Solid-state Route Research Articles

Aminophosphonate/sand nanocomposites for La(III) sorption: Application to REE concentrate

Two α-aminophosphonate anlages (methyl- and phenyl-derivatives, MeAP and PhAP, respectively) were synthesized via an in-situ reaction. Moreover, their corresponding sand nanocomposites, MeAPNC and PhAPNC, respectively, were prepared using an eco-friendly, inexpensive and facile solid-state synthetic route. These materials were extensively characterized by CHNSP/O, XRD, FTIR, SEM-EDX, TEM, and PZC. Lanthanum sorption characteristics were investigated and compared through the study of pH dependence (optimal pH: 4.5), equilibration time (achieved at 120 and 90 min for α-APs and nanocomposites, respectively), and sorption isotherms. The Sips isotherm and pseudo-second-order (PSORE) kinetics were the optimal models for fitting the experimental data. Sorption isotherms showed that methyl-derivatives (≈1.29–1.359 mmol/g) were more effective than their corresponding phenyl-derivatives (≈0.941–0.986 mmol/g) due to steric hindrance, acid-base differences, and inductive effects. Sorbents showed appreciated stability with just a 4.5–10.5 % loss in performance over six reuse cycles using HCl (0.2 M). Notably, sand incorporation slightly increased capacity with half-organic-portion in composites, as well as enhanced kinetics and regeneration efficiency. La(III) sorption is spontaneous, exothermic, and increases randomness across all sorbents. Finally, the prepared sorbents have proven effective sorption for Nd(III) beside La(III) with high selectivity from acidic complex monazite liquor.

Comprehensive analysis of the synthesized Zinc-doped yttrium titanate pyrochlore solid solution: Structural, vibrational, and electrochemical insights

A novel Zinc-doped Yttrium Titanate (YTZ) solid solution with a pyrochlore structure, synthesized via a solid-state route, was investigated for its potential in hydrogen storage applications. Comprehensive characterization using various techniques confirmed the formation of a cubic crystal structure with the Fd-3m space group for compositions within the ZnO content range from x = 0 to 0.30. A subtle increase in the lattice parameter (a) was observed with increasing substitution levels (x). This increase is attributed to the substitution of Zn2+ on Ti4+ sites and the concomitant creation of vacancies in both the anionic and cationic sublattices, as revealed by quantitative Rietveld analysis. The YTZ solid solution exhibits semiconducting behavior with a band gap ranging from 3.10 to 3.25 eV that may contribute to its hydrogen storage properties. Notably, the YTZ0.25 composition displayed a remarkable hydrogen storage capacity of 1200 mAh/g. This can be attributed to the presence of active redox species, favorable morphology, and the structural vacancies introduced by Zn2+ substitution, which facilitate hydrogen interaction. These findings position YTZ solid solution as a promising candidate for clean energy technologies, particularly in the realm of hydrogen storage.

Rare-Earth/d10 Dual-Metal Oxychalcogenides as Infrared Nonlinear-Optical Materials.

Oxychalcogenides are receiving increasing interest as nonlinear-optical (NLO) materials because of the possible combination of advantages from oxides and chalcogenides. Here, two new pentanary oxythiogermanates Eu2MGe2OS6 [M = Zn (1), Cd (2)] were obtained by the facile metal oxide-boron-sulfur solid-state route. They crystallize with a melilite-type structure and feature {[MGe2OS6]4-}∞ layers built by Ge2OS6 dimers and MS4 tetrahedra. Their optical band gaps are 2.37 and 2.38 eV. As the first NLO rare-earth (RE)/d10 dual-metal oxychalcogenides, they exhibit phase-matchable NLO responses and enhanced laser-induced damage thresholds. Theoretical calculations show that the NLO responses are predominantly contributed by the EuOS7 motifs. This work provides the potential of RE/d10 dual-metal-based NLO materials.

