Localized Surface Plasmon Resonance Response Research Articles

Localized surface plasmon resonances of size-selected large silver nanoclusters (n = 70-100) soft-landed on a C60 organic substrate.

Silver nanoclusters (Agn NCs) exhibit a remarkable optical property known as localized surface plasmon resonance (LSPR) in the visible to ultraviolet wavelengths. In this study, we address the size gap in LSPR responses between small NCs and nano-islands by synthesizing large Agn NCs with a countable number of atoms (n = 70-100) using a magnetron sputtering method, which were precisely size-selected and soft-landed onto substrates. The monodispersed Agn NCs were immobilized on a pre-decorated substrate with fullerene (C60) molecules, and their LSPR behaviors were characterized using two-photon photoemission (2PPE) spectroscopy. Due to the distinct polarization selectivity of incident light associated with LSPR, the intensity ratio between p- and s-polarized lights (Ip/Is) in 2PPE spectroscopy serves as a reliable indicator of LSPR and its structural correlations. From n = 70 to 100, the Ip/Is value gradually decreases as the cluster size increases. This decrease is attributed to the enhancement of s-polarized light (Is), indicating that large Agn NCs on a C60 substrate undergo a deformation from spherical to flattened geometries, particularly above approximately n = 55.

Enhancing the Extinction Efficiency and Plasmonic Response of Bimetallic Nanoparticles of Au-Ag in Robust Thin Film Sensing Platforms

The extinction efficiency of noble metal nanoparticles (NPs), namely gold (Au) and silver (Ag), are dependent on their size and surrounding dielectric. Exploiting the Localized Surface Plasmon Resonance (LSPR) phenomenon, the composition and structure of the NPs might be tailored to achieve a configuration that optimizes their response (sensitivity) to environmental changes. This can be done by preparing a bimetallic system, benefiting from the chemical stability of Au NPs and the higher scattering efficiency of Ag NPs. To enhance the LSPR sensing robustness, incorporating solid supports in the form of nanocomposite thin films is a suitable alternative. In this context, the NPs composed of gold (Au), silver (Ag), and their mixture in bimetallic Au-Ag NPs, were grown in a titanium dioxide (TiO2) matrix using reactive DC magnetron sputtering. Thermal treatment at different temperatures (up to 700 °C) tuned the LSPR response of the films and, consequently, their sensitivity. Notably, the bimetallic film with Au/Ag atomic ratio 1 exhibited the highest refractive index sensitivity (RIS), with a value of 181 nm/RIU, almost one order of magnitude higher than monometallic Au-TiO2. The nanostructural analysis revealed a wide NP size distribution of bimetallic NPs with an average size of 31 nm, covering about 20% of the overall surface area. These findings underscore the significant potential of bimetallic film systems, namely AuAg-TiO2, in LSPR sensing enhancement.

Investigation of LSPR Coupling Effects toward the Rational Design of CsxWO3–δ Based Solar NIR Filtering Coatings

AbstractThe optical range of localized surface plasmon resonance (LSPR) is extended into the infrared region, thanks to the development of highly doped semiconductor nanocrystals. Particularly, the near‐infrared (NIR) range holds a significant interest in managing solar radiation. However, practical applications necessitate the arrangement of particles, which is known to possibly impact their optical properties through LSPR coupling effects. How such coupling modifies the LSPR response in semiconductor hosts remains largely unexplored. In this study, a protocol for producing composite coatings composed of cesium‐doped tungsten bronze nanocrystals embedded in a silica matrix is presented. Achieving individual dispersion of nanocrystals is made possible through careful selection of a surface polyglycerol ligand exchange. This allows to tune the interparticle distance by adjusting the nanocrystal volume fraction in the composite. The findings demonstrate that LSPR coupling effects significantly influence the LSPR intensity of nanocrystals in the composite when the nanocrystal‐to‐nanocrystal distance matches their size. Beyond elucidating the LSPR coupling effect, this study provides insights into the potential use of Cs‐HTB nanocrystals for solar control applications. Through the optimization of morphology and film structure, remarkable selectivity is obtained in terms of maintaining good transparency in the visible range while achieving high absorption in the NIR.

Rational Synthesis of Au-CdS Composite Photocatalysts for Broad-Spectrum Photocatalytic Hydrogen Evolution.

