Synchrotron X-ray Diffraction Measurements Research Articles

Superconducting properties and electronic structure of CuAl2-type transition-metal zirconide Fe1-xNixZr2

CuAl2-type transition-metal (Tr) zirconides are a superconductor family, and the Tr-site element substitution largely modifies its transition temperature (Tc). Here, we synthesized polycrystalline samples of Fe1-xNixZr2 by arc melting. The crystal structure and the superconducting properties were studied through synchrotron X-ray diffraction, magnetic susceptibility, electrical resistivity, and specific heat measurements. Bulk superconductivity was observed for 0.4 ≤ x ≤ 0.8, and the highest Tc of 2.8 K was observed for x = 0.6. The obtained superconductivity phase diagram exhibits a dome-shaped trend, which is similar to unconventional superconductors, where magnetic fluctuations are essential for superconductivity. In addition, from the c/a lattice constant ratio analysis, we show the possible relationship between the suppression of bulk superconductivity in the Ni-rich compositions and a collapsed tetragonal transition.

Pressure-induced superconductivity and phase transition in PbSe and PbTe

Abstract The IV-VI semiconducting chalcogenides are a large material family with distinct physical behavior. Here, we systematically investigate the effect of pressure on the electronic and crystal structure in PbSe and PbTe by combining high-pressure electrical transport and synchrotron x-ray diffraction (XRD) measurements. The resistivity of PbSe and PbTe changes dramatically under high pressure and a non-monotonic evolution of ρ(T) is observed. Both PbSe and PbTe are found to undergo semiconductor-metal transition upon compression and show superconductivity under higher pressure. The structural evolutions from the Fm-3m to Pnma phase and then to the Pm-3m phase in PbSe are verified by the x-ray diffraction. The present findings reveal the internal correlation between the structural evolution and the physical properties in lead chalcogenides.

Thermal and structural analysis of binary mixtures of pyrimidine liquid crystals using Modulated Differential Calorimetry and Synchrotron X-ray Diffraction measurements.

We present a systematic experimental dataset on the temperature dependence of specific heat capacity in a binary mixture of the second and seventh homologous series of 5-alkyloxy-2-(4-nonyloxy-phenyl) pyrimidine(PhP) liquid crystal compound. These binary mixtures exhibit nematic, smectic-A, and smectic-C phases within a concentration range of xPhP1 = 0 to 0.45. The liquid crystalline phases are structurally characterized using synchrotron X-ray diffraction. We determine the apparent molecular length in the nematic phase, smectic layer spacing, average distance between the long axes of molecules, correlation length, and orientational order parameters (<P2> and <P4>) as functions of temperature. The tilt angle in the SmC phase is inferred from the layer spacing data. To examine the critical behavior near the nematic to smectic A(NA) and smectic A to the smectic C (AC) phase transitions, we evaluate the critical exponents: α from specific heat capacity, β from the fitting of the temperature-dependent tilt angle, and ν‖, ν⊥from the temperature-dependent longitudinal (ξ‖) and transverse (ξ⊥) correlation lengths. Modulated Differential Scanning Calorimetry (MDSC) measurements indicate the absence of phase shift, latent heat and imaginary specific heat capacity, suggesting that the AC transitions are second-order for all binary mixtures. The results obtained from heat capacity reveal that both the AC and NA transitions exhibit non-universal behaviours with effective exponents lying between the tricritical and 3D-XY values and follow nearly identical curve with decreasing width of the Sm-A and N phases. The Josephson hyperscaling relation is verified for both the NA and AC transitions in different mixtures. Moreover, knowing the heat capacity critical exponent α and the order parameter critical exponent β, the susceptibility critical exponent γ for the AC transition can be estimated from Rushbrooke equality α+2β+γ=2, with γ values ranging from 1.015 to 1.313, indicating the system's crossover character and apparently validating the Rushbrooke equality.

