As-prepared Products Research Articles

Nanocasting synthesis of mesoporous CeO2 particle abrasives from mesoporous SiO2 hard templates for enhanced chemical mechanical polishing performance

Mesoporous abrasive particles exhibit superior chemical mechanical polishing/planarization (CMP) performance, as compared with the corresponding bulk materials. Nevertheless, the lack of control over the shape and particle size or distribution extremely restricts the development of mesoporous abrasives and their potential applications. To overwhelm these drawbacks, pure and ytterbium-doped mesoporous ceria (mCeO2 and mCeYbO2) spheres with well-defined morphology and good uniformity were synthesized via a straightforward nanocasting strategy using high-quality mesoporous silica spheres as hard templates and metal nitrates as precursors. The resulting samples were characterized by X-ray diffraction, scanning electron microscopy, transmission electron microscopy, selected area electron diffraction, X-ray photoelectron spectroscopy, Raman spectroscopy, UV–vis diffuse reflectance spectroscopy, photoluminescence spectroscopy, Zeta potential, and N2 adsorption-desorption measurements. The as-prepared mCeO2 and mCeYbO2 products exhibited enriched surface defects (trivalent Ce, vacancy oxygen, hydroxyls) and polycrystalline porous frameworks with a surface area of up to 160 m2/g and pore size of 4–7 nm. Benefiting from these synergistic attributes, the flexible and defective particle abrasives enabled significant improvements in both surface quality and removal efficiency during oxide-CMP, as compared to commercial CeO2. A possible CMP mechanism was proposed on the basis of the physical contact state, adsorption and adhesion behavior, as well as tribochemical interaction occurred at CeO2–SiO2 interfaces. This work demonstrates highly promising abrasive materials advancement combining architecture and defect engineering towards high-performance oxide-CMP.

Preparation and Properties of Elastic Mullite Fibrous Porous Materials with Excellent High-Temperature Resistance and Thermal Stability.

Mullite fiber felt is a promising material that may fulfill the demands of advanced flexible external thermal insulation blankets. However, research on the fabrication and performance of mullite fiber felt with high-temperature resistance and thermal stability is still lacking. In this work, mullite fibers were selected as raw materials for the fabrication of mullite fibrous porous materials with a three-dimensional net structure. Said materials' high-temperature resistance and thermal stability were investigated by assessing the effects of various heat treatment temperatures (1100 °C, 1300 °C, and 1500 °C) on the phase composition, microstructure, and performance of their products. When the heat treatment temperature was below 1300 °C, both the phase compositions and microstructures of products exhibited stability. The compressive rebound rate of the product before and after 1100 °C reached 92.9% and 84.5%, respectively. The backside temperature of the as-prepared products was 361.6 °C when tested at 1500 °C for 4000 s. The as-prepared mullite fibrous porous materials demonstrated excellent high-temperature resistance, thermal stability, thermal insulation performance, and compressive rebound capacity, thereby indicating the great potential of the as-prepared mullite fibrous porous materials in the form of mullite fiber felt within advanced flexible external thermal insulation blankets.

Modular Assembly of Pyrrolo[3,4-c]isoquinolines through Rh-Catalyzed Cascade C-H Activation/Annulation of O-Methyl Aryloximes with Maleimides.

An efficient and practical strategy for the construction of pyrrolo[3,4-c]isoquinolines via Rh(III)-catalyzed cascade C-H activation and subsequential annulation process from easily available O-methyl aryloximes and maleimides has been disclosed. This facile protocol does not require any inert atmosphere protection with good efficiency in a low loading of catalyst and exhibits good functional group tolerance and broad substrate scope. Notably, the as-prepared products show potential photophysical properties.

Solid-state synthesis and ion transport characteristics of the β-KSbF4 for all-solid-state fluoride-ion batteries

