Hollow Carbon Nanospheres Research Articles

Kinetically promoted hydrogen generation by Ru nanoparticles decorated CoB2O4 on mesoporous carbon spheres with rich oxygen vacancies for NaBH4 hydrolysis

Developing heterostructured catalysts with highly active and reusable is an urgent task to achieve green hydrogen production via NaBH4. Herein, we proposed a novel NaCl template method, which involves solid-state physical grinding of metal salts, reducing agents and prepared carbon spheres with the participation of sodium chloride to synthesize Ru-particles decorated CoB2O4 supported on hollow mesoporous carbon nanospheres (Ru/CoB2O4@C) catalysts for efficient and durable H2 generation through alkaline hydrolysis of NaBH4. The optimized catalyst with a Ru content of 3.0 wt% exhibits a high hydrogen generation rate of 8139 mL min−1gcat-1 and a low activation energy of 33.2 kJ mol−1 for NaBH4 hydrolysis, which is one of the most efficient catalysts reported recently. The extraordinary performance is mainly attributed to the synergistic effect between Ru and CoB2O4 species and abundant oxygen vacancies, which facilitate charge redistribution and provide more active sites, thereby enhancing the catalytic activity. Density functional theory calculations support the proposed Michaelis-Menten mechanism, where BH4− and H2O are adsorbed on electron-rich Ru and electron-deficient CoB2O4 surfaces, respectively, and the reaction energy barrier for the rupture of the B-H bond as the rate-determining step is only 1.37 eV, synergistically promoting the hydrolysis of NaBH4. Our study provides an innovative method for designing efficient and stable catalysts for green hydrogen generation.

Development of the Pipette-Tip Micro-Solid-Phase Extraction for Extraction of Rutin From Moringa oleifera Lam. Using Activated Hollow Carbon Nanospheres as Sorbents.

Herein, a micro-solid-phase extraction (μSPE) method was developed using a pipette tip for rutin extraction, employing activated hollow carbon nanospheres (HCNSs) as the sorbent. Characterization of the activated carbon nanospheres through TGA, FTIR, and SEM analysis confirmed the success of the activation process. The study demonstrated the efficacy of PT-μSPE in rutin extraction under pH 2 conditions with a standard concentration of 2 mg·L-1. The optimal mass of HCNSs was found to be 2 mg, and a loading volume of 500 μL resulted in the maximum recovery of rutin. Propan-2-ol was the best elution solvent with 15 aspirating/dispensing cycles. The correlation of determination (R 2) for the calibration curve was found to be 0.9991, and the LOD and LOQ values were 0.604 and 1.830 mg·L-1, respectively. The applicability of the method was demonstrated by extracting rutin from a complex Moringa oleifera leaf extract with the relative standard deviation (RSD) of 3.26%, thereby validating this method as feasible for the extraction of useful bioactive compounds from complex plant samples.

Using waste to treat waste: facile synthesis of hollow carbon nanospheres from lignin for water decontamination.

Lignin, the most abundant natural material, is considered as a low-value commercial biomass waste from paper mills and wineries. In an effort to turn biomass waste into a highly valuable material, herein, a new-type of hollow carbon nanospheres (HCNs) is designed and synthesized by pyrolysis of biomass dealkali lignin, as an efficient nanocatalyst for the elimination of antibiotics in complex water matrices. Detailed characterization shows that HCNs possess a hollow nanosphere structure, with abundant graphitic C/N and surface N and O-containing functional groups favorable for peroxydisulfate (PDS) activation. Among them, HCN-500 provides the maximum degradation rate (95.0%) and mineralization efficiency (74.4%) surpassing those of most metal-based advanced oxidation processes (AOPs) in the elimination of oxytetracycline (OTC). Density functional theory (DFT) calculations and high-resolution mass spectroscopy (HR-MS) were employed to reveal the possible degradation pathway of OTC elimination. In addition, the HCN-500/PDS system is also successfully applied to real antibiotics removal in complex water matrices (e.g. river water and tap water), with excellent catalytic performances.

Simultaneously enabling superior ICE and high rate/cycling stability with a hollow carbon nanosphere anode for sodium-ion storage

Hollow carbon nanosphere anode materials were manipulated by a pyrolysis temperature-mediated microstructure strategy to simultaneously achieve high ICE and superior rate/cycling stability.