Effect of Sr2+ substitution on structural, morphological, electrical and dielectric properties of Ca2MgSi2O7 ceramic

Despite the excellent properties of ceramic materials for electronic devices, this study systematically investigates the significant effects of strontium (Sr2⁺) substitution on the structural, morphological, electrical, and dielectric behavior of Ca2-xSrxMgSi2O7 (x = 0, 0.2, 0.4, 0.6) ceramics. The composite was prepared via a solid-state route and characterized using techniques such as FESEM-EDAX, BET, XRD, Hall Effect measurements, and an LCR meter, respectively. The surface morphology of the structure was initiated to be smooth, compact, dense, island-shaped and porous. It is noted that the grain size reduced (from 1.10 μm to 0.72 μm) while the surface area enlarged (from 90 m2/g to 122 m2/g) with Sr substitution. XRD study showed that all the ceramics samples, after sintering at 1250 °C for 5 h. Higher amount of Sr, enhanced the crystallinity, as validated by the peak intensification. Correspondingly, the electrical resistivity and dielectric permittivity of Ca2-xSrxMgSi2O7 was decreased with Sr substitution. Particularly, the Ca1.6Sr0.4MgSi2O7 unveiled the lowermost electrical resistivity (76 Ω cm) and dielectric permittivity (εr = 848) but the uppermost dielectric loss (tan δ = 1.06) at 1 kHz. The attained outcomes exhibited the appropriateness of these samples for use in capacitor and antennas design.

Correlation between chemical bond characteristics and microwave dielectric properties of KLa(MoO4)2 ceramics

This investigation details the synthesis process of KLa(MoO4)2 ceramic utilizing a solid-state route method, alongside an analysis of its structural characteristics and the correlation between chemical bonds and microwave dielectric properties. The KLa(MoO4)2 phase was identified to possess a Monoclinic structure (C2/c space group). Sintering the sample at 820 °C resulted in a maximum relative density of 94.6% and impressive microwave characteristics: εr = 9.63, Q×f = 50,100 GHz, and τf = -75.7 ppm/°C. Correlations between relative density and dielectric properties were observed. Further, application of the P-V-L bond theory facilitated the analysis of chemical bond parameters and their impact on microwave dielectric properties. The dielectric properties were correlated to chemical bond iconicity, packing fraction, lattice energy and bond valences.

Enhanced electrochemical performance of K0.67[Ni0.3Mn0.6Co0.1] O2 as a cathode material for secondary K-Ion batteries: Improved K-Ion insertion and reduced charge transfer barrier

Potassium-ion batteries, with their high operating voltage and cost-efficiency, emerged as promising contenders for large-scale energy storage system. Nevertheless, the practical application is hindered by the significant challenges of achieving high capacity and good rate capability in cathodes. Herein, a novel layered oxide cathode, K0.67[Ni0.3Mn0.6Co0.1] O2 (KNMCO), has been synthesized via solid-state (S-KNMCO) and co-precipitation (C-KNMCO) routes. The X-Ray diffraction (XRD) peaks of KNMCO are identified in R3 m space group and well-indexed to hexagonal unit cell. The FE-SEM shows non-spherical morphologies for both samples. Additionally, high-resolution transmission electron microscopy (HR-TEM) images of the synthesized cathode materials shows the interlayer spacing of S-KNMCO is higher than that of C-KNMCO. Furthermore, the electrochemical performance of S-KNMCO and C-KNMCO is characterized using K-metal as anode and electrolyte KPF6 in EC/DEC (1:1, v/v). The S-KNMCO and C-KNMCO exhibit the maximum specific discharge capacity of ∼101 mAhg-1 and ∼66 mAhg-1 at the current rate of C/20 respectively. Additionally, these cells show the good rate capability and coulombic efficiency (∼94%). This research offers novel perspectives on the development of cathode substances for KIBs.

