High Temperature Annealing Conditions Research Articles

Sensitivity analysis of cesium and strontium release from TRISO particle under irradiation and high temperature conditions

This paper presents a systematic sensitivity analysis of the diffusivity parameters of cesium and strontium inside Tristructural isotropic (TRISO) fuel particle and their dependence on irradiation and high temperature annealing conditions. The BISON fuel performance code was used to model the base irradiation and the high temperature tests performed within the AGR-1 experiment. The sensitivity analysis results quantified the contributions of the various diffusion parameters to BISON predictions of Cs and Sr release from compacts exposed to a number of different irradiation and thermal conditions. Informed by the Sobol indices, a calibration study provided an optimized set of diffusion parameters that improved the accuracy of BISON predictions. Finally, we describe an analysis of the influence of irradiation and thermal conditions on the Cs and Sr release and characterize their dependence on the testing conditions. The systematic approach in this study allows us to better understand the transport mechanism of Cs and Sr inside TRISO particle, and to identify a number of future needs to fully resolve the discrepancy between BISON predictions of Cs and Sr release with the AGR-1 experimental observations.

Effective band gap engineering in multi-principal oxides (CeGdLa-Zr/Hf)Ox by temperature-induced oxygen vacancies

Oxygen vacancy control has been one of the most efficient methods to tune the physicochemical properties of conventional oxide materials. A new conceptual multi-principal oxide (MPO) is still lacking a control approach to introduce oxygen vacancies for tuning its inherent properties. Taking multi-principal rare earth-transition metal (CeGdLa-Zr/Hf) oxides as model systems, here we report temperature induced oxygen vacancy generation (OVG) phenomenon in MPOs. It is found that the OVG is strongly dependent on the composition of the MPOs showing different degrees of oxygen loss in (CeGdLaZr)Ox and (CeGdLaHf)Ox under identical high temperature annealing conditions. The results revealed that (CeGdLaZr)Ox remained stable single phase with a marginal decrease in the band gap of about 0.08 eV, whereas (CeGdLaHf)Ox contained two phases with similar crystal structure but different oxygen vacancy concentrations causing semiconductor-to-metal like transition. Due to the intrinsic high entropy, the metallic atoms sublattice in (CeGdLaHf)Ox remains rather stable, regardless of the interstitial oxygen atoms ranging from almost fully occupied (61.84 at%) to almost fully empty (8.73 at%) state in the respective crystal phases. Such highly tunable oxygen vacancies in (CeGdLa-Zr/Hf) oxides show a possible path for band gap engineering in MPOs for the development of efficient photocatalysts.

A combined rate theory-population balance model of the evolution of irradiation-induced helium bubbles in metals during annealing

A multiscale model describing the evolution of helium bubbles in the irradiated materials is established based on the rate equations and the population balance equation. The size distribution of the helium bubbles and the evolution law of the statistical average size and number density of the bubbles with time changing predicted by the model are in good agreement with the experimental statistics. The influence of annealing temperature, annealing time, irradiation energy, irradiation flux, and coarsening mechanisms on the evolution of helium bubbles are numerically simulated and discussed, taking FeCrAl alloy as the irradiated material. The results show that the bubble evolution is dominated by the Ostwald ripening mechanism under high temperature annealing conditions (≥ 1073 K), and the time dependence of the average size and density of helium bubbles is consistent with the existing theoretical results. And the number of shrinking helium bubbles caused by Ostwald ripening is effectively reduced by the bubble coalescence effect, leading to further growth of the proportion of large-sized helium bubbles. Consequently, a Gaussian bubble size distribution has been obtained modeling the coupling of the Ostwald ripening mechanism and the bubble coalescence mechanism. The generation rates of helium and vacancy in the material during irradiation, as well as their ratio, are significant factors that can affect the nucleation and evolution of helium bubbles.

Crystallization of SrAl12O19 Nanocrystals from Amorphous Submicrometer Particles.

