High-resolution Transmission Electron Microscopy Observations Research Articles

Copper nanoparticle and point defect formation in Cu+-Na+ ion-exchanged glass using protons of 2 MeV energy.

There are several applications for irradiating materials with protons that could provide alternative methodologies to synthesize and induce the formation of new compounds of different size scales. In this study, we explored the effects of proton irradiation oncommercial glass silicate that was previously subjected to a Cu+-Na+ ion exchange (IE) treatment at 600 °C for a duration of 60 min. The ion-exchanged glass samples were irradiated with protons (p+) of 2 MeV energy at doses in the range of thousands of grays (3.3 × 103, 7.9 × 103 Gy) and hundreds of thousands of grays (3.6 × 105 Gy). Significant changes in the optical and structural properties were observed post the radiation treatment. The UV-Visible absorption spectra of the irradiated samples revealed the appearance of overlapping absorption bands, which could be deconvoluted into three Gaussian-shaped bands peaking at 566, 620 and 680 nm. These three bands could be attributed to the surface plasmon resonance (SPR) of copper nanoparticles, non-bridging oxygen hole centers (NBOHCs) and self-trapped hole (STH) defects, respectively. Prominent photoluminescence (PL) was observed in the Cu-exchanged and irradiated samples, mainly induced by the presence of both Cu+ and Cu2O. Increasing the irradiation dose led to an increase in the PL intensity due to the conversion of Cu2+ ions into Cu+. This result was confirmed by electron paramagnetic resonance (EPR) spectroscopy that shows a decrease in the Cu2+ signal when increasing the dose of proton exposure. Transmission electron microscopy (TEM) and high-resolution TEM (TEM and HRTEM) observations confirmed the presence of copper nanoparticles (CuNPs) in the doped and p+ irradiated Cu-exchanged glass silicate samples. These CuNPs were found to be crystalline with an average size of 12.39 nm.

Pressure-induced ferroelectric and electronic transitions in two-dimensional ferroelectric semiconductor of NbOCl2 up to 41.7 GPa

NbOCl2, a representative van der Waals ferroelectric (FE) semiconductor, has become the research frontier due to its peculiar appeal in both fundamental research studies and potential applications. In the present work, the high-pressure structural, vibrational, and electrical transport properties of NbOCl2 under different hydrostatic environments were systematically investigated over a wide pressure range of 1.7–41.7 GPa using a diamond anvil cell coupled with in situ Raman spectroscopy, electrical conductivity, and high-resolution transmission electron microscopy (HRTEM) observations. Upon non-hydrostatic compression, NbOCl2 underwent a FE-to-antiferroelectric phase transition at 3.4 GPa, followed by a semiconductor-to-metal transformation at 15.7 GPa. Under hydrostatic compression, the FE transformation and metallization of NbOCl2 were postponed by ∼2.0 and ∼4.0 GPa due to the effect of helium pressure-transmitting medium. Upon decompression, the phase transition was demonstrated to be reversible under different hydrostatic environments, which was well corroborated by HRTEM analyses. In addition, the linear relations between electrical current and sinusoidal voltage with the nonlinearity factors of ∼1.0 reflect the Ohmic response of NbOCl2 before and after the FE transition. Our findings on NbOCl2 provide a guideline for exploring other layered FE materials under high pressure and establishing a design paradigm for new generations of FE-based devices.