Laser additive manufacturing of Ti and Ce co-modified 2195 difficult-to-process aluminum alloy: Grain refinement, cracking suppression and enhanced mechanical properties

High cracking susceptibility of Al-Li alloys with Ti/CeB6 addition is thoroughly suppressed in laser powder bed fusion (LPBF) processing of Ti/Ce co-modified 2195 alloys at relatively high scan speeds, while the cracking suppression mechanism and phase formation in these composites are not clarified. In this work, microstructure evolution and mechanical performance of the LPBF-fabricated Ti/Ce co-modified 2195 are investigated to reveal their cracking suppression and strengthening mechanisms. The results show that apparent grain refinement of the composites is ascribed to high supercooling from rapid formation of constitutional supercooling zone in front of solid–liquid interfaces by high-Q-value Ti solute, and heterogeneous nucleation of in situ formed Al3Ti and Al11Ce3 precipitates. Their synergistic interactions promote formation of fine equiaxed grains and thus inhibit crack initiation. The composites exhibit high microhardness of 100 ± 5 HV0.2, nano-hardness of 1.6 ± 0.1 GPa and elastic modulus of 97 ± 3 GPa, where the elastic modulus increases by ∼27% and ∼31% compared to those of LPBF-processed and conventionally manufactured 2195 alloys, respectively. A tensile strength of ∼336 MPa and an elongation of ∼3% are obtained from in-situ synchrotron X-ray diffraction measurement. The improved properties are derived from grain refinement and Orowan strengthening. Based on the optimal processing parameter and composition, a bracket component filled with lattice structures is designed and manufactured with good manufacturing quality and processing accuracy.

In Situ Observation of Topotactic Linker Reorganization in the Aperiodic Metal-Organic Framework TRUMOF-1.

We use in situ synchrotron X-ray diffraction measurements to monitor the solvothermal crystallization mechanism of the aperiodic metal-organic framework TRUMOF-1. Following an initial incubation period, TRUMOF-1 forms as a metastable intermediate that subsequently transforms into an ordered product with triclinic crystal symmetry. We determine the structure of this ordered phase, which we call msw-TRUMOF-1, and show that it is related to TRUMOF-1 through topotactic reorganization of linker occupancies. Our results imply that the connectivity of TRUMOF-1 can be reorganized, as required for data storage and manipulation applications.

Fluorinated Amide-Based Electrolytes Induce a Sustained Low-Charging Voltage Plateau under Conditions Verifying the Feasibility of Achieving 500 Wh kg-1 Class Li-O2 Batteries.

Although lithium-oxygen batteries (LOBs) hold the promise of high gravimetric energy density, this potential is hindered by high charging voltages. To ensure that the charging voltage remains low, it is crucial to generate discharge products that can be easily decomposed during the successive charging process. In this study, we discovered that the use of amide-based electrolyte solvents containing a fluorinated moiety can notably establish a sustained voltage plateau at low-charging voltages at around 3.5 V. This occurs under conditions that can verify the feasibility of achieving a benchmark energy density value of 500 Wh kg-1. Notably, the achievement of the low-voltage plateau was accomplished solely by relying on the intrinsic properties of the electrolyte solvent. Indeed, synchrotron X-ray diffraction measurements have shown that the use of fluorine-containing amide-based electrolyte solvents results in the formation of highly decomposable discharge products, such as amorphous and Li-deficient lithium peroxides.

Evolution of magnetization of Bi1-ySmyFe1-xTixO3 ceramics at the morphotropic phase boundary attested by multistep magnetization measurements, time aging and electric field

Bi1-ySmyFe1-xTixO3 ceramics with compositions at the rhombohedral- orthorhombic morphotropic phase boundary (y = 0.1, 0.12, 0 ≤ x ≤ 0.1) were prepared by solid state reaction method. Analysis of the crystal structure of the compounds based on the results of laboratory and synchrotron X-ray diffraction measurements as well as Raman spectroscopy experiments revealed a coexistence of the rhombohedral phase (SG R3c) and the anti-polar orthorhombic phase (SG Pbam) in the compounds Bi0.88Sm0.12Fe1-xTixO3 with 0 ≤ x ≤ 0.1; the compounds Bi0.9Sm0.10Fe1-xTixO3 are characterized by the mixed structural state for the concentration range 0 ≤ x ≤ 0.06 and by the single phase rhombohedral state within 0.06 < x ≤ 0.1. Room temperature magnetization measurements demonstrate a gradual increase of remanent magnetization with Ti content in the compounds of both systems up to the maximal value of MR ∼0.28 emu/g for compounds with x = 0.06 which is followed by a decrease in magnetization with further titanium doping. Temperature decrease leads to a reduction of remanent magnetization which is mainly caused by a partial recovery of spatially modulated spin structure occurred in the compounds of both systems. Time aging of the compounds for about ∼1 year leads to a drastic increase of MR, which is caused by a change in the structural phase ratio, homogeneity of the structural state and a contribution of unbounded spins demonstrated by low field measurements. Subjecting of the annealed compounds to external electric field of E ∼40 kV/cm leads to a decrease of magnetization associated with backward structural transformations and redistribution of the local structural defects in the compounds.

