Structural characterization of buried nitride layers formed by nitrogen ion implantation in silicon

The synthesis of buried silicon nitride insulating layers was carried out by SIMNI (separation by implanted nitrogen) process using implantation of 140 keV nitrogen (¹⁴N⁺) ions at fluence of 1.0 × 10¹⁷, 2.5 × 10¹⁷ and 5.0 × 10¹⁷ cm⁻² into 〈1 1 1〉 single crystal silicon substrates held at elevated temperature (410 °C). The structures of ion-beam synthesized buried silicon nitride layers were studied by X-ray diffraction (XRD) technique. The XRD studies reveal the formation of hexagonal silicon nitride (Si₃N₄) structure at all fluences. The concentration of the silicon nitride phase was found to be dependent on the ion fluence. The intensity and full width at half maximum (FWHM) of XRD peak were found to increase with increase in ion fluence. The Raman spectra for samples implanted with different ion fluences show crystalline silicon (c-Si) substrate peak at wavenumber 520 cm⁻¹. The intensity of the silicon peak was found to decrease with increase in ion fluence.     

Defect characterization in boron implanted silicon after flash annealing

Flash-assisted rapid thermal processing (fRTP) has gained considerable interests for fabrication of ultra-shallow junction in silicon. fRTP can significantly reduce boron diffusion, while attaining boron activation at levels beyond the limits of traditional rapid thermal annealing. The efficiency of fRTP for defect annealing, however, needs to be systematically explored. In this study, a (1 0 0) silicon wafer was implanted with 500 eV boron ions to a fluence of 1 × 10¹⁵ cm⁻². fRTP was performed with peak temperatures ranging from 1100 °C to 1300 °C for approximately one milli-second. High resolution transmission electron microscopy and secondary ion mass spectrometry were performed to characterize as-implanted and annealed samples. The study shows that fRTP at 1250 °C can effectively anneal defects without causing boron tail diffusion.     

Dense plasma focus ion-based titanium nitride coating on titanium

We report the synthesis of titanium nitride coating on a titanium substrate by utilizing energetic nitrogen ions emitted from a 2.3 kJ dense plasma focus device for 30 focus shots. The number of nitrogen ions transferred to the sample by a single ion pulse of about 140 ns duration in the energy interval (40-600 keV) is about 1.09 × 10¹² with a mean energy per ion of 58 keV. The corresponding energy flux delivered to the titanium surface is estimated to be 6.17 × 10¹⁴ keV cm⁻³ ns⁻¹ leading to a transient temperature rise of the top layer of about 5400 K which helps layer growth. The coating is investigated on the basis of its morphological, compositional and hardness properties. X-ray diffraction analysis of the sample reveals the formation of a nanocrystalline titanium nitride coating having (1 1 1) and (2 0 0) plane reflections with an average crystallite size of 40 nm. The compressive residual stresses in the nitride coating have been evaluated to be 2.80 GPa and 6.81 GPa corresponding to (1 1 1) and (2 0 0) plane orientations. A complete restructuring of the manually polished titanium substrate has been observed with appearance of nano-sized multidimensional granular surface morphologies. The thickness of the nitride coating is about 1 μm, whereas the coating has a nitrogen content of 35.35 at.% and 13.78 ± 3.57 wt.% and a surface hardness of 8.19 GPa.     

Swift heavy ion induced phase transition in CdTe films deposited by spray pyrolysis in presence of electric field

CdTe polycrystalline thin films possessing hexagonal phase regions are obtained by spray deposition in presence of a high electric field. Thin film samples are irradiated with 100 MeV Ag ions using Pelletron accelerator to study the swift heavy ion induced effects. The ion irradiation results in the transformation of the metastable hexagonal regions in the films to stable cubic phase due to the dense electronic excitations induced by beam irradiation. The phase transformation is seen from the X-ray diffraction patterns. The band gap of the CdTe film changes marginally due to ion irradiation induced phase transformation. The value changes from 1.47 eV for the as deposited sample to 1.44 eV for the sample irradiated at the fluence 1×10¹³ ions/cm². The AFM images show a gradual change in the shape of the particles from rod shape to nearly spherical ones after irradiation.     

