Folding a 2-D powder diffraction image into a 1-D scan: a new procedure

A new procedure aiming at folding a powder diffraction 2-D into a 1-D scan is presented. The technique consists of three steps: tracking the beam centre by means of a Simulated Annealing (SA) of the diffraction rings along the same axis, detector tilt and rotation determination by a Hankel Lanczos Singular Value Decomposition (HLSVD) and intensity integration by an adaptive binning algorithm. The X-ray powder diffraction (XRPD) intensity profile of the standard NIST Si 640c sample is used to test the performances. Results show the robustness of the method and its capability of efficiently tagging the pixels in a 2-D readout system by matching the ideal geometry of the detector to the real beam-sample-detector frame. The whole technique turns out in a versatile and user-friendly tool for the $2\vartheta$ scanning of 2-D XRPD profiles.Comment: 11 pages, 1 table, 2 figure

The effects of MgO, Na2O and SO3 on industrial clinkering process: phase composition, polymorphism, microstructure and hydration, using a multidisciplinary approach

Preprint publicado en: Materials Characterization Volume 155, September 2019, 109809The present investigation deals with how minor elements (their oxides: MgO, Na2O and SO3) in industrial kiln feeds affect (i) chemical reactions upon clinkering, (ii) resulting phase composition and microstructure of clinker, (iii) hydration process during cement production. Our results show that all these points are remarkably sensitive to the combination and interference effects between the minor chemical species mentioned above. Upon clinkering, all the industrial raw meals here used exhibit the same formation temperature and amount of liquid phase. Minor elements are preferentially hosted by secondary phases, such as periclase. Conversely, the growth rate of the main clinker phases (alite and belite) is significantly affected by the nature and combination of minor oxides. MgO and Na2O give a very fast C3S formation rate at T > 1450 K, whereas Na2O and SO3 boost C2S After heating, if SO3 occurs in combination with MgO and/or Na2O, it does not inihibit the C3S crystallisation as expected. Rather, it promotes the stabilisation of M1-C3S, thus indirectly influencing the aluminate content, too. MgO increseases the C3S amount and promotes the stabilisation of M3-C3S, when it is in combination with Na2O. Na2O seems to be mainly hosted by calcium aluminate structure, but it does not induce the stabilisation of the orhtorhombic polymorph, as supposed to occur. Such features play a key role in predicting the physicalmechanical performance of a final cement (i.e. rate of hydration and hardening) when used as a bulding material.The present study has been partly funded by the project PRIN 2017 (2017L83S77), of the Italian Ministry for Education, University and Research (MIUR)

Piezoelectric effect and electroactive phase nucleation in self-standing films of unpoled PVDF nanocomposite films

Novel polymer-based piezoelectric nanocomposites with enhanced electromechanical properties open new opportunities for the development of wearable energy harvesters and sensors. This paper investigates how the dissolution of different types of hexahydrate metal salts affects β-phase content and piezoelectric response (d33) at nano-and macroscales of polyvinylidene fluoride (PVDF) nanocomposite films. The strongest enhancement of the piezoresponse is observed in PVDF nanocomposites processed with Mg(NO3)2·6H2O. The increased piezoresponse is attributed to the synergistic effect of the dipole moment associated with the nucleation of the electroactive phase and with the electrostatic interaction between the CF2group of PVDF and the dissolved salt through hydrogen bonding. The combination of nanofillers like graphene nanoplatelets or zinc oxide nanorods with the hexahydrate salt dissolution in PVDF results in a dramatic reduction of d33, because the nanofiller assumes a competitive role with respect to H-bond formation between PVDF and the dissolved metal salt. The measured peak value of d33reaches the local value of 13.49 pm/V, with an average of 8.88 pm/V over an area of 1 cm2. The proposed selection of metal salt enables low-cost production of piezoelectric PVDF nanocomposite films, without electrical poling or mechanical stretching, offering new opportunities for the development of devices for energy harvesting and wearable sensors

Dissolution enhancement of gliclazide using pH change approach in presence of twelve stabilizers with various physico-chemical properties