Aptamer-functionalized hollow carbon nanospheres for the targeted chemo-photothermal therapy of breast tumor

The aptamer-modified HCNs/DOX/PEG with photothermal and chemotherapeutic effects can effectively promote the targeted drug delivery and the precise ablation of the photothermal agent, which achieving good treatment efficient on MCF-7 cells.

Glucose-based highly-porous activated carbon nanospheres (g-ACNSs) for high capacity hydrogen storage

The high density of sp2 defects and specific surface area result in an exceptional H2 storage capacity and stability of hollow carbon nanospheres.

Tailoring hierarchical pore structures in carbon scaffolds for hydrogen storage of nanoconfined magnesium

Various carbon scaffolds have been developed for the nanoconfinement of Mg/MgH2 to achieve the synergistic effects of nanosizing-induced kinetic improvement, Mg-scaffold interaction-induced catalytic enhancement, and mechanical stress-driven thermodynamic stability tuning for advanced hydrogen storage. Yet, systematic studies linking the chemo-structural features of the carbon scaffolds and the hydrogen storage properties of Mg/MgH2 nanoparticles within the scaffolds remain largely unexplored. Here, we investigate the pore-dependent Mg nanoconfinement and its hydrogen storage behavior using hollow carbon nanospheres (HCNs) as scaffolds, dictated by their distinct pore properties. Contrary to the conventional wisdom of nanoconfinement, the Mg nanoparticles confined by the HCN with large mesopores exhibit faster hydrogen sorption kinetics and improved thermodynamic characteristics than those with small mesopores. The detailed analyses reveal that the interplay between reversible mechanical stress upon hydrogenation and nanosizing-induced facile kinetics leads to the observed experimental results. Ab initio computations further show that compressive stress retards bulk diffusion while at the same time enhances the surface hydrogen desorption, suggesting the need for stress optimization within the composite. Our study provides a design guideline for Mg strain engineering and the subsequent carbon scaffold structures for hydrogen storage, possibly leading to advanced hydrogen storage of confined Mg.

Hollow and Silver-Cored Carbon Nanospheres as Effective Sulfur Hosts for Lithium-Sulfur Batteries

Lithium sulfur (Li–S) batteries are considered to be one of the most promising “beyond lithium-ion” energy storage technologies and the development of alternative battery chemistries is required to alleviate our reliance on the burning of fossil fuels 1. The high theoretical specific capacity of sulfur (1672mAh g-1) leads to a theoretical specific energy of ~2510 Wh kg-1, which is significantly greater than the state-of-the-art lithium-ion batteries 2. Further to this, sulfur is environmentally benign, low cost, and Li–S batteries do not rely on cobalt, or manganese 3, which are expensive, toxic, and have known ethical implications associated with their extraction and refining 4.While Li–S batteries boast many theoretical advantages, their practical application has been plagued with an array of limitations, mainly attributed to the poor electrical conductivity of sulfur, the significant volumetric expansions (80%) that can occur during cycling, and the soluble polysulfide intermediates 5. To tackle this, current research efforts have focused on using porous carbon materials (PCMs) to prepare sulfur/carbon composite cathodes 6,7. PCMs offer improved electrical conductivity, a large specific surface area, and pore diameters that are less than 1nm—which may confine the soluble polysulfides within the cathode matrix 8.In this study, the synthesis of hollow and silver-cored carbon nanospheres (HCNS, Ag-CNS) is detailed and their use as a multifunctional sulfur host for Li–S batteries is assessed. Ag-CNS are synthesised via a hydrothermal procedure from a simple saccharide solution coupled with a silver precursor. These Ag-CNS are further processed to prepare HCNS by etching the internal silver nanoparticle with an acid solution. The hydrothermal procedure described in this study offers a simplification to traditional HCNS synthesis methods which typically require the removal of templates, such as silica nanospheres, through etching with hazardous chemicals such as hydrofluoric acid.In this work, the structural and physical properties of HCNS and Ag-CNS are characterised using transmission electron microscopy, scanning electron microscopy, nitrogen gas adsorption, X-ray diffraction, Raman spectroscopy, Fourier-transform infrared spectroscopy, and thermogravimetric analysis. The electrochemical performance of these materials, when used as a sulfur host, is investigated through the preparation, and testing of half cells with lithium metal anodes. Electrochemical testes include cyclic voltammetry and galvanostatic cycling data at different C-rates.

