Scalable Synthesis of Self-Assembling Monodisperse Phosphorescent Nanospheres Enabling Multi-Mode Angle-Dependent and Thermal-Responsive Photonic Gels

Scalable Synthesis of Self-Assembling Monodisperse Phosphorescent Nanospheres Enabling Multi-Mode Angle-Dependent and Thermal-Responsive Photonic Gels | Research Square window.SnipcartSettings = { analytics: { enabled: false } }; (function() { var accessVector = localStorage.getItem('access_vector') || ''; window.dataLayer = window.dataLayer || []; if (accessVector) { window.dataLayer.push({ user: { profile: { profileInfo: { snid: accessVector } } } }); } })(); (function(w,d,s,l,i){w[l]=w[l]||[];w[l].push({'gtm.start':new Date().getTime(),event:'gtm.js'});var f=d.getElementsByTagName(s)[0],j=d.createElement(s),dl=l!='dataLayer'?'&l='+l:'';j.async=true;j.src='https://www.googletagmanager.com/gtm.js?id='+i+dl;f.parentNode.insertBefore(j,f);})(window,document,'script','dataLayer','GTM-K279D39R'); Browse Preprints In Review Journals COVID-19 Preprints AJE Video Bytes Research Tools Research Promotion AJE Professional Editing AJE Rubriq About Preprint Platform In Review Editorial Policies Our Team Advisory Board Help Center Sign In Submit a Preprint Cite Share Download PDF Article Scalable Synthesis of Self-Assembling Monodisperse Phosphorescent Nanospheres Enabling Multi-Mode Angle-Dependent and Thermal-Responsive Photonic Gels Xuegang Lu, Changxing Wang, Yayun Ning, Yifan Yue, Guoli Du, Yuechi Xie, and 5 more This is a preprint; it has not been peer reviewed by a journal. https://doi.org/ 10.21203/rs.3.rs-6358279/v1 This work is licensed under a CC BY 4.0 License Status: Published Journal Publication published 18 Jul, 2025 Read the published version in Nature Communications → Version 1 posted You are reading this latest preprint version Abstract Developing room-temperature phosphorescent (RTP) materials with microscale periodic structures presents a promising prospect for future optical applications but remains extremely challenging due to the complex integration of luminescent and structural components. Herein, we present an emerging strategy for mass-producing monodisperse RTP silica nanospheres (RTP SiO 2 NPs) using a modified Stöber method, where organic molecules are embedded in silica networks and undergone in situ carbonization, aggregation and crystallization to form phosphorescent carbon dots under high temperature calcination. These NPs can self-assemble into photonic crystal (PC) structures, enabling the straightforward integration of structural color, fluorescence (FL) and RTP to achieve multimodal luminescent properties. The angle-dependent photonic bandgap (PBG) generated by the physical periodic structure modulates light propagation in RTP PC gel, creating unique FL and RTP angle-dependent chromatic responses. Temperature-induced refractive index changes between SiO 2 and the liquid matrix further enable dynamic control of light scattering states, significantly altering transmittance and emission intensities of FL and RTP. This successful fusion of physical photonic structures with chemical luminescence offers new approach for constructing advanced multimodal luminescent devices. Physical sciences/Optics and photonics/Optical materials and structures/Photonic crystals Physical sciences/Optics and photonics/Optical materials and structures/Nanoparticles Figures Figure 1 Figure 2 Figure 3 Figure 4 Figure 5 Introduction Room-temperature phosphorescence (RTP) materials, characterized by long-lived emission and low energy dissipation, offer transformative potential across optoelectronic applications including sensing, displaying, decoration, information encryption, and environmental monitoring. 1 – 6 Recent advances in nanotechnology and programmable self-assembly have driven a paradigm shift in RTP modulation, from manipulating complex chemical structures to tuning robust physical microstructures. 7 , 8 However, conventional RTP materials often face challenges in the precise design of physical morphology and structure, especially in the large-scale production, where the morphology and structure of RTP materials are difficult to maintain consistency. By precisely controlling the physical structure and morphology of phosphorescent materials, not only can new light signals be generated through modulation of physical microstructures, such as transmitted light, scattered light and reflected light, to achieve multi-mode luminescence, but potential interactions between different light signals can also be realized. 9 For example, integrating RTP materials with periodic nanostructures allows the formation of a photonic bandgap (PBG), which can modulate the propagation of the phosphorescence itself. 10 Therefore, developing cost-effective, high-throughput and scalable manufacturing strategies of phosphorescent materials while ensuring the uniformity and regularity of the physical structures is the key issue in developing RTP materials with intrinsic physical light modulation capabilities. Furthermore, when the external environment such as light, temperature, electric fields and magnetic fields changes, stimuli-responsive chromic materials (SRCM) undergo reversible color changes, which has garnered significant research interest in the field of smart materials. 11 – 15 Typically, the crystal structure, physical arrangement and chemical properties of these materials change under stimulation, hereby altering their light absorption, reflection, transmission and emission performances. Despite the transformative potential of SRCM across multidisciplinary applications, critical challenges are still remained in their functional implementation. On one hand, traditional SRCM typically require external energy input, exhibiting high response lag and short emission lifetimes. 16 , 17 On the other hand, the single optical expressions of most SRCM fail to achieve precise matching of optical signals with physical or chemical parameters in complex environments. 18 , 19 Theoretically, by rationally designing and integrating the stimulus matrix, physical structure and optical modulation units, SRCM with multi-dimensional optical responses can be realized. 20 , 21 Independent or synergistic responses between different optical signals can not only provide rich visual effects and high conversion efficiency, but also improve response accuracy and sensitivity. However, to date, the proposed design and manufacturing strategies for multi-mode integrated stimulus-responsive optical devices are very limited. Therefore, efficient design of optical devices with high optical freedom and customized response remains a significant challenge. To address the above challenges, we have developed a universal strategy for preparing RTP SiO 2 nanoparticles (RTP SiO 2 NPs) with uniform spherical structures, by calcining SiO 2 NPs encapsulating organic small molecules (Fig. 1 a). During the calcination process, the embedded organic molecules in SiO 2 matrix undergo in situ formation of fluorescent carbon dots (FL CDs) through carbonization, aggregation and crystallization, while the covalent C-Si bond network between the CDs and SiO 2 matrix is gradually build up, stabilizing the triplet excited state through spatial confinement to produce stable RTP emission. Notably, this strategy is universally applicable to various incorporated organic molecules, significantly reducing preparation costs, improving operational convenience, and enabling scalable production of RTP SiO 2 NPs (> 100 g/batch). As-prepared RTP SiO 2 NPs maintain their original self-assembly ability, and the resulting photonic crystals (PCs) through simple evaporation-induced self-assembly exhibit multimodal luminescent properties, including structural color (SC), FL and RTP. More intriguingly, photonic gel (PC gel) assembled from RTP SiO 2 NPs, relying on the PBG generated by their periodic microstructures, can regulate the propagation state of FL and RTP, thus achieving cooperative interactions of multiple optical signals (Fig. 1 b). Due to the angle dependence of the PBG, the photon resonance peaks of FL and RTP also show angle-dependent behavior. Therefore, by combining the static FL and RTP emissions with the dynamic photonic resonance peaks, a novel angle-dependent chromatic phenomenon can be realized. Furthermore, due to the differing temperature sensitivities of the refractive index of RTP SiO 2 NPs and liquid matrix, the PC gel demonstrates a temperature dependent dynamic refractive index matching characteristic. As the temperature decreases, the originally matched refractive index of the two phases gradually tends to mismatch, resulting in the PC gel changing from transparent state to white scattering state, and the enhanced light scattering ability significantly enhances the emission intensities of FL and RTP. Clearly, by combining physical structures with chemical luminescence, our findings provide a feasible approach for constructing optical devices with multi-stimulus response and customized optical signal expression. Results Morphology, Optical and Self-Assembly Properties of Monodisperse RTP SiO 2 NPs The preliminary molecular-doped SiO 2 NPs are prepared by adding glucose molecules to the precursor during the traditional Stöber method, followed by calcination at 575°C to obtain RTP SiO 2 NPs. As shown in Fig. 2 a, the Transmission electron microscope (TEM) image of RTP SiO 2 NPs shows monodisperse, homogeneous and regular spherical morphology with average particle size of 284 nm, and the morphology and particle size are insusceptible in calcination (Supplementary Fig. 1 and Fig. 2 ). Energy dispersive spectrometer (EDS) elemental mapping images clearly display that there are only C, O and Si elements in RTP SiO 2 NPs, and the uniform distribution of C elements within the spherical regions, indicating that glucose molecules are successfully encapsulated in SiO 2 NPs (Fig. 2 b and Supplementary Fig. 3). Furthermore, RTP SiO 2 NPs with particle diameters ranging from 206 nm to 284 nm can be easily prepared by adjusting the ethanol content during the reaction (Supplementary Fig. 4). As illustrated in Fig. 2 c, under excitation at 365 nm UV light, the RTP SiO 2 NPs display blue FL emission at 466 nm, while the green RTP emission band is centered at 504 nm. Whether FL or RTP, RTP SiO 2 NPs exhibit strong excitation dependent emission behavior, covering almost the entire visible band (Fig. 2 d and Supplementary Fig. 5). After exposure to different excitation light sources, even the white light, RTP SiO 2 NPs present colorful afterglow, and the afterglow persisting is over 17 s at 365 nm excitation (Supplementary Fig. 6 and Supplementary Movie 1). We preliminarily speculate that this excitation dependent optical behavior may be caused by different defective luminescent states formed by organic molecules or generation of different fluorescent molecules during the calcination process. 22 , 23 Besides, the time-resolved RTP emission spectra of RTP SiO 2 NPs excited at 365 nm further confirms the long-lived RTP emission with an optimum decay lifetime of 2 s at the 504 nm emission band (Fig. 2 e). Furthermore, as the temperature increasing from 77 K to 317 K, a noticeable decrease in RTP emission intensity and RTP decay lifetime is observed, confirming the absence of a thermally enhanced process, and presenting typical phosphorescence characteristics (Supplementary Fig. 7). 24 , 25 In addition, the optical intensity of RTP SiO 2 NPs also maintains excellent stability even in different organic solvents and metal ion solutions (Supplementary Fig. 8), which reflects a good anti-quenching ability, and further proves that the chemiluminescence center of RTP SiO 2 NPs is located in the interior of SiO 2 NPs. Interestingly, by simple evaporation-induced self-assembly, RTP SiO 2 NPs can be arranged in periodic array structures. As presented in Fig. 2 f and g, the RTP SiO 2 NPs exhibit an ordered close-packed state with two or more layers, respectively. Scanning electron microscopy (SEM) has also confirmed that the synthesized RTP SiO 2 NPs are capable of forming highly ordered, closely packed periodic structures, which exhibit the characteristics of PC structure (Fig. 2 h). 26 In addition, RTP SiO 2 NPs can also achieve PC array in the form of simple cubic close-packed arrangement (Supplementary Fig. 9). Therefore, the multimodal PC assembled from RTP SiO 2 NPs not only retain its intrinsic FL and RTP emission capabilities, but also possess the ability to manipulate light through its physical microstructures, thereby achieving vivid structural colors. As shown in Fig. 2 i, the assembled multimodal PC displays angle-dependent structural colors, bright blue FL and time-dependent green RTP under different light stimulation (Supplementary Movie 2). As the observation angle ( θ ) decreases from 90 o to 20 o , the structural colors of the multimodal PC gradually transition from red to blue, which is consistent with the angle-dependent reflection spectra (Fig. 2 j). This phenomenon is in accordance with Bragg's law for traditional PC, as described by Eq. ( 1 ): 27 $$\:\lambda\:\propto\:d\bullet\:sin\theta\:$$ 1 where d refers to the distance between the adjacent centers of the RTP SiO 2 NPs, and θ is the angle between the PCs surface and the incident light or reflect light. Moreover, the multimodal PC self-assembled from RTP SiO 2 NPs with varying diameters exhibit distinct structural colors (Supplementary Fig. 10, Fig. 11 and Fig. 12), whereas FL and RTP emission exhibit diameter-independent properties and the persistence of afterglow is more than 9 s (Supplementary Fig. 13 and Fig. 14). Mechanism Investigations of RTP SiO NPs Production by Calcination Generally, the realization of phosphorescent materials needs to meet two basic requirements, one is the chemically defective luminescence centers, the other is a rigid environment to stabilize the triplet excitons in these luminescent centers. 