Monodispersed Cu sites assembled on ultrathin 2D C3N4 for efficient electrocatalytic CO2 methanation

Electrocatalytic CO2 reduction (ECO2R) to methane is a promising technology that could effectively realize carbon resource integration and energy recycling. Currently, Cu-based catalysts are the most effective catalysts for this process, and a long-term goal of high selectivity and high stability still remains elusive. In this study, a controllable and multistep solid-state pyrolysis route is implemented to successfully introduce atomically dispersed Cu sites (Cu SA) into the two-dimensional carbon nitride (2D C3N4) matrices. The active site density and morphology structure of the Cu SA-2D C3N4 catalyst could be precisely controlled by adjusting the calcination process. Through the strategic combination of an ultrathin 2D structure and uniformly dispersed active sites, the Cu SA-2D C3N4 maximizes the exposure of active sites while suppressing competitive C–C coupling reactions. Ultimately, the optimized Cu SA-2D C3N4-30 exhibit a Faradaic efficiency of 62.9 % for CO2-to-CH4 conversion with a partial current density of 172.4 mA cm−2 at −1.68 V vs. RHE. This work demonstrates an advanced Cu-based electrocatalyst that effectively improves the performance of electrocatalytic CO2 methanation.

Structural phase transition from rhombohedral to monoclinic phase and physical properties of (1-x) Bi0.85La0.15FeO3 – (x) Ca0.5Sr0.5TiO3 ceramics prepared by the solid-state route

In the present work, a series of solid solutions were synthesized using the solid-state reaction method for x = 0.0, 0.05, 0.10, and 0.15 in system (1-x)Bi0.85La0.15FeO₃-(x)Ca0.5Sr0.5TiO3 or ((1-x)BLFO-(x)CSTO) ceramics. Structural, optical, dielectric, and ferroelectric properties were studied in detail to investigate the impact of CSTO doping in BFO. Rietveld analysis of X-ray diffraction data of all samples revealed the formation of a single-phase solid solution with a distorted rhombohedral perovskite structure for x = 0.00 and 0.05, characterized by R3c symmetry, a mix of rhombohedral (R3c) and monoclinic (Cc) phases for x = 0.10 (R3c 31 % and Cc 69 %), whereas for x = 0.15 a single-phase solid solution with Cc symmetry was found. UV–visible analysis demonstrated that the optical band gap was increased from 2.11 eV for x = 0.0 to 2.21 eV for x = 0.15 in the visible range, and can be used in photovoltaics applications. The room temperature dielectric properties were measured, and a crucial role of CSTO was revealed in modifying the dielectric properties of BLFO ceramics; the dielectric constant and dielectric loss at 10 kHz change from εr = 82 and tanδ = 0.88 for x = 0.0 to εr = 116 and tanδ = 1.08 for x = 0.15. The leakage current density decreases while increasing the CSTO % from x = 0.0 to 0.15 due to the suppression of oxygen and Bi vacancies, a fact that is further reflected in the ferroelectric properties of CSTO-doped BFO ceramics. Room temperature ferroelectric properties improved with CSTO doping, and Pr was found to be 0.24 μC/cm2, 0.28 μC/cm2, and 0.84 μC/cm2 for x = 0.05, 0.10, and 0.15, respectively.

A Honeycomb Layered Na2SnO3 as Novel Photocatalyst for Degradation of Rose Bengal Dye

AbstractA layered Na2SnO3 with honeycomb structure was synthesized by solid state route using sodium carbonate and tin oxide. The prepared sample was characterized by different physicochemical characterization techniques like X‐ray diffraction (XRD), field emission scanning electron microscopy (FESEM), energy dispersive X‐ray spectroscopy (EDS), X‐ray photoelectron spectroscopy (XPS), ultraviolet visible spectroscopy (UV–vis), photoluminescence spectra (PL), N2 adsorption technique (Brunauer–Emmett–Teller, electrochemical impedance spectroscopy (EIS). The photodegradation of rose bengal dye under UV light was studied. Due to honeycomb structure and high surface area of Na2SnO3, the complete degradation of rose Bengal was observed in 90 min under UV light irradiation. Results of photocatalytic dye degradation reaction demonstrated that Na2SnO3 can be employed as photocatalyst under UV light irradiation.