Modified Solid Electrolyte Interphases with Alkali Chloride Additives for Aluminum-Sulfur Batteries with Enhanced Cyclability

Al-S batteries are promising energy storage devices, employing high-capacity and low-cost Al (2980 mA h g-1, 8050 mAh cm-3) and sulfur (1672 mAh g-1) as the anode and cathode, respectively. However, Al-S batteries suffer from the notorious shuttle effect of polysulfides as other intensively investigated metal-sulfur batteries. Up to now, several strategies have been proposed to improve the poor reversibility and lifespan of Al-S batteries. At the cathode side, materials that can adsorb polysulfides have been employed as the host material of sulfur to reduce the dissolution of polysulfides,1,2 e.g., heteroatom-functionalized and/or hierarchical porous carbonaceous materials, metal-organic frameworks (MOFs), boron nitrides, and Mxenes.3,4 Nonetheless, AMAs, which also play an important role in the shuttle process, have received little attention up to now. Suitable engineering of electrolytes enabling an electronically insulating solid electrolyte interphase (SEI) on AMAs may suppress the deposition of low-solubility Al2S3 and/or short-chain polysulfides further promoting the cell cycling performance.Herein, alkali chlorides are, for the first time, proposed as electrolyte additives to modify the SEI on AMAs and suppress the polysulfide shuttle in Al-S batteries.5 It is demonstrated that adding NaCl to the conventional [AlCl3]1.3[EmimCl]1 electrolyte can enhance the cyclability of Al-S batteries by forming a thicker, NaxAlyO2-containing SEI layer on AMAs. In addition to NaCl, LiCl and KCl as electrolyte additives also lead to improvement of Al-S batteries’ lifespan. These findings provide a new path to suppress the detrimental polysulfides shuttle effect in Al-S batteries, resulting in their improved cycle performance. References (1) Smajic, J.; Wee, S.; Simoes, F. R. F.; Hedhili, M. N.; Wehbe, N.; Abou-Hamad, E.; Costa, P. M. F. J. Capacity Retention Analysis in Aluminum-Sulfur Batteries. ACS Appl. Energy Mater. 2020, 3 (7), 6805–6814.(2) Zhang, Y.; Ma, L.; Tang, R.; Zheng, X.; Wang, X.; Dong, Y.; Kong, G.; Zhao, F.; Wei, L. The Host Hollow Carbon Nanospheres as Cathode Material for Nonaqueous Room-Temperature Al–S Batteries. Int. J. Hydrogen Energy 2021, 46 (7), 4936–4946.(3) Guo, Y.; Jin, H.; Qi, Z.; Hu, Z.; Ji, H.; Wan, L. J. Carbonized-MOF as a Sulfur Host for Aluminum–Sulfur Batteries with Enhanced Capacity and Cycling Life. Adv. Funct. Mater. 2019, 29 (7), 1–6.(4) Wang, Z.; Zheng, X.; Chen, A.; Han, Y.; Wei, L.; Li, J. Unraveling the Anchoring Effect of MXene-Supported Single Atoms as Cathodes for Aluminum−Sulfur Batteries. ACS Mater. Lett. 2022, 4, 8, 1436-1445.(5) Xu, C.; Diemant, T.; Liu, X.; Passerini, S. Modified Solid Electrolyte Interphases with Alkali Chloride Additives for Aluminum–Sulfur Batteries with Enhanced Cyclability. Adv. Funct. Mater. 2023. 2214405.

Engineering contact curved interface with high-electronic-state active sites for high-performance potassium-ion batteries.

Potassium-ion batteries (PIBs) have attracted ever-increasing interest due to the abundant potassium resources and low cost, which are considered a sustainable energy storage technology. However, the graphite anodes employed in PIBs suffer from low capacity and sluggish reaction kinetics caused by the large radius of potassium ions. Herein, we report nitrogen-doped, defect-rich hollow carbon nanospheres with contact curved interfaces (CCIs) on carbon nanotubes (CNTs), namely CCI-CNS/CNT, to boost both electron transfer and potassium-ion adsorption. Density functional theory calculations validate that engineering CCIs significantly augments the electronic state near the Fermi level, thus promoting electron transfer. In addition, the CCIs exhibit a pronounced affinity for potassium ions, promoting their adsorption and subsequently benefiting potassium storage. As a result, the rationally designed CCI-CNS/CNT anode shows remarkable cyclic stability and rate capability. This work provides a strategy for enhancing the potassium storage performance of carbonaceous materials through CCI engineering, which can be further extended to other battery systems.