28 Therefore, we first explore the formation of chemically luminescent centers within RTP SiO 2 NPs during the calcination process. Compared with the uncalcined SiO 2 NPs, a large number of structural defects are generated inside the calcined particles, and these defects have obvious lattice fringes with a lattice spacing of approximately 0.21 nm (Fig. 3 a). Upon etching away the silica network with hydrofluoric acid, the exposed internal defect structure is revealed to be composed of spherical nanoparticles and retains similar lattice spacing, exhibiting the characteristic fluorescent CDs structure. 29 , 30 Hence, it is obvious that during the calcination process, glucose molecules undergo in-situ carbonization, aggregation and crystallization within the SiO 2 NPs to generate CDs. Furthermore, the formation and growth process of CDs is studied by calcining SiO 2 NPs doped with glucose molecules at different temperatures. It is found that the calcination temperature of 325 o C is sufficient to convert the glucose molecules inside the SiO 2 NPs into CDs (Supplementary Fig. 15), and the size of CDs increases with increasing calcination temperature, growing from 2.82 nm at 325 o C to 7.47 nm at 575 o C (Fig. 3 b). Moreover, the RTP spectra and time-resolved RTP spectra of RTP SiO 2 NPs calcined at different temperatures show optimum intensity and the longest RTP lifetime at 575 o C calcination (Supplementary Fig. 16 and Fig. 17). It can be inferred that as the calcination temperature increases (from 325 o C to 575 o C), the crystalline structure of the CDs derived from glucose becomes more stable, and the non-radiative transitions of electrons is weaken, leading to a higher overall luminescence efficiency (Supplementary Fig. 18 and Fig. 19). 31 High-resolution TEM (HR-TEM) has successfully validated this point. As presented in Fig. 3 c, the generated CDs exhibit characteristics of small size and low crystallinity at 325 o C calcination temperature, and these small-sized CDs grow and simultaneously aggregate as the temperature increases to 425°C, forming larger-sized CDs with high lattice defects. As the temperature further increases to 575 o C, the defect structures within the CDs are gradually filled and reduced, resulting in the formation of large-sized CDs with high crystallinity. It is worth mentioning that the captured arrangement of carbon atoms deviates from the hexagonal honeycomb structure, which may be attributed to the varying spatial orientations of the CDs. 32 The corresponding intensity ratio between crystalline G band (I G ) and disordered D band (I D ) in Raman spectra increases from 0.827 to 1.111 with the calcination temperature rising from 325 o C to 575 o C, which is consistent with the HR-TEM results (Supplementary Fig. 20). Consequently, the chemiluminescence centers of RTP SiO 2 NPs after calcination are derived from internal in-situ generated CDs, and further confirms that even a single organic small-molecule carbon source can also be converted to CDs through carbonation, aggregation and crystallization within the silica matrix (Fig. 3 d). Subsequently, we analyze the reasons for the formation of stable triplet states (T 1 ) responsible for the long-lived RTP of CDs during the calcination process. The temperature-dependent Fourier transform-infrared spectroscopy (FT-IR) show a gradual increase in the C-Si bonds at approximately 807 cm − 1 with increasing calcination temperature, while the Si-O-Si/Si-O-C groups at approximately 1046–1299 cm − 1 gradually decrease, indicating that during the calcination process, some Si-O-Si/Si-O-C bonds break and form new C-Si covalent bonds with the CDs (Supplementary Fig. 21). Besides, the fitted high-resolution Si 2p results spectra of RTP SiO 2 NPs show an increase in the relative content of C-Si bonds at 102.1 eV as increasing calcination temperature (Supplementary Fig. 22). Notably, the C 1s and O 1s band of RTP SiO 2 NPs verify the presence of O-related defect states, which provide a guarantee for long-lived RTP (Supplementary Fig. 23, Fig. 24 and Fig. 25). Taken together, during the calcination process, the growth and crystallization of CDs are accompanied by a simultaneous formation of a rigid covalent C-Si network with SiO 2 matrix, which facilitates the stabilization of triplet excitons and effectively suppresses the non-radiative transitions of the T 1 , thereby generating long-lived RTP emission. 33 , 34 Theoretical calculations based on the distribution of molecular surface electrostatic potential (ESP) and density functional theory (DFT) are carried out to further reveal the mechanism of RTP property from RTP SiO 2 NPs. Based on HR-TEM and FT-IR results, the molecular structure of CDs at 325 o C,475 o C and 575 o C calcination conditions are selected and designed as computational models (Supplementary Fig. 26). With the increase of calcination temperature, the ESP of the CDs inside the RTP SiO 2 NPs gradually shifts to a neutral dominant electron density, where the blue region, red region and green region indicate the lower electron density, densely electron-dense region and neutrality, respectively (Fig. 3 e). This calculation results indicate that the high crystallinity and abundant C-Si covalent bonds formed under high-temperature calcination (575 o C) can render the molecular structure more stable, which provides a rigid environment for restricting excited molecular motions of luminescent centers, and thus suppressing non-radiative processes. 35 In addition, the HOMO-LUMO energy gap of the CDs decreases from 3.0928 eV to 2.0237 eV with the increase of the calcination temperature (Fig. 3 f and Supplementary Fig. 27). The lower the HOMO-LUMO energy gap, the higher the efficiency in the generation and capture of electron excitons, which facilitates the formation and transition of triplet excitons. Based on the aforementioned analysis, the internal carbon source within SiO 2 NPs and the calcination process are the two critical factors for achieving RTP. Therefore, we deduce that the preparation of spherical RTP SiO 2 NPs is irrelevant to the type of introduced carbon-containing small organic molecules during the Stöber method. As illustrated in Fig. 3 g, in addition to glucose, 12 different kinds of organic molecules are selected, including nitrogen-containing organic molecules and fluorescent dye molecules. Evidently, the SiO 2 NPs doped with these molecules all exhibit long-lived RTP decay characteristics after calcination (Supplementary Fig. 28), demonstrating the universality of this strategy. The inexpensive of the precursor and convenient preparation method ensures the feasibility of large-scale production of RTP SiO 2 NPs. By proportionally scaling up the reaction precursors during the synthesis process, it is possible to effortlessly produce a large quantity of spherical RTP nanospheres, with the mass exceeding 700 g (Fig. 3 h). Photonic Bandgap-Induced Angle-dependent Chromatic Behavior of PC Gels Subsequently, RTP SiO 2 NPs with different diameters are dispersed in a mixture of ethanol, ethoxylated trimethylolpropane triarchy-late (ETPTA), poly (ethylene glycol) diacrylate (PEGDA) and ethylene glycol (EG) to prepare blue, green and red photonic gels (B-, G-, R-PC gels) using a supersaturated evaporation-induced self-assembly method in solvent. These PC gels possess SC, FL and RTP simultaneously under different light stimulation conditions (Fig. 4 a). However, there are significant differences in the emission intensities and color of FL and RTP for the three PC gels. Evidently, the PBG generated by the ordered array of RTP SiO 2 NPs through non-close packing exerts a regulatory influence on their own FL and RTP emissions (Fig. 4 b, Supplementary Fig. 29). When the emission band of FL and RTP align with the PBG, it means the transition energy levels of the molecules match the lattice constant of the photonic crystal, and specific resonant coupling interactions are activated, which enhances the energy transfer efficiency between photons, thereby increasing the intensity of FL and RTP (Fig. 4 c). 36 – 38 Therefore, the FL emission is stronger in the B-PC gel, whereas the RTP exhibits a stronger emission in the G-PC gel. On the other hand, owing to the broad emission characteristics of FL and RTP in PC gel, it is possible to realize PBG-induced color variations in FL and RTP through the modulation of the PBG to facilitate resonance enhancement of a specific emission bandgap. As depicted in Fig. 4 d, the angle-dependent multimodal photonic device is fabricated by spin-coating a R-PC gel with a thickness of 0.5 mm onto a black light-absorbing substrate and covering it with high-transparency quartz glass. Then, the incident light area (white or UV light) and the light-signal reception area (SC, FL and RTP) are partially separated using a black opaque light-absorbing plate. Fixing the incident light angle (θ 1 ) at 90°, the angle-dependent PBG gradually blue-shifts from 611 nm to 405 nm as the observation angle (θ 2 ) decreases from 90 o to 30 o (Supplementary Fig. 30). As anticipated, the blue shift of the PBG leads to a noticeable shift in the additional PBG resonance peaks of the FL and RTP emissions from the R-PC gel (Fig. 4 e and 4 f). When the emission wavelengths of FL and RTP fall within the PBG range of PC gel, their propagation is significantly suppressed. These specific wavelength bands of FL and RTP undergo multiple reflections within the PC structure, which enhances photon-matter interaction efficiency and remarkably improves the resonant coupling efficiency between luminescent molecules (or excitons) and the PBG of photonic crystals. Furthermore, due to the anisotropic property of the PC gel structure, the PBG exhibits direction-dependent bandgap characteristics in different spatial orientations, which enables specific FL and RTP wavelength bands to satisfy matching conditions only within predetermined angle ranges, thereby inducing directional resonant coupling. Therefore, the overall detected FL and RTP spectra show a superposition of the constant FL or RTP peaks with the angle-dependent PBG resonance enhancement peaks, resulting in an angle-dependent chromatic behavior. Interestingly, as the observation angle decreases from 90° to 30°, the color changes of three optical signals in the R-PC gel are visible to the naked eye. Under white light illumination, the SC of the R-PC gel gradually changes from red to violet as the observation angle decreases from 90 o to 30 o , and under UV light illumination or turned off, the FL of the R-PC gel gradually transitions from pink to blue, while the RTP shifts from yellow-green to cyan (Fig. 4 g and Supplementary Movie 3). It is worth mentioning that the angle-dependent chromatic behavior for FL and RTP only exists in highly ordered photonic crystal structures (with angle dependent PBG), while it is difficult to observe such chromatic behavior for poorly ordered PC structures (Supplementary Fig. 31). Besides, as the observation angle changes, the PBG gradually matches with the emission wavelengths, enabling the detection of stronger FL and RTP signals, and the enhancement effects of FL and RTP are most pronounced at θ 2 = 40° and θ 2 = 50°, respectively (Fig. 4 h). 39 The above angle-dependent chromatic behavior of FL and RTP also exits in the B-PC gel and G-PC gel (Supplementary Fig. 32, Fig. 33 and Fig. 34). The influence of the incident angle of excitation light on the optical behavior of PC gel is further investigated. As the incident angle (θ 1 ) of the UV light decreases from 90° to 30°, the wavelengths of the FL and RTP spectra measured at θ 2 = 90° remain constant, while the emission intensities gradually decrease (Fig. 4 i and Supplementary Fig. 35). Since the PBG of PC gel is located in the violet band at a low angle, the propagation of external incident UV light is prohibited when it is incident on the PC gel surface at a low incidence angle, and the UV light is reflected from the structure by Bragg reflection, which reduces the excitation energy delivered to the embedded RTP SiO 2 NPs, thereby suppressing the emission intensity of FL and RTP. 40 Meanwhile, the incident angle of the excitation light also affects the RTP decay lifetime of the PC gel (Fig. 4 j and Supplementary Fig. 36). Based on the above discussion, the FL and RTP of the PC gels are affected by both the incident angle of excitation light and the observation angle, where the former is mainly responsible for the modulation of the emission intensity, while the latter is used to realize the angle-dependent chromatic behavior (Fig. 4 k). In short, compared with complex chemical regulation, this angle-dependent physical modulation exhibits transient, highly stable and reproducible characteristics. Thermal-Induced Self-Scattering Enhanced Luminescence and Chromatic Properties of PC Gels The prepared PC gels also have unique thermal-induced self-scattering enhanced luminescence properties. As shown in Fig. 5 a, since R-PC gel is composed of polymer matrix with a temperature-sensitive refractive index (RI) and a temperature-independent SiO 2 NPs, the gel has temperature-regulated dynamic refractive index, and the RI-matching point is approximately 40 o C. As the temperature decreases from 40 o C to 0 o C, the refractive index between the two phases gradually mismatches, resulting in an increase in the light scattering capacity of the R-PC gel, thereby reducing the overall transmittance (Supplementary Fig. 37). 