Preparation of spherical Gd2Zr2O7 powders by RF induction thermal plasma process

Spherical Gd2Zr2O7 (GZO) powders with a uniform particle size distribution are successfully prepared using a novel industrial approach, which combines spray-drying process and thermal plasma sintering technology together. In this, GZO powders with pyrochlore structure as the main phase are first synthesized via a solid-state reactive route using a mixture of the milled Gd2O3 powders and ZrO2 powders as starting materials. The influence of sintering temperature on the microstructure of prepared powders is researched. Then, GZO granules are prepared after wet-grinding and spray-drying process, which exhibit a spherical shape with the average particle size of 46.5 μm. RF induction thermal plasma is finally used to sinter the granulated particles, and the influence of feeding rate on the properties of spherical powders is investigated. The apparent density of plasma sintered GZO spherical powders is increased from 1.53 g/cm3 to 2.29 g/cm3 when the feeding rate of granulated powders is 80 g/min, and further increased up to 3.90 g/cm3 when the feeding rate is 15 g/min. Such powders are in potential demand for plasma sprayed coatings and additive manufacturing techniques, and the successful synthesis of spherical GZO powders may guide the way toward the preparation of many other spherical rare earth zirconates powders.

Na0.5Bi0.5TiO3 as an efficient catalyst for degradation of Dyes, Cr (VI) reduction and biomedical applications

In present study, we prepared Na0.5Bi0.5TiO3 (NBTO3) having perovskite structure via solid-state route. NBTO3 sample was characterized to examine the physico-chemical, optical and photoelectrochemical assets of samples using various analytical techniques. Photocatalytic activity of NBTO3 was investigated for methylene blue and rose Bengal dye degradation and toxic Cr (VI) reduction. Furthermore, NBTO3 was evaluated for antimicrobial and antioxidant activity. These findings highlight the versatile role of the prepared NBTO3 as an efficient catalyst for environmental remediation making it a promising material for various applications. The rate and mechanism related with photodegradation reaction were evaluated by kinetics and radical trap based quenching experiment. Moreover, the reusability study confirmed that even after four cycles, the material’s photocatalytic activity was still high.

Visible to infrared wide wavelength range luminescence of Sr2LaNbO6: Yb3+/Nd3+/Ho3+ phosphor under 808/980 nm excitation and temperature sensing application

Here, the Sr2LaNbO6: Yb3+/Nd3+/Ho3+ phosphors are prepared through solid-state route. The upconversion (UC)/downshifting (DS) luminescence and temperature performances of all samples are investigated in detail. Under 808 nm excitation, the infrared emission band (∼2000 nm) of Ho3+ ions is obtained. Especially, the energy transfer process of Nd3+ → Yb3+ → Ho3+ has increased the emission intensity of ∼2000 nm. Moreover, the infrared emission band presents thermal enhancement. Under 980 nm excitation, the UC emission band 500–960 nm is investigated. The green and red light of Ho3+ ion, near infrared light of Nd3+ ions are achieved. In addition, the possible luminescence mechanism of Sr2LaNbO6: Yb3+/Nd3+/Ho3+ phosphor is discussed. At last, the optical temperature sensing characteristics of the phosphor are studied according to the luminescence intensity ratio (LIR) technology. The maximum relative sensitivity of Sr2LaNbO6: Yb3+/Nd3+/Ho3+ reaches 5.476 % K−1 at 293 K. These results prove that the Sr2LaNbO6: Yb3+/Nd3+/Ho3+ phosphor presents the luminescence in infrared and visible range. The Sr2LaNbO6:Yb3+/Nd3+/Ho3+ phosphor also can be applied to design optical temperature sensor.

