LiMgPO4:Tb,B - A new sensitive OSL phosphor for dosimetry

Optically Stimulated Luminescence (OSL) technique has emerged as a serious competitor to Thermally Stimulated Luminescence (TSL) technique in various dosimetric applications, especially after the development of crystalline alumina (Al₂O₃:C) doped with carbon. Since then, several attempts are being made to develop other possible materials for OSL based dosimetric applications. Efforts conducted in our laboratory in this direction have led to the development of a new phosphor, Lithium Magnesium Phosphate doped with terbium and boron (LiMgPO₄:Tb,B). This phosphor is prepared by solid-state diffusion method involving conventional air furnaces with operating temperature 1000 °C and easily amenable to large scale production without compromising primary dosimetric advantages. In this work we present some of the dosimetric OSL characteristics of this phosphor. The phosphor exhibits a main TSL peak at 250 °C. The phosphor also emits OSL, when the irradiated phosphor is stimulated with 470 nm light with the OSL sensitivity 1.3 times that of commercially available Al₂O₃:C. Photoluminescence (PL) emission spectrum consists of sharp lines characteristics of Tb³⁺ emission. The OSL discs made out of this phosphor are reusable up to at least 50 cycles, the phosphor exhibits dose linearity up to 1 kGy. Minimum detectable dose is found to be 20 μGy and fading of the OSL signal is found to be about 16% in four days, after which the OSL signal stabilizes.     

The preparation of fine-grain doped graphite and its properties

Fine-grain doped graphite was prepared by the ball-milling dispersion method for the first time. Such composite has not only high thermal conductivity and excellent bending strength (116 MPa), but also better oxidation resistance at elevated temperature and outgassing properties than those of composite doped with normal size carbides. Correlations between microstructure and properties of such composites are also discussed in detail.     

Amorphous phase and anisotropy induced by glancing incident ion beams in Co-Nb films

Co-Nb amorphous films were prepared with the aid of glancing incident ion beams during deposition process. Influence of ion interaction to phase formation and fine microstructure was studied. Amorphous range is about 19 to 63 at.% Co fractions, which is wider than that obtained by perpendicular ion bombardment (28 to 68 at.% of Co fractions). A ripple or a bamboo raft pattern with nano-scale periodicity is observed in the TEM (transmission electron microscopy), SEM (scanning electron microscopy) and AFM (atomic force microscopy) images. The sizes of the image patterns are characterized by correlation length calculated from height-height correlation function (HHCF). The correlation length along the ion incidence is longer than that perpendicular to the ion incidence. Analysis regards that the glancing incident ion beams have high efficiency in both rapid cooling and ion mixing (IM). The main pattern feature in the images mainly comes from surface erosion. Other fine microstructure and the difference among the images result from surface diffusion or viscous flow effect.     

Thermoluminescence properties of nanocrystalline K2Ca2(SO4)3:Eu irradiated with gamma rays and proton beam

Thermoluminescence properties of nanocrystalline K₂Ca₂(SO₄)₃:Eu prepared by ball milling technique have been studied and the nanophosphor’s suitability as an effective gamma radiation and proton beam dosimeter material has been examined. It is found that the nanophosphor is suitable for dosimetry over a very wide range of doses ∼1 Gy to 1 kGy for gamma radiation. And for proton beam the same nanophosphor shows a more or less linear response for the dose range 0.1-100 Gy. A comparative study of this nanophosphor with its corresponding microcrystalline form (prepared by solid-state diffusion method) as well as the nanocrystalline form prepared by (the more conventional) co-precipitation technique has shown that the nanophosphor prepared by the ball milling technique is in almost all respects better than the other two forms reported earlier.     

Deep drawing of tungsten plates for structural divertor applications in future fusion devices

The reference design of a helium cooled divertor for future fusion reactors makes use of hundreds of thousands of finger units consisting of a pressurized structural part called a thimble. Due to the high number of parts needed, the thimble has to be fabricated by mass production techniques like deep drawing. As the thimble is a pressurized part exposed to an internal pressure of 100 bar, the demands for the material are high, which means that it requires the best available tungsten material. Former work has shown that pure tungsten material has the best impact properties and has to be preferred over other commercially available tungsten materials, such as that doped with potassium or strengthened with oxides like lanthanum oxide.Furthermore the inherent weakness of the grain boundaries has to be taken into account, which requires the need for grains that are aligned to the contour of the part (grain boundary alignment).This paper describes the successful deep drawing of a 1 mm tungsten plate in high vacuum at 600 °C. In doing this, a thimble can be machined with grains that follow the contour. Furthermore the characterization of a 1 mm tungsten plate is conducted by tensile tests at room temperature and at 600 °C, as well as by Charpy tests taking into account the anisotropic material behaviour.     

