The microstrain-accompanied structural phase transition from h-MoO₃ to α-MoO₃ investigated by in situ X-ray diffraction

• Zeqian Zhang,
• Honglong Shi,
• Boxiang Zhuang,
• Minting Luo and
• Zhenfei Hu

Beilstein J. Nanotechnol. 2023, 14, 692–700, doi:10.3762/bjnano.14.55

• α-MoO3 is still unclear. Here, to reveal the features of the structural phase transition from h-MoO3 to α-MoO3, we performed in situ X-ray diffraction experiments at temperatures ranging from 30 to 450 °C. The Rietveld refinement results indicate water molecules at the (0 0 0.25) site inside the

• , the space group is Pnma, and the refined lattice parameters are 3.9804(4) × 14.1545(1) × 3.6967(2) Å. To determine the transition temperature of the h-MoO3→α-MoO3 phase transition, the mass fraction of α-MoO3 was determined via Rietveld refinement, as shown in Figure 1b. When the temperature was

• reside in the crystal structure of h-MoO3. To determine the crystal structures of h-MoO3 and α-MoO3, slowly scanned XRD patterns were acquired from the carefully ground powders calcinated at 375 °C and 450 °C, respectively. For the hexagonal phase h-MoO3, we performed Rietveld refinement based on two

Two-step single-reactor synthesis of oleic acid- or undecylenic acid-stabilized magnetic nanoparticles by thermal decomposition

• Mykhailo Nahorniak,
• Pamela Pasetto,
• Jean-Marc Greneche,
• Volodymyr Samaryk,
• Sandy Auguste,
• Anthony Rousseau,
• Nataliya Nosova and
• Serhii Varvarenko

Beilstein J. Nanotechnol. 2023, 14, 11–22, doi:10.3762/bjnano.14.2

• not correlate with the amount of stabilizer used. However, a large excess of NPM stabilizer was not obtained (samples TMO-III, TMU-III). The Rietveld refinement allowed us to determine a coherent diffracting domain size nanoparticle of 6 nm by using LaB6 as a reference compound (Table 1). The

• crystallites obtained by estimating the expansion of the X-ray diffraction line (DXRD calculated with Scherer, optionally Rietveld, refinement), which indicated a single magnetic domain characteristic of the TMO-I nanoparticle sample. When a stabilizer with a shorter carbon chain (i.e., UA) is used under the

Sodium doping in brookite TiO₂ enhances its photocatalytic activity

• Boxiang Zhuang,
• Honglong Shi,
• Honglei Zhang and
• Zeqian Zhang

Beilstein J. Nanotechnol. 2022, 13, 599–609, doi:10.3762/bjnano.13.52

• , oxalic acid, and sodium hydroxide. It exhibits excellent photocatalytic activity in methylene blue solution (MB), which is about three times higher than that of the quasi-spherical brookite TiO2. The crystal structure of NaxTi1−xO2 was determined by the Rietveld refinement method and verified by the

• ). However, the occupancy of the Ti atomic site is refined to be 0.8579(1), indicating that the Ti atomic site should be partially occupied by lighter Na atoms (due to the existence of sodium in the brookite phase). Figure 5a shows a typical Rietveld refinement pattern of the sample calcinated at 400 °C. The

• characterization To inspect the structure evolution of the titanium dioxide with the calcinating temperature, the as-prepared products were examined by an X-ray diffractometer (Bruker D8 Advance) using Cu Kα radiation (λ = 1.5406 Å). The Rietveld refinement of patterns was performed in the GSAS-II software [35

A new method for obtaining the magnetic shape anisotropy directly from electron tomography images

• Cristian Radu,
• Ioana D. Vlaicu and
• Andrei C. Kuncser

Beilstein J. Nanotechnol. 2022, 13, 590–598, doi:10.3762/bjnano.13.51

• diffractometer. MAUD software has been used for Rietveld refinement. Software Description Magn3t is using as main input data a previously 3D reconstructed volume of voxels. There is a wide range of solutions for 3D reconstruction of image series provided either for micro tomography or electron tomography (Avizo

• nanoparticles has been used for further tests. A −67 to +67 tomographic tilt series has been obtained with 1° steps. The series has been aligned using Tomviz [31] and ImageJ [32] software. The aligned series has been reconstructed using Genfire. The Rietveld refinement of the XRD spectra (Figure 4a) revealed