Effects of quenching on domain switching and electric field-induced phase transformations in Na0.5Bi0.5TiO3-NaNbO3 ceramics

Quenching from high temperatures has been identified as a useful means to enhance the piezoelectric properties and thermal stability of bismuth-based perovskite ferroelectrics. In the present work, it is demonstrated that quenching leads to improvement of depolarization temperature, ferroelectric and piezoelectric properties in Na0.5Bi0.5TiO3-NaNbO3 (NBT-0.1NN) ceramics. In-situ synchrotron x-ray diffraction measurements indicated an irreversible transformation from cubic to coexisting cubic and rhombohedral phases during the application of a high electric field, for both as-sintered and quenched ceramics. These results confirm the non-ergodic relaxor ferroelectric nature of the materials. DC poling induced a transformation to single-phase rhombohedral structure in both cases, with highly textured domain configurations. These well-oriented ferroelectric domain states were relatively stable under subsequent bipolar electric field cycling. For the pre-poled NBT-0.1NN ceramics, the quenched samples were found to exhibit the highest intrinsic (lattice strain) and extrinsic (domain switching) contributions to electrostrain, due to the increased rhombohedral distortion.

Effects of Fe substitution for Mn on structural, magnetic and magnetocaloric properties of TbMn2-xFexSi2

The structural and magnetic properties of TbMn2-xFexSi2 compounds (x = 0.0–0.4) have been investigated in details by high-resolution synchrotron x-ray and neutron powder diffraction, specific heat, and dc magnetization measurements. The replacement of Fe for Mn in TbMn2-xFexSi2 does not change the crystal structure but leads to a significant contraction of the unit cell (dV/dx ∼ - 6 Å3) and modification of three magnetic phase transition temperatures – the Curie temperatures Tc1, Tc2 and the Néel temperature TN. For example, the Tc1, Tc2 and TN values of TbMn2Si2 decrease from Tc1 = 50 K, Tc2 = 64 K and TN = 500 K to Tc1 = 27 K, Tc2 = 37 K and TN = 440 K for TbMn1.6Fe0.4Si2. Detailed neutron diffraction investigations have allowed us to determine the magnetic structures and construct the magnetic phase diagram as well as confirm the presence of magnetoelastic coupling effects. The significantly different responses of Tc1 and Tc2 to applied magnetic fields (e.g. dTc1/dB = 0.52 K/T and dTc2/dB = 4.7 K/T for TbMn1.6Fe0.4Si2), leads to expansion of the temperature region (ΔT = Tc2- Tc1) for the canted ferromagnetic state Fmc-ii between Tc1 and Tc2. In the case of TbMn1.6Fe0.4Si2, ΔT increases from ΔT = 9 K for applied magnetic field B = 0.2 T to ΔT = 36 K for B = 6 T, resulting in plateau-like behaviour of magnetic entropy change and enhances the relative cooling power (RCP) in this system. Under a change of magnetic field of 0 T – 5 T, the maximum value of the magnetic entropy changes -ΔSmax and adiabatic temperature change, ΔTad are derived to be -ΔSmax = 13.1 J/kg K and ΔTad = 8.4 K with the RCP = 411 J/kg for x=0.4 sample. The plateau-like magnetocaloric effect and relatively large RCP make these materials potentially suitable for application in cryogenic magnetic refrigeration.

Exploring the Structural, Optical and Photoluminescence Performances of CuCo2O4 and ZnMn2O4 Alloying

The performance of the structural, linear/ nonlinear optical and photoluminescent properties of CuCo2O4 and ZnMn2O4 alloying was investigated. (1−x)CuCo2O4/(x)ZnMn2O4 (x = 0, 0.10, 0.15, 0.2) samples were prepared by the sol-gel and hydrothermal procedures. Synchrotron X-ray diffraction measurements were employed to investigate the structural and microstructural properties applying the Rietveld refinement method. Fourier transform infraed and Raman techniques were applied to explore the structures’ variation and chemical bonding of the obtained phases. Ultraviolet–visible diffuse reflectance spectroscopy measurements were collected to explore the optical properties. The optical band gap values were determined using the Kubelka-Munk method. All samples exhibited two band gaps in the visible-NIR regions. Upon composing with ZnMn2O4, the band gaps of CuCo2O4 declined for x = 0.1 and 0.15, followed by an increase at x = 0.2. The possible electronic band structure of the samples and the photoluminescent performance of the prepared samples was investigated. The observed PL patterns manifest wide and asymmetrical emissions. The CIE chromaticity diagram for all samples was plotted. The obtained findings of (1−x)CuCo2O4/(x)ZnMn2O4 nominate their efficient role in optical device fabrication and photocatalyst applications.

