3D Carbon Microspheres with a Maze-Like Structure and Large Mesopore Tunnels Built From Rapid Aerosol-Confined Coherent Salt/Surfactant Templating.

Hierarchically porous carbons with tailor-made properties are essential for applications wherein rich active sites and fast mass transfer are required. Herein, a rapid aerosol-confined salt/surfactant templating approach is proposed for synthesizing hierarchically porous carbon microspheres (HPCMs) with a maze-like structure and large mesopore tunnels for high-performance tri-phase catalytic ozonation. The confined assembly in drying microdroplets is crucial for coherent salt (NaCl) and surfactant (F127) dual templating without macroscopic phase separation. The HPCMs possess tunable sizes, a maze-like structure with highly open macropores (0.3-30 µm) templated from NaCl crystal arrays, large intrawall mesopore tunnels (10-45 nm) templated from F127, and rich micropores (surface area >1000 m2 g-1 ) and oxygen heteroatoms originated from NaCl-confined carbonization of phenolic resin. The structure formation mechanism of the HPCMs and several influencing factors on properties are elaborated. The HPCMs exhibit superior performance in gas-liquid-solid tri-phase catalytic ozonation for oxalate degradation, owing to their hierarchical pore structure for fast mass transfer and rich defects and oxygen-containing groups (especially carbonyl) for efficient O3 activation. The reactive oxygen species responsible for oxalate degradation and the influences of several structure parameters on performance are discussed. This work may provide a platform for producing hierarchically porous materials for various applications.

Hierarchically Porous Carbon Rods Derived from Metal-Organic Frameworks for Aqueous Zinc-Ion Hybrid Capacitors.

Aqueous zinc-ion hybrid capacitors (ZIHCs), as ideal candidates for high energy-power supply systems, are restricted by unsatisfied energy density and poor cycling durability for further applications. The construction of a surface-functionalized carbon cathode is an effective strategy for improving the performance of ZIHCs. Herein, a high-performance ZIHC is achieved using oxygen-rich hierarchically porous carbon rods (MDPC-X) prepared by the pyrolysis of a metal-organic framework (MOF) assisted by KOH activation. The MDPC-X samples displayed high electric double-layer capacitance (EDLC) and pseudocapacitance owing to their oxygen-rich surfaces, abundant electroactive sites, and short ions/electron transfer lengths. The surface oxygen functional groups for the reversible chemical adsorption/desorption of Zn2+ are identified using ex situ X-ray photoelectron spectroscopy (XPS) and scanning electron microscopy (SEM). Consequently, the as-assembled ZIHC exhibited a high capacity of 323.4 F g-1 (161.7 mA h g-1) at 0.5 A g-1 and a retention of 147 F g-1 (73.5 mA h g-1) at an ultrahigh current density of 50 A g-1, corresponding to high energy and power densities of 145.5 W h kg-1 and 45 kW kg-1, respectively. Furthermore, an excellent cycling life with 96.5% of capacity retention is also maintained after 10 000 cycles at 10 A g-1, demonstrating its promising potential for applications.

Lab-on-Device Synthesis of Hierarchical Macro/Mesoporous WO3 Semiconducting Films for High-Performance H2S Sensing.

The performance consistency of the gas sensor is strongly dependent on the interface binding between the sensitive materials and the electrodes. Traditional powder coating methods can inevitably lead to differences in terms of substrate-film interface interaction and device performance, affecting the stability and lifetime. Thus, efficient growth of sensitive materials on device substrates is crucial and essential to enhance the sensing performance, especially for stability. Herein, hierarchically ordered macro/mesoporous WO3 films are in situ synthesized on the electrode via a facile soft/hard dual-template strategy. Orderly arrayed uniform polystyrene (PS) microspheres with tailored size (ca. 1.2 µm) are used as a hard template, and surfactant Pluronic F127 as a soft template can co-assemble with tungsten precursor into ordered mesostructure in the interstitials of PS colloidal crystal induced by solvent evaporation. Benefiting from its rich porosity and high stability, the macro/mesoporous WO3-based sensor shows high sensitivity (Rair/Rgas = 307), fast response/recovery speed (5/9 s), and excellent selectivity (SH2S/Smax > 7) toward 50 ppm H2S gas (a biomarker for halitosis). Significantly, the sensors exhibit an extended service life with a negligible change in sensing performance within 60 days. This lab-on-device synthesis provides a platform method for constructing stable nanodevices with good consistency and high stability, which are highly desired for developing high-performance sensors.