• ), segmented data volume (b), different outputs of Magn3t (c, d). XRD pattern of Fe3O4 MNPs and associated Rietveld refinement (in red) (a). Tomviz perspectives on experimental tomogram data as obtained by Genfire (b) and tomogram data after segmentation and particle separation using Magn3t (c). Each of the

Biocompatibility and cytotoxicity in vitro of surface-functionalized drug-loaded spinel ferrite nanoparticles

• Sadaf Mushtaq,
• Khuram Shahzad,
• Tariq Saeed,
• Anwar Ul-Hamid,
• Bilal Haider Abbasi,
• Nafees Ahmad,
• Waqas Khalid,
• Muhammad Atif,
• Zulqurnain Ali and
• Rashda Abbasi

Beilstein J. Nanotechnol. 2021, 12, 1339–1364, doi:10.3762/bjnano.12.99

• cytotoxicity of these nanocarriers for potential anticancer drug delivery systems. Results and Discussion Physical characterizations The X-ray diffraction (XRD) data of all samples was analyzed using Rietveld refinement techniques in the Fullprof Suit program. The data was refined according to their space

Free and partially encapsulated manganese ferrite nanoparticles in multiwall carbon nanotubes

• Saja Al-Khabouri,
• Salim Al-Harthi,
• Toru Maekawa,
• Mohamed E. Elzain,
• Ashraf Al-Hinai,
• Ahmed D. Al-Rawas,
• Abbsher M. Gismelseed,
• Ali A. Yousif and
• Myo Tay Zar Myint

Beilstein J. Nanotechnol. 2020, 11, 1891–1904, doi:10.3762/bjnano.11.170

• diffraction pattern was refined using Rietveld refinement techniques (Figure 5a). There is a shift in the X-ray diffraction peaks of partially encapsulated manganese ferrite nanoparticles in comparison to the X-ray diffraction peaks of free manganese ferrite nanoparticles [29]. Moreover, as an example, the

• are in the inner part of the tubes. (m,n) HRTEM images at the location identified by a circle in (i). (a) Rietveld refinement of the XRD pattern of MnFe2O4/MWCNTs. (b) HRTEM image of the (111) plane showing the interfringe distance measurement. UPS spectrum of MnFe2O4/MWCNTs and pristine MWCNTs. Inset

An advanced structural characterization of templated meso-macroporous carbon monoliths by small- and wide-angle scattering techniques

• Felix M. Badaczewski,
• Marc O. Loeh,
• Torben Pfaff,
• Dirk Wallacher,
• Daniel Clemens and
• Bernd M. Smarsly

Beilstein J. Nanotechnol. 2020, 11, 310–322, doi:10.3762/bjnano.11.23

• analysis or Rietveld refinement suffer from the turbostratic arrangement of the carbon stacks and do not achieve meaningful results, a novel approach similar to Rietveld refinement is used [28]. The algorithm of the approach is capable to fit the entire wide-angle scattering curve of turbostratic carbon

Air oxidation of sulfur mustard gas simulants using a pyrene-based metal–organic framework photocatalyst

• Ghada Ayoub,
• Mihails Arhangelskis,
• Xuan Zhang,
• Florencia Son,
• Timur Islamoglu,
• Tomislav Friščić and
• Omar K. Farha

Beilstein J. Nanotechnol. 2019, 10, 2422–2427, doi:10.3762/bjnano.10.232

• -400 (see section S.2.1, Table S1 in Supporting Information File 1 for crystal structure details) was established from PXRD data, by Rietveld refinement (Figure S1, Supporting Information File 1) of a model generated from UiO-67 (CCDC code WIZMAV03). The morphology of the materials was confirmed by

Improved adsorption and degradation performance by S-doping of (001)-TiO₂

• Xiao-Yu Sun,
• Xian Zhang,
• Xiao Sun,
• Ni-Xian Qian,
• Min Wang and
• Yong-Qing Ma

Beilstein J. Nanotechnol. 2019, 10, 2116–2127, doi:10.3762/bjnano.10.206

• a calibration curve. Results and Discussion The crystal structures of all samples were characterized by XRD. Figure 1 shows the experimental data and the results calculated by Rietveld refinement of 1-S0 (a) and 2-S2 (b). The calculated results match well with the experimental data indicating that