High heat flux testing of 12-14Cr ODS ferritic steels

The thermal performance of Fe-(12-14)Cr-2W-0.3Ti-0.3Y₂O₃ ODS reduced activation ferritic steels, which are considered as candidate first wall materials for the future fusion power reactors and were manufactured by mechanical alloying in hydrogen and hot isostatic pressing, was assessed by high heat flux (HHF) testing with the electron beam JUDITH facility at the Forschungszentrum Jülich (FZJ), Germany. An analysis of the microhardness and microstructure of the specimens was done before and after HHF tests.In general, both materials present a ferritic (α-Fe, bcc) microstructure with a wide range of grain sizes from 100 to 500 nm up to a few micrometers. The coarse grains are almost dislocation-free, while the smaller ones are surrounded by tangles of dislocations. Oxide and carbide impurities (about a few hundreds nm in size) and a high density of Y-Ti-O nano-clusters, with a mean size of about 5 nm, are also present. The microhardness, density and tensile strength of the 14Cr material are slightly larger than those of the 12Cr material.HHF tests revealed that there is no difference in thermal performance, level of degradation and erosion behaviour of 12Cr and 14Cr ODS steels. The onset of melting of the materials occurs for an energy density between 1 and 1.5 MJ/m². Below this value only some kind of thermal etching takes place. This is a significant improvement compared to stainless steel, for which severe plastic deformation at the material surface was observed.     

Synthesis & fabrication of lithium-titanate pebbles for ITER breeding blanket by solid state reaction & spherodization

⁶Li produces tritium by (n, α) nuclear reaction, ⁶Li + ¹n → ⁴He + ³H. Lithium titanate (Li₂TiO₃) enriched with ⁶Li, is the most promising candidate for solid test blanket module (TBM) material for fusion reactors. Various processes are reported in literature for the fabrication of Li₂TiO₃ pebbles for its use as TBM material. A process has been developed based on the solid state reaction of lithium-carbonate and titanium-dioxide for the synthesis of lithium titanate and pebble fabrication by extrusion, spherodization and sintering. This paper discusses the sequence of steps followed in this process and the properties obtained. Analytical grade titanium-dioxide and lithium-carbonate were taken in stoichiometric ratio and were milled to ensure thorough intimate mixing and obtain fine particles less than 45 μm before its calcination at 900 °C. Following calcination, the agglomerated product was again milled to fine particles of size less than 45 μm. Aqueous solution of ploy-vinyl-alcohol was added as binder prior to its feeding in the extruder. The extruded strips were spherodized and spherical pebbles were dried and sintered at 900 °C for different duration. Pebbles of desired density and porosity were obtained by suitable combination of sintering temperature and duration of sintering. Properties of the prepared pebbles were also characterized for sphericity, pore size distribution, grain size, crushing load strength, etc. The values were found to be conforming to the desired properties for use as solid breeder. The attractive feature of this process is almost no waste generation.     

Behavior of crystalline silicon under huge electronic excitations: A transient thermal spike description

Recent experimental works devoted to the phenomena of mixing observed at metallic multilayers Ni/Si irradiated by swift heavy ions irradiations make it necessary to revisit the insensibility of crystalline Si under huge electronic excitations. Knowing that Ni is an insensitive material, such observed mixing would exist only if Si is a sensitive material. In order to extend the study of swift heavy ion effects to semiconductor materials, the experimental results obtained in bulk silicon have been analyzed within the framework of the inelastic thermal spike model. Provided the quenching of a boiling (or vapor) phase is taken as the criterion of amorphization, the calculations with an electron-phonon coupling constant g(300 K) = 1.8 × 10¹² W/cm³/K and an electronic diffusivity D_e(300 K) = 80 cm²/s nicely reproduce the size of observed amorphous tracks as well as the electronic energy loss threshold value for their creation, assuming that they result from the quenching of the appearance of a boiling phase along the ion path. Using these parameters for Si in the case of a Ni/Si multilayer, the mixing observed experimentally can be well simulated by the inelastic thermal spike model extended to multilayers, assuming that this occurs in the molten phase created at the Ni interface by energy transfer from Si.     