Novel proton-conducting hexagonal perovskites Ba7In6–xYxAl2O19 for solid oxide fuel cells

The solid solution Ba7In6–xYxAl2O19 (0≤x≤0.25) with a hexagonal perovskite-like structure was prepared by the solid-state route. The introduction of yttrium was accompanied by an increase in lattice parameters. The total conductivity as a function of pO2 and T was measured at different humidity. The partial conductivities were found by transport number measurements and were fitted based on the defect formation model. Oxygen-ion and proton conductivities were found to increase with Y3+ content as a result of an increase in cell volume and free volume, which was accompanied by a decrease in the activation energy of both oxygen-ion and proton conductivity. Oxygen-ion conductivity and proton conductivity dominated below 500 °C in dry (pH2O=3.5×10−5 atm) and in wet (pH2O=1.92×10−2 atm) conditions, respectively. Doping makes it possible to increase proton conductivity by an order of magnitude (500 °C) and significantly increase the proton transport numbers.The prepared phases exhibited excellent chemical stability during thermal treatment in carbon dioxide (pCO2=1 atm).

Potential improvement in thermoelectric properties of SnTe polycrystals via anionic and cationic substitution

Heat is produced by all machinery, including microprocessors and jet engines, as well as by industrial processes that produce goods from steel to food. There is still a strong desire for alternative energy sources in this day of ecologically conscious and sustainable energy needs. The recovery of heat from waste heat into beneficial electrical energy provides a simple energy source with enormous potential. Thermoelectrics is one of the popular technologies, which can convert heat into electricity, making them useful for power generation. Tin telluride (SnTe), a significant type of newly developed thermoelectric material, has drawn a lot of attention due to its low toxicity and environmentally friendly characteristics. Here, we synthesize Bi/Se co-doped SnTe (Sn1-xBixTe0.97Se0.03 (x = 0, 0.02, 0.04, 0.06)) samples by employing the solid-state metathesis route. The results of this work suggest that the combined action of cationic and anionic substitution of Bi and Se to SnTe matrix could potentially modify the microstructure and band structure of SnTe, thereby effectively improving its electronic, mechanical, and thermal transport properties. In line with the experimental findings, the samples show degenerate semiconducting electronic transport behaviour throughout the temperature range. The maximum Seebeck coefficient is found to be ∼84 μV/K and the total thermal conductivity is reduced to 1.6 W/mK at 573 K in a 6 % Bi-doped sample, which is 2.2 times less than the pristine sample. The Sn0.94Bi0.06Te0.97Se0.03 sample has a maximum ZT of approximately 0.23 at 573 K, which is three times higher than the pristine sample because of the combined regulation of cation-anion co-doping and an elevated power factor of 936 μW/K2m in Sn0.96Bi0.04Te0.97Se0.03 sample at 573 K, which is 1.82 times higher than that of pristine SnTe. Considering these findings, it appears that Bi-Se co-doped SnTe is a promising material for thermoelectric applications.

Structural, magnetic, optical and electronic properties of Gd2NiIrO6

Polycrystalline Gd2NiIrO6 double perovskite compound was synthesized by the solid-state route. Rietveld refinement of the X-ray diffraction pattern revealed that the compound was crystallized in a monoclinic structure with P21/n space group (IUCr. No. 14). The scanning electron micrograph showed that the grains were spherical and well distributed with an average grain size of around 1 μm. The temperature-dependent magnetic measurements showed magnetic transitions at 165 K and 149 K in the low-temperature region. Below the transition temperatures, weak ferromagnetism was evidenced by field-dependent magnetization measurements. Exchange bias effects were observed which were driven by Dzyaloshinsky–Moriya interactions in the compound. The UV–visible measurement evidenced that the compound had an optical band gap of 1.8 eV. The electronic structure calculations using the DFT + U method revealed that Gd2NiIrO6 compound exhibited a bandgap only when on-site correlations for the d-states were included, and the calculation showed that the AF1 configuration was energetically favourable.

