored, in the last few years, the construction and design of beamlines optimized for the study of cultural heritage materials, which may require ad hoc setups, specific spatial resolutions, and detection limits. In the field of cultural heritage, integrated approaches combining different techniques are often required, even at large facilities, where some beamlines offer the possibility of performing different types of measurements at the same point of analysis, complementing preliminary information usually obtained by conventional laboratory and/or portable in situ methods. An overview of the last ten years of synchrotron applications for the study of pigments is given, with discussion of upstream and downstream challenges to methods and techniques. The possibilities offered by the synchrotron techniques are illustrated by a case study of a particular class of painted ceramics, as an example of different research questions that are solved by a combination of SR-based methods. Full article

In the estuary and nearshore environments, suspended particulate matter (SPM) plays a particularly important role. This article presents a study on the suspended particulate matter and microbial communities in the euphotic zone of China’s nearshore and estuarine regions. The study used various analytical techniques, including ICP-OES, SR-XRD, confocal Raman microscopy, ESEM, and EDX, to investigate the spatial distribution and elemental and mineral compositions of the suspended particulate matters. The study found that semiconducting minerals, such as iron oxide, sulfide minerals (hematite, goethite, and pyrrhotite), and titanium oxide minerals (rutile and anatase), were widely present in the suspended particulate matter. This discovery highlights the photochemical activity of suspended particulate matter in the euphotic zone. Furthermore, a correlation analysis of microbial communities revealed that the content of suspended particulate matter was positively correlated with denitrifying bacteria and metal-reducing bacteria in seawater. This study provides valuable insight into the ecosystem dynamics and biogeochemical cycling of estuaries and coastal seas, which are critical for sustaining the biodiversity and productivity of these ecosystems. Full article

Copper-based chalcogenides have emerged as promising thermoelectric materials due to their high thermoelectric performance, tunable transport properties, earth abundance and low toxicity. We have presented an overview of experimental results and first-principal calculations investigating the thermoelectric properties of various polymorphs of Cu₂SnS₃ (CTS), Cu₂ZnSnS₄ (CZTS), and Cu₂ZnSnSe₄ (CZTSe) synthesized by high-energy reactive mechanical alloying (ball milling). Of particular interest are the disordered polymorphs of these materials, which exhibit phonon-glass–electron-crystal behavior—a decoupling of electron and phonon transport properties. The interplay of cationic disorder and nanostructuring leads to ultra-low thermal conductivities while enhancing electronic transport. These beneficial transport properties are the consequence of a plethora of features, including trap states, anharmonicity, rattling, and conductive surface states, both topologically trivial and non-trivial. Based on experimental results and computational methods, this report aims to elucidate the details of the electronic and lattice transport properties, thereby confirming that the higher thermoelectric (TE) performance of disordered polymorphs is essentially due to their complex crystallographic structures. In addition, we have presented synchrotron X-ray diffraction (SR-XRD) measurements and ab initio molecular dynamics (AIMD) simulations of the root-mean-square displacement (RMSD) in these materials, confirming anharmonicity and bond inhomogeneity for disordered polymorphs. Full article

The structural and thermophysical characteristics of an Ni-rich NiTi alloy rod produced on a laboratory scale was studied. The soak temperature of the solution heat-treatment steps above 850 °C taking advantage of the precipitate dissolution to provide a matrix homogenization, but it takes many hours (24 to 48) when used without thermomechanical steps. Therefore, the suitable reheating to apply between the forging process steps is very important, because the product’s structural characteristics are dependent on the thermomechanical processing history, and the time required to expose the material to high temperatures during the processing is reduced. The structural characteristics were investigated after solution heat treatment at 900 °C and 950 °C for 120 min, and these heat treatments were compared with as-forged sample structural characteristics (one hot deformation step after 800 °C for a 30 min reheat stage). The phase-transformation temperatures were analyzed through differential scanning calorimetry (DSC), and the structural characterization was performed through synchrotron radiation-based X-ray diffraction (SR-XRD) at room temperature. It was observed that the solution heat treatment at 950 °C/120 min presents a lower martensitic reversion finish temperature (A_f); the matrix was fully austenitic; and it had a hardness of about 226 HV. Thus, this condition is the most suitable for the reheating stages between the hot forging-process steps to be applied to this alloy to produce materials that can display a superelasticity effect, for applications such as crack sensors or orthodontic archwires. Full article

