Growth Of Nanosheets Research Articles

Vertically growth of MoS2 nanosheets on g-C3N4 towards enhanced electrocatalytic performance

MoS2 nanosheets were vertically grown in S-doped graphitic carbon nitride (g-C3N4) nanosheets to enhance electrochemical performance. Dicyandiamide was used as a precursor while sodium molybdate and thioacetamide were as additives, and sulfur was introduced into the carbon lattice of thin-layered g-C3N4 by a two-step thermal polymerization. S-g-C3N4/MoS2 (SCN/MoS2) heterojunctions were then created by a solvothermal synthesis. Subsequently, the electrochemical performance of the heterojunctions was explored. The result suggested that the surface of S-g-C3N4 nanosheets load on uniformly arranged layered MoS2 possession revealed the smallest Tafel slope of 77.2 mV dec−1. After 1000 cycles, no significant change was observed for the linear sweep voltammetry curves. The SCN/MoS2 heterojunction revealed a specific capacity of 588 F g−1 after being assembled into an asymmetric supercapacitor. Superior thin g-C3N4 nanosheets and constituting a composite with strong interfacial electronic coupling with MoS2, doping with heteroatomic elements, and changing the surface structure of g-C3N4 enhanced the charge transfer kinetics and improved the electrochemical performance.

Dual-Responsive MnO2-Loaded Carbonaceous Nanobottle Motors Fabricated by Interfacial Superassembly for On-The-Fly MicroRNA Sensing.

Diverse nanomotors with advanced motion manipulation have been proposed to revolutionize the way problems in many fields are solved. However, rational and controllable synthetic methods of multifunctional nanomotor are still limited. Herein, dual-responsive MnO2-loaded carbonaceous nanobottle motors (MnO2 NBMs) are developed through an interfacial superassembly strategy. Asymmetric carbonaceous nanobottles are first synthesized, and the reductive carbonaceous shell induces an oxidation-reduction reaction with KMnO4 for in-situ growth of MnO2 nanosheets, which enables the nanomotor to perform either self-diffusiophoretic or self-thermophoretic motion in response to H2O2 and near-infrared light, respectively. Inspired by bioaffinity sensing, the nanomotors are sequentially assembled with functional nanoparticles and hairpin DNA to construct swimming functional MnO2 NBMs (MnO2 FNBMs) probes. The probes can move around complex samples to improve target miRNA transport and accelerate receptor-target interaction. Coupling with the photocurrent-signal amplification, the self-assembly of photoelectrochemical (PEC) biosensors has been achieved for sensitive microRNA detection. Trace amounts of miRNA-155 can be quickly detected with a wide detection range (100 fM to 100nM). Moreover, the direct detection of microRNA in tumor cell lysates by the biosensor is demonstrated. Given the merits of automation and miniaturization, the proposed strategy provides a promising method for fast and effective self-assembly of biosensors.

Nitrogen plasma-induced phase engineering and titanium carbide/carbon nanotubes dual conductive skeletons endow molybdenum disulfide with significantly improved lithium storage performance

MoS2/Ti3C2 MXene composite has emerged as a promising anode material for lithium storage due to the synergistic combination of high specific capacity offered by MoS2 and conductive skeleton provided by Ti3C2 MXene. However, its two-dimensional/two-dimensional (2D/2D) structure is susceptible to collapse after long cycles, while the inherent low conductivity of MoS2 limits its rate performance. In this study, we developed a novel approach combining plasma-induced phase engineering with dual skeleton structure design to fabricate a unique P-MoS2/Ti3C2/CNTs anode material featuring highly conductive 1T phase MoS2 and a stable one-dimensional/two-dimensional (1D/2D) architecture. Within this architecture, growth of MoS2 nanosheets on the surface of Ti3C2 cross-linked by carbon nanotubes (CNTs) was achieved. The resulting Ti3C2/CNTs dual skeleton not only provides robust mechanical support to prevent structural collapse during long cycles but also offers increased specific surface area and additional Li+ storage space, thereby enhancing the lithium storage capacity of the composite. Subsequent N2 plasma treatment induced a phase transition in MoS2 from 2H to 1T configuration. Density functional theory (DFT) calculations confirmed that the induced 1T-MoS2 exhibits higher conductivity and lower Li+ diffusion barrier compared to 2H-MoS2. Benefiting from these synergistic effects, our P-MoS2/Ti3C2/CNTs anode demonstrated remarkable electrochemical performance including a high reversible specific capacity of 1120 mAh g−1 at 0.1 A g−1, excellent cycling stability with a specific capacity retention of 670 mAh g−1 after 600 cycles at 1 A/g, and superior rate performance with a specific capacity of 614 mAh g−1 at 2 A g−1. This combined modification strategy will serve as guidance for designing other energy storage materials.