Enhanced photocatalytic antibacterial activity of Au-coated Ni–Ti–O nanotubes for biomedical applications

Nickel-titanium (NiTi) alloy is a smart material exhibiting superelasticity, contributing to low stiffness and facilitating integration with bone structures. However, NiTi alloy's bioactivity and antibacterial activity limit its dental applications. In this study, we fabricated nickel titanium oxide (Ni–Ti–O) nanotubes with the potential for bioactivity and photocatalytic properties on the surface of NiTi alloy. Specifically, we applied a coating of gold (Au) nanoparticles to the surface of Ni–Ti–O nanotubes, in order to leverage the antibacterial activity through the photocatalytic effect under 470 nm visible light. Field-emission scanning electron microscopy (FE-SEM) and high-resolution transmission electron microscopy (HR-TEM) observations revealed that Au was deposited mainly at the top surface of Ni–Ti–O nanotubes (diameter: 12.76 ± 2.91 nm, height: 721.12 ± 50.25 nm). X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), and diffuse reflectance spectroscopy (DRS) analyses revealed that the Ni–Ti–O nanotubes were NiTiO3 crystalline phases with low crystallinity. Therefore, based on the methylene blue (MB) degradation test, the photocatalytic effect was only achieved under visible light at 470 nm, facilitated by the presence of Au. The antibacterial colony forming unit test and enzymatic activity tests demonstrated that Au-coated Ni–Ti–O nanotubes displayed excellent antibacterial activity under 470 nm visible light irradiation, which was also attributed to photocatalytic effect. Consequently, the combination of Au-coated Ni–Ti–O nanotubes and visible light-based photofunctionalization holds promise for expressing antibacterial properties in dental applications.

Graphene-like materials supported on sepiolite clay synthesized at relatively low temperature

The preparation of solids with graphitic structure usually requires synthesis procedures using very high temperatures. In this work, a comparative study involving different experimental strategies of synthesis at relatively low temperature was carried out to obtain graphene-like materials supported on microporous sepiolite (SEP) clay. The final objective was the optimization of the development of new clay-graphitic nanostructured materials to achieve porous solids while saving energy and time during the preparation stages. The pyrolysis of sucrose (SUC), used as carbon precursor, was accomplished by microwave (MW) pyrolysis or tube furnace (TF) pyrolysis at 200 or 500 °C followed by a hydrothermal carbonization (HTC) step. The resulting carbon-clay nanoarchitectures were characterized by Raman and Infrared spectroscopy, X-ray diffraction, elemental analysis, electron microscopy, and nitrogen adsorption-desorption isotherms. The MW200 and TF200 treatments caramelized SUC and the post-HTC step was fundamental to obtain porous carbonaceous materials. The TF500 pyrolysis produced predominantly crystalline carbon, while the MW500 pyrolysis formed an amorphous material. Moreover, the high-resolution transmission electron microscopy observations of TF500 sample revealed a crystalline material with a d-spacing of 0.33 nm, matching the graphitic lattice. All the treatment conditions performed at 500 °C i.e., MW or TF followed or not by HTC, resulted in mesoporous carbons with a specific surface area above 200 m2 g−1. The MW pyrolysis saved 100 min of the reaction time in comparison to TF pyrolysis to obtain the carbonaceous porous materials.

A phenomenological model for predicting the size of soot primary particles emitted from an aero-engine combustor

Soot particles emitted from aero-engines are harmful to airport local air quality, and the adverse impact from soot particles is closely related to particle morphology, microstructure and chemical properties. To understand those properties of aviation soot particles, combustion experiments using conventional aviation fuel RP-3 were conducted on a Rich-Burn/Quick-Quench/Lean-Burn (RQL) aero-engine combustor. The soot emissions from the RQL combustor were analyzed via a high resolution transmission electron microscope (HRTEM), and the size distributions of primary particles at different power levels were determined based on the HRTEM images. Since the primary particle size is strongly related to the power level and follows an S-shaped curve, a phenomenological model with low-computational complexity and general applicability was established. Furthermore, the model was validated by using previously published experimental data of a CFM56–2C1 aero-engine burning four different fuels, including sustainable aviation fuels (SAF), demonstrating the influence of fuel properties on primary particle sizes at different power levels.Novelty and Significance Statement: In this paper, combustion experiments were conducted on an RQL combustor burning RP-3 fuel. Based on the HRTEM observation, the log-normal size distributions of primary particles at different power levels were determined. Furthermore, based on the fact that the relationship between primary particle size and power level followed an S-shaped curve, a phenomenological model linking primary particle size and combustor power was proposed and validated.