Hierarchically Micro- and Mesoporous Zeolitic Imidazolate Frameworks Through Selective Ligand Removal.

A new method to engineer hierarchically porous zeolitic imidazolate frameworks (ZIFs) through selective ligand removal (SeLiRe) is presented. This innovative approach involves crafting mixed-ligand ZIFs (ML-ZIFs) with varying proportions of 2-aminobenzimidazole (NH2-bIm) and 2-methylimidazole (2-mIm), followed by controlled thermal treatments. This process creates a dual-pore system, incorporating both micropores and additional mesopores, suggesting selective cleavage of metal-ligand coordination bonds. Achieving this delicate balance requires adjustment of heating conditions for each mixed-ligand ratio, enabling the targeted removal of NH2-bIm from a variety of ML-ZIFs while preserving their inherent microporous framework. Furthermore, the distribution of the initial thermolabile ligand plays a pivotal role in determining the resulting mesopore architecture. The efficacy of this methodology is aptly demonstrated through the assessment of hierarchically porous ZIFs for their potential in adsorbing diverse organic dyes in aqueous environments. Particularly striking is the performance of the 10%NH2-ZIF-2 h, which showcases an astonishing 40-fold increase in methylene blue adsorption capacity compared to ZIF-8, attributed to larger pore volumes that accelerate the diffusion of dye molecules to adsorption sites. This versatile technique opens new avenues for designing micro/mesoporous ZIFs, particularly suited for liquid media scenarios necessitating efficient active site access and optimal diffusion kinetics, such as purification, catalysis, and sensing.

Hierarchical Magnetic Carbon Nanoflowers for Ultra-Efficient Electromagnetic Wave Absorption.

Porous carbon nanomaterials are widely applied in the electromagnetic wave absorption (EMWA) field. Among them, an emerging flower-like carbon nanomaterial, termed carbon nanoflowers (CNFs), has attracted tremendous research attention due to their unique hierarchical flower-like structure. However, the design of flower-like carbon nanomaterials with different magnetic cores for EMWA has rarely been reported. Herein, a general template method is proposed to achieve a set of high-quality magnetic CNFs, namely Co@Void@CNFs, CoNi@CNFs, and Ni@CNFs. The prepared magnetic CNFs have highly accessible surface area and internal space, rich heteroatom content, multi-scale pore system, and uniform and highly dispersed magnetic nanoparticles, as a result, deliver superior EMWA performance. Specifically, when the thickness is 2.6 mm, the Co@Void@CNFs exhibit a maximum refection loss (RLmax) of -56.6 dB and an effective absorption bandwidth (EAB) from 8.0 to 12.1 GHz covering the whole X band. The CoNi@CNFs have an RLmax of up to -57.6 dB and a wide EAB of 5.6 GHz at just 1.9 mm. For the Ni@CNFs, possess an ultra-broad EAB of 6.1 GHz, covering the entire Ku band at 2.0 mm. Overall, the hierarchical magnetic carbon nanoflowers proposed here offer new insights toward realizing multifunctional integrated carbon nanomaterials for EMWA.

Wood-Structured Nanomaterials as Highly Efficient, Self-Standing Electrocatalysts for Water Splitting.

Electrocatalytic water splitting (EWS) driven by renewable energy is widely considered an environmentally friendly and sustainable approach for generating hydrogen (H2), an ideal energy carrier for the future. However, the efficiency and economic viability of large-scale water electrolysis depend on electrocatalysts that can efficiently accelerate the electrochemical reactions taking place at the two electrodes. Wood-derived nanomaterials are well-suited for serving as EWS catalysts because of their hierarchically porous structure with high surface area and low tortuosity, compositional tunability, cost-effectiveness, and self-standing integral electrode configuration. Here, recent advancements in the design and synthesis of wood-structured nanomaterials serving as advanced electrocatalysts for water splitting are summarized. First, the design principles and corresponding strategies toward highly effective wood-structured electrocatalysts (WSECs) are emphasized. Then, a comprehensive overview of current findings on WSECs, encompassing diverse structural designs and functionalities such as supported-metal nanoparticles (NPs), single-atom catalysts (SACs), metal compounds, and heterostructured electrocatalysts based on engineered wood hosts are presented. Subsequently, the application of these WSECs in various aspects of water splitting, including the hydrogen evolution reaction (HER), oxygen evolution reaction (OER), overall water splitting (OWS), and hybrid water electrolysis (HWE) are explored. Finally, the prospects, challenges, and opportunities associated with the broad application of WSECs are briefly discussed. This review aims to provide a comprehensive understanding of the ongoing developments in water-splitting catalysts, along with outlining design principles for the future development of WSECs.