Incorporation of plasmonic metal nanomaterials can significantly enhance the visible light response of semiconductor photocatalysts via localized surface plasmon resonance (LSPR) mechanisms. However, the surfaces of plasmonic metal nanomaterials are often covered with surfactant molecules, which is undesired when the nanomaterials are used for photocatalytic hydrogen evolution, since surfactant molecules could significantly compromise the nanomaterials' cocatalyst functionalities by blocking the active sites and/or by inhibiting the surface charge transfer process. Herein, we demonstrate a method that assembles Au nanoparticles (NPs) into Au colloidosomes (AuCSs) without modifying their surfaces with surfactants. The resulting AuCSs were then coupled with CdS for the formation of Au-CdS composite photocatalysts through an in situ deposition method. The assembly of Au NPs induced a broader and stronger LSPR response for AuCSs, while the absence of surfactants allowed them to act efficiently as cocatalysts. This essentially enhanced the electron-hole pair generation rate and further their utilization efficiency, leading to an extremely high hydrogen evolution rate of 235.8 mmol·g-1·h-1 under simulated sunlight excitation.

Enhanced Light Scattering Using a Two-Dimensional Quasicrystal-Decorated 3D-Printed Nature-Inspired Bio-photonic Architecture

A number of strategies have been exploited so far to trap photons inside living cells to obtain high-contrast imaging. Also, launching light inside biological materials is technically challenging. Using photon confinement in a three-dimensional (3D)-printed biomimetic architecture in the presence of a localized surface plasmon resonance (LSPR) promoter can overcome some of these issues. This work compares optical confinement in natural and 3D-printed photonic architectures, namely, fish scale, in the presence of atomically thin Al70Co10Fe5Ni10Cu5 quasicrystals (QCs). Due to their wideband LSPR response, the QCs work as photon scattering hotspots. The architecture acts as an additive source of excitation for the two-dimensional (2D) QCs via total internal reflection (TIR). The computational analysis describes the surface plasmon-based scattering property of 2D QCs. The 3D-printed fish scale’s image contrast with the 2D Al70Co10Fe5Ni10Cu5 QC has been compared with other 2D materials (graphene, h-BN, and MoS2) and outperforms them. The present study conceptually presents a new approach for obtaining high-quality imaging of biological imaging, even using high-energy photons.

Fully Aqueous Self-Assembly of a Gold-Nanoparticle-Based Pathogen Sensor.

Surface plasmon resonance (SPR) is a very sensitive measure of biomolecular interactions but is generally too expensive for routine analysis of clinical samples. Here we demonstrate the simplified formation of virus-detecting gold nanoparticle (AuNP) assemblies on glass using only aqueous buffers at room temperature. The AuNP assembled on silanized glass and displayed a distinctive absorbance peak due to the localized SPR (LSPR) response of the AuNPs. Next, assembly of a protein engineering scaffold was followed using LSPR and a sensitive neutron reflectometry approach, which measured the formation and structure of the biological layer on the spherical AuNP. Finally, the assembly and function of an artificial flu sensor layer consisting of an in vitro-selected single-chain antibody (scFv)-membrane protein fusion was followed using the LSPR response of AuNPs within glass capillaries. In vitro selection avoids the need for separate animal-derived antibodies and allows for the rapid production of low-cost sensor proteins. This work demonstrates a simple approach to forming oriented arrays of protein sensors on nanostructured surfaces that uses (i) an easily assembled AuNP silane layer, (ii) self-assembly of an oriented protein layer on AuNPs, and (iii) simple highly specific artificial receptor proteins.

Novel Glycolipid Chips with a Double Layer of Au Nanoparticles for Biological Toxin Detection.

Glycolipid chips having a double layer of Au nanoparticles are proposed for detection of biological toxins. The sugar-modified chips constitute an under and an upper layer of Au nanoparticles of 20-80 nm diameter on glass plates, and Au nanoparticles of each layer are linked with 1,8-octanedithiol by a self-assembled monolayer (SAM) technique. A tris-sialo glycosphingolipid, ganglioside GT1b, having lipoic amide at the sphingosine part was immobilized on the Au outside surface of the upper layer, and botulinum toxin (type A heavy chain) was detected by localized surface plasmon resonance (LSPR). The GT1b-Cer-coated chip having a double layer of Au nanoparticles enhanced the toxin detection by LSPR more than those with single monolayers. The LSPR response changed according to the sizes of Au nanoparticles in each under and upper layer. The combination of 60 and 40 nm Au nanoparticles in the under and upper layer, respectively, gave the best result, which enabled the toxin detection at concentrations below 5 ng/mL with the portable LSPR device.