41 Meanwhile, the strong light scattering at low temperature can also affect the FL and RTP emission. Compared with the RI-matching state at 40 o C, the emission intensity of FL and RTP at 0 o C increase by 128-fold and 87-fold, respectively (Fig. 5 b). Besides, the RTP lifetime in the scattered state is extended by 25-fold compared to the transparent state (Fig. 5 c). Importantly, the temperature-dependent multiple optical signals of PC gel can be easily captured. As the temperature decreases gradually from 40°C to 0°C, the PC gel turns from transparent state to white scattering state, and the blue FL is also accompanied by a significant enhancement in this process (Fig. 5 d and Supplementary Movie 4). Moreover, in the RI-matched transmittance state, the RTP signal of the PC gel is difficult to capture, while in the scattering state, the RTP signal exhibits a bright and persistent afterglow (Fig. 5 e and Supplementary Movie 5). Therefore, the overall optical signals of the PC gel, including transmitted light, scattered light, FL and RTP, can be modulated by simply changing temperature, and this modulation has a stable reproducibility (Fig. 5 f). The intrinsic physical mechanism of the thermal-induced self-scattering enhanced FL and RTP properties of the R-PC gel is further investigated. The scattering intensity of UV-excited light collected on the PC gel increases with decreasing temperature, suggesting that the scattering state at low temperatures can amplify the intensity of excitation light, thus leading to stronger photoexcitation of the inside RTP SiO 2 NPs (Supplementary Fig. 38). In other words, the interfacial scattering enhancement firstly induces multiple omni-directional scattering of the incident UV light inside the gel, which improves the overall excitation efficiency of RTP SiO 2 NPs (Fig. 5 g). 42 Additionally, the collected FL decay spectra have a FL lifetime of 11.8 ns in the scattered state, which is longer than the 7.7 ns FL lifetime in the transmitted state (Supplementary Fig. 39). Considering that the scattering band of R-PC gel covers its own emission band, and there is a certain overlap between the excitation band and the emission band (Supplementary Fig. 40), these RTP SiO 2 NPs subjected to stronger excitation light will also emit strong scattered FL and RTP in all directions under the scattering state, and then their respective scattered light are continuously transferred, absorbed and re-emitted among particles, greatly contributing to the efficiency of energy utilization, thus further enhancing the FL and RTP intensities. 43 In addition, the R-PC gel shows enhanced luminescence accompanied by color changes in the temperature interval from 20 o C to 40 o C. As shown in Fig. 5 h, the intensity assigned to the FL peak of R-PC gel at approximately 450 nm gradually increases, while the FL band enhanced by PBG resonance peak at 611 nm gradually decreases with the temperature decreasing from 40 o C to 20 o C. A similar trend is also observed in the temperature-dependent RTP spectra (Supplementary Fig. 41). Therefore, the thermochromic behavior of R-PC gel is achieved by appropriately modulating the ambient temperature to cause the two fluorescent emissions to compete with each other (Fig. 5 i and 5 j). The strong scattering at low temperatures induces a decrease in the reflectivity of the PC gel, hindering the resonance-enhanced interactions of the PBG for specific bands of FL or RTP (Supplementary Fig. 42). In conclusion, this R-PC gel composed of spherical phosphor nanoparticles not only integrates multiple optical signals, but also has multi-modal and multi-dimensional stimulus response properties, which provides a new road for designing intelligent optical devices. Discussion In summary, we demonstrate a scalable and universal approach for synthesizing monodisperse RTP SiO 2 NPs with uniform spherical geometry. During high-temperature calcination, the introduced organic small molecules embedded in silica networks undergo in situ carbonization and crystallization to form CDs, while the covalent silica network stabilizes triplet excited states through spatial confinement, enabling robust RTP emission. The resulting RTP SiO 2 NPs retain programmable self-assembly capabilities, generating photonic crystals that synergistically integrate structural color, FL and RTP into a single multimodal optical platform. To harness dynamic interactions between PBG effects and FL or RTP emission, we engineered metastable multi-mode PC gels with angle-dependent PBG modulation. These gels exhibit unprecedented angle chromatic responses, where light propagation is modulated by the angle dependence of PBG, resulting in rare FL-RTP angle responses. Furthermore, the thermally tunable refractive index mismatch between SiO 2 NPs and the liquid matrix enables dynamic modulation of light scattering and transmission pathways, yielding temperature-gated self-scattering effects that amplify both FL and RTP intensities. The strategy of large-scale preparation of monodisperse RTP SiO 2 NPs and the successful integration of physical photonic structure and chemiluminescence provide new approach for constructing advanced multi-mode luminescent devices. Methods Reagents and materials Ammonia, tetraethyl orthosilicate, ethoxylated trimethylolpropane triarchy-late (average Mn ~ 428 MW), poly(ethylene glycol) diacrylate (PEG average Mn ~ 400 MW), ethylene glycol, glucose, tartaric acid, p-phthalic acid, vitamin C, urea, dopamine, melamine, thiourea, rhodamine B, rhodamine 6G, quinine sulphate and sulforhodamine B are obtained from Shanghai Aladdin Reagent Co., Ltd.. Tetraethyl orthosilicate is purchased from Damao Chemical Reagent Factory. Ethanol is purchased from Tianjin Fuyu Fine Chemical Co., Ltd.. All reagents are of analytical grade and used directly without further purification. Deionized water is produced through a Millipore water purification system (Milli-Q, Millipore) and used throughout the study. Synthesis of RTP SiO NPs Monodisperse RTP SiO 2 NPs is synthesized through a modified Stöber method and their sizes can be regulated by adjusting ethanol ratio during the preparation process. Firstly, 6 mL of glucose aqueous solution (1 mol/L), 130 mL of ethanol and 16 mL of ammonia are mixed homogeneously in a 500 mL three-necked flask and heated to 60 o C. Then, the mixture of 12 mL of tetraethyl orthosilicate and 10 mL ethanol is added and stirred at 60 o C for 100 minutes in a water bath environment. The white suspension obtained is repeatedly centrifuged three times with ethanol at 7000 rpm. The collected white precipitate is dried at 50 o C for 48 h to obtain organic small molecule doped SiO 2 NPs. Then, quartz crucible with CDs@SiO 2 NPs is transferred to a high temperature box-type electric resistance furnace, heated up to 575 o C in 3 hours and kept for 2 hours, finally cooled naturally to room temperature and obtained the RTP SiO 2 NPs. Preparation of PCs assembled by RTP SiO 2 NPs The RTP SiO 2 NPs are uniformly dispersed in ethanol to form a white suspension (4 wt.%). Then, the commercial glass is stabilized in the suspension at an inclination angle of 30 o . The ethanol is evaporated at an ambient temperature of 50 o C to allow the RTP SiO 2 NPs to uniformly self-assemble on the glass sheet to form PCs. The PCs with different colors can be prepared by selecting different particle sizes of RTP SiO 2 NPs. Preparation of PC gels Briefly, RTP SiO 2 NPs (0.12 cm 3 ) are dispersed in a mixture of ethanol (3 mL), ETPTA (140 µL), PEGDA (70 µL) and EG (70 µL) under sonication. The PC gel is obtained by evaporating the mixture at 90 o C for 2 hours to ethanol the alcohol, and the volume fraction of RTP SiO 2 NPs, ETPTA, PEGDA and EG in the PC gel is 30%, 35%, 17.5% and 17.5%, respectively. PC gel with different colors can be prepared with different particle sizes of RTP SiO 2 NPs. Subsequently, the prepared PC gel is filled into a customized black light-absorbing plate and quartz glass interlayer to achieve the optical behavior of angle-dependent chromatic. Characterization Optical reflectance spectra, transmittance spectra, FL spectra and RTP spectra are captured utilizing a fiber optic spectrometer (PG2000-Pro), and all RTP emission spectra are measured at 10 ms delay time after turning the externally equipped UV lamp off. The UV-vis absorption spectra are measured with a PerkinElmer PE Lambda 950 spectrometer. Temperature-dependent afterglow spectra and RTP lifetime decay profile is collected with the FLS1000 instrument equipped with the OXFORD accessory. The morphologies of PCs and PC gel are analyzed using a Zeiss Sigma 300 field emission scanning electron microscope. TEM images, HAADF-STEM images and their corresponding EDS mapping images are obtained on a JEM-2100 apparatus operating at 200 kV. HR-TEM images are taken by a 300 KV double spherical aberration corrected electron microscope, JEM-ARM300F2 (Grand ARM). The FT-IR spectra is acquired on a Nicolet iS50 FTIR spectrometer. The XPS measurements are performed on an Thermo Scientific K-Alpha spectrometer. Digital photographs of the device are captured using an iPhone 13. Theoretical Calculations Quantum chemical studies are performed employing density functional theory (DFT) implemented in the Optimal Reciprocal Collision Avoidance (ORCA) program. To explore the mechanism by which stiff C-Si bonds, dense silica-oxygen structure and the degree of crystallinity of CDs affect the phosphorescence characteristics of CDs. Based on the results of, HR-TEM, FT-IR spectroscopy and XPS characterization, there are variations in the Si-O-C and Si-C covalent bonds from CDs-325 o C, CDs-475 o C, and CDs-575 o C, which are chosen as the study models of CDs-325 o C, CDs-475 o C and CDs-575 o C, respectively. The input files are generated employing Avogadro. Geometry optimization of CDs-325 o C, CDs-475 o C and CDs-575 o C models is initially performed at the B97-3c level, followed by single-point-energy (SPE) calculations employing the high-precision basis set B3LYP/def2-TZVP. To gain a more thorough understanding of the electronic structure, it is further investigated that SPE calculations provide the basis for the distribution of frontier molecular orbitals and the electrostatic potential (ESP). The molecular visualization programs Jmol and Chemcraft are used for the analysis. Declarations Acknowledgements This work was supported by the National Key R&D Program of China (2022YFE0109500), the National Natural Science Foundation of China (No. 62475212, 61975162), and the Shaanxi Province Natural Science Foundation (No. 2020JM-062). We thank Dr. D. He at the Instrument Analysis Center of Xi’an Jiaotong University for the kinetic decay curves spectra experiments. We thank the Xi'an Yizhichen Biotechnology Co., Ltd. for their help in purchasing reagents for this experiment. Author contributions The overall experimental design was conceived by C.W., Y.N., and Y.Y., and together, they coordinated the full project. C.W., and Y.N. designed the materials and conducted experiments. C.W., X.W., Y.X., and J.L. characterized, and analyzed the materials. C.W., Y.N., Y.X., G.D., and J.L. built underwater sensing and performed data collection and analysis. All authors also discussed and interpreted the experimental data and results. C.W. and N.B. performed the theoretical calculations. C.W. wrote the manuscript with contributions from all authors. X.L. and S.Y. reviewed and edited the paper. All authors discussed the results and commented on the paper. Competing interests The authors declare no conflict of interest. Data availability The data required to reproduce the findings are included in the article and its Supplementary Information. All other information can be obtained from the corresponding author upon request. Source data are provided with this paper. References Gu L et al (2019) Colour-tunable ultra-long organic phosphorescence of a single-component molecular crystal. Nat Photon 13:406–411. https://doi.org/10.1038/s41566-019-0408-4 Dai X-Y, Huo M, Dong X, Hu Y-Y, Liu Y (2022) Noncovalent polymerization-activated ultrastrong near-infrared room-temperature phosphorescence energy transfer assembly in aqueous solution. 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Adv Mater Technol 10:2400865. https://doi.org/10.1002/admt.202400865​ Li J et al (2022) Dynamic refractive index-matching for adaptive thermoresponsive smart windows. Small 18:2201322. https://doi.org/10.1002/smll.202201322​ Wang Y, Liu P, Vogelbacher F, Li M, Shen W (2022) Bioinspired multiscale optical structures towards efficient light management in optoelectronic devices. Mater Today Nano 19:100225. https://doi.org/10.1016/j.mtnano.2022.100225​ Shi X et al (2014) Efficient luminescence of long persistent phosphor combined with photonic crystal. ACS Appl Mater Interfaces 6:6317–6321. https://doi.org/10.1021/am501420w​ Additional Declarations There is NO Competing Interest. Supplementary Files SupplementaryInformation.docx Supplementary Fig. 1-42. SupplementaryMovie1.mov Supplementary Movie 1: The behavior of color afterglow of RTP SiO 2 NPs under different excitation light. SupplementaryMovie2.mov Supplementary Movie 2: Demonstration of angle-dependent structural color, fluorescence and time-dependent afterglow of self-assembled multimode PCs. SupplementaryMovie3.mov Supplementary Movie 3: The process of angle-dependent chromatic behavior of R-PC gel. SupplementaryMovie4.mov Supplementary Movie 4: The process of stretching-induced transition from transparent state to the scattering state, and self-scattering FL enhancement behavior of R-PC gel. SupplementaryMovie5.mov Supplementary Movie 5: Demonstration of RTP properties of PC gel in the matched and unmatched state of refractive index. Cite Share Download PDF Status: Published Journal Publication published 18 Jul, 2025 Read the published version in Nature Communications → Version 1 posted You are reading this latest preprint version Research Square lets you share your work early, gain feedback from the community, and start making changes to your manuscript prior to peer review in a journal. 