Recent advances in one-dimensional tubular composites with MoO₃-based micro/nanorods as templates

Abstract

Template-mediated strategies are a versatile and scalable approach for fabricating one-dimensional (1D) tubular composites, while molybdenum trioxide (MoO₃) micro/nanorods have emerged as promising templates for engineering hollow nanostructures. In this minireview, we systematically introduce recent advancements in a series of MoO₃-based micro/nanorods for guiding the formation of 1D tubular composites with different structural characteristics. We summarize the various rational design strategies, such as hard-templating and self-templating methodologies, as well as derivative strategies with organic polymer coating and functional oxide coating for MoO₃-derived 1D tubular composites. Notably, the architectures, structures, compositions, and morphologies of these composites are discussed for their applications in catalysis, protein adsorption, and enzyme-mimic reactions, among others. Finally, we critically evaluate the prospects, challenges, and opportunities for advancing MoO₃-derived 1D tubular nanostructures toward next-generation nanocatalytic and environmental remediation technologies.

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1. Introduction

One-dimensional (1D) hollow composites have attracted significant attention due to their high specific surface area, unique structures, and exposed active sites. The high specific surface area enhances mass transport, and the exposed active sites improve substrate accessibility. Thus, 1D hollow composites exhibit extensive applications with improved performance as a promising matrix for energy storage, catalysis, adsorption and sensing. However, direct preparation often shows low efficiency and yield. As an alternative, the template-engineering strategy especially becomes powerful and efficient for the preparation of 1D hollow composites. Thus, some materials with micro/nanorod structures are first prepared and then used as templates to guide the assembly of functional materials. According to special applications, the templates can be removed or retained. Therefore, the templates should be easily prepared as micro/nanorod structures and removed.

MoO₃ is easily prepared as a unique 1D micro/nanorod structure and shows great potential as a template for the fabrication of 1D hollow nanostructures.^1,2 However, the evolutionary pathway of MoO₃-templated synthesis underscores the continuous refinement of its one-dimensional morphology. Hard-templating strategies have often been hindered by two major challenges: the incomplete removal of the MoO₃ core and the consequent structural collapse of the deposited shell. These limitations have motivated the shift toward self-templating approaches, which utilize in situ chemical transformation of MoO₃ precursors to entirely circumvent the etching step and enable the synthesis of Mo-based derivative materials. Nevertheless, structural collapse and aggregation during conversion remain challenges. A pivotal advancement addressed this through surface engineering, where pre-formed rigid overlayers (e.g., polymers or covalent organic frameworks) act as structural scaffolds. These supports preserve the rod-like morphology throughout the transformation, thereby facilitating a strategic transition from mere morphological replication to synergistic structure and composition design.^3–12

