Organic Inorganic Hybrid Nanocomposites Research Articles

Synthesis and characterization of ureidopyrimidinone-functionalized polyurethane acrylates and their hybrid nanocomposites for UV coating applications

AbstractIn this study, ureidopyrimidinone moieties (UPy), capable of physical crosslinking via quadruple hydrogen bonding, were successfully incorporated into UV-curable polyurethane acrylate prepolymers. First, a hydroxyl-terminated unsaturated ester monomer was synthesized and reacted with isophorone diisocyanate to create a hydroxyl-terminated UV-curable urethane oligomer (U–OH). Then, isocyanate-terminated building blocks (UPy moieties and an acrylate-based photosensitive monomer) were synthesized and used in various ratios to functionalize U–OH for the preparation of a series of UV-curable UPy-containing polyurethane acrylate (PUA) resins. The resulting products were structurally characterized using 1H NMR and FTIR spectroscopy. Furthermore, organic–inorganic hybrid nanocomposites were obtained by introducing silane coupling agents into PUA resins using the sol–gel process. A series of UV-curable UPy-containing PUA coatings and hybrid nanocomposites were prepared, and their synergistic effect on coating properties was investigated. The dynamic mechanical analysis revealed that the Tg of the samples increased with increasing UPy content, although the mechanical properties remained largely unaltered, as shown by the stress–strain test. The studies also demonstrated that the hybrid nanocomposites exhibited higher decomposition temperatures and better thermal stability compared to pure PUAs. All the coatings exhibited good transparency in the visible region. An optical microscope was used to investigate the self-healing property by scratching the plexiglass panels with a razor blade. Among the other samples, the coating with the highest percentage of UPy content exhibited the best self-healing ability after heat treatment at 90 °C for 10 min. Graphical abstract

Novel highly efficient ternary ZnO wrapped PPy-NTs/g-C3N4 nanocomposite as an epoxy coating for corrosion protection

The main goal of this study is to develop an epoxy coating coupled with an organic–inorganic hybrid nanocomposite that can be used as a corrosion-inhibiting pigment on carbon steel. Herein, polypyrrole nanotubes (PPy-NTs), polypyrrole nanotubes/g-C3N4 (PPy-NTs/g-C3N4) and novel nano-composite polypyrrole nanotubes/g-C3N4/ZnO (PGZ) were prepared by facile wet impregnation approach. The developed pigments were investigated using XRD, FTIR, FE-SEM equipped EDS. Electrochemical impedance spectroscopy (EIS) and polarization measurements were used to assess the behavior of the prepared pigments on the anticorrosion performance of epoxy resin coatings. EIS experiments revealed that introducing nano-pigments to neat coatings enhanced the epoxy resin and charge transfer resistance. The anticorrosion performance of the three nano-pigments was assessed as follows: PGZ ˃ PPy-NTs/g-C3N4˃ PPy-NTs.

Advanced Anticorrosive Graphene Oxide-Doped Organic-Inorganic Hybrid Nanocomposite Coating Derived from Leucaena leucocephala Oil.

Metal corrosion poses a substantial economic challenge in a technologically advanced world. In this study, novel environmentally friendly anticorrosive graphene oxide (GO)-doped organic-inorganic hybrid polyurethane (LFAOIH@GO-PU) nanocomposite coatings were developed from Leucaena leucocephala oil (LLO). The formulation was produced by the amidation reaction of LLO to form diol fatty amide followed by the reaction of tetraethoxysilane (TEOS) and a dispersion of GOx (X = 0.25, 0.50, and 0.75 wt%) along with the reaction of isophorane diisocyanate (IPDI) (25-40 wt%) to form LFAOIH@GOx-PU35 nanocomposites. The synthesized materials were characterized by Fourier transform infrared spectroscopy (FTIR); 1H, 13C, and 29Si nuclear magnetic resonance; and X-ray photoelectron spectroscopy. A detailed examination of LFAOIH@GO0.5-PU35 morphology was conducted using X-ray diffraction, scanning electron microscopy, energy-dispersive X-ray spectroscopy, and transmission electron microscopy. These studies revealed distinctive surface roughness features along with a contact angle of around 88 G.U preserving their structural integrity at temperatures of up to 235 °C with minimal loading of GO. Additionally, improved mechanical properties, including scratch hardness (3 kg), pencil hardness (5H), impact resistance, bending, gloss value (79), crosshatch adhesion, and thickness were evaluated with the dispersion of GO. Electrochemical corrosion studies, involving Nyquist, Bode, and Tafel plots, provided clear evidence of the outstanding anticorrosion performance of the coatings.