M2N nitride phases of 9% chromium steels for nuclear applications

M₂N nitride phases of 9% chromium steels with an extra-low carbon content have been investigated using a transmission electron microscope and an energy-dispersive X-ray (EDX) spectroscopy. The steel samples were normalized for 1 h at 1050 °C and then tempered at 600-780 °C for 30 min to 5 h followed by an air cooling. Through the analyses of the electron micro-diffraction patterns and EDX data for the precipitate particles on the extracted carbon replica, two types of Cr-rich M₂N nitride phases with the same hexagonal structure but totally different lattice parameters, a = 2.80 Å/c = 4.45 Å and a = 7.76 Å/c = 4.438 Å, were determined in the steels. Four types of Cr-rich M₂N phases with different lattice parameters probably existed in the steels. The M₂N phase revealed a decrease in its Cr content, an increase in its V content as the tempering temperature was increased, and no obvious change in its content for the metal fraction with an increasing tempering time.     

Investigations on the effect of 100 MeV Ni ions irradiated chloride vapour phase epitaxy (Cl-VPE) grown GaN epilayers

Gallium nitride (GaN) epilayers have been grown by chloride vapour phase epitaxy (Cl-VPE) technique and the grown GaN layers were irradiated with 100 MeV Ni ions at the fluences of 5 × 10¹² and 2 × 10¹³ ions/cm². The pristine and 100 MeV Ni ions irradiated GaN samples were characterized using X-ray diffraction (XRD), UV-visible transmittance spectrum, photoluminescence (PL) and atomic force microscopy (AFM) analysis. XRD results indicate the presence of gallium oxide phases after Ni ion irradiation, increase in the FWHM and decrease in the intensity of the GaN (0 0 0 2) peak with increasing ion fluences. The UV-visible transmittance spectrum and PL measurements show decrease in the band gap value after irradiation. AFM images show the nanocluster formation upon irradiation and the roughness value of GaN increases with increasing ion fluences.     

Deuterium retention of boron-titanium and reduction of deuterium retention after helium ion irradiations

Deuterium ion irradiations with an ion with energy of 1.7 keV were conducted for boron-titanium (B-Ti) film prepared by electron beam evaporation and hot pressed titanium-boride, TiB₂. The amount of retained deuterium was measured for these materials using a technique of thermal desorption spectroscopy. The amount of deuterium retained in TiB₂ was comparable with that in B-Ti. Desorption peaks of deuterium in B-Ti were 470 K and 620 K, corresponding to a desorption in the low temperature regime observed in boron (B) and a desorption in titanium (Ti), respectively. The desorption peaks in TiB₂ were 620 K and 750 K, which correspond to the desorption in Ti and that in the high temperature regime in B, respectively. The desorption temperature in B-Ti was approximately 100 K lower than that in TiB₂. This difference is discussed based upon chemical bindings and amorphous/crystal structures of B-Ti and TiB₂. Irradiation of helium ion with energy of 5 keV was conducted for B-Ti after the deuterium ion irradiation. The amount of retained deuterium decreased and the desorption temperature shifted to the lower temperature regime, as the helium ion fluence increased. The shift to the low temperature regime is due to the enhancement of amorphous structure of B in B-Ti.     

Synthesis of dysprosium and cerium nitrides by a mechanically induced gas-solid reaction

A high energy ball milling process was used to produce dysprosium nitride and cerium nitride powders at room temperature. Dysprosium and cerium metal flakes were milled in a 275 kPa nitrogen atmosphere for 24 h at ambient temperatures. X-ray diffraction confirmed the formation of phase pure dysprosium nitride and cerium nitride powders. The median particle size of the resultant dysprosium nitride was measured as 4 μm using a laser scattering technique. The particle size of the cerium nitride was not measured due to its reactive nature.     

Formation of dislocation loops in silicon by ion irradiation for silicon light emitting diodes

We have studied the influence of the ion species, ion energy, fluence, irradiation temperature and post-implantation annealing on the formation of shallow dislocation loops in silicon, for fabrication of silicon light emitting diodes. The substrates used were (1 0 0) Si, implanted with 20-80 keV boron at room temperature and 75-175 keV silicon at 100 and 200 °C. The implanted fluences were from 5 × 10¹⁴ to 1 × 10¹⁵ ions/cm². After irradiation the samples were processed for 15 s to 20 min at 950 °C by rapid thermal annealing. Structural analysis of the samples was done by transmission electron microscopy and Rutherford backscattering spectrometry. In all irradiations the silicon substrates were not amorphized, and that resulted in the formation of extrinsic perfect and faulted dislocation loops with Burgers vectors a/2〈1 1 0〉 and a/3〈1 1 1〉, respectively, sitting in {1 1 1} habit planes. It was demonstrated that by varying the ion implantation parameters and post-irradiation annealing, it is possible to form various shapes, concentration and distribution of dislocation loops in silicon.     