All-solid-state fluoride ion batteries (FIBs) have been recently considered as a post-lithium-ion battery system due to their high safety and high energy density. Just like all solid-state lithium batteries, the key to the development of FIBs lies in room-temperature electrolytes with high ionic conductivity. β-KSbF4 is a kind of promising solid-state electrolyte for FIBs owing to its rational ionic conductivity and relatively wide electrochemical stability window at room temperature. However, the previous synthesis routes of β-KSbF4 required the use of highly toxic hydrofluoric acid and the ionic conductivity of as-prepared product needs to be further improved. Herein, the β-KSbF4 sample with an ionic conductivity of 1.04 × 10−4 S cm−1 (30 °C) is synthesized through the simple solid-state route. In order to account for the high ionic conductivity of the as-synthesized β-KSbF4, X-ray diffraction (XRD), scanning electron microscopy (SEM), and energy dispersive X-ray spectroscopy (EDS) are used to characterize the physicochemical properties. The results show that the as-synthesized β-KSbF4 exhibits higher carrier concentration of 1.0 × 10−6 S cm−1 Hz−1 K and hopping frequency of 1.31 × 106 Hz at 30 °C due to the formation of the fluorine vacancies. Meanwhile, the hopping frequency shows the same trend as the changes of ionic conductivity with the changes of temperature, while the carrier concentration is found to be almost constant. The two different trends indicate the hopping frequency is mainly responsible for the ionic conduction behavior within β-KSbF4. Furthermore, the all-solid-state FIBs, in which Ag and Pb + PbF2 are adopted as cathode and anode, and β-KSbF4 as fluoride ion conductor, are capable of reversible charge and discharge. The assembled FIBs show a discharge capacity of 108.4 mA h g−1 at 1st cycle and 74.2 mA h g−1 at 50th cycle. Based on an examination of the capacity decay mechanism, it has been found that deterioration of the electrolyte/electrode interface is an important reason for hindering the commercial application of FIBs. Hence, the in-depth comprehension of the ion transport characteristics in β-KSbF4 and the interpretation of the capacity fading mechanism will be conducive to promoting development of high-performance FIBs.

Effect of different salt precursors on zinc ferrite synthesis and their photo-Fenton activity

Polycrystalline and mesocrystalline zinc ferrite were successfully fabricated via a solvo-thermal method using different salt precursors. This study found that when iron sulfate salt was used as a precursor, polycrystalline zinc ferrite was formed. Polycrystalline zinc ferrite is a well-dispersed 400-nm sphere solid particle. Primary nano-crystals have highly preferred orientations; however, defects exist among the particles. When iron chloride salt was used as a substitute as a prime material, mesocrystalline zinc ferrite was synthesised. The products are shaped as hollow-spheres with an average size of approximately 500 nm and are composed of nano-crystal sub-units aligned in a highly oriented crystallographic structure. Zinc ferrite mesocrystalline samples have many voids, and the inter-spaces of their structure indicate the high porosity hollow-sphere architecture of zinc ferrite. The experimental results show that specific adsorption of Cl− and SO42− ions on the surface plays a crucial role during the growth process of products with different morphologies and crystallographic structures. Cl− adsorption on the surface may promote the formation of mesocrystal hollow-sphere particles; whereas, SO42− gives rise to polycrystalline solid spheres. The use of the as-prepared products as catalysts for the photo-Fenton degradation of Rhodamine B (RhB) with an H2O2 oxidant under visible-light irradiation and the effects of reaction conditions, including pH, catalyst amount and H2O2 contratentation on the removal of RhB, were investigated. The reuse of the catalysts and a possible catalytic mechanism were also proposed. These results indicate that mesocrystalline hollow-sphere zinc ferrite is a favourable catalyst for dye degradation photo-Fenton processes.

Sulfidated nanoscale zero-valent iron derived from iron sludge for tetracycline removal: Role of sulfur and iron in reactivity and mechanisms

Iron sludge, produced during the drinking water treatment process, can be recycled as potential iron resource to create environmental functional material. In this study, sulfur-iron composites derived from iron sludge (S–Fe composites) was synthesized through sulfidation and carbonization, and used for the tetracycline (TC) removal under aerobic and anoxic conditions. The reactivities of these as-prepared products were strongly depended on pyrolysis temperatures. In particular, sulfidated nanoscale zero-valent iron loaded on carbon (S-nFe0@CIS) carbonized at 800 °C exhibited the highest TC removal efficiency with 86.6% within 30 min at circumneutral pH compared with other S–Fe composites. The crystalline structure of α-Fe0, FeSx and S0 as main active sites in S-nFe0@CIS promoted the degradation of TC. Moreover, the Fe/S molar ratios significantly affected the TC removal rates, which reached the best value as the optimal S/Fe of 0.27. The results illustrated that the optimized extent of sulfidation could facilitate electron transfer from nFe0 towards contaminants and accelerate Fe(III)/Fe(II) cycle in reaction system compared to bared nFe0@CIS. We revealed that removal of TC by S-nFe0@CIS in the presence of dissolved oxygen (DO) is mainly attributed to oxidation, adsorption and reduction pathways. Their contribution to TC removal were 31.6%, 25.2% and 28.8%, respectively. Furthermore, this adsorption-oxygenation with the formation of S-nFe0@CIS-TC* complexes was a surface-mediated process, in which DO was transformed by the structural FeSx on complex surface to •OH with the generation of H2O2 intermediate. The intermediates of TC and toxicity analysis indicate that less toxicity products generated through degradation process. This study provides a new reclamation of iron sludge and offers a new insight into the TC removal by S-nFe0@CIS under aerobic conditions.