Hierarchically Porous Covalent Organic Frameworks: Synthesis Methods and Applications.

Covalent organic frameworks (COFs) with high porosity have garnered considerable interest for various applications owing to their robust and customizable structure. However, conventional COFs are hindered by their narrow pore size, which poses limitations for applications such as heterogeneous catalysis and guest delivery that typically involve large molecules. The development of hierarchically porous COF (HP-COF), featuring a multi-scale aperture distribution, offers a promising solution by significantly enhancing the diffusion capacity and mass transfer for larger molecules. This review focuses on the recent advances in the synthesis strategies of HP-COF materials, including topological structure design, in-situ templating, monolithic COF synthesis, defect engineering, and crystalline self-transformation. The specific operational principles and affecting factors in the synthesis process are summarized and discussed, along with the applications of HP-COFs in heterogeneous catalysis, toxic component treatment, optoelectronics, and the biomedical field. Overall, this review builds a bridge to understand HP-COFs and provides guidance for further development of them on synthesis strategies and applications.

ExpoNano: A Strategy Based on Hyper-Cross-Linked Polymers Achieves Urinary Exposome Assessment for Biomonitoring.

Urinary analysis of exogenous and endogenous molecules constitutes an efficient, noninvasive approach to evaluate human health status. However, the exposome characterization of urinary molecules remains extremely challenging with current techniques. Herein, we develop an ExpoNano strategy based on hyper-cross-linked polymers (HCPs) to achieve ultrahigh-throughput measurement of exo/endogenous molecules in urine. The strategy includes a simple trapping-detrapping procedure (15 min) with HCPs in enzymatically treated urine, followed by mass spectrometer determination. Molecules that can be determined by ExpoNano have a wide range of molecular weight (75-837 Da) and Log Kow (octanol-water partition coefficient; -9.86 to 10.56). The HCPs can be repeatedly used five times without decreasing the trapping efficiency. Application of ExpoNano in a biomonitoring study revealed a total of 63 environmental chemicals detected in >50% of the urine pools collected from Chinese adults living in 13 cities, with a median concentration of 0.026-47 ng/mL, while nontargeted analysis detected an additional 243 exogenous molecules. Targeted and nontargeted analysis also detected 926 endogenous molecules in pooled urine. Collectively, the ExpoNano strategy demonstrates unique advantages over traditional urine analysis approaches, including a wide range of analytes, satisfactory trapping efficiency, high simplicity and reusability, and extremely reduced time demand and financial cost.

Hierarchically Porous Few-Layer Carbon Nitride and Its High H+ Selectivity for Efficient Photocatalytic Seawater Splitting.

Photocatalysts for seawater splitting are severely restricted because of the presence of multiple types of ions in seawater that cause corrosion and deactivation. As a result, new materials that promote adsorption of H+ and hinder competing adsorption of metal cations should enhance utilization of photogenerated electrons on the catalyst surface for efficient H2 production. One strategy to design advanced photocatalysts involves introduction of hierarchical porous structures that enable fast mass transfer and creation of defect sites that promote selective hydrogen ion adsorption. Herein, we used a facile calcination method to fabricate the macro-mesoporous C3N4 derivative, VN-HCN, that contains multiple nitrogen vacancies. We demonstrated that VN-HCN has enhanced corrosion resistance and elevated photocatalytic H2 production performance in seawater. Experimental results and theoretical calculations reveal that enhanced mass and carrier transfer and selective adsorption of hydrogen ions are key features of VN-HCN that lead to its high seawater splitting activity.

Zeolitic Imidazolate Frameworks Derived Co9 S8 /Nitrogen-Doped Hollow Porous Carbon Spheres as Efficient Bifunctional Electrocatalysts for Rechargeable Zinc-Air Batteries.