Green and scalable synthesis of nanocrystalline kuramite

• Andrea Giaccherini,
• Giuseppe Cucinotta,
• Stefano Martinuzzi,
• Enrico Berretti,
• Werner Oberhauser,
• Alessandro Lavacchi,
• Giovanni Orazio Lepore,
• Giordano Montegrossi,
• Maurizio Romanelli,
• Antonio De Luca,
• Massimo Innocenti,
• Vanni Moggi Cecchi,
• Matteo Mannini,
• Antonella Buccianti and
• Francesco Di Benedetto

Beilstein J. Nanotechnol. 2019, 10, 2073–2083, doi:10.3762/bjnano.10.202

• SEM micrographs of the powders deposited on an aluminum stub after coating the sample with Au. The phase determination of the synthetic products was carried out on the Rietveld refinement of the XRD pattern by using the “GSAS II” software [46]. The instrumental parameters for the Rietveld refinement

• associated phases. Still, the compositional data of the final products require further consideration after a discussion of the results obtained with other characterization techniques. X-ray diffraction We performed a Rietveld refinement of the experimental patterns in the framework of the tetragonal CTS

• that all the samples appear very similar when compared with one another and their lamellar aspect is consistent with previous reports [35][45]. The Rietveld refinement and the analysis of the Raman spectra confirm the result of the compositional analysis and supports the conclusion that kuramite is the

The impact of crystal size and temperature on the adsorption-induced flexibility of the Zr-based metal–organic framework DUT-98

• Simon Krause,
• Volodymyr Bon,
• Hongchu Du,
• Rafal E. Dunin-Borkowski,
• Ulrich Stoeck,
• Irena Senkovska and
• Stefan Kaskel

Beilstein J. Nanotechnol. 2019, 10, 1737–1744, doi:10.3762/bjnano.10.169

• the samples with smaller crystals, the majority of crystals or crystal domains remain in the op phase and only part of the sample undergoes contraction upon solvent removal by supercritical activation. A quantitative phase analysis of the op–cp mixture by Rietveld refinement was not possible due to

The effect of magneto-crystalline anisotropy on the properties of hard and soft magnetic ferrite nanoparticles

• Hajar Jalili,
• Bagher Aslibeiki,
• Ali Ghotbi Varzaneh and
• Volodymyr A. Chernenko

Beilstein J. Nanotechnol. 2019, 10, 1348–1359, doi:10.3762/bjnano.10.133

• −xO4 NPs, with x = 0–1 in steps of 0.2, from soft magnetic (Fe3O4) to hard magnetic (CoFe2O4) ferrite, with a significant variation of the magnetic anisotropy. The phase purity and the formation of crystalline NPs with a spinel structure were confirmed through Rietveld refinement. The effect of Co

• ; Rietveld refinement; Introduction Technological advances in various fields have motivated the design and the fabrication of nanostructures with tuned and improved properties. Among nanostructured materials, magnetic nanoparticles (NPs) are interesting from both fundamental and technological points of view

• : 49 Å, B-site: 64 Å) [24]. Therefore, the unsystematic variations and insignificant (in the error range) difference in the lattice constant could be attributed to the change of the cation distribution in the A-and B-sites. The XRD patterns of the samples were analyzed using the Rietveld refinement

Size-selected Fe₃O₄–Au hybrid nanoparticles for improved magnetism-based theranostics

• Maria V. Efremova,
• Yulia A. Nalench,
• Eirini Myrovali,
• Anastasiia S. Garanina,
• Ivan S. Grebennikov,
• Polina K. Gifer,
• Maxim A. Abakumov,
• Marina Spasova,
• Makis Angelakeris,
• Alexander G. Savchenko,
• Michael Farle,
• Natalia L. Klyachko,
• Alexander G. Majouga and
• Ulf Wiedwald

Beilstein J. Nanotechnol. 2018, 9, 2684–2699, doi:10.3762/bjnano.9.251

• File 1, Figure S1. The volume fraction of magnetite and gold can be evaluated using the average NP diameter (assuming spherical Au–Fe3O4 NPs) by TEM and from fitting by modified Rietveld refinement from XRD. Importantly, the ratio of Fe3O4 to Au is almost constant at about 97% for MNP-15, MNP-25, and