Design of a fuel element for a lead-cooled fast reactor

The options of a lead-cooled fast reactor (LFR) of the fourth generation (GEN-IV) reactor with the electric power of 600 MW are investigated in the ELSY Project. The fuel selection, design and optimization are important steps of the project. Three types of fuel are considered as candidates: highly enriched Pu-U mixed oxide (MOX) fuel for the first core, the MOX containing between 2.5% and 5.0% of the minor actinides (MA) for next core and Pu-U-MA nitride fuel as an advanced option. Reference fuel rods with claddings made of T91 ferrite-martensitic steel and two alternative fuel assembly designs (one uses a closed hexagonal wrapper and the other is an open square variant without wrapper) have been assessed. This study focuses on the core variant with the closed hexagonal fuel assemblies. Based on the neutronic parameters provided by Monte-Carlo modeling with MCNP5 and ALEPH codes, simulations have been carried out to assess the long-term thermal-mechanical behaviour of the hottest fuel rods. A modified version of the fuel performance code FEMAXI-SCK-1, adapted for fast neutron spectrum, new fuels, cladding materials and coolant, was utilized for these calculations. The obtained results show that the fuel rods can withstand more than four effective full power years under the normal operation conditions without pellet-cladding mechanical interaction (PCMI). In a variant with solid fuel pellets, a mild PCMI can appear during the fifth year, however, it remains at an acceptable level up to the end of operation when the peak fuel pellet burnup ∼80 MW d kg⁻¹ of heavy metal (HM) and the maximum clad damage of about 82 displacements per atom (dpa) are reached. Annular pellets permit to delay PCMI for about 1 year. Based on the results of this simulation, further steps are envisioned for the optimization of the fuel rod design, aiming at achieving the fuel burnup of 100 MW d kg⁻¹ of HM.     

Investigation on boron carbide oxidation for nuclear reactor safety: Experiments in highly oxidising conditions

The oxidation kinetics of boron carbide pellets were investigated in steam/argon mixtures in the temperature range 1200-1800 °C for steam partial pressures between 0.2 and 0.8 bar and total flows (steam + argon) between 2.5 and 10 g/min resulting in gas velocities from 1.01 to 5.34 m/s. A kinetic model for boron carbide pellet oxidation depending on temperature, steam partial pressure and flow velocity is obtained. The activation energy of the oxidation process was determined to be 163 ± 8 kJ/mol. The strong influence of temperature and steam partial pressure on the boron carbide oxidation kinetics is confirmed. The obtained data suggest the coexistence of two kinetic regimes, one at 1200 °C and the other at 1400-1800 °C, with different dependence on steam partial pressure.     

Ion beam modification of metals

Energetic ions beams may be used in various ways to modify and so improve the tribological properties of metals. These methods include: — ion implantation of selected additive species; — ion beam mixing of thin deposited coatings; — ion-beam-assisted deposition of thicker overlay coatings.

The first of these techniques has been widely used to modify the electronic properties of semiconductors, but has since been extended for the treatment of all classes of material. Tool steels can be strengthened by the ion implantation of nitrogen or titanium, to produce fine dispersions of hard second-phase precipitates. Solid solution strengthening, by combinations of substitutional and interstitial species, such as yttrium and nitrogen, has also been successful. Both ion beam mixing (IBM) and ion-beam-assisted deposition (IBAD) use a combination of coating and ion bombardment. In the first case, the objective is to intermix the coating and substrate by the aid of radiation-enhanced diffusion. In the latter case, the coating is densified and modified during deposition and the process can be continued in order to build up overlay coatings several μm in thickness. The surface can then be tailored, for instance to provide a hard and adherent ceramic such as silicon nitride, boron nitride or titanium nitride. It is an advantage that all the above processes can be applied at relatively low temperatures, below about 200° C, thereby avoiding distortion of precision components. Ion implantation is also being successfully applied for the reduction of corrosion, especially at high temperatures or in the atmosphere and to explore the mechanisms of oxidation. Ion-assisted coatings, being compact and adherent, provide a more substantial protection against corrosion: silicon nitride and boron nitride are potentially useful in this respect. Examples will be given of the successful application of these methods for the surface modification of metals and alloys, and developments in the equipment now available for industrial application of ion beams will also be reviewed.     