Behavior of tungsten with exposure to deuterium plasmas

Four kinds of tungsten (W) materials, i.e. (1) foil of 50 μm thick (f-W), (2) polycrystalline (Pc-W) with grain size of ∼3 μm, (3) recrystallized (Re-W) with grain size of ∼50 μm and (4) vacuum plasma spraying (VPS-W) coatings, were irradiated employing linear plasma generators, with fluxes ?1 × 10²² D/m²/s and energies ?100 eV/D. Scanning electron microscopy (SEM) was used to observe blister formation at the surfaces. The SEM surface morphology and cross section observation indicates that blister formation is related to the microstructure and surface state of different material grades. Results of trapping and deuterium retention measured by thermal desorption spectroscopy (TDS) and nuclear reaction analysis (NRA) show also a close correlation between the retention and the microstructure and surface state.     

High-temperature mechanical properties improvement on modified 9Cr-1Mo martensitic steel through thermomechanical treatments

In the framework of the development of generation IV nuclear reactors and fusion nuclear reactors, materials with an improved high temperature (≅650 °C) mechanical strength are required for specific components. The 9-12%Cr martensitic steels are candidate for these applications. Thermomechanical treatments including normalisation at elevated temperature (1150 °C), followed by warm-rolling in metastable austenitic phase and tempering, have been applied on the commercial Grade 91 martensitic steel in order to refine its microstructure and to improve its precipitation state. The temperature of the warm-rolling was set at 600 °C, and those of the tempering heat-treatment at 650 °C and 700 °C thanks to MatCalc software calculations. Microstructural observations proved that the warm-rolling and the following tempering heat-treatment lead to a finer martensitic microstructure pinned with numerous small carbide and nitride particles. The hardness values of thermomechanically treated Grade 91 steel are higher than those of the as-received Grade 91. It is also shown that the yield stress and the ductility of the thermomechanically treated Grade 91 steel are significantly improved compared to the as-received material. Preliminary creep results showed that these thermomechanical treatments improve the creep lifetime by at least a factor 14.     

Combustion synthesis of 5 and 10 mol% YO1.5 doped ThO2 powders

Nanocrystalline 5 and 10 mol% YO_1.5 doped ThO₂ powders were prepared by the combustion technique using citric acid as a fuel and nitrates as oxidants. The auto-ignition of the fuel-deficient precursors (prepared by thermal dehydration of the aqueous solutions containing metal nitrates and citric acid in required molar ratio) directly resulted in the well crystalline powders of the desired solid solutions along with traces of carbonaceous material. The as-prepared and calcined powders were characterized by X-ray diffraction (XRD), high-temperature XRD and by their sinterability. The YO_1.5 doped ThO₂ powders when cold-pressed and sintered at 1300 °C for 2 h resulted in ?95% of their theoretical densities with nanograin microstructure.     

Development and characterisation of a new ODS ferritic steel for fusion reactor application

This paper describes the microstructure, tensile properties and Charpy impact resistance of a reduced activation oxide dispersion strengthened ferritic steel Fe-14Cr-2W-0.3Ti-0.3Y₂O₃ produced by mechanical alloying of a pre-alloyed, gas atomised steel powder with Y₂O₃ particles, compaction by hot extrusion at 1100 °C, hot rolling at 700 °C and heat treatment at 1050 °C for 1 h. At room temperature the material exhibits a high ultimate tensile strength of about 1420 MPa and high yield strength of about 1340 MPa in the transverse direction. In the longitudinal direction the values are about 10% lower, due to the anisotropy of the microstructure (elongated grains in the rolling direction). At 750 °C the material still exhibits relatively high yield strengths of about 325 MPa and 305 MPa in the longitudinal and transverse directions, respectively. The material exhibits reasonable uniform and total elongation values over the temperature range 23-750 °C, in both transverse and longitudinal directions. The material exhibits weak Charpy impact properties in the transverse direction. Charpy impact properties are slightly better in the longitudinal direction, with upper shelf energy of about 4.2 J and a ductile-to-brittle transition temperature of about 8.8 °C.     