Advanced instrumentation and modern analysis tools such as transmission electron microscopy (TEM) have led to phenomenal progress in understanding crystallization, in particular from solution, which is a prerequisite for the design-based preparation of a target crystal. Nevertheless, little has been understood about the crystallization pathway under high-temperature annealing (HTA) conditions. Metal oxide crystals are prominent materials that are usually obtained via HTA. Despite the widespread application of hydro-/solvothermal methods on the laboratory scale, HTA is the preferred method in many industries for the mass production of metal oxide crystals. However, poor control over the morphology and grain sizes of these crystals under extreme HTA conditions limits their applications. Here, applying ex-situ TEM, the transformation of a single amorphous spherical submicrometer precursor particle of SrAl12O19 (SA6) at 1150 °C toward a nanosized thermodynamically favored hexagonal crystal is explored. It is illustrated in real space, step by step, how both kinetic and thermodynamic factors contribute to this faceting and morphology evolution. These results demonstrate a nonclassical nucleation and growth process consisting of densification, crystallite domain formation, oriented attachment, surface nucleation, 2-dimensional (2D) growth, and surface diffusion of the atoms to eventually result in the formation of a hexagonal platelet crystal. The TEM images further delineate a parent crystal driving the crystal lattice and morphological orientation of a network of interconnected platelets.

Towards understanding the influence of Mg content on phase transformations in the La3-xMgxNi9 alloys by in-situ neutron powder diffraction study

The present work is focused on the studies of the phase-structural transformations in the La3-xMgxNi9 (x ​= ​1.0, 1.1 and 1.2) alloys as active materials of negative electrodes in the Nickel-Metal Hydride (Ni/MH) batteries. The phase equilibria and phase-structural transformations in the alloys were probed by in situ neutron powder diffraction (NPD) at the temperatures ranging from 300 ​K to 1273 ​K using the measurements of the equilibrated alloys at 8 setpoint temperatures of 300, 973, 1073, 1123, 1173, 1223, 1248 and 1273 ​K.Prepared by induction melting initial alloys were found to be multi-phase structured, containing up to 6 individual intermetallic compounds with different stoichiometric compositions. With the increase of the temperature and holding time, various transformations took place in the studied alloys. These included the formations and transformations of super-stacking intermetallics with variable ratios (La ​+ ​Mg)/Ni, 1:3, 2:7 and 5:19.With increasing temperatures, several systematic changes took place. (a) Abundances of (La,Mg)2Ni4 AB2 and (La,Mg)Ni3 AB3 type intermetallics gradually decreased before they melted/decomposed above 1073 ​K; (b) The (La,Mg)2Ni7 A2B7 type intermetallics began to decrease in abundances above 1123 ​K; (c) The transformation in the (La,Mg)5Ni19 intermetallics from 3R to 2H proceeded above 1223 ​K.The increase of Mg content had no obvious influence on (La,Mg)2Ni4 and (La,Mg)2Ni7 phases, and corresponding reactions R1 and R3 took place at the same temperatures as in the La–Ni system. However, with increasing Mg content the melting point of (La,Mg)5Ni19 phase increased while the melting point of the (La,Mg)Ni3 phase it decreased, leading to the variation of the reaction temperatures of the corresponding processes.The present study will assist in optimizing phase-structural composition of the alloys in the La–Mg–Ni system which contain Mg-modified layered structures by tailoring the high temperature annealing conditions.

Thermal stability of epitaxial α-Ga2O3 and (Al,Ga)2O3 layers on m-plane sapphire

Here, we have explored the thermal stability of α-(Al,Ga)2O3 grown by the molecular-beam epitaxy on m-plane sapphire under high-temperature annealing conditions for various Al compositions (i.e., 0%, 46%, and 100%). Though uncapped α-Ga2O3 undergoes a structural phase transition to the thermodynamically stable β-phase at high temperatures, we find that an aluminum oxide cap grown by atomic layer deposition preserves the α-phase. Unlike uncapped α-Ga2O3, uncapped α-(Al,Ga)2O3 at 46% and 100% Al content remain stable at high temperatures. We quantify the evolution of the structural properties of α-Ga2O3, α-(Al,Ga)2O3, and α-Al2O3 and the energy bandgap of α-Ga2O3 up to 900 °C. Throughout the anneals, the α-Ga2O3 capped with aluminum oxide retains its high crystal quality, with no substantial roughening.