TEM characterization of defects in κ-(In x Ga1−x )2O3 thin film grown on (001) FZ-grown ε-GaFeO3 substrate by mist CVD

We have characterized defects in κ-(In x Ga1–x )2O3 thin films grown on (001) FZ-grown ε-GaFeO3 substrates by mist CVD using TEM. We found two types of defects: dislocation half-loops and microdefects. The half-loops are U-shaped and lie on the (100) plane. From contrast experiment, their Burgers vector was determined to be parallel to 〈010〉. While the microdefects were observed just above the interface between the κ-(In x Ga1–x )2O3 film and the ε-GaFeO3 substrate. They are 5–15 nm in size and accompany strong strain field. From (010) high-resolution transmission electron microscopic observation, it has been found that they are planar defects lying on the (001) plane. From these results, generation mechanisms of these defects are discussed.

Plasma-activated high-strength non-isothermal anodic bonding for efficient fabrication of the micro atomic vapor cells

Microfabricated alkali metal vapor cells are the core components for miniaturizing quantum devices, such as atomic clocks, atomic gyroscopes, and atomic magnetometers. Alkali metals are prone to thermal migration at the bonding interface during the sealing of the vapor cell, which leads to bonding failure. In this study, a non-isothermal anodic bonding process based on plasma activation was developed to achieve high-strength bonding at low temperatures using the temperature gradient to keep the alkali metal away from the bonding interface. This procedure eliminates interference from the alkali metal and significantly increases the success rate of anodic bonding of vapor cells. Simulation results for the temperature field and the residual stresses during anodic bonding demonstrate that the procedure is theoretically feasible. The effect of plasma treatment on the contact angle and roughness of the bonding surface revealed a mechanism for improving the bond strength. In addition, the construction of an integrated processing platform made it possible to perform non-isothermal anode bonding, injection of alkali metal, filling of inert gases, and recovery and recycling of noble gases. The high strength and good hermeticity of the bonding interface were demonstrated by the bond strength, cross-sectional high-resolution transmission electron microscopy observations, and leakage rate tests. Finally, the absorption spectrum and free-induction decay signal of the fabricated vapor cell were measured.

Pressure-Driven Structural and Electronic Transitions in a Two-Dimensional Janus WSSe Crystal.

In this work, we presented the first report on the high-pressure structural stability and electrical transport characteristics in WSSe under different hydrostatic environments through Raman spectroscopy, electrical conductivity, and high-resolution transmission electron microscopy (HRTEM) coupled with first-principles theoretical calculations. For nonhydrostatic conditions, WSSe endured a phase transition at 15.2 GPa, followed by a semiconductor-to-metal crossover at 25.3 GPa. Furthermore, the bandgap closure was accounted for the metallization of WSSe as derived from theoretical calculations. Under hydrostatic conditions, ∼ 2.0 GPa pressure hysteresis was detected for the emergence of phase transition and metallization in WSSe because of the feeble deviatoric stress. Upon depressurization, the reversibility of the phase transition was substantiated by those of microscopic HRTEM observations under different hydrostatic environments. Our high-pressure investigation on WSSe advances the insightful understanding of the crystalline structure and electronic properties for the Janus transition-metal dichalcogenide (TMD) family and boosts prospective developments in functional devices.