Synthesis of polysubstituted pyridazines via Cu-mediated C(sp3)-C(sp3) coupling/annulation of saturated ketones with acylhydrazones.

Pyridazine is a significant skeleton that widely exists in drugs and bioactive molecules. We herein describe expeditious approaches to access polysubstituted pyridazines from readily accessible unactivated ketones and acylhydrazones via Cu-promoted C(sp3)-C(sp3) coupling/cyclization sequences in a single-step fashion. Notably, the disparate 3,4,6-trisubstituted pyridazines and 3,5-disubstituted pyridazines could be obtained by tailoring the ketone's structure and reaction conditions. These transformations feature good functional group compatibility, excellent step-economy, and chemoselectivity. The potential synthetic utility of these conversions is illustrated by scale-up reactions and late-stage derivatizations of the as-prepared pyridazine products.

Structural regulation of asphalt-based hard carbon microcrystals based on liquid-phase crosslinking to enhance sodium storage

Air-oxidation is an effective strategy to obtain promising carbon materials from asphalt for sodium-ion batteries. However, this method would generate a vast amount of gaseous pollutant, which pose challenges for recycling. Herein, a simple, cost-effective and environmentally friendly liquid-phase oxidation method is proposed. The oxygen-containing functional groups (-NO2) are introduced into asphalt, which effectively prevents the melting of asphalt and rearrangement of carbon layers during subsequent carbonization process. As a result, a carbon material with notable disorder degree, large interlayer spacing and abundant closed pores, is prepared. The as-prepared product demonstrates an impressive initial Coulombic efficiency of 88.3 % and an enhanced specific capacity of 317.0 mA h g−1, which is 2.6 times that of the pristine product. Moreover, when assembled with a Na3.32Fe2.34(P2O7)2 cathode, the full-cell delivers a high reversible capacity of 271.7 mA h g−1 at 30 mA g−1 with superb cycle life. This study offers a novel oxidation strategy and provides a solution for producing highly disordered carbon anodes from soft carbon precursors.

Structural characterization, luminescence properties and applications of Eu3+ ion-doped bismuth molybdate phosphor via a molten salt-assisted approach

A molten salt-assisted method for the synthesis of Eu[Formula: see text]-doped bismuth molybdate (BMO: Eu[Formula: see text]) phosphor was proposed. (BMO: Eu[Formula: see text]) phosphors with different phase structures were obtained by changing the calcination temperature. The applications in LED devices and latent fingerprint recognition of the obtained product were explored. The results of structural characterizations and scanning electron microscope (SEM) photographs analysis prove that the products exhibit different crystal structures and morphologies with the change of calcination temperature. Based on the above findings, the as-prepared products have potential applications in the field of WLED and potential fingerprint recognition.

Sulfur-Doped NiFe Hydroxide Nanobowls with Wrinkling Patterns for Photothermal Cancer Therapy.

Hierarchical multiscale wrinkling nanostructures have shown great promise for many biomedical applications, such as cancer diagnosis and therapy. However, synthesizing these materials with precise control remains challenging. Here, we report a sulfur doping strategy to synthesize sub-1 nm NiFe hydroxide ultrathin nanosheets (S-NiFe HUNs). The introduction of sulfur affects the reduction of the band gap and the adjustment of the electronic structure, thereby improving the light absorption ability of the S-NiFe HUNs. Additionally, S-NiFe HUNs show a multilayered nanobowl-like structure that enables multiple reflections of incident light inside the nanostructure, which improved the utilization of incident light and achieved high photothermal conversion. As a result, the as-prepared product with hydrophilic modification (dS-NiFe HUNs) demonstrated enhanced tumor-killing ability in vitro. In a mouse model of breast cancer, dS-NiFe HUNs combined with near-infrared light irradiation greatly inhibited tumor growth and prolonged the mice survival. Altogether, our study demonstrates the great potential of dS-NiFe HUNs for cancer photothermal therapy applications.