Ag@Pt等离激元复合纳米结构中热电子级联传输增 强电催化反应

A popular strategy for constructing localized surface plasmon resonance (LSPR)-enhanced plasmonic metal heterostructure catalysts is to fabricate a composite of highly active materials with plasmonic metal nanomaterials. However, this kind of combination not only decreases the LSPR response intensity but also changes the hot electron transport pathway inside the heterogeneous structure, which induces the ineffective transfer of plasmonic hot electrons to the surface of the heterostructures and hinders the effective enhancement of catalytic activity. Herein, simple Ag@Pt bimetallic nanocubes are selected to explore the mechanism of hot electrons from excitation and transmission within a plasmonic metal het-erostructure and their contribution to the electrochemical hydrogen evolution reaction (HER). The corresponding experimental and theoretical results confirm that the hot electrons (holes) become a dominant plasmon decay pathway owing to the introduction of thin Pt shells and HER can be significantly enhanced by hot electrons via a cascaded manner, i.e., first being excited in Ag, then pumped from Ag atoms to Pt atoms and accumulated on the surface of Pt. This work provides an important reference for the design and application of plasmonic metal heterostructure catalysts.

Amplification-Free, High-Throughput Nanoplasmonic Quantification of Circulating MicroRNAs in Unprocessed Plasma Microsamples for Earlier Pancreatic Cancer Detection.

Pancreatic ductal adenocarcinoma (PDAC) is a deadly malignancy that is often detected at an advanced stage. Earlier diagnosis of PDAC is key to reducing mortality. Circulating biomarkers such as microRNAs are gaining interest, but existing technologies require large sample volumes, amplification steps, extensive biofluid processing, lack sensitivity, and are low-throughput. Here, we present an advanced nanoplasmonic sensor for the highly sensitive, amplification-free detection and quantification of microRNAs (microRNA-10b, microRNA-let7a) from unprocessed plasma microsamples. The sensor construct utilizes uniquely designed -ssDNA receptors attached to gold triangular nanoprisms, which display unique localized surface plasmon resonance (LSPR) properties, in a multiwell plate format. The formation of -ssDNA/microRNA duplex controls the nanostructure-biomolecule interfacial electronic interactions to promote the charge transfer/exciton delocalization processes and enhance the LSPR responses to achieve attomolar (10-18 M) limit of detection (LOD) in human plasma. This improve LOD allows the fabrication of a high-throughput assay in a 384-well plate format. The performance of nanoplasmonic sensors for microRNA detection was further assessed by comparing with the qRT-PCR assay of 15 PDAC patient plasma samples that shows a positive correlation between these two assays with the Pearson correlation coefficient value >0.86. Evaluation of >170 clinical samples reveals that oncogenic microRNA-10b and tumor suppressor microRNA-let7a levels can individually differentiate PDAC from chronic pancreatitis and normal controls with >94% sensitivity and >94% specificity at a 95% confidence interval (CI). Furthermore, combining both oncogenic and tumor suppressor microRNA levels significantly improves differentiation of PDAC stages I and II versus III and IV with >91% and 87% sensitivity and specificity, respectively, in comparison to the sensitivity and specificity values for individual microRNAs. Moreover, we show that the level of microRNAs varies substantially in pre- and post-surgery PDAC patients (n = 75). Taken together, this ultrasensitive nanoplasmonic sensor with excellent sensitivity and specificity is capable of assaying multiple biomarkers simultaneously and may facilitate early detection of PDAC to improve patient care.

Point-of-Care Biosensing of Urinary Tract Infections Employing Optoplasmonic Surfaces Embedded with Metal Nanotwins.