Post irradiation plastic properties of F82H derived from the instrumented tensile tests

F82H (Fe-8Cr-2W) and its variant doped with 2%Ni were irradiated up to 20 dpa at 300 °C in the High Flux Isotope Reactor (HFIR) at Oak Ridge National Laboratory. Post irradiation tensile testing was performed at room temperature. During testing, the images of the specimens including the necked region were continuously recorded. Tests on cold worked material were also carried out for comparison. From the load-displacement curves and the strain distributions obtains from the images, flow stress levels and strain hardening behavior was evaluated. A preliminary constitutive equation for the plastic deformation of irradiated F82H is presented. The results suggest that the irradiation mainly causes defect-induced hardening while it did not strongly affect strain hardening at the same flow stress level for F82H irradiated at 300 °C. The strain hardening of Ni doped specimens was, however, strongly affected by irradiation. Results provide basics to determine allowable stress levels at temperatures below 400 °C.     

Nanoparticles of Al2O3:Cr as a sensitive thermoluminescent material for high exposures of gamma rays irradiations

Aluminum Oxide (Al₂O₃) doped with proper activators is a highly sensitive phosphor commonly used for radiation dosimetry using thermoluminescence (TL) technique. Nanoparticles of this material activated with Chromium (Cr) have been synthesized using the propellant chemical combustion technique and studied for their TL response. They were characterized by X-ray diffraction and scanning electron microscope. The synthesized material has spherical nanoparticles with grain size around 25 nm. These nanoparticles were exposed to heavy doses from γ-rays of ¹³⁷Cs. The TL glow curves show a prominent peak at around 474 K. This peak is found to be sensitive for high exposures of γ-rays and has linear response in the range of 100 Gy-20 kGy without showing saturation. This remarkable result suggests that Al₂O₃:Cr nanoparticles might be used for the dosimetry of food and seed irradiations.     

8 MeV electron irradiation effect on the dielectric and optical properties of iminodiacetic acid doped ferroelectric triglycine sulphate crystals

Single crystal of iminodiacetic acid (5 mol%) doped Tri Glycine Sulphate (IDATGS) was grown by slow evaporation from its aqueous solution at constant temperature, using solution growth method. The dielectric constant (ε′) and pyroelectric current (I_P) were measured over the temperature range of 30-60 °C in the ferroelectric direction. The measured values of ε′ and I_P were found to be smaller compared to pure triglycine sulphate (TGS) crystal parameters. But increased transition temperature was observed for doped crystals. Curie Weiss constants C_P and C_f in the paraelectric and ferroelectric phases were also determined. The doped crystal was irradiated with graded dosages from 5 to 80 kGy of electron beam from 8 MeV Microtron at room temperature and radiation effects on optical and dielectric properties were studied. The UV-Vis absorption spectrum indicates that the UV lower cutoff shifts towards the higher wavelength region (red shift) and the optical band gap is found to be decreasing with the increase of electron dose. It is also observed that the electron irradiation effects in pure and doped TGS were found to be long lasting. The dielectric study shows that there is a gradual reduction in dielectric constant at T_C and shifting of Curie temperature towards lower temperature region with the increase in electron radiation dose. The material figures of merit were found increased after the crystal was irradiated. Induced changes in the physical and optical properties due to irradiation may help one to tailor the device quality and characteristics.     

Effects of 80 KeV proton radiation on the optical properties and microstructure of type-GG17 glass as rubidium lamp envelope

Effect of 80 KeV proton radiation with fluences of 10¹⁴-2 × 10¹⁶ protons/cm² on the optical properties and microstructure of type-GG17 borosilicate glass as a candidate material for rubidium spectra lamp envelope was investigated. The change in microstructure before and after proton radiation was evaluated by means of UV-vis-NIR spectroscopy, X-ray photoelectron spectroscopy (XPS) and positron annihilation lifetime spectrometer (PALS). The experimental results show that under radiation of 80 KeV some broken Si-O bonds were induced and thus the number of non-bridge oxygen (NBO) increased. These irradiation-induced defects caused the degeneration of optical property and loosened glass structure which accelerates rubidium diffusion into lamp envelop.     

