Single Nanostructures Research Articles

Construction of Methotrexate-Loaded Bi2S3 Coated with Fe/Mn-Bimetallic Doped ZIF-8 Nanocomposites for Cancer Treatment Through the Synergistic Effects of Photothermal/Chemodynamic/Chemotherapy.

A combination of therapeutic modalities in a single nanostructure is crucial for a successful cancer treatment. Synergistic photothermal therapy (PTT) can enhance the effects of chemodynamic therapy (CDT) and chemotherapy, which could intensify the therapeutic efficacy to induce cancer cell apoptosis. In this study, Fe and Mn on a zeolitic imidazolate framework (ZIF-8) (Fe/Mn-ZIF-8; FMZ) were synthesized through ion deposition. Furthermore, bismuth sulfide nanorods (Bi2S3 NRs; BS NRs) were synthesized via a hydrothermal process and coated onto FMZ to generate the core-shell structure of the Bi2S3@FMZ nanoparticles (B@FMZ). Next, methotrexate (MTX) was loaded effectively onto the porous surface of ZIF-8 to form the B@FMZ/MTX nanoparticles. The Fenton-like reaction catalyzes Fe2+/Mn2+ ions by decomposing H2O2 in the tumor microenvironment, resulting in the formation of toxic hydroxyl radicals (·OH), which promotes the CDT effect of killing cancer cells. Furthermore, under 808 nm laser irradiation, these B@FMZ nanoparticles showed a strong PTT effect, owing to the presence of intense BS NRs as a photothermal agent. The B@FMZ nanoparticles exhibited a prominent drug release efficiency of 87.25% at pH 5.5 under near-infrared laser irradiation due to the PTT effect can promote the drug delivery performance. The B@FMZ nanoparticles were subjected to dual-modal imaging, guided magnetic resonance imaging, and X-ray computed tomography imaging. Both in vitro and in vivo results suggested that the B@FMZ/MTX nanoparticles exhibited enhanced antitumor effects through the combined therapeutic effects of PTT, CDT, and chemotherapy. Therefore, these nanoparticles exhibit good biocompatibility and are promising candidates for cancer treatment.

Striking gold: study explores light resonance with layered metallic arrays

Overcoming the limitations of single gold nanostructures to expand color gamut

Single ZnO Nanowire for Electrical and Optical NO2 Gas Sensing: Origin of Reversible and Irreversible Gas Effects Investigated by Photoluminescence Spectroscopy.

In this work, the gas sensing properties of a single ZnO nanowire (NW) are investigated, simultaneously in terms of photoluminescence (PL) and photocurrent (PC) response to NO2 gas, with the purpose of giving new insights on the gas sensing mechanism of a single 1D ZnO nanostructure. A single ZnO NW sensing device was fabricated, characterized, and compared with a sample made of bundles of ZnO NWs. UV near-band-edge PL emission spectroscopy was carried out at room temperature and by lowering the temperature down to 77 K, which allows detection of resolved PL peaks related to different excitonic transition regions. Surface effects were observed in PL maps, considering different nano and microstructures. Electrical and optical measurements were acquired at the same time during the NO2 gas exposure, allowing for the comparison of PL and PC response times and signal recovery. During NO2 gas desorption, irreversible behavior in the surface-related and donor-acceptor pair (DAP) regions is interpreted as the effect of an initial transient when electronic transfer from the gas molecules to the bulk occurs through the ZnO NW surface which acts as a channel. To the best of our knowledge, this is the first work which investigates the simultaneous PL optical and PC electrical response signals of a single ZnO NW to gas exposure.

Polarized Upconversion of sub-100 nm Single Nanoparticles.

Upconversion nanoparticles are popular as imaging probes due to their advantages in photostability and controllable emission dimensions. However, upconversion polarization remains largely uncharted with previous reports limited to microstructures. In this work, we report the observation of polarized upconversion emissions from β-NaYF4 single nanostructures below 100 nm. At the sub-100 nm scale, nanorods, nanodiscs, and nanoplates exhibit distinctive polarization degrees despite the same doping concentrations of lanthanides. We find this varied polarization degree results from the crystallographic orientation of nanostructure in relation to the light field and can be linked to the distinctive emission spectrum profile with varied Stark splitting transition ratios from Er3+. Our findings provide a comprehensive understanding of the polarization properties of upconversion nanoparticles, revealing a previously unexplored aspect of light emission. This discovery expands our knowledge of upconversion nanoparticles and also opens new possibilities for their use in future imaging and sensing applications, where polarization sensitivity is crucial.