MoO₃ micro/nanorods possess a layered structure and multiple valence states with abundant interactions as versatile templates for the integration of functional materials to obtain 1D hollow nanomaterials. Additionally, their high aspect ratio and stability enhance flexibility and accessibility for creating hollow structures with controllable dimensions and morphologies. Moreover, MoO₃ micro/nanorods are easily prepared in large quantities using simple hydrothermal or sol–gel strategies, making them cost-effective for the industrial-scale production of tubular nanostructures.^13,14 These attributes collectively position MoO₃ micro/nanorods as a versatile template for the rational design of hollow nanomaterials with tailored functionalities to improve the performance of integrated functional materials. Thus, the MoO₃ micro/nanorod-based template strategy offers several distinct advantages for engineering 1D hollow nanomaterials: (1) anisotropic morphology control: the inherent 1D rod-like structure of MoO₃ enables the as-prepared hollow nanotubes with high aspect ratios and uniform diameters, being critical for applications with directional mass/electron transport (e.g., catalysis and energy storage). (2) Facile template removal: the MoO₃ template can be selectively etched with mild basic solutions, leading to the formation of hollow architectures without residual template fragments. (3) Self-templating capability: MoO₃ is easily transferred to MoS₂, NiMoO₄, and MoO₂ through phase transformations after sulfidation, nickel-mediated hydrothermal reaction or reduction conditions, while the 1D micro-/nanostructures are retained. Thus, a series of MoO₃-based template materials are selected for improved performance. (4) Surface reactivity: the layered MoO₃ structure facilitates the conformal coating of polymers (e.g., PPy), carbon, or metal oxides, enabling precise control over shell thickness and composition. In addition to the aforementioned advantages, MoO₃ templates also offer the following several benefits compared to traditional templates like nanorods, SiO₂, carbon nanotubes, and metal oxide templates: (1) inherent 1D morphology: MoO₃ naturally forms layered orthorhombic structures that easily grow into nanorods without the need for shape-directing agents. This makes its synthesis far simpler than that relying on CNTs or SiO₂ templates. (2) Tunable architecture: the interlayer spacing of MoO₃ enables ion/molecule intercalation. This capability enables precise regulation of wall thickness and porosity, which is a feature not achievable with carbon nanotubes or metal oxide templates. (3) Intrinsic surface reactivity: owing to its Lewis acidic and redox-active surface, MoO₃ allows for direct polymerization or deposition of functional coatings. By comparison, inert templates, like CNTs or SiO₂, often require pre-functionalization.^15–20 Thus, a series of MoO₃-based micro/nanorods can be selected as templates to tune the composites, structures, and performance of 1D hollow nanomaterials. In combination with charge distribution, active site availability, structural design, morphological control, and surface functionalization, significant breakthroughs are expected in the activity, selectivity, and stability of various applications, as illustrated in Fig. 1.

Fig. 1 The preparation of 1D tubular composites using MoO₃ micro/nanorods as templates. MoO₃-based micro/nanorods are used for the preparation of 1D tubular composites with hard-templating and self-templating strategies with polymers, organic–inorganic species, CNTs, oxides and others as the matrices. The functions and merits of tubular materials are integrated.

The central focus of this minireview is to illustrate the intricate correlations of MoO₃ 1D tubular composite's structural parameters, compositional features and functional applications. By evaluating these structure–function relationships, we provide targeted optimization for specific catalytic reactions and adsorption processes. Finally, we propose a forward-looking perspective on integrating tubular nanostructures with multifunctional components to create adaptive platforms for enzyme-mimic reactions, adsorption capacities and energy storage.

2. Hard templating

2.1 Design and synthesis of a hard-templating strategy

The hard templating method presents a conceptually straightforward strategy for synthesizing hollow nanostructures.²¹ The hard templating process involves three sequential steps: (1) synthesis of MoO₃ templates with tailored shapes; (2) conformal coating/deposition of target materials via sol–gel chemistry, hydrothermal reactions, or electrochemical methods; and (3) selective removal of the MoO₃ core through chemical etching or thermal decomposition to yield hollow tubules.^22,23 Although the MoO₃ template did not constitute the final elemental composition of the material, it determined the final nanotube structure. Han et al. successfully synthesized a precisely structured tubular architecture composed of carbon-coated Fe₃O₄, characterized by a hierarchically porous design.²⁴ An efficient two-step method was developed by Hu et al. to synthesize hierarchical MoO₃/SnS₂ core–shell nanocables, where ultrathin SnS₂ nanosheets are vertically grown on MoO₃ nanobelts to form a heterointerface.²⁵ Yuan et al. fabricated hierarchical hollow FeCo-LDH@CoSx microtubes by sequentially depositing FeCo-LDH and ZIF-67 onto MoO₃ microrod templates, with subsequent sulfidation and template etching.²⁶

2.2 One-dimensional N-doped carbon nanotubes (NCNTs)

NCNTs have the advantage of high specific surface area, exceptional chemical stability, porous structure and rapid electron transfer kinetics.^27–32 The distinctive characteristic of NCNTs renders them an indispensable material for cutting-edge applications in advanced electrocatalysis, energy storage, and sensing technologies. By further enhancing the binding interactions between NCNTs and catalytic species, we can improve catalytic performance.^33–37

