Diffraction Data Research Articles

Crystal structures, dielectric properties, and lattice vibrational characteristics of Zn1-xCaxWO4 (x = 0–0.25) composite ceramics

In this work, Zn1-xCaxWO4 (x=0–0.25, ZCWO) composite ceramics were prepared by using the conventional solid-state sintering method at 1070 ℃. The impact of Ca2+ substitution on the lattice vibrational characteristics and dielectric responses of the ZCWO composite ceramics was investigated in detail. The formation of composite ceramics was verified by the Rietveld refined X-ray diffraction data of the ZCWO samples. The lattice vibrational characteristics were also identified and analyzed by the Raman and infrared reflection spectra combined with the theoretical simulations. The vibrational modes analysis of the Raman spectra showed that the internal modes of the ZCWO ceramics correspond to the vibrations of the W-O octahedrons. From the Fourier transform infrared reflectance spectra, the existence of three new vibrational modes of Au (315 cm−1), Au (834 cm−1), and Eu (885 cm−1) at x = 0.15–0.25 was observed, which belong to the modes of the CaWO4 ceramic. In addition, the intrinsic dielectric properties fitted by the four-parameter semiquantum model were in direct agreement with the theoretical values obtained from the Clausius-Mossotti & damping equations and the measured values. Besides, the contribution of each lattice vibrational mode to the intrinsic properties of the ZCWO ceramics was thoroughly studied, which shows that external mode 1 contributes the most to the intrinsic properties. The structure-property relationships of the ZCWO ceramics were established using the Raman modes as a media. The optimum dielectric properties of the ZCWO ceramics were obtained when x = 0.25: εr =13.98 (10.48 GHz), Q × f = 32,188 GHz.

Scaling and Merging Time-Resolved Laue Data with Variational Inference.

Time-resolved X-ray crystallography (TR-X) at synchrotrons and free electron lasers is a promising technique for recording dynamics of molecules at atomic resolution. While experimental methods for TR-X have proliferated and matured, data analysis is often difficult. Extracting small, time-dependent changes in signal is frequently a bottleneck for practitioners. Recent work demonstrated this challenge can be addressed when merging redundant observations by a statistical technique known as variational inference (VI). However, the variational approach to time-resolved data analysis requires identification of successful hyperparameters in order to optimally extract signal. In this case study, we present a successful application of VI to time-resolved changes in an enzyme, DJ-1, upon mixing with a substrate molecule, methylglyoxal. We present a strategy to extract high signal-to-noise changes in electron density from these data. Furthermore, we conduct an ablation study, in which we systematically remove one hyperparameter at a time to demonstrate the impact of each hyperparameter choice on the success of our model. We expect this case study will serve as a practical example for how others may deploy VI in order to analyze their time-resolved diffraction data.

Mechanochemical synthesis of (Mg1−x Fe x )2SiO4 olivine phases relevant to Martian regolith: structural and spectroscopic characterizations

Abstract To fabricate metals from the base materials for future Mars exploration, synthesis of representative olivine phases and their structural and spectroscopic characterizations are of crucial importance. Using mechanochemical technique that mimics the mechanical weathering, a complete solid solution of (Mg1−x Fe x )2SiO4 has been synthesized to investigate the associated crystal chemical properties. X-ray powder diffraction data Rietveld analysis confirms that each polycrystalline sample crystallizes in space group Pbnm. The average crystallite size ranges between 80(1) nm and 223(4) nm. Each lattice parameter increases with increasing Fe-content due to the larger Fe2+ radius than that of Mg2+, following Vegard’s rule. For a given nominal chemical composition, substitution of Mg with Fe at the M1-site (4a: 0,0,0) is preferred to the M2-site (4c: x,y,¼). As a consequence, the average Fe-content lies slightly below the equivalence line for x = 0.2–0.8, indicating that the Fe/Mg ratio in the amorphous scattering content is most likely greater than unity. Characteristic Raman spectral features of the olivines have been explained in terms of the chemical composition (x). Simple regression models are demonstrated based on both X-ray diffraction and Raman spectroscopic data for the calculation of Mg/Fe in olivines. Diffuse reflectance UV/Vis spectra RATD analysis shows each olivine phase possesses direct band-gap between 3.38(3) eV and 4.90(3) eV. This study could keep valuable information to relevant databases for future human missions on Mars, in particular, for precise estimation of the representative olivines from the remote X-ray diffraction and spectroscopic data.

