
A niobium (Nb)-doped micro arc oxidized coating (MAO) was fabricated on a titanium substrate, and microwave hydrothermal (MH) post-treatment was applied to regulate the microstructure of the coating, aiming to enhance bone-implant osseointegration and antibacterial performance. The experimental results showed that the as-prepared MAO coating was composed of nanocrystalline TiO2 and a large amount of amorphous phase containing oxygen, Nb, calcium, phosphorus, and other bioactive elements. After MH treatment, short rod-like hydroxyapatite (HA) crystals were uniformly formed on the porous surface of the Nb-doped MAO coating, resulting in a well-ordered crystalline structure with tight interfacial bonding between the HA crystals and the MAO coating. The incorporation of Nb and MH post-treatment synergistically optimized the surface microtopography and chemical composition of the MAO coating, which markedly enhanced in vitro bioactivity, in vivo osseointegration, and antibacterial properties.
Alkaline ferrocyanide-polysulfide redox flow batteries (Fe/S RFBs) have emerged as a promising candidate for grid-scale energy storage, primarily owing to their low raw material costs, intrinsic operational safety, and the inherent decoupling of power and energy in their design. Yet the intrinsically sluggish S22-/S2- chemistry restricts their power output and cycling durability. To tackle this, we developed a copper sulfide (CuS) and waste-asphalt-derived carbon co-modified carbon felt electrode (CuS-WA/CF), where waste-asphalt pyrolytic carbon serves as an interlayer to guide uniform copper electrodeposition. Subsequently, sulfidation converts the copper into well-dispersed CuS nanoparticles. This rational design increases the specific surface area by approximately 8.4-fold (from 9.55 to 80.46 m2 g-1) and markedly boosts electrochemical activity and conductivity. As a result, the assembled Fe/S RFB with CuS-WA/CF as the anode delivers a peak power density of 259.2 mW cm-2, which is 61.4% higher than the pristine-CF counterpart. At 40 mA cm-2, the cell maintained an average energy efficiency (EE) of 77.7% across 10,000 constant-current charge-discharge cycles. In a separate test using a higher-concentration ferrocyanide catholyte and excess anolyte, the cell delivered an average EE of 84.0% across 25,000 capacity-limited cycles. Beyond the performance gains, this work turns waste asphalt into a functional carbon source, offering a low-cost, scalable route toward the practical deployment of Fe/S RFBs for renewable integration.
Lightweight electromagnetic wave absorption materials with integrated multifunctionality are highly desirable for advanced civilian and military applications operating in complex environments. Herein, gradient microcellular flaky carbonyl iron powder (FCIP)/graphene (GP)/styrene-ethylene-butylene-styrene block copolymer (SEBS) materials are constructed via a one-step supercritical N2 foaming strategy by precisely regulating foaming parameters and cell size, thereby generating a gradient microcellular architecture along the thickness direction. This singular gradient structure effectively alleviates the impedance mismatch while simultaneously enhancing electromagnetic absorption through multiple loss mechanisms, including dielectric loss, magnetic loss, and multiple reflection and scattering. As a result, the gradient microcellular FCIP/GP/SEBS materials exhibit markedly improved microwave absorption (MA) performance relative to their uniform counterpart, achieving a reflection loss of -67.34 dB at 2.21 mm and an effective absorption bandwidth of 9.40 GHz at 1.99 mm, nearly covering the entire X and Ku bands. In addition, radar cross-section simulations on a plate and an F-35 fighter model confirm the excellent radar stealth capability of the gradient microcellular materials. Besides, the materials also exhibit favorable mechanical performance, excellent hydrophobicity, and stable photothermal and magnetothermal conversion, endowing them with thermal management and multi-field-responsive functionalities. This work provides a facile and scalable strategy for designing lightweight, broadband, and multifunctional MA materials with significant application potential for stealth protection, energy conversion, and service in harsh environments.
Magnetic materials dominated by shape anisotropy constitute an indispensable category of functional materials in scientific research and industrial applications. Beyond the switching field of the phases (nanowires) themselves, long-range magnetostatic interactions exert a fundamental influence on their magnetization mechanisms and modulate their overall performance. This study comprehensively investigates the role of magnetostatic interactions in the magnetization reversal process of nanowire arrays. To achieve this, the in situ horizontal magnetic field was observed using Lorentz transmission electron microscopy to investigate the magnetization reversal behavior of nanowire arrays. For the first time, the clear and precise microstructures of nanowires and the corresponding magnetization curves of target microscopic regions were acquired. In addition, the significance of magnetostatic interactions was clarified via combination with theoretical analyses. First-order reversal curve analysis, Henkel curve analysis of the macroscopic bulk material, and micromagnetic simulations were conducted to further investigate these interactions. The experimental and theoretical results show that modulating the strength of these interactions via the structural regulation of the phases (nanowires) facilitates the achievement of magnetic materials with tailored properties.
