XRD Rietveld Refinement Research Articles

A new single-phase NaBi(WO4)2:Dy3+, Eu3+ phosphor with excellent thermal stability for NUV-excited warm white LEDs

A variety of Dy3+ single-doped and Dy3+, Eu3+ co-doped NaBi(WO4)2 phosphors were synthesized by the high temperature solid state method. The XRD patterns and Rietveld refinement measurement were operated to identify the crystalline phases. When the NaBi(WO4)2: 0.08Dy3+, yEu3+ phosphors were excited by 352 nm light, the energy transfer efficiency can be reach to 72.576% and the type of energy transfer mechanism was dominated by the dipole-dipole interaction. The thermal stability of specific NaBi(WO4)2: 0.08Dy3+, 0.1Eu3+ phosphor was tested and the PL emission intensity at 423 K drops to about 77.2% of that at 303 K, and the warm white light can be obtained after varying the Eu3+ ion concentration. Aforementioned results manifest that these as-prepared samples are expected to be the potential single-phase phosphors used in the areas of solid state lighting.

Electrospinning synthesis, crystal structure, and ethylene glycol sensing properties of orthorhombic SmBO3 (B[dbnd]Fe, Co) perovskites

The target of this work is to survey the consequences of various B (BFe, Co) sites of SmBO3 perovskite on crystal structure and ethylene glycol gas-sensitive properties. To this end, two samples based on SmFeO3 and SmCoO3 nanofibers with orthorhombic phase were prepared by a straightforward and efficient electrospinning technique and calcined at 700 °C. The XRD Rietveld refinements and tolerance factor (t) were implemented to research the crystal structure by the lattice parameters, size of BOB angles and t value, BET test shows that as-prepared two samples own different pore sizes, and XPS analyzes the composition and chemical state toward two samples, which indicates that more oxygen vacancies exist in SmFeO3 surface. Then, the gas-sensing performance of SmFeO3 and SmCoO3 nanofibers were compared at their optimal working temperature of 200 °C. The gas-sensing inquiries exhibit that the response of sensor based on SmFeO3 nanofiber (14.3) is almost 6.5 times higher than that of SmCoO3 (2.2) toward 100 ppm ethylene glycol. Finally, the sensing mechanisms of SmFeO3 and SmCoO3 nanofibers were also explained based on pore size, oxygen vacancy, lattice distortion and electrical conductance.

Enhanced mechanical and thermal properties of ferroelastic high-entropy rare-earth-niobates

A novel class of high-entropy rare-earth-niobates (RENbO4) was synthesized via solid-state reaction method. The XRD Rietveld refinement, Raman, and SEM-EDS results implied that the uniform doped element distribution. Unique ferroelastic domain structure formed by t-m phase transition brings the excellent ductility for RENbO4 ceramics (Poisson's ratios > 0.3), where 7RENbO4 exhibits enhanced mechanical properties (Hv = 4.96±0.08 GPa, KⅠc = 2.05±0.14 MPa•m0.5). Moreover, due to the lattice distortion derived from high-entropy effects, high-entropy rare-earth-niobates present lower thermal conductivity (6RENbO4, 2.30-1.40 W m−1 K−1, 100-1000°C) and higher thermal expansion coefficients (5RENbO4, 9.03 × 10−6 K−1, 719°C). These moderate properties indicate a potential materials design for TBCs application.

A new quaternary Li0.19Al2.72O3.64N0.36 transparent ceramic with high hardness

A new quaternary Li0.19Al2.72O3.64N0.36 transparent ceramic with the Vickers hardness of 17.91 ± 0.2 GPa at a load of 9.8 N and the in-line transmittance of 83.4% at 3.5 µm was prepared by hot isostatic press sintering (HIP) after pressureless sintering. The 7Li and 27Al magic-angle spinning (MAS) NMR spectra combined with the XRD Rietveld refinement was adopted to analyze the crystal structure. It is revealed that all the lithium ions are located in octahedra and the cation vacancies are mainly concentrated in tetrahedra. Based on the bond valance models, the complicated relationship among composition, crystal structure and intrinsic hardness of the spinel-type transparent ceramic were disclosed. Compared with the γ-AlON, the higher hardness of Li0.19Al2.72O3.64N0.36 transparent ceramic is attributed to the coupling effect of enhanced hardness of bonds in octahedra and the slightly weakened hardness of bonds in tetrahedra.