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process of monodisperse spherical RTP SiO\u003csub\u003e2\u003c/sub\u003e NPs and self-assembled multimode luminescent PCs. \u003cstrong\u003eb\u003c/strong\u003e Schematic illustration of angle-dependent chromatic behavior and thermal-induced self-scattering enhanced luminescence properties of PC gels.\u003c/p\u003e","description":"","filename":"Fig.1.png","url":"https://assets-eu.researchsquare.com/files/rs-6358279/v1/dffd2f3637f5e2cb80c8abed.png"},{"id":80023101,"identity":"11336059-b902-44ac-b039-89be1089b2df","added_by":"auto","created_at":"2025-04-07 05:30:51","extension":"png","order_by":2,"title":"Figure 2","display":"","copyAsset":false,"role":"figure","size":74134178,"visible":true,"origin":"","legend":"\u003cp\u003e\u003cstrong\u003eMorphology characterization, optical properties and self-assembly behavior of RTP SiO\u003c/strong\u003e\u003csub\u003e\u003cstrong\u003e2\u003c/strong\u003e\u003c/sub\u003e\u003cstrong\u003e NPs\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003ea \u003c/strong\u003eTEM image of RTP SiO\u003csub\u003e2\u003c/sub\u003e NPs (Scale bar: 2 µm). \u003cstrong\u003eb\u003c/strong\u003e High-angle annular dark field scanning transmission electron microscopy (HAADF-STEM) and EDS elemental mapping images of RTP SiO\u003csub\u003e2\u003c/sub\u003e NPs (Scale bar: 200 nm). \u003cstrong\u003ec\u003c/strong\u003e FL and RTP spectra of RTP SiO\u003csub\u003e2\u003c/sub\u003e NPs under 365 nm excitation wavelength. Insets show photographs of the RTP SiO\u003csub\u003e2\u003c/sub\u003e NPs under 365 nm UV excitation lamp on and off. \u003cstrong\u003ed\u003c/strong\u003e Excitation-phosphorescence mapping of the aqueous RTP SiO\u003csub\u003e2\u003c/sub\u003e NPs at room temperature. \u003cstrong\u003ee\u003c/strong\u003e Time-resolved emission spectra of RTP SiO\u003csub\u003e2\u003c/sub\u003e NPs under 365 nm excitation wavelength, the inset image is lifetime decay profile of the RTP for RTP SiO\u003csub\u003e2\u003c/sub\u003e NPs under 365 nm excitation wavelength. \u003cstrong\u003ef\u003c/strong\u003e and \u003cstrong\u003eg\u003c/strong\u003e TEM images of RTP SiO\u003csub\u003e2\u003c/sub\u003e NPs in the self-assembled state (Scale bar: 500 nm). \u003cstrong\u003eh\u003c/strong\u003e SEM image of the closely packed RTP SiO\u003csub\u003e2\u003c/sub\u003e NPs (Scale bar: 500 nm). \u003cstrong\u003ei\u003c/strong\u003e The photographs of the angle-dependent structural colors, FL and RTP of the multi-modal PCs under daylight, 365 nm UV lamp on and off, respectively. \u003cstrong\u003ej\u003c/strong\u003e Angle-dependent reflection spectra of the multimodal PCs self-assembled by RTP SiO\u003csub\u003e2\u003c/sub\u003e NPs with diameter of 284 nm.\u003c/p\u003e","description":"","filename":"Fig.2.png","url":"https://assets-eu.researchsquare.com/files/rs-6358279/v1/fdbef4d88a942dab6b6e30db.png"},{"id":80023734,"identity":"e08de7d1-b0ca-4d5f-ade3-dfd03c73767b","added_by":"auto","created_at":"2025-04-07 05:38:51","extension":"png","order_by":3,"title":"Figure 3","display":"","copyAsset":false,"role":"figure","size":96884674,"visible":true,"origin":"","legend":"\u003cp\u003e\u003cstrong\u003eRTP mechanism of RTP SiO\u003c/strong\u003e\u003csub\u003e\u003cstrong\u003e2\u003c/strong\u003e\u003c/sub\u003e\u003cstrong\u003e NPs, the universality of strategy and large-scale preparation\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003ea\u003c/strong\u003e TEM images of SiO\u003csub\u003e2\u003c/sub\u003e NPs doped with glucose molecules before calcination, after calcination and after hydrofluoric acid etching, the scale bars from left to right are 100 nm, 100 nm, 5 nm and 50 nm, respectively. \u003cstrong\u003eb\u003c/strong\u003e The relationship between diameter of CDs formed inside RTP SiO\u003csub\u003e2\u003c/sub\u003e NPs and calcination temperature. \u003cstrong\u003ec\u003c/strong\u003e HR-TEM images of CDs growth inside SiO\u003csub\u003e2\u003c/sub\u003e NPs at different calcination temperatures, the scale bars are 5 nm. \u003cstrong\u003ed\u003c/strong\u003e Schematic diagram of the growth process of CDs inside the SiO\u003csub\u003e2\u003c/sub\u003e NPs during the calcination process. \u003cstrong\u003ee\u003c/strong\u003e The molecular surface electrostatic potential for the molecular structure of CDs at 325 \u003csup\u003eo\u003c/sup\u003eC,475 \u003csup\u003eo\u003c/sup\u003eC and 575 \u003csup\u003eo\u003c/sup\u003eC calcination conditions designed by HR-TEM images. \u003cstrong\u003ef\u003c/strong\u003e The calculated energy gaps of HOMO and LUMO for the corresponding molecular structure of CDs. \u003cstrong\u003eg\u003c/strong\u003e The phosphorescent lifetime of RTP SiO\u003csub\u003e2\u003c/sub\u003e NPs synthesized by doping various organic small molecules. \u003cstrong\u003eh\u003c/strong\u003e Photographs of large-scale prepared RTP SiO\u003csub\u003e2\u003c/sub\u003e NPs under sunlight, UV radiation and after UV shut-off.\u003c/p\u003e","description":"","filename":"Fig.3.png","url":"https://assets-eu.researchsquare.com/files/rs-6358279/v1/22747c37b79646684339576f.png"},{"id":80023740,"identity":"4259c0bc-4da5-46e7-9b26-d0bd095d2b39","added_by":"auto","created_at":"2025-04-07 05:38:52","extension":"png","order_by":4,"title":"Figure 4","display":"","copyAsset":false,"role":"figure","size":46771200,"visible":true,"origin":"","legend":"\u003cp\u003e\u003cstrong\u003eAngle-dependent chromatic behavior of photonic gels\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003ea\u003c/strong\u003e Photographs of PC gels with varying particle sizes of RTP SiO\u003csub\u003e2\u003c/sub\u003e NPs under daylight, 365 nm UV lamp on and off, respectively. \u003cstrong\u003eb\u003c/strong\u003e The SEM images of R-PC gel prepared by 284 nm diameter of RTP SiO\u003csub\u003e2\u003c/sub\u003e NPs (Scale bar: 2 µm). \u003cstrong\u003ec\u003c/strong\u003e The matching situation between the PBG of B-, G- and R-PC gels with the FL and RTP of RTP SiO\u003csub\u003e2\u003c/sub\u003e NPs. \u003cstrong\u003ed\u003c/strong\u003e Schematic illustration for achieving angle-dependent chromatic behavior of PC gels. \u003cstrong\u003ee\u003c/strong\u003e and \u003cstrong\u003ef\u003c/strong\u003e Angle-dependent FL and RTP spectra of R-PC gel. \u003cstrong\u003eg\u003c/strong\u003e The photographs of the angle-dependent SC, FL and RTP of the R-PC gel under daylight, 365 nm UV lamp on and off, respectively. \u003cstrong\u003eh\u003c/strong\u003e The relationship between the intensities of FL and RTP of R-PC gel and the observation angle, where I\u003csub\u003eθ\u003c/sub\u003e is the intensity at different θ\u003csub\u003e2\u003c/sub\u003e and I\u003csub\u003eθ=90\u003c/sub\u003e is the intensity at θ\u003csub\u003e2\u003c/sub\u003e=90\u003csup\u003eo\u003c/sup\u003e. \u003cstrong\u003ei\u003c/strong\u003e Scanning θ\u003csub\u003e1\u003c/sub\u003e-dependent two-dimensional RTP spectra of R-PC gel. \u003cstrong\u003ej\u003c/strong\u003e RTP decay lifetime measured at different θ\u003csub\u003e1\u003c/sub\u003e. \u003cstrong\u003ek\u003c/strong\u003e The color arrays formed by photographs of PC gel collected at different θ\u003csub\u003e1\u003c/sub\u003e and θ\u003csub\u003e2\u003c/sub\u003e, the size of each unit module is 1×1 cm.\u003c/p\u003e","description":"","filename":"Fig.4.png","url":"https://assets-eu.researchsquare.com/files/rs-6358279/v1/8c451f75ac01525c13637479.png"},{"id":80023739,"identity":"b27e6c88-bcc2-42d4-bcd2-3d1dc4e01fa7","added_by":"auto","created_at":"2025-04-07 05:38:52","extension":"png","order_by":5,"title":"Figure 5","display":"","copyAsset":false,"role":"figure","size":55074919,"visible":true,"origin":"","legend":"\u003cp\u003e\u003cstrong\u003eThermal-induced self-scattering enhanced luminescence and thermochromic properties of PC gels\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003ea \u003c/strong\u003eTemperature dependence of the refractive index of RTP SiO\u003csub\u003e2\u003c/sub\u003e NPs and ETPTA/PEGDA/EG matrix. \u003cstrong\u003eb\u003c/strong\u003e The FL spectra and RTP spectra of R-PC gel at 0 \u003csup\u003eo\u003c/sup\u003eC and 40 \u003csup\u003eo\u003c/sup\u003eC, respectively. \u003cstrong\u003ec\u003c/strong\u003e The RTP lifetime decay spectra of R-PC gel at 0 \u003csup\u003eo\u003c/sup\u003eC and 40 \u003csup\u003eo\u003c/sup\u003eC, respectively. \u003cstrong\u003ed\u003c/strong\u003e Photographs of the transparent state of R-PC gel varying with the temperature, and FL photographs of R-PC gel in different temperature environments under 365 nm UV light. \u003cstrong\u003ee\u003c/strong\u003e The time-dependent RTP photographs of R-PC gel taken at 0 \u003csup\u003eo\u003c/sup\u003eC and 40 \u003csup\u003eo\u003c/sup\u003eC, respectively. \u003cstrong\u003ef\u003c/strong\u003e Cyclic performance of the thermal-induced self-scattering enhanced luminescence properties of R-PC gel. \u003cstrong\u003eg\u003c/strong\u003e A plausible mechanism for thermal-induced self-scattering enhancement of the FL and RTP. \u003cstrong\u003eh\u003c/strong\u003e Temperature-dependent FL spectra of R-PC gel, θ\u003csub\u003e1\u003c/sub\u003e=90\u003csup\u003eo\u003c/sup\u003e and θ\u003csub\u003e2\u003c/sub\u003e=90\u003csup\u003eo\u003c/sup\u003e. \u003cstrong\u003ei\u003c/strong\u003e The corresponding relationship between the intensity ratio of self-emission peak (I\u003csub\u003eFL\u003c/sub\u003e or I\u003csub\u003eRTP\u003c/sub\u003e) and PBG resonance peak (I\u003csub\u003eP\u003c/sub\u003e) with temperature. \u003cstrong\u003eh\u003c/strong\u003e The corresponding CIE chromaticity diagram of FL and RTP spectra under different temperature.\u003c/p\u003e","description":"","filename":"Fig.5.png","url":"https://assets-eu.researchsquare.com/files/rs-6358279/v1/e435fd18414b9ad980d82182.png"},{"id":80023100,"identity":"adb1e0ca-b783-4641-920f-9b355400c5cc","added_by":"auto","created_at":"2025-04-07 05:30:51","extension":"docx","order_by":1,"title":"","display":"","copyAsset":false,"role":"supplement","size":13433671,"visible":true,"origin":"","legend":"\u003cp\u003eSupplementary Fig. 1-42.\u003c/p\u003e","description":"","filename":"SupplementaryInformation.docx","url":"https://assets-eu.researchsquare.com/files/rs-6358279/v1/f78200df2a416d200407f243.docx"},{"id":80023114,"identity":"fb7767a3-0efa-4dd4-a138-f147f7c03487","added_by":"auto","created_at":"2025-04-07 05:30:51","extension":"mov","order_by":2,"title":"","display":"","copyAsset":false,"role":"supplement","size":19588027,"visible":true,"origin":"","legend":"\u003cp\u003eSupplementary Movie 1: The behavior of color afterglow of RTP SiO\u003csub\u003e2\u003c/sub\u003e NPs under different excitation light.\u003c/p\u003e","description":"","filename":"SupplementaryMovie1.mov","url":"https://assets-eu.researchsquare.com/files/rs-6358279/v1/a0cf886baac7a3701fc394dd.mov"},{"id":80023730,"identity":"2e25843d-24a3-4d37-9842-1b53a33fd03c","added_by":"auto","created_at":"2025-04-07 05:38:51","extension":"mov","order_by":3,"title":"","display":"","copyAsset":false,"role":"supplement","size":41574761,"visible":true,"origin":"","legend":"\u003cp\u003eSupplementary Movie 2: Demonstration of angle-dependent structural color, fluorescence and time-dependent afterglow of self-assembled multimode PCs.\u003c/p\u003e","description":"","filename":"SupplementaryMovie2.mov","url":"https://assets-eu.researchsquare.com/files/rs-6358279/v1/ac02daaf090454a071e7c9f2.mov"},{"id":80023124,"identity":"344c4f9b-e6d1-42d4-bc13-1e4ff2653abc","added_by":"auto","created_at":"2025-04-07 05:30:51","extension":"mov","order_by":4,"title":"","display":"","copyAsset":false,"role":"supplement","size":21076304,"visible":true,"origin":"","legend":"\u003cp\u003eSupplementary Movie 3: The process of angle-dependent chromatic behavior of R-PC gel.\u003c/p\u003e","description":"","filename":"SupplementaryMovie3.mov","url":"https://assets-eu.researchsquare.com/files/rs-6358279/v1/5f0773299c8927efca2fdf38.mov"},{"id":80023134,"identity":"0270d8e3-10f6-4e0c-8460-3880108b6512","added_by":"auto","created_at":"2025-04-07 05:30:51","extension":"mov","order_by":5,"title":"","display":"","copyAsset":false,"role":"supplement","size":20523439,"visible":true,"origin":"","legend":"\u003cp\u003eSupplementary Movie 4: The process of stretching-induced transition from transparent state to the scattering state, and self-scattering FL enhancement behavior of R-PC gel.