Photothermal Effect Research Articles

Multifunctional and Sprayable 2D MoS2/Silk Sericin Bio-Nanocomposite Dressings with Enhanced Photothermal Effect for Infected Wound Healing

Multifunctional and Sprayable 2D MoS2/Silk Sericin Bio-Nanocomposite Dressings with Enhanced Photothermal Effect for Infected Wound Healing

The Role of Photo in Oxygen Evolution Reaction: A Review.

Photo enhanced oxygen evolution reaction has recently emerged as an advanced strategy with great application prospects for highly efficient energy conversion and storage. In the course of photo enhanced oxygen evolution reactions, the other works focus has predominantly centered on catalysts while inadvertently overlooking the pivotal role of photo. Consequently, this manuscript embarks upon a comprehensive review of recent advancements in photo-driven, aiming to illuminate this critical dimension. A detailed introduction to the photothermal effect, photoelectronic effect, photon-induced surface plasmon resonance, photo and heterojunction, photo-induced reversible geometric conversion, photo-induced energy barrier reduction, photo-induced chemical effect, photo-charging, and the synthesis of laser/photo-assisted catalysts, offering prospects for the development of each case is provided. A detailed introduction to the photothermal effect, photoelectronic effect, photon-induced surface plasmon resonance, photo and heterojunction, photo-induced reversible geometric conversion, photo-induced energy barrier reduction, photo-induced chemical effect, photo-charging, and the synthesis of laser/photo-assisted catalysts is provided. At the same time, the overpotential and Tafel slope of some catalysts mentioned above at 10mAcm-2 is collected, and calculated the lifting efficiency of light on them, offering prospects for the development of each case.

Cellular Trojan Horse initiates bimetallic Fe-Cu MOF-mediated synergistic cuproptosis and ferroptosis against malignancies.

Disruptions in metal balance can trigger a synergistic interplay of cuproptosis and ferroptosis, offering promising solutions to enduring challenges in oncology. Here, we have engineered a Cellular Trojan Horse, named MetaCell, which uses live neutrophils to stably internalize thermosensitive liposomal bimetallic Fe-Cu MOFs (Lip@Fe-Cu-MOFs). MetaCell can instigate cuproptosis and ferroptosis, thereby enhancing treatment efficacy. Mirroring the characteristics of neutrophils, MetaCell can evade the immune system and not only infiltrate tumors but also respond to inflammation by releasing therapeutic components, thereby surmounting traditional treatment barriers. Notably, Lip@Fe-Cu-MOFs demonstrate notable photothermal effects, inciting a targeted release of Fe-Cu-MOFs within cancer cells and amplifying the synergistic action of cuproptosis and ferroptosis. MetaCell has demonstrated promising treatment outcomes in tumor-bearing mice, effectively eliminating solid tumors and forestalling recurrence, leading to extended survival. This research provides great insights into the complex interplay between copper and iron homeostasis in malignancies, potentially paving the way for innovative approaches in cancer treatment.

Hydrogen Bonding-Induced Aggregation of Chiral Functionalized AuNS@Ag NPs for Photothermal Enantioanalysis.

Toward the challenges of signaling transduction amplified in enantioselective recognition, we herein devised an innovative strategy for highly selective recognition of amino acids and their derivatives, leveraging photothermal effects. In this approach, bifunctional l-ascorbic acid is employed to reduce silver ions in situ on Au nanostars. Simultaneously, its oxidate (l-dehydroascorbic acid) is bonded to the silver shell as a chiral selector to prepare chiral nanoparticles (C-AuNS@Ag NPs) with the ability to recognize stereoisomers and sensitively modulate the photothermal effect. l-Dehydroascorbic acid can selectively capture one of the enantiomers of the two forms through hydrogen bonding and drive aggregation of the nanoparticles, which sharply enhances the photothermal effect. Consequently, the two forms of the system exhibit a significant temperature difference, which enables the discrimination and quantification of enantiomers. Our strategy verifies that six chiral amino acids and their derivatives can be discriminated with enantioselective response values of up to 79. Additionally, the chiral recognition mechanism was revealed through density functional theory (DFT) calculations, providing a paradigm shift in the development of enantiomeric recognition strategies.

Exosome-Coated Prussian Blue Nanoparticles for Specific Targeting and Treatment of Glioblastoma.