Our group designed a series of hierarchical NCNT architectures. For instance, Zhang et al. fabricated triple-walled M@N-doped carbon @M microtubes (M = Fe₃O₄, Cu/Cu₂O, MnO₂, and MoS₂), as shown in Fig. 2. Initially, they employed a one-pot oxidative polymerization approach to synthesize MoO₃@PPy composites. Subsequently, Fe₃O₄ NPs were uniformly distributed and deposited on both the internal and external surfaces of the NCNTs via a high-temperature thermal decomposition process.^38,39 Additionally, the PPy shell exhibits the capability to adsorb Fe³⁺ ions, which is attributed to the robust coordination interactions occurring between Fe³⁺ ions and the nitrogen atoms within the PPy structure.⁴⁰ For example, Fe₃O₄@NCMTs demonstrate structural superiority, and this superiority could potentially arise from void-confinement effects as well as optimized substrate access and electron transfer.⁴¹ The C@Fe₃O₄@C/Ni structure has the potential to enhance the dispersion and surface accessibility of Ni NPs. Notably, its inner and outermost nitrogen-doped porous graphitic carbon layers work in a synergistic manner. This structure not only improves mass transport kinetics and electronic conductivity but also offers robust protection to the Fe₃O₄ and Ni NPs.⁴² Furthermore, based on our previous studies, we accomplished precise control over the hierarchical porosity of 1D magnetic metal silicate microtubes.^43–45 Recently, Miao et al. conducted NCMTs@Fe₃O₄@SiO₂@C/Ni–Co–Cu,⁴⁶ and Zheng et al. developed a biosensing platform utilizing NCMTs@Fe₃O₄@Cusilicate, which achieves the ultrasensitive detection of carcinoembryonic antigen (CEA).^47,48 These composite materials contain uniformly dispersed metallic NPs embedded within carbon layers. Due to their hierarchical architecture, large specific surface area, and high metal nanoparticle density, these materials exhibit exceptional catalytic performance.

Fig. 2 (A) Schematic of the formation of the Fe₃O₄@N-doped carbon@Fe₃O₄ microtubes using a multi-step conversion route. (B–E) TEM images of the Fe₃O₄@N-doped carbon@Fe₃O₄ microtubes upon increasing the weight ratio between Fe(acac)₃ and the N-doped carbon microtubes from 0.5 : 1; 2 : 1; 4 : 1; and 10 : 1. (F) the X-ray diffraction patterns of the N-doped carbon microtubes (a) and Fe₃O₄@N-doped carbon@Fe₃O₄ microtubes using different ratios of Fe(acac)₃ to N-doped carbon microtubes: (b) 1 : 2, (c) 2 : 1, (d) 4 : 1 and (e) 10 : 1.

2.3 Organic–inorganic hybrid coating methods

MoO₃ micro/nanorods were coated with three distinct polymeric layers: organic polymers, metal–organic polymers, and inorganic–organic hybrid polymers. Organic polymer coatings effectively stabilize MoO₃'s unique 1D tubular structure, endow its surfaces with redox-active groups, and markedly enhance its electrical conductivity.^49–52 Subsequently, the MoO₃ cores underwent selective removal through thermal decomposition or etching processes. This operation enabled the successful construction of core–shell structures.^53–57 These hollow nanocomposites exhibit significantly larger surface areas, readily accessible active sites, and a diverse array of multiple functions. Owing to these characteristics, they demonstrate exceptional suitability for applications in catalysis, energy storage, and environmental remediation.^58–63

During our research, we successfully developed certain composites with organic–inorganic hybrid coatings, utilizing MoO₃ microrods as sacrificial templates. Through subsequent coating of PPy and the PDA-Ni²⁺ complex in an ammonia solution, PPy@PDA-Ni²⁺ microtubes were successfully synthesized. Following an annealing treatment, these microtubes were transformed into Ni NP-anchored N-doped carbon microtubes, which exhibited excellent performance in 4-NP reduction.⁶⁴