3D nanostructure prediction of porous carbons via gas adsorption

Structural characterization of porous carbon materials is critical for the evaluation of their synthesis procedures and performance. Throughout the last decades, many methods have been employed to determine porosity properties from gas adsorption such as surface area, pore size distribution (PSD) and real density. However, gas adsorption models use 1D structures of carbon nanopores, although adsorption and separation properties of nanoporous carbons are governed by 3D pore parameters. Estimating the 3D nanostructure of nanoporous carbons using gas adsorption would accelerate progress in research and implementation of nanoporous carbons. We report here a promising 3D pore nanostructural characterization from gas adsorption. Using atomistic simulations, we have generated a database of realistic 3D porous carbon structures spanning a wide range of pore sizes and geometries. After calculating their gas adsorption isotherms, we employed a numerical procedure to find the relative contribution for each of the structures to the adsorption isotherm of a nanoporous carbon sample. These contributions allowed us to estimate the surface area and pore size distribution of carbon materials; moreover (and perhaps more importantly!), we will show that the plausible 3D pore structures correlate very well with the local carbon structure as experimentally determined by high-resolution TEM observations and can successfully predict adsorption of different molecules. This is a powerful procedure that can be extended to other materials, and with enough computer power, to larger pore sizes.

Martensitic transformation pathways and crystallographic orientation relationships in steel

Martensite is one of the most important structures determining the ability to tailor the performance of steel and several other engineering materials. In previous studies, the face-centered cubic (FCC) to hexagonal close-packed (HCP) (or body-centered cubic (BCC)) martensitic transformation and the FCC to body-centered tetragonal (BCT) (or BCC) martensitic transformation during deformation and quenching were widely investigated; these transformations usually improve the plasticity and strength of steel, respectively. In this work, detailed transmission electron microscopy (TEM) observations and electron diffraction pattern analyses of the BCT and BCC twins are performed along the [110], [131], and [1¯53] zone axes. The transformation of BCT twins into BCC twins along the [131] zone axis is also analyzed through in situ heating during the TEM observations. The high-resolution TEM observations of mutually perpendicular BCT variants are consistent with the atomic arrangement obtained for the quenching pathway during the martensitic transformation. In addition, different orientation relationships between austenite and martensite are explained in terms of the atomic migration occurring during the deformation pathway and the quenching pathway of the martensitic transformation.

Copper bonding silicon nitride substrate using atmosphere plasma spray

Silicon nitride (Si3N4) is an excellent engineering ceramic with high strength, fracture toughness, wear resistance, and good chemical and thermal stability. Recently, the enhanced thermal conductivity enables Si3N4 to have potential application prospects in the electronic and orthopedic fields. Metal bonding with Si3N4 is often the key to these applications. Here we report a facile approach for the titanium-activated Cu bonding on Si3N4 substrates using an atmosphere plasma spray (APS) process. With X-ray diffraction (XRD) and high-resolution transmission electron microscopy (HRTEM) observation, it was shown that the interaction between the pre-bonded Ti (by APS) on Si3N4 promoted the adhesion and high bonding strength of APS Cu on Si3N4. The interfacial structure and phases were characterized, and tensile strength, electrical resistivity, thermal conductivity, and residual stress of Cu bonded Si3N4 were measured accordingly. The APS deposited Cu layer is dense, has a high purity, and is joined firmly with Ti pre-bonded Si3N4 substrate. The maximum tensile strength between Cu and Si3N4 is as high as 89.4 MPa. The Si3N4 substrate bonded with highly dense Cu demonstrates a low surface resistivity of 8.72 × 10−4 Ω∙mm, and high thermal conductivity of 98.12 W/m·K, which shows potential applications in electronic devices.

New strategy to improve the overall performance of single-crystal superalloys by designing a bimodal γ′ precipitation microstructure