Facile synthesis of FeNi alloy-supported N-doped Mo2C hollow nanospheres for the oxygen evolution reaction

The rapid depletion of fossil fuels results in significant environmental pollution. Consequently, researching environmentally friendly and cost-effective electrocatalysts with exceptional oxygen evolution reaction (OER) capabilities holds immense importance in enhancing the efficient utilization of resources. In this paper, a straightforward and cost-effective method was employed to produce Fe-Ni alloy-supported N-doped carbon hollow nanospheres (FeNi/Mo2C/NC) using self-assembled molybdenum dopamine spheres (Mo-PDA-HS) as a substrate. The inclusion of iron and nickel addressed the issue of aggregation and collapse in Mo-PDA-HS nanostructures at high temperatures, while adjusting the electronic structure of the composites to achieve efficient OER activity. The composite displayed a low overpotential (η10 mA = 304 mV) and a minimal Tafel slope (41.8 mV/dec-1). This study introduces a simple strategy for constructing structurally robust and non-aggregating Mo2C nanostructures, along with a direct method for designing cost-effective and high-performance catalysts for OER.

BIMMOF-derived ZnS/Co9S8 heterojunctions decorated hollow carbon nanospheres as advanced anode materials for lithium-ion batteries

Metal-organic frameworks (MOFs) offer significant advantages for constructing bimetallic sulfides as anode materials for lithium-ion batteries. However, the crystal structure of pure MOFs tends to collapse during ion insertion and detachment, resulting in somewhat limited electrochemical performance. Here, the crystal size of the bimetallic organic framework (BIMMOF) is reduced by in situ growth on hollow carbon spheres (HCS) by the solvothermal method. As a result, the well-dispersed BIMMOF-derived ZnS/Co9S8 heterojunction anode material was obtained with hollow carbon spheres as support. Due to the unique structure of ZnS/Co9S8@N-HCS with ultrafine size and the synergistic effect of Zn2+ and Co2+, this anode material has excellent electrochemical performance. Especially, it exhibits a capacity of 1595 mAh g−1 after 100 cycles at 100 mA g−1 and maintains a capacity of 1109 mAh g−1 after 1800 cycles at 2500 mA g−1. The remarkable lithium storage properties demonstrated by the ZnS/Co9S8 heterostructure provide inspiration for the wide adoption of this structural design strategy to improve the electrochemical performance of bimetallic sulfide anodes.

Integration of Highly Graphitic Three-Dimensionally Ordered Macroporous Carbon Microspheres with Hollow Metal Oxide Nanospheres for Ultrafast and Durable Lithium-Ion Storage

Achieving excellent electrochemical performance at high charging rate has been a long-cherished dream in the field of lithium-ion batteries (LIBs). As a part of the efforts to meet the goal, an innovative strategy for the synthesis of 3D porous highly graphitic carbon microspheres, to which numerous hollow metal oxide nanospheres are anchored, for use as anode in LIBs is introduced. Hollow carbon nanosphere-aggregated microspheres prepared from the spray drying process are graphitized with the aid of metal catalysts, and subsequent oxidation selectively removed amorphous carbon, leading to the formation of highly conductive graphitic carbon matrix. Numerous hollow metal oxide nanospheres formed simultaneously during the oxidation process via nanoscale Kirkendall diffusion are anchored onto the carbonaceous matrix, effectively reinforcing the structural integrity by alleviating volume changes and reducing lithium-ion diffusion lengths. The synergistic effect of combining hollow metal oxide nanospheres with high theoretical capacity with conductive carbon matrix led to accelerated electrochemical kinetics, resulting in high capacity at high charging rate. In addition, trapping the hollow metal oxide nanospheres inside hollow carbon nanospheres could effectively alleviate the volume changes, which led to high structural stability. When applied as LIB anodes, the microspheres exhibit a capacity of 411 mA h g−1 after 2500 cycles at 10.0 A g−1, with ~80% capacity retention. The anode exhibits a high capacity of 274 mA h g−1 at an extremely high current density of 50.0 A g−1, thus demonstrating the structural merits of the microspheres.