Tuning the Superspin Dynamics in Inverse Spinel Ferrite Nanoparticle Ensembles via Indirect Cation Substitution

We used magnetic and synchrotron X-ray diffraction measurements to investigate the possibility of tuning the strength of magnetic interparticle interactions in nanoparticle ensembles via chemical manipulation. Our main result comes from temperature-resolved in-phase ac-susceptibility data collected on 8 nm average-diameter Ni0.25Zn0.75Fe2O4 (Ni25) and Ni0.5Zn0.5Fe2O4 (Ni50) nanoparticles at different frequencies, χ′ vs. T|f. We found that the relative peak temperature variation per frequency decade, ϕ=∆TT·∆log(f)—a known measure of interparticle interaction strength—exhibits a four-fold increase, from ϕ = 0.04 in Ni50 to ϕ = 0.16 in Ni25. This corresponds to a fundamental change in the nanoparticles’ superspin dynamics, as proven by the fit of phenomenological models to magnetic relaxation data. Indeed, the Ni25 ensemble exhibits superparamagnetic behavior, where the temperature dependence of the superspin relaxation time, τ, is described in the Dorman–Bessais–Fiorani (DBF) model: τT=τrexp⁡EB+EadkBT, with parameters τr = 4 × 10−12 s, and (EB + Ead)/kB = 1473 K. On the other hand, the nanoparticles in the Ni50 ensemble freeze collectively upon cooling in a spin-glass fashion according to a critical dynamics law: τ(T)=τ0TTg−1zν, with τ0 = 4 × 10−8 s, Tg = 145 K, and zν = 7.2. Rietveld refinements against powder X-ray diffraction data reveal the structural details that underlie the observed magnetic behavior: an indirect cation replacement mechanism by which non-magnetic Zn ions are incorporated in the tetrahedral sites of the inverse spinel.

Growth of Size-Tunable Ag2O Polyhedra and Revelation of Their Bulk and Surface Lattices.

By primarily adjusting the reagent amounts, particularly the volume of AgNO3 solution introduced, Ag2O cubes with decreasing sizes from 440 to 79 nm, octahedra from 714 to 106 nm, and rhombic dodecahedra from 644 to 168 nm are synthesized. 733 nm cuboctahedra are also prepared for structural analysis. With in-house X-ray diffraction (XRD) peak calibration, shape-related peak shifts are recognizable. Synchrotron XRD measurements at 100 K reveal the presence of bulk and surface layer lattices. Bulk cell constants also deviate slightly. They show a negative thermal expansion behavior with shrinking cell constants at higher temperatures. The Ag2O crystals exhibit size- and facet-dependent optical properties. Bandgaps red-shift continuously with increasing particle sizes. Optical facet effect is also observable. Moreover, synchrotron XRD peaks of a mixture of Cu2O rhombicuboctahedra and edge- and corner-truncated cubes exposing all three crystal faces can be deconvoluted into three components with the bulk and the [111] microstrain phase as the major component. Interestingly, while the unheated Cu2O sample shows clear diffraction peak asymmetry, annealing the sample to 450 K yields nearly symmetric peaks even when returning the sample to room temperature, meaning even moderately high temperatures can permanently change the crystal lattice.

In situ electric field-dependent structural changes in (Ba,Ca)(Zr,Ti)O3 with varying grain size

The functional properties of piezoelectric ceramic materials, such as barium titanate, are highly dependent on grain size. Lead-free polycrystalline Ba0.85Ca0.15Zr0.1Ti0.9O3 (BCZT) samples were prepared with a combination of the hydrothermal method and spark plasma sintering to achieve grain sizes from 100 nm to 10 μm by varying the maximum sintering temperature. In this range, a transition from a nearly linear dielectric to a ferroelectric response can be seen in macroscopic electromechanical measurements, demonstrating the importance of grain size on functional properties in BCZT. Furthermore, in situ electric field-dependent synchrotron x-ray diffraction measurements were performed to quantify the intrinsic and extrinsic strain contributions and their variations with grain size. At lower grain sizes, the data revealed a significant loss of extrinsic contributions in the piezoelectric behavior, limiting the response to intrinsic contribution associated with lattice strain. For BCZT, a critical grain size between approximately 0.08 and 0.18 μm is proposed, below which no piezoelectric response was observed.