Glioblastoma is one of the most aggressive and invasive types of brain cancer with a 5-year survival rate of 6.8%. With limited options, patients often have poor quality of life and are moved to palliative care after diagnosis. As a result, there is an extreme need for a novel theranostic method that allows for early diagnosis and noninvasive treatment as current peptide-based delivery standards may have off-target effects. Prussian Blue nanoparticles (PBNPs) have recently been investigated as photoacoustic imaging (PAI) and photothermal ablation agents. However, due to their inability to cross the blood-brain barrier (BBB), their use in glioblastoma treatment is limited. By utilizing a hybrid, biomimetic nanoparticle composed of a PBNP interior and a U-87 cancer cell-derived exosome coating (Exo:PB), we show tumor-specific targeting within the brain and selective thermal therapy potential due to the strong photoconversion abilities. Particle characterization was carried out and showed a complete coating around the PBNPs that contains exosome markers. In vitro cellular uptake patterns are similar to native U-87 exosomes and when exposed to an 808 nm laser, show localized cell death within the specified region. After intravenous injection of Exo:PB into subcutaneously implanted glioblastoma mice, they have shown effective targeting and eradication of tumor volume compared to PEG-coated PBNPs (PEG:PB). Through systemic administration of Exo:PB particles into orthotopic glioblastoma-bearing mice, the PBNP signal was detected in the brain tumor region through PAI. It was seen that Exo:PB had preferential tumor accumulation with less off-targeting compared to the RGD:PB control. Ex vivo analysis validated specific targeting with a direct overlay of Exo:PB with the tumor by both H&E staining and Ki67 labeling. Overall, we have developed a novel biomimetic material that can naturally cross the BBB and act as a theranostic agent for systemic targeting of glioblastoma tissue and photothermal therapeutic effect.

Realizing Ultrasensitive and Accurate Point-of-Care Profiling for ATP with a Triple-Mode Strategy Based on the ATP-Induced Reassembly of a Copper Coordination Polymer Nanoflower.

New strategies for accurate and reliable detection of adenosine triphosphate (ATP) with portable devices are significant for biochemical analysis, while most recently reported approaches cannot satisfy the detection accuracy and independent of large instruments simultaneously, which are unsuitable for fast, simple, and on-site ATP monitoring. Herein, a unique, convenient, and label-free point-of-care sensing strategy based on novel copper coordination polymer nanoflowers (CuCPNFs) was fabricated for multimode (UV-vis, photothermal, and RGB values) onsite ATP determination with high selectivity, sensitivity, and accuracy. The resulting CuCPNFs with a 3D hierarchical structure exhibit the ATP-triggered decomposition behavior because the competitive coordination between ATP and the copper ions of CuCPNFs can result in the formation of ATP-Cu, which reveals preeminent peroxidase mimics activity and can accelerate the oxidation of 3, 3', 5, 5'-tetramethylbenzidine (TMB) to form oxTMB. During this process, the detection system displayed not only color changes but also a strong NIR laser-driven photothermal effect. Thus, the photothermal and color signal variations are easily monitored by a portable thermometer and a smartphone. This multimode point-of-care platform can meet the requirements of onsite, without bulky equipment, accuracy, and reliability all at once, greatly enhancing its application in practice and paving a new way in ATP analysis.

The Influence of Light-Generated Radicals for Highly Efficient Solar-Thermal Conversion in an Ultra-Stable 2D Metal-Organic Assembly.

Solar-thermal water evaporation is a promising strategy for clean water production, which needs the development of solar-thermal conversion materials with both high efficiency and high stability. Herein, we reported an ultra-stable cobalt(II)-organic assembly NKU-123 with light-generated radicals, exhibiting superior photothermal conversion efficiency and high stability. Under the irradiation of 808 nm light, the temperature of NKU-123 rapidly increases from 25.5 to 215.1 °C in 6 seconds. The solar water evaporator based on NKU-123 achieves a high solar-thermal water evaporation rate of 1.442 and 1.299 kg m-2 h-1 under 1-sun irradiation with a water evaporation efficiency of 97.8 and 87.9 % for pure water and seawater, respectively. A detailed mechanism study revealed that the formation of light-generated radicals leads to an increase of spin density of NKU-123 for enhancing the photothermal effect, which provides insights into the design of highly efficient photothermal materials.