Total ionization dose effects of N-type tunnel field effect transistor (TFET) with ultra-shallow pocket junction

N-type tunnel field effect transistors (TFETs) with Si1−xGex/Si hetero-junction in the ultra-shallow N+ pocket region have been fabricated. This paper investigates the total ionization dose (TID) effects on the electrical characteristics of these N-type TFET devices, including transfer and output characteristics, via a 60Co γ-ray irradiation source. TID has little impact on the on-state current for TFETs with and without P well. With the increase in total dose, however, a shift in the transfer characteristics, such as the off-state current and subthreshold slope is observed. Under the same TID condition, TFETs with P well exhibit more robustness as compared to TFETs without P well. The characteristics under room temperature and high temperature annealing conditions after irradiation are also investigated. The underlying mechanisms, such as the interplay among bulk trapped charge in gate oxide-induced inversion and interface trap-induced trap-assisted-tunneling, are identified by TCAD simulation and are discussed in detail.

Flexible Bandpass Filter Fabricated on Polyimide Substrate by Surface Modification and In Situ Self-Metallization Technique.

Polymer, especially polyimide (PI), is the best suitable substrate material for the design of flexible electronics. The compact silver can be reduced on the surface of PI films by surface modification and in situ self-metallization technique. The formed silver layers have good electrical and mechanical flexibility. A flexible bandpass filter on a PI flexible substrate by surface modification and in situ self-metallization technique at room temperature are presented in this work. Measured results show that the proposed flexible bandpass filter could achieve a fractional bandwidth of 80.8% with an insertion loss (IL) of less than 0.6 dB. The performance of the designed filter is almost constant under different bending, folding, and rolling conditions. The formed silver layers also present good adhesion with PI substrates. This technology provides an alternative approach for manufacturing flexible filters without high-temperature thermal annealing, costly equipment, and vacuum conditions.

Comparative study of n-GaN transition group refractory metal Ohmic electrode

Ohmic contact is directly related to the performance of GaN device and is one of the important factors affecting device performance. In recent years, many research groups have studied the electrode materials and annealing conditions of n-type GaN Ohmic contacts. In this paper, the ohmic contact properties and structural characteristics of the Hf/Al electrode of a transition group metal refractory metal Hf system under different annealing conditions are studied, and compared with those of the Ti-based ohmic contact Ti/Al electrode. The specific contact resistivity of each electrode is measured by a dot-type transmission line model, and the structural characteristics of the electrode are analyzed by using an Auger electron spectrometer which can be analyzed in depth. The results show that the Hf/Al electrode under the same annealing condition exhibits superior ohmic contact performance compared with the conventional Ti/Al electrode. At the same time, the lowest specific contact resistivity of the Hf/Al electrode annealed in an N<sub>2</sub> atmosphere at a low temperature of 650 ℃ for 60 s is 4.28×10<sup>–5</sup> Ω·cm<sup>2</sup>. The in-depth analysis of Auger electron spectrum shows that the Hf/Al electrode has a solid phase reaction with the n-type GaN material. In addition, the cross section of each electrode is observed by auger electron spectroscopy. In the Hf/Al electrode sample, the metal-semiconductor interface does not show voids after annealing. This situation occurs at the sample interface where the Ti/Al electrode is annealed at 650 ℃ for 60 s in N<sub>2</sub> atmosphere and annealed at 850 ℃ for 30 s in N<sub>2</sub> atmosphere. This is one of the reasons why the Hf/Al electrode sample has a lower specific contact resistivity. At the same time, the surface of Hf/Al electrode and Ti/Al electrode annealed at 850 ℃ are characterized by using scanning electron microscope. It is found that the surfaces of both electrodes subject to high temperature annealing show a similar granular rough surface, and this rough surface has a certain influence on the electrical properties of the GaN device. The rough surface formed by the electrode under such high temperature annealing conditions is an urgent problem to be solved in the future research. In summary, the study in this paper indicates the use of Hf/Al to form an ohmic contact with n-type GaN under a low temperature annealing condition.