Crystal Structure and Ferroelectric Evidence of BaZnSi3 O8 , a Low-Permittivity Microwave Dielectric Ceramic.

BaZnSi3 O8 ceramic was prepared by the conventional solid-state method and sintered at 1100 °C. XRD and synchrotron Rietveld refinement analyses revealed the BaZnSi3 O8 ceramic presented a monoclinic structure with a space group of P21 /a (No.14), which is reported for the first time. The BaZnSi3 O8 ceramic presented a weak ferroelectricity, which was confirmed by the P-E loop and the 90° nanoscale ferroelectric domain. Although ϵr -T displayed two ϵr abnormal peaks at 400 °C and 460 °C, the Curie temperature (Tc ) was located at 460 °C according to the dielectric loss and Curie-Weiss law. Moreover, the BaZnSi3 O8 ceramic exhibited optimized microwave dielectric properties with ϵr =6.55, Q×f=52400 GHz, and τf =-24.5 ppm/°C. Hence, the BaZnSi3 O8 ceramic in the ternary BaO-ZnO-SiO2 system possessed both weak ferroelectricity and microwave dielectric properties. These results are expected to break the technical barrier of ferroelectric phase shifter applications in microwave and even millimeter-wave frequency bands.

Ratiometric fluorescence temperature-sensing properties of Eu3+ and Tm3+ in Gd4.67Si3O13 oxide host

A series of Eu3+ and Yb3+-Tm3+ doped Gd4.67Si3O13 (GS) phosphors were designed by using solid-state reaction method, and their photoluminescence properties were studied for optical temperature sensing applications. Single-phase samples were checked from XRD patterns and Rietveld refinement. Strong red emission of Eu3+ was obtained in the GS:Eu3+ phosphors upon 393 nm excitation. By employing the emissions from 5D1 and 5D0 levels of Eu3+, it has been found that the ratio of 535 and 577 nm emission intensities follows a linear relationship with absolute temperature. High sensitivities were obtained in the 5 mol% Eu3+ doped GS phosphor. It is important to find that the relative sensitivity shows a larger value at higher temperature, indicating the phosphor is more suitable to be used at relatively high temperature. By codoping Yb3+ and Tm3+ into the GS host, the upconversion (UC) luminescence of Tm3+ was received. The corresponding UC luminescent features and mechanism were investigated from the decay curves and pump-power-dependent spectra. Two kinds of fluorescence intensity ratio techniques were employed for the optical temperature sensing, i.e., I697/I648 and I697/I789. The high relative sensitivity (SR) and small SR variation interval for I697/I648 reveal good optical temperature-sensing performance. Owing to the large energy gap between 3H4 and 3F3 levels of Tm3+, high SR value can be achieved for I697/I789.

Role of charge compensation mechanism and defect dipoles on properties of Mn doped BCT ceramics

Single-phase Mn doped Barium Calcium Titanate (BCT) (Ba0.80Ca0.20Ti1-xMnxO3; x = 0.000, 0.005, 0.010, 0.015 and 0.020) lead free ceramics have been prepared by conventional solid-state reaction method. XRD studies and Rietveld refinement confirmed the existence of tetragonal phase (P4mm) for all prepared ceramic compositions. The average grain size increased up to x = 0.005 and thereafter it decreased with increase in Mn content in BCT compositions. Analysis of temperature-dependent dielectric study revealed phase transformation from tetragonal to cubic phase and defect dipole induced anomaly in paraelectric region of temperature-dependent dielectric constant (εʹ–T) curve. Degree of diffusiveness increased with Mn doping in BCT ceramics as confirmed by evaluating diffused phase transition (DPT) parameters (γ and δc) by Power Law fitting and width of diffused phase transition (Dʹ) obtained from derivative of εʹ–T curve. Ferroelectric (P-E loops) study revealed that ceramic composition with x = 0.015 Mn content showed the highest remnant polarization (Pr) and maximum polarization (Pmax) of 14.10 μC/cm2 and 24.20 μC/cm2 respectively. Enhancement in energy storage properties with applied electric fields have been observed at room temperature. Maximum energy storage density Wrec ̴ 190.89 mJ/cm3 with an efficiency of 48.63% has been obtained for x = 0.015. A large piezoelectric charge coefficient (d33) of 460 pC/N has been obtained for x = 0.020. The room temperature magnetic measurements shows feeble ferromagnetism for Mn doped samples. These studies suggest the application of these ceramics for multilayer ceramic capacitors, energy storage, and high power applications.