The occlusion of sorption sites during gradual electrochemical degradation is widely implicated in the capacitance fade of carbon-based supercapacitors, yet how pore architecture influences the tolerance of electrodes to pore blocking remains insufficiently studied. This work demonstrates that pore interconnectivity plays a key role in determining the tolerance of carbon electrodes to site occlusion. Alongside electrochemical tests, structural characterization of conventional activated carbons revealed how their narrow micropores are susceptible to accessibility loss while under potentiostatic operation, thus suffering rapid capacitance losses and equivalent series resistance (ESR) increments. In contrast, a carbon developed with a well-interconnected micro-mesoporous network demonstrated up to 14-fold longer lifetime under identical conditions. Critically, this improved durability translated to an 11-fold increase in cumulative energy delivered prior to End-of-Life of the device, as compared to carbons whose structures are initially optimized for maximizing capacitance. Further post-mortem analyses indicated that carbons with improved pore interconnectivity can tolerate a greater buildup of pore-blocking by-products before reaching capacitive failure, thus showing how pore network architecture mitigates or exacerbates the progressive occlusion of ion-accessible regions. We propose that highly interconnected pore structures feature alternative pathways that maintain the accessibility of sorption sites under constant operation. These findings establish pore interconnectivity as a key principle for extending the durability of supercapacitors under demanding voltage and temperature conditions.
To overcome the strength bottleneck of CoCrNi medium-entropy alloys (MEAs), this work systematically investigates the influence of Ti and Al addition strategies and ultrasonic impact treatment (UIT) on CoCrNi MEAs. Results indicate that the addition of TiAl master alloy promotes uniform dispersion of Ti-Al-O composite precipitates with a core-shell heterostructure, achieving synergistic enhancement of strength and plasticity. The alloy exhibits a yield strength (YS) of 589.1 MPa, an ultimate tensile strength of 973.5 MPa, and elongation of 34.4%. Further application of UIT refines the grain structure, induces high-density dislocations and stacking faults, and optimizes precipitate morphology. As a result, YS is enhanced to 692.7 MPa at 298 K and 997.7 MPa at 77 K, improvements of 17.6% and 40.6% compared to the as-deposited alloy. However, this strengthening is accompanied by a reduction in elongation, reflecting a typical strength-ductility trade-off. Despite the reduced ductility, UIT-treated alloy exhibits excellent strength at 77 K, highlighting its potential for cryogenic engineering applications where high strength is prioritized. Molecular dynamics simulations reveal the dynamic evolution of dislocation nucleation and stacking faults under impact loading. Quantitative analysis based on load-unload-reload testing indicates that heterogeneous deformation-induced strengthening provides a dominant contribution to the overall flow stress. The microstructural origin of this strengthening effect stems from the long-range stress fields and short-range obstruction effects arising from high-density dislocations, nanoprecipitates, and stacking faults introduced by UIT. These features continuously impede dislocation motion, thereby significantly enhancing deformation resistance.
High-resolution transmission electron microscopy (HRTEM) is indispensable for atomic-scale characterization yet fundamentally limited by the inherent phase loss in conventional detectors including CCD. To overcome this barrier, we propose Wave-Reconstruction Generative Adversarial Networks (WRGAN) that directly predict wave function amplitude and phase from single HRTEM images. Our physics-guided framework employs a Unet++ generator within a Generative Adversarial Networks (GAN) architecture via defining a physics-guided consistency loss. A key advantage is that WRGAN, trained solely on simulated data, demonstrates robust performance when directly applied to experimental images. Validation on experimental Nb8W9O47 image shows predicted amplitudes and phases closely match the groundtruth wave functions. Significantly, WRGAN successfully resolves upper and lower surface projections in noisy single-wall carbon nanotube (SWCNT) images, enabling near-atomic-resolution 3D reconstruction.