Low-temperature, plasma assisted, cyclic synthesis of MoS2

Thin film reaction based synthesis techniques are promising for large area, uniform two-dimensional transition metal dichalcogenide (TMD) layers such as MoS2. In this work, the impact of the initial molybdenum film composition (metallic versus oxidized) is explored. Alternating steps of Mo sputtering and H2S soaks are used in conjunction with plasma assisted synthesis techniques to synthesize films at low temperatures. Raman, photoluminescence, x-ray photoelectron spectroscopy, and atomic force microscopy are used to physically characterize the films' atomic structure, stoichiometry, and topography, while devices were fabricated to characterize their electronic properties. MoS2 synthesized from metallic Mo films were found to exhibit better atomic and electronic structure than MoS2 synthesized from MoOx films. Additionally, slowing the rate of synthesis by segmenting growth into repeating cycles resulted in much higher film quality. To understand the impact of atomic structure and stoichiometry on device performance, films synthesized at low temperature were exposed to various high temperature annealing conditions to induce changes in film structure and composition. Physical and electrical characterization reveal that stoichiometry has a significantly weaker influence on electronic performance than grain size and atomic structure. These results provide valuable information on the optimization of low temperature thin film reactions for TMD syntheses.

Application of Flash Lamp Annealing on Nitrogen-Doped Amorphous Indium-Gallium-Zinc-Oxide Thin Film Transistors

Amorphous nitrogenated indium-gallium-zinc oxide (a-IGZO:N) thin films were deposited on highly doped silicon (n+Si) wafer substrates and heat-treated by millisecond flash lamp annealing (FLA) at different preheating temperatures to enhance the electrical characteristics of oxynitride thin film transistors (TFTs). A one-dimensional conduction/radiation heat transfer simulation was conducted to predict the temperature fields in the Si substrate, which indicated that the film temperatures during FLA instantaneously rose above 700°C. The electrical characteristics of the a-IGZO:N TFTs were compared with those produced by conventional furnace annealing of one hour. As a result of the FLA process, a remarkable improvement in the TFT device performance was observed in terms of the electrical output characteristics and transfer curves of the a-IGZO:N TFTs. Morphological analyses were conducted using X-ray diffraction, atomic force microscopy, and field emission scanning electron microscopy, indicating the possibility of partial crystallization of the a-IGZO:N channel layers under high-temperature annealing conditions, but the best TFT performance was found for the amorphous phase of IGZO:N.

Thermal conductivity and stability of multilayered thermal barrier coatings under high temperature annealing conditions

Pyrochlore oxides have most of the relevant attributes for use as next generation thermal barrier coatings (TBCs) such as phase stability, low sintering kinetics and low thermal conductivity. One of the issues with the pyrochlore oxides is their lower toughness and therefore higher erosion rate compared to the current state of the art TBC material, yttria (6–8wt.%) stabilized zirconia (YSZ). In this work, sintering characteristics were investigated for novel multilayered coating consisted of alternating layers of pyrochlore oxide viz. Gd2Zr2O7 and t′ low k (rare earth oxide doped YSZ). Thermal gradient and isothermal high temperature (1316°C) annealing conditions were used to investigate sintering and cracking in these coatings. The results are then compared with that of relevant monolayered coatings and a baseline YSZ coating.

Colloidal and transparent opal-matrix nanocomposites filled with europium-doped silica sols

Three-dimensional ordered opal-matrix composites filled with europium-doped silica sols have been produced using methods of colloid chemistry. According to elemental analysis data, the Eu concentration in the nanocomposites was ∼30 ppm. A uniform europium distribution over the tetrahedral and octahedral pores of the 3D opal matrix was ensured by repeatedly filling the opal pores with silica sols doped with europium salts or europium oxide. Varying high-temperature annealing conditions, one can control the microstructure of 3D ordered nanocomposites, producing opaline and transparent photonic crystals. The microstructure of opal photonic crystals has the form of an ordered fcc lattice of amorphous silica spheres, whose tetrahedral and octahedral pores are filled with mesoporous europium-doped glass. Partial sintering of the silica spheres and mesoporous glass in transparent photonic crystals results in a periodic arrangement of quantum dots enriched in Eu-doped silica.