The development of nonprecious metal-based electrocatalysts with remarkable catalytic activity and long-cycling lifespan toward oxygen reduction reaction (ORR) and evolution reaction (OER) is especially important for rechargeable zinc-air batteries (ZABs). Herein, monodispersed Co9 S8 nanoparticles embedded in nitrogen-doped hierarchically porous hollow carbon spheres (Co9 S8 NPs/NHCS) are synthesized through a template-assisted strategy followed by a co-assembly, thermal annealing, and sulfurization process. Benefiting from larger specific surface area, hierarchically porous hollow structure, and carbon nanotubes self-growth, the obtained Co9 S8 NPs/NHCS-0.5 electrocatalyst exhibits decent performance for ORR (E1/2 =0.85 V) and OER (E10 =1.55 V). A rechargeable ZAB assembled using the Co9 S8 NPs/NHCS-0.5 as air cathode delivers a maximum power density of 116 mW cm-2 , high open circuit voltage of 1.47 V, and good durability (no obvious voltage decay after 1200 cycles (200 hours)). Such a hierarchically porous hollow structure of Co9 S8 NPs/NHCS-0.5 provides a confined space shell and an interconnected hollow core to achieve outstanding bifunctional catalytic activity and cycling stability, which surpass the benchmark Pt/C-RuO2 .

Synthesis of Hierarchically Porous Bioactive Glass and Its Mineralization Activity.

Mesoporous bioactive glass is a promising biomaterial for bone tissue engineering due to its good biocompatibility and bioactivity. In this work, we synthesized a hierarchically porous bioactive glass (HPBG) using polyelectrolyte-surfactant mesomorphous complex as template. Through the interaction with silicate oligomers, calcium and phosphorus sources were successfully introduced into the synthesis of hierarchically porous silica, and HPBG with ordered mesoporous and nanoporous structures was obtained. The morphology, pore structure and particle size of HPBG can be controlled by adding block copolymer as co-template or adjusting the synthesis parameters. The ability to induce hydroxyapatite deposition in simulated body fluids (SBF) demonstrated the good in vitro bioactivity of HPBG. Overall, this work provides a general method for the synthesis of hierarchically porous bioactive glasses.

High-Performance Zinc-Air Batteries Based on Bifunctional Hierarchically Porous Nitrogen-Doped Carbon.

Active and durable bifunctional electrocatalysts for the oxygen reduction reaction (ORR) and oxygen evolution reaction (OER) on the cathode are required for high-performance rechargeable metal-air batteries. Herein, the synthesis of hierarchically porous nitrogen-doped carbon (HPNC) with bifunctional oxygen electrocatalysis for Zn-air batteries is reported. The HPNC catalyst possesses a large surface area of 1459 m2 g-1 and exhibits superior electrocatalytic activity toward ORR and OER simultaneously with a low OER/ORR overpotential of 0.62 V, taking the difference between the potential at 10 mA cm-2 for OER and half-wave potential for ORR in 0.1 m KOH. Adopting HPNC as the air cathode, primary and rechargeable Zn-air batteries are fabricated. The primary batteries demonstrate a high open-circuit potential of 1.616 V, a specific capacity of 782.7 mAh gZn -1 and a superb peak power density of 201 mW cm-2 . The rechargeable batteries can be cycled stably for over 360 cycles or 120 h at the current density of 5 mA cm-2 . As elucidated by density functional theory, N-doping is preferred on defective sites with pentagon configuration and on the edge in the form of pyridinic-N-type. The high content of these two motifs in HPNC leads to the superior ORR and OER activities, respectively.

A Single-Atom Fe-N-C Catalyst with Ultrahigh Utilization of Active Sites for Efficient Oxygen Reduction.

Fe-N-C single-atom catalysts (SACs) are emerging as a promising class of electrocatalysts for the oxygen reduction reaction (ORR) to replace Pt-based catalysts. However, due to the limited loading of Fe for SACs and the inaccessibility of internal active sites, only a small portion of the sites near the external surface are able to contribute to the ORR activity. Here, this work reports a metal-organic framework-derived Fe-N-C SAC with a hierarchically porous and concave nanoarchitecture prepared through a facile but effective strategy, which exhibits superior electrocatalytic ORR activity with a half-wave potential of 0.926 V (vs RHE) in alkaline media and 0.8 V (vs RHE) in acidic media while maintaining excellent stability. The superior ORR activity of the as-designed catalyst stems from the unique architecture, where the hierarchically porous architecture contains micropores as Fe SAC anchoring sites, meso-/macro-pores as accessible channels, and concave shell for increasing external surface area. The unique architecture has dramatically enhanced the utilization of previously blocked internal active sites, as confirmed by a high turnover frequency of 3.37 s-1 and operando X-ray absorption spectroscopy analysis with a distinct shift of adsorption edge.

Super-Large-Scale Hierarchically Porous Films Based on Self-Assembled Eye-Like Air Pores for High-Performance Daytime Radiative Cooling.