Hirshfeld atom refinement and dynamical refinement of hexagonal ice structure from electron diffraction data.

Reaching beyond the commonly used spherical atomic electron density model allows one to greatly improve the accuracy of hydrogen atom structural parameters derived from X-ray data. However, the effects of atomic asphericity are less explored for electron diffraction data. In this work, Hirshfeld atom refinement (HAR), a method that uses an accurate description of electron density by quantum mechanical calculation for a system of interest, was applied for the first time to the kinematical refinement of electron diffraction data. This approach was applied here to derive the structure of ordinary hexagonal ice (Ih). The effect of introducing HAR is much less noticeable than in the case of X-ray refinement and it is largely overshadowed by dynamical scattering effects. It led to only a slight change in the O-H bond lengths (shortening by 0.01 Å) compared with the independent atom model (IAM). The average absolute differences in O-H bond lengths between the kinematical refinements and the reference neutron structure were much larger: 0.044 for IAM and 0.046 Å for HAR. The refinement results changed considerably when dynamical scattering effects were modelled - with extinction correction or with dynamical refinement. The latter led to an improvement of the O-H bond length accuracy to 0.021 Å on average (with IAM refinement). Though there is a potential for deriving more accurate structures using HAR for electron diffraction, modelling of dynamical scattering effects seems to be a necessary step to achieve this. However, at present there is no software to support both HAR and dynamical refinement.

Expanded Insights into Martian Mineralogy: Updated Analysis of Gale Crater’s Mineral Composition via CheMin Crystal Chemical Investigations

This study presents mineral composition estimates of rock and sediment samples analyzed with the CheMin X-ray diffraction instrument on board the NASA Mars Science Laboratory rover, Curiosity, in Gale crater, Mars. Mineral composition is estimated using crystal-chemically derived algorithms applied to X-ray diffraction data, specifically unit-cell parameters. The mineral groups characterized include those found in major abundance by the CheMin instrument (i.e., feldspar, olivine, pyroxene, and spinel oxide). In addition to estimating the composition of the major mineral phases observed in Gale crater, we place their compositions in a stratigraphic context and provide a comparison to that of martian meteorites. This work provides expanded insights into the mineralogy and chemistry of the martian surface.

Investigation of kesterite to stannite phase transition and band gap engineering in Cu2Zn1-xCoxSnS4 thin films prepared by sol-gel spin coating

In this study, the Cu2Zn1-xCoxSnS4 (CZn1-xCoxTS) films with partial cation substitution of cobalt are synthetized by sol gel spin coating, followed by sulfurization treatment. The incorporation of cobalt cation in the CZTS crystalline lattice as well as the phase transition from kesterite to stannite were confirmed by the X-ray diffraction (XRD) and Raman spectroscopy data. The XRD pattern shows peak-shifting toward higher 2θ by increasing the Co concentration, indicating a decrease in lattice parameters. The red shift of Raman peaks by increasing x from 0 to 0.6, confirms the phase transition. The CZn1-xCoxTS morphology was observed by scanning electron microscopy, showing large grain size as x increases and a good distribution of elements for all films. X-ray photoelectron spectroscopy was employed to study the valence of cations/anions and to probe the chemical bonds. The optical band gap showed a parabolic behavior versus the molar ratio Co/(Co + Zn), this deviation from Vegard’s law being induced by the difference in electronegativity between cobalt and zinc. The pure CZTS has a band gap of 1.47 eV, while for CZn0.6Co0.4TS the gap is 1.17 eV, which indicates that the incorporation of cobalt cation produces a red-shift of the band to band transition energy.

Dynamics of charge carriers in La2CuO4 cuprates: Conductivity variation, scaling formalisms, and electric modulus study