Low-cost fabrication and physicochemical characterization of ZnFe2O4 nanoparticles as an efficient multifunctional inorganic pigment

The pursuit of low-cost manufacturing of newly effective pigments is a pressing economic need. Thus, in this work, low-cost ZnFe2O4 spinel nanoparticles (ZF-NPs) with an average diameter of 20 nm were successfully synthesized using a simple sol–gel method, which can be extended for large-scale fabrication of a reddish nano pigment. TGA/DTA, XRD, DRS, HRTEM, and SEM/EDX investigations were used to characterize the as-prepared product. The color of synthesized NPs was studied using CIE L*a*b* colorimetric method with color coordinates of L* = 41.7, a* = 72.2, and b* = 48.8. The newly developed pigment was examined to be superior to the traditional pigment (M6001/Fe2O3: L* = 30.4, a* = 42.16, and b* = 45.7). After that, the synthesized nano pigment was integrated into both ink and paint formulations as a multifunctional coating. The inclusion of synthesized nano pigment in metal coating printing ink formulation was done to produce a good alternative and cost-effective substitute for the commercially available pigment used in the inks industry. Also, the effect of the fabricated nanoparticles on corrosion resistance and thermal stability of epoxy-based paint formulations was evaluated using different standard tests. Therefore, the ZnFe2O4 pigment should be applied as a highly efficient inorganic nano pigment.

Propylene Metathesis over Molybdenum Silicate Microspheres with Dispersed Active Sites.

In this work, we demonstrate that amorphous and porous molybdenum silicate microspheres are highly active catalysts for heterogeneous propylene metathesis. Homogeneous molybdenum silicate microspheres and aluminum-doped molybdenum silicate microspheres were synthesized via a nonaqueous condensation of a hybrid molybdenum biphenyldicarboxylate-based precursor solution with (3-aminopropyl)triethoxysilane. The as-prepared hybrid metallosilicate products were calcined at 500 °C to obtain amorphous and porous molybdenum silicate and aluminum-doped molybdenum silicate microspheres with highly dispersed molybdate species inserted into the silicate matrix. These catalysts contain mainly highly dispersed MoOx species, which possess high catalytic activity in heterogeneous propylene metathesis to ethylene and butene. Compared to conventional silica-supported MoOx catalysts prepared via incipient wetness impregnation (MoIWI), the microspheres with low Mo content (1.5-3.6 wt %) exhibited nearly 2 orders of magnitude higher steady-state propylene metathesis rates at 200 °C, approaching site time yields of 0.11 s-1.

Perovskite-Derived Bismuth with I- and Cs+ Dual Modification for High-Efficiency CO2 -to-Formate Electrosynthesis and Al-CO2 Batteries.

Bi-based materials are one of the most promising candidates for electrochemical CO2 reduction reaction (CO2 RR) to formate; however, the majority of them still suffer from low current density and stability that essentially constrain their potential applications at the industrial scale. Surface modification represents an effective approach to modulate the electrode microenvironment and the relative binding strength of key intermediates. Herein, it isdemonstrated that the surface comodification with halides and alkali metal ions from the conversion of Bi-based halide perovskite nanocrystals is a viable strategy to boost the CO2 RR performance of Bi for formate electrosynthesis. Cs3 Bi2 I9 nanocrystals are prepared by a hot-injection method. The as-prepared products feature well-defined hexagonal shape and uniform size distribution. When used as the precatalyst, Cs3 Bi2 I9 nanocrystals are converted to Cs+ and I- comodified Bi. The resultant catalyst exhibits high formate Faradaic efficiency close to 100%, and remarkable partial current density up to 44mA cm-2 in an H-cell and up to 276 mA cm-2 in a flow cell. Moreover, Cs3 Bi2 I9 is used as the cathode catalyst and paired with an Al anode in an Al-CO2 battery for simultaneous CO2 valorization and power generation.