Artificial olfaction, inspired by biological sensory systems, offers new opportunities in environmental, industrial, and healthcare applications. Semiconducting metal oxide based chemoresistive gas sensors provide a scalable and core interface for chemical detection and therefore constitute the most extensively explored front end for artificial olfactory systems. Nevertheless, conventional chemoresistive sensing that relies on surface charge transfer remains constrained by incomplete response and recovery, humidity interference, cross selectivity, and strong temperature dependence. This review surveys material- and device-level strategies developed to address these bottlenecks, with an emphasis on nanostructuring approaches that improve gas accessibility and reaction kinetics. Moving beyond device-level performance, the review further situates oxide-based gas sensing within a hierarchical neuromorphic olfactory framework. In biological systems, chemical information is represented by distributed activation patterns and temporal dynamics that extend beyond individual receptor responses. Within this broader context, emerging oxide-based transduction concepts that extend conventional chemoresistive operation are also discussed. Recent artificial olfactory system studies have begun to explore alternative oxide-based transduction mechanisms that extend beyond conventional chemoresistive operation. Among these emerging approaches, chemo-memristive responses based on vacancy-mediated ion redox processes are briefly discussed as one possible pathway toward more tightly coupled sensing and signal encoding at the device level. Such developments reflect ongoing efforts to more closely couple sensing and signal processing at the device level. By integrating insights from nanostructured oxide sensors and neuromorphic encoding principles, this review outlines conceptual pathways toward artificial olfactory systems that extend beyond standalone gas detection toward more integrated sensory information processing architectures.
Ultrafast transmission electron microscopy (UTEM) is an advanced experimental technique that integrates a femtosecond (fs) laser with transmission electron microscopy to capture material dynamic processes at exceptionally high spatiotemporal resolution. This review aims to provide an overview on the recent progresses on UTEM from technical principles, instrument developments to scientific applications and future prospects. The fundamental operation principle of UTEM involves exciting the sample with a pump laser/electric pulse, followed by probing with a time-delayed electron pulse. By precisely varying the delay time between the pump and probe pulses, electron imaging, diffraction or spectroscopy at fs-nanometer/atomic scale can be achieved. Based on these capabilities, these advances have recently culminated in techniques such as five-dimensional scanning transmission electron microscopy and Attosecond electron microscopy, which push the boundaries toward quantitative strain mapping and sub-cycle dynamics. UTEM has demonstrated significant applications in the study of microscopic dynamics in correlated materials, semiconductors, catalysts, nanophotonics, etc. It enables direct visualization of fundamental dynamic processes such as carrier relaxation, lattice vibrations, phase transitions, near-field evolution and magnetic domain switching, etc., thereby deepening the understanding of non-equilibrium states and providing critical insights for the design of novel functional devices. With ongoing advancements in fs electron sources and high-sensitivity electron detectors, the temporal resolution and detection sensitivity of UTEM continue to improve, highlighting its substantial potential in nanometer/atomic-scale ultrafast science. Future technique developments are expected to drive major breakthroughs in condensed matter physics, materials science, chemical reactions and even biological structure dynamics, offering a powerful tool for exploring the ultrafast microscopic world.
This study overcomes the long-standing strength-ductility trade-off in titanium alloy welding and additive manufacturing by introducing a novel laser-manufactured wire-powder synchronous feeding strategy incorporating oxygen-iron (O-Fe) microalloying. Through controlled experiments and multiscale characterization, the mechanism by which trace O-Fe additions regulate weld microstructure and mechanical properties is elucidated. The results show that O-Fe microalloying particles modify the growth conditions of acicular alpha/alpha ', reducing its aspect ratio and alleviating stress concentration at alpha/(3 phase boundaries. The microalloying elements substantially refine the grains during solidification through solute redistribution and a pronounced increase in undercooling. Quantitative analyses demonstrate that O-Fe microalloying reduces columnar grain width by 64.8%, modifies the aspect ratio of acicular alpha/alpha ' through solute redistribution with a 20.3% increase in minor axis and a 40.4% decrease in major axis, and achieves 63.9% grain refinement through elevated alpha/(3 interfacial energy and promoted heterogeneous nucleation. The optimized Ti-6Al-4V-0.5O-2.3Fe alloy exhibits exceptional mechanical performance, with a tensile strength of 1,266.6 MPa representing a 41.3% improvement and an elongation of 15.5% indicating an 80.2% enhancement, demonstrating great potential for high-performance industrial applications.