\u003c/p\u003e","description":"","filename":"SupplementaryMovie4.mov","url":"https://assets-eu.researchsquare.com/files/rs-6358279/v1/232f0d62148bcbd295532978.mov"},{"id":80023738,"identity":"e15a1e55-12e4-4abe-9feb-1839a8d7dfa6","added_by":"auto","created_at":"2025-04-07 05:38:52","extension":"mov","order_by":6,"title":"","display":"","copyAsset":false,"role":"supplement","size":4243119,"visible":true,"origin":"","legend":"\u003cp\u003eSupplementary Movie 5: Demonstration of RTP properties of PC gel in the matched and unmatched state of refractive index.\u003c/p\u003e","description":"","filename":"SupplementaryMovie5.mov","url":"https://assets-eu.researchsquare.com/files/rs-6358279/v1/107f129c5a7bf5b48f3bcd1d.mov"}],"financialInterests":"There is \u003cb\u003eNO\u003c/b\u003e Competing Interest.","formattedTitle":"Scalable Synthesis of Self-Assembling Monodisperse Phosphorescent Nanospheres Enabling Multi-Mode Angle-Dependent and Thermal-Responsive Photonic Gels","fulltext":[{"header":"Introduction","content":"\u003cp\u003eRoom-temperature phosphorescence (RTP) materials, characterized by long-lived emission and low energy dissipation, offer transformative potential across optoelectronic applications including sensing, displaying, decoration, information encryption, and environmental monitoring.\u003csup\u003e\u003cspan class=\"CitationRef\"\u003e1\u003c/span\u003e\u0026ndash;\u003cspan class=\"CitationRef\"\u003e6\u003c/span\u003e\u003c/sup\u003e Recent advances in nanotechnology and programmable self-assembly have driven a paradigm shift in RTP modulation, from manipulating complex chemical structures to tuning robust physical microstructures.\u003csup\u003e\u003cspan class=\"CitationRef\"\u003e7\u003c/span\u003e,\u003cspan class=\"CitationRef\"\u003e8\u003c/span\u003e\u003c/sup\u003e However, conventional RTP materials often face challenges in the precise design of physical morphology and structure, especially in the large-scale production, where the morphology and structure of RTP materials are difficult to maintain consistency. By precisely controlling the physical structure and morphology of phosphorescent materials, not only can new light signals be generated through modulation of physical microstructures, such as transmitted light, scattered light and reflected light, to achieve multi-mode luminescence, but potential interactions between different light signals can also be realized.\u003csup\u003e\u003cspan class=\"CitationRef\"\u003e9\u003c/span\u003e\u003c/sup\u003e For example, integrating RTP materials with periodic nanostructures allows the formation of a photonic bandgap (PBG), which can modulate the propagation of the phosphorescence itself.\u003csup\u003e\u003cspan class=\"CitationRef\"\u003e10\u003c/span\u003e\u003c/sup\u003e Therefore, developing cost-effective, high-throughput and scalable manufacturing strategies of phosphorescent materials while ensuring the uniformity and regularity of the physical structures is the key issue in developing RTP materials with intrinsic physical light modulation capabilities.\u003c/p\u003e\n\u003cp\u003eFurthermore, when the external environment such as light, temperature, electric fields and magnetic fields changes, stimuli-responsive chromic materials (SRCM) undergo reversible color changes, which has garnered significant research interest in the field of smart materials.\u003csup\u003e\u003cspan class=\"CitationRef\"\u003e11\u003c/span\u003e\u0026ndash;\u003cspan class=\"CitationRef\"\u003e15\u003c/span\u003e\u003c/sup\u003e Typically, the crystal structure, physical arrangement and chemical properties of these materials change under stimulation, hereby altering their light absorption, reflection, transmission and emission performances. Despite the transformative potential of SRCM across multidisciplinary applications, critical challenges are still remained in their functional implementation. On one hand, traditional SRCM typically require external energy input, exhibiting high response lag and short emission lifetimes.\u003csup\u003e\u003cspan class=\"CitationRef\"\u003e16\u003c/span\u003e,\u003cspan class=\"CitationRef\"\u003e17\u003c/span\u003e\u003c/sup\u003e On the other hand, the single optical expressions of most SRCM fail to achieve precise matching of optical signals with physical or chemical parameters in complex environments.\u003csup\u003e\u003cspan class=\"CitationRef\"\u003e18\u003c/span\u003e,\u003cspan class=\"CitationRef\"\u003e19\u003c/span\u003e\u003c/sup\u003e Theoretically, by rationally designing and integrating the stimulus matrix, physical structure and optical modulation units, SRCM with multi-dimensional optical responses can be realized.\u003csup\u003e\u003cspan class=\"CitationRef\"\u003e20\u003c/span\u003e,\u003cspan class=\"CitationRef\"\u003e21\u003c/span\u003e\u003c/sup\u003e Independent or synergistic responses between different optical signals can not only provide rich visual effects and high conversion efficiency, but also improve response accuracy and sensitivity. However, to date, the proposed design and manufacturing strategies for multi-mode integrated stimulus-responsive optical devices are very limited. Therefore, efficient design of optical devices with high optical freedom and customized response remains a significant challenge.\u003c/p\u003e\n\u003cp\u003eTo address the above challenges, we have developed a universal strategy for preparing RTP SiO\u003csub\u003e2\u003c/sub\u003e nanoparticles (RTP SiO\u003csub\u003e2\u003c/sub\u003e NPs) with uniform spherical structures, by calcining SiO\u003csub\u003e2\u003c/sub\u003e NPs encapsulating organic small molecules (Fig.\u0026nbsp;\u003cspan class=\"InternalRef\"\u003e1\u003c/span\u003ea). During the calcination process, the embedded organic molecules in SiO\u003csub\u003e2\u003c/sub\u003e matrix undergo in situ formation of fluorescent carbon dots (FL CDs) through carbonization, aggregation and crystallization, while the covalent C-Si bond network between the CDs and SiO\u003csub\u003e2\u003c/sub\u003e matrix is gradually build up, stabilizing the triplet excited state through spatial confinement to produce stable RTP emission. Notably, this strategy is universally applicable to various incorporated organic molecules, significantly reducing preparation costs, improving operational convenience, and enabling scalable production of RTP SiO\u003csub\u003e2\u003c/sub\u003e NPs (\u0026gt;\u0026thinsp;100 g/batch). As-prepared RTP SiO\u003csub\u003e2\u003c/sub\u003e NPs maintain their original self-assembly ability, and the resulting photonic crystals (PCs) through simple evaporation-induced self-assembly exhibit multimodal luminescent properties, including structural color (SC), FL and RTP. More intriguingly, photonic gel (PC gel) assembled from RTP SiO\u003csub\u003e2\u003c/sub\u003e NPs, relying on the PBG generated by their periodic microstructures, can regulate the propagation state of FL and RTP, thus achieving cooperative interactions of multiple optical signals (Fig.\u0026nbsp;\u003cspan class=\"InternalRef\"\u003e1\u003c/span\u003eb). Due to the angle dependence of the PBG, the photon resonance peaks of FL and RTP also show angle-dependent behavior. Therefore, by combining the static FL and RTP emissions with the dynamic photonic resonance peaks, a novel angle-dependent chromatic phenomenon can be realized. Furthermore, due to the differing temperature sensitivities of the refractive index of RTP SiO\u003csub\u003e2\u003c/sub\u003e NPs and liquid matrix, the PC gel demonstrates a temperature dependent dynamic refractive index matching characteristic. As the temperature decreases, the originally matched refractive index of the two phases gradually tends to mismatch, resulting in the PC gel changing from transparent state to white scattering state, and the enhanced light scattering ability significantly enhances the emission intensities of FL and RTP. Clearly, by combining physical structures with chemical luminescence, our findings provide a feasible approach for constructing optical devices with multi-stimulus response and customized optical signal expression.\u003c/p\u003e\n\u003cp\u003e\u0026nbsp;\u003c/p\u003e"},{"header":"Results","content":"\u003cdiv id=\"Sec3\" class=\"Section2\"\u003e\n\u003ch2\u003eMorphology, Optical and Self-Assembly Properties of Monodisperse RTP SiO\u003csub\u003e2\u003c/sub\u003e NPs\u003c/h2\u003e\n\u003cp\u003eThe preliminary molecular-doped SiO\u003csub\u003e2\u003c/sub\u003e NPs are prepared by adding glucose molecules to the precursor during the traditional St\u0026ouml;ber method, followed by calcination at 575\u0026deg;C to obtain RTP SiO\u003csub\u003e2\u003c/sub\u003e NPs. As shown in Fig.\u0026nbsp;\u003cspan class=\"InternalRef\"\u003e2\u003c/span\u003ea, the Transmission electron microscope (TEM) image of RTP SiO\u003csub\u003e2\u003c/sub\u003e NPs shows monodisperse, homogeneous and regular spherical morphology with average particle size of 284 nm, and the morphology and particle size are insusceptible in calcination (Supplementary Fig.\u0026nbsp;1 and Fig.\u0026nbsp;\u003cspan class=\"InternalRef\"\u003e2\u003c/span\u003e). Energy dispersive spectrometer (EDS) elemental mapping images clearly display that there are only C, O and Si elements in RTP SiO\u003csub\u003e2\u003c/sub\u003e NPs, and the uniform distribution of C elements within the spherical regions, indicating that glucose molecules are successfully encapsulated in SiO\u003csub\u003e2\u003c/sub\u003e NPs (Fig.\u0026nbsp;\u003cspan class=\"InternalRef\"\u003e2\u003c/span\u003eb and Supplementary Fig.\u0026nbsp;3). Furthermore, RTP SiO\u003csub\u003e2\u003c/sub\u003e NPs with particle diameters ranging from 206 nm to 284 nm can be easily prepared by adjusting the ethanol content during the reaction (Supplementary Fig.\u0026nbsp;4).\u003c/p\u003e\n\u003cp\u003eAs illustrated in Fig.\u0026nbsp;\u003cspan class=\"InternalRef\"\u003e2\u003c/span\u003ec, under excitation at 365 nm UV light, the RTP SiO\u003csub\u003e2\u003c/sub\u003e NPs display blue FL emission at 466 nm, while the green RTP emission band is centered at 504 nm. Whether FL or RTP, RTP SiO\u003csub\u003e2\u003c/sub\u003e NPs exhibit strong excitation dependent emission behavior, covering almost the entire visible band (Fig.\u0026nbsp;\u003cspan class=\"InternalRef\"\u003e2\u003c/span\u003ed and Supplementary Fig.\u0026nbsp;5). After exposure to different excitation light sources, even the white light, RTP SiO\u003csub\u003e2\u003c/sub\u003e NPs present colorful afterglow, and the afterglow persisting is over 17 s at 365 nm excitation (Supplementary Fig.\u0026nbsp;6 and Supplementary Movie 1). We preliminarily speculate that this excitation dependent optical behavior may be caused by different defective luminescent states formed by organic molecules or generation of different fluorescent molecules during the calcination process.\u003csup\u003e\u003cspan class=\"CitationRef\"\u003e22\u003c/span\u003e,\u003cspan class=\"CitationRef\"\u003e23\u003c/span\u003e\u003c/sup\u003e Besides, the time-resolved RTP emission spectra of RTP SiO\u003csub\u003e2\u003c/sub\u003e NPs excited at 365 nm further confirms the long-lived RTP emission with an optimum decay lifetime of 2 s at the 504 nm emission band (Fig.\u0026nbsp;\u003cspan class=\"InternalRef\"\u003e2\u003c/span\u003ee). Furthermore, as the temperature increasing from 77 K to 317 K, a noticeable decrease in RTP emission intensity and RTP decay lifetime is observed, confirming the absence of a thermally enhanced process, and presenting typical phosphorescence characteristics (Supplementary Fig.\u0026nbsp;7).\u003csup\u003e\u003cspan class=\"CitationRef\"\u003e24\u003c/span\u003e,\u003cspan class=\"CitationRef\"\u003e25\u003c/span\u003e\u003c/sup\u003e In addition, the optical intensity of RTP SiO\u003csub\u003e2\u003c/sub\u003e NPs also maintains excellent stability even in different organic solvents and metal ion solutions (Supplementary Fig.\u0026nbsp;8), which reflects a good anti-quenching ability, and further proves that the chemiluminescence center of RTP SiO\u003csub\u003e2\u003c/sub\u003e NPs is located in the interior of SiO\u003csub\u003e2\u003c/sub\u003e NPs.\u003c/p\u003e\n\u003cp\u003eInterestingly, by simple evaporation-induced self-assembly, RTP SiO\u003csub\u003e2\u003c/sub\u003e NPs can be arranged in periodic array structures. As presented in Fig.\u0026nbsp;\u003cspan class=\"InternalRef\"\u003e2\u003c/span\u003ef and g, the RTP SiO\u003csub\u003e2\u003c/sub\u003e NPs exhibit an ordered close-packed state with two or more layers, respectively. Scanning electron microscopy (SEM) has also confirmed that the synthesized RTP SiO\u003csub\u003e2\u003c/sub\u003e NPs are capable of forming highly ordered, closely packed periodic structures, which exhibit the characteristics of PC structure (Fig.\u0026nbsp;\u003cspan class=\"InternalRef\"\u003e2\u003c/span\u003eh).\u003csup\u003e\u003cspan class=\"CitationRef\"\u003e26\u003c/span\u003e\u003c/sup\u003e In addition, RTP SiO\u003csub\u003e2\u003c/sub\u003e NPs can also achieve PC array in the form of simple cubic close-packed arrangement (Supplementary Fig.\u0026nbsp;9). Therefore, the multimodal PC assembled from RTP SiO\u003csub\u003e2\u003c/sub\u003e NPs not only retain its intrinsic FL and RTP emission capabilities, but also possess the ability to manipulate light through its physical microstructures, thereby achieving vivid structural colors. As shown in Fig.