Designing an efficient organic–inorganic hybrid nanocomposite for simultaneous oxidative/adsorptive desulfurization of model and real fuel oils

In this study, an efficient organic–inorganic hybrid nanocomposite was designed for deep oxidative/adsorptive removal of dibenzothiophene (DBT) from model and real fuel oils employing surface molecularly imprinted polymer (SMIP) and mesoporous silica nanoparticles (MSNs). On the surface of silanol-functionalized MCM-48-HPW prepared at different 12-tungstophosphoric acid (HPW wt%) as the oxidation catalyst, an imprinted polymethacrylic acid polymer (PMAA) as a selective adsorbent of DBT was formed using different amounts of DBT template. Then, various oxidant/sulfur molar ratios were applied during the desulfurization reactions according to the central composite design (CCD). The successful synthesis of the optimum SMIP-PMAA@MCM-48-HPW nanocomposite was confirmed by FTIR, XRD, N2-adsorption, SEM, TEM, TGA, and NMR techniques. The desulfurization percentage of the model oil reached 98.54% under the optimum conditions, and the catalyst percentage was found to be the most significant parameter for desulfurization efficiency. Comparison experiments showed that the combined role of oxidation and adsorption had an extensive impact on desulfurization efficiency. Under the optimized conditions, 96% DBT from gasoline was removed by the optimum nanocomposite. The optimum nanocomposite showed good stability and could be reused five times without a remarkable decrease in the desulfurization ability.

Customized Microenvironments Spontaneously Facilitate Coupled Engineering of Real-Life Large-Scale Clean Water Capture and Pollution Remediation.

Harnessing abundant renewable resources and pollutants on a large scale to address environmental challenges, while providing sustainable freshwater, is a significant endeavour. This study presents the design of fully functional solar vaporization devices (SVD) based on organic-inorganic hybrid nanocomposites (CCMs-x). These devices exhibit efficient photothermal properties that facilitate multitargeted interfacial reactions, enabling simultaneous catalysis of sewage and desalination. The localized interfacial heating generated by the photothermal effect of CCMs-x triggers surface-dominated catalysis and steam generation. The CCMs-x SVD achieves a solar water-vapor generation rate of 1.41kg m-2 h-1 (90.8%), and it achieves over 95% removal of pollutants within 60min under one-sun for practical application. The exceptional photothermal conversion rate of wastewater for environmental remediation and water capture is attributed to customized microenvironments within the system. The integrated parallel reaction system in SVD ensures it is a real-life application in multiple scenarios such as municipal/medical wastewater and brine containing high concentrations. Additionally, the SVD exhibits long-term durability, antifouling functionality toward complex ionic contaminants. This study not only demonstrates a one-stone-two-birds strategy for large-scale direct production of potable water from polluted seawater, but also opens up exciting possibilities for parallel production of energy and water resources.

Preparation of thermally stable organic-inorganic hybrid nanocomposites from chemically functionalized oxidized graphite by in situ catalytic oxidative decarboxylation

ABSTRACT In this study, the preparation of thermally stable organic-inorganic hybrid nanocomposites from chemically functionalized oxidized graphite is carried out by in-situ catalytic oxidative decarboxylation of 3,5-dinitrobenzoic acid (reactant) in the presence of potassium persulfate (oxidant), silver nitrate (catalyst) and graphite (support) under thermal or microwave conditions. The effects of heat transfer and dosages of reactant, catalyst and oxidant on the crystalline structure and the morphology of nanocomposites are studied in detail. The prepared nanocomposites are characterized by EDS, elemental mapping, FE-SEM, FT-IR and XRD. The thermal stability of nanocomposites is examined by TGA and DSC. EDS shows that nanocomposites are composed of C, O, N, S, K and Ag elements. FT-IR exhibits that the graphitic layers in nanocomposites are mainly oxidized and functionalized with carboxyl, carbonyl, hydroxyl, epoxy, sulfate, nitrate and nitroaryl groups. Addition of nitroaryl groups to nanocomposites is also supported by an increase found in their C and N contents. XRD demonstrates the coexistence of both oxidized amorphous carbon and graphite in combination with different levels of organic and inorganic phases. The prepared nanocomposites show good thermal stability. The total area of the DSC curve in these nanocomposites compared to graphite is enhanced.