Size-Dependent High-Pressure Behavior of Pure and Eu3+-Doped Y2O3 Nanoparticles: Insights from Experimental and Theoretical Investigations.

We report a joint high-pressure experimental and theoretical study of the structural, vibrational, and photoluminescent properties of pure and Eu3+-doped cubic Y2O3 nanoparticles with two very different average particle sizes. We compare the results of synchrotron X-ray diffraction, Raman scattering, and photoluminescence measurements in nanoparticles with ab initio density-functional simulations in bulk material with the aim to understand the influence of the average particle size on the properties of pure and doped Y2O3 nanoparticles under compression. We observe that the high-pressure phase behavior of Y2O3 nanoparticles depends on the average particle size, but in a different way to that previously reported. Nanoparticles with an average particle size of ~37 nm show the same pressure-induced phase transition sequence on upstroke and downstroke as the bulk sample; however, nanoparticles with an average particle size of ~6 nm undergo an irreversible pressure-induced amorphization above 16 GPa that is completed above 24 GPa. On downstroke, 6 nm nanoparticles likely consist of an amorphous phase.

A Scalable Robust Microporous Al-MOF for Post-Combustion Carbon Capture.

Herein, a robust microporous aluminum tetracarboxylate framework, MIL-120(Al)-AP, (MIL, AP: Institute Lavoisier and Ambient Pressure synthesis, respectively) is reported, which exhibits high CO2 uptake (1.9mmol g-1 at 0.1bar, 298 K). In situ Synchrotron X-ray diffraction measurements together with Monte Carlo simulations reveal that this structure offers a favorable CO2 capture configuration with the pores being decorated with a high density of µ2-OH groups and accessible aromatic rings. Meanwhile, based on calculations and experimental evidence, moderate host-guest interactions Qst (CO2) value of MIL-120(Al)-AP (-40kJ mol-1) is deduced, suggesting a relatively low energy penalty for full regeneration. Moreover, an environmentally friendly ambient pressure green route, relying on inexpensive raw materials, is developed to prepare MIL-120(Al)-AP at the kilogram scale with a high yield while the Metal- Organic Framework (MOF)is further shaped with inorganic binders as millimeter-sized mechanically stable beads. First evidences of its efficient CO2/N2 separation ability are validated by breakthrough experiments while operando IR experiments indicate a kinetically favorable CO2 adsorption over water. Finally, a techno-economic analysis gives an estimated production cost of ≈ 13 $ kg-1, significantly lower than for other benchmark MOFs. These advancements make MIL-120(Al)-AP an excellent candidate as an adsorbent for industrial-scale CO2 capture processes.

Pressure-induced magnetic phase and structural transition in SmSb2

Abstract Motivated by the recent discovery of unconventional superconductivity around a magnetic quantum critical point in pressurized CeSb2, here we present a high-pressure study of an isostructural antiferromagnetic (AFM) SmSb2 through electrical transport and synchrotron x-ray diffraction measurements. At P C ~2.5 GPa, we found a pressure-induced magnetic phase transition accompanied by a Cmca→P4/nmm structural phase transition. In the pristine AFM phase below P C, the AFM transition temperature of SmSb2 is insensitive to pressure; in the emergent magnetic phase above P C, however, the magnetic critical temperature increases rapidly with increasing pressure. In addition, at ambient pressure, the magnetoresistivity (MR) of SmSb2 increases suddenly upon cooling below the AFM transition temperature and presents linear nonsaturating behavior under high field at 2 K. With increasing pressure above P C, the MR behavior remains similar to that observed at ambient pressure, both in terms of temperature- and field-dependent MR. This leads us to argue an AFM-like state for SmSb2 above P C. Within the investigated pressure of up to 45.3 GPa and the temperature of down to1.8 K, we found no signature of superconductivity in SmSb2.