In this work, we conducted a detailed investigation of the structural properties and the dynamics of the charges in the La2CuO4 Ruddlesden–Popper system that is prepared via the conventional solid-state process. Via the X-ray diffraction data and using the Rietveld refinement, we found that the compound exhibits a single crystallographic phase with a Bmab space group. The DC-conductivity investigation shows that the studied ceramic exhibits two electrical behaviors. Below 460 °C, the occurrence of a semiconductor behavior is attributed to the effect of the Variable range hopping conduction process. At high temperatures, the electrical nature of the material is linked to the thermally activated small polaron hopping conduction process via an activation energy Ea = 1.40 eV. Over the explored temperature range, conductivity spectra of the Ruddlesden–Popper are analyzed using the universal Double Jonscher power law. The dispersion region can be attributed to the coexistence of both hopping and tunneling processes. The conductivity spectra of the La2CuO4 Ruddlesden–Popper nicely follow the time-temperature superposition (TTSP) principle. This confirms that similar sources are responsible for relaxation and conduction processes. Using the Summerfield scaling approach, the superposition of the conductivity spectra into a single master curve confirms that the relaxation process is the microstructure's response independent. From the electrical modulus investigation, we found that the studied compound exhibits a non-Debye relaxation nature, over the explored temperature interval. Contribution of grain and grain boundary were resolved by complex modulus spectroscopy analysis. In addition, we found the absence of the electrode contribution at low frequencies. The correlation between both Z″ and the M″ peaks indicates that the conduction and relaxation processes are not related to the same origins.

Structural and optical properties of green-synthesised tricobalt tetroxide nanoparticles

In this study, we investigated the structural and optical properties of garlic extract-based green-synthesised tricobalt tetroxide nanoparticles. Transmission electron microscopy revealed a particle size range of 8–22 nm for the prepared powder sample. Powder x-ray diffraction data and Rietveld refinement results confirmed the spinel cubic crystal structure of the tricobalt tetroxide nanoparticles, with an average crystallite size of 11.23 nm. This crystal structure corresponds to the Fd3̅m space group and has an average lattice constant of 0.791 nm. The bond lengths of Co3+–O2− and Co2+–O2− are measured to be 0.188 nm and 0.190 nm, respectively. The FTIR data provided evidence of the presence of various functional bands, which helped qualitatively determine the purity of the sample. The UV–vis spectrum estimated two direct energy band gap values (3.7 eV and 2.2 eV) that may be useful for efficient interaction with a wide range of ray spectra to create more electron–hole pairs for various photo-responsive applications, such as dye degradation, solar cells, and optoelectronic components.

Second-harmonic generation effect enhanced by Li substitution for Na in Li1(LiXNa5−X)Mo9O30

Large single crystals of the solid-solution series ▪ were grown by the Czochralski method by varying the Li substitution for Na. Structure analyses with X-ray single-crystal diffraction data elucidated statistic disorder of Li with Na at three independent Na sites. The resulting Li substitution X = 0, 1.2, and 2.8 could be confirmed by neutron activation analysis. Second-harmonic generation (SHG) light intensities and non-linear optical (NLO) coefficients were determined in three crystallographic main directions by Maker fringe measurements. DFT calculations delivered absolute NLO magnitudes. UV/Vis optical spectra revealed that the transmission rises from X = 0 to X = 2.8. However, the SHG effect is at largest in ▪ (X = 1.2), so far investigated in this study.

Highly Recyclable and Versatile La0.5Nd0.2Ca0.3MnO3 and La0.5Nd0.2Ca0.25K0.05MnO3 Perovskite Catalysts for Effective Removal of Organic Contaminants

AbstractWastewater contamination, particularly from dye effluents containing organic colorants originating from industrial sources, represents a significant environmental and public health hazard. This study is dedicated to removal of these abundant coloured effluents in wastewater, addressing the imperative need for effective remediation strategies to safeguard ecosystems and human well‐being. In this regard, bare and K‐doped perovskite manganites La0.5Nd0.2Ca0.3MnO3 (LCM) and La0.5Nd0.2Ca0.25K0.05MnO3 (LCKM) nanoparticles respectively were synthesized in order to study their catalytic behaviour for degradation of coloured effluents. The Rietveld analysis applied to the X‐ray diffraction data provides confirmation of orthorhombic symmetry. For exploring the catalytic properties, rhodamine‐B (RhB) dye was chosen as model dye pollutant. The achieved degradation efficiency is substantial, reaching 99 % within a brief period of 10–12 min. Following these results, we have also carried out the degradation of some other dyes such as methylene blue (MB) and methyl orange (MO). It was observed that MO dye was more efficiently degraded in quick time as compared to all the other dyes due to its anionic nature. Furthermore, the comparative catalytic efficiencies of LCM and LCKM catalysts were explained on the basis of Mn3+/Mn4+ redox pairs and it was observed that LCKM had shown better degradation efficiency than LCM.