A thermoresponsive nanocomposite integrates NIR-II-absorbing small molecule with lonidamine for pyroptosis-promoted synergistic immunotherapy

Photothermal immunotherapy is regarded as the ideal cancer therapeutic modality to against malignant solid tumors; however, its therapeutic benefits are often modest and require improvement. In this study, a thermoresponsive nanoparticle (BTN@LND) composed of a photothermal agent (PTA) and pyroptosis inducer (lonidamine) were developed to enhance immunotherapy applications. Specifically, our “two-step” donor engineering strategy produced the strong NIR-II-absorbing organic small-molecule PTA (BTN) that exhibited high NIR-II photothermal performance (ε1064 = 1.51 × 104 M−1 cm−1, η = 75.8%), and this facilitates the diagnosis and treatment of deep tumor tissue. Moreover, the fabricated thermally responsive lipid nanoplatform based on BTN efficiently delivered lonidamine to the tumor site and achieved spatiotemporal release triggered by the NIR-II photothermal effect. In vitro and in vivo experiments demonstrated that the NIR-II photothermal therapy (PTT)-mediated on-demand release of cargo effectively faciliated tumor cell pyroptosis, thereby intensifying the immunogenic cell death (ICD) process to promote antitumor immunotherapy. As a result, this intelligent component bearing photothermal and chemotherapy can maximally suppress the growth of tumors, thus providing a promising approach for pyroptosis/NIR-II PTT synergistic therapy against tumors.Graphical

The Influence of Light‐Generated Radicals for Highly Efficient Solar‐Thermal Conversion in an Ultra‐Stable 2D Metal‐Organic Assembly

AbstractSolar‐thermal water evaporation is a promising strategy for clean water production, which needs the development of solar‐thermal conversion materials with both high efficiency and high stability. Herein, we reported an ultra‐stable cobalt(II)‐organic assembly NKU‐123 with light‐generated radicals, exhibiting superior photothermal conversion efficiency and high stability. Under the irradiation of 808 nm light, the temperature of NKU‐123 rapidly increases from 25.5 to 215.1 °C in 6 seconds. The solar water evaporator based on NKU‐123 achieves a high solar‐thermal water evaporation rate of 1.442 and 1.299 kg m−2 h−1 under 1‐sun irradiation with a water evaporation efficiency of 97.8 and 87.9 % for pure water and seawater, respectively. A detailed mechanism study revealed that the formation of light‐generated radicals leads to an increase of spin density of NKU‐123 for enhancing the photothermal effect, which provides insights into the design of highly efficient photothermal materials.

Roll-to-Roll Manufacturing of Breathable Superhydrophobic Membranes.

Self-cleaning and anti-biofouling are both advantages for lotus-leaf-like superhydrophobic surfaces. Methods for creating superhydrophobicity, including chemical bonding low surface energy molecular fragments and constructing surface morphology with protrusions, micropores, and trapped micro airbags by traditional physical strategies, unfortunately, have encountered challenges. They often involve complex synthesis processes, stubborn chemical accumulation, brutal degradation, or infeasible calculation and imprecise modulation in fabricating hierarchical surface roughness. Here, a scalable method to prepare high-quality, breathable superhydrophobic membranes is proposed by developing a successive roll-to-roll laser manufacturing technique, which offers advantages over conventional fabrication approaches in enabling automatically large-scale production and ensuring cost-effectiveness. Nanosecond laser writing and femtosecond laser drilling produce surface microstructures and micropore arrays, respectively, endowing the membrane with superior antiwater capability with hierarchical microstructures forming a barrier and blocking water infiltration. The membrane's breathability is carefully optimized by tailoring micropore arrays to allow for the adequate passage of water vapor while maintaining superhydrophobicity. These membranes combine the benefits of anti-aqueous corrosive liquid behaviors, photothermal effects, thermoplastic properties, and stretchable performances as promising comprehensive materials in diverse scenes.

A Green Synthesis of Au-Ag Alloy Nanoparticles using Polydopamine Chemistry: Evaluation of their Anticancer Potency Towards Both MCF-7 Cells and their Cancer Stem Cells Subgroup.