Ammonia (NH3) plays a crucial role in global agriculture and the development of emerging hydrogen energy systems. However, developing highly efficient catalysts for NH3 synthesis under mild conditions remains a significant challenge due to kinetic and thermodynamic limitations. In this study, we report a Ru/CeO2 catalyst synthesized using a metal-organic framework (MOF)-derived strategy, which allows for simultaneous control over the morphology of CeO2 (nanorod shaped), the concentration of oxygen vacancies, and the dispersion of Ru. The optimized catalyst containing 0.5 wt.% Ru delivered an impressive NH3 synthesis rate of 4,665 mu mol gcat-1 h-1 at 400 degrees C and 50 bar, while maintaining excellent stability for 45 h of continuous operation. In addition, it achieved a high NH3 conversion of 93% at 550 degrees C and 1 bar. Notably, its performance surpasses that of conventional Ru-based catalysts by nearly twofold when normalized to the Ru loading. Comprehensive characterizations, including in situ X-ray photoelectron spectroscopy, Raman spectroscopy, and scanning transmission electron microscopy, reveal the formation of abundant oxygen vacancies, sub-nanometer Ru clusters, and strong metal support interaction. These factors collectively enhance the activation of N2 and its hydrogenation. This study highlights the effectiveness of MOF-templated defect engineering in developing robust Ru/CeO2 catalysts and provides valuable insights into structure-performance relationships. The dual functionality in both NH3 synthesis and decomposition highlights the potential of this approach for energy-efficient NH3-based energy systems.
Within ferroelastic domain architectures, a -domains typically nucleate between the c -domain matrix to accommodate lattice mismatch through various configurations. The domain switching behavior is generally coupled with c -domain reversal and occurs irreversibly as a secondary effect, rather than as an independently controlled phenomenon. This inherent coupling has hindered efforts to dynamically manipulate a -domain configurations, despite their significant potential in domain engineering. Here, we demonstrated the selective and reversible switching of a -domain in epitaxial PbTiO3/SrRuO3 heterostructures. To this end, we applied the sub-coercive field while localizing structural perturbations, by which a -domains are excited and then can be switched. Piezoresponse force microscopy measurements and thermodynamic modeling revealed that these metastable a -domain states access lower-energy elastic pathways. Our results challenge the conventional view of a -domains as passive components and open new opportunities for designing reconfigurable ferroelastic domain architectures.
The development of high-performance self-recoverable near-infrared (NIR) mechanoluminescent materials is crucial for advancing applications. In this work, we presented a self-recoverable NIR mechanoluminescent material, platelike SrAl12O19, through singly doped with Cr3+ and co-doped with lanthanide ions (Nd3+, Yb3+, Er3+) in one step. By modulating the Cr3+ doping concentration, we achieved precise control over the mechanoluminescence (ML) intensity as well as the spectral tunability between characteristic R-line emission (~ 690 nm) and the broadband emission (750-950 nm). Moreover, energy transfer from Cr3+ to lanthanide ions enables multispectral ML emission extending into the NIR-II window (1,000-1,700 nm). The resultant material exhibits excellent ML self-recoverability and high chemical stability. The co-doped system was demonstrated with great potential in dynamic stress visualization, naked-eye-invisible information encryption and special identification under challenging conditions (e.g., underwater). We further demonstrated practical applications by fabricating dual-mode flexible NIR mechanoluminescent paper sheets and sprayable coatings. This work contributes to the advancement of new NIR mechanoluminescent materials with unique morphological features for various scenarios, including the advancement of intelligent sensing and multi-level anti-counterfeiting technologies.
Lithium niobate (LiNbO3) is a key material in photonics and optoelectronics, valued for its ferroelectric, electro-optic, and nonlinear optical properties. Despite its high Curie temperature and significant spontaneous polarization, which are advantageous for light modulation and frequency conversion, undoped LiNbO3 suffers from intrinsically weak luminescence, thereby restricting its application in light-emitting devices. Doping with rare earth ions such as erbium (Er3+), neodymium (Nd3+), and praseodymium (Pr3+) significantly enhances its luminescent properties by introducing efficient photon-emitting energy levels. This review provides a comprehensive overview of the luminescent properties of pure and doped LiNbO3, with a particular focus on doping and co-doping strategies using rare earth and transition-metal ions to enhance their photoluminescence efficiency, thermal stability, and spectral tunability. The roles of dopant site occupancy, defect engineering, and charge compensation mechanisms are discussed in detail. Co-doping approaches are highlighted as promising routes to synergistically tailor emission characteristics and mitigate concentration quenching. Furthermore, the review explores recent advances in LiNbO3-based luminescent devices, including waveguide-integrated photonic components, resonators, and thin films. Finally, future challenges and perspectives are outlined for the rational design of high-performance LiNbO3-based luminescent materials in next-generation photonic technologies.
