Principal component analysis for automatic extraction of solid-state kinetics from combined in situ experiments

2018 ◽  
Vol 20 (29) ◽  
pp. 19560-19571 ◽  
Author(s):  
Pietro Guccione ◽  
Luca Palin ◽  
Benny Danilo Belviso ◽  
Marco Milanesio ◽  
Rocco Caliandro
Keyword(s):  
Principal Component Analysis ◽  
Raman Spectroscopy ◽  
Solid State ◽  
Powder Diffraction ◽  
Principal Component ◽  
Automatic Extraction ◽  
X Ray ◽  
Solid State Kinetics ◽  
In Situ Experiments

A new algorithm to extract in an automatic way kinetic parameters from a set of measurements from in situ experiments is presented and applied to X-ray powder diffraction and Raman spectroscopy.

Hydrogen Desorption Reactions of the Na-Mg-B-H System

2010 ◽  
Vol 72 ◽  
pp. 164-169 ◽  
Author(s):  
Daphiny Pottmaier ◽  
Sebastiano Garroni ◽  
Maria Dolors Barò ◽  
Marcello Baricco
Keyword(s):  
Solid State ◽  
Research And Development ◽  
Ball Milling ◽  
Powder Diffraction ◽  
Hydrogen Desorption ◽  
X Ray ◽  
New Compounds ◽  
Desorption Reaction

Hydrogen storage in the solid state has shown increasing research and development, and recently an approach in mixing two hydride systems together by ball milling (reactive hydride composites) has been investigated in more detail, e.g. NaBH4 plus MgH2. Thermodynamic destabilization may occur by new compounds formation during dehydrogenation, e.g. MgB2. A study of the the role of O2/H2O contamination for the reaction 2NaBH4 + MgH2 ↔ 2NaH + MgB2 + 4H2 was conducted using in-situ X-ray powder diffraction. Desorption reaction is observed to begin by a competition of MgH2 and NaBH4 decomposition due to higher reactivity promoted by ball milling processing summed to O2/H2O contamination. Oxidation of NaBH4 into NaBO2 is observed to happen in higher degree than MgH2/Mg into MgO for the Na-Mg-B-H system.

scholarly journals Hydrates and polymorphs of lead squarate Pb(C4O4): Structural transformations studied by in situ X-ray powder diffraction and solid state NMR

Polyhedron ◽  
2019 ◽  
Vol 164 ◽  
pp. 123-131 ◽  
Author(s):  
Thierry Bataille ◽  
Amira Bouhali ◽  
Cassandre Kouvatas ◽  
Chahrazed Trifa ◽  
Nathalie Audebrand ◽  
...  
Keyword(s):  
Solid State ◽  
Powder Diffraction ◽  
Solid State Nmr ◽  
Structural Transformations ◽  
X Ray

In situsimultaneous Raman/high-resolution X-ray powder diffraction study of transformations occurring in materials at non-ambient conditions

2007 ◽  
Vol 40 (4) ◽  
pp. 684-693 ◽  
Author(s):  
Enrico Boccaleri ◽  
Fabio Carniato ◽  
Gianluca Croce ◽  
Davide Viterbo ◽  
Wouter van Beek ◽  
...  
Keyword(s):  
Solid State ◽  
High Resolution ◽  
Powder Diffraction ◽  
Added Value ◽  
Experimental Setup ◽  
Ambient Conditions ◽  
X Ray ◽  
Uv Lamp ◽  
Kinetics Of

Materials containing disordered moieties and/or amorphous or liquid-like phases or showing surface- or defect-related phenomena constitute a problem with respect to their characterization using X-ray powder diffraction (XRPD), and in many cases Raman spectroscopy can provide useful complementary information. A novel experimental setup has been designed and realized for simultaneousin situRaman/high-resolution XRPD experiments, to take full advantage of the complementarities of the two techniques in investigating solid-state transformations under non-ambient conditions. The added value of the proposed experiment is the perfect synchronization of the two probes with the reaction coordinate and the elimination of possible bias caused by different sample holders and conditioning modes used in `in situbut separate' approaches. The setup was tested on three solid-state transformations: (i) the kinetics of the fluorene–TCNQ solid-state synthesis, (ii) the thermal swelling and degradation of stearate–hydrotalcite, and (iii) the photoinduced (2 + 2)-cyclization of (E)-furylidenoxindole. These experiments demonstrated that, even though the simultaneous Raman/XRPD experiment is more challenging than separate procedures, high-resolution XRPD and Raman data can be collected. A gas blower allows studies from room temperature to 700 K, and 100 K can be reached using a nitrogen cryostream. The flexibility of the experimental setup allows the addition of ancillary devices, such as a UV lamp used to study photoreactivity.

scholarly journals CO2 adsorption in Y zeolite: a structural and dynamic view by a novel principal-component-analysis-assisted in situ single-crystal X-ray diffraction experiment

2019 ◽  
Vol 75 (2) ◽  
pp. 214-222 ◽  
Author(s):  
Eleonora Conterosito ◽  
Luca Palin ◽  
Rocco Caliandro ◽  
Wouter van Beek ◽  
Dmitry Chernyshov ◽  
...  
Keyword(s):  
Principal Component Analysis ◽  
Single Crystal ◽  
Principal Component ◽  
Active Species ◽  
Data Sets ◽  
X Ray Diffraction ◽  
Y Zeolite ◽  
X Ray ◽  
First Time

The increasing efficiency of detectors and brightness of X-rays in both laboratory and large-scale facilities allow the collection of full single-crystal X-ray data sets within minutes. The analysis of these `crystallographic big data' requires new tools and approaches. To answer these needs, the use of principal component analysis (PCA) is proposed to improve the efficiency and speed of the analysis. Potentialities and limitations of PCA were investigated using single-crystal X-ray diffraction (XRD) data collected in situ on Y zeolite, in which CO2, acting as an active species, is thermally adsorbed while cooling from 300 to 200 K. For the first time, thanks to the high sensitivity of single-crystal XRD, it was possible to determine the sites where CO2 is adsorbed, the increase in their occupancy while the temperature is decreased, and the correlated motion of active species, i.e. CO2, H2O and Na+. PCA allowed identification and elimination of problematic data sets, and better understanding of the trends of the occupancies of CO2, Na+ and water. The quality of the data allowed for the first time calculation of the enthalpy (ΔH) and entropy (ΔS) of the CO2 adsorption by applying the van 't Hoff equation to in situ single-crystal data. The calculation of thermodynamic values was carried out by both traditional and PCA-based approaches, producing comparable results. The obtained ΔH value is significant and involves systems (CO2 and Y zeolite) with no toxicity, superb stability and chemical inertness. Such features, coupled with the absence of carbonate formation and framework inertness upon adsorption, were demonstrated for the bulk crystal by the single-crystal experiment, and suggest that the phenomenon can be easily reversed for a large number of cycles, with CO2 released on demand. The main advantages of PCA-assisted analysis reside in its speed and in the possibility of it being applied directly to raw data, possibly as an `online' data-quality test during data collection, without any a priori knowledge of the crystal structure.

Manipulating the dynamics of mechanochemical ternary cocrystal formation

2019 ◽  
Vol 55 (66) ◽  
pp. 9793-9796 ◽  
Author(s):  
Hannes Kulla ◽  
Adam A. L. Michalchuk ◽  
Franziska Emmerling
Keyword(s):  
Raman Spectroscopy ◽  
Real Time ◽  
Powder Diffraction ◽  
X Ray

In situ real-time X-ray powder diffraction and Raman spectroscopy reveal formation pathways of ternary co-crystals by mechanochemistry.

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