Synthesis of Zintl Phase Metal Silicide Thermoelectric Materials in Magnesium/Zinc Flux.

Zintl phases have potential applications as thermoelectric materials for power generation and cooling owing to their complex crystal structures and unique electronic properties. We carried out reactions of silicon with barium and strontium in excess Mg/Zn flux to synthesize (Ba/Sr)5+xMg19-xSi12 Zintl phases, investigating the effect of varying Ba/Sr ratio on site mixing and thermoelectric properties. (Ba/Sr)5+xMg19-xSi12 compounds with 0 < x < 3 are charge-balanced Zintl phases which adopt the hexagonal Ho5Ni19P12 structure type (space group P6̅2m). Density of states calculations indicate that these materials are semimetals. Single-crystal X-ray diffraction data and elemental analysis for Ba5Mg19Si12, Ba4.86Sr2.94Mg16.20Si12, Ba3.63Sr4.20Mg16.17Si12, Ba1.93Sr5.99Mg16.08Si12, and Sr7.82Mg16.18Si12 show occupation of barium and strontium cations in Ho sites, while strontium mixes with magnesium on a specific Ni site. Powder XRD data of products show that they are single phase throughout the sample. Thermoelectric measurements indicate that increasing strontium content and mixing on three cation sites decreases thermal conductivity; it is hypothesized that improved overall thermoelectric behavior is likely due to the rattling of the Sr cations in their positions.

Texture tomography, a versatile framework to study crystalline texture in 3D.

Crystallographic texture is a key organization feature of many technical and biological materials. In these materials, especially hierarchically structured ones, the preferential alignment of the nano constituents heavily influences the macroscopic behavior of the material. To study local crystallographic texture with both high spatial and angular resolution, we developed Texture Tomography (TexTOM). This approach allows the user to model the diffraction data of polycrystalline materials using the full reciprocal space of the crystal ensemble and describe the texture in each voxel via an orientation distribution function, hence it provides 3D reconstructions of the local texture by measuring the probabilities of all crystal orientations. The TexTOM approach addresses limitations associated with existing models: it correlates the intensities from several Bragg reflections, thus reducing ambiguities resulting from symmetry. Further, it yields quantitative probability distributions of local real space crystal orientations without further assumptions about the sample structure. Finally, its efficient mathematical formulation enables reconstructions faster than the time scale of the experiment. This manuscript presents the mathematical model, the inversion strategy and its current experimental implementation. We show characterizations of simulated data as well as experimental data obtained from a synthetic, inorganic model sample: the silica-witherite biomorph. TexTOM provides a versatile framework to reconstruct 3D quantitative texture information for polycrystalline samples; it opens the door for unprecedented insights into the nanostructural makeup of natural and technical materials.

Study on the spectral characteristics and chemical structure of Taixi Anthracite

Taixi anthracite is a rare form of coal in both China and the world, characterized by low ash, sulfur, phosphorus, high carbon content, conductivity, and calorific value. Our team employed a solid-phase microwave method [1] to graphitize Taixi anthracite and graft it with natural rubber to create a composite with outstanding properties. However, since the molecular structure of Taixi anthracite was unknown, establishing a molecular model for the reaction becomes crucial for the functionalization of anthracite. In this study, By combining elemental analysis, nuclear magnetic resonance carbon spectroscopy, Fourier transform infrared spectroscopy and X-ray photoelectron spectroscopy, the molecular carbon content of Taixi anthracite is 89 %, the XBP value is 0.37, and the chemical formula of the lowest relative molecular weight of Taixi anthracite is C181H77O4NS0.1. The results of computer simulation show that Taixi anthracite is assembled into coal macromolecular structure by 10 molecular structure units of 5 kinds of coal according to 2:1:2:2:3 ratio, and the geometric optimization, annealing simulation and inverse verification are carried out. The aggregation model is established by using X-ray diffraction data and computer simulation techniques.we innovatively constructed five groups of macromolecular structure units of Taixi anthracite to characterize the results and simulate the minimum energy configuration of single chains and aggregate states. This research provides a molecular-level theoretical basis for the functionalization of Taixi anthracite.

Laue-DIALS: open-source software for polychromatic X-ray diffraction data.