Difference between Internal and External Hydration of Hardened Cement Paste under Microwave Curing

In order to investigate the difference between internal and external hydration of hardened cement paste under microwave curing, a comparative study on the hydration products, hydration degree, fracture morphology, and pore structure between the inner part and outer part of hardened cement paste (Φ120 mm × 120 mm) under microwave curing was carried out by XRD‐Rietveld refinement, TG‐DSC, SEM, and MIP methods. The results show that the total hydration degree of the inner part is lower at early ages, but with the hydration, there is little difference in the hydration degree between inner and outer parts at later ages. Apart from granular AFt crystal formed in the inner part of hardened cement paste, there is little difference in the fracture morphology between internal and external hydration. The total porosity of the outer part is lower than that of the inner part.

An efficient method for large-scale preparation of high-purity α-Si3N4 nanowires and their electrochemical performance

An efficient and catalyst-free method for the large-scale preparation of high-purity α-Si3N4 nanowires was demonstrated by annealing absorbent cotton and silicic acid in a flowing nitrogen atmosphere. The pyrolysis of absorbent cotton generated a fluffy structure constructed by carbon microfibers, which could promote the growth of α-Si3N4 nanowires. The nanowires were characterized by XRD and XRD Rietveld refinement, SEM and TEM. The results indicated that the nanowires have diameters of 50–100 nm and lengths of tens to hundreds of microns. Vapor-solid (VS) mechanism was proposed to be responsible for the formation of nanowires. The α-Si3N4 nanowires were then applied as anode materials for lithium-ion batteries (LIBs), exhibiting good rate capability and cycling property.

Synthesis and characterization of cryptomelane (α-MnO2) nanoparticles: Influence of phthalic acid adsorption and oxidation on the mineral structure

Cryptomelane (α-MnO2) nanoparticles synthesis was achieved via a Sol-Gel route in mild conditions. XRD analysis showed that the α-MnO2 phase was of high purity and crystallized in the monoclinic space group I2/m, with 12 nm average crystallite size (D). After interaction with an organic pollutant (Phthalic acid, PA), excepting the pronounced decrease in β angle, α-MnO2 cell parameters slightly changed, probably resulting from leaching of K+ cations. Adsorption isotherm of PA on α-MnO2 nanoparticles was fitted in L2 type Langmuir model. Accordingly, an outer-sphere PA-Mn surface complex was suggested. Further, the mineral oxide exerted a low activity in the decarboxylation of PA. Raman analysis illustrated the major bands, of α-MnO2, and their evolution after adsorption indicated the effect of PA on the phase structure, as revealed by the XRD Rietveld refinement. AFM analysis showed stick shaped nanoparticles with D = 15 nm, but the interaction with PA induced aggregation.

Rietveld Refinement Based Quantitative Phase Analysis (QPA) of Ouargla (Part of Grand Erg Oriental in Algeria) Dunes Sand

In this paper, XRD Rietveld refinements by using MAUD (Materials Analysis Using Diffraction) software have been performed to determine the quantitative identification of the crystalline phases in the dunes sand of Ouargla (Algeria). The main XRD reflections were related to quartz (SiO2), gypsum (CaSO42(H2O)) and bassanite (CaSO40.67(H2O)). Structural (space group, lattice parameters and unit cell volume), microstructural (crystallite size and microstrain) and percentages have been determined for each constituting phase. The XRD patterns of natural sample of Ouargla dunes sand indicated that the quartz in this sand has high crystalline nature and (101) is the preferred orientation of quartz growth. It has been appeared that quartz has the hexagonal structure at α- phase. The crystallite sizes of quartz, gypsum and bassanite were 970.57 nm, 522.70 and 99.98 nm respectively. Some comparisons have been made with other recent works. The refined XRD patterns show that quartz and gypsum were the main components in this sand, with 72.11% and 23.77% respectively, in addition to 4.34% of basanite. All this was done with goodness of fit (GOF) 1.70.

Communication—Luminescence Properties of a Novel l Rb2KGaF6:Mn4+ Red-Emitting Phosphor for Solid-State Lighting

A novel red-emitting Rb2KGaF6:Mn4+ phosphor with octahedral particulate morphology was presented. The XRD Rietveld refinement results indicate that the phosphor crystallized into the cubic phase of Fm m space group with double perovskite structure. The photo-luminescence spectrum exhibits intense red emission lines with zero-phonon line (ZPL) and v 6 peak locating at 620 and 628 nm respectively. The optical parameters of low color temperature (T c = 3824 K) and high color rendering index (R a = 90.2 ) from white LED imply its potential application in solid-state lighting.