Limited chemotherapy efficacy and cancer stem cells (CSCs)-induced therapeutic resistance are major difficulties for tumour treatment. Adopting more efficient therapies to eliminate bulk-sensitive cancer cells and resistant CSCs is urgently needed. Based on the potential and functional complementarity of gold and silver nanoparticles (AuNPs or AgNPs) on tumour treatment, bimetallic NPs (alloy) have been synthesized to obtain improved or even newly emerging bioactivity from a combination effect. This study reported a facile, green and economical preparation of Au-Ag alloy NPs using biocompatible polydopamine (PDA) as a reductant, capping, stabilizing and hydrophilic agent. These alloy NPs were quasi-spherical with rough surfaces and recorded in diameters of 80 nm. In addition, these alloy NPs showed good water dispersity, stability and photothermal effect. Compared with monometallic counterparts, these alloy NPs demonstrated a dramatically enhanced cytotoxic/pro-apoptotic/necrotic effect towards bulk-sensitive MCF-7 and MDA-MB-231 cells. The underlying mechanism regarding the apoptotic action was associated with a mitochondria-mediated pathway, as evidenced by Au3+/Ag+ mediated Mitochondria damage, ROS generation, DNA fragmentation and upregulation of certain apoptotic-related genes (Bax, P53 and Caspase 3). Attractively, these Au-Ag alloy NPs showed a remarkably improved inhibitory effect on the mammosphere formation capacity of MCF-7 CSCs. All the positive results were attributed to incorporated properties from Au, Ag and PDA, the combination effect of chemotherapy and photothermal therapy and the nano-scaled structure of Au-Ag alloy NPs. In addition, the high biocompatibility of Au-Ag alloy NPs supported them as a good candidate in cancer therapy.

Photo-thermal catalysis for sustainable energy production and environmental treatment

Photo-thermal-catalysts (PTC) exceptional features and ability to concurrently solve sustainable energy requirements and environmental problems have drawn scientific interest. The photo-thermal effect is the process by which photo-thermal conversion materials transform radiant energy from light into thermal energy. The photo-thermal therapy of energy and environmental treatment faces the urgent task of developing effective photo-thermal agents to address complicated problem demands. In this study, we take a look at the fundamental principles and underlying process of photo-thermal material catalysis. In addition, this review provides a concise summary of the most up-to-date findings concerning photo-thermal catalysis materials, which have been aggressively researched for a wide-spread sustainable energy and environment treatment uses. In order to motivate the creation of a high-efficiency photo-thermal catalytic pathway, the criteria and techniques for designing photo-thermal catalysts are presented. This will make it possible for a better absorption of the whole spectrum of solar energy as well as a greater conversion of solar energy to heat. Theoretical direction is offered for the continued development of this technology, and the promise of the practical use of photo-thermal catalysis for different solar-driven interfacial photo-thermal conversion technologies is anticipated. This paper offers a unique perspective on photo-thermal catalysis focussing on the synergistic effects and suggesting a potential route for future applications.

Composite Microparticles from Microfluidics for Chemo-/Photothermal Therapy of Hepatocellular Carcinoma.

Hydrogel microcarrier-based drug delivery systems are of great value in the combination therapy of tumors. Current research directions concentrate on the development of more economic, convenient, and effective combined therapeutic platforms. Herein, we developed novel adhesive composite microparticles (MPPMD) with combined chemo- and photothermal therapy ability via microfluidic electrospray technology for local hepatocellular carcinoma treatment. These composite microparticles consisted of doxorubicin (DOX)-loaded and polydopamine-wrapped mesoporous silicon and alginate. Benefiting from such a strategy of hierarchical structure drug loading, DOX could be gradually released from the system, effectively avoiding the direct toxicity of chemotherapeutics to the body. Additionally, the designed microparticles could not only effectively treat tumors by releasing the chemotherapy drug DOX but also show excellent photothermal properties under the irradiation of near-infrared light, achieving combined chemo- and photothermal treatment effects. Based on these advantages, the MPPMD could remarkably eliminate tumor cells in vitro and enormously restrict tumor development in vivo. These results illustrate that such composite microparticles are ideal combination treatment platforms, possessing promising expectations for cancer therapy.

A photo-responsive self-healing hydrogel loaded with immunoadjuvants and MoS2 nanosheets for combating post-resection breast cancer recurrence.