This paper reports the precise analysis of the eutectic mixing behavior of 1,3-distearoyl-2-oleoyl-sn-glycerol (SOS) and trilaurin (LLL), as a typical model case of the mixture of cocoa butter (CB) and cocoa butter substitute (CBS). SOS was mixed with LLL at several mass fractions of LLL (w_LLL); the mixtures obtained were analyzed for polymorphic phase behavior using differential scanning calorimetry (DSC) and synchrotron radiation X-ray diffractometry (SR-XRD). In melt crystallization with constant-rate cooling, SOS and LLL formed eutectics in their metastable polymorphs, allowing the occurrence of a compatible solid solution at w_LLL ≥ 0.925. With subsequent heating, the resultant crystals transformed toward more stable polymorphs, then melted in a eutectic manner. For mixtures aged at 25 °C after melt crystallization, eutectics were found in the extended w_LLL region, even at w_LLL = 0.975. These results indicate that phase separation between SOS and LLL progressed in their solid solution under stabilization. The crystal growth of the separated SOS fraction may cause fat-bloom formation in compound chocolate containing CB and CBS. To solve this problem, the development of retardation techniques against phase separation is expected. Full article

T92 heat-resistant steel is among the most promising candidate materials for structural components in the Generation IV (GEN-IV) reactors. The effects of tempering temperature on the microstructure and mechanical properties of the T92 steel were studied. The microstructural evolution of the T92 steel subjected to various temperatures of the tempering process were investigated using scanning electron microscopy (SEM), transmission electron microscopy (TEM), and synchrotron radiation X-ray diffraction (SR-XRD). The mechanical properties of Vickers hardness, tensile test, and impact test were also investigated. The results showed that the grain size of the prior austenite does not significantly change during the tempering process, while the width of the martensite lath and the size of the carbide precipitates increased with increasing tempering temperature. The hardness and yield strength of the T92 steel decreased, and the plasticity and impact energy increased with increasing tempering temperature. Coarsening of the carbide precipitates during the tempering process was considered to be the dominant factor that reduced the yield strength in the T92 steel. Full article

The determination of microstructural details for powder materials is vital for facilitating their selective laser melting (SLM) process. Four widely used steels (316L, H13, P20 and 18Ni300) have been investigated to detail their powders’ microstructures as well as laser absorptivity to understand their SLM processing from raw material perspective. Phase components of these four steel powders were characterized by X-ray diffraction (XRD), synchrotron radiation X-ray diffraction (SR-XRD) and scanning electron microscopy (SEM). X-ray photoelectron spectroscopy (XPS) and transmission electron microscopy (TEM) were utilized to reveal the surface structure of these four steel powders. It is found that phase components of H13, P20 and 18Ni300 are mainly composed of martensite and a small amount of austenite due to the high cooling rate during gas atomization processing, while 316L is characterized by austenite. XPS results show that the four steel powders all possess a layered surface structure, consisting of a thin iron oxide layer at the outmost surface and metal matrix at the inner surface. It is found that the presence of such oxide layer can improve the absorptivity of steel powders and is beneficial for their SLM process. Full article

The fine phase transformation process of chalcocite (Cu₂S) leaching in acidic ferric sulfate solution was studied by leaching experiments and synchrotron radiation X-ray diffraction (SRXRD) tests. The results showed that the dissolution process of chalcocite was divided into two stages. In the first stage, Cu₂S was firstly transformed to Cu₅FeS₄ and Cu_2−xS, then the galvanic effect between Cu₅FeS₄ and Cu_2−xS accelerated the dissolution process of Cu_1.8S → Cu_1.6S → CuS, and finally Cu₅FeS₄ was also transformed to CuS. While in the second stage, CuS was transformed to elemental sulfur, which formed the passivation layer and inhibited the leaching of chalcocite. Specifically, Cu₅FeS₄ was detected during the chalcocite leaching process by SRXRD for the first time. This research is helpful for revealing the detailed leaching process of chalcocite. Full article