Metal-free polymer daytime radiative cooling coatings with hierarchical eye-like air pores are proposed and fabricated with a super-large-scale film-stretching method. The hierarchically porous film (HPF) can be further coated with polymethyl methacrylate (PMMA) micro-hemispheres, forming coated HPF (cHPF), which do not dramatically change the optical or thermal properties. The cHPF is slightly better with a lower solar absorptivity (2.4%) and a higher thermal emissivity over the atmospheric transparency window (90.1%). The low solar absorptivity is due to the strong scattering of the hierarchical eye-like air pores, while the molecular vibrations and the focusing effect of the PMMA micro-hemispheres contribute to the high emissivity. An average mid-day temperature reduction of 7.92 °C is achieved relative to the air temperature, and the average cooling power reaches 116.0 W m-2 , which are much better than the cooling performances of the commercial cooling cushion. During the day, the cHPF-covered simulated building is up to 6.47 and 4.84 °C cooler than the ambient and the white painted counterpart, respectively. The film is durable and resistant to chemical etching, and very promising to use globally, especially in warm and tropical regions.

Highly Controllable Hierarchically Porous Ag/Ag2 S Heterostructure by Cation Exchange for Efficient Hydrogen Evolution.

Establishing the hierarchical porous architectures has been considered to be the most efficient approach to realize the efficient mass diffusion and large exposed active sites of designed micro/nanomaterial catalysts for hydrogen evolution reactions (HER). In this work, the nonequivalent cation exchange strategy is developed to fabricate the hierarchically porous Ag/Ag2 S heterostructure based on the rapid cation exchange by the metal-organic framework (MOF)-derived CoS. The as-prepared Ag/Ag2 S inherits the original 3D hollow morphology of CoS with porous nature, possessing abundant S-vacancies and lattice strain simultaneously due to the coordination loss and in-situ epitaxial growth of metallic Ag on the surface. Owing to the optimizations of lattice and electronic structures, the unique hierarchically porous Ag/Ag2 S heterostructure exhibits superior catalytic performance than previously reported catalysts derived from MOF. Theoretical calculations have confirmed that the co-existence of Ag cluster and sulfur vacancies activates the electroactivity of the interfacial defective region to boost the HER process. The binding strength of the proton and energetic trend of HER has been optimized with the formation of Ag/Ag2 S heterostructure, which guarantees the efficient generation of H2 . This study opens a new strategy for the utilization of the nonequivalent cation exchange strategy to efficiently synthesize advanced electrocatalysts with high performances.

Triple combination of natural microbial action, etching, and gas foaming to synthesize hierarchical porous carbon for efficient adsorption of VOCs.

Fungi residue, vinasse, and biogas residue differ from general biomass waste due to natural microbial action. Microbial fermentation helps create natural channels for the permeation of activators and produces proteins for natural nitrogen doping. Inspired by these advantages on porous carbon synthesis, this study adopted dual activators of KOH and KHCO3 to synthesize porous carbon with different pore ratios for efficient adsorption of volatile organic compounds (VOCs). The fungi residue possessed the least lignin due to the most severe microbial action, contributing to the best pore structures after activation. The etching effect from potassium compounds and gas foaming from the carbonate decomposition contributed to creating hierarchical porous carbon with ultra-high surface area, ca. 1536.8-2326.5 m2/g. However, KHCO3 addition also caused nitrogen erosion, such that lower adsorption capacity was attained even with a higher surface area when the mass ratio of KOH/KHCO3 decreased from 2.5:0.5 to 2:1. The maximum adsorption capacities of chlorobenzene (CB) and benzene (PhH) reached 594.0 and 394.3 mg/g, respectively. Pore structure variations after adsorption were evaluated by freeze treatment to discover the adsorption mechanism. The surface area after CB and PhH adsorption decreased 40.3% and 34.5%, respectively. Most of the mesopores might transform into micropores due to the mono/multilayer stacking of adsorbates. The VOC adsorption kinetics were simulated by the Pseudo-first- and -second-order models and Y-N model. This paper provides a new approach for high-value biomass waste utilization after microbial action to synthesize efficient adsorbents for VOCs.

Molecular Surgery at Microporous MOF for Mesopore Generation and Renovation.

