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Liquid Phase Studies of Nanomaterials
摘要： Liquid cell transmission electron microscopy (LCTEM) is a relatively new technique enabling researchers to study dynamic phenomena in materials sciences, life sciences and electrochemistry. LCTEM has proved to be a remarkable tool for observing colloidal nanoparticle syntheses at fairly high temporal and spatial resolutions offered by transmission electron microscopy (TEM). Though the idea of observing syntheses in their native media is not new, a practical approach has only been made possible through massive improvements in microfabrication technology to fabricate liquid cells.[1] The idea is to use thin window materials such as SiN membranes (50 nm or less) to encapsulate tens of cubic nanometers of liquid in a stable thin profile suitable forTEM imaging considering the vacuum environment of the microscope (Fig. 1).
关键词： Radiolysis,Nanoparticles,Electron beam irradiation,Solvent,Liquid cell TEM
更新于2025-09-23 15:21:21
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Controlled synthesis of gold nanoparticles in copolymers nano-molds by x-ray radiolysis
摘要： We show by x-ray and neutron small angle scattering that gold nanoparticles with controlled sizes and morphologies can be obtained by the metallic reduction of AuCl4- ions trapped in 3D organic molds by x-ray radiolysis. The molds are spherical frozen micelles of polystyrene‐b‐poly(dimethylaminoethyl methacrylate) (PS‐b‐PDMAEMA) block copolymer in acidic aqueous solution with a PS spherical core surrounded by a corona of PDMAEMA chains in good solvent. The behavior of micelles is controlled by the [AuCl4-]/[DMAEMA] ratio RAuCl4-/DMAEMA. At low gold concentration, AuCl4- ions condense on the positively charged DMAEMA moieties without changing the behavior of the PDMAEMA chains. At intermediate gold concentration, the ions induce a progressive contraction of the corona’s chains and dehydration of micelles. At large gold concentration, the corona becomes a fully dry phase loaded with gold ions, which induces micelle aggregation. The radiolysis of the solution by an intense x-ray beam produces different types of gold nanoparticles with respect to RAuCl4-/DMAEMA and irradiation time. At RAuCl4-/DMAEMA = 0.033, the irradiation produces in a first step gold clusters in the micelle corona which in a second step merge to form nanoparticles of a similar size to the one of the micelle. Conversely, at RAuCl4-/DMAEMA = 0.33, micelles do not operate as templates but only as nucleation zones and large nanoparticles grow outside the micelles.
关键词： gold nanoparticles,copolymers template,x-ray radiolysis,small angle scattering,synthesis
更新于2025-09-23 15:21:01
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Tests under irradiation of optical fibers and cables devoted to corium monitoring in case of severe accident in a Nuclear Power Plant
摘要： The DISCOMS project, which stands for “DIstributed Sensing for COrium Monitoring and Safety”, considers the potential of distributed sensing technologies, based on remote instrumentations and Optical Fiber Sensing cables embedded into the concrete floor under the reactor vessel, to monitor the status of this third barrier of confinement. This paper focuses on the selection and testing of singlemode (SM) optical fibers with limited RIA (Radiation Induced Attenuation) to be compliant with remote distributed instruments optical budgets, the ionizing radiation doses to sustain, and their reduction provided by the concrete basemat shielding. The tests aimed at exposing these fibers and the corresponding sensitive optical cables, to the irradiation doses expected during the normal operation of the reactor (up to 60 years for the European Pressurized Reactor), followed by a severe accident. Several gamma and mixed (neutron-gamma) irradiations were performed at CEA Saclay facilities: POSé?DON irradiator and ISIS reactor, up to a gamma cumulated dose of about 2 MGy and fast neutron fluence (E > 1 MeV) of 6 x 1015 n/cm2. The first gamma test permitted to assess the RIA at various optical wavelengths, and to select three radiation tolerant singlemode fibers (RIA < 5 dB/100 m, at 1550 nm operating wavelength). The second one was performed on voluminous strands of sensitive cables encapsulating selected optical fibers, up to approximately the same accumulated dose, at two temperatures: 30°C and 80°C. A significant increase of the RIA, without any saturation tendency, appeared for fibers inserted into cables, correlated with the increase of the hydroxyl attenuation peak at 1380 nm. Molecular hydrogen generated by the radiolysis of compounds of the cable is at the origin of this phenomenon. A third gamma irradiation run permitted to measure the radiolytic hydrogen production yield of some compounds of a dedicated temperature cable sample. The efficiency of a carbon coating layer over the silica cladding, acting as a barrier against hydrogen diffusion, was also successfully confirmed. Finally, the efficiency of this carbon coating layer has also been tested under neutron irradiation, then qualified as a protection barrier against hydrogen diffusion in the optical fiber cores.
关键词： carbon coating layer,radiation effects,optical fibers,hydrogen diffusion,gamma,radiolysis,rad-hard optical fiber,neutron,distributed measurement
更新于2025-09-23 15:21:01