Development of sustainable polybenzoxazine-based organic–inorganic hybrid nanocomposites for high voltage insulator applications

Development of sustainable polybenzoxazine-based organic–inorganic hybrid nanocomposites for high voltage insulator applications

Active-site-rich binary metal oxides integrated organic–inorganic hybrid nanocomposite: Electrochemical simultaneous detection of multi-drugs of isoprenaline and resorcinol in real samples

In recent years, awareness on human health is increasing, which also increased the use of drugs to efficiently cure or halt the disease. Besides their certain beneficiary effects, it also triggers some alarming conditions in the body when the drug crosses a certain limit. Therefore, there is a need to develop efficient methods to detect the amount of the drug in the human body. In this work, for the first time, we developed a novel zinc manganate incorporated on polydopamine encapsulated reduced graphene oxide hybrid nanocomposite (rGO-pDA-ZnMnO3 HNC) efficient electro-catalyst for the simultaneous electrochemical detection of multi-drugs of Isoprenaline (IP) and Resorcinol (RC). The incorporation of the ZnMnO3 on rGO-pDA sheets indicates excellent conductivity due to its enhanced active sites and high surface area. The rGO-pDA-ZnMnO3 HNC was drop-casted on the surface of GCE and used as a superior electro-catalyst for individual and simultaneous detection of multi-drugs using CV and DPV. The DPV results showed excellent electrochemical performance, like IP and RC in linear ranges (LR) of 0.004 – 85.99 and 0.04 – 27.9 µM and lower limit values (LOD) of 3.1 and 7.1 nM, respectively. Further, the modified GCE has excellent interference capability, repeatability, and stability. Finally, the practical impact was demonstrated in real-time samples of human urine, tap water, and hair dyes. Remarkably, the recovery rate of IP and RC is ∼99 % and ∼98 %, respectively with RSD of less than 3 %, which authenticates the usefulness of the proposed sensor for real-time applications.

Multifunctional Architectures of Cyclic Dipeptide Copolymers and Composites, and Modulation of Multifaceted Amyloid-β Toxicity.

Alzheimer's disease (AD) is a major neurodegenerative disorder primarily characterized by the β-amyloid (Aβ42) misfolding and aggregation-associated multifaceted amyloid toxicity encompassing oxidative stress, neuronal death, and severe cognitive impairment. Modulation of Aβ42 aggregation via various structurally anisotropic macromolecular systems is considered effective in protecting neuronal cells. In this regard, we have developed a cyclic dipeptide (CDP)-based copolymer (CP) and explored its material and biomedical properties. Owing to the structural versatility, CDP-CP forms solvent-dependent anisotropic architectures ranging from dense fibers and mesosheets to vesicles, which are shown to interact with dyes and nanoparticles and mimic synthetic protocells, providing a conceptually new approach to achieve advanced functional materials with the hierarchical organization. CP upon interaction with gold nanoparticles (GNP) and polyoxometalate (POM) generated faceted architectures (CP-GNP) and the nanocomposite (CP-POM), respectively. CP-GNP and CP-POM have shown remarkable ability to inhibit Aβ42 aggregation, dissolve the preformed aggregates, and scavenge reactive oxygen species (ROS) to ameliorate multifaceted amyloid toxicity. In cellulo studies show that CP-GNP and CP-POM protect neuronal cells from Aβ42-induced toxicity and reduce lipopolysaccharide (LPS)-activated neuroinflammation at sub-micromolar concentration. To our knowledge, this is the first report on the hierarchical organization of CDP-CP into 1D-to-2D architectures and their organic-inorganic hybrid nanocomposites to combat the multifaceted amyloid toxicity.