\u0026nbsp;\u003cspan class=\"InternalRef\"\u003e2\u003c/span\u003ei, the assembled multimodal PC displays angle-dependent structural colors, bright blue FL and time-dependent green RTP under different light stimulation (Supplementary Movie 2). As the observation angle (\u003cem\u003e\u0026theta;\u003c/em\u003e) decreases from 90\u003csup\u003eo\u003c/sup\u003e to 20\u003csup\u003eo\u003c/sup\u003e, the structural colors of the multimodal PC gradually transition from red to blue, which is consistent with the angle-dependent reflection spectra (Fig.\u0026nbsp;\u003cspan class=\"InternalRef\"\u003e2\u003c/span\u003ej). This phenomenon is in accordance with Bragg's law for traditional PC, as described by Eq.\u0026nbsp;(\u003cspan class=\"InternalRef\"\u003e1\u003c/span\u003e):\u003csup\u003e\u003cspan class=\"CitationRef\"\u003e27\u003c/span\u003e\u003c/sup\u003e\u003c/p\u003e\n\u003cdiv id=\"Equ1\" class=\"Equation\"\u003e\n\u003cdiv id=\"FileID_Equ1\" class=\"mathdisplay\"\u003e$$\\:\\lambda\\:\\propto\\:d\\bullet\\:sin\\theta\\:$$\u003c/div\u003e\n\u003cdiv class=\"EquationNumber\"\u003e1\u003c/div\u003e\n\u003c/div\u003e\n\u003cp\u003ewhere \u003cem\u003ed\u003c/em\u003e refers to the distance between the adjacent centers of the RTP SiO\u003csub\u003e2\u003c/sub\u003e NPs, and \u003cem\u003e\u0026theta;\u003c/em\u003e is the angle between the PCs surface and the incident light or reflect light. Moreover, the multimodal PC self-assembled from RTP SiO\u003csub\u003e2\u003c/sub\u003e NPs with varying diameters exhibit distinct structural colors (Supplementary Fig.\u0026nbsp;10, Fig.\u0026nbsp;11 and Fig.\u0026nbsp;12), whereas FL and RTP emission exhibit diameter-independent properties and the persistence of afterglow is more than 9 s (Supplementary Fig.\u0026nbsp;13 and Fig.\u0026nbsp;14).\u003c/p\u003e\n\u003cp\u003e\u0026nbsp;\u003c/p\u003e\n\u003c/div\u003e\n\u003ch3\u003eMechanism Investigations of RTP SiO NPs Production by Calcination\u003c/h3\u003e\n\u003cp\u003eGenerally, the realization of phosphorescent materials needs to meet two basic requirements, one is the chemically defective luminescence centers, the other is a rigid environment to stabilize the triplet excitons in these luminescent centers.\u003csup\u003e\u003cspan class=\"CitationRef\"\u003e28\u003c/span\u003e\u003c/sup\u003e Therefore, we first explore the formation of chemically luminescent centers within RTP SiO\u003csub\u003e2\u003c/sub\u003e NPs during the calcination process. Compared with the uncalcined SiO\u003csub\u003e2\u003c/sub\u003e NPs, a large number of structural defects are generated inside the calcined particles, and these defects have obvious lattice fringes with a lattice spacing of approximately 0.21 nm (Fig.\u0026nbsp;\u003cspan class=\"InternalRef\"\u003e3\u003c/span\u003ea). Upon etching away the silica network with hydrofluoric acid, the exposed internal defect structure is revealed to be composed of spherical nanoparticles and retains similar lattice spacing, exhibiting the characteristic fluorescent CDs structure.\u003csup\u003e\u003cspan class=\"CitationRef\"\u003e29\u003c/span\u003e,\u003cspan class=\"CitationRef\"\u003e30\u003c/span\u003e\u003c/sup\u003e Hence, it is obvious that during the calcination process, glucose molecules undergo in-situ carbonization, aggregation and crystallization within the SiO\u003csub\u003e2\u003c/sub\u003e NPs to generate CDs. Furthermore, the formation and growth process of CDs is studied by calcining SiO\u003csub\u003e2\u003c/sub\u003e NPs doped with glucose molecules at different temperatures. It is found that the calcination temperature of 325 \u003csup\u003eo\u003c/sup\u003eC is sufficient to convert the glucose molecules inside the SiO\u003csub\u003e2\u003c/sub\u003e NPs into CDs (Supplementary Fig.\u0026nbsp;15), and the size of CDs increases with increasing calcination temperature, growing from 2.82 nm at 325 \u003csup\u003eo\u003c/sup\u003eC to 7.47 nm at 575 \u003csup\u003eo\u003c/sup\u003eC (Fig.\u0026nbsp;\u003cspan class=\"InternalRef\"\u003e3\u003c/span\u003eb). Moreover, the RTP spectra and time-resolved RTP spectra of RTP SiO\u003csub\u003e2\u003c/sub\u003e NPs calcined at different temperatures show optimum intensity and the longest RTP lifetime at 575 \u003csup\u003eo\u003c/sup\u003eC calcination (Supplementary Fig.\u0026nbsp;16 and Fig.\u0026nbsp;17). It can be inferred that as the calcination temperature increases (from 325 \u003csup\u003eo\u003c/sup\u003eC to 575 \u003csup\u003eo\u003c/sup\u003eC), the crystalline structure of the CDs derived from glucose becomes more stable, and the non-radiative transitions of electrons is weaken, leading to a higher overall luminescence efficiency (Supplementary Fig.\u0026nbsp;18 and Fig.\u0026nbsp;19).\u003csup\u003e\u003cspan class=\"CitationRef\"\u003e31\u003c/span\u003e\u003c/sup\u003e High-resolution TEM (HR-TEM) has successfully validated this point. As presented in Fig.\u0026nbsp;\u003cspan class=\"InternalRef\"\u003e3\u003c/span\u003ec, the generated CDs exhibit characteristics of small size and low crystallinity at 325 \u003csup\u003eo\u003c/sup\u003eC calcination temperature, and these small-sized CDs grow and simultaneously aggregate as the temperature increases to 425\u0026deg;C, forming larger-sized CDs with high lattice defects. As the temperature further increases to 575 \u003csup\u003eo\u003c/sup\u003eC, the defect structures within the CDs are gradually filled and reduced, resulting in the formation of large-sized CDs with high crystallinity. It is worth mentioning that the captured arrangement of carbon atoms deviates from the hexagonal honeycomb structure, which may be attributed to the varying spatial orientations of the CDs.\u003csup\u003e\u003cspan class=\"CitationRef\"\u003e32\u003c/span\u003e\u003c/sup\u003e The corresponding intensity ratio between crystalline G band (I\u003csub\u003eG\u003c/sub\u003e) and disordered D band (I\u003csub\u003eD\u003c/sub\u003e) in Raman spectra increases from 0.827 to 1.111 with the calcination temperature rising from 325 \u003csup\u003eo\u003c/sup\u003eC to 575 \u003csup\u003eo\u003c/sup\u003eC, which is consistent with the HR-TEM results (Supplementary Fig.\u0026nbsp;20). Consequently, the chemiluminescence centers of RTP SiO\u003csub\u003e2\u003c/sub\u003e NPs after calcination are derived from internal in-situ generated CDs, and further confirms that even a single organic small-molecule carbon source can also be converted to CDs through carbonation, aggregation and crystallization within the silica matrix (Fig.\u0026nbsp;\u003cspan class=\"InternalRef\"\u003e3\u003c/span\u003ed).\u003c/p\u003e\n\u003cp\u003eSubsequently, we analyze the reasons for the formation of stable triplet states (T\u003csub\u003e1\u003c/sub\u003e) responsible for the long-lived RTP of CDs during the calcination process. The temperature-dependent Fourier transform-infrared spectroscopy (FT-IR) show a gradual increase in the C-Si bonds at approximately 807 cm\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e with increasing calcination temperature, while the Si-O-Si/Si-O-C groups at approximately 1046\u0026ndash;1299 cm\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e gradually decrease, indicating that during the calcination process, some Si-O-Si/Si-O-C bonds break and form new C-Si covalent bonds with the CDs (Supplementary Fig.\u0026nbsp;21). Besides, the fitted high-resolution Si 2p results spectra of RTP SiO\u003csub\u003e2\u003c/sub\u003e NPs show an increase in the relative content of C-Si bonds at 102.1 eV as increasing calcination temperature (Supplementary Fig.\u0026nbsp;22). Notably, the C 1s and O 1s band of RTP SiO\u003csub\u003e2\u003c/sub\u003e NPs verify the presence of O-related defect states, which provide a guarantee for long-lived RTP (Supplementary Fig.\u0026nbsp;23, Fig.\u0026nbsp;24 and Fig.\u0026nbsp;25). Taken together, during the calcination process, the growth and crystallization of CDs are accompanied by a simultaneous formation of a rigid covalent C-Si network with SiO\u003csub\u003e2\u003c/sub\u003e matrix, which facilitates the stabilization of triplet excitons and effectively suppresses the non-radiative transitions of the T\u003csub\u003e1\u003c/sub\u003e, thereby generating long-lived RTP emission.\u003csup\u003e\u003cspan class=\"CitationRef\"\u003e33\u003c/span\u003e,\u003cspan class=\"CitationRef\"\u003e34\u003c/span\u003e\u003c/sup\u003e\u003c/p\u003e\n\u003cp\u003eTheoretical calculations based on the distribution of molecular surface electrostatic potential (ESP) and density functional theory (DFT) are carried out to further reveal the mechanism of RTP property from RTP SiO\u003csub\u003e2\u003c/sub\u003e NPs. Based on HR-TEM and FT-IR results, the molecular structure of CDs at 325 \u003csup\u003eo\u003c/sup\u003eC,475 \u003csup\u003eo\u003c/sup\u003eC and 575 \u003csup\u003eo\u003c/sup\u003eC calcination conditions are selected and designed as computational models (Supplementary Fig.\u0026nbsp;26). With the increase of calcination temperature, the ESP of the CDs inside the RTP SiO\u003csub\u003e2\u003c/sub\u003e NPs gradually shifts to a neutral dominant electron density, where the blue region, red region and green region indicate the lower electron density, densely electron-dense region and neutrality, respectively (Fig.\u0026nbsp;\u003cspan class=\"InternalRef\"\u003e3\u003c/span\u003ee). This calculation results indicate that the high crystallinity and abundant C-Si covalent bonds formed under high-temperature calcination (575 \u003csup\u003eo\u003c/sup\u003eC) can render the molecular structure more stable, which provides a rigid environment for restricting excited molecular motions of luminescent centers, and thus suppressing non-radiative processes.\u003csup\u003e\u003cspan class=\"CitationRef\"\u003e35\u003c/span\u003e\u003c/sup\u003e In addition, the HOMO-LUMO energy gap of the CDs decreases from 3.0928 eV to 2.0237 eV with the increase of the calcination temperature (Fig.\u0026nbsp;\u003cspan class=\"InternalRef\"\u003e3\u003c/span\u003ef and Supplementary Fig.\u0026nbsp;27). The lower the HOMO-LUMO energy gap, the higher the efficiency in the generation and capture of electron excitons, which facilitates the formation and transition of triplet excitons.\u003c/p\u003e\n\u003cp\u003eBased on the aforementioned analysis, the internal carbon source within SiO\u003csub\u003e2\u003c/sub\u003e NPs and the calcination process are the two critical factors for achieving RTP. Therefore, we deduce that the preparation of spherical RTP SiO\u003csub\u003e2\u003c/sub\u003e NPs is irrelevant to the type of introduced carbon-containing small organic molecules during the St\u0026ouml;ber method. As illustrated in Fig.\u0026nbsp;\u003cspan class=\"InternalRef\"\u003e3\u003c/span\u003eg, in addition to glucose, 12 different kinds of organic molecules are selected, including nitrogen-containing organic molecules and fluorescent dye molecules. Evidently, the SiO\u003csub\u003e2\u003c/sub\u003e NPs doped with these molecules all exhibit long-lived RTP decay characteristics after calcination (Supplementary Fig.\u0026nbsp;28), demonstrating the universality of this strategy. The inexpensive of the precursor and convenient preparation method ensures the feasibility of large-scale production of RTP SiO\u003csub\u003e2\u003c/sub\u003e NPs. By proportionally scaling up the reaction precursors during the synthesis process, it is possible to effortlessly produce a large quantity of spherical RTP nanospheres, with the mass exceeding 700 g (Fig.\u0026nbsp;\u003cspan class=\"InternalRef\"\u003e3\u003c/span\u003eh).\u003c/p\u003e\n\u003cp\u003e\u0026nbsp;\u003c/p\u003e\n\u003ch3\u003ePhotonic Bandgap-Induced Angle-dependent Chromatic Behavior of PC Gels\u003c/h3\u003e\n\u003cp\u003eSubsequently, RTP SiO\u003csub\u003e2\u003c/sub\u003e NPs with different diameters are dispersed in a mixture of ethanol, ethoxylated trimethylolpropane triarchy-late (ETPTA), poly (ethylene glycol) diacrylate (PEGDA) and ethylene glycol (EG) to prepare blue, green and red photonic gels (B-, G-, R-PC gels) using a supersaturated evaporation-induced self-assembly method in solvent. These PC gels possess SC, FL and RTP simultaneously under different light stimulation conditions (Fig.\u0026nbsp;\u003cspan class=\"InternalRef\"\u003e4\u003c/span\u003ea). However, there are significant differences in the emission intensities and color of FL and RTP for the three PC gels. Evidently, the PBG generated by the ordered array of RTP SiO\u003csub\u003e2\u003c/sub\u003e NPs through non-close packing exerts a regulatory influence on their own FL and RTP emissions (Fig.\u0026nbsp;\u003cspan class=\"InternalRef\"\u003e4\u003c/span\u003eb, Supplementary Fig.\u0026nbsp;29). When the emission band of FL and RTP align with the PBG, it means the transition energy levels of the molecules match the lattice constant of the photonic crystal, and specific resonant coupling interactions are activated, which enhances the energy transfer efficiency between photons, thereby increasing the intensity of FL and RTP (Fig.\u0026nbsp;\u003cspan class=\"InternalRef\"\u003e4\u003c/span\u003ec).\u003csup\u003e\u003cspan class=\"CitationRef\"\u003e36\u003c/span\u003e\u0026ndash;\u003cspan class=\"CitationRef\"\u003e38\u003c/span\u003e\u003c/sup\u003e Therefore, the FL emission is stronger in the B-PC gel, whereas the RTP exhibits a stronger emission in the G-PC gel.\u003c/p\u003e\n\u003cp\u003eOn the other hand, owing to the broad emission characteristics of FL and RTP in PC gel, it is possible to realize PBG-induced color variations in FL and RTP through the modulation of the PBG to facilitate resonance enhancement of a specific emission bandgap. As depicted in Fig.