Facile fabrication of Au-Ag alloy nanoparticles/Ag nanowires SERS substrates with bimetallic synergistic effect for ultra-sensitive detection of crystal violet and alkali blue 6B

The bimetallic nanostructure of Au and Ag can integrate two distinct properties into a novel substrate compared to single metal nanostructures. This work presents a rapid and sensitive surface-enhanced Raman scattering (SERS) substrate for detecting illegal food additives and dyes of crystal violet (CV) and alkali blue 6B (AB 6B). Au-Ag alloy nanoparticles/Ag nanowires (Au-Ag ANPs/Ag NWs) were prepared by solid-state ionics method and vacuum thermal evaporation method at 5μA direct current electric field (DCEF), the molar ratio of Au to Ag was 1:18.34. Many 40 nm-140 nm nanoparticles regularly existed on the surface of Ag NWs with the diameters from 80 nm to 150 nm. The fractal dimension of Au-Ag ANPs/Ag NWs is 1.69 due to macroscopic dendritic structures. Compared with single Ag NWs, the prepared Au-Ag ANPs/Ag NWs substrates show superior SERS performance because of higher surface roughness, the SERS active of Ag NWs and bimetallic synergistic effect caused by Au-Ag ANPs, so the limit of detections (LOD) of Au-Ag ANPs/Ag NWs SERS substrates toward detection of CV and AB 6B were as low as 10-16mol/L and 10-9mol/L, respectively. These results indicate that Au-Ag ANPs/Ag NWs substrates can be used for rapid and sensitive detection of CV and AB 6B and have great development potential for detection of illegal food additives and hazardous substances in the fields of environmental monitoring and food safety.

Technologies for investigating single-molecule chemical reactions

Abstract Single molecules, the smallest independently stable units in the material world, serve as the fundamental building blocks of matters. Among different branches of single-molecule sciences, single-molecule chemical reactions, by revealing the behavior and properties of individual molecules at the molecular scale, are particularly attractive because they can advance the understanding of chemical reaction mechanisms and help to address key scientific problems in broad fields such as physics, chemistry, biology, and materials science. This review provides a timely, comprehensive overview of single-molecule chemical reactions based on various technical platforms such as scanning probe microscopy, single-molecule junction, single nanostructure, single-molecule fluorescence detection, and crossed molecular beam. We present multidimensional analyses of single-molecule chemical reactions, offering new perspectives for research in different areas like photocatalysis/electrocatalysis, organic reactions, surface reactions, and biological reactions. Finally, we discuss the opportunities and challenges in this thriving field of single-molecule chemical reaction.

Hyperspectral dark-field optical microscopy correlated to atomic force microscopy for the analysis of single plasmonic nanoparticles: tutorial

Plasmonic nanostructures are actively investigated for their optical properties and for a wide range of applications in nanophotonics, biosensing, photocatalysis, hot carrier physics, and advanced cancer therapies. The localized surface plasmon resonance (LSPR) can be excited in gold or silver nanoparticles or in more complex nanostructures and gives rise to a wide range of unique optical properties. It is often critical to be able to localize individual plasmonic nanoparticles and simultaneously measure their spectrum. This is known as hyperspectral microscopy. In this tutorial, we describe and carefully explain how to achieve this goal with an optical microscope equipped with a dark-field objective and an optical spectrometer. The images and the scattering spectra of spherical gold nanoparticles with diameters of 90, 70, 50, and 25 nm are recorded. We compare them with the scattering spectra predicted with the Mie formula (LSPR peaks measured at 553, 541, 535, and 534 nm, respectively). The optical images are limited by the diffraction, and this is discussed in the framework of the Abbe equation. We also describe a strategy to easily correlate the optical images with atomic force microscope images of the samples. This allows us to precisely relate the morphology of the nanoparticles with their optical images, their color, and their optical spectrum. The case of non-spherical nanostructures, namely, dimers of nanoparticles, is also discussed. This approach allows a relatively low-cost setup and efficient characterization method that will be helpful for teachers who want to introduce their students to the wide topics of plasmonics. This will also be useful for labs seeking an affordable method to investigate the plasmonic properties of single nanostructures.