Controllable growth of large 1T-NbTe2 nanosheets on mica by chemical vapor deposition and its magnetic properties

Two-dimensional (2D) magnetic materials have recently attracted broad attention for their potential technological applications. Here, we report controllable growth of NbTe2 nanosheets on mica substrate by atmospheric chemical vapor deposition. Different from the SiO2/Si substrates, dangling bonds on the surface of the mica are absent, which induces low nucleation density and higher lateral growth rate. As a result, the lateral size of NbTe2 nanosheets on mica substrates can be significantly larger than those on SiO2/Si substrates. Large single crystal NbTe2 nanosheets with a lateral size of up to 151 µm were fabricated on a mica. High-resolution transmission electron microscope image, XRD patterns and Raman spectra reveal the NbTe2 nanosheets adopt the single crystal with 1T phase. Furthermore, the NbTe2 nanosheets on mica demonstrate ferromagnetic properties with a Curie temperature of up to 162 K. Our work paves the way for the atmospheric chemical vapor deposition growth and applications of many more 2D magnets.

In situ growth of ZnIn2S4 nanosheets on 2D NiFeS sheets from vulcanization of Ni–Fe LDH for enhancing photocatalytic hydrogen production

In this paper, 2-dimensional (2D) ZnIn2S4/NiFeS novel junctions were constructed through in-situ growing ZnIn2S4 nanosheets on 2D large NiFeS sheets with large specific area which were prepared from vulcanization of layer-structured Ni–Fe LDH by a solvent-thermal method. The rough and porous surface of FeNiS, as demonstrated by SEM pictures, endowed the heterojunction large interfacial area and more active sites for hydrogen evolution. Various tests indicate that the integration of a small amount of NiFeS in the heterojunction greatly improved carrier separation efficiency, migration rate, and surface H2 evolution activity, leading to the enhanced photocatalytic hydrogen production ability. Optimal 0.6%-NFS/ZIS composite shows the highest photocatalytic H2 evolution rate of 1506 μmol h−1 g−1, 2.4 times that of ZnIn2S4. This study provides a novel and cost-effective approach improving photocatalytic H2 evolution activity of sulfides in visible-light-driven water splitting.

Highly selective thin B-oriented MFI zeolite membranes on scalable modified stainless steel supports

Enhancing the separation performance of molecular sieve membranes relies significantly on precise control over their membrane morphology and microstructure. This involves creating thin, closely packed, oriented, and uniform coatings of seed crystals, enabling subsequent intergrowth to establish continuous membranes. To address industrial needs, it is crucial to generate a thin and flawless membrane efficiently producible on a large-scale support. Porous stainless supports offer scalability and easy integration into membrane modules. In this study, we present a novel and straightforward process for modifying stainless-steel supports to seed zeolite membrane layers. High-performance, b-oriented MFI zeolite membranes can be synthesized on these modified stainless-steel supports through scalable filtration seeding of MFI zeolite nanosheets followed by secondary growth. By employing a carefully designed pre-treatment procedure, we achieved the growth of well-intergrown, highly b-oriented MFI zeolite membranes on the modified stainless-steel support, establishing a robust interaction with the substrate. The membranes, fabricated through gel-free secondary growth of nanosheets deposited on a scalable stainless-steel support using this technique, demonstrate ultra-selective capabilities in separating para-xylene from ortho-xylene, with a high separation factor of 388.

Preparation of MoSe2 nanosheets/nitrogen-doped carbon nanotubes and their electrochemical energy storage properties

Lithium-sulfur batteries can be used as excellent energy storage devices, but they still face some challenges in the practical application, such as the poor electrical conductivity of sulfur, the volume expansion of sulfur during the discharge process, and the dissolution of polysulfides. In this study, polypyrrole-coated molybdenum trioxide nanorods were used as templates for the simultaneous in-situ growth of MoSe2 nanosheets on the outer/inner sides of nitrogen-doped carbon nanotubes. When the MoSe2/N-carbon nanotubes (MoSe2/NC NTs) were used as sulfur carriers for lithium-sulfur battery, the large specific surface area of the N-carbon nanotubes facilitated the homogeneous loading of MoSe2 nanosheets and exposed more catalytically active sites of the MoSe2 nanosheets, increasing the contact area of electrolyte. In addition, the N-doped carbon nanotubes have excellent electrical conductivity, which greatly promotes the electrical conductivity of the cathode. The density functional theory calculations, adsorption experiments, and XPS results all confirm that the MoSe2/NC NTs are able to anchor lithium polysulfides through strong adsorption, thus effectively mitigating the shuttle effect of polysulfides. This study supplies a novel route for the preparation of sulfur host for advanced lithium-sulfur batteries.

