Validation of a Miniaturized Spectrometer for Trace Detection of Explosives by Surface-Enhanced Raman Spectroscopy

Surface-enhanced Raman spectroscopy (SERS) measurements of some common military explosives were performed with a table-top micro-Raman system integrated with a Serstech R785 miniaturized device, comprising a spectrometer and detector for near-infrared (NIR) laser excitation (785 nm). R785 was tested as the main component of a miniaturized SERS detector, designed for in situ and stand-alone sensing of molecules released at low concentrations, as could happen in the case of traces of explosives found in an illegal bomb factory, where solid microparticles of explosives could be released in the air and then collected on the sensor's surface, if placed near the factory, as a consequence of bomb preparation. SERS spectra were obtained, exciting samples in picogram quantities on specific substrates, starting from standard commercial solutions. The main vibrational features of each substance were clearly identified also in low quantities. The amount of the sampled substance was determined through the analysis of scanning electron microscope images, while the spectral resolution and the detector sensitivity were sufficiently high to clearly distinguish spectra belonging to different samples with an exposure time of 10 s. A principal component analysis procedure was applied to the experimental data to understand which are the main factors affecting spectra variation across different samples. The score plots for the first three principal components show that the examined explosive materials can be clearly classified on the basis of their SERS spectra

LIBS experiments for quantitative detection of retained fuel

Abstract Laser Induced Breakdown Spectroscopy (LIBS) provides chemical information from atomic and ionic plasma emissions generated by laser vaporization of a sample. At the ENEA research center, in collaboration with IPPLM, an equipment has been set up to qualitatively and quantitatively determine the chemical composition of impurities deposited on Plasma Facing Components (PFC). The strength of the LIBS, for its capability of light elements detection, is fully exploited to determine the deuterium content since this element can be considered as the best choice proxy for tritium; the latter being is of great importance in assessing safe conditions to assure the continuous operation in nuclear fusion tokamak. Here we present the results of the Double Pulse LIBS (DP-LIBS) probing of deuterated samples with the simultaneous optical detection by medium-resolution and high-resolution spectrometer. Deuterium emission at 656.1 nm has been detected then the elemental composition has been quantified by applying the Calibration Free (CF) approach. The obtained results demonstrate that the DP-LIBS technique combined with CF analysis is suitable for the quantitative determination of tritium content inside the PFCs of next fusion devices like ITER

Detection by LIBS of the deuterium retained in the FTU toroidal limiter

In this paper the Laser Induced Breakdown Spectroscopy (LIBS) measurement of the deuterium (used as a proxy for tritium) retained in and the surface elemental composition of the FTU Mo (TZM) toroidal limiter tiles, carried out from remote (∼2.5 m) during short breaks of the operations or during machine maintenance, are reported. Single pulse technique has been used with the FTU vessel under high vacuum or in Nitrogen or Argon atmosphere. In vacuum experiments Dα and Hα lines have been detected with good resolution, while in Ar atmosphere (5 × 104 Pa) the two lines were partially overlapped due to Stark broadening. First results of measurements in N2 atmosphere (105 Pa) showed no presence of Dα and Hα lines. These measurements were also carried out for supporting the foreseen use of a robotic arm for an extended LIBS analysis of retained deuterium in the FTU vessel components. Keywords: LIBS, FTU tokamak, Toroidal limiter, Deuterium retentio

Development of On-Line Tritium Monitor Based Upon Artificial Diamond for Fusion Applications

In this paper a novel on-line tritium monitor is presented. It is made with a single crystal diamond detector (SCD) covered with a thin layer of LiF 95% enriched in ⁶Li. Thermal neutrons impinging on the LiF layer produce α and T ions which are detected by the active diamond. The pulse height spectrum shows two separated peaks due to α and T ions respectively. By a proper calibration in a reference thermal flux the number of ⁶Li atoms and thus the absolute n+⁶Li→α+T reaction rate per unitary flux can be established. Once calibrated the detector can be used to measure the tritium production. Due to the many outstanding properties of diamond this detector could operate in the harsh working conditions of a fusion breeding blanket. A test of this detector was performed at the 14 MeV Frascati Neutron Generator (FNG). The detector was inserted inside a mock-up of the European Helium Cooled Lithium Lead (HCLL) Tritium Blanket Module (TBM), designed to validate the neutronic database for fusion application. The mock-up of the TBM was designed to perform a full set of experiments to validate tritium production code prediction comparing the experimental results with calculations. The measured tritium rates with the Li-Diamond detector are described in this paper. Comparison with calculations is in progress and will be reported in a future paper

Thermal and fast neutron detection in chemical vapor deposition single-crystal diamond detectors