2.4 Functional oxide coating methods

The functional oxide coating strategy has the advantage of a hierarchically porous structure, extremely high specific surface area, hierarchical porosity, multi-component interfaces, and optimally adjusted carbon coating thickness. These features make it promising for applications in advanced nanocomposites, including energy conversion, catalysis, and sensing.^65–70 MoO₃ microrods also served as sacrificial templates, and FeOOH and PDA-Ni²⁺ served as Fe₃O₄ and C/Ni precursors, respectively. PDA-Ni²⁺ was polymerized on MoO₃@FeOOH core using an extended Stöber method, and ammonia-mediated etching removed the MoO₃ template and stabilized the PDA-Ni²⁺ coating at the same time.⁷¹ In another study, NiCo-LDH NSs were vertically grown on the MoO₃@FeOOH nanorods using a urea-assisted co-precipitation method, resulting in the formation of a hierarchical dual-layer architecture.⁷² After alkaline etching, the MoO₃ cores were dissolved, leaving hollow structures with FeOOH/NiCo-LDH shells.⁷³ The FeOOH intermediate not only enhances the adhesion between the MoO₃ template and the NiCo-LDH overlayer but also incorporates redox-active Fe into the overall structure. Simultaneously, the NiCo-LDH overlayer provides an abundant array of catalytic sites and establishes efficient ion-transport pathways. Subsequently, the MoO₃@FeOOH and MoO₃@NiCo-LDH nanorods were further modified with SiO₂ and PDA. MoO₃ microrods served as sacrificial templates, and the extended Stöber method achieved the sequential deposition of SiO₂ and PDA-Ni²⁺ layers and enhanced the dispersibility and density of the Ni nanoparticles. As shown in Fig. 3, the Fe₃O₄@SiO₂@C/Ni nanocomposite demonstrated exceptional catalytic performance in 4-NP and exhibited remarkably selective adsorption capabilities toward His-rich proteins. The test results demonstrate that the superior catalytic performance and stability of the material originate from its well-defined porous structure, abundant active sites, and strong magnetic properties.⁷⁴

Fig. 3 (A) A schematic of the fabrication procedures of the sandwich-like C@Fe₃O₄@C/Ni microtubes; (B) the UV-vis absorption spectra evaluate the catalytic ability of the as-prepared C@Fe₃O₄@C/Ni microtubes: (a and b) illustration of the 4-NP reduction; (c) successive reduction of 4-NP using C@Fe₃O₄@C/Ni-500 as a catalyst; (d) C_t/C₀ and ln(C_t/C₀) versus reaction time for the reduction of 4-NP over C@Fe₃O₄@C/Ni-500; (e) successive reduction of 4-NP using C@Fe₃O₄@C/Ni-700 as a catalyst; and (f) C_t/C₀ and ln(C_t/C₀) versus reaction time for the reduction of 4-NP over C@Fe₃O₄@C/Ni-700; SEM and TEM images of C@Fe₃O₄@C/Ni-500 (C and D) and PPy@FeOOH@RF-Ni²⁺(E and F).

3. Self-templating strategy

3.1 Design and synthesis of self-templating

Unlike hard-templating methods, self-templating synthesis guides the formation of the nanostructure's shape and contributes to the final material composition. From a synthetic perspective, MoO₃ templates are transformed into hierarchical hollow tubular frameworks composed of Mo-based compounds.^75–77