Tumor recurrence after surgical resection remains a significant challenge in breast cancer treatment. Immune checkpoint blockade therapy, as a promising alternative therapy, faces limitations in combating tumor recurrence due to the low immune response rate. In this study, we developed an implantable photo-responsive self-healing hydrogel loaded with MoS2 nanosheets and the immunoadjuvant R837 (PVA-MoS2-R837, PMR hydrogel) for in situ generation of tumor-associated antigens at the post-surgical site of the primary tumor, enabling sustained and effective activation of the immune response. This PMR hydrogel exhibited potential for near-infrared (NIR) light response, tissue adhesion, self-healing, and sustained adjuvant release. When implanted at the site after tumor resection, NIR irradiation triggered a photothermal effect, resulting in the ablation of residual cancer cells. The in situ-generated tumor-associated antigens promoted dendritic cell (DC) maturation. In a mouse model, PMR hydrogel-mediated photothermal therapy combined with immune checkpoint blockade effectively inhibited the recurrence of resected tumors, providing new insights for combating post-resection breast cancer recurrence.

Tensile Strain‐Mediated Bimetallene Nanozyme for Enhanced Photothermal Tumor Catalytic Therapy

Nanozymes have demonstrated significant potential in combating malignant tumor proliferation through catalytic therapy. However, the therapeutic effect is often limited by insufficient catalytic performance. In this study, we propose the utilization of strain engineering in metallenes to fully expose the active regions due to their ultrathin nature. Here, we present the first report on a novel tensile strain‐mediated local amorphous RhRu (la‐RhRu) bimetallene with exceptional intrinsic photothermal effect and photo‐enhanced multiple enzyme‐like activities. Through geometric phase analysis, electron diffraction profile, and X‐ray diffraction, it is revealed that crystalline–amorphous heterophase boundaries can generate approximately 2% tensile strain in the bimetallene. The ultrathin structure and in‐plane strain of the bimetallene induce an amplified strain effect. Both experimental and theoretical evidence support the notion that tensile strain promotes multiple enzyme‐like activities. Functioning as a tumor microenvironment (TME)‐responsive nanozyme, la‐RhRu exhibits remarkable therapeutic efficacy both in vitro and in vivo. This work highlights the tremendous potential of atomic‐scale tensile strain engineering strategy in enhancing tumor catalytic therapy.

Tensile Strain-Mediated Bimetallene Nanozyme for Enhanced Photothermal Tumor Catalytic Therapy.

Nanozymes have demonstrated significant potential in combating malignant tumor proliferation through catalytic therapy. However, the therapeutic effect is often limited by insufficient catalytic performance. In this study, we propose the utilization of strain engineering in metallenes to fully expose the active regions due to their ultrathin nature. Here, we present the first report on a novel tensile strain-mediated local amorphous RhRu (la-RhRu) bimetallene with exceptional intrinsic photothermal effect and photo-enhanced multiple enzyme-like activities. Through geometric phase analysis, electron diffraction profile, and X-ray diffraction, it is revealed that crystalline-amorphous heterophase boundaries can generate approximately 2% tensile strain in the bimetallene. The ultrathin structure and in-plane strain of the bimetallene induce an amplified strain effect. Both experimental and theoretical evidence support the notion that tensile strain promotes multiple enzyme-like activities. Functioning as a tumor microenvironment (TME)-responsive nanozyme, la-RhRu exhibits remarkable therapeutic efficacy both in vitro and in vivo. This work highlights the tremendous potential of atomic-scale tensile strain engineering strategy in enhancing tumor catalytic therapy.

Tailoring Photoweldable Shape Memory Polyurethane with Intrinsic Photothermal / Fluorescence Via Engineering Metal‐Phenolic Systems

AbstractMultifunctional shape memory polymers are significant for next‐generation intelligent systems as smart materials. However, their practical applications are limited by toughness, manufacturability, and functional integration strategies. Besides, while 4D printing is used to construct deformable devices, the limited accessible shapes and difficulty of integrating multiple materials hindered the development of multifunctional devices. Herein, metal‐phenolic coordination is used as crosslinks to tailor tough shape memory polyurethanes with intrinsic photothermal effect and/or tunable fluorescence. The reversible dissociation of metal‐phenolic complexes upon loading provides an efficient energy dissipation for the polymer network. The photothermal/fluorescent properties of target polyurethane can be effortlessly programmed by changing the coordinated metals and functional ligands. The obtained fluorescent polyurethane displays tunable fluorescence through the reversible dissociation‐association of dynamic bonds upon thermal stimulus. Moreover, relying on light‐triggered hybrid exchange reactions among various metal‐phenolic coordination bonds, heterogeneous interfaces can be merged to manufacture exquisite 3D shape‐shifting devices and integrate more advanced functions. As demonstrations, intrinsic photothermal‐responsive shape memory stent, and 3D fluorescent encryption device are produced based on photo‐welding instead of 4D printing. This study not only provides a convenient supramolecular strategy for constructing multifunctional smart materials but also demonstrates a feasible method for making personalized integrated architectures.