Novel synthesis of γ-Al2O3/carbon hollow nanosphere nanocomposite for the optimal removal of Ni2+ ions from wastewater and reuse in blood fingerprint enhancement

This study aimed to solve environmental problems, particularly water quality and escalating crime rates. The carbon hollow nanosphere was prepared from orange peels by a reflux method. The carbon hollow nanosphere was coated with Gamma-aluminium oxide (γ-Al2O3 NPs) via the hydrothermal method. The samples were analysed using Fourier-transform infrared spectroscopy, Scanning electron microscopy, Transmission Electron Microscopy, Brunauer–Emmett–Teller, Thermogravimetric analysis, and X-Ray diffraction analysis. The surface area of γ-Al2O3/carbon hollow nanosphere nanocomposite was confirmed to be 578,039 m2/g, and the Ni2+ ions were analysed using ICP-OES. With a maximum adsorption capacity of 56.980 mg/g and a pH 9, batch adsorption experiments revealed that the uptake of Ni2+ ions best fitted the Langmuir adsorption isotherm, and the pseudo-second-order kinetics model effectively described the uptake of Ni2+ ions with a higher R2 of 0.999. Thermodynamic measurements showed the endothermic and spontaneous nature of the Ni2+ ions adsorption using the γ-Al2O3/carbon hollow nanospheres nanocomposite. The adsorbent was then used to identify latent blood fingerprints, and it was discovered that Ni2+-γ-Al2O3/carbon hollow nanosphere generated clear images of blood fingerprints on different substrates.Graphical abstract

Sensitive electrochemical detection of benzocaine based on hollow carbon nanobowl modified electrode

Benzocaine (BZC) is a widely used anaesthetic drug coupled with multiple undesirable side effects, thus developing sensitive method for its detection is of great importance; meanwhile, hollow carbon nanospheres (HCS) have received intense interests in electroanalysis resulted from its unique merits, but the related close structures restrain the availability factor of the internal surfaces, hence suppressing their analytical performance. In this work, a novel nanomaterial with open structure, hollow carbon nanobowl (HCB) was prepared and adopted as the electrode material for fabricating a highly sensitive electrochemical sensor of BZC. The obtained results revealed the as-prepared HCB can display more superior sensing performance than conventional HCS. After optimizing various experimental conditions including the modified amount of HCB, accumulation time and the buffer pH value, the detection of BZC was performed at HCB modified electrode, and a considerably low detection limit (4.0 nM) coupled with high sensitivity (2.1527 μA μM−1) was obtained. In addition, the further experiments demonstrated that the HCB modified electrode possesses superior capability in repeatability, stability, selectivity and practical application. It’s thus expected that the as-designed HCB-based sensing platform has important application for BZC and other targets detection.

Fluffy ultrathin WO3 nanoneedle clusters in-situ grown in mesoporous hollow carbon nanospheres as advanced anode for lithium-ion batteries

Fluffy ultrathin WO3 nanoneedle clusters are in-situ grown in mesoporous hollow carbon nanospheres (MHCSs) via unique material impregnation and confined molten reaction in MHCS nanoreactors. Through transmission electron microscopy, scanning electron microscopy, X-ray diffraction, Raman spectra and X-ray photoelectron spectroscopy analyses, it can be found that WO3 nanoneedles with 5–10 nm in thickness and ∼140 nm in length are encapsulated within each MHCS with 150–250 nm in diameter and 30–40 nm in shell thick. Thermal gravimetric analysis reveals the WO3 content of 83.5 wt%. Lithium storage performance was evaluated by galvanostatic charge/discharge cycling, cyclic voltammogram and electrochemical impedance spectroscopy. The composite exhibits remarkable rate performance (average discharge capacity of 1352 mAh g−1 at 0.1 A g−1 and 105 mAh g−1 at 10 A g−1) and excellent cycling performance (1094 mAh g−1 at 0.2 A g−1 after 50 cycles, 760 mAh g−1 at 1 A g−1 after 500 cycles, 351 mAh g−1 at 5 A g−1 after 2000 cycles). The composite also presents outstanding kinetics properties, such as high Li+ diffusion coefficient, strong capacitive effect, and low electrochemical impedance. The superior electrochemical performance is attributed to unique “ship-in-a-bottle” structure. MHCSs facilitate electron transfer and ion diffusion, buffer volume change of WO3 and maintain the integrity of WO3. Furthermore, fluffy ultrathin nanoneedle cluster structure endows WO3 with high electrochemical activity.

Formulating N-Doped Carbon Hollow Nanospheres with Highly Accessible Through-Pores to Isolate Fe Single-Atoms for Efficient Oxygen Reduction.