A Symmetry Concept for the Self-Assembly Synthesis of Mn-MIL-100 Using a Capping Agent and Its Adsorption Performance with Methylene Blue

In this study, a facile strategy of regulated self-assembly synthesis of Mn-MIL-100, using sodium acetate (CH3COONa) as a mono-dentate ligand capping agent (CA), was proposed. The as-prepared product is denoted Mn-MIL-100-CA. The coordination modulation of CH3COONa, led by its interference in the connectivity and symmetry of the metal centers and organic nodes, plays a vital role in the synthesis process. The crystallinity, morphology, topology, and properties of such MOF products were improved, since the self-assembly process of Mn-MIL-100-CA was promoted and regulated effectively. The materials were systematically characterized via XRD, SEM, N2 isotherms, XPS, and TGA in terms of crystallization behavior, morphology, topology, chemical composition, and thermal and water stability. The ability of Mn-MIL-100 and Mn-MIL-100-CA to remove methylene blue (MB) from an aqueous solution was investigated using a UV–vis spectrophotometer. The results indicate that with the addition of a molar ratio of 50% CH3COONa, Mn-MIL-100-CA particles developed a regularly symmetrical morphology, i.e., ‘spherical pyramid-like structure’ crystals with a dimension of 2~5 μm. Their specific surface area and pore volume increased by 59.2% and 56.7%, respectively. The increased proportion of Mn3+ implies reduced crystal defects and improved crystal structural order and integrity, and therefore an enhanced water stability. Mn-MIL-100-CA exhibited excellent adsorption performance towards MB from aqueous solution. The equilibrium adsorption value was as high as 1079.9 mg/g, which is 44.7% higher than that of Mn-MIL-100 without the addition of CA. The good adsorption capacity and excellent water stability mean that Mn-MIL-100-CA has great potential for the practical removal of MB dye pollutants from water.

Synthesis of alloyed PtPd nanowires and study on their electro-catalytic performance to methanol oxidation reaction

Alloying Pt with foreign metal to modulate the electronic structure and controlling the geometric morphology of Pt nanomaterials to tailor the surface structure are two extensively applied strategies to promote the electrocatalytic activity of Pt nanomaterials in fuel cell reactions. The former enhances the intrinsic catalytic activity of the nano-catalysts while the latter increases the number of active sites for catalytic reactions. So why not combine the two strategies to construct highly efficient Pt-based nano-catalysts? Within this work, we successfully synthesized one-dimensional PtPd nanowires through a one-pot method by exploiting the similarities of Pt and Pd, like identical lattice constants. The as-prepared products had alloyed structures and ultrafine profiles of nanowires. The electrochemical test indicated that the PtPd nanowires as-prepared possessed superior catalytic activity to methanol oxidation reaction with the mass activity of 2071 mAmg−1, significantly better than that of the commercial Pt/C (473 mAmg−1). Density functional theory calculation showed that with the introduction of Pd, the d-band electron center of Pt would downshift and the adsorbed interaction between CO intermediates (CO∗) with the surface of catalysts would diminish, which would improve the resistance of the catalysts to the toxicity of CO∗, thus enhancing the electro-catalytic activity and stability. Apart from the alloying effect, the unique structure of the one-dimensional ultra-fine nanowires could guarantee adequate atoms would be involved to expose and provide sufficient active sites for reactions, which was another essential factor in the promotion of the electro-catalytic performance.

Controllable synthesis of blue-emitting CsPbBr3 nanoplates via a SnBr2-mediated solvothermal reaction method

Blue-emitting CsPbX3 (X = Cl, Br, I) nanocrystals (NCs) have potential applications in white light illumination and full-color luminescent displays. However, current methods for synthesizing blue-emitting CsPbX3 NCs face challenges in poor controllability, low photoluminescence quantum yields (PLQYs), and the harmful effects of short-wavelength blue light. In this work, we report on a SnBr2-mediated solvothermal method for the controllable synthesis of blue-emitting CsPbBr3 nanoplates (NPLs) that exhibit high optical purity within the harmless blue light range. The pioneering use of SnBr2 as a mediator in solvothermal reactions plays a crucial role in the controllable synthesis process. By increasing the amount of SnBr2, the as-prepared products gradually transform from CsPbBr3 NCs to mixed CsPbBr3/Cs4PbBr6 NCs, and finally to CsPbBr3 NPLs. By further adjusting the solvothermal reaction conditions, CsPbBr3 NPLs with controlled thickness (2.34–3.53 nm), regulated blue-light emission (459.4–466.6 nm) and a high PLQY up to 63.17% can be obtained. This study provides a feasible method for the controllable synthesis of perovskite NPLs and opens up new possibilities for the application of perovskite blue light-emitting devices.