Purpose. The micronization using milling process to enhance dissolution rate is extremely inefficient due to a high energy input, and disruptions in the crystal lattice which can cause physical or chemical instability. Therefore, the aim of the present study is to use in situ micronization process through pH change method to produce micron-size gliclazide particles for fast dissolution hence better bioavailability. Methods. Gliclazide was recrystallized in presence of 12 different stabilizers and the effects of each stabilizer on micromeritic behaviors, morphology of microcrystals, dissolution rate and solid state of recrystallized drug particles were investigated. Results. The results showed that recrystallized samples showed faster dissolution rate than untreated gliclazide particles and the fastest dissolution rate was observed for the samples recrystallized in presence of PEG 1500. Some of the recrystallized drug samples in presence of stabilizers dissolved 100% within the first 5 min showing at least 10 times greater dissolution rate than the dissolution rate of untreated gliclazide powders. Micromeritic studies showed that in situ micronization technique via pH change method is able to produce smaller particle size with a high surface area. The results also showed that the type of stabilizer had significant impact on morphology of recrystallized drug particles. The untreated gliclazide is rod or rectangular shape, whereas the crystals produced in presence of stabilizers, depending on the type of stabilizer, were very fine particles with irregular, cubic, rectangular, granular and spherical/modular shape. The results showed that crystallization of gliclazide in presence of stabilizers reduced the crystallinity of the samples as confirmed by XRPD and DSC results. Conclusion. In situ micronization of gliclazide through pH change method can successfully be used to produce micron-sized drug particles to enhance dissolution rate

Structural and magnetic properties of Mn3-xCdxTeO6 (x = 0, 1, 1.5 and 2)

Mn3TeO6 exhibits a corundum-related A3TeO6 structure and a complex magnetic structure involving two magnetic orbits for the Mn atoms [*]. Mn3-xCdxTeO6 (x=0, 1, 1.5 and 2) ceramics were synthesized by solid state reaction and investigated using X-ray powder diffraction, electron microscopy, calorimetric and magnetic measurements. Cd2+ replaces Mn2+ cations without greatly affecting the structure of the compound. The Mn and Cd cations were found to be randomly distributed over the A-site. Magnetization measurements indicated that the samples order antiferromagnetically at low temperature with a transition temperature that decreases with increasing Cd doping. The nuclear and magnetic structure of one specially prepared 114Cd containing sample: Mn1.5(114Cd)1.5TeO6, was studied using neutron powder diffraction over the temperature range 2 to 295 K. Mn1.5(114Cd)1.5TeO6 was found to order in an incommensurate helical magnetic structure, very similar to that of Mn3TeO6 [*]. However, with a lower transition temperature and the extension of the ordered structure confined to order 240(10) {\AA}. [*] S. A. Ivanov et al. Mater. Res. Bull. 46 (2011) 1870.Comment: 20 pages, 8 figure

Possibility to realize spin-orbit-induced correlated physics in iridium fluorides

Recent theoretical predictions of "unprecedented proximity" of the electronic ground state of iridium fluorides to the SU(2) symmetric $j_{\mathrm{eff}}=1/2$ limit, relevant for superconductivity in iridates, motivated us to investigate their crystal and electronic structure. To this aim, we performed high-resolution x-ray powder diffraction, Ir L$_3$-edge resonant inelastic x-ray scattering, and quantum chemical calculations on Rb$_2$[IrF$_6$] and other iridium fluorides. Our results are consistent with the Mott insulating scenario predicted by Birol and Haule [Phys. Rev. Lett. 114, 096403 (2015)], but we observe a sizable deviation of the $j_{\mathrm{eff}}=1/2$ state from the SU(2) symmetric limit. Interactions beyond the first coordination shell of iridium are negligible, hence the iridium fluorides do not show any magnetic ordering down to at least 20 K. A larger spin-orbit coupling in iridium fluorides compared to oxides is ascribed to a reduction of the degree of covalency, with consequences on the possibility to realize spin-orbit-induced strongly correlated physics in iridium fluorides

Formation of Nanometer-Thick Water Layer at High Humidity on Dynamic Crystalline Material Composed of Multi-Interactive Molecules

Crystalline powders self-assembled from interactive discrete molecules reversibly transformed from a porous structure to a 2D one with a nanometer-thick H2O layer by hydration/dehydration. Multi-point weak intermolecular interactions contributed to maintenance of each phase. This structure transformation induced a humidity-dependent ion conductivity change from insulator to 3.4 x 10(-3) S cm(-1).open1122sciescopu