New organotin(IV) complexes with a bis-acyl-hydrazone ligand: Synthesis, crystal structure and immobilization on magnetic mesoporous silica nanoparticles as a strategy in cancer therapy

The new binuclear organotin(IV) complexes, (Me2Sn)2L (1) and (Ph2Sn)2L (2), have been synthesized from reaction of R2SnCl2 (R = Me or Ph) with bis(2-hydroxy-1-naphthaldehyde) Succinic dihydrazone (H4L). The synthesized compounds have been characterized by elemental analysis and IR, 1H NMR, and 119Sn NMR spectroscopy. The structures of 1 have been also determined by X-ray crystallography. Both complexes are binuclear with bis-hydrazone coordinated via enolic and phenolic oxygens and imine nitrogen in two tridentate ONO domains. Dihydrazone ligand and its diphenyltin(IV) complex were also chemically immobalized on functionalized magnetic mesoporous silica nanoparticles. The new organic-inorganic hybrid nanocomposites were characterized by FT‐IR, PXRD, BET, TGA, VSM, FE‐SEM, HRTEM and EDX techniques. Then, the in vitro cytotoxicity of the synthesized compounds against A549 cancer cell lines was evaluated. Diphenyltin(IV)-loaded magnetic mesoporous silica nanoparticles, Fe3O4@mSiO2-SnPh2, displayed the highest cytotoxic activity compared to other nanoparticles and also was able to reduce the cell viability in a more efficient manner in comparison with the free (Ph2Sn)2L. The inverted microscopy morphology and acridine orange staining indicate that A549 cells progress to cell death after being treated with Fe3O4@mSiO2-SnPh2 nanoparticles.

Organic–inorganic hybrid nanocomposites for the photoreduction of CO2: environment and energy technologies

Organic–inorganic hybrid nanocomposites for the photoreduction of CO2: environment and energy technologies

Engineering the Properties of Transparent Hybrid Coating toward High Hardness, Excellent Flexibility, and Multifunction.

Transparent functional coatings with glass-like hardness and polymer-like flexibility are highly desirable for flexible and foldable displays. Although several coatings have been developed toward this goal, achieving a functional coating with 9H pencil hardness and extremely low bending radius of curvature (rc) remains a great challenge due to the inherent conflict between hardness and flexibility. To overcome this trade-off, a facile strategy is developed herein. The coating is an organic-inorganic hybrid nanocomposite that is prepared from thiol-acrylate polymerization of acrylo polyhedral oligomeric silsesquioxane and multifunctional thiols. The former provides the desired hardness, while the latter affords high flexibility and the maximum level of chemical bonding for organic-inorganic phases. Because of the good miscibility and varied functionality of monomers, we are able to manipulate the composition and internal structure of coating systematically, endowing it with high transparency (98%, 550 nm), super hardness (9H), excellent low modulus (1.85 GPa, the most flexible one to date), and the ability to withstand steel wool's abrasion and repeated bending (rc = 0.8 mm) 10 000 times on PET film. On the final coating, both antifouling and antibacterial abilities are integrated without sacrificing its other properties after postfunctionalizing a zwitterionic layer. This work balances the hardness-flexibility conflict effectively and provides some useful protective coatings for next-generation displays.

Experimental Insights into Mesoporous Polyaniline-Based Nanocomposites for Anionic and Cationic Dye Removal.

This work presents the preparation of inorganic-organic hybrid nanocomposites, namely three-dimensional polyaniline (Pani)/activated silica gel (ASG) (3D Pani@ASG), their characterization, and in removing application as a potential adsorbent for cationic brilliant green (BG), crystal violet (CV), and anionic Congo red (CR), and methyl orange (MO) dyes. Pani@ASG nanocomposites have been prepared by the in situ polymerization method and characterized using various techniques such as Fourier transform infrared (FTIR), X-ray diffraction (XRD), field-emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM) with selected area electron diffraction, thermogravimetric analysis with derivative thermogravimetry, zeta potential analyses, and Brunauer-Emmett-Teller (BET). The scanning electron microscopy (SEM) study confirms the average particle size of the Pani@ASG nanocomposite is in the range of 5 nm. FESEM, TEM, FTIR, and XRD analysis proved the successful decoration of ASG over Pani. The BET result of Pani@ASG shows a mesoporous nature with a pore diameter of less than 3 nm and a surface area of 423.90 m2 g-1. Both SEM and TEM analyses show the proportional distribution of ASG over Pani's surface. The adsorption trend of BG and MO on the studied materials at pH 7 was found as follows: Pani@ASG > Pani > ASG. The highest sorption capacities of MO and BG on Pani@ASG were 161.29 and 136.98 mg/g (T = 298.15 K, and Pani@ASG dose: 0.04 g for MO and 0.06 g for BG), which were greater compared with bare Pani and bare ASG, respectively. The interaction mechanism behind the adsorption of BG and MO dyes onto the Pani@ASG nanocomposite includes electrostatic interaction, π-π interaction, and hydrogen bonding. The mechanistic pathway and the interactions between the targeted dyes and Pani@ASG were further studied using adsorption isotherm, adsorption kinetics, and thermodynamics.