Most X-ray sources are inherently polychromatic. Polychromatic ("pink") X-rays provide an efficient way to conduct diffraction experiments as many more photons can be used and large regions of reciprocal space can be probed without sample rotation during exposure-ideal conditions for time-resolved applications. Analysis of such data is complicated, however, causing most X-ray facilities to discard >99% of X-ray photons to obtain monochromatic data. Key challenges in analyzing polychromatic diffraction data include lattice searching, indexing and wavelength assignment, correction of measured intensities for wavelength-dependent effects, and deconvolution of harmonics. We recently described an algorithm, Careless, that can perform harmonic deconvolution and correct measured intensities for variation in wavelength when presented with integrated diffraction intensities and assigned wavelengths. Here, we present Laue-DIALS, an open-source software pipeline that indexes and integrates polychromatic diffraction data. Laue-DIALS is based on the dxtbx toolbox, which supports the DIALS software commonly used to process monochromatic data. As such, Laue-DIALS provides many of the same advantages: an open-source, modular, and extensible architecture, providing a robust basis for future development. We present benchmark results showing that Laue-DIALS, together with Careless, provides a suitable approach to the analysis of polychromatic diffraction data, including for time-resolved applications.

Luminescence and dosimetry investigations of Eu(III) doped Ca2CeVO6 novel double perovskite

A novel composition of vanadate double perovskite Ca2CeVO6 doped with Eu3+ was successfully synthesized using combustion synthesis, wherein the doping levels of Eu3+ ranged from 1 to 6 mol%. The Rietveld refinement of the powder X-ray diffraction (XRD) data confirmed the orthorhombic structure of the phosphors. Scanning electron microscopy (SEM) and energy-dispersive X-ray analysis (EDAX) were employed to investigate the surface morphology and elemental distribution in the phosphor, respectively. Under the excitation at 280 nm and 467 nm, the phosphor exhibited strong down-conversion red photoluminescence (PL) emission, attributed to Eu3+ transitions (5D0-7FJ, where J = 0–3) originating from its 4f states. The intensity of PL emission shows increasing trend with increasing doping concentration. However, exceeding the threshold doping concentrations led reduction in PL intensity due to multipolar interaction effects. Additionally, the Eu3+ doped Ca2CeVO6 phosphors were subjected to irradiation with a radioactive 90Sr/90Y beta source to explore their thermoluminescence (TL) properties. Post-irradiation, the phosphors displayed prominent TL glow curves, with the most intense peak at around 94 °C, followed by peaks at 160 °C and 288 °C. The TL intensity of these peaks exhibited a linear dose response within the dose range of 1 Gy–50 Gy. Besides, the TL fading and reproducibility tests showed satisfactory results. Furthermore, Tmax-Tstop experiments revealed the presence of three trap centres within the trap depth range of 0.7–2.1 eV in the Ca2CeVO6:Eu3+ phosphor. Additionally, the glow curve deconvolution (GCD) was employed to determine trapping parameters, providing valuable insights into the TL behaviour of the phosphor. Overall, the results suggest that the novel phosphor under study holds promise for its applications in lighting devices and TL dosimetry (TLD).

Nearly close-packed atomic arrangements in BaTi2O5 glass

Recent advancements in glass synthesis have led to the creation of novel oxide glasses without tetrahedral corner-sharing networks. Of particular interest are glasses with high atomic packing densities, showcasing improved functionalities. Conventional analyses revealed the presence of not only four-coordinated polyhedra but also five- or six-coordinated polyhedra, which are connected via corner-sharing, edge-sharing, or face-sharing linkages. This study adapted the reduced atomic arrangement (RAA) method to analyze densely packed oxide glasses. The RAA method revealed a near-close-packed structure within a 10 Å range throughout BaTi2O5 glass, with Ba2+ and O2− ions arranged accordingly. Moreover, the structural model derived from relaxing the closest-packed arrangement via molecular dynamics simulations faithfully replicated the X-ray diffraction data. These findings suggest that minor deviations from the closest-packed atomic arrangement can initiate glass formation without corner-sharing tetrahedral networks. The RAA method proves highly effective in understanding glass formation mechanisms in unconventional oxide glasses.

A New Approach to the Synthesis of [1,2,4]Triazolo[1,5-a]pyrimidines by Reaction of 1,2,4,5-Tetrazines with 2-Aminoxazoles

A new transformation of 3,6-diphenyl-1,2,4,5-tetrazine was discovered during the solvent-free reaction with 2-amino-4-aryloxazoles, leading to the formation of 2,5,7-triaryl[1,2,4]triazolo[1,5-a]pyrimidines. Stucture of products was also confirmed by single crystal X-ray diffraction data. A possible mechanism for this reaction was proposed.