Modelling of fission gas release from irradiated UO2 fuel under high-temperature annealing conditions

The new model for the vacancy field evolution in grains during annealing of irradiated fuel was developed and implemented in the MFPR code. The model simulates time and spatial variation of the vacancy concentration in the presence of extended vacancy sources (grain boundaries and dislocations) and sinks (growing intragranular bubbles). Being combined with the models for dislocation creep and for bubbles biased migration in the vacancy gradient, the new model self-consistently describes the processes of gas release and microstructure evolution observed in the annealing tests.

Scanning Tunnelling Microscopy of Suspended Graphene

We have obtained for the first time atomic resolution STM images of free-standing graphene, and have found UHV high temperature annealing conditions to controllably achieve atomically clean surfaces. This is an important premise for fundamental studies of the interaction of pristine graphene with foreign atom species, in particular metals.

Growth of oriented Au nanostructures: Role of oxide at the interface

We report on the formation of oriented gold nanostructures on Si(100) substrate by annealing procedures in low vacuum (≈10−2 mbar) and at high temperature (≈975 °C). Various thicknesses of gold films have been deposited with SiOx (using high vacuum thermal evaporation) and without SiOx (using molecular beam epitaxy) at the interface on Si(100). Electron microscopy measurements were performed to determine the morphology, orientation of the structures and the nature of oxide layer. Interfacial oxide layer, low vacuum and high temperature annealing conditions are found to be necessary to grow oriented gold structures. These gold structures can be transferred by simple scratching method.

Weak Localization and Universal Conductance Fluctuations on Epitaxial Graphene Grown on the C-Face of 8°off-Axis 4H-SiC Substrates

We report magnetotransport measurements in single epitaxial graphene layers grown on the C-face of an 8° off-axis 4H-SiC substrate using high temperature annealing conditions with a graphite cap covering the sample. The graphene sheets were found p-type doped, with mobilities varying between 1000 and 11000 cm²/V.s from device to device at 1.6 K. We examine the signature of weak localization and universal conductance fluctuations at weak magnetic field and we show that the phase coherence lengths extracted from the two phenomena are in satisfactory agreement.

Multidimensional characterization, Landau levels and Density of States in epitaxial graphene grown on SiC substrates

Using high-temperature annealing conditions with a graphite cap covering the C-face of, both, on axis and 8° off-axis 4H-SiC samples, large and homogeneous single epitaxial graphene layers have been grown. Raman spectroscopy shows evidence of the almost free-standing character of these monolayer graphene sheets, which was confirmed by magneto-transport measurements. On the best samples, we find a moderate p-type doping, a high-carrier mobility and resolve the half-integer quantum Hall effect typical of high-quality graphene samples. A rough estimation of the density of states is given from temperature measurements.

Growth of monolayer graphene on 8° off-axis 4H–SiC (000–1) substrates with application to quantum transport devices

Using high temperature annealing conditions with a graphite cap covering the C-face of an 8deg off-axis 4H-SiC sample, large and homogeneous single epitaxial graphene layers have been grown. Raman spectroscopy shows evidence of the almost free-standing character of these monolayer graphene sheets, which was confirmed by magneto-transport measurements. We find a moderate p-type doping, high carrier mobility and half integer Quantum Hall effect typical of high quality graphene samples. This opens the way to a fully compatible integration of graphene with SiC devices on the wafers that constitute the standard in today's SiC industry.

SEM/EDS study of metal-assisted oxide desorption

Strongly-enhanced desorption of a thick (100 nm) silicon oxide layer by the pre-sputtering of a thin germanium surface film was observed under high-temperature vacuum annealing conditions. High-resolution SEM imaging reveals that germanium nanoislands are first formed on the sample surface, and that these then act as nucleation centres for the formation of voids in the oxide, leading to a rapid desorption of the silicon oxide layer. EDS analysis of the silicon surface after oxide decomposition shows that the introduced germanium impurities are fully consumed in this desorption process.