Insights into molecular and bulk mechanical properties of glassy carbon through molecular dynamics simulations and mechanical tensile testing

With increasing interest in the use of glassy carbon (GC) for a broad range of application areas, the need for developing a fundamental understanding of its mechanical properties has come to the forefront. Furthermore, recent theoretical and modeling works that highlight the synthesis of GC via the pyrolysis of polymer precursors has explored the possibilities of a revisit to the investigation of their mechanical properties at a fundamental level. Although there are isolated reports on the experimental determination of its elastic modulus, insights into the stress-strain behavior of a GC material under tension and compression obtained through simulations, either at the molecular level or for the bulk materials, are missing. This study fills the gap at the molecular level and investigates the mechanical properties of GC using molecular dynamics (MD) simulations, which model the atomistic-level formation and breaking of bonds using bond-order-based reactive force field formulations. The molecular model considered in this simulation has a characteristic 3D cage-like structure of five-, six-, and seven-membered carbon rings and graphitic domains of a flat graphene-like structure. The GC molecular model was subjected to loading under varying strain rates (0.4, 0.6, 1.25, and 2.5 ns−1) and temperatures (300 K–800 K) in each of the three axes: x, y, and z. The simulations show that the GC nanostructure has distinct stress-strain curves under tension and compression. In tension, MD modeling predicted a mean elastic modulus of 5.71GPa for a single GC nanostructure with some dependency on the strain rate and temperature, whereas, in compression, the elastic modulus was also found to depend on the strain rate and temperature and was predicted to have a mean value of 35 GPa. To validate the simulation results and develop experimental insights into the bulk behavior, mechanical tests were conducted on dog-bone-shaped testing coupons that were subjected to uniaxial tension and loaded until failure. The GC test coupons demonstrated a bulk modulus of 17 ±2.69 GPa in tension, which compares well with those reported in the literature. However, comparing MD simulation outcomes to those of uniaxial mechanical testing reveals that the bulk modulus of GC in tension found experimentally is higher than the modulus of single GC nanostructures predicted by MD modeling, which inherently underestimates the bulk modulus. With regard to failure modes, the MD simulations predicted failure in tension accompanied by the breaking of carbon rings within the molecular structure. In contrast, the mechanical testing demonstrated that failure modes are dominated by brittle failure planes largely due to the amorphous structure of GC.

An innovative method of the vertical coupling effect improvement to the tandem Cu(In, Ga)Se2/perovskite solar cells using Ag cluster nanostructures

The efficiency of double-junction CIGS/Perovskite-based solar cells has significantly improved through recent research. This study presents a new plasmonic structure for these optical devices, utilizing cluster nanostructures to increase photon absorption between 650 and 1137 nm wavelength ranges. The proposed nanostructure includes two vertically coupled silver nanoparticles embedded at the center of the bottom active layer (CIGS) that absorb most of the incoming light to CIGS within the active layer. The electric field produced by the coupling of the nanoparticles has a superior performance. To analyze the effect of nanoparticle coupling on CIGS/Perovskite solar cell performance, evaluated the short-circuit current density and power conversion efficiency for single and cluster nanostructures with a single nanoparticle in the middle of CIGS. The structures with a single nanoparticle displayed Jsc = 16.89 mA cm−2 and PCE = 31.76%, while the cluster nanostructure represents Jsc = 19 mA cm−2 and PCE = 35.81%. Not only did the use of the cluster nanostructure significantly improve absorption and performance compared to the bare case, but it also exhibited a suitable improvement compared to the single nanoparticle.

Shaping single crystalline BaTiO3 nanostructures by focused neon or helium ion milling

The realization of perovskite oxide nanostructures with controlled shape and dimensions remains a challenge. Here, we investigate the use of helium and neon focused ion beam (FIB) milling in an ion microscope to fabricate BaTiO3 nanopillars of sub-500 nm in diameter starting from BaTiO3 (001) single crystals. Irradiation of BaTiO3 with He ions induces the formation of nanobubbles inside the material, eventually leading to surface swelling and blistering. Ne-FIB is shown to be suitable for milling without inducing surface swelling. The resulting structures are defect-free single crystal nanopillars, which are enveloped, on the top and lateral sidewalls, by a point defect-rich crystalline region and an outer Ne-rich amorphous layer. The amorphous layer can be selectively etched by dipping in diluted HF. The geometry and beam-induced damage of the milled nanopillars depend strongly on the patterning parameters and can be well controlled. Ne ion milling is shown to be an effective method to rapidly prototype BaTiO3 crystalline nanostructures.