Crystal Structure and Microwave Dielectric Characteristics of Novel Ba(Eu1/5Sm1/5Nd1/5Pr1/5La1/5)2Ti4O12 High-Entropy Ceramic

High-permittivity Ba(Eu1/5Sm1/5Nd1/5Pr1/5La1/5)2Ti4O12 (BESNPLT) high-entropy ceramics (HECs) were synthesized via a solid-state route. The microstructure, sintering behavior, phase structure, vibration modes, and microwave dielectric characteristics of the BESNPLT HECs were thoroughly investigated. The phase structure of the BESNPLT HECs was confirmed to be a single-phase orthorhombic tungsten-bronze-type structure of Pnma space group. Permittivity (εr) was primarily influenced by polarizability and relative density. The quality factor (Q×f) exhibited a significant correlation with packing fraction, whereas the temperature coefficient (TCF) of the BESNPLT HECs closely depended on the tolerance factor and bond valence of B-site. The BESNPLT HECs sintered at 1400 °C, demonstrating high relative density (>97%) and optimum microwave dielectric characteristics with TCF = +38.9 ppm/°C, Q×f = 8069 GHz (@6.1 GHz), and εr = 87.26. This study indicates that high-entropy strategy was an efficient route in modifying the dielectric characteristics of tungsten-bronze-type microwave ceramics.

Layered sodium manganese oxides for toxic nitrogen dioxide gas removal in ambient conditions

In this study, Na0.7MnO2 samples were successfully synthesized using a solid-state synthesis route with Na and Mn acetate precursors. The resulting Na0.7MnO2 crystallized in a hexagonal lattice with space group P63/mmc. These materials were investigated for their capacity to adsorb 100 ppm of NO2 gas at room temperature. Na0.7MnO2 exhibited an exceptional NO2 adsorption capacity of 163.3 mg/g, surpassing many previously reported porous and non-porous materials. Comprehensive experimental and spectroscopic analyses confirmed the formation of NO, NO2–, and NO3– species, following NO2 adsorption on the Na0.7MnO2 surface. Theoretical calculations further supported the chemisorption of NO2 gas molecules on the Na0.7MnO2 surface, with a maximum adsorption energy of –1.937 eV. Spectroscopic and Bader charge analyses confirmed that the NO2 gas molecule acted as a charge acceptor species on the oxide surface. This work represents the first detailed study validating Na0.7MnO2 as an effective room-temperature adsorbent for capturing and mineralizing NO2 gas. The exceptional NO2 adsorption capacity and the mechanistic insights into the adsorption process suggest the promising potential of Na0.7MnO2 and related oxides for applications in NO2 gas capture and conversion.

Thermodynamic properties of MnV2O6 and Mn2V2O7 at high temperatures

MnV2O6 and Mn2V2O7 are the key compounds during the manganese salt roasting for extracting vanadium from vanadium bearing slag. Thermodynamic properties of MnV2O6 and Mn2V2O7 are dispensable to get insight into the multi-phase reaction mechanism and clarify the phase evolution. In this study, the MnV2O6 and Mn2V2O7 compounds were synthesized through solid-state roasting routes under a nitrogen gas atmosphere, and their crystal structure and thermodynamic properties were determined using X-ray powder diffraction, differential scanning calorimetry, and drop calorimetry. The enthalpy increments of MnV2O6 and Mn2V2O7 were experimentally measured for temperatures ranging from 573 K to 1023 K and 573 K to 1173 K, respectively, using drop calorimetry for the first time. Based on the experimentally measured enthalpy increments, the temperature dependence of the molar heat capacity of MnV2O6 and Mn2V2O7 was then derived. Furthermore, thermodynamic properties such as enthalpy, entropy, and Gibbs free energy were also calculated. Finally, the Gibbs free energy of the chemical reactions during the roasting of vanadium slag was evaluated, and compared with other roasting techniques.