Annular gas ionization detector for low energy heavy ion backscattering spectrometry

A gas ionization chamber for use in backscattering spectrometry has been built. It has the shape of a hollow cylinder and can be placed in-line with the incident ion beam. The entrance window for detected particles is composed of a circular array of silicon nitride membranes. A low noise preamplifier with cooled FET is used for charge amplification. The detector resolution has been measured for a variety of ions in the mass range from He to Si and for energies between 0.5 and 8 MeV. The energy resolution of the ionization chamber surpasses the one of a state-of-the-art silicon charged particle detector for all ions heavier than Li. For Si ions the improvement in resolution is more than a factor of 2. The device does not suffer from any radiation damage. For He particles around 1 MeV the resolution is between 13 and 16 keV (FWHM). Therefore the new detector is not only well suited for heavy ion backscattering spectrometry but can also be applied for standard He RBS, allowing the use of a single detector for all types of projectiles in a wide energy range.     

Caesium isothermal migration behaviour in sintered titanium nitride: New data and comparison with previous results on iodine and xenon

Titanium nitride has been proposed as a fission product barrier in fuel structures for gas cooled fast reactor (GFR) systems. The thermal migration of Cs was studied by implanting 800 keV ¹³³Cs⁺⁺ ions into sintered samples of TiN at an ion fluence of 5 × 10¹⁵ cm⁻². Thermal treatments at temperatures ranging from 1500 to 1650 °C were performed under a secondary vacuum. Concentration profiles were determined by 2.5 MeV ⁴He⁺ elastic backscattering. The results reveal that the global mobility of caesium in the host matrix is low compared to xenon and iodine implanted in the same conditions. Nevertheless, the evolution of caesium depth profile during thermal treatment presents similarities with that of xenon. Both species are homogeneously transported towards the surface and the transport rate increases with the temperature. In comparison, iodine exhibits singular migration behaviour. Several assumptions are proposed to explain the better retention of caesium in comparison with both other species. The potential role played by the oxidation is underlined since even a slight modification of the surface stoichiometry may modify species mobility. More generally, the apparition of square-like shapes on the surface of the samples after implantations and thermal treatments is discussed.     

Progress of in-air microbeam system at the Wakasa Wan Energy Research Center

Modifications of an in-air microbeam system at the Wakasa Wan Energy Research Center designed to improve its performance are described. In the previous setup, a silicon nitride membrane (area: 1 × 1 mm²; thickness: 100 nm) was used for the beam exit window and the distance between the window and the sample was restricted to ?1.7 mm. Due to this restriction, the beam spot size obtained using the previous setup was 13 × 13 μm². To reduce the beam spot size, the beam exit window was replaced by a silicon nitride membrane (area: 3 (horizontal) × 2 (vertical) mm²; thickness: 200 nm). In this setup, the sample can be moved as close as 0.7 mm to the window, enabling a beam spot size of 7 × 6 μm² to be achieved. An additional Si-PIN X-ray detector was installed to estimate the relative number of beam particles. It detects X-rays from the beam exit window. The number of the X-rays from the beam exit window (which is proportional to the number of beam particles) is used for quantitative analysis and for online monitoring of the beam current. This system has the potential to be used for simultaneous particle-induced X-ray emission (PIXE) and particle-induced gamma-ray emission (PIGE) measurements and for studying dental medicine.     

Equilibrium charge state distributions for boron and carbon ions emerging from carbon and aluminum targets

Equilibrium charge state distributions of boron and carbon ions through carbon and aluminum targets were measured with an energy range of 3-6 MeV. Comparisons of the data with relevant semi-empirical models for the equilibrium mean charge states and for the charge state distribution widths could provide valuable insight on the underlying mechanisms for a fast ion to lose or capture electrons. In-depth examinations of the experimental results in combination with semi-empirical models suggest that equilibrium charge state distributions are well represented by Gaussian distributions.     

Analysis and design of the Alfven wave antenna system for the SUNIST spherical tokamak

Analysis and design of the Alfven wave antenna system for the SUNIST spherical tokamak are presented. Two candidate antenna concepts, folded and unfolded, are analyzed and compared with each other. In the frequency range of Alfven resonance the impedance spectrums of both two concept antennas for major modes are numerically calculated in a 1-D MHD framework. The folded concept is chosen for engineering design. The antenna system is designed to be simple and requires least modification to the vacuum vessel. The definition of the antenna shape is guided by the analyses with constraints of existing hardware layouts. Each antenna unit consists of two stainless steel straps with a thickness of 1 mm. A number of boron nitride tiles are assembled together as the side limiters for plasma shielding. Estimation shows that the structure is robust enough to withstand the electromagnetic force and the heat load for typical discharge duty cycles.     