Advanced single-crystal superalloys, developed to improve the high temperature capability of gas turbines, often underperform in low-temperature conditions. This limitation compromises the overall reliability of turbine blades under complex service environments. This study introduces a novel strategy to enhance the overall performance of a fourth-generation single-crystal superalloy. Rapid liquid-nitrogen quenching following the aging treatment promotes extensive nucleation of ultrafine γ′ particles (γ′γ) with an average size of ∼10 nm, precipitated under extremely low supersaturation, as evidenced by high-resolution transmission electron microscopy (HRTEM) and atom probe tomography investigations. The combination of differential scanning calorimetry analysis, density functional theory calculations, and kinetic models verifies the high stability of γ′γ particles at low-temperature conditions around 900 °C. HRTEM observations reveal Orowan bypassing and dislocation cutting of γ′γ particles, leading to additional precipitation hardening by limiting dislocation motion in the γ phase and shear of primary precipitates. Consequently, a bimodal precipitation microstructure comprising γ′γ particles and primary γ′ phase significantly reduces the strain rate of low-temperature creep and nearly doubles the creep rupture life at 800 °C/735 MPa. Simultaneously, high-temperature properties at 900 °C/392 MPa and 1100 °C/137 MPa remain comparable to those of the original microstructure as the primary γ/γ′ microstructure is minimally affected by rapid cooling. This advancement improves overall performance and redefines the importance of small precipitates, broadening microstructure design concepts for future superalloy development.

Delayed plasticity during spherical nanoindentation of an iron-chromium-aluminum alloy: Effect of ferric ion irradiation

Spherical nanoindentation of an iron-chromium-aluminum alloy was conducted to study the effect of ferric-ion (Fe3+) irradiation on the time-dependent plasticity behavior in the surface layers of this alloy. It was observed that the initiation of plasticity by the appearance of displacement burst or “pop-in” event occurred after a period of waiting time in the apparent elastic regime and that Fe3+ irradiation at 360 °C and up to ∼0.5 displacements per atom could make it happen under the lower applied loads but with a reduced magnitude. Through the experimental data, an activation volume and activation energy were extracted for the delayed plasticity. The results show that Fe3+-irradiation significantly reduced its activation volume from ∼3.05b3 to ∼1.75b3 (where b = Burgers vector), but slightly increased its activation energy from ∼0.65 to ∼0.71 eV. On the other hand, high-resolution scanning transmission electron microscopy observations reveal that the irradiation at the elevated temperature created interstitial atom pair onto the (100) habit plane that can serve as the nucleation site of a 〈100〉 dislocation loop while eliminating the pre-existing dislocations. Consequently, it is indicated that heterogeneous nucleation of the dislocation loop was predominant in the delayed plasticity initiation of this alloy and that the nucleation of the interstitial-type dislocation loop was involved due to Fe3+-irradiation.

Phase transition of hafnon, HfSiO4, at high pressure

AbstractThe high‐pressure behavior of hafnon has been systematically investigated by combining in situ synchrotron X‐ray diffraction, Raman, high‐resolution transmission electron microscopy (HRTEM) techniques, and theoretical simulations. Hafnon starts phase transition at 26.6 GPa and completes the transition to an irreversible scheelite phase (, Z = 4, a0 = 4.712 Å, and c0 = 10.378 Å) at ∼45 GPa. The HRTEM observation of an interface between hafnon and scheelite phases allows atomic scale understanding of the transition process with a relationship of (200)h‖(112)s, //, and . Hafnon shows a significantly lower transition pressure (∼12.6 GPa), as calculated from the relative enthalpies, than the measured pressure (∼26 GPa), indicating a kinetically hindered process involved in the transition. A high pressure low symmetry phase in hafnon () is identified by the simultaneous appearance of two Raman modes (∼75 and 450 cm−1) at 26.6 GPa and their subsequent simultaneous disappearance at 36.7 GPa. These results are important to understanding the mechanism of the zircon‐scheelite transition for both zircon and hafnon.

Nano-refinement of the face-centered cubic Zr(Fe,Cr)2 secondary phase particles in Zircaloy-4 alloy via localized-shearing/bending-driven fracture under high-temperature compression