Recently, a compact solid-state neutron detector capable of simultaneously detecting thermal and fast neutrons was proposed [M. Marinelli et al., Appl. Phys. Lett. 89, 143509 (2006)]. Its design is based on a p-type/intrinsic/metal layered structure obtained by Microwave Plasma Chemical Vapor Deposition (CVD) of homoepitaxial diamond followed by thermal evaporation of an Al contact and a ⁶LiF converting layer. Fast neutrons are directly detected in the CVD diamond bulk, since they have enough energy to produce the ¹²C(n, α)⁹Be reaction in diamond. Thermal neutrons are instead converted into charged particles in the ⁶LiF layer through the ⁶Li(n, α)T nuclear reaction. These charged particles are then detected in the diamond layer. The thickness of the ⁶LiF converting layer and the CVD diamond sensing layer affect the counting efficiency and energy resolution of the detector both for low- (thermal) and high-energy neutrons. An analysis is carried out on the dynamics of the ⁶Li(n, α)T and the ¹²C(n, α)⁹Be reactions products, and the distribution of the energy released inside the sensitive layer is calculated. The detector counting efficiency and energy resolution were accordingly derived as a function of the thickness of the ⁶LiF and CVD diamond layers, both for thermal and fast neutrons, thus allowing us to choose the optimum detector design for any particular application. Comparison with experimental results is also reported

Analysis of the Response of CVD Diamond Detectors for UV and sX-Ray Plasma Diagnostics Installed at JET

Abstract Diamond detectors are very promising candidates for plasma diagnostics in a harsh environment. In fact, they have several proprieties which make them suitable for magnetic fusion devices: radiation hardness, high thermal conductivity, high resistivity, high carrier mobility and a large bandgap (5.5 eV). The latter makes them insensitive to visible radiation and allows low noise measurements without any cooling. In 2008 two CVD (Chemical Vapour Deposition) single crystal diamond (SCD) detectors were installed at the JET tokamak as extreme UV and soft X-Ray diagnostics [1]. In this work the neutron background in these detectors was measured shielding the UV and soft X-Ray radiation by closing a local vacuum valve. The UV detector was found to be insensitive to the neutron flux, while the soft X Ray detector signal exhibited spikes during the highest neutron rate pulse (neutron rate 10 16 n / s , which corresponds to a flux of φ n ∼10 5 n / cm 2 s in the detector location). These spikes were found to be due to the (n,p) reaction within the plastic filter in front of the soft X-Ray detector. The UV SCD was also used to perform time of flight (ToF) measurements in laser ablation experiments. ToFs were found to be an order of magnitude higher than expected if only the drift velocity is considered. This discrepancy could be due to a delay between the arrival time of the impurities in the plasma and their emission in an energy range which SCD is sensitive to ( Eph >5.5 eV). The delay is found to be comparable with the expected ionization times for edge plasma conditions

Fundamental studies of the adhesion of explosives to textile and non-textile surfaces

This paper describes the use of atomic force microscopy (AFM) to investigate the interactions between explosives crystals and different surfaces. Crystals of TNT, PETN and RDX were mounted onto tipless AFM cantilevers and repeatedly brought into contact with a range of surfaces (n = 15), including textile and non-textile surfaces. The adhesion force during each contact was measured, and the results are presented in this work. The results suggest that explosives crystals display a higher adhesion to smoother, non-textile surfaces, particularly glass. This finding may be of use for forensic explosives investigators when deciding the best types of debris to target for explosives recovery

Characterization of damage induced by heavy neutron irradiation on multilayered 6LiF-single crystal chemical vapor deposition diamond detectors

High performance neutron detectors sensitive to both thermal and fast neutrons are of great interest to monitor the high neutron flux produced, e.g., by fission and fusion reactors. An obvious requirement for such an application is neutron irradiation hardness. This is why diamond based neutron detectors are currently under test in some of these facilities. In this paper the damaging effects induced in chemical vapor deposition (CVD) diamond based detectors by a neutron fluence of ~2 × 10¹⁶ neutrons/cm² have been studied and significant changes in spectroscopic, electrical, and optical properties have been observed. The detectors are fabricated using high quality synthetic CVD single crystal diamond using the p-type/intrinsic/Schottky metal/⁶LiF layered structure recently proposed by Marinelli et al [Appl. Phys. Lett. 89, 143509 (2006)], which allows simultaneous detection of thermal and fast neutrons. Neutron radiation hardness up to at least 2 × 10¹⁴ n/cm² fast (14 MeV) neutron fluence has been confirmed so far [see Pillon et al, Fusion Eng. Des. 82, 1174 (2007)]. However, at the much higher neutron fluence of ~2 × 10¹⁶ neutrons/cm² damage is observed. The detector response to 5.5 MeV ²⁴¹Am α-particles still shows a well resolved α-peak, thus confirming the good radiation hardness of the device but a remarkable degradation and a significant instability with time of charge collection efficiency and energy resolution arise. Symmetric, nearly Ohmic I-V (current-voltage) characteristics have been recorded from the metal/intrinsic/p-doped diamond layered structure, which before neutron irradiation acted as a Schottky barrier diode with a strong rectifying behavior. The nature and the distribution of the radiation induced damage have been deeply examined by means of cathodoluminescence spectroscopy. A more heavily damaged area into the intrinsic diamond at the same position and with the same extension of the ⁶LiF layer has been found, the increased damage being ascribed to the highly ionizing particles produced in the ⁶LiF layer by thermal neutrons through the nuclear reaction ⁶Li(n, α)T