Influence of Na substitution on structural, magnetic, optical and photocatalytic properties of bismuth ferrite nanoparticles

We have reported the influence of Na substitution on structural, magnetic, optical and photocatalytic properties of sol–gel route synthesized Bi1−xNaxFeO3 (x = 0.0, 0.02, 0.04, 0.06 and 0.08) nanoparticles. Rietveld refinement of the XRD data and electron microscopy techniques revealed the phase purity and nanocrystalline nature of Bi1−xNaxFeO3 samples. The substitution of Na1+ leads to the structural distortion in BiFeO3 nanoparticles which is apparent from the XRD Rietveld refinement and Raman spectroscopy studies. The ferromagnetic ordering parameters increase with increasing Na content in BiFeO3 nanoparticles and the highest magnetization 0.91 emu/g at 30kOe is observed for x = 0.08 sample. The observed enhanced ferromagnetic behaviour of Bi1−xNaxFeO3 nanoparticles are also endorsed by the ESR analysis. The energy bandgap of BiFeO3 nanoparticles is altered by aliovalent Na ions substitution from 2.16 to 2.03 eV. Compared to pristine BiFeO3, the Na-substituted BiFeO3 nanoparticles revealed the much-advanced photocatalytic activity of methylene blue (MB) and crystal violet (CV) under UV–visible light irradiation. In the irradiation time of 100 min, Bi0.96Na0.04FeO3 nanoparticles showed ~ 95% MB and ~ 84% CV degradation. The outstanding changes in the magnetic and photocatalytic properties of Bi1−xNaxFeO3 nanoparticles are due to the differences in the ionic radii, aliovalency between the Bi3+ and Na1+ ions and oxygen vacancies.

Structural refinement and electrochemical properties of one dimensional (ZnO NRs)1\u2212x(CNs)x functional hybrids for serotonin sensing studies

Herein, the efficient serotonin (5-HT) sensing studies have been conducted using the (ZnO NRs)1−x(CNs)x nanocomposites (NCs) having appropriate structural and electrochemical properties. Initially, the different compositions of ZnO nanorods (NRs), with varying content of carbon nanostructures (CNs=MWCNTs and RGO), are prepared using simple in-situ wet chemical method and thereafter these NCs have been characterized for physico-chemical properties in correlation to the 5-HT sensing activity. XRD Rietveld refinement studies reveal the hexagonal Wurtzite ZnO NRs oriented in (101) direction with space group ‘P63mc’ and both orientation as well as phase of ZnO NRs are also retained in the NCs due to the small content of CNs. The interconnectivity between the ZnO NRs with CNs through different functional moieties is also studied using FTIR analysis; while phases of the constituents are confirmed through Raman analysis. FESEM images of the bare/NCs show hexagonal shaped rods with higher aspect ratio (4.87) to that of others. BET analysis and EIS measurements reveal the higher surface area (97.895 m2/g), lower charge transfer resistance (16.2 kΩ) for the ZCNT 0.1 NCs to that of other NCs or bare material. Thereafter, the prepared NCs are deposited on the screen printed carbon electrode (SPCE) using chitosan as cross-linked agent for 5-HT sensing studies; conducted through cyclic voltammetry (CV) and square wave voltammetry (SWV) measurements. Among the various composites, ZCNT0.1 NCs based electrodes exhibit higher sensing activity towards 5-HT in accordance to its higher surface area, lower particle size and lower charge transfer resistance. SWV measurements provide a wide linear response range (7.5–300 μM); lower limit of detection (0.66 μM), excellent limit of quantification (2.19 μM) and good reproducibility to ZCNT 0.1 NCs as compared to others for 5-HT sensing studies.