Classical constitutive models explicitly couple macroscopic mechanical responses with underlying microstructural evolution, which is crucial for capturing complex deformation mechanisms across varying strain rates. However, current deep learning (DL) constitutive models predominantly focus on macroscopic stress-strain mapping, often neglecting these critical microstructural transitions. To bridge this gap, this work proposes a mechanics-informed deep learning constitutive model (MIDLCM) that integrates gated recurrent units and multi-head attention with a mechanics-informed layer and a mechanics-informed loss, enabling simultaneous prediction of stress response and microstructural descriptors. Trained on a CrFeNi FCC alloy dataset spanning strain rates from 10-4 to 5,000 s-1, MIDLCM accurately reproduces strain-rate-dependent stress-strain behavior and captures the associated evolution of dislocation density and twin volume fraction. Crucially, the model successfully represents the distinct dislocation accumulation regimes and the dynamic transition of plasticity mechanisms - from dislocation-dominated to twinning-assisted - across extreme dynamic loading, consistent with experimental trends and crystal-plasticity-based references. Ablation studies show that attention-based temporal encoding and mechanics-informed constraints contribute complementary improvements while preserving inference efficiency. By explicitly tracking these internal state variables, the proposed framework provides a mechanism-level interpretable and computationally efficient microstructure-mechanics coupled alternative for rate-dependent constitutive modeling and is readily extendable to other alloy systems and loading paths.
Pyrochlore-type oxides are considered potential oxide-ion conductors due to their high concentration of oxygen vacancies in the unit cell. In this work, the pyrochlore-type Ca1.46Ti1.38Nb1.11O7 was synthesized and its crystal structure was characterized by Rietveld refinement. A high oxygen vacancy concentration in the material was confirmed by thermogravimetry (TG) and X-ray photoelectron spectroscopy (XPS). TG, XPS, and electron paramagnetic resonance collectively demonstrated the change in oxygen vacancy concentration of the material following atmosphere switching. The electrical properties of Ca1.46Ti1.38Nb1.11O7 under different atmospheres were characterized by electrochemical impedance spectroscopy. The conductivity of Ca1.46Ti1.38Nb1.11O7 was 4.20 × 10-2 S cm-1 in 5% H2/Ar, 9.22 × 10-3 S cm-1 in Ar and 2.92 × 10-5 S cm-1 in air at 900 °C. Bond valence site energy calculations indicated that oxide ions diffuse three-dimensionally in Ca1.46Ti1.38Nb1.11O7. Ca1.46Ti1.38Nb1.11O7 is a promising solid electrolyte for oxygen sensors. This work investigates the structure-property relationship between oxygen vacancies and conductivity in pyrochlore-type oxides.
The polytetrafluoroethylene (PTFE) binder-based roll-to-roll dry coating process has emerged as a promising alternative to conventional slurry-based methods for fabricating thick electrodes in high-energy-density lithium-ion batteries (LIBs). However, applying nano-sized lithium iron phosphate (LiFePO4, LFP) to this process remains challenging, as the high specific surface area of nano-sized LFP leads to the formation of short and thin PTFE fiber network that cannot ensure the mechanical integrity of dry cathode at low PTFE binder content. Consequently, the nano-sized LFP dry cathode suffers from poor flexibility and mechanical brittleness, limiting its applicability in roll-to-roll processing. In this study, we investigated the fibrillization behavior of PTFE binders depending on the particle size of LFP, to elucidate the origin of mechanical degradation in nano-sized LFP dry cathodes. Our results revealed that nano-sized LFP facilitates excessive PTFE fibrillization, generating fragile and weak networks with short and long PTFE fibers, leading to the mechanical degradation of nano-sized LFP dry cathodes. To address this issue, we introduced a two-step extrusion process that promotes the formation of thick and long PTFE fiber networks within nano-sized LFP dry cathodes. This strategy enabled the fabrication of flexible and mechanically robust nano-sized LFP cathode film with only 2 wt% PTFE binder. The developed LFP dry cathodes exhibited excellent compatibility with thick electrode designs and achieved high areal capacities (7 mAh cm-2, 2.7 g/cc), offering a scalable solution for next-generation LFP-based LIBs.