\u0026nbsp;\u003cspan class=\"InternalRef\"\u003e4\u003c/span\u003ed, the angle-dependent multimodal photonic device is fabricated by spin-coating a R-PC gel with a thickness of 0.5 mm onto a black light-absorbing substrate and covering it with high-transparency quartz glass. Then, the incident light area (white or UV light) and the light-signal reception area (SC, FL and RTP) are partially separated using a black opaque light-absorbing plate. Fixing the incident light angle (\u0026theta;\u003csub\u003e1\u003c/sub\u003e) at 90\u0026deg;, the angle-dependent PBG gradually blue-shifts from 611 nm to 405 nm as the observation angle (\u0026theta;\u003csub\u003e2\u003c/sub\u003e) decreases from 90\u003csup\u003eo\u003c/sup\u003e to 30\u003csup\u003eo\u003c/sup\u003e (Supplementary Fig.\u0026nbsp;30). As anticipated, the blue shift of the PBG leads to a noticeable shift in the additional PBG resonance peaks of the FL and RTP emissions from the R-PC gel (Fig.\u0026nbsp;\u003cspan class=\"InternalRef\"\u003e4\u003c/span\u003ee and \u003cspan class=\"InternalRef\"\u003e4\u003c/span\u003ef). When the emission wavelengths of FL and RTP fall within the PBG range of PC gel, their propagation is significantly suppressed. These specific wavelength bands of FL and RTP undergo multiple reflections within the PC structure, which enhances photon-matter interaction efficiency and remarkably improves the resonant coupling efficiency between luminescent molecules (or excitons) and the PBG of photonic crystals. Furthermore, due to the anisotropic property of the PC gel structure, the PBG exhibits direction-dependent bandgap characteristics in different spatial orientations, which enables specific FL and RTP wavelength bands to satisfy matching conditions only within predetermined angle ranges, thereby inducing directional resonant coupling. Therefore, the overall detected FL and RTP spectra show a superposition of the constant FL or RTP peaks with the angle-dependent PBG resonance enhancement peaks, resulting in an angle-dependent chromatic behavior. Interestingly, as the observation angle decreases from 90\u0026deg; to 30\u0026deg;, the color changes of three optical signals in the R-PC gel are visible to the naked eye. Under white light illumination, the SC of the R-PC gel gradually changes from red to violet as the observation angle decreases from 90\u003csup\u003eo\u003c/sup\u003e to 30\u003csup\u003eo\u003c/sup\u003e, and under UV light illumination or turned off, the FL of the R-PC gel gradually transitions from pink to blue, while the RTP shifts from yellow-green to cyan (Fig.\u0026nbsp;\u003cspan class=\"InternalRef\"\u003e4\u003c/span\u003eg and Supplementary Movie 3). It is worth mentioning that the angle-dependent chromatic behavior for FL and RTP only exists in highly ordered photonic crystal structures (with angle dependent PBG), while it is difficult to observe such chromatic behavior for poorly ordered PC structures (Supplementary Fig.\u0026nbsp;31). Besides, as the observation angle changes, the PBG gradually matches with the emission wavelengths, enabling the detection of stronger FL and RTP signals, and the enhancement effects of FL and RTP are most pronounced at \u0026theta;\u003csub\u003e2\u003c/sub\u003e\u0026thinsp;=\u0026thinsp;40\u0026deg; and \u0026theta;\u003csub\u003e2\u003c/sub\u003e\u0026thinsp;=\u0026thinsp;50\u0026deg;, respectively (Fig.\u0026nbsp;\u003cspan class=\"InternalRef\"\u003e4\u003c/span\u003eh).\u003csup\u003e\u003cspan class=\"CitationRef\"\u003e39\u003c/span\u003e\u003c/sup\u003e The above angle-dependent chromatic behavior of FL and RTP also exits in the B-PC gel and G-PC gel (Supplementary Fig.\u0026nbsp;32, Fig.\u0026nbsp;33 and Fig.\u0026nbsp;34).\u003c/p\u003e\n\u003cp\u003eThe influence of the incident angle of excitation light on the optical behavior of PC gel is further investigated. As the incident angle (\u0026theta;\u003csub\u003e1\u003c/sub\u003e) of the UV light decreases from 90\u0026deg; to 30\u0026deg;, the wavelengths of the FL and RTP spectra measured at \u0026theta;\u003csub\u003e2\u003c/sub\u003e\u0026thinsp;=\u0026thinsp;90\u0026deg; remain constant, while the emission intensities gradually decrease (Fig.\u0026nbsp;\u003cspan class=\"InternalRef\"\u003e4\u003c/span\u003ei and Supplementary Fig.\u0026nbsp;35). Since the PBG of PC gel is located in the violet band at a low angle, the propagation of external incident UV light is prohibited when it is incident on the PC gel surface at a low incidence angle, and the UV light is reflected from the structure by Bragg reflection, which reduces the excitation energy delivered to the embedded RTP SiO\u003csub\u003e2\u003c/sub\u003e NPs, thereby suppressing the emission intensity of FL and RTP.\u003csup\u003e\u003cspan class=\"CitationRef\"\u003e40\u003c/span\u003e\u003c/sup\u003e Meanwhile, the incident angle of the excitation light also affects the RTP decay lifetime of the PC gel (Fig.\u0026nbsp;\u003cspan class=\"InternalRef\"\u003e4\u003c/span\u003ej and Supplementary Fig.\u0026nbsp;36). Based on the above discussion, the FL and RTP of the PC gels are affected by both the incident angle of excitation light and the observation angle, where the former is mainly responsible for the modulation of the emission intensity, while the latter is used to realize the angle-dependent chromatic behavior (Fig.\u0026nbsp;\u003cspan class=\"InternalRef\"\u003e4\u003c/span\u003ek). In short, compared with complex chemical regulation, this angle-dependent physical modulation exhibits transient, highly stable and reproducible characteristics.\u003c/p\u003e\n\u003cp\u003e\u0026nbsp;\u003c/p\u003e\n\u003ch3\u003eThermal-Induced Self-Scattering Enhanced Luminescence and Chromatic Properties of PC Gels\u003c/h3\u003e\n\u003cp\u003eThe prepared PC gels also have unique thermal-induced self-scattering enhanced luminescence properties. As shown in Fig.\u0026nbsp;\u003cspan class=\"InternalRef\"\u003e5\u003c/span\u003ea, since R-PC gel is composed of polymer matrix with a temperature-sensitive refractive index (RI) and a temperature-independent SiO\u003csub\u003e2\u003c/sub\u003e NPs, the gel has temperature-regulated dynamic refractive index, and the RI-matching point is approximately 40 \u003csup\u003eo\u003c/sup\u003eC. As the temperature decreases from 40 \u003csup\u003eo\u003c/sup\u003eC to 0 \u003csup\u003eo\u003c/sup\u003eC, the refractive index between the two phases gradually mismatches, resulting in an increase in the light scattering capacity of the R-PC gel, thereby reducing the overall transmittance (Supplementary Fig.\u0026nbsp;37).\u003csup\u003e\u003cspan class=\"CitationRef\"\u003e41\u003c/span\u003e\u003c/sup\u003e Meanwhile, the strong light scattering at low temperature can also affect the FL and RTP emission. Compared with the RI-matching state at 40 \u003csup\u003eo\u003c/sup\u003eC, the emission intensity of FL and RTP at 0 \u003csup\u003eo\u003c/sup\u003eC increase by 128-fold and 87-fold, respectively (Fig.\u0026nbsp;\u003cspan class=\"InternalRef\"\u003e5\u003c/span\u003eb). Besides, the RTP lifetime in the scattered state is extended by 25-fold compared to the transparent state (Fig.\u0026nbsp;\u003cspan class=\"InternalRef\"\u003e5\u003c/span\u003ec). Importantly, the temperature-dependent multiple optical signals of PC gel can be easily captured. As the temperature decreases gradually from 40\u0026deg;C to 0\u0026deg;C, the PC gel turns from transparent state to white scattering state, and the blue FL is also accompanied by a significant enhancement in this process (Fig.\u0026nbsp;\u003cspan class=\"InternalRef\"\u003e5\u003c/span\u003ed and Supplementary Movie 4). Moreover, in the RI-matched transmittance state, the RTP signal of the PC gel is difficult to capture, while in the scattering state, the RTP signal exhibits a bright and persistent afterglow (Fig.\u0026nbsp;\u003cspan class=\"InternalRef\"\u003e5\u003c/span\u003ee and Supplementary Movie 5). Therefore, the overall optical signals of the PC gel, including transmitted light, scattered light, FL and RTP, can be modulated by simply changing temperature, and this modulation has a stable reproducibility (Fig.\u0026nbsp;\u003cspan class=\"InternalRef\"\u003e5\u003c/span\u003ef).\u003c/p\u003e\n\u003cp\u003eThe intrinsic physical mechanism of the thermal-induced self-scattering enhanced FL and RTP properties of the R-PC gel is further investigated. The scattering intensity of UV-excited light collected on the PC gel increases with decreasing temperature, suggesting that the scattering state at low temperatures can amplify the intensity of excitation light, thus leading to stronger photoexcitation of the inside RTP SiO\u003csub\u003e2\u003c/sub\u003e NPs (Supplementary Fig.\u0026nbsp;38). In other words, the interfacial scattering enhancement firstly induces multiple omni-directional scattering of the incident UV light inside the gel, which improves the overall excitation efficiency of RTP SiO\u003csub\u003e2\u003c/sub\u003e NPs (Fig.\u0026nbsp;\u003cspan class=\"InternalRef\"\u003e5\u003c/span\u003eg).\u003csup\u003e\u003cspan class=\"CitationRef\"\u003e42\u003c/span\u003e\u003c/sup\u003e Additionally, the collected FL decay spectra have a FL lifetime of 11.8 ns in the scattered state, which is longer than the 7.7 ns FL lifetime in the transmitted state (Supplementary Fig.\u0026nbsp;39). Considering that the scattering band of R-PC gel covers its own emission band, and there is a certain overlap between the excitation band and the emission band (Supplementary Fig.\u0026nbsp;40), these RTP SiO\u003csub\u003e2\u003c/sub\u003e NPs subjected to stronger excitation light will also emit strong scattered FL and RTP in all directions under the scattering state, and then their respective scattered light are continuously transferred, absorbed and re-emitted among particles, greatly contributing to the efficiency of energy utilization, thus further enhancing the FL and RTP intensities.\u003csup\u003e\u003cspan class=\"CitationRef\"\u003e43\u003c/span\u003e\u003c/sup\u003e\u003c/p\u003e\n\u003cp\u003eIn addition, the R-PC gel shows enhanced luminescence accompanied by color changes in the temperature interval from 20 \u003csup\u003eo\u003c/sup\u003eC to 40 \u003csup\u003eo\u003c/sup\u003eC. As shown in Fig.\u0026nbsp;\u003cspan class=\"InternalRef\"\u003e5\u003c/span\u003eh, the intensity assigned to the FL peak of R-PC gel at approximately 450 nm gradually increases, while the FL band enhanced by PBG resonance peak at 611 nm gradually decreases with the temperature decreasing from 40 \u003csup\u003eo\u003c/sup\u003eC to 20 \u003csup\u003eo\u003c/sup\u003eC. A similar trend is also observed in the temperature-dependent RTP spectra (Supplementary Fig.\u0026nbsp;41). Therefore, the thermochromic behavior of R-PC gel is achieved by appropriately modulating the ambient temperature to cause the two fluorescent emissions to compete with each other (Fig.\u0026nbsp;\u003cspan class=\"InternalRef\"\u003e5\u003c/span\u003ei and \u003cspan class=\"InternalRef\"\u003e5\u003c/span\u003ej). The strong scattering at low temperatures induces a decrease in the reflectivity of the PC gel, hindering the resonance-enhanced interactions of the PBG for specific bands of FL or RTP (Supplementary Fig.\u0026nbsp;42). In conclusion, this R-PC gel composed of spherical phosphor nanoparticles not only integrates multiple optical signals, but also has multi-modal and multi-dimensional stimulus response properties, which provides a new road for designing intelligent optical devices.\u003c/p\u003e\n\u003cp\u003e\u0026nbsp;\u003c/p\u003e"},{"header":"Discussion","content":"\u003cp\u003eIn summary, we demonstrate a scalable and universal approach for synthesizing monodisperse RTP SiO\u003csub\u003e2\u003c/sub\u003e NPs with uniform spherical geometry. During high-temperature calcination, the introduced organic small molecules embedded in silica networks undergo in situ carbonization and crystallization to form CDs, while the covalent silica network stabilizes triplet excited states through spatial confinement, enabling robust RTP emission. The resulting RTP SiO\u003csub\u003e2\u003c/sub\u003e NPs retain programmable self-assembly capabilities, generating photonic crystals that synergistically integrate structural color, FL and RTP into a single multimodal optical platform. To harness dynamic interactions between PBG effects and FL or RTP emission, we engineered metastable multi-mode PC gels with angle-dependent PBG modulation. These gels exhibit unprecedented angle chromatic responses, where light propagation is modulated by the angle dependence of PBG, resulting in rare FL-RTP angle responses. Furthermore, the thermally tunable refractive index mismatch between SiO\u003csub\u003e2\u003c/sub\u003e NPs and the liquid matrix enables dynamic modulation of light scattering and transmission pathways, yielding temperature-gated self-scattering effects that amplify both FL and RTP intensities. The strategy of large-scale preparation of monodisperse RTP SiO\u003csub\u003e2\u003c/sub\u003e NPs and the successful integration of physical photonic structure and chemiluminescence provide new approach for constructing advanced multi-mode luminescent devices.