Hierarchically porous MOFs (HP-MOFs) present advantageous synergism of micro- and mesopore but challenging in synthetic control at molecular scale. Herein, we present the first example of reversible and controllable mesopore generation and renovation in a microporous MOF of HKUST-1 via synthetic manipulation at molecular scale. An ammonia-gas etching strategy is proposed to create mesopores in carboxylate-based microporous MOFs and thus produce HP-MOFs. Gas-phase etching ensures uniform mesopore formation inside the MOF crystals via plane-oriented cutting the carboxylate-metal bonds off without affecting the crystal size and morphology. The mesopore size is controlled by the etching temperature, while the mesopore volume could be tuned by adjusting etchant pressure. The generated mesopores could be renovated using MOF precursors solutions so that to achieve controllable mesopore generation/closure, and encapsulation of the adsorbed molecules. This work demonstrates a powerful protocol for precisely tailoring and tuning the properties of MOF materials at molecular scale.

Highly Efficient Porous Carbon Electrocatalyst with Controllable N-Species Content for Selective CO2 Reduction.

We report a straightforward strategy to design efficient N doped porous carbon (NPC) electrocatalyst that has a high concentration of easily accessible active sites for the CO2 reduction reaction (CO2 RR). The NPC with large amounts of active N (pyridinic and graphitic N) and highly porous structure is prepared by using an oxygen-rich metal-organic framework (Zn-MOF-74) precursor. The amount of active N species can be tuned by optimizing the calcination temperature and time. Owing to the large pore sizes, the active sites are well exposed to electrolyte for CO2 RR. The NPC exhibits superior CO2 RR activity with a small onset potential of -0.35 V and a high faradaic efficiency (FE) of 98.4 % towards CO at -0.55 V vs. RHE, one of the highest values among NPC-based CO2 RR electrocatalysts. This work advances an effective and facile way towards highly active and cost-effective alternatives to noble-metal CO2 RR electrocatalysts for practical applications.

Micro-Blooming: Hierarchically Porous Nitrogen-Doped Carbon Flowers Derived from Metal-Organic Mesocrystals.

Synthesis of 3D flower-like zinc-nitrilotriacetic acid (ZnNTA) mesocrystals and their conformal transformation to hierarchically porous N-doped carbon superstructures is reported. During the solvothermal reaction, 2D nanosheet primary building blocks undergo oriented attachment and mesoscale assembly forming stacked layers. The secondary nucleation and growth preferentially occurs at the edges and defects of the layers, leading to formation of 3D flower-like mesocrystals comprised of interconnected 2D micropetals. By simply varying the pyrolysis temperature (550-1000 °C) and the removal method of in the situ-generated Zn species, nonporous parent mesocrystals are transformed to hierarchically porous carbon flowers with controllable surface area (970-1605 m2 g-1 ), nitrogen content (3.4-14.1 at%), pore volume (0.95-2.19 cm3 g-1 ), as well as pore diameter and structures. The carbon flowers prepared at 550 °C show high CO2 /N2 selectivity due to the high nitrogen content and the large fraction of (ultra)micropores, which can greatly increase the CO2 affinity. The results show that the physicochemical properties of carbons are highly dependent on the thermal transformation and associated pore formation process, rather than directly inherited from parent precursors. The present strategy demonstrates metal-organic mesocrystals as a facile and versatile means toward 3D hierarchical carbon superstructures that are attractive for a number of potential applications.

General Approach to Produce Nanostructured Binary Transition Metal Selenides as High-Performance Sodium Ion Battery Anodes.

Multiple transition metals containing chalcogenides have recently drawn boosted attraction as anodes for sodium ion batteries (SIBs). Their greatly enhanced electrochemical performances can be attributed to the superior intrinsic conductivities and richer redox reactions, comparative to mono metal chalcogenides. To employ various binary metals comprising selenides (B-TMSs) for SIBs, discovery of a simplistic, scalable and universal synthesis approach is highly desirable. Herein, a simple, facile, and comprehensive strategy to produce various combinations of nanostructured B-TMSs is presented. As a proof of concept, optimized, high surface area bearing, and hierarchical nanosheets of iron-nickel selenide (FNSe), iron-cobalt selenide, and nickel-cobalt selenide are produced and employed in SIBs. These B-TMSs exhibit adequately high energy capacities, excellent rate capabilities, and an extraordinarily stable life of 2600 cycles. As far as it is known, it is the first work to discuss sodium storage of FNSe, so various in situ and ex situ battery analyses are carried out to probe the sodium storage mechanism. When employed in sodium full batteries, these B-TMSs present reasonably high reversible specific capacities even after 100 cycles. Overall, the presented strategy will pave the way for facile synthesis of numerous binary transition metal chalcogenides that are the potential materials for energy storage and conversion systems.