We report the synthesis of gold nanotwins (Au NTs) on a solid and transparent glass substrate which in turn has been employed for the selective optoplasmonic detection of Escherichia coli (EC) bacteria in human urine for the point-of-care diagnosis of urinary tract infections (UTIs). As compared to the single nanoparticle systems (Au NPs), the Au NTs show an enriched localized surface plasmon resonance (LSPR) due to the enhancement of the electric field under electromagnetic irradiation, e.g., photon, which helps in improving the limits of detection. For this purpose, initially a simple glass surface has been coated with Au NPs, with the help of the linker 3-aminopropyl-triethoxysilane - APTES. The surface has been linked further with another Au NP with the help of the 1,10-alkane-dithiol linker with two thiol ends, which eventually leads to the development of the optoplasmonic surface with Au NTs and an enhanced LSPR response. Subsequently, the EC specific aptamer has been chemically immobilized on the surface of Au NTs with the blocking of free sites via bovine serum albumin (BSA). Remarkably, Raman spectroscopy unfolds a 7-fold increase in the peak intensities with the Au NTs on the glass surface as compared to the surface coated with isolated Au NPs. The enhancement in the LSPR response of glass substrates coated with Au NTs and the EC specific aptamer has been further utilized for the selective and sensitive detection of UTIs. The results have been verified with the help of UV-visible spectroscopy to establish the utility of the proposed sensing methodology. An extensive interference study with other bacterial species unveils the selectivity and specificity of the proposed optoplasmonic sensors toward EC with a detection range of 5 × 103 to 107 CFU/mL. Intuitively, the method is more versatile in a sense that the sensor can be made specific to any other pathogens by simply changing the design of the aptamer. Finally, a low-cost, portable, and point-of-care optoplasmonic transduction setup is designed with a laser light illumination source, a sample holder, and a sensitive photodetector for the detection of UTIs in human urine.

SERS and EC-SERS detection of local anesthetic procaine using Pd loaded highly reduced graphene oxide nanocomposite substrate

The localized surface plasmon resonance (LSPR) excitations are critical towards achieving sizable spectral enhancements of the Raman scattered light. Herein, the synthesis of palladium-based highly reduced graphene oxide (Pd-HRG) with LSPR properties as an effective surface-enhanced Raman scattering (SERS) substrate and its utility in the highly sensitive detection of procaine are reported. The concentration detection of procaine samples was optimized by applying a set of pre-concentration parameters. The Pd-HRG nanocomposite showed a remarkable LSPR response with a Raman enhancement factor of 8.7 × 102. The Pd-HRG is employed to modify fluorine doped tin oxide electrode (Pd-HRG/FTO), resulted with an enhancement factor of 7.5 × 104 corresponding to the EC-SERS technique. The electronic and surface properties of synthesized Pd-HRG and functionalized FTO electrode were evaluated using Raman, infrared, EIS, XRD, FESEM and EDX techniques. Quantum chemical calculations were carried out to elaborate on the nature of interaction of procaine molecules with a nanostructured surface model. Pd-HRG, with an efficient and cost-effective fabrication, can be considered as a promising EC-SERS substrate for the detection of organic therapeutic drugs.

Plasmon Tuning of Liquid Gallium Nanoparticles through Surface Anodization.

In this work, tunable plasmonic liquid gallium nanoparticles (Ga NPs) were prepared through surface anodizing of the particles. Shape deformation of the Ga NPs accompanied with dimpled surface topographies could be induced during electrochemical anodization, and the formation of the anodic oxide shell helps maintain the resulting change in the particle shape. The nanoscale dimple-like textures led to changes in the localized surface plasmon resonance (LSPR) wavelength. A maximal LSPR red-shift of ~77 nm was preliminarily achieved using an anodization voltage of 0.7 V. The experimental results showed that an increase in the oxide shell thickness yielded a negligible difference in the observed LSPR, and finite-difference time-domain (FDTD) simulations also suggested that the LSPR tunability was primarily determined by the shape of the deformed particles. The extent of particle deformation could be adjusted in a very short period of anodization time (~7 s), which offers an efficient way to tune the LSPR response of Ga NPs.

Phase-Controlled Synthesis and Quasi-Static Dielectric Resonances in Silver Iron Sulfide (AgFeS2 ) Nanocrystals.

Ternary metal-chalcogenide semiconductor nanocrystals are an attractive class of materials due to their tunable optoelectronic properties that result from a wide range of compositional flexibility and structural diversity. Here, the phase-controlled synthesis of colloidal silver iron sulfide (AgFeS2 ) nanocrystals is reported and their resonant light-matter interactions are investigated. The product composition can be shifted selectively from tetragonal to orthorhombic by simply adjusting the coordinating ligand concentration, while keeping the other reaction parameters unchanged. The results show that excess ligands impact precursor reactivity, and consequently the nanocrystal growth rate, thus deterministically dictating the resulting crystal structure. Moreover, it is demonstrated that the strong ultraviolet-visible extinction peak exhibited by AgFeS2 nanocrystals is a consequence of a quasi-static dielectric resonance (DR), analogous to the optical response observed in CuFeS2 nanocrystals. Spectroscopic studies and computational calculations confirm that a negative permittivity at ultraviolet/visible frequencies arises due to the electronic structure of these intermediate-band (IB) semiconductor nanocrystals, resulting in a DR consisting of resonant valence-band-to-intermediate-band excitations, as opposed to the well-known localized surface plasmon resonance response typically observed in metallic nanostructures. Overall, these results expand the current library of an underexplored class of IB semiconductors with unique optical properties, and also enrich the understanding of DRs in ternary metal-iron-sulfide nanomaterials.