\u003c/p\u003e \u003cdiv id=\"Sec8\" class=\"Section2\"\u003e \u003cdiv id=\"Sec9\" class=\"Section3\"\u003e \u003c/div\u003e \u003c/div\u003e\n\n "},{"header":"Methods","content":"\u003ch2\u003eReagents and materials\u003c/h2\u003e\n\u003cp\u003eAmmonia, tetraethyl orthosilicate, ethoxylated trimethylolpropane triarchy-late (average Mn\u0026thinsp;~\u0026thinsp;428 MW), poly(ethylene glycol) diacrylate (PEG average Mn\u0026thinsp;~\u0026thinsp;400 MW), ethylene glycol, glucose, tartaric acid, p-phthalic acid, vitamin C, urea, dopamine, melamine, thiourea, rhodamine B, rhodamine 6G, quinine sulphate and sulforhodamine B are obtained from Shanghai Aladdin Reagent Co., Ltd.. Tetraethyl orthosilicate is purchased from Damao Chemical Reagent Factory. Ethanol is purchased from Tianjin Fuyu Fine Chemical Co., Ltd.. All reagents are of analytical grade and used directly without further purification. Deionized water is produced through a Millipore water purification system (Milli-Q, Millipore) and used throughout the study.\u003c/p\u003e\n\u003ch3\u003eSynthesis of RTP SiO NPs\u003c/h3\u003e\n\u003cp\u003eMonodisperse RTP SiO\u003csub\u003e2\u003c/sub\u003e NPs is synthesized through a modified St\u0026ouml;ber method and their sizes can be regulated by adjusting ethanol ratio during the preparation process. Firstly, 6 mL of glucose aqueous solution (1 mol/L), 130 mL of ethanol and 16 mL of ammonia are mixed homogeneously in a 500 mL three-necked flask and heated to 60 \u003csup\u003eo\u003c/sup\u003eC. Then, the mixture of 12 mL of tetraethyl orthosilicate and 10 mL ethanol is added and stirred at 60 \u003csup\u003eo\u003c/sup\u003eC for 100 minutes in a water bath environment. The white suspension obtained is repeatedly centrifuged three times with ethanol at 7000 rpm. The collected white precipitate is dried at 50 \u003csup\u003eo\u003c/sup\u003eC for 48 h to obtain organic small molecule doped SiO\u003csub\u003e2\u003c/sub\u003e NPs. Then, quartz crucible with CDs@SiO\u003csub\u003e2\u003c/sub\u003e NPs is transferred to a high temperature box-type electric resistance furnace, heated up to 575 \u003csup\u003eo\u003c/sup\u003eC in 3 hours and kept for 2 hours, finally cooled naturally to room temperature and obtained the RTP SiO\u003csub\u003e2\u003c/sub\u003e NPs.\u003c/p\u003e\n\u003ch2\u003ePreparation of PCs assembled by RTP SiO\u003csub\u003e2\u003c/sub\u003e NPs\u003c/h2\u003e\n\u003cp\u003eThe RTP SiO\u003csub\u003e2\u003c/sub\u003e NPs are uniformly dispersed in ethanol to form a white suspension (4 wt.%). Then, the commercial glass is stabilized in the suspension at an inclination angle of 30\u003csup\u003eo\u003c/sup\u003e. The ethanol is evaporated at an ambient temperature of 50 \u003csup\u003eo\u003c/sup\u003eC to allow the RTP SiO\u003csub\u003e2\u003c/sub\u003e NPs to uniformly self-assemble on the glass sheet to form PCs. The PCs with different colors can be prepared by selecting different particle sizes of RTP SiO\u003csub\u003e2\u003c/sub\u003e NPs.\u003c/p\u003e\n\u003ch2\u003ePreparation of PC gels\u003c/h2\u003e\n\u003cp\u003eBriefly, RTP SiO\u003csub\u003e2\u003c/sub\u003e NPs (0.12 cm\u003csup\u003e\u003cspan class=\"CitationRef\"\u003e3\u003c/span\u003e\u003c/sup\u003e) are dispersed in a mixture of ethanol (3 mL), ETPTA (140 \u0026micro;L), PEGDA (70 \u0026micro;L) and EG (70 \u0026micro;L) under sonication. The PC gel is obtained by evaporating the mixture at 90 \u003csup\u003eo\u003c/sup\u003eC for 2 hours to ethanol the alcohol, and the volume fraction of RTP SiO\u003csub\u003e2\u003c/sub\u003e NPs, ETPTA, PEGDA and EG in the PC gel is 30%, 35%, 17.5% and 17.5%, respectively. PC gel with different colors can be prepared with different particle sizes of RTP SiO\u003csub\u003e2\u003c/sub\u003e NPs. Subsequently, the prepared PC gel is filled into a customized black light-absorbing plate and quartz glass interlayer to achieve the optical behavior of angle-dependent chromatic.\u003c/p\u003e\n\u003ch2\u003eCharacterization\u003c/h2\u003e\n\u003cp\u003eOptical reflectance spectra, transmittance spectra, FL spectra and RTP spectra are captured utilizing a fiber optic spectrometer (PG2000-Pro), and all RTP emission spectra are measured at 10 ms delay time after turning the externally equipped UV lamp off. The UV-vis absorption spectra are measured with a PerkinElmer PE Lambda 950 spectrometer. Temperature-dependent afterglow spectra and RTP lifetime decay profile is collected with the FLS1000 instrument equipped with the OXFORD accessory. The morphologies of PCs and PC gel are analyzed using a Zeiss Sigma 300 field emission scanning electron microscope. TEM images, HAADF-STEM images and their corresponding EDS mapping images are obtained on a JEM-2100 apparatus operating at 200 kV. HR-TEM images are taken by a 300 KV double spherical aberration corrected electron microscope, JEM-ARM300F2 (Grand ARM). The FT-IR spectra is acquired on a Nicolet iS50 FTIR spectrometer. The XPS measurements are performed on an Thermo Scientific K-Alpha spectrometer. Digital photographs of the device are captured using an iPhone 13.\u003c/p\u003e\n\u003ch2\u003eTheoretical Calculations\u003c/h2\u003e\n\u003cp\u003eQuantum chemical studies are performed employing density functional theory (DFT) implemented in the Optimal Reciprocal Collision Avoidance (ORCA) program. To explore the mechanism by which stiff C-Si bonds, dense silica-oxygen structure and the degree of crystallinity of CDs affect the phosphorescence characteristics of CDs. Based on the results of, HR-TEM, FT-IR spectroscopy and XPS characterization, there are variations in the Si-O-C and Si-C covalent bonds from CDs-325\u003csup\u003eo\u003c/sup\u003eC, CDs-475 \u003csup\u003eo\u003c/sup\u003eC, and CDs-575 \u003csup\u003eo\u003c/sup\u003eC, which are chosen as the study models of CDs-325 \u003csup\u003eo\u003c/sup\u003eC, CDs-475 \u003csup\u003eo\u003c/sup\u003eC and CDs-575 \u003csup\u003eo\u003c/sup\u003eC, respectively. The input files are generated employing Avogadro. Geometry optimization of CDs-325\u003csup\u003eo\u003c/sup\u003eC, CDs-475 \u003csup\u003eo\u003c/sup\u003eC and CDs-575 \u003csup\u003eo\u003c/sup\u003eC models is initially performed at the B97-3c level, followed by single-point-energy (SPE) calculations employing the high-precision basis set B3LYP/def2-TZVP. To gain a more thorough understanding of the electronic structure, it is further investigated that SPE calculations provide the basis for the distribution of frontier molecular orbitals and the electrostatic potential (ESP). The molecular visualization programs Jmol and Chemcraft are used for the analysis.\u003c/p\u003e"},{"header":"Declarations","content":"\u003cp\u003eAcknowledgements\u003c/p\u003e\n\u003cp\u003eThis work was supported by the National Key R\u0026amp;D Program of China (2022YFE0109500), the National Natural Science Foundation of China (No. 62475212, 61975162), and the Shaanxi Province Natural Science Foundation (No. 2020JM-062). We thank Dr. D. He at the Instrument Analysis Center of Xi\u0026rsquo;an Jiaotong University for the\u0026nbsp;kinetic decay curves\u0026nbsp;spectra experiments. We thank the Xi\u0026apos;an Yizhichen Biotechnology Co., Ltd. for their help in purchasing reagents for this experiment.\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003eAuthor contributions\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003eThe overall experimental design was conceived by C.W., Y.N., and Y.Y., and together, they coordinated the full project. C.W., and Y.N. designed the materials and conducted experiments. C.W., X.W., Y.X., and J.L. characterized, and analyzed the materials. C.W., Y.N., Y.X., G.D., and J.L. built underwater sensing and performed data collection and analysis. All authors also discussed and interpreted the experimental data and results. C.W. and N.B. performed the theoretical calculations. C.W. wrote the manuscript with contributions from all authors. X.L. and S.Y. reviewed and edited the paper. All authors discussed the results and commented on the paper.\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003eCompeting interests\u0026nbsp;\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003eThe authors declare no conflict of interest.\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003eData availability\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003eThe data required to reproduce the findings are included in the article and its Supplementary Information. All other information can be obtained from the corresponding author upon request. Source data are provided with this paper.\u003c/p\u003e"},{"header":"References","content":"\u003col\u003e\u003cli\u003e\u003cspan\u003eGu L et al (2019) Colour-tunable ultra-long organic phosphorescence of a single-component molecular crystal. 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ACS Appl Mater Interfaces 6:6317\u0026ndash;6321. \u003cspan class=\"ExternalRef\"\u003e\u003cspan class=\"RefSource\"\u003ehttps://doi.org/10.1021/am501420w​\u003c/span\u003e\u003cspan address=\"10.1021/am501420w​\" targettype=\"DOI\" class=\"RefTarget\"\u003e\u003c/span\u003e\u003c/span\u003e\u003c/span\u003e\u003c/li\u003e\u003c/ol\u003e"}],"fulltextSource":"","fullText":"","funders":[],"hasAdminPriorityOnWorkflow":false,"hasManuscriptDocX":true,"hasOptedInToPreprint":true,"hasPassedJournalQc":"","hasAnyPriority":true,"hideJournal":false,"highlight":"","institution":"","isAcceptedByJournal":true,"isAuthorSuppliedPdf":false,"isDeskRejected":"","isHiddenFromSearch":false,"isInQc":false,"isInWorkflow":false,"isPdf":false,"isPdfUpToDate":true,"isWithdrawnOrRetracted":false,"journal":{"display":true,"email":"[email protected]","identity":"nature-portfolio","isNatureJournal":true,"hasQc":false,"allowDirectSubmit":false,"externalIdentity":"","sideBox":"","snPcode":"","submissionUrl":"","title":"Nature Portfolio","twitterHandle":"","acdcEnabled":false,"dfaEnabled":false,"editorialSystem":"ejp","reportingPortfolio":"","inReviewEnabled":true,"inReviewRevisionsEnabled":false},"keywords":"","lastPublishedDoi":"10.21203/rs.3.rs-6358279/v1","lastPublishedDoiUrl":"https://doi.org/10.21203/rs.3.rs-6358279/v1","license":{"name":"CC BY 4.0","url":"https://creativecommons.org/licenses/by/4.0/"},"manuscriptAbstract":"\u003cp\u003eDeveloping room-temperature phosphorescent (RTP) materials with microscale periodic structures presents a promising prospect for future optical applications but remains extremely challenging due to the complex integration of luminescent and structural components. Herein, we present an emerging strategy for mass-producing monodisperse RTP silica nanospheres (RTP SiO\u003csub\u003e2\u003c/sub\u003e NPs) using a modified St\u0026ouml;ber method, where organic molecules are embedded in silica networks and undergone in situ carbonization, aggregation and crystallization to form phosphorescent carbon dots under high temperature calcination. These NPs can self-assemble into photonic crystal (PC) structures, enabling the straightforward integration of structural color, fluorescence (FL) and RTP to achieve multimodal luminescent properties. The angle-dependent photonic bandgap (PBG) generated by the physical periodic structure modulates light propagation in RTP PC gel, creating unique FL and RTP angle-dependent chromatic responses. Temperature-induced refractive index changes between SiO\u003csub\u003e2\u003c/sub\u003e and the liquid matrix further enable dynamic control of light scattering states, significantly altering transmittance and emission intensities of FL and RTP. This successful fusion of physical photonic structures with chemical luminescence offers new approach for constructing advanced multimodal luminescent devices.\u003c/p\u003e","manuscriptTitle":"Scalable Synthesis of Self-Assembling Monodisperse Phosphorescent Nanospheres Enabling Multi-Mode Angle-Dependent and Thermal-Responsive Photonic Gels","msid":"","msnumber":"","nonDraftVersions":[{"code":1,"date":"2025-04-07 05:30:45","doi":"10.21203/rs.3.rs-6358279/v1","editorialEvents":[],"status":"published","journal":{"display":true,"email":"[email protected]","identity":"nature-communications","isNatureJournal":true,"hasQc":false,"allowDirectSubmit":false,"externalIdentity":"NCOMMS","sideBox":"Learn more about [Nature Communications](http://www.nature.com/ncomms/)","snPcode":"","submissionUrl":"https://mts-ncomms.nature.com/","title":"Nature Communications","twitterHandle":"","acdcEnabled":true,"dfaEnabled":true,"editorialSystem":"ejp","reportingPortfolio":"Nature Communications","inReviewEnabled":true,"inReviewRevisionsEnabled":false}}],"origin":"","ownerIdentity":"0883cfbe-da49-4357-be72-2c20e25a7b6f","owner":[],"postedDate":"April 7th, 2025","published":true,"recentEditorialEvents":[],"rejectedJournal":[],"revision":"","amendment":"","status":"published-in-journal","subjectAreas":[{"id":46682227,"name":"Physical sciences/Optics and photonics/Optical materials and structures/Photonic crystals"},{"id":46682228,"name":"Physical sciences/Optics and photonics/Optical materials and structures/Nanoparticles"}],"tags":[],"updatedAt":"2025-08-07T07:07:41+00:00","versionOfRecord":{"articleIdentity":"rs-6358279","link":"https://doi.org/10.1038/s41467-025-61967-9","journal":{"identity":"nature-communications","isVorOnly":false,"title":"Nature Communications"},"publishedOn":"2025-07-18 04:00:00","publishedOnDateReadable":"July 18th, 2025"},"versionCreatedAt":"2025-04-07 05:30:45","video":"","vorDoi":"10.1038/s41467-025-61967-9","vorDoiUrl":"https://doi.org/10.1038/s41467-025-61967-9","workflowStages":[]},"version":"v1","identity":"rs-6358279","journalConfig":"researchsquare"},"__N_SSP":true},"page":"/article/[identity]/[[...version]]","query":{"redirect":"/article/rs-6358279","identity":"rs-6358279","version":["v1"]},"buildId":"8U1c8b4HqxoKbykW_rLl7","isFallback":false,"isExperimentalCompile":false,"dynamicIds":[84888],"gssp":true,"scriptLoader":[]}