Effect of nitrogen flow ratios on the microstructure and properties of (TiVCr)N coatings by reactive magnetic sputtering

The present paper reports the influence of growth conditions on the characteristics of (TiVCr)N coatings prepared by dc reactive magnetron sputtering at various N₂-to-total (N₂ + Ar) flow ratios, R_N. The crystal structures, microstructure, and mechanical, electrical and optical properties under the R_N were characterized. Results indicate that the TiVCr alloy and nitride coatings exhibited a single body-centered cubic type (BCC) and a face-centered cubic (FCC) solid solution structure, respectively. As the R_N increases, the preferred orientation (TiVCr)N coatings changed to (2 0 0). The grain size also had a significant increase. The microstructure of the coatings obviously changed from a porous to a compact and dense columnar structure. Accordingly, the physical properties of the coatings were improved due to the densification of the structure. The hardness of the (TiVCr)N was enhanced to about 15 GPa, and the electrical resistivity was lowered to 10,000 μΩ-cm.     

CHF experiment and CFD analysis in a 2 × 3 rod bundle with mixing vane

In this study, the CHF enhancement using various mixing vanes is evaluated and the flow characteristics are investigated through the CHF experiments and CFD analysis.CHF tests were performed using 2 × 2 and 2 × 3 rod bundles and with R-134a as the working fluid. The test section geometry was identical to that of commercial PWR fuel assembly not including the heated length (1.125 m) and number of fuel rods. From the CHF tests, it was found that the CHF enhancement using mixing vanes under higher mass flux (1400 kg/m² s) and lower pressure (15 bar) conditions is larger than the CHF enhancements under other conditions. Among the mixing vanes used in this study, the swirl vane showed the best performance under relatively low pressure (15 bar) and mass flux (300-1000 kg/m² s) conditions and the hybrid vane performed best near the PWR operating conditions.The detailed flow characteristics were also investigated by CFD analysis using the same conditions as the CHF tests. To calculate the subcooled boiling flow, the wall partitioning model was applied to the wall boundary and various two-phase parameters were also considered. The reliability of the CFD analysis in the boiling analysis was confirmed by comparing the average void fractions of the analysis and the experiments: the results agreed well. From the CFD analysis, the void fraction flattening as a result of the lateral velocity induced by the mixing vane was observed. By the lateral motion of the liquid, the void fraction in the near wall was decreased and that of the core region was increased resulting in the void fraction flattening. The decrease of the void fraction in the near wall region promoted liquid supply to the wall and consequently the CHF increased. For the quantification of the void flatness, an index was developed and the applicability of the index in the CHF assessment was confirmed.     

Xenon-ion-induced and thermal mixing of Co/Si bilayers and their interplay

Studies on ion-irradiated transition-metal/silicon bilayers demonstrate that interface mixing and silicide phase formation depend sensitively on the ion and film parameters, including the structure of the metal/Si interface. Thin Co layers e-gun evaporated to a thickness of 50 nm on Si(1 0 0) wafers were bombarded at room temperature with 400-keV Xe⁺ ions at fluences of up to 3 × 10¹⁶ cm⁻². We used either crystalline or pre-amorphized Si wafers the latter ones prepared by 1.0-keV Ar-ion implantation. The as-deposited or Xe-ion-irradiated samples were then isochronally annealed at temperatures up to 700 °C. Changes of the bilayer structures induced by ion irradiation and/or annealing were investigated with RBS, XRD and HRTEM. The mixing rate for the Co/c-Si couples, Δσ²/Φ = 3.0(4) nm⁴, is higher than the value expected for ballistic mixing and about half the value typical for spike mixing. Mixing of pre-amorphized Si is much weaker relative to crystalline Si wafers, contrary to previous results obtained for Fe/Si bilayers. Annealing of irradiated samples produces very similar interdiffusion and phase formation patterns above 400 °C as in the non-irradiated Co/Si bilayers: the phase evolution follows the sequence Co₂Si → CoSi → CoSi₂.