Temperature-Sensitive Localized Surface Plasmon Resonance of α-NiS Nanoparticles.

The presented work shows a synthesis route to obtain nanoparticles of the hexagonal α-NiS phase and core–shell particles where the same material is grown onto previously prepared Au seeds. In the bulk, this nickel sulfide phase is known to exhibit a metal–insulator type phase transition (MIT) at 265 K which drastically alters its electrical conductivity. Since the produced nanoparticles show a localized surface plasmon resonance (LSPR) in the visible range of the electromagnetic spectrum, the development of their optical properties depending on the temperature is investigated. This is the first time an LSPR of colloidal nanoparticles is monitored regarding such a transition. The results of UV–vis absorbance measurements show that the LSPR of the particles can be strongly and reversibly tuned by varying the temperature. It can be switched off by cooling the nanoparticles and switched on again by reheating them above the transition temperature. Additional to the phase transition, the temperature-dependent magnetic susceptibility of α-NiS and Au-NiS nanoparticles suggests the presence of different amounts of uncompensated magnetic moments in these compounds that possibly affect the optical properties and may cause the observed quantitative differences in the LSPR response of these materials.

Photoswitchable Machine-Engineered Plasmonic Nanosystem with High Optical Response for Ultrasensitive Detection of microRNAs and Proteins Adaptively

Modulating optoelectronic properties of inorganic nanostructures tethered with light-responsive molecular switches by their conformational change in the solid state is fundamentally important for advanced nanoscale-device fabrication, specifically in biosensing applications. Herein, we present an entirely new solid-state design approach employing the light-induced reversible conformational change of spiropyran (SP)-merocyanine (MC) covalently attached to gold triangular nanoprisms (Au TNPs) via alkylthiolate self-assembled monolayers to produce a large localized surface plasmon resonance response (∼24 nm). This shift is consistent with the increase in thickness of the local dielectric shell-surrounded TNPs and perhaps short-range dipole-dipole (permanent and induced) interactions between TNPs and the zwitterionic MC form. Water contact angle measurement and Raman spectroscopy characterization unequivocally prove the formation of a stable TNP-MC structural motif. Utilizing this form, we fabricated the first adaptable nanoplasmonic biosensor, which uses an identical structural motif for ultrasensitive, highly specific, and programmable detection of microRNAs and proteins at attomolar concentrations in standard human plasma and urine samples, and at femtomolar concentrations from bladder cancer patient plasma (n = 10) and urine (n = 10), respectively. Most importantly, the TNP-MC structural motif displays a strong binding affinity with receptor molecules (i.e., single-stranded DNA and antibody) producing a highly stable biosensor. Taken together, the TNP-MC structural motif represents a multifunctional super biosensor with the potential to expand clinical diagnostics through simplifying biosensor design and providing highly accurate disease diagnosis.

Localized SPR for Pb(II) ion sensing utilizing chitosan/reduced graphene oxide nanocomposite

In this work, a simple and highly sensitive localized surface plasmon resonance (LSPR) technique had been developed for detection of Pb(II) utilizing chitosan/reduced graphene oxide (CS/rGO) nanocomposite as the sensing material. Gold nanoparticles (AuNP) had been incorporated with the nanocomposite material to induce strong LSPR responses. CS/rGO nanocomposite was coated on top of AuNP and had been utilized as active layer for Pb(II) ion sensing. The morphology and physical properties of gold nanoparticle-chitosan/reduced graphene oxide (AuNP-CS/rGO) nanocomposite was studied using field-emission scanning electron microscopy (FESEM), atomic force microscopy (AFM) and x-ray diffraction (XRD) analysis. FESEM exhibits a rough and wrinkle surface of AuNP-CS/rGO after the addition of rGO. AFM shows a higher surface roughness for AuNP-CS/rGO due to the presence of oxygen atoms in rGO where these oxygen atoms provide more sites for adsorption of Pb(II), hence enhance the sensitivity of the sensor. A good sensitivity of the LSPR sensor for detection of Pb(II) utilizing AuNP-CS/rGO was obtained which is 1.544 ppm-1 and the linearity of the sensor are 0.99 and 0.97. In stability study, AuNP-CS/rGO exhibits a good repeatability with relative standard deviation of 2% for 0.01 ppm.