Overcoming the strength-ductility trade-off remains a challenge for both traditional and emerging high-strength steels. The unique thermal history during additive manufacturing (AM) of metals and alloys includes cellular solute enrichment of alloying elements, enabling the formation of metastable austenite with a cellular morphology after intercritical (alpha + gamma) annealing. Intercritical heat treatment reconstructs the trace retained austenite in the as-printed microstructure, together with reverted austenite from the martensitic matrix, into an interconnected cellular austenite network (similar to 40 vol.%). Yet solute-gradient partitioning can over-stabilize this cellular austenite, suppressing transformation-induced plasticity (TRIP) and work hardening under room-temperature tensile straining and making its stability difficult to tune using conventional heat-treatment schedules. Here, we effectively tune the thermal stability of cellular austenite in laser powder bed fusion (L-PBF) 18Ni300 maraging steel through a multi-step intercritical annealing strategy, so that TRIP can be readily activated during room-temperature tensile loading. Serial ex-situ electron backscatter diffraction (EBSD)/X-ray diffraction (XRD) measurements at comparable locations indicated a substantially larger austenite-to-martensite (gamma -> alpha') transformation (41.5% -> 22.3%) as compared to the conventional single-step annealed counterpart (37.7% -> 28.1%), consistent with an earlier TRIP onset. Consequently, the optimized condition exhibits significantly enhanced ductility and an extended uniform work-hardening regime (over 50% improvement), attributable to the reduced stability of reverted austenite, which facilitates earlier and more extensive strain-induced gamma -> alpha' transformation. Finally, we propose a microstructure design concept of "cellular structure - retained austenite - cellular austenite network" for strength - ductility synergy, providing a transferable paradigm for strengthening and toughening of other AM metals.
The plasticity of bulk metallic glasses (BMGs) is closely correlated with the nature of shear bands; however, the structural origin of shear bands remains elusive due to the difficulty of obtaining direct observations. In this study, we investigated the microstructural evolution of shear bands during thermal relaxation by examining the local atomic-scale response to heating. Zr52.5Cu17.9Ni14.6Al10Ti5 BMGs were subjected to two specifically designed deformation methods, namely, cold rolling and high-pressure torsion (HPT), to generate shear bands with varying volume fractions and rejuvenation states. In situ synchrotron diffraction results revealed a more pronounced growth of medium-range ordering at sub-Tg temperatures in the deformed BMGs than in the as-cast sample. The HPT-deformed BMG, with the highest volume fraction and distribution complexity of shear bands, demonstrated the most rapid increase in the ordering process. The transition of cluster connection modes possibly explained the anomalous emergence of medium-range order in the shear bands of deformed BMGs during sub-Tg relaxation or tension. Our study offers new insights into the atomic structure origins of shear bands, contributing to a deeper understanding of BMG plasticity.
The development of highly efficient microwave absorbers presents a significant challenge, driven by the growing issue of severe electromagnetic pollution. In this context, precise structural design emerges as a decisive factor for enhancing the microwave absorption capabilities. In this work, the hollow Ni0.5Zn0.5Fe2O4/C/Ni microspheres were fabricated through hydrothermal method, calcination treatment and further annealing. The results of the morphology observation demonstrate that the heterogeneous Ni0.5Zn0.5Fe2O4/C/Ni composites are hollow microspheres, consisting of many nanoparticles. Strikingly, the appearance of metallic Ni alongside increased carbon graphitization results from the partial reduction of Ni2+ by carbon during high-temperature annealing in the Ar atmosphere, which can be beneficial to the dielectric loss. The hollow Ni0.5Zn0.5Fe2O4/C/Ni microspheres possess outstanding microwave absorption capabilities, mainly owning to the better interface and dipole polarization, eddy current loss, conduction loss and natural resonance loss, multiply reflection and scattering between the microspheres. The hollow Ni0.5Zn0.5Fe2O4/C/Ni microspheres annealed at 700 °C exhibited an optimal reflection loss (RL) value of -35.79 dB at 2.5 mm and an effective absorption bandwidth (EAB) of 5.29 GHz at 2.0 mm. The present study reveals a design approach for heterostructures, which offers novel insights into the fabrication of high-performance microwave absorbing materials.