Oriented growth of NiCo metal–organic framework nanosheets on electrode materials for ternary mixed metal oxide supercapacitors

Metal–organic frameworks (MOFs) are porous structures that possess high specific surface areas, making them promising cathode materials for energy storage devices. However, solving the problems of random growth and easy aggregation of MOF nanosheets remains a challenge. In this study, hydrothermal and calcination methods were used to successfully create nickel cobalt molybdenum metal oxide (NCMO) nanoflowers, followed by the directional growth of NiCo–MOF on its surface. The oriented growth of NiCo–MOF nanosheets on NCMO nanospheres effectively prevented agglomeration, forming NCMO@NiCo–MOF with enhanced electrochemical sensitivity and a large quantity of active sites. When used as an electrode, NCMO@NiCo–MOF forms a large contact area with the electrolyte, demonstrating a high specific capacitance of 1724 F g−1 at a current density of 1 A g−1. Furthermore, at a power density of 824.8 W kg−1, an asymmetric supercapacitor constructed from NCMO@NiCo–MOF and activated carbon exhibited a high energy density of 44.5 Wh kg−1. This study presents a facile method for the assembly of MOF nanosheets for three-dimensional supercapacitors.

Z-Scheme Heterojunction of Hierarchical Cu2S/CdIn2S4 Hollow Cubes to Boost Photoelectrochemical Performance.

The exaltation of light-harvesting efficiency and the inhibition of fast charge recombination are pivotal to the improvement of photoelectrochemical (PEC) performance. Herein, a direct Z-scheme heterojunction is designed of Cu2S/CdIn2S4 by in situ growth of CdIn2S4 nanosheets on the surface of hollow CuS cubes and then annealing at 400°C. The constructed Z-scheme heterojunction is demonstrated with electron paramagnetic resonance and redox couple (p-nitrophenol/p-aminophenol) measurements. Under illumination, it shows the photocurrent 6 times larger than that of hollow Cu2S cubes, and affords outstanding PEC performance over the known Cu2S and CdIn2S4-based photocatalysts. X-ray photoelectron spectroscopy and density functional theory results demonstrate a strong internal electric field formed in Cu2S/CdIn2S4 Z-scheme heterojunction, which accelerates the Z-scheme charge migration, thereby promoting electron-hole separation and enhancing their utilization efficiency. Moreover, the hollow structure of Cu2S is conducive to shortening the charge transport distance and improving light-harvesting capability. In proof-of-concept PEC application, a PEC detection method for miRNA-141 based on the sensitivity of benzo-4-chloro-hexadienone to light absorption on Cu2S/CdIn2S4 modified electrode is developed with good selectivity and a limit of detection of 32 aM. This work provides a simple approach for designing photoactive materials with highly efficient PEC performance.

Construction of heterojunctions with in situ growth of ZnIn2S4 nanosheets on the surface of atomically dispersed Cu-modified MOFs for high-performance visible-light photocatalytic antibiotic degradation

Metal-organic frameworks (MOFs) are ideal candidates for obtaining composites with excellent photocatalytic properties due to their reasonable band gaps and high specific surface area. In this study, Cu@UiO-66-NH2@ZnIn2S4 nanocomposites were prepared by a two-step photoinduction method and hydrothermal method. The prepared catalysts in a range of ratios showed high visible light degradation of tetracycline hydrochloride (TC). Among them, 10%-Cu@UIO-66-NH2/ZnIn2S4 showed the best catalytic activity and photoelectrochemical performance. In this catalytic system, the high specific surface area and porosity of UIO-66-NH2 provide sites for the high dispersion of Cu. In addition, the introduction of Cu also reduces the band gap, which is conducive to the electron transfer between the interfaces, which results in the formation of type II heterojunctions with a unique and highly efficient electron transfer mechanism, and also enables the photocatalytic process to generate more active radicals (O2–, OH, h+). In addition, the stability of the catalyst was tested, as well as the possible degradation pathways were hypothesized to evaluate its toxicity. Thus, this study provides a strategy for the preparation of stable and efficient photocatalysts..