Kim et al. reported an innovative approach, employing a two-step hydrothermal synthesis technique to successfully achieve a morphological transformation from MoO₃ nanorods to NiMoO₄ nanotubes.⁷⁸ A self-templating approach was employed by Adhikari et al. to fabricate hollow nanostructured molybdenum trioxide encapsulated within a PPy shell.⁷⁹ Furthermore, Tang et al. synthesized a novel MoS₂/SnS@C hollow nanotube using a straightforward solvothermal approach. They found that this unique hollow nanotube not only reinforces the structural stability of the material but also offers an efficient and spacious pathway for facilitating sodium-ion migration.⁸⁰ Chen et al. proposed a metal-cation-directed self-assembly method to fabricate hierarchical hollow MoS₂ nanotubes. Metal cations induce substantial 1T-phase MoS₂ formation, offering a practical way to create high-1T-content hollow MoS₂ nanostructures.⁸¹ Wang et al. utilized FeOOH/NiMoO₄@PDA as precursors, and NCMTs were embedded with FeNi₃ and MoO₂ NPs. The NCMTs@MoO₂/FeNi₃ composite displays outstanding uniformity and possesses a well-defined hierarchical hollow architecture.⁸² The synthesis of NiMoO₄@FeOOH/NiMoO₄@NiMoO₄ and FeOOH/(NiCo)MoO₄ demonstrates the effectiveness of combining structural design, electronic tuning, and computational modeling. This multi-method approach enhances electrochemical performance and material stability, highlighting its potential for advanced energy technologies.^83,84 He et al. successfully developed hierarchical TiO₂@MoS₂ hollow microtubes through a combination of hydrothermal, sol–gel, and sulfidation processes. TiO₂ served as an excellent solid support, significantly inhibiting the aggregation of MoS₂ NSs. Notably, sulfidation hydrothermal treatment converts the amorphous phase of TiO₂ microtubes into mesoporous anatase TiO₂ microtubes. This hollow architecture exhibits synergistic integration, with interfacial adsorption effects occurring between MoS₂ NSs and mesoporous TiO₂. Through experimental data, the TiO₂@MoS₂ microtubes show the highest removal efficiency (81.31%) for aqueous RhB, significantly outperforming pure TiO₂ microtubes (3.90%) or pure MoS₂ nanosheets (43.77%). This enhancement stems from the synergistic interaction between TiO₂ and MoS₂, which boosts photocatalytic degradation. The findings offer insights for designing efficient photocatalysts for pollutant removal.⁸⁵

Decorating organic molecules and organic–inorganic molecules via a polymer-confined sulfidation strategy on the surface of MoS₂ can improve the performance.⁸⁶ We developed a hydrothermal method to yield a series of tubular MoS₂-based nanocomposites based on MoO₃@PANI/PPy/APTES/COF microcables.^87–90 Decorating MoS₂ NSs with organic matrices has exhibited markedly enhanced performance in sensing, photoelectron catalysis, energy storage, and lubrication.^91–93 As a representative of organic conductive polymers, PANI demonstrates outstanding structural stability.^94,95 Li et al. successfully synthesized hierarchical PANI microtubes, which were subsequently enveloped by MoS₂ NSs to form a core–shell heterostructure. Then, the outer MoS₂ shell underwent further modification by being doped with Fe₃O₄ NPs and noble metal NPs. This meticulous modification facilitated the establishment of a highly versatile multifunctional heterostructure interface, exhibiting synergistic properties for advanced applications.⁹⁶ In another study, through a dissolution-regrowth mechanism, the MoO₃@PPy microtubes were transformed into hollow PPy@MoS₂ sheet-like nanostructures.⁹⁷ This architecture offers dual advantages: (1) the sheet-like morphology of MoS₂ significantly enhances electrical conductivity while effectively minimizing the agglomeration of nanosheets. (2) The conductive PPy core serves as a facilitator for the in situ reduction and uniform dispersion of Ag, Au, or Pd NPs on the MoS₂ surface, as shown in Fig. 4. For example, MoO₃@FeOOH as a precursor enables the targeted and selective deposition of Fe-doped MoS₂ nanosheets onto conductive PPy microtubes.⁹⁸

Fig. 4 (A) Schematic synthesis of PPy@MoS₂@Au/Ag/Pd composites. (B) Schematic of the synthetic procedure of Ag₂S/MoS₂@PPy nanotubes. SEM and TEM images of (C and D) MoO_3−x, (E and F) MoO₃@Ag nanorods, (G and H) MoO₃@Ag@PPy nanorods, and (I and J) Ag₂S/MoS₂@PPy nanotubes.