Oxygen vacancy modulated optical and dielectric properties of photoactive γ-Fe2WO6

Ferrite compounds have gained scientific attention for their multifunctional attributes. This investigation explores the structural, optical, dielectric and conductivity properties of polycrystalline γ-Fe2WO6 synthesized by the solid state route. The X-ray diffraction confirmed the orthorhombic structure and single-phase formation, while the electron microscopy showed uniform distribution of dense micrometer-sized grains in γ-Fe2WO6. The FTIR spectroscopy analysis validated the presence of active stretching and bending modes, signifying oxygen anion vibration at both Fe and W sites. The simultaneous presence of Fe2+ and Fe3+ ions in the matrix, as confirmed by X-ray photoelectron spectroscopy (XPS), results in an augmented optical energy band gap and contributes to dielectric permittivity due to the charge carrier hopping mechanism between the trap sites. The compound manifests semiconductor attributes, evident in its indirect optical band gap measuring 1.7 eV. It is observed that the compound has effectively degraded the Methylene Blue (MB) under the visible light within 40 min with a degradation efficiency up to 63 %. The material's electrical conductivity, follows the Jonscher's power law, signifies its semiconductor nature and adheres to the Small Polaron tunneling model for charge conduction between neighboring sites. The impedance (Z′) curves exhibit dielectric relaxation (≤ 10 kHz) with a similar activation energy to the dc conductivity study. The activation energy, determined from both the impedance and conductivity analyses, indicates a connection with the migration of oxygen vacancies within the material. Our observation reveals the presence of oxygen vacancies, which possibly act as in-gap electron traps, enhancing the correlated optical and ac conductivity properties, making it an appealing material for diverse multifunctional applications.

Exploring a New, Scalable Synthesis Route to Disordered Rock Salt (DRX) Cathode Materials

The global demand for lithium-ion batteries (LIBs) is ever-increasing as many nations seek to achieve a net carbon neutrality by the late 2030s. LiNi x Mn y Co1–x–y O2, (NMC) is one of the most widely-used Li-ion cathode active materials. Despite its excellent performance (e.g., reversible capacities up to ~220 mA h g–1 and 500+ cycles), NMC contains both Ni and Co, which are expensive and have vulnerable supply chains. Li-excess disordered rock salt (DRX) materials are promising new cathode materials that utilize earth-abundant transition metals such as Mn and Ti. Through a combination of cationic and anionic charge compensation, DRX materials can attain specific energies ≥700 Wh kg–1. Doping F– into the DRX structure (Li1+x Mn y Ti2–1–x–y O2–z F z ) has been reported to improve the material’s cycling stability. Despite their promising properties, most DRX cathodes are prepared through solid-state synthesis routes which require high-energy milling, provide little-to-no control over the particle morphology, and are difficult to scale.In this work, we developed a scalable combustion synthesis route (the glycine nitrate process) to produce high purity, high performance DRX cathodes. More specifically, we prepared two DRX precursors with nominal compositions of Li1.2Mn0.5Ti0.3O1.95 and Li1.2Mn0.7Ti0.1O1.85. When the precursors were heated under Ar to 1000 °C for 1 – 4 h, only 50% Li1.2Mn0.5Ti0.3O1.95 adopted a DRX structure, and no DRX formed for Li1.2Mn0.7Ti0.1O1.85. However, adding LiF to the precursors facilitates DRX phase formation during annealing and yields high purity DRX powders with the nominal compositions Li1.25Mn0.5Ti0.3O1.95F0.05 and Li1.35Mn0.7Ti0.1O1.85F0.15. In situ X-ray diffraction was employed to study the synthesis process, revealing DRX begins to form at just 600 °C, which is much lower than traditional solid-state routes. Furthermore, electrochemical tests on the Li1.35Mn0.7Ti0.1O1.85F0.15 cathode reveal these materials attain excellent performance with initial reversible capacities up to 215 mA h g–1 and stable cycling performance. These promising results demonstrate that combustion synthesis is a viable method for the scale-up of DRX materials.This research was conducted at Oak Ridge National Laboratory, managed by UT Battelle, LLC, for the U.S. Department of Energy (DOE) and was sponsored by the Vehicle Technologies Office (VTO) under the Office of Energy Efficiency and Renewable Energy (EERE). Some measurements were conducted at the Center for Nanophase Materials Sciences (CNMS), which is a DOE Office of Science User Facility.