A hydrogel-assisting surface-confined corrosion strategy toward self-supported amorphous NiFe-layered double hydroxides enabling high-performance hybrid solid-state supercapacitors

Layered double hydroxides (LDHs) are promising energy materials for supercapacitors. It is demonstrated that the integrated performance of the amorphous LDHs is superior to that of crystalline materials. However, it is still a great obstacle to producing amorphous LDHs. Herein, a simple and facile strategy is proposed to synthesize the self-supported amorphous NiFe-LDHs using a surface-confined method. The corrosion process takes place in a cost-effective hydrogel at ambient temperature and pressure, which can synchronously change the chemical structure and morphology of the NiFe-LDHs. This method is also proved to be effective in fabricating S-doped amorphous NiFe-LDHs. The as-prepared products show excellent electrochemical performance in the charge-discharge process with fast kinetics, low impedance, good stability, and significant capacity, which is superior to most reported crystalline electrode materials. Moreover, the assembled hybrid solid-state supercapacitor devices display excellent capacitive performance including high energy density, superb rate capability and outstanding long-term cycling stability. This work offers a new sight into economically synthesizing amorphous mixed-metal compositions for high-performance supercapacitors.

Robust and functional polyamide 11 tubular product featuring helical flow-regulated interpenetrating configuration of carbon nanofiber

Miniaturized functional tubular product (MFTP) as a pivotal block of the potable smart devices has been widely applied in advanced industries, however, conventionally-extruded tube often suffers from easy detachment of head-to-end contracting points and weak mechanical reliability along normal direction. Herein, we proposed a facile strategy to prepare polyamide 11 tubular product with a helically-interpenetrating network by manipulating reversed helical flow in rotation extrusion. Compared to the axially-align configuration in conventionally-extruded tube featuring unidirectional reinforcement and easy-disconnecting head-to-end configuration, the helically-interpenetrating CNF network shared similar characteristic to the tracheid-like helical structure existing in wood, providing the composite tube with robust mechanical properties in all directions, but also boosting the initial conductivity and electrical stability under mechanical deformation. With the benefits of outstanding capabilities of robust performance and excellent conductive property, the as-prepared tubular product can be endowed with some special functions including excellent antistatic and electrothermal properties, guaranteeing the safe application in low temperature, vibration environment as a hydraulic brake tube. The helically flow-driven melt-processing was featured with low cost, high efficiency and suitable for continuous industrial fabrication, opening up a facile and effective strategy to prepare excellent MFTP with the hollow and thin wall.

One stone three birds: Chestnut-like CoZn-LDH via one-step facile route for both energy conversion and storage

Herein, we prepared three-function chestnut-like CoZn-LDH by a facile one-step solvothermal method with excellent performance for energy conversion and storage. Specifically, the as-prepared products yielded outstanding water splitting performance (η10 = 160 mV for hydrogen evolution reaction and η50 = 330 mV for oxygen evolution reaction) and high areal specific capacitance (2.24 F cm−2 at 10 mA cm−2). In addition, according to the electrochemical measurements, the viewpoint for explaining the coexistence of three functions (oxygen evolution reaction, hydrogen evolution reaction and capacitive performance) in chestnut-like CoZn-LDH was proposed for the first time. Last but not least, this work definitely shed light on the construction of multifunctional material.

Octahedron-Shaped Nano FeCo2O4 Phase Materials: Wet Chemical Synthesis and Characterization Studies

Background: Amongst the different spinel cobaltites investigated to date, the FeCo2O4 phase has been relatively less studied in detail despite the potential applications in several areas. As the nanostructured spinels are sensitive to the processing conditions, we have extended our research interest in FeCo2O4 phase materials. Objective: The objective of this study is (i) to synthesize the FeCo2O4 nanomaterials by different approaches using different precursors and (ii) to investigate the structural, thermal, optical, and microstructural properties of different materials by various characterization techniques. Methods: Different approaches such as hexamine-assisted combustion synthesis, co-precipitation, and solvothermal methods were employed to obtain FeCo2O4 nanomaterials using different precursors. Results: The XRD pattern of the as-prepared product of the solvothermal method is significantly different from other processed as-prepared products. The annealed FeCo2O4 materials obtained by coprecipitation using nitrates and/or chlorides showed nearly a single phase of FeCo2O4 nanomaterials. Conclusion: The phase formation of FeCo2O4 materials is sensitive to the presently employed synthesis conditions. The XRD patterns confirmed the deficient crystalline nature of the as-prepared materials produced by sol-gel combustion and co-precipitation methods. The annealed materials obtained by the co-precipitation using nitrates and chlorides showed nearly a single FeCo2O4 phase. The observed particle sizes of the FeCo2O4 phase materials are octahedral shaped with different sizes of 89 to 344 nm. The optical property studied using the FT-IR technique shows IR bands at 500 ~ 630 cm-1.