Anti-ROS and NIR-II-responsive Hyaluronic Acid Microneedle Loaded with Baicalin Nanoparticles for Treatment of Psoriasis.

In the work, we designed a natural medicine baicalin for the treatment of psoriasis with the aid of hyaluronic acid (HA)-based MNs patches. In order to improve the solubility of baicalin and increase its residence time in infected part, which was made into nanoparticles by complexation with humic acid and Eu2+. The baicalin nanoparticles loaded-MNs exhibited satisfactory rigidity, minimum injury, and controlled drug delivery. The anti-reactive oxygen species (anti-ROS) and anti-inflammatory action were verified by the effective scavenging oxygen and nitrogen radicals. In addition, the loading of baicalin nanoparticles brought remarkable photothermic effect to the MNs, enabled the device to release a controlled drug under near-infrared region II (NIR-II) laser irradiation. With the aid of NIR-II laser, the baicalin-mediated treatment of psoriasis was significant improved by expediting radical scavenging and suppressing inflammation. The design of baicalin MNs provided a new idea for the treatment of chronic disease. This article is protected by copyright. All rights reserved.

An innovative stepwise activated coupling reaction for fabricating functional fluorescence probes with potential photosensitive applications

Coupling bright organic emitters with biocomponents such as proteins and amino acids to fabricate biocompatible optical functional materials is receiving increasing attention. Previous reports of an efficient, typical reaction between maleic anhydride (MAH) and amino groups indicated that MAH derivatives have great potential for bioconjugation applications. However, the obstacle of complex synthesis methods and weak fluorescence to this kind of derivative structures based on MAH, have greatly limited their applications. Herein, an innovative strategy was developed based on stepwise activated coupling via a multi-step process. First, a series of donor–acceptor emitting frameworks was constructed by introducing different commercially available electron donors into the electron-withdrawing squaric acid core. Then, these frameworks were further activated to obtain different 3,4-diaryl MAH precursors for bioconjugation, which contributed to a novel light-triggered ring-enlargement effect. Importantly, the MAH precursors triggered catalyst-free coupling reactions at ambient temperature with organic small molecules and biological macromolecules containing primary amine groups. Different fluorescent precursors and abundant biological components were effectively combined, and a water-soluble, biocompatible photosensitizer with efficient photodynamic and photothermal therapy effects was obtained. This strategy is expected to have great potential for biological imaging and theragnostic applications.

Single‐Atom Titanium on Mesoporous Nitrogen, Oxygen‐Doped Carbon for Efficient Photo‐thermal Catalytic CO2 Cycloaddition by a Radical Mechanism

Developing efficient and earth‐abundant catalysts for CO2 fixation to high value‐added chemicals is meaningful but challenging. Styrene carbonate has great market value, but the cycloaddition of CO2 to styrene oxide is difficult due to the high steric hindrance and weak electron‐withdrawing ability of the phenyl group. To utilize clean energy (such as optical energy) directly and effectively for CO2 value‐added process, we introduce earth‐abundant Ti single‐atom into the mesoporous nitrogen, oxygen‐doped carbon nanosheets (Ti‐CNO) by a two‐step method. The Ti‐CNO exhibits excellent photothermal catalytic activities and stability for cycloaddition of CO2 and styrene oxide to styrene carbonate. Under light irradiation and ambient pressure, an optimal Ti‐CNO produces styrene carbonate with a yield of 98.3%, much higher than CN (27.1%). In addition, it shows remarkable stability during 10 consecutive cycles. Its enhanced catalytic performance stems from the enhanced photothermal effect and improved Lewis acidic/basic sites exposed by the abundant mesopores. The experiments and theoretical simulations demonstrate the styrene oxide•+ and CO2•‐ radicals generated at the Lewis acidic (Tiδ+) and basic sites of Ti‐CNO under light irradiation, respectively. This work furnishes a strategy for synthesizing advanced single‐atom catalysts for photo‐thermal synergistic CO2 fixation to high value products via a cycloaddition pathway.