Fluoropolymer-based hybrid superhydrophobic nanocomposite coating with antifouling and self-cleaning properties for efficient oil/water separation

The production of industrial and domestic effluents possessing oily contaminated water has become a global concern as a result of environmental contamination and pollution. Newly synthesized organic-inorganic hybrid nanocomposites with special wetting and anti-wetting properties have been adopted in recent times to address this problem. However, this method has faced a few setbacks in curbing the situation, which leaves the problem persistent. In order to realize the full potential of hybrid composites in combating oil/water contamination, we synthesize a robust organic-inorganic superhydrophobic hybrid nanocomposite containing Polyvinylidene fluoride (PVDF) and silicon hydroxide (SiO2) to coat cellulose filter paper for effective and efficient separation of oil/water mixtures. With a simple dip-coating technique, the superhydrophobic hybrid composite obtain a superhydrophobicity with a water contact angle as high as 161˚ on the filter paper. The coated membrane possessed a robust mechanical property as well as chemical stability which withstands a sandpaper abrasion test of up to 80 cycles and could retain its superhydrophobicity in acidic, neutral and alkaline media after 24hrs of immersion respectively. Moreover, the coated surface possessed nanopores which allows it to be used in oil water separation applications both under pressure and gravity with a separation efficiency of up to 99.7 % and can also be recycled many times for use. The excellent antifouling and self-cleaning ability of the coated membrane also prevents the adhesion of contaminants from the surface. The outstanding performance of the facilely and cost-effective fabricated superhydrophobic hybrid composite reveals a great potential for curbing the problems of oil contamination while addressing some existing barriers to the full potential realization of hybrid composites.

Synthesis and characterization of a new hybrid nanocomposite based on di-substituted heteropolyanion-quantum dots as a high-performance nanocatalyst for organic dye removal from wastewater

In this manuscript, a new hybrid nanocatalyst (PMo10Ni2/ZnS@CS) based on di-substituted heteropolyanion (PMo10Ni2) and ZnS quantum dot was synthesized via the hydrothermal method. PMo10Ni2/ZnS@CS is a candidate for removal of environmental pollutants. The synthesized hybrid nanocatalyst was analyzed by TEM, UV-vis, FT-IR, XRD, and EDX techniques. The results of XRD analysis showed the average crystallite size of the PMo10Ni2/ZnS@CS nanocomposite particles is about 33 nm, which was consistent with the TEM results. The nano-catalytic activity of PMo10Ni2/ZnS@CS hybrid nanocomposite was investigated in photocatalytic decolorization of organic dyes. The experimental results showed that the inorganic-organic hybrid nanocomposite (PMo10Ni2/ZnS@CS) had excellent photocatalytic efficiency with 98% dye removal. The recovery of the photocatalyst in the decolorization process was investigated and the results indicate a reduction of photocatalytic power after the second and third stage recovery, respectively. In the present study, PMo10Ni2/ZnS@CS was proposed as a heterogeneous nanocatalyst with broad nanocatalytic applications of dye removal.

Morphological investigation of ternary and semicrystalline organic–inorganic hybrid nanocomposite

Morphological investigation of ternary and semicrystalline organic–inorganic hybrid nanocomposite

Nanoengineered biomimetic hydrogels: A major advancement to fabricate 3D-printed constructs for regenerative medicine.

Nanostructured compounds already validated as performant reinforcements for biomedical applications together with different fabrication strategies have been often used to channel the biophysical and biochemical features of hydrogel networks. Ergo, a wide array of nanostructured compounds has been employed as additive materials integrated with hydrophilic networks based on naturally-derived polymers to produce promising scaffolding materials for specific fields of regenerative medicine. To date, nanoengineered hydrogels are extensively explored in (bio)printing formulations, representing the most advanced designs of hydrogel (bio)inks able to fabricate structures with improved mechanical properties and high print fidelity along with a cell-interactive environment. The development of printing inks comprising organic-inorganic hybrid nanocomposites is in full ascent as the impact of a small amount of nanoscale additive does not translate only in improved physicochemical and biomechanical properties of bioink. The biopolymeric nanocomposites may even exhibit additional particular properties engendered by nano-scale reinforcement such as electrical conductivity, magnetic responsiveness, antibacterial or antioxidation properties. The present review focus on hydrogels nanoengineered for 3D printing of biomimetic constructs, with particular emphasis on the impact of the spatial distribution of reinforcing agents (0D, 1D, 2D). Here, a systematic analysis of the naturally-derived nanostructured inks is presented highlighting the relationship between relevant length scales and size effects that influence the final properties of the hydrogels designed for regenerative medicine.