Light-Activated Chemoresistive and Plasmonic-Resonant Optical Sensors for NO2 and H2 Sensing Based on ZnO Doped Nanoparticles

Light-Activated Chemoresistive and Plasmonic-Resonant Optical Sensors for NO2 and H2 Sensing Based on ZnO Doped Nanoparticles

In Situ Imaging of Cellular Reactive Oxygen Species and Caspase-3 Activity Using a Multifunctional Theranostic Probe for Cancer Diagnosis and Therapy.

In this work, a multifunctional theranostic nanoprobe (Au-Ag-HM) was skillfully designed for simultaneous imaging of intracellular reactive oxygen species (ROS) and caspase-3 activity. The Au-Ag-HM was fabricated by coloading of silver nanoparticles (AgNPs) and hematoporphyrin monomethyl ether (HMME) to Au nanoflowers (AuNFs). When Au-Ag-HM was devoured by cancer cells, HepG2 cells were used as the model, and under laser irradiation, the photogenerated intracellular ROS by the photosensitizer HMME would induce the apoptosis of cancer cells. Meanwhile, the intracellular ROS triggered the oxidative etching of AgNPs on Au-Ag-HM, which led to a tremendous localized surface plasmon resonance response and scattering color changes in Au-Ag-HM, allowing in situ dark-field imaging of the ROS level in cancer cells. On the other hand, the ROS-induced activation of cellular caspase-3, which cleaved the C-peptide-containing caspase-3-specific recognition sequence (DEVD) and allowed HMME to release from the nanoprobe, resulted in a significant fluorescence recovery related to caspase-3 activity. Both photogenerated ROS and enhanced caspase-3 activity contributed to the synergistic effect of laser-mediated chemotherapy and photodynamic therapy. Therefore, the as-prepared theranostic probe could be used for simultaneous detection of cellular ROS and caspase-3 activity, distinguishing between tumor cells and normal cells, inducing the apoptosis of cancer cells, and providing a new method for diagnosis and therapy of cancer.

Controlling mid-infrared plasmons in graphene nanostructures through post-fabrication chemical doping

Engineering the doping level in graphene nanostructures to yield controlled and intense localized surface plasmon resonance (LSPR) is fundamental for their practical use in applications such as molecular sensing for point of care or environmental monitoring. In this work, we experimentally study how chemical doping of graphene nanostructures using ethylene amines affects their mid-infrared plasmonic response following the induced change in electrical transport properties. Combining post-fabrication silanization and amine doping allows to prepare the surface to support a strong LSPR response at zero bias. These findings pave the way to design highly doped graphene LSPR surfaces for infrared sensors operating in real environments.

Real-time synthesis and detection of plasmonic metal (Au, Ag) nanoparticles under monochromatic X-ray nano-tomography

Plasmonic nanostructures are of immense interest of research due to its widespread applications in microelectronics, photonics, and biotechnology, because of its size and shape-dependent localized surface plasmon resonance response. The great efforts have been constructed by physicists, chemists, and material scientists to deliver optimized reaction protocol to tailor the size and shape of nanostructures. Real-time characterization emerges out as a versatile tool in perspective to the optimization of synthesis parameters. Moreover, in the past decades, radiation-induced reduction of metallic-salt to nanoparticles dominates over the conventional direct chemical reduction process which overcomes the production of secondary products and yields ultra-high quality and pure nanostructures. Here we show, the real-time/in-situ synthesis and detection of plasmonic (Au andAg) nanoparticles using single synchrotron monochromatic 6.7 keV X-rays based Nano-Tomography beamline. The real-time X-ray nano-tomography of plasmonic nanostructures has been first-time successfully achieved at such a low-energy that would be leading to the possibility of these experiments at laboratory-based sources. In-situ optical imaging confirms the radiolysis of water molecule resulting in the production of e_{aq}^-,,OH^bullet , and O_2^- under X-ray irradiation. The obtained particle-size and size-distribution by X-ray tomography are in good agreement to TEM results. The effect of different chemical environment media on the particle-size has also been studied. This work provides the protocol to precisely control the size of nanostructures and to synthesize the ultrahigh-purity grade monodisperse nanoparticles that would definitely enhance the phase-contrast in cancer bio-imaging and plasmonic photovoltaic application.