Multidimensional Engineering Induced Interfacial Polarization by in-Situ Confined Growth of MoS2 Nanosheets for Enhanced Microwave Absorption.

Interface design has enormous potential for the enhancement of interfacial polarization and microwave absorption properties. However, the construction of interfaces is always limited in components of a single dimension. Developing systematic strategies to customize multidimensional interfaces and fully utilize advantages of low-dimensional materials remains challenging. Two-dimensional transition metal dichalcogenides (TMDCs) have garnered significant attention owing to their distinctive electrical conductivity and exceptional interfacial effects. In this study, a series of hollow TMDCs@C fibers are synthesized via sacrificial template of CdS and confined growth of TMDCs embedded in the fibers. The complex permittivity of the hollow TMDCs@C fibers can be adjusted by tuning the content of CdS templates. Importantly, the multidimensional interfaces of the fibers contribute to elevating the microwave absorption performance. Among the hollow TMDCs@C fibers, the minimum reflection loss (RLmin) of the hollow MoS2@C fibers can reach -52.0dB at the thickness of 2.5mm, with a broad effective absorption bandwidth of 4.56GHz at 2.0mm. This work establishes an alternative approach for constructing multidimensional coupling interfaces and optimizing TMDCs as microwave absorption materials.

Linear-Organic-Ions In Situ-Intercalated MoS2 for Unveiling Capacitive Energy Storage Relies on the Chain Length.

Intercalating linear-organic-ions into the MoS2 interlayer is beneficial for optimizing electrons/ions' capacitive storage behavior. The chain length, as an important parameter of linear organic ions, can lead to differences in the dispersion, polarity, critical micelle concentration of organic ions, and steric hindrance to the growth of MoS2 nanosheets. Up until now, the relationship between chain length, synthesis of intercalated-MoS2, and capacitive energy storage has not been unveiled. Herein, we have designed an in situ-intercalation route that is simple, efficient, and high yield for inserting four types of linear organic ions into the interlayer of MoS2 to synthesize four types of in situ-intercalated MoS2 samples. After organic-ion intercalation, the expanded interlayer spacing achieved the introduction of intercalation-type pseudocapacitors, as confirmed by ex situ XRD. Improved extra capacitance is verified due to the enlarged ion storage space from a synergistic spatial effect in the broken-shell-hollow ball. Additionally, the generation of high-valent Mo (+5 and +6) and S-vacancies is beneficial for energy storage. More importantly, according to density functional theory (DFT) calculations, as the chain length increases, the number of negative adsorption sites and the total adsorption ability also increase, leading to significantly improved specific capacitance. This work will provide an archetype for the preparation of in situ-intercalated layered materials and unveil capacitive energy storage that relies on the organic-ion chain length.

Wood Ion Pumps Enabled by Light-Responsive MoS2-Decorated Nanocellulosic Channels.

Light-driven active ion transport discovered in nanomaterials (e.g., graphene, metal-organic framework, and MXene) implicates crucial applications in membrane-based technology and energy conversion systems. However, it remains a challenge to achieve bulk assembly. Herein, we employ the scalable wood as a framework for in situ growth of MoS2 nanosheets to facilitate light-responsive ion transport. Owing to the aligned and negatively charged wood nanochannels, the MoS2-decorated wood exhibits an excellent nanofluidic conductivity of 8.3 × 10-5 S cm-1 in 1 × 10-6 M KCl. Asymmetric light illumination creates the separation of electrons and holes in MoS2 nanosheets, enabling ions to move uphill against a wide range of concentration gradients. As a result, the MoS2-decorated wood can pump ions uphill against a 20-fold concentration gradient at a light intensity of 300 mW cm-2. When the illumination is applied to the opposite side, the osmotic current along the 20-fold concentration gradient can be enhanced to 75.1 nA, and the corresponding osmotic energy conversion power density increases to more than 12.6 times that of the nonilluminated state. Based on the light-responsive behaviors, we are extending the use of MoS2-decorated wood as the ionic elements for nanofluidic circuits, such as ion switches, ion diodes, and ion transistors. This work provides a facile and scalable strategy for fabricating light-controlled nanofluidic devices from biomass materials.

Single-Atom Iron Catalysts with Core-Shell Structure for Peroxymonosulfate Oxidation.