• and gold are clearly observed. Rietveld refinement, combining the powder diffraction reference data of Fe3O4 (ICDD PDF-2 No. 00-019-0629) and Au (ICDD PDF-2 No. 03-065-8601), is applied (not shown). The extracted lattice constants, crystallite size and phase volume fractions are listed in Table 1

Impact of the anodization time on the photocatalytic activity of TiO₂ nanotubes

• Jesús A. Díaz-Real,
• Geyla C. Dubed-Bandomo,
• Juan Galindo-de-la-Rosa,
• Luis G. Arriaga,
• Janet Ledesma-García and
• Nicolas Alonso-Vante

Beilstein J. Nanotechnol. 2018, 9, 2628–2643, doi:10.3762/bjnano.9.244

• rutile, confirming their role in the crystalline stability [47][48]. The crystallite size was calculated by using Scherrer equation or Rietveld refinement, and the lattice parameters were estimated using the software TOPAS. The results are summarized in Table 2, where it was found using both methods that

Single-crystalline FeCo nanoparticle-filled carbon nanotubes: synthesis, structural characterization and magnetic properties

• Rasha Ghunaim,
• Maik Scholz,
• Christine Damm,
• Bernd Rellinghaus,
• Rüdiger Klingeler,
• Bernd Büchner,
• Michael Mertig and
• Silke Hampel

Beilstein J. Nanotechnol. 2018, 9, 1024–1034, doi:10.3762/bjnano.9.95

• ratios (e.g., Fe3Co7, FeCo, Fe7Co3), whereas our XRD diffraction pattern revealed the presence of a homogenous bcc phase of pure Fe50Co50 nanoparticles. Rietveld refinement identifying the exact structure of an annealed sample of Fe50Co50@CNT prepared by the second filling approach was also carried out

• approach. c) Rietveld refinement for the annealed Fe5 0Co50@CNT sample prepared by the second approach. Relative sample mass loss for a sample prepared by the first (i.e., solution) approach (black) and the other by the second approach (purple) of Fe50Co50@CNT during the combustion process of the

• . Nowka for XRD Rietveld refinement, G. Kreutzer for TEM measurements and S. Gaß for support with the magnetic measurements. RG acknowledges the German Academic Exchange Service (DAAD) for funding.

Effect of annealing treatments on CeO₂ grown on TiN and Si substrates by atomic layer deposition

• Silvia Vangelista,
• Rossella Piagge,
• Satu Ek and
• Alessio Lamperti

Beilstein J. Nanotechnol. 2018, 9, 890–899, doi:10.3762/bjnano.9.83

• atmosphere by using a graphite dome. Thickness, interface and surface roughness, and electronic density have been determined by data fitting using the MAUD software program [24]. MAUD has also been used for Rietveld refinement of GIXRD patterns, allowing to determine CeO2 cell parameter and crystallite size

Systematic control of α-Fe₂O₃ crystal growth direction for improved electrochemical performance of lithium-ion battery anodes

• Nan Shen,
• Miriam Keppeler,
• Barbara Stiaszny,
• Holger Hain,
• Filippo Maglia and
• Madhavi Srinivasan

Beilstein J. Nanotechnol. 2017, 8, 2032–2044, doi:10.3762/bjnano.8.204

• -Fe2O3-E1.5, α-Fe2O3-D1.5, α-Fe2O3-B1.5 and α-Fe2O3-N1.5). The reflections reported in Figure 2 indicate well-crystalized materials that can be indexed to α-Fe2O3 (JAPDS card No. 330664). The lattice constants were calculated using Rietveld refinement and found to be in the range of 5.030 to 5.033 Å for

Nanocrystalline TiO₂/SnO₂ heterostructures for gas sensing

• Barbara Lyson-Sypien,
• Anna Kusior,
• Mieczylaw Rekas,
• Jan Zukrowski,
• Marta Gajewska,
• Katarzyna Michalow-Mauke,
• Thomas Graule,
• Marta Radecka and
• Katarzyna Zakrzewska

Beilstein J. Nanotechnol. 2017, 8, 108–122, doi:10.3762/bjnano.8.12

• diffractometer. Based on Rietveld refinement it was possible to determine the weight fractions of cassiterite SnO2, rutile TiO2 and anatase TiO2, the lattice constants and the crystallite sizes, dXRD. The 119Sn Mössbauer effect measurements were performed in transmission geometry using an MS-4 RENON spectrometer