Contact X-ray microscopy of living cells by using LiF crystal as imaging detector

In this paper, the use of lithium fluoride (LiF) as imaging radiation detector to analyse living cells by single-shot soft X-ray contact microscopy is presented. High resolved X-ray images on LiF of cyanobacterium Leptolyngbya VRUC135, two unicellular microalgae of the genus Chlamydomonas and mouse macrophage cells (line RAW 264.7) have been obtained utilizingX-ray radiation in the water window energy range from a laser plasma source. The used method is based on loading of the samples, the cell suspension, in a special holder where they are in close contactwith a LiF crystal solid-state Xray imaging detector. After exposure and sample removal, the images stored in LiF by the softX-ray contactmicroscopy technique are read by an optical microscope in fluorescence mode. The clear image of the mucilaginous sheath the structure of the filamentous Leptolyngbya and the visible nucleolus in the macrophage cells image, are noteworthiness results. The peculiarities of the used X-ray radiation and of the LiF imaging detector allow obtaining images in absorption contrast revealing the internal structures of the investigated samples at high spatial resolution. Moreover, thewidedynamicrangeof theLiF imaging detector contributes to obtain high-quality images. In particular, we demonstrate that this peculiar characteristic of LiF detector allows enhancing the contrast and reveal details even when they were obscured by a nonuniform stray light

Dosimetric characterization of a microDiamond detector in clinical scanned carbon ion beams

Purpose: To investigate for the first time the dosimetric properties of a new commercial synthetic diamond detector (PTW microDiamond) in high-energy scanned clinical carbon ion beams generated by a synchrotron at the CNAO facility. Methods: The detector response was evaluated in a water phantom with actively scanned carbon ion beams ranging from 115 to 380 MeV/u (30-250 mm Bragg peak depth in water). Homogeneous square fields of 3×3 and 6×6 cm2 were used. Short- and medium-term (2 months) detector response stability, dependence on beam energy as well as ion type (carbon ions and protons), linearity with dose, and directional and dose-rate dependence were investigated. The depth dose curve of a 280 MeV/u carbon ion beam, scanned over a 3×3 cm² area, was measured with the microDiamond detector and compared to that measured using a PTW Advanced Markus ionization chamber, and also simulated using FLUKA Monte Carlo code. The detector response in two spread-out-Bragg-peaks (SOBPs), respectively, centered at 9 and 21 cm depths in water and calculated using the treatment planning system (TPS) used at CNAO, was measured. Results: A negligible drift of detector sensitivity within the experimental session was seen, indicating that no detector preirradiation was needed. Short-term response reproducibility around 1% (1 standard deviation) was found. Only 2% maximum variation of microDiamond sensitivity was observed among all the evaluated proton and carbon ion beam energies. The detector response showed a good linear behavior. Detector sensitivity was found to be dose-rate independent, with a variation below 1.3% in the evaluated dose-rate range. A very good agreement between measured and simulated Bragg curves with both microDiamond and Advanced Markus chamber was found, showing a negligible LET dependence of the tested detector. A depth dose curve was also measured by positioning the microDiamond with its main axis oriented orthogonally to the beam direction. A strong distortion in Bragg peak measurement was observed, confirming manufacturer recommendation on avoiding such configuration. Very good results were obtained for SOBP measurements, with a difference below 1% between measured and TPS-calculated doses. The stability of detector sensitivity in the observation period was within the experimental uncertainty. Conclusions: Dosimetric characterization of a PTW microDiamond detector in high-energy scanned carbon ion beams was performed. The results of the present study showed that this detector is suitable for dosimetry of clinical carbon ion beams, with a negligible LET and dose-rate dependence