ࡱ> VXUY )bjbjWW .:==% ]84H,$I2[[[HHHHHHH$VJJL^I[[[[[Ioooo[tH[Hoo FHt ⿬H4Project Achievements The principal achievements of the project concern the demonstration of the fundamental concept of refractive chemi-optical functionality in nanoscopic and nanocomposite media. Such lossless alterations enabled in materials which were designed and synthesised in this project, allowed the implementation of innovative remote sensing schemes by integrated prototype devices. Specific highlights of the project include both innovative materials and methods applied. In the limited time frame, not all proposed materials were possible to be pursued; neither a final optimisation could be achieved. Despite this, the basic principles were proved and some reliable specifications were formulated, which in some cases are comparable to those of well advanced commercial systems. The NANOPHOS results have set the basis for further developments in terms of research and commercialisation. Partners have already started new relevant national initiatives and formed alliances for further exploitation and research actions, evidencing the full success of the project. Novel materials growth and synthesis: Methods and Sensor Media The highlighted achievement in this category is the production of novel nanoscopic materials exhibiting refractive type, lossless, sensing functionalities, thus enabling the implementation of remote type interrogation schemes, at room temperature. Achievements include the new methods produced for this purpose. The operations presented are clearly the state-of-the-art in the field, and open up some new topics for further development. Metal oxide single layer materials Nanoscopic nature and functioning, in perfect agreement with the original hypothesis Pulsed laser deposition and magnetron sputtering Materials growth commenced with a wide range of metal oxides and a selection narrowed the range in order to achieve optimised structures Metal oxide multilayered structures Designed for interferometric optical response implemented by use of sputtering and PLD Thermal processing was used to modify oxide microstructure and composition. Structures grown were of the form of M/MOx/M and used both transition and noble metals for the growth. Trilayer etalon and multilayer structures have been produced and investigated, e.g. Zn/ZnO/Zn, Pt/SnOx/Pt and [Ru/SnOx]n systems. Systems operating inteferometrically and they combined for the first time to achieve a diffractive performance. Inorganic nanocomposites Developed with sol-gel methods ORMOCER developed silica composites comprising CoCl2, NiCl2, and Au nanoclusters. Controlled size nanomaterials were grown in the matrix and produced significant results. Polymer materials functionalised to detect nitroaromatics and also hydrocarbons Studied with respect to their selectivity properties and their optical functionality. Hybrid composites polymers comprising nanomaterials Synthesis of mono-disperse polymers using anionic polymerisation Functional Materials PEO:CoCl2 P2VP PIAA, doped with Au nanoparticles Ultrathin Au island films developed using a simple and robust technology based on evaporation on silanized glass substrates Optical transducers produced for transmission localized surface plasmon resonance (T-LSPR) spectroscopy A new route to Au nanoparticle (NP) functionalization by reversible binding to polymer resins was developed Useful in specialized NP modification, controlled NP release, NP separation and purification, chemical reactions on immobilized NPs, and others. Photonic Interfaces: Fabrication and Interrogation Synthetic materials were found to produce diffractive effects due to their morphology alteration and such scheme used here is a very positive and new result. The development of diffractive interfaces and their use for lossless photonic sensors is another main achievement of the project. m-line grating interrogation device, as well as nonlinear optical sensing were demonstrated for the first time and these represent clear advances in the state-of-the-art. The alteration of grating efficiency was estimated to be minor in some cases, such as for example of nitroaromatics and thus the effort was redirected to the production of waveguide devices. Special interfaces including multilayers, ultrathin metal layers and composites have been demonstrated for the first time and are clearly positive advances. More specifically, the NANOPHOS innovations include: Diffractive optics tailored single layer and multilayer structures. Design and fabrication by lithographic schemes of gratings, complex computer generated and Fresnel type structures. The materials have been interrogated in free space and some first results for the detection of CO have been demonstrated especially using a trilayer structure. Materials processing approaches for the functionalization and interface tailoring of sputter deposited oxides via doping and thermal treatment were developed. Dry etching processes of oxide-based structures to achieve highly