• components SnO2 and TiO2. Table 3 recapitulates the results of XRD Rietveld refinement performed for TiO2/SnO2 nanopowders, and the SSA values determined from BET measurements. The FSS parameters were chosen intentionally in order to obtain approximately the same SSA, and according to the expectation the SSA

• reference atmosphere and R is the electrical resistance under exposure to the detected gas. Possible combinations of α and β and the resulting chemisorbed oxygen species. The results of BET and XRD Rietveld refinement of TiO2–SnO2 nanomaterials; “A” denotes anatase, “R” rutile and “C” cassiterite; SSA

Microwave synthesis of high-quality and uniform 4 nm ZnFe₂O₄ nanocrystals for application in energy storage and nanomagnetics

• Christian Suchomski,
• Ben Breitung,
• Ralf Witte,
• Michael Knapp,
• Sondes Bauer,
• Tilo Baumbach,
• Christian Reitz and
• Torsten Brezesinski

Beilstein J. Nanotechnol. 2016, 7, 1350–1360, doi:10.3762/bjnano.7.126

• source, focusing Ge 111 monochromator and a Dectris Mythen strip detector. Rietveld refinement was performed by use of the FullProf software. X-ray photoelectron spectroscopy data were obtained on a VersaProbe PHI 5000 Scanning ESCA Microprobe from Physical Electronics with an Al Kα radiation source and

• size was estimated to be 3.7 nm in diameter, which is in excellent agreement with the crystallite size determined by Rietveld refinement. In a nutshell, the results from electron microscopy, XRD, XPS, 57Fe Mössbauer spectroscopy as well as DC and AC magnetometry are all consistent and confirm the

Synthesis and electrochemical performance of Li₂Co_1−xM_xPO₄F (M = Fe, Mn) cathode materials

• Nellie R. Khasanova,
• Oleg A. Drozhzhin,
• Stanislav S. Fedotov,
• Darya A. Storozhilova,
• Rodion V. Panin and
• Evgeny V. Antipov

Beilstein J. Nanotechnol. 2013, 4, 860–867, doi:10.3762/bjnano.4.97

• carried out by Rietveld refinement with the program JANA 2006 [17]. SEM investigation of powdered samples was performed with a JEOL JSM-6490LV scanning electron microscope equipped with an energy dispersive X-ray spectroscopy (EDX) attachment. The electrochemical evaluation was performed in two-electrode

Synthesis and thermoelectric properties of Re₃As_6.6In_0.4 with Ir₃Ge₇ crystal structure

• Valeriy Y. Verchenko,
• Anton S. Vasiliev,
• Alexander A. Tsirlin,
• Vladimir A. Kulbachinskii,
• Vladimir G. Kytin and
• Andrei V. Shevelkov

Beilstein J. Nanotechnol. 2013, 4, 446–452, doi:10.3762/bjnano.4.52

• solution Re3As6.7In0.3 (the composition obtained from the Rietveld refinement of the X-ray powder diffraction data, see Table 1), the DOS is reduced to 5.15 states/(eV·f.u.), given the rigid-band shift with the assumption that Re3As7 possesses 56 valence electrons per f.u. and Re3As6.7In0.3 55.4 electrons

• . Further optimization of the thermoelectric properties by varying the chemical composition of Re3As7−xInx is proposed. The plot of Rietveld refinement for the S1 sample. Experimental and difference curves, and positions of Bragg peaks are shown on the plot. Marked with numbers: 1: Re3As6.70(3)In0.30(3); 2

Mesoporous MgTa₂O₆ thin films with enhanced photocatalytic activity: On the interplay between crystallinity and mesostructure

• Jin-Ming Wu,
• Igor Djerdj,
• Till von Graberg and
• Bernd M. Smarsly

Beilstein J. Nanotechnol. 2012, 3, 123–133, doi:10.3762/bjnano.3.13

• of MgTa2O6 in the KLE-templated mesoporous film increased with increasing calcination temperature from 760 up to 1100 °C. The average grain size, which was estimated by applying the Rietveld refinement, is shown in Figure 2 as a function of the calcination temperature for both mesoporous and

• nonporous films. Owing to the lower overall crystallinity of the investigated material and a high background in some of the analyzed XRD patterns, the microstrain part in the size-microstrain procedure within the Rietveld refinement was not refined and was kept to the instrumental values determined by the