Leveraging this platform, as shown in Fig. 5, Lu et al. developed programmable metal-nanoparticle-supported nanozymes (MNNs) on PPy@MoS₂ matrices. These metal NPs can modulate the catalytic properties of PPy@MoS₂ nanocomposites, enabling them to act as an ideal alternative to DNA-AuNP conjugates in sensor arrays. The sensor array demonstrated outstanding discriminatory capability, even when subjected to analysis within the highly complex matrix of physiological fluids. This exceptional performance enabled precise and accurate differentiation among blind samples, serum proteins, heat-denatured proteins, and clinical cancer biomarkers.⁹⁹

Fig. 5 (A) Working principle of the mammalian olfactory system; (B) modulation of the catalytic oxidation of metal-NP-supported nanozyme (MNN) by different proteins; (C) colorimetric sensor arrays for pattern recognition of proteins and oral bacteria based on the MNNs; (D) color change patterns of TMB oxidation catalyzed by the MNN sensor array in the presence of different proteins; and (E) colorimetric response patterns (A/A₀) at 652 nm against different proteins. The error bar shows the standard deviation of five independent measurements. (F) Canonical score plots for the first two factors of colorimetric response patterns obtained from PCA with 95% confidence ellipses (n = 5). (G) Heat map derived from colorimetric response patterns for 11 proteins. (H) Hierarchical cluster analysis (HCA) plot for the discrimination of 11 proteins. The concentration of each protein was 250 nM.

Besides, APTES establishes covalent linkages with the MoO₃ surface via its –Si–OH functional group. This covalent interaction augments the intrinsic properties of the resulting nanocomposites and significantly enhances their dispersion stability when suspended in polar solvents.¹⁰⁰ Using MoO₃ microrods as self-sacrificial templates, we crafted a tubular structure through an APTES-modified synthesis, yielding a precisely structured APTES@MoS₂ tubular composite.¹⁰¹ Furthermore, by finely adjusting the interfacial interactions at the COF/MoS₂ heterojunction, we can strategically optimize the reaction pathways, thereby enhancing the catalytic performance.^102,103 Guo et al. fabricated hierarchical COFs@MoS₂-Pd hybrid architectures, wherein the vertically oriented MoS₂ NSs provide a wealth of active sites and facilitate the dense and uniform distribution of Pd NPs, which exhibited excellent performance in the reduction of 4-NP and enzyme-like catalysis.¹⁰⁴

4. Conclusion and outlook

This minireview summarizes recent advances for 1D tubular composites with MoO₃-based micro/nanorods as templates. The integration of MoO₃-derived templates with functional components, including carbonaceous matrices, metal oxides, and conductive polymers, yields a variety of tubular nanocomposites. These nanocomposites exhibit distinct structural advantages and superior electronic/catalytic properties. Despite having achieved significant progress in template-directed synthesis, 1D hollow nanostructures continue to face critical challenges using MoO₃-based micro/nanorods as templates. Looking ahead, several promising research directions are poised to shape the future of this field. First, there is a growing impetus toward the design of multi-component and multi-shelled hollow structures. Future work will likely focus on the sequential deposition of more than two functional layers (e.g., ternary metal sulfides and their hybrids with conductive polymers) onto the MoO₃ template, creating complex tubular structures with intimately coupled interfaces for enhanced synergistic effects. Second, the precision control over the microstructure of the deposited shells represents a critical frontier. Moving beyond simple coating, strategies to engineer defects, crystallinity, and porosity at the atomic or nanoscale within the shell walls will be crucial for maximizing the density and accessibility of active sites. This includes developing milder etching processes that preserve the integrity of these delicate nanostructures. Third, expanding the functional repertoire of these materials beyond electrocatalysis and energy storage is a key trend. Their application in areas such as sensors, nanoreactors, and biomedical devices (e.g., for drug delivery or theranostics) remains largely unexplored. Finally, bridging the gap between fundamental studies and practical applications requires a stronger emphasis on scalability and stability. Future efforts must address the challenges of large-scale, reproducible synthesis and rigorously evaluate the long-term operational stability of these 1D hollow composites under harsh conditions. In conclusion, the future of MoO₃-templated 1D hollow nanomaterials lies in moving from structural complexity to functional intelligibility, paving the way for their deployment in next-generation technologies.

Conflicts of interest

The authors declare no competing financial interest.

Data availability

This review paper does not contain original data. All the figures were cited from the literature after permission.

Acknowledgements

This study was supported by the National Natural Science Foundation of China (Grants 22374096 and 22174077) and the Class III Peak Discipline of Shanghai-Materials Science and Engineering (High-Energy Beam Intelligent Processing and Green Manufacturing).

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