Nanoparticles are extensively introduced to improve the mechanical, physical, and chemical properties of alloys. In the present study, the underlying nano-refinement mechanisms of face-centered cubic Zr(Fe, Cr)2 secondary phase particles (SPPs) that precipitated in Zircaloy-4 alloy under high-temperature compression were investigated in detail by utilizing high-resolution transmission electron microscopy (HRTEM) and conventional TEM techniques. The frequently observed Zr(Fe, Cr)2 SPPs were incoherent with the matrix and exhibited brittle fracture behaviors without measurable plasticity. HRTEM observations revealed two mechanisms underlying the nano-refinement of incoherent micro-sized SPPs via localized shear fracture on {112¯}SPP and nanoprecipitate-assisted bending fracture, respectively. The latter was, for the first time, found to occur when the movements of large SPPs were blocked by nanometer-sized SPP during alloy deformation. Accordingly, two force models were proposed to visualize their potential nano-refinement processes. The knowledge attained from this study sheds new light on the deformation behaviors of Zr(Fe, Cr)2 SPPs and their associated size refinement mechanisms under high-temperature compression, and is expected to greatly benefit the process optimization of zirconium alloys to achieve precipitate nano-refinement.

High density of stacking faults strengthened TaN/TiN multilayer

Multilayer coatings with individual layer thickness on the nanoscale exhibit superior mechanical properties because of their high interface density. However, compared to artificial phase interfaces, planar defects like twin and stacking faults (SFs) are hardly investigated in ceramic multilayer systems. We choose to combine the group VB transition metal nitride (TMN) TaN with its extremely low stacking faults energy (SFE) and TiN to form a superlattice (SL). TiN/TaN multilayers with a bilayer period (Λ) from 8 nm to 100 nm were prepared by dc magnetron sputtering. These as-deposited films show a peak hardness 36 ± 2.4 GPa at Λ=20 nm. The extensive high-resolution transmission electron microscopy (HRTEM) observations reveal that the dissociation of full dislocations results in the network of SFs and the formation of Lomer-Cottrell lock arrays inside the TaN layer. Meanwhile, further dislocation analysis indicated the Shockley partials cross slip at the interface. These findings provide us with a new perspective for designing TMN multilayers with planar defects.

Flash-ignition of carbon black synthesized from acetylene diffusion flames and its application as ignition agents

The study proposes a new ignition agent composed of a mixture of carbon black and ferrocene, which can be triggered using a flash lamp. This low-cost alternative to costly materials like carbon nanotubes, fullerenes, or energetic metal nanoparticles, involves adding a tiny amount of ferrocene to carbon black to ignite gaseous fuels and other energetic materials. The carbon black generated by the laminar diffusion flame of acetylene can be ignited using the commercial camera flash. Scanning electron microscope and high-resolution transmission electron microscopy observations reveal that the carbon black used in the study has no distinct single-walled carbon nanotubes, multi-walled carbon nanotubes, or graphene structures. The flash-ignition test showed that the carbon black could be ignited with an ordinary camera flash lamp, with the oxidation reaction becoming more vital as the camera-flash energy output increases. Additionally, the flash-ignition reaction becomes more intense with finer carbon black particles, even with the camera flash lamp's energy output remaining the same. Furthermore, adding ferrocene to carbon black enhances the effect of flash ignition. The study evaluated the carbon black/ferrocene mixture using thermogravimetric analysis and spectrophotometer to determine its purity, ignition temperature, and photo-physical properties. It also measured the burning of the mixture with the Two-color Pyrometry, finding that the burning temperature of the proposed ignition agents was high enough to ignite the gaseous fuels and the energetic materials. Finally, the mechanism of ferrocene in promoting the flash ignition of carbon black is proposed.

Lateral Bending of Ag Nanowires toward Controllable Manipulation

Nanowires (NWs) provide opportunities for building high-performance sensors and devices at micro-/nanoscales. Directional movement and assembly of NWs have attracted extensive attention; however, controllable manipulation remains challenging partly due to the lack of understanding on interfacial interactions between NWs and substrates (or contacting probes). In the present study, lateral bending of Ag NWs was investigated under various bending angles and pushing velocities, and the mechanical performance corresponding to microstructures was clarified based on high-resolution transmission electron microscope (HRTRM) detections. The bending-angle-dependent fractures of Ag NWs were detected by an atomic force microscope (AFM) and a scanning electron microscope (SEM), and the fractures occurred when the bending angle was larger than 80°. Compared with an Ag substrate, Ag NWs exhibited a lower system stiffness according to the nanoindentation with an AFM probe. HRTRM observations indicated that there were grain boundaries inside Ag NWs, which would be contributors to the generation of fractures and cracks on Ag NWs during lateral bending and nanoindentation. This study provides a guide to controllably manipulate NWs and fabricate high-performance micro-/nanodevices.