Single crystalline molybdenum nanostructure for generating reflective micro-focal spot X-rays: Structure-controllable preparation and characteristic-selectable radiation

The use of properly designed nanostructured anode targets enables direct generation of high performance X-rays. In particular, this scheme has attracted widespread research interest for obtaining micro-focal spot X-ray radiation. In this study, we developed a thermal evaporating deposition technique and achieved controllable preparation of different single crystalline molybdenum (Mo) nanostructures by exploiting the lattice matching relationship between the substrate and the product crystal orientation. When used as an anode target for a reflective X-ray radiation device, these nanostructured Mo single crystals exhibit advantages over traditional targets at larger radiation angles. Further experimental and simulation results demonstrate the geometric characteristics of these Mo nanostructures and their correlation with the radiation intensity, focal spot size, and brightness of the generated X-rays. Among them, a unique frustum of square pyramid single crystalline Mo nanostructure stands out, due to its combination of three-dimensional body feature of nanostructures and radiation plane feature of planar targets. The research results not only provide a class of nanostructured anode target materials for reflective X-ray sources with different radiation angle requirements, but also make it possible to design and develop miniaturized devices for X-ray sources with selectable radiation performance and micro-focal spot.

A calculation method for optical properties of yolk shell based on deep learning.

The yolk shell is widely used in optoelectronic devices due to its excellent optical properties. Compared to single metal nanostructures, yolk shells have more controllable degrees of freedom, which may make experiments and simulations more complex. Using neural networks can efficiently simplify the computational process of yolk shell. In our work, the relationship between the size and the absorption efficiency of the yolk-shell structure is established using a backpropagation neural network (BPNN), significantly simplifying the calculation process while ensuring accuracy equivalent to discrete dipole scattering (DDSCAT). The absorption efficiency of the yolk shell was comprehensively described through the forward and reverse prediction processes. In forward prediction, the absorption spectrum of yolk shell is obtained through its size parameter. In reverse prediction, the size parameters of yolk shells are predicted through absorption spectra. A comparison with the traditional DDSCAT demonstrated the high precision prediction capability and fast computation of this method, with minimal memory consumption.

Enhanced second harmonic generation from supercavity mode and magnetic resonance in dumbbell-shaped silicon nanoblock

Abstract Electromagnetic multipole resonance can be excited by dielectric nanostructures of appropriate size to effectively promote light-matter interaction. The interactions between light and nanostructures have the capability to enhance the electromagnetic field in the near field, thereby improving the nonlinear effect of nanostructures. We illustrate that the supercavity mode and magnetic dipole resonance are activated by a single dumbbell-shaped silicon nanoblock (DS-SiNB), to trap the near-field electromagnetic field energy. Enhanced second harmonic generation is achieved by exploiting the localized electromagnetic field at the surface of the nanostructure. Numerical simulations reveal that magnetic quadrupole (MQ) and total electric dipole (TED) can be coupled to the same radiation channel by adjusting continuously the aspect ratio Lout/Ly (the outer edge length to the length of DS-SiNB) of the nanoblock. When the aspect ratio Lout/Ly = 1, the supercavity mode formed by the interference of MQ and TED is excited at λ1 = 1124 nm. And, the strong magnetic resonance mode formed by the coupling of two magnetic dipoles (MD) in the same direction is also excited at λ2 = 1124 nm. Supercavity mode and strong magnetic dipole resonance can effectively capture electromagnetic fields on the surface of nanostructures to attain enhanced second harmonic generation (SHG). Our study presents a novel approach to enhance the nonlinear optical effect of a single silicon nanostructure, which can lead to the development of more efficient nonlinear optical devices.

Plasmonic Properties of Self-Assembled Gold Nanocrescents: Implications for Chemical Sensing.

A bottom-up approach, the Langmuir-Blodgett technique, is used for the preparation of composite thin films of gold nanoparticles and polymers: poly(styrene-b-2-vinylpyridine), poly-2-vinylpyridine, and polystyrene. The self-assembly of poly(styrene-b-2-vinylpyridine) at the air-water interface leads to the formation of surface micelles, which serve as a template for the organization of gold nanoparticles into ring assemblies. By using poly-2-vinylpyridine in conjunction with low surface pressure, the distance between nanostructures can be increased, allowing for optical characterization of single nanostructures. Once deposited on a solid substrate, the preorganized gold nanoparticles are subjected to further growth by the reduction of additional gold, leading to a variety of nanostructures which can be divided into two categories: nanocrescents and circular arrays of nanoparticles. The optical properties of individual structures are investigated by optical dark-field spectroscopy and numerical calculations. The plasmonic behavior of the nanostructures is elucidated through the correlation of optical properties with structural features and the identification of dominant plasmon modes. Being based on a self-assembly approach, the reported method allows for the formation of interesting plasmonic materials under ambient conditions, at a relatively large scale, and at low cost. These attributes, in addition to the resonances located in the near-infrared region of the spectrum, make nanocrescents candidates for biological and chemical sensing.