It is challenging yet promising to design highly accessible N-doped carbon skeletons to fully expose the active sites inside single-atom catalysts. Herein, mesoporous N-doped carbon hollow spheres with regulatable through-pore size can be formulated by a simple sequential synthesis procedure, in which the condensed SiO2 is acted as removable dual-templates to produce both hollow interiors and through-pores, meanwhile, the co-condensed polydopamine shell is served as N-doped carbon precursor. After that, Fe─N─C hollow spheres (HSs) with highly accessible active sites can be obtained after rationally implanting Fe single-atoms. Microstructural analysis and X-ray absorption fine structure analysis reveal that high-density Fe─N4 active sites together with tiny Fe clusters are uniformly distributed on the mesoporous carbon skeleton with abundant through-pores. Benefitted from the highly accessible Fe─N4 active sites arising from the unique through-pore architecture, the Fe─N─C HSs demonstrate excellent oxygen reduction reaction (ORR) performance in alkaline media with a half-wave potential up to 0.90V versus RHE and remarkable stability, both exceeding the commercial Pt/C. When employing Fe─N─C HSs as the air-cathode catalysts, the assembled Zn-air batteries deliver a high peak power density of 204mWcm-2 and stable discharging voltage plateau over 140h.

Confined synthesis of ternary FeCoMn single-atom nanozyme in N-doped hollow mesoporous carbon nanospheres for synergistic chemotherapy and chemodynamic cancer therapy

Recently, nanozymes show increasing biological applications and promising possibilities for therapeutic intervention, while their mediated therapeutic outcomes are severely compromised due to their insufficient catalytic activity and specificity. Herein, ternary FeCoMn single atoms were incorporated into N-doped hollow mesoporous carbon nanospheres by in situ confinement pyrolysis at 800 °C as high-efficiency nanozyme. The confinement strategy endows the as-prepared nanozyme with the enhanced catalase- and oxidase-like activities. Specifically, the FeCoMn TSAs/N-HCSs nanozyme can decompose intracellular H2O2 to generate O2 and subsequently convert O2 to cytotoxic superoxide radicals (O2∙–), which can initiate cascade enzymatic reactions in tumor microenvironment (TME) for chemodynamic therapy (CDT). Moreover, the cancer therapy was largely enhanced by loading with doxorubicin (DOX). Impressively, the FeCoMn TSAs/N-HCSs nanozyme-mediated CDT and the DOX-induced chemotherapy endow the DOX@FeCoMn TSAs/N-HCSs with effective tumor inhibition, showing the superior therapeutic efficacy.

Electrochemical Determination of Tyrosine by a Silver Nanoparticle – Hollow Carbon Sphere Modified Glassy Carbon Electrode (GCE)

The accurate and sensitive determination of tyrosine is of paramount value. In this work, we reported the synthesis and characterization of a new nanohybrid composed of silver nanoparticles and hollow carbon nanospheres (Ag/HMCS) for the amperometric sensing of tyrosine. The Ag/HMCS nanohybrid was used to modify electrodes and to fabricate an amperometric sensor for tyrosine at a working potential of 450 mV in aqueous 0.1 M phosphate buffer at pH 7.0. Under optimal conditions, the sensor determined tyrosine from 0.08 to 100 μM with a detection limit of 0.02 μM.

NiCo2 O4 /Hollow Mesoporous Carbon Nanosphere Hybrids Enabling Super-Hydrophobicity, Thermal Insulation, and Highly Efficient Microwave Absorption.

The combination of 2D magnetic nanosheets and mesoporous carbon with unique interfaces shows considerable prospects for microwave absorption (MA). However, traditional assembly procedures make it impossible to accurately manage the assembly of magnetic nanosheets in carbon matrices. Herein, a reverse strategy for preparing complex magnetic nanosheet cores inside carbon-based yolk-shell structures is developed. This innovative approach focuses on controlling the initial crystallite formation sites in a hydrothermal reaction as well as the inflow and in situ growth behavior of 2D NiCo-layered double hydroxide precursors based on the capillary force induced by hollow mesoporous carbon nanospheres. Accordingly, the as-prepared YS-CNC-2 absorber exhibits remarkable MA performances, with an optimal reflection loss as low as -60.30dB at 2.5mm and an effective absorption bandwidth of 5.20GHz at 2.0mm. The loss of electromagnetic waves (EMW) depends on natural resonance loss, dipole polarization relaxation, and multiple scattering behavior. Ontopof that, the functionalized super-hydrophobic MA coating is produced in spraying and curing processes utilizing YS-CNC-2 nanoparticles and fumed silica additives in the polydimethylsiloxane matrix. The excellent thermal insulation, self-cleaning capability, and durability in diverse solutions of the coating promise potential applications for military equipment in moist situations.