anisotropic etch profiles and smooth side-walls were elaborated. Diffractive unprocessed interfaces due to the nanostructure of the material were synthesised. Such effects were altered by the exposure to the chemical environment due to the alteration of the local structure and reversible physicochemical complexation effects. The successful results concerning the production of humidity, ammonia and alcohol sensors led to the integration of respective prototypes. Diffractive interfaces produced by direct femtosecond laser etching on hybrid and sol-gel based composites were found to produce advantageous results and improved performance. Successful results include the detection of alcohols and other analytes. m-line prism coupling and grating coupling sensing methods applied on metal oxide and polymer waveguides have been developed. The original project objectives on HC gas detection (butane, propane) using guided waves were fulfilled. By using various inorganic layers including ZnO, SnOx, etc, refractive index variations as low as 10-6 were detected, and optical detection in the 100 to 1000 ppm range has been demonstrated. Integration led to grating coupler schemes for robustness and efficiency. Transmission localized surface plasmon resonance (T-LSPR) transducers based on Au-island technology were developed. Ultrathin structures were coated using a variety of polymers (polystyrene, polystyrene sulfonate, polyisoprene, poly(2-vinilpyridine) and were tested as sensing layers in T-LSPR transducers. T-LSPR transducers with polymer coatings showed fast (on the scale of tens of seconds) and fully reversible response to various vapors. The use of hybrid layers on the ultrathin structure in order to produce a composite transducer is a further novelty. Successful results include detection of toluene, chloroform, methanol etc as well as the demonstration of certain selectivity of detection. Nonlinear optical sensing, using a range of ultrathin materials in z-scan and Kerr configurations showed promising results for the first time and were in line with the original objectives of the project. This is the first time that such sensing reaction has been demonstrated and opens up new avenues for obtaining high sensing discrimination. Sensor integration Based on the testing results, two types of devices have been integrated and these represent innovative prototypes and further achievements of the project. The main advance here is the noncontact, remote and lossless chemioptical functionality, that enables the realisation of point sensing at room temperature, with zero power supply in the remote sensing head and minor overall power consumption: Free-space remote point sensor The device comprises (a) the sensor head comprising the active sensor medium, a thin film system with suitable interface, and a retro-reflective element which is positioned at a remote point in space and (b) the interrogator system with laser source and detector and (c) data acquisition / logging / storage/ processing system on a portable computer, that is the base station. The device is very versatile as it can be equipped interchangeably with various sensor media. The system comprises a reference arm to alleviate for laser instabilities as well as various controls for efficient detection, noise reduction, turbulence monitoring etc. The operation principles and the actual device have been demonstrated in various versions with (i) three (3) near point enclosed devices, (ii) two (2) remote interrogation prototypes systems. The second system is more advanced in terms of miniaturisation and controls, and further systems are underway for future exploitation. Extensions include a plurality of multiplexed systems and their networking. Specific devices integrated and delivered are: Temperature sensor based on Ru/SnOx multilayer Humidity sensor based PEO/CoCl2 composite layer Ammonia sensor based on TMOS/NiCl2 composite layer Methanol sensor based on P2VP/Au composite layer m-line grating coupler device The device operates on the m-line coupling principle but uses a grating coupler for robustness and miniaturisation. It comprises (a) the lithographically submicron etched active material in order to provide the means for waveguide coupling (b) enclosure for gas insertion (c) diode laser source and optics (d) high resolution CCD to detect the m-line (e) data acquisition and image processing system for detecting variations of the dark line and reference them to the gas analysis. The system is capable of detecting hydrocarbons and specifically tested for butane and propane in the range of 100-1000ppm.     ?@A9 [ \ ^ l n 5 ^ _       w05;OZjkdeXY3v 5B*mH  5B*CJ B*mH nH B*H*B*H*B*mH 5B*5CJ5B*5CJ$R ?@A7 9 ] m n 5 $8$ & F $ & F $ & F$x$ZkefYZr s t u v "":";"$$U&V&&&&&'L'M'N'l'm')))))))))))0 vw1SW+$ & F$ & F $ & F $h$ & F $$ & F #$YZkefYZr s t u v $h$ & F$ "":";"$$U&V&&&&&'L'M'N'l'm'))))) $ & F $ & F$8$h$ & F$ !";"&&&&&&')'N'l')))))))))) jU5B*B*)))))))$8,1h. 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