Self-Powered Phase Transition Driven by Triboelectric Nanogenerator

The phase transition of SrCoO2.5 (BM-SCO) is very popular in recent reports based on its special structure. The oxygen vacancy channel of BM-SCO provides a convenient condition for phase transformation to SrCoO3-δ (PV-SCO), with prospects in smart windows, memristive devices, and magnetic recording. The traditional method for phase transition is thermal annealing, while the electric-field-controlled ionic liquid (IL) gating is also a convenient method. Herein, we use a triboelectric nanogenerator as a self-powered system, which can provide a constant voltage for the IL and achieve ion injection to induce phase transition, and this procedure proved to be reversible. X-ray diffraction scanning and high-resolution transmission electron microscope observation showed that the crystal structures of the two phases are significantly different. Besides, BM-SCO is antiferromagnetic, PV-SCO is ferromagnetic, and the optical transmittance also changes during the phase transition. As for the applications of this film, we used IL gating to modulate the resistive switching behavior, which shows a change between high-resistance state and low-resistance state during the phase transition and can be used in resistive random access memory devices.

Identification and Biological Evaluation of a Water-Soluble Fullerene Nanomaterial as BTK Kinase Inhibitor.

Thanks to recent advances in synthetic methodology, water-soluble fullerene nanomaterials that interfere with biomolecules, especially DNA/RNA and selected proteins, have been found with tremendous potential for applications in nanomedicine. Herein, we describe the synthesis and evaluation of a water-soluble glycine-derived [60]fullerene hexakisadduct (HDGF) with T h symmetry, which is a first-in-class BTK protein inhibitor. We synthesized and characterized glycine derived [60]fullerene using NMR, ESI-MS, and ATR-FT-IR. DLS and zeta potential were measured and high-resolution transmission electron microscopy (HRTEM) observations were performed. The chemical composition of the water-soluble fullerene nanomaterial was examined by X-ray photoelectron spectrometry. To observe aggregate formation, the cryo-TEM analysis was carried out. The docking studies and molecular dynamic simulations were performed to determine interactions between HDGF and BTK. The in vitro cytotoxicity was evaluated on RAJI and K562 blood cancer cell lines. Subsequently, we examined the induction of cell death by autophagy and apoptosis by determining the expression levels of crucial genes and caspases. We investigated the direct association of HDGF on inhibition of the BTK signalling pathway by examining changes in the calcium levels in RAJI cells after treatment. The inhibitory potential of HDGF against non-receptor tyrosine kinases was evaluated. Finally, we assessed the effects of HDGF and ibrutinib on the expression of the BTK protein and downstream signal transduction in RAJI cells following anti-IgM stimulation. Computational studies revealed that the inhibitory activity of the obtained [60]fullerene derivative is multifaceted: it hampers the BTK active site, interacting directly with the catalytic residues, rendering it inaccessible to phosphorylation, and binds to residues that form the ATP binding pocket. The anticancer activity of produced carbon nanomaterial revealed that it inhibited the BTK protein and its downstream pathways, including PLC and Akt proteins, at the cellular level. The mechanistic studies suggested the formation of autophagosomes (increased gene expression of LC3 and p62) and two caspases (caspase-3 and -9) were responsible for the activation and progression of apoptosis. These data illustrate the potential of fullerene-based BTK protein inhibitors as nanotherapeutics for blood cancer and provide helpful information to support the future development of fullerene nanomaterials as a novel class of enzyme inhibitors.