Understanding the relationship between the local crystal structure and the ferrimagnetic ordering of CoxMn3-xO4 (x = 0–0.5) solid solutions

The local crystal structure alterations in the tetrahedral positions of the hausmannite Mn3O4 structure by Co2+ ions and its consequence on the magnetic ordering are studied in detail. The cation composition, bond distance and bond angle of the CoxMn3-xO4 series (x = 0.0. 0.1, 0.3 and 0.5) is determined by XRD Rietveld refinement. The charge state of the elements Co, Mn and O are investigated using XPS measurements, which confirm the bivalent cobalt ion occupation in the tetrahedral lattice. Considerable reduction in tetrahedral and axial octahedral bonds with the introduction of Co2+ ions dramatically increased the Curie temperature (TC) from 43 K (Mn3O4) to 62 K (Co0.5Mn2.5O4). The Lotgering-Srinivasan-Seehra model is employed to study the canted spin arrangement and the exchange interactions of Co0.5Mn2.5O4. The presence of cluster glass transition at TP = 42 K in Co0.3Mn2.7O4 is well-established through the AC susceptibility measurements and it is further substantiated by Vogel-Fulcher law and dynamic scaling power law. The origin of the cluster glass state is confirmed by the calculated strong geometric frustration factor (f = 19.5), due to the inhomogeneous distribution of cobalt ions in the intermediate concentrations. Field cooled isothermal magnetic measurements corroborated the exchange bias phenomenon in the Co0.3Mn2.7O4 sample, because of the interaction between ferrimagnetic-cluster glass phases occurring below the spin freezing temperature TP.

A novel synthesis route to obtain magnetic nanocrystalline cobalt ferrite with photo-Fenton activity

A novel unconventional coprecipitation procedure (UCP) followed by a simple and fast microwave-assisted hydrothermal (MAH) treatment was used to synthesize a new nanocrystalline magnetic cobalt ferrite (CoFe2O4/MAH) with photo-Fenton activity. The Co-ferrite nanoparticles were obtained at room temperature in the absence of surfactants and their photo-Fenton activity was evaluated through lignin degradation. It was found that microwave hydrothermal treatment is mandatory to obtain magnetic and photoactive Co-ferrite. According to XRD Rietveld refinements and FTIR, the photoactivity was mainly attributed to the Co2+ cation migration from octahedral to tetrahedral sites in the ferrite structure during the MAH treatment, leading, consequently, to a higher Fe3+ incorporation at octahedral sites, which strongly participate in the photo-Fenton degradation mechanism. The magnetic property of the CoFe2O4/MAH ferrite nanoparticles was confirmed by magnetometry and provided an easy catalyst separation.

A novel efficient Mn4+-activated Ba2YTaO6 far-red emitting phosphor for plant cultivation LEDs: Preparation and photoluminescence properties

Novel efficient Ba2YTaO6:Mn4+ (BYT:Mn4+) far-red emitting double-perovskite phosphors for plant cultivation LEDs were reported in this article. These phosphors were successfully synthesized via a traditional high-temperature solid-state reaction method, and their crystal structure, luminescence properties, fluorescence decay lifetimes, Commission Internationale de l'Eclairage (CIE) chromaticity coordinates, internal quantum efficiency, and thermal stability have been systematically investigated. XRD Rietveld refinement demonstrated that the BYT:Mn4+ compound crystallized into cubic crystal system with Fm3‾m space group, and the lattice parameter were a = b = c = 8.445 (7) Å, α = β = γ = 90°, and V = 602.231 (10) Å3. Interestingly, the obtained samples showed an intense far-red emission band centered at 690 nm under excitation of 360 nm, which matched well with the absorption band of phytochrome PFR. In BYT:Mn4+ phosphors, the Mn4+ ions occupied the TaO6 octahedron by replacing the Ta5+ site, and the optimal doping concentration of Mn4+ ions was determined to be 0.4 mol%. The CIE chromaticity coordinates and internal quantum efficiency of BYT:0.4%Mn4+ phosphors were (0.7283, 0.2717) and 41.5%, respectively. In addition, when the temperature reached at 423 K, the emission intensity of BYT:0.4%Mn4+ phosphors remained 37% of that at 303 K. Therefore, all of these investigations demonstrated that BYT:Mn4+ phosphors could be used as potential far-red emitting phosphors for plants cultivation LEDs.