Active strong coupling of exciton and nanocavity based on GSST-WSe2 hybrid nanostructures

The strong coupling between optical resonance microcavity and matter excitations provides a practical path for controlling light-matter interactions. However, conventional microcavity, whose functions are fixed at the fabrication stage, dramatically limits the modulation of light-matter interactions. Here, we investigate the active strong coupling of resonance mode and exciton in GSST-WSe2 hybrid nanostructures. It is demonstrated that significant spectral splitting is observed in single nanostructures, tetramers, and metasurfaces. We further confirm the strong coupling by calculating the enhanced fluorescence spectra. The coupling effect between the excited resonance and exciton is dramatically modulated during the change of GSST from amorphous to crystalline, thus realizing the strong coupling switching. This switching property has been fully demonstrated in several systems mentioned earlier. Our work is significant in guiding the study of actively tunable strong light-matter interactions at the nanoscale.

Controlled synthesis of Co3O4@CoP heterostructured nanoarrays as efficient electrocatalysts in alkaline seawater and urea

How to prepare clean energy has always been a problem to be solved by the modern green chemical industry. Compared with the electrolysis of water to produce hydrogen, electrolysis of seawater for raw material requirements are lower and more widely used. However, the lacks of maturity of the technology, the high cost and the generation of harmful gases such as chlorine in the electrocatalytic process have hindered the development of this process. This study demonstrates a construction of heterogeneous structure based on Co ions as an efficient multifunctional catalyst for overall seawater splitting and urea oxidation. This hybrid structure can combine nanosheets and nanowires, thus exposing the catalyst to more active sites and shortening the ion diffusion path. Comparing the hybrid structure with the single structure, Co3O4@CoP exhibits excellent multifunctional catalytic activity in alkaline seawater and urea. In the oxygen evolution reaction, the working potential is only 1.60 V and 1.70 V at a current density of 50 mA/cm2 and 100 mA/cm2. And in the hydrogen evolution reaction, the working potential was only −0.16 V at a current density of −10 mA/cm2, demonstrating excellent bifunctional activity. On this basis, the catalyst also demonstrated excellent activity for urea oxidation reaction in alkaline environment, with an operating potential of only 1.28 V at a current density of 10 mA/cm2. And the durability of this catalyst is good, it can keep 5 mA/cm2 for 12 h under the constant voltage of 1.45 V, but the initial potential falls off too fast, and there is a decline in performance, which is closely related to the corrosion of Cl- present in seawater. It was shown by density functional theory (DFT) that hierarchical nanostructures can increase the transfer rate of reaction intermediates and the water adsorption energy. At the end of this study, by comparing single nanostructures with hybrid nanostructures, it can be reasonably conjectured that the accompanying increase in the number the heterostructure is resistant to Cl- corrosion in seawater.

Concentrated Solar Light Photoelectrochemical Water Splitting for Stable and High-Yield Hydrogen Production.

Photoelectrochemical water splitting is a promising technique for converting solar energy into low-cost and eco-friendly H2 fuel. However, the production rate of H2 is limited by the insufficient number of photogenerated charge carriers in the conventional photoelectrodes under 1 sun (100mWcm-2) light. Concentrated solar light irradiation can overcome the issue of low yield, but it leads to a new challenge of stability because the accelerated reaction alters the surface chemical composition of photoelectrodes. Here, it is demonstrated that loading Pt nanoparticles (NPs) on single crystalline GaN nanowires (NWs) grown on n+-p Si photoelectrode operates efficiently and stably under concentrated solar light. Although a large number of Pt NPs detach during the initial reaction due to H2 gas bubbling, some Pt NPs which have an epitaxial relation with GaN NWs remain stably anchored. In addition, the stability of the photoelectrode further improves by redepositing Pt NPs on the reacted Pt/GaN surface, which results in maintaining onset potential >0.5V versus reversible hydrogen electrode and photocurrent density >60mAcm-2 for over 1500 h. The heterointerface between Pt cocatalysts and single crystalline GaN nanostructures shows great potential in designing an efficient and stable photoelectrode for high-yield solar to H2 conversion.