Intertwined crystal structure, magnetic, and charge transport properties in mixed valent A-site ordered manganite NdBaMn2O6

In the present work, we report a correlation between crystal structure, magnetic, and electrical properties in an exotic magnetic compound, NdBaMn2O6 having ∼92% ordering between Nd and Ba, investigated using temperature-dependent synchrotron x-ray diffraction (XRD), dc magnetization and transport measurements. Temperature-dependent XRD data reveals that the compound undergoes various complex crystallographic phase transitions from high-temperature (T > 320 K) P4/mmm phase to intermediate (320 K – 280 K) Cmmm phase to a mixed (Cmmm and P21am) phase (280 K – 220 K) and to low-temperature P21am phase (T < 220 K). It is found that these crystallographic phase compositions play a crucial role in controlling its magnetic and transport properties. Temperature-dependent dc magnetization data show a sharp drop at the onset of mixed phase (Cmmm + P21am) at 280 K followed by a broad hump at ∼ 220 K where mixed phase to P21am transition occurs, thus indicating a correlation between the structural and magnetic properties. The dc magnetization in the mixed phase region is calculated by considering a superposition of the magnetic moments of Cmmm and P21am phases weighted by the fraction of each phase, which exactly follows the experimental magnetization data. Temperature variation of resistivity data shows a jump at ∼260 K, a temperature corresponding to 50–50% phase composition of Cmmm and P21am phases. The compound shows insulating behavior over a whole temperature range as confirmed from the resistivity data. Further, application of magnetic field causes a shift of magnetic and transport transition temperatures which may be due to the magnetic field induced structural transition in the system.

Optically Electroactive Polymer Synthesized in a Liquid Crystal with Cyclosporin A─Circularly Polarized Electron Spin Resonance.

Cyclosporine A (CsA), a naturally derived biomaterial and physiologically active substance, is commonly used as an immunosuppressant. In this study, CsA was revealed to function as a chiral inducer of cholesteric liquid crystals (CLCs) with a high helical twisting power. CsA induced helical structures in 4-cyano-4'-pentylbiphenyl, a synthetic liquid crystal (LC) used for general purposes. Electrochemical polymerization in CLC with CsA was also performed. The polymer prepared in CLC showed electro-optical activity via chiral induction by CsA. Synchrotron X-ray diffraction measurements indicated that the polymer film prepared in the CLC formed in the manner of LC molecular arrangement through molecular form imprinting from the LC order, although the polymer exhibited no liquid crystallinity. The polymer showed structural color and laser light oscillation diffraction derived from its periodic structure. The anisotropy of the circularly polarized electron spin resonance signals for the resulting polymer with respect to the magnetic field was observed.

Experimental observation of two-dimensional phase in compressed FeF2

Iron difluoride (FeF2) has attracted considerable attention for its physical characteristics and practical applications, and its compression behaviors usually play a key role in the in-depth understanding of this compound. Since its high-pressure crystal structure evolution determining a more profound comprehension remains disputable, we carried out extensive experiments to focus on the pressure-induced structural phase transitions of FeF2. Through in situ high-pressure synchrotron x-ray diffraction measurements, we not only confirmed a reported high-pressure orthorhombic Pbca phase at 11 GPa but also identified an interesting two-dimensional structure with hexagonal close packed symmetry (P-3m1) that appears above 25 GPa at room temperature. Furthermore, the spontaneous strain fitting and electronic transport measurements suggest that its ambient rutile-type structure (P42/mnm) evolves into an orthorhombic structure (Pnnm) through a second-order phase transition at 5 GPa. These experimental results elaborate on the pressure-induced phase transitions of FeF2 on the order of P42/mnm → Pnnm → Pbca → P-3m1, shedding light on a rare three-dimensional to two-dimensional configuration transition in difluorides.

Effects of Ni doping on structural, magnetic and catalytic properties of copper ferrite

The aim of this work was to obtain information about the influence of small quantities of Ni2+ ion on the structural and magnetic properties of the tetragonally distorted of Cu1−xNixFe2O4 series (with x = 0.00, 0.05, 0.1, and 0.15 respectively). The tested ferrite system was synthesized by combustion of citrate–nitrate precursors. The synchrotron X-ray diffraction measurements determined the phase transition temperatures (tetragonal → cubic) of all samples. The change of structures under the influence of temperature shows a phase transition in the range of 390 – 400 °C for x = 0.00, 330 – 370 °C for x = 0.05, 210 – 330 °C for x = 0.1 and 140 – 210 °C for x = 0.15, respectively. The initial phase transition temperature decreases linearly with the decreasing c/a ratio of the crystallographic lattice parameters for the Cu1−xNixFe2O4 oxides. Hysteresis measurements were made to determine the saturation magnetization (MS) and coercive field (µ0Hc) of the samples. The values of magnetic moments at room temperature determined from magnetization measurements are very similar to those obtained from theoretical x-ray diffraction calculations. Magnetic moment values per formula unit are estimated to range from 1.16 μB to 1.5 μB. It was found that the catalytic activity of N2O decomposition of samples increases with increasing nickel content.