The catalytic mechanism of Ag⁺ for chalcopyrite bioleaching by mesophilic culture (at 30 °C) and thermophilic culture (at 48 °C) was investigated using synchrotron radiation-based X-ray diffraction (SR-XRD) and S K-edge and Fe L-edge X-ray absorption near edge structure (XANES) spectroscopy. Bioleaching experiments showed that copper extraction from chalcopyrite bioleaching by both cultures was promoted significantly by Ag⁺, with more serious corrosion occurring on the minerals surface. SR-XRD and XANES analyses showed that the intermediates S⁰, jarosite and secondary minerals (bornite, chalcocite and covellite) formed for all bioleaching experiments. For these secondary minerals, the formation of bornite and covellite was promoted significantly in the presence of Ag⁺ for both cultures, while Ag⁺ has almost no effect on the formation of chalcocite. These results provided insight into the catalytic mechanisms of Ag⁺ to chalcopyrite bioleaching by the mesophilic and thermophilic cultures, which are both probably due to the rapid formation of bornite by Ag⁺ and the conversion of bornite to covellite. Full article

The effect of Ni-content on phase transformation behavior of NiTi-20 at. % Zr high temperature shape memory alloy (HTSMA) is investigated over a small composition range, i.e., 49.8, 50.0 and 50.2 at. % Ni, by differential scanning calorimetry (DSC), high-energy synchrotron radiation X-ray diffraction (SR-XRD), scanning electron microscopy (SEM), and transmission electron microscopy (TEM). All samples show a monoclinic B19^′ martensitic structure at room temperature. It is shown that even with these small variations in Ni-content, the alloy shows vastly different transformation temperatures and responds in a drastically different manner to aging treatments at 550 and 600 °C. Lastly, a discussion on H-phase composition with respect to bulk composition is presented. Full article

The nature and size of the real active species of nanoparticulated metal supported catalysts is still an unresolved question. The technique of choice to measure particle sizes at the nanoscale, HRTEM, has a practical limit of 1 nm. This work is aimed to identify the catalytic role of subnanometer species and methods to detect and characterize them. In this frame, we investigated the sensitivity to redox pretreatments of Ag/Fe/TiO₂, Ag/Mg/TiO₂ and Ag/Ce/TiO₂ catalysts in CO oxidation. The joint application of HRTEM, SR-XRD, DRS, XPS, EXAFS and XANES methods indicated that most of the silver in all samples is in the form of Ag species with size <1 nm. The differences in catalytic properties and sensitivity to pretreatments, observed for the studied Ag catalysts, could not be explained taking into account only the Ag particles whose size distribution is measured by HRTEM, but may be explained by the presence of the subnanometer Ag species, undetectable by HRTEM, and their interaction with supports. This result highlights their role as active species and the need to take them into account to understand integrally the catalysis by supported nanometals. Full article

The features of the crystal structures and spontaneous polarization (P_s) under an electric field (E) have been reviewed for (1 − x)(Bi_0.5Na_0.5)TiO₃–xBaTiO₃ (BNT–BT). In-situ measurements of high-resolution synchrotron radiation X-ray diffraction (SR-XRD) under electric fields show that single crystals with x = 0 (BNT) and 5% have a monoclinic distortion in space group Cc at 25 °C. The SR-XRD study combined with density functional theory (DFT) calculations demonstrates that BNT–5%BT exhibits a rotation of P_s in the monoclinic a–c plane by 2° under an E of 70 kV/cm along the <001> pseudo-cubic direction, which is much larger than BNT. Full article