Deformable Smart DNA Nanomachine for Synergistic Intracellular Cancer-Related miRNAs Imaging and Chemo-Gene Therapy of Drug-Resistant Tumors.

Diagnosis and treatment of tumor especially drug-resistant tumor remains a huge challenge, which requires intelligent nanomedicines with low toxic side effects and high efficacy. Herein, deformable smart DNA nanomachines are developed for synergistic intracellular cancer-related miRNAs imaging and chemo-gene therapy of drug-resistant tumors. The tetrahedral DNA framework (MA-TDNA) with fluorescence quenched component and five antennas is self-assembled first, and then DOX molecules are loaded on the MA-TDNAs followed by linking MUC1-aptamer and Mcl-1 siRNA to the antennas of MA-TDNA, so that the apt-MA-TDNA@DOX-siRNA (DNA nanomachines) is constructed. The DNA nanomachine can respond to two tumor-related miRNAs in vitro and in vivo, which can undergo intelligent miRNA-triggered opening of the framework, resulting in the "turn on" of the fluorescence for sensitively and specifically sensing intracellular miRNAs. Meanwhile, both miRNA-responded rapid release and pH-responded release of DOX are achieved for chemotherapy of tumor. In addition, the gene therapy of the DNA nanomachines is achieved due to the miRNA-specific capture and the RNase H triggered release of Mcl-1 siRNA. The DNA nanomachines intergrading both tumor imaging and chemo-gene therapy in single nanostructures realized efficient tumor-targeted, image-guided, and microenvironment-responsive tumor diagnosis and treatment, which provides a synergetic antitumor effect on drug-resistant tumor.

Investigation of encapsulated water wire within self-assembled hydrophilic nanochannels, in a modified γ4-amino acid crystals: Tracking thermally induced changes of intermolecular interactions within a crystalline hydrate

Nanostructures formed by the self-assembly of modified/unmodified amino acids have the potential to be useful in several biological/nonbiological applications. In that regard, the greater conformational space provided by γ-amino acids, owing to their additional backbone torsional degrees of freedom and enhanced proteolytic stability, compared to their α-counterparts, should be explored. Though, modified single amino acid-based nanomaterials such as nanobelts or hydrogels are developed by utilizing the monosubstituted γ-amino acids derived from the backbone homologation of phenylalanine (Phe). Examples of a single γ-amino acid-based porous nanostructure capable of accommodating solvent molecules are not really known. The crystal structures of a modified γ4(R)Phe residue, Boc-γ4(R)Phe-OH, at different temperatures, showed that hydrogen-bonded water molecules are forming a wire inside hydrophilic nanochannels. The dynamics of intermolecular interactions between the water wire and the inner wall of the channel with relation to the temperature change was investigated by analyzing the natural bonding orbital (NBO) calculation results performed with the single crystal structures obtained at different temperature points. The NBO results showed that from 325 K onward, the strength of water–water interactions in the water wire are getting weaker, whereas, for the water–inner wall interactions, it getting stronger, suggesting a favorable change in the orientation of water molecules with temperatures, for the latter.

Synthesis of core-shell NiO/BFO nanocomposites for microwave absorbing applications

Magnetic core-shell nanostructures are often employed in high-performance microwave-absorbing applications due to their strong concurrent magnetic-dielectric losses. However, microwave absorbers designed using a single core-shell nanostructure may not attain the desired bandwidth of absorption. Herein, we introduce core-shell nanocomposites of (100-x)NiO/(x)BiFeO3 (x = 0, 25, 50, 75, & 100), prepared by a facile two-step sol-gel wet-chemical method for high-efficiency absorbing applications. Measurements of microwave absorption performance show that the core-shell 50NiO/50BiFeO3 (x = 50) nanocomposite exhibits a remarkable reflection loss of up to −27.3 dB at a matching thickness of 1.9 mm, and the corresponding −10 dB reflection loss bandwidth extends to 6.8 GHz (in X- and Ku-bands). The study suggests that the fabricated core-shell nanocomposite has the potential to be a promising candidate for lightweight microwave absorbing applications. This is evidenced by its showcased improved efficiency, attributed to the synergistic effects of magnetic-dielectric losses, multiple internal reflections, superior impedance matching, and enhanced interfacial polarization at NiO/BiFeO3 interfaces.