The chemical tolerance of ketoenamine covalent organic frameworks (COFs) is excellent; however, the tight crystal structure and low surface area limit their applications in the field of catalysis. In this work, a porous single-atom iron catalyst (FeSAC) with a core-shell structure and high surface area was synthesized by using Schiff base COF nanospheres as the core and ketoenamine COF nanosheets growth on the surfaces. Surface defects were created using sodium cyanoborohydride etching treatment to increase specific surface area. The dye degradation experiments by peroxymonosulfate (PMS) catalyzed by the FeSAC proved that methylene blue can be degraded with a degradation rate constant of 0.125 min-1 under the conditions of 0.1 g L-1 catalyst dosage and 0.05 g L-1 peroxymonosulfate. The FeSAC/PMS system effectively degrades various pollutants in the pH range of 4-10 with over 80% efficiency for four cycles and can be recovered by soaking in iron salt solution. Free radical quenching experiments confirmed that singlet oxygen and superoxide radicals are the main active species for catalysis.

Effects of Plasma Ions/Radicals on Kinetic Interactions in Nanowall Deposition: A Review

Recent advances in the growth of carbon nanowalls (CNWs) and vertical graphene nanosheets using various plasma‐enhanced chemical vapor deposition (PECVD) methods are reviewed in this article. Growth methods are classified into hot‐ and cold‐wall reactors equipped with diverse plasma generation systems, and their respective characteristics are summarized, with particular attention to the behavior of reactive species, such as ions and radicals, generated within the plasma. Recent progress in this research domain is outlined for each method, and an organized account of the chemical kinetic phenomena occurring within the plasma is provided. Finally, future perspectives are discussed. Fundamental data are obtained through real‐time in situ measurements of ions and radicals, and the construction of a database from these data offers microscopic insights that significantly enhance processing outcomes for macroscopically controlling the mechanical shapes and chemical properties of CNWs.

Protonated Z-scheme CdS-covalent organic framework heterojunction with highly efficient photocatalytic hydrogen evolution

The low efficiency of photocatalytic hydrogen production from water is mainly suffer from limited light absorption, charge separation and water delivery to the active centers. Herein, an inorganic–organic Z-scheme heterojunction (CdS-COF-Ni) is constructed by in-situ growth of CdS nanosheets on the porphyrin-based covalent organic framework with nickel ions (COF-Ni) in the porphyrin centers. A built-in electric field is formed at the interface, which accelerates the separation and transfer of photogenerated charges. Moreover, through the surface protonation treatment in ascorbic acid (AC) solution, the hydrophilicity of the obtained composite is obviously increased and facilitates the transport of water molecules to the photocatalytic centers. Under the synergistic effect of the interfacial interaction and surface protonation treatment, the photocatalytic hydrogen production rate is optimized to be 18.23 mmol h−1 g−1 without adding any cocatalysts, which is 21 times that of CdS. After a series of photoelectrochemical measurements, in situ X-ray photoelectron spectroscopy (XPS) analysis, and density functional theory (DFT) calculations, it is found that the photocatalytic charge transfer pathway conforms to the Z-scheme mechanism, which not only greatly accelerates the separation and transfer of photogenerated charges, but also retains a high reduction capacity for water splitting. This work offers a good strategy for constructing highly efficient organic–inorganic heterojunctions for water splitting.

Construction of polarized 2D/2D g-C3N4/BiOCl nanosheet dual piezoelectric Z-scheme heterojunction and its efficient charge separation mechanism

A multi-electric field synergistic strategy based on heterojunction construction and polarization engineering enhances carrier separation and migration, achieving excellent piezoelectric photocatalytic performance of g-C3N4 based materials. Here, through the in-situ growth of BiOCl nanosheets (BOCs) on g-C3N4 nanosheets (GCNs), a 2D/2D Z-scheme GCNs/BOCs heterojunction was successfully fabricated, and its outstanding piezo-photocatalytic property was demonstrated. Compared to individual BOCs and GCNs, the high degradation rate (97.64 %) of rhodamine B (RhB) can be achieved over the optimal composite (GCNs/BOCs-50) after 50 min irradiation. Inspiringly, the polarized GCNs/BOCs-50 composite degraded RhB almost completely within 30 min under the simultaneous light irradiation and ultrasound, which reduced the photocatalytic time by 40 %, and its k reached 0.1410 min−1 (12.59 and 2.48 times that of BOCs and GCNs). This work is of great significance for designing a novel heterojunction photocatalysts using polarized ferroelectric materials.

Precursor-Confined Chemical Vapor Deposition of 2D Single-Crystalline SexTe1-x Nanosheets for p-Type Transistors and Inverters.