Heat capacity and high temperature electrical transport properties of TbNiC2

The single phase polycrystalline TbNiC2 sample was obtained by annealing at 1073 K. The compound adopts structure of CeNiC2-type, confirmed by XRD Rietveld refinement: space group Amm2, a = 3.6000(2) Å, b = 4.5129(2) Å, c = 6.0563(3), RB(I) = 3.72%, Rp = 5.46%. The orthorhombic CeNiC2 crystal structure prototype is shown to be derived from the hexagonal AlB2 one (space group P6/mmm) following the Bärnighausen formalism via translationengleiche. Zero-field heat capacity measurements of TbNiC2 in the range of 1.9–300 K reveal Sommerfeld coefficient γ = 8(1) mJ mol−1 K−2, phonon coefficient β = 1.18(1)∙10−4 J mol−1 K−4 with the derived Debye temperature of ΘD ≈ 404 K and antiferromagnetic state below TN = 25 K with a spin-wave excitation gap of Δ = 26(2) K. The 4f-electron contribution to the magnetic entropy change indicates a doublet ground state for a non-Kramer's Tb3+ ion. Thermopower and electrical resistivity of TbNiC2 have been measured in the range of 310–855 K and reveal values characteristic for metallic systems. Seebeck coefficient decreases with increasing temperature approximately linearly in the all studied interval, and its sign changes from positive to negative one at ~660 K, whereby the electrical resistivity increases from 310 K reaching maximum at ~640 K and afterwards decreases slightly. Maximum power factor value of 27 μW m−1 K−2 has been observed at 310 K.

Synergy effects between Li0.42Zn0.27Ti0.11Fe2.2O4 nanoparticles and CuO-Bi2O3 mixtures in low-temperature sintered LiZnTi ferrites with enhanced gyromagnetic and microwave dielectric properties

Promoting grain growth and optimizing microstructure are valid strategies for enhancing gyromagnetic and microwave dielectric properties of low-temperature sintered ferrite materials. Here, a modified low-temperature sintering technique was attempted for the synthesis of LiZnTi ferrites that have compact microstructure and improved performances. Trace amounts of CuO-Bi2O3 mixtures (0.50 wt%) were adopted as sintering additives to promote grain growth and to reduce the sintering temperature. Meanwhile, Li0.42Zn0.27Ti0.11Fe2.2O4 nanoparticles (∼21.9 nm) were synthesized using a sol-gel auto-combustion method and were used to optimize the microstructure and to restrain abnormal grain growth. XRD Rietveld refinement and SEM images revealed that uniform and dense LiZnTi ferrites with single-phase spinel structure were obtained. Results demonstrated that co-doping of Li0.42Zn0.27Ti0.11Fe2.2O4 nanoparticles and CuO-Bi2O3 mixtures allows low-temperature sintering (900 °C) to be achieved and also promotes grain growth and densification. In particular, LiZnTi ferrites that were modified with 5.00 wt% Li0.42Zn0.27Ti0.11Fe2.2O4 nanoparticles and 0.50 wt% CuO-Bi2O3 sintering additives exhibited narrow ferromagnetic resonance linewidth (ΔH, ∼145 Oe) and low dielectric loss tangent (tanδε, ∼2.45 × 10−4) at ∼9.50 GHz, high saturation flux density (Bs, ∼364 mT), and high squareness ratio (Br/Bs, ∼0.89). Such a modified sintering technique at a low sintering temperature, as reported in this work, provides a reference for other advanced ferrites.

Cation exchange in Ni–Cu–Zn aluminate spinels revealed by EXAFS

Nanocrystalline Ni–Cu–Zn aluminate powders (Ni1-xCuxAl2O4, Cu1-xZnxAl2O4, and Zn1-xNixAl2O4) with different divalent ion concentrations (0 ​≤ ​x ​≤ ​1) were successfully synthesized by the sol-gel auto combustion method using diethanolamine (DEA) as a novel fuel. The structural, morphological, and the local atomic structures of each calcined sample were investigated by XRD, TEM, and synchrotron EXAFS measurements. The XRD results confirmed the formation of single-phase spinel structure with Fd-3m space group of all samples. When XRD Rietveld refinement and Williamson-Hall analysis were applied to the XRD data, the exact crystallite size and structural parameters were obtained. The EXAFS spectra showed the main translocation trends in the trivalent (Al3+) and divalent (Ni2+, Cu2+, Zn2+) ions between the tetrahedral (A) and octahedral (B) sublattices. Furthermore, the degree of inversion in these spinel aluminates is completely dissimilar and identified as 0.493–0.499 for Ni1-xCuxAl2O4, 0.254–0.498 for Cu1-xZnxAl2O4 and 0.093–0.453 for Zn1-xNixAl2O4 series, as indicated by the multiple-edge curve-fitting analysis of Ni, Cu, and Zn K-edge EXAFS spectra. These values comprise essential data for comprehension of numerous relevant properties.