Environmental gas sensors based on electroactive hybrid organic-inorganic nanocomposites using nanostructured materials.

Advanced gas sensing devices are urgently demanded in the modern scientific world to control air pollution and protect human life. For this purpose, semiconducting electroactive materials can revolutionize the idea of conventional gas sensors. Chemi-resistive gas sensors based on electroactive hybrid organic-inorganic nanocomposites are incredibly promising gas sensing materials because they possess the advantages of excellent selectivity, high sensitivity, low response time, repeatability, high stability, cost-effectiveness, and simple fabrication techniques, and they can be operated at room temperature. This review emphasizes the recent developments of organic-inorganic hybrid nanocomposite-based electroactive gas sensors, including metal oxide nanocomposites, which are potential gas sensing materials due to the presence of numerous charge carriers. The review also focuses on nanostructured materials of different dimensions, such as semiconducting quantum dots, carbon dots, nanotubes, nanowires, and nanosheets, used for developing these gas sensing compounds and their significance and challenges. Some possible fabrication techniques for developing efficient gas sensors with different morphologies are discussed, with their probable sensing mechanism behind the detection of toxic vapours. Subsequently, a summary and possible outcome of this study, along with the various achievements and prospects in this field, are also discussed.

An Activatable Hybrid Organic-Inorganic Nanocomposite as Early Evaluation System of Therapy Effect.

Delays in evaluating cancer response to radiotherapy (RT) usually reduce therapy effect or miss the right time for treatment optimization. Hence, exploring timely and accurate methods enabling one to gain insights of RT response are highly desirable. In this study, we have developed an apoptosis enzyme (caspase-3) activated nanoprobe for early evaluation of RT efficacy. The nanoprobe bridged the nanogapped gold nanoparticles (AuNNPs) and the second near-infrared window (NIR-II) fluorescent (FL) molecules (IR-1048) through a caspase-3 specific peptide sequence (DEVD) (AuNNP@DEVD-IR1048). After X-ray irradiation, caspase-3 was activated to cut DEVD, turning on both NIR-II FL and PA imaging signals. The increased NIR-II FL/PA signals exhibited a positive correlation with the content of caspase-3. Moreover, the amount of the activated caspase-3 was negatively correlated with the tumor size. The results underscore the role of the caspase-3 activated by X-ray irradiation in bridging the imaging signals variation and tumor inhibition rate. Overall, activatable NIR-II FL/PA imaging was successfully used to timely predict and evaluate the RT efficacy. The evaluation system based on biomarker-triggered living imaging has the capacity to guide treatment decisions for numerous cancer types.

An Activatable Hybrid Organic–Inorganic Nanocomposite as Early Evaluation System of Therapy Effect

AbstractDelays in evaluating cancer response to radiotherapy (RT) usually reduce therapy effect or miss the right time for treatment optimization. Hence, exploring timely and accurate methods enabling one to gain insights of RT response are highly desirable. In this study, we have developed an apoptosis enzyme (caspase‐3) activated nanoprobe for early evaluation of RT efficacy. The nanoprobe bridged the nanogapped gold nanoparticles (AuNNPs) and the second near‐infrared window (NIR‐II) fluorescent (FL) molecules (IR‐1048) through a caspase‐3 specific peptide sequence (DEVD) (AuNNP@DEVD‐IR1048). After X‐ray irradiation, caspase‐3 was activated to cut DEVD, turning on both NIR‐II FL and PA imaging signals. The increased NIR‐II FL/PA signals exhibited a positive correlation with the content of caspase‐3. Moreover, the amount of the activated caspase‐3 was negatively correlated with the tumor size. The results underscore the role of the caspase‐3 activated by X‐ray irradiation in bridging the imaging signals variation and tumor inhibition rate. Overall, activatable NIR‐II FL/PA imaging was successfully used to timely predict and evaluate the RT efficacy. The evaluation system based on biomarker‐triggered living imaging has the capacity to guide treatment decisions for numerous cancer types.