Two-dimensional (2D) tellurium (Te) is emerging as a promising p-type candidate for constructing complementary metal-oxide-semiconductor (CMOS) architectures. However, its small bandgap leads to a high leakage current and a low on/off current ratio. Although alloying Te with selenium (Se) can tune its bandgap, thermally evaporated SexTe1-x thin films often suffer from grain boundaries and high-density defects. Herein, we introduce a precursor-confined chemical vapor deposition (CVD) method for synthesizing single-crystalline SexTe1-x alloy nanosheets. These nanosheets, with tunable compositions, are ideal for high-performance field-effect transistors (FETs) and 2D inverters. The preformation of Se-Te frameworks in our developed CVD method plays a critical role in the growth of SexTe1-x nanosheets with high crystallinity. Optimizing the Se composition resulted in a Se0.30Te0.70 nanosheet-based p-type FET with a large on/off current ratio of 4 × 105 and a room-temperature hole mobility of 120 cm2·V-1·s-1, being eight times higher than thermally evaporated SexTe1-x with similar composition and thickness. Moreover, we successfully fabricated an inverter based on p-type Se0.30Te0.70 and n-type MoS2 nanosheets, demonstrating a typical voltage transfer curve with a gain of 30 at an operation voltage of Vdd = 3 V.

P-N Heterojunction formation: Metal Sulfide@Metal Oxide Chemiresistor for ppb H2S Detection from Exhaled Breath and Food Spoilage at Flexible Room Temperature.

The development of a portable, low-cost sensor capable of accurately detecting H2S gas in exhaled human breath at room temperature is highly anticipated in the fields of human health assessment and food spoilage evaluation. However, achieving outstanding gas sensing performance and applicability for flexible room-temperature operation with parts per billion H2S gas sensors still poses technical challenges. To address this issue, this study involves the in situ growth of MoS2 nanosheets on the surface of In2O3 fibers to construct a p-n heterojunction. The In2O3@MoS2-2 sensor exhibits a high response of 460.61 to 50 ppm of H2S gas at room temperature, which is 19.5 times higher than that of the pure In2O3 sensor and 322.1 times higher than that of pure MoS2. The In2O3@MoS2-2 also demonstrates a minimum detection limit of 3 ppb and maintains a stable response to H2S gas even after being bent 50 times at a 60° angle. These exceptional gas sensing properties are attributed to the increase in oxygen vacancies and chemisorbed oxygen on In2O3@MoS2-2 nanofibers as well as the formation of the p-n heterojunction, which modulates the heterojunction barrier. Furthermore, in this study, we successfully applied the In2O3@MoS2-2 sensor for oral disease and detection of food spoilage conditions, thereby providing new design insights for the development of portable exhaled gas sensors and gas sensors for evaluating food spoilage conditions at room temperature.

New insights into chitosan-induced biomimetic mineralization of hierarchical spherical nesquehonite: Characterization, DFT calculations and construction mechanism

Recently, CO2 mineralization with magnesium salts is a cost-effective method for CO2 utilization and sequestration. The obtained hydrated magnesium carbonate can serve as high-value added functional materials. Inspired by biomineralization, nesquehonite (NSQ) was prepared via chitosan-induced mineralization of MgCl2-(NH4)2CO3, achieving indirect mineralization of CO2. The effects of chitosan (CTS) addition, reaction temperature, and reaction time on the phase composition and micromorphology of the products were systematically investigated. When the chitosan addition was 2%, the reaction temperature was 60℃, and the reaction time was 300 min, the obtained product was hierarchical spherical NSQ with an average diameter of 10 μm. The construction mechanism of the hierarchical spherical NSQ was elucidated. Zeta potential and 1H NMR analyses indicated the interaction of CTS with Mg2+, binding Mg2+ through –OH and –NH2 groups, thereby prolonging the nucleation and growth process of NSQ. FT-IR, XPS, TEM, and AFM analyses revealed that CTS induced directional growth of nanosheets by chemisorption on the crystal surface. Ultimately, through CTS bridging, the nanosheets aggregated and assembled into NSQ sphere. DFT calculations further indicated that CTS forms Mg-O and Mg-N bonds with Mg2+ and that there are Mg-O, Mg-N bonds and hydrogen bonding interactions between CTS and NSQ. This work provides new insights into the preparation of hierarchical NSQ via a biomimetic mineralization mechanism. Additionally, NSQ with a multiscale hierarchical structure has a promising future in the fields of adsorbents, templating agents, and drug carriers.