Comparison of the effects of cadmium-shielded and boron carbide-shielded irradiation channel of the Ghana Research Reactor-1

The MCNP model for the Ghana Research Reactor-1 (GHARR-1) was redesigned to incorporate cadmium-shielded irradiation channel as well as boron carbide-shielded channel in one of the outer irradiation channels. Further investigations were made after initial work in the cadmium-shielded channel to consider the boron carbide-shielded channel and both results were compared to determine the best material for the shielded channel. Before arriving at the final design of only one shielded outer irradiation channel extensive investigations were made into several other possible designs; as all the other designs that were considered did not give desirable results of neutronic performance. The concept of redesigning a new MCNP model which has a shielded channel is to equip GHARR-1 with the means of performing efficient epithermal neutron activation analysis. The use of epithermal neutron activation analysis can be very useful in many experiments and projects (e.g. it can be used to determine uranium and thorium in sediment samples). After the simulation, a comparison of the results from the boron carbide-shielded channel model for the GHARR-1 and the epicadmium-shielded channel was made. The inner irradiation channels of the two designs recorded peak values of approximately 1.18 × 10¹² ± 0.0036 n/cm² s, 1.32 × 10¹² ± 0.0036 n/cm² s and 2.71 × 10¹¹ ± 0.0071 n/cm² s for the thermal, epithermal and fast neutron flux, respectively. Likewise the outer irradiation channels of the two designs recorded peak values of approximately 7.36 × 10¹¹ ± 0.0042 n/cm² s, 2.53 × 10¹¹ ± 0.0074 n/cm² s and 4.73 × 10¹⁰ ± 0.0162 n/cm² s for the thermal, epithermal and fast neutron flux, respectively. The epicadmium design recorded a peak thermal flux of 7.08 × 10¹¹ ± 0.0033 n/cm² s and an epithermal flux of 2.09 × 10¹¹ ± 0.006 n/cm² s in the irradiation channel where the shield was installed. Also, the boron carbide design recorded no peak thermal flux but an epithermal flux of 1.18 × 10¹¹ ± 0.0079 n/cm² s in the irradiation channel where the shield was installed. The final multiplication factor (k_eff) of the boron carbide-shielded channel model for the GHARR-1 was recorded as 1.00282 ± 0.0007 while that of the epicadmium designed model was recorded as 1.00332 ± 0.0007. Also, a final prompt neutron lifetime of 1.5237 × 10⁻⁴ ± 0.0008 s was recorded for the cadmium designed model while a value of 1.5245 × 10⁻⁴ ± 0.0008 s was recorded for the boron carbide-shielded design of the GHARR-1.     

Deuterium retention in sintered boron carbide exposed to a deuterium plasma

Depth profiles of deuterium up to a depth of 10 μm have been measured using the D(³He,p)⁴He nuclear reaction in a resonance-like technique after exposure of sintered boron carbide, B₄C, at elevated temperatures to a low energy (≈200 eV/D) and high ion flux (≈10²¹ m⁻² s⁻¹) D plasma. The proton yield was measured as a function of incident ³He energy and the D depth profile was obtained by deconvolution of the measured proton yields using the program SIMNRA. D atoms diffuse into the bulk at temperatures above 553 K, and accumulate up to a maximum concentration of about 0.2 at.%. At high fluences (?10²⁴ D/m²), the accumulation in the bulk plays a major role in the D retention. With increasing exposure temperature, the amount of D retained in B₄C increases and exceeds a value of 2 × 10²¹ D/m² at 923 K. The deuterium diffusivity in the sintered boron carbide is estimated to be D = 2.6 × 10⁻⁶exp{−(107 ± 10) kJ mol⁻¹/RT} m² s⁻¹.     

TEM investigations of MN nitride phases in a 9% chromium ferritic/martensitic steel with normalization conditions for nuclear reactors

The investigations on the precipitate phases in a 9%Cr ferritic/martensitic steel under different normalization conditions have been made by using a transmission electron microscope and an energy-dispersive X-ray spectroscopy. Hot-rolled steel samples were normalized at 1050-1200 °C for 1-2 h followed by an air cooling to room temperature. MN vanadium nitride precipitates with a plate-like morphology and a chemical formula of about (V_0.4Nb_0.4Cr_0.2)N have been observed at triple junctions, grain boundaries and within matrix in the steel samples normalized at 1050-1150 °C for 1-2 h, but they were dissolved out at 1200 °C within 1 h. Vanadium nitride is a stable phase at 1050 °C according to thermocalc prediction of equilibrium phases in the steel. With increasing normalizing temperature and time, there was no a striking change in the chemical composition of metallic elements in the MN phase, but a considerable increase in the size of the MN precipitate.