Synthesis and Structure of Barium Hexaferrite BaFe12–xInxO19 (x = 0–1)

This study presents the results of the synthesis and examination of indium-substituted barium hexaferrite samples with the formula BaFe12–xInxO19. The ferrites were obtained via a solid state synthesis method. The substitution level of indium, represented by x(In), was varied from 0 to 1 in 0.25 increments. The stoichiometric formulas of the compounds were calculated using the EDS data. The powder X-ray diffraction analysis indicated that all samples form a single crystalline phase with the M-type hexaferrite structure. Parameters of the crystal unit cell were calculated from powder diffraction data. An expansion of the crystal lattice parameters was observed as iron was substituted with indium, from x = 0 to x = 0.84. The Curie temperatures of the synthesized ferrites were determined using differential scanning calorimetry (DSC) method. It is established that the Curie temperature decreases from 452 to 292°C with In content growth from x = 0 to x = 0.84 in the BaFe12–xInxO19.

Variations in soil erodibility (K-factor) for the Chernozems depending on the method of texture determination

Soil erodibility (K-factor) is an important parameter in erosion modeling, is one of five factors of the Revised Universal Soil Loss Equation (RUSLE), and generally represents the soil's response to rainfall and run-off erosivity. The erodibility could be determined based on direct measurements of soil properties and mathematical calculations. In this study, the K-factor was calculated based on a formula from RUSLE, proposed by Renard et al. (1997). All input parameters: soil organic carbon (SOC), soil structure, and permeability classes were measured by one method, but particle size distribution – in two ways by sedimentation and laser diffraction methods to assess the impact the K-factor variability and the values of soil erosion rates. The 107 soil samples of Chernozems from Kursk Oblast (Russia) were studied. The texture for the most of samples was classified as silty loam in both analyses. However, the laser diffraction underestimates the clay content by an average of 13.2% compared to the pipette method. The average K-factor estimated based on laser diffraction data was 0.050, and 0.034 t ha h ha−1 MJ−1 mm−1 – sedimentation method. Thus, depending on the method of soil texture analysis, the RUSLE calculated soil loss could underestimated/overstated by 32% (or 4 t ha-1 yr-1 on average in the study site). Therefore, we propose a regression equation-based conversion method of laser diffraction data to sedimentation method data for Chernozems.The Laska-TM laser analyzer measured on ∼ 13% less clay fraction (more on ∼ 8% silt and ∼ 5% fine sand) compared with sedimentation method data.For erosional researchers/modelers it is suggested to state the method of soil texture analysis (based on sedimentation law or laser diffraction) was used for RUSLE K-factor calculations.To convert K-factor values (for Chernozems) calculated and based on data of the sedimentation method to laser sedimentation – it suggested utilize the coefficient 1.47 (0.68 – vice versa).

Structure of ZnxFe3−xO4 nanoparticles studied by neutron diffraction and its relation with their response in magnetic hyperthermia experiments

The mixed zinc-ferrite spinel magnetic nanoparticles (MNPs) with the general formula ZnxFe3−xO4 are among the most extensively studied families of Fe oxides due to their interesting and diverse chemical, electronic, and magnetic properties. These systems offer the possibility of surface functionalization and possess high biocompatibility, making them highly attractive for applications in biomedicine, such as magnetic fluid hyperthermia (MFH). The efficiency of the MFH process relies on the magnetic, structural and morphological properties of the MNPs. The substitution with the Zn ion and the cationic distribution, as well as the synthesis process employed, have a direct impact on the final properties of these oxides. Therefore, it is essential to have tools that enable a comprehensive characterization of the system to assess its performance in MFH. In this study, we have synthesized four ZnxFe3−xO4 MNP systems using three different methods: two by thermal decomposition at high temperatures, one by co-precipitation, and another by co-precipitation followed by ball milling. We analyze the effect of these various synthesis processes on the magnetic and crystallographic properties, aiming to correlate them with the response of each system in MFH. Neutron diffraction data are employed to determine the cation site occupation and to investigate the correlation with the synthesis method. MFH measurements were conducted in media of diverse viscosities, revealing different values of specific loss power, thus demonstrating a clear dependence on the synthesis process and Zn content.