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COMSOL Results for the Nominal Steady-State Operation of the Proposed 95-MW LEU Silicide Core for HFIR Conversion

Engineering design studies are being performed to determine the feasibility of converting the High Flux Isotope Reactor (HFIR) from highly enriched uranium (HEU) to low-enriched uranium (LEU) fuel at Oak Ridge National Laboratory. This activity is sponsored by the Office of Reactor Conversion and Uranium Supply (ORCUS) under the auspices of the US Department of Energy National Nuclear Security Administration’s Office of Material Management and Minimization. HFIR is a very high flux, pressurized, light water–cooled and moderated, flux trap–type research reactor with a core made of involute shaped U 3 O 8 /Al cermet fuel plates and coolant channels. HFIR currently operates at a thermal power of 85 MW and supports key national and international missions in neutron scattering, isotope production, materials/fuels irradiation, neutron activation analysis, gamma irradiation, and neutrino research. Advanced multiphysics computational fluid dynamics models have been developed in the COMSOL Multiphysics software to simulate the steady-state operating conditions for the proposed low-and high-density LEU U 3 Si 2 -Al (uranium silicide dispersion) fuel designs. The COMSOL models for HFIR inner and outer fuel element models incorporate various essential inputs and physics such as spatially dependent nuclear heat deposition, multilayer heat conduction, conjugate heat transfer, turbulent flows (using Reynolds-averaged Navier Stokes turbulence models), structural mechanics (thermal–structural interactions and fuel swelling), and oxide layer build-up. This report presents the best-estimate thermal hydraulics results for the low- and high-density optimized silicide LEU core designs at 95 MW steady-state nominal operation.

21 SPECIFIC NUCLEAR REACTORS AND ASSOCIATED PLANTS↗

Thermal analysis research applicable to space station technology needs

Thermal analysis, optimization, and software research and development at the NASA Langley Research Center which is applicable to analytical design calculations for space station structures are summarized. Topics discussed include integrated thermal-structural software, improved thermal radiation analysis, solution techniques for transient temperatures, unified thermal-structural finite elements, thermal structural sensitivity analysis and optimization, and concept and performance analysis for heat pipes.

Adelman, H. M.↗

Orbit on demand - Structural analysis finds vertical launchers weigh less

Structural considerations arising from favored design concepts for the next generation on-demand launch vehicles are explored. The two emerging concepts are a two stage fully reusable vertical take-off vehicle (V-2) and a horizontal take-off, two stage subsonic boost launch vehicle (H-2-Sub). Both designs have an 1100 n. mi. cross-range capability, with the V-2 orbiter having small wings with winglets for hypersonic trim and the H-2-Sub requiring larger, swept wings. The rockets would be cryogenic, while airbreathing initial boosters would be either turbofans, turbojets and/or ramjets. Dynamic loading is lower in the launch of a V-2. The TPS is a critical factor due to thinner leading edges than on the Shuttle and may require heat-pipe cooling. Airframe structures made of metal matrix composites have passed finite element simulations of projected loads and can now undergo proof-of-concept tests, although whisker-reinforced materials may be superior once long-whisker technology is developed.

Taylor, A. H.↗

Influence of Chemical Composition on Rupture Properties at 1200 Degrees F. of Forged Chromium-Cobalt-Nickel-Iron Base Alloys in Solution-Treated and Aged Condition

The influence of systematic variations of chemical composition on rupture properties at 1200 degrees F. was determined for 62 modifications of a basic alloy containing 20 percent chromium, 20 percent nickel, 20 percent cobalt, 3 percent molybdenum, 2 percent tungsten, 1 percent columbium, 0.15 percent carbon, 1.7 percent manganese, 0.5 percent silicon, 0.12 percent nitrogen and the balance iron. These modifications included individual variations of each of 10 elements present and simultaneous variations of molybdenum, tungsten, and columbium. Laboratory induction furnace heats were hot-forged to round bar stock, solution-treated at 2200 degrees F., and aged at 1400 degrees F. The melting and fabrication conditions were carefully controlled in order to minimize all variable effects on properties except chemical composition. Information is presented which indicates that melting and hot-working conditions play an important role in high-temperature properties of alloys of the type investigated.

Reynolds, E E↗

Chondrule precursors and cooling paths: The sulfur evidence

The behavior of moderately volatile elements (Na and S) is controversial but critical in understanding chondrule precursors and heating processes. Sulfide appeared to be present in most chondrules, but S should have been vaporized during chondrule formation. In fact, S is extensively redistributed in the course of metamorphism, and its abundance at the end of chondrule formation can only be inferred from the least equilibrated chondrites. Our study of 530 chondrules from Renazzo (CR2) and Semarkona (LL3.0) shows partial volatilization of S during chondrule formation and our melting experiments define conditions for total loss or partial retention of S.

Zanda, B.↗

Aeroheating Thermal Model Correlation for Mars Global Surveyor (MGS) Solar Array

The Mars Global Surveyor (MGS) Spacecraft made use of aerobraking to gradually reduce its orbit period from a highly elliptical insertion orbit to its final science orbit. Aerobraking produces a high heat load on the solar arrays, which have a large surface area exposed to the airflow and relatively low mass. To accurately model the complex behavior during aerobraking, the thermal analysis needed to be tightly coupled to the spatially varying, time dependent aerodynamic heating. Also, the thermal model itself needed to accurately capture the behavior of the solar array and its response to changing heat load conditions. The correlation of the thermal model to flight data allowed a validation of the modeling process, as well as information on what processes dominate the thermal behavior. Correlation in this case primarily involved detailing the thermal sensor nodes, using as-built mass to modify material property estimates, refining solar cell assembly properties, and adding detail to radiation and heat flux boundary conditions. This paper describes the methods used to develop finite element thermal models of the MGS solar array and the correlation of the thermal model to flight data from the spacecraft drag passes. Correlation was made to data from four flight thermal sensors over three of the early drag passes. Good correlation of the model was achieved, with a maximum difference between the predicted model maximum and the observed flight maximum temperature of less than 5%. Lessons learned in the correlation of this model assisted in validating a similar model and method used for the Mars Odyssey solar array aeroheating analysis, which were used during onorbit operations.

Amundsen, Ruth M.↗

Cooled Ceramic Matrix Composite Panel Successfully Tested in Rocket Exhaust

Actively cooled ceramic matrix composite (CMC) components are enabling or enhancing for a broad range of hypersonic and reusable launch vehicle propulsion systems. Teaming with other NASA centers, the Air Force, and industry, the Glenn Ceramics Branch has successfully tested multiple cooled CMC panel concepts in high-heat-flux, high-pressure, flowing rocket engine combustion gas environments. Sub-element components survived multiple cycles and the severe thermal gradients imposed by combustion gas temperatures in excess of 5500 F and cryogenic hydrogen or ambient temperature water internal coolants. These demonstrations are critical for the continued development of this class of materials, and the research is expected to continue with additional concepts and increasingly larger and more complex geometries being fabricated and tested in a broad range of engine operating conditions.

Eckel, Andrew J.↗

Space Shuttle Main Engine Debris Testing Methodology and Impact Tolerances

In the wake of the Space Shuttle Columbia disaster every effort is being made to determine the susceptibility of Space Shuttle elements to debris impacts. Ice and frost debris is formed around the aft heat shield closure of the orbiter and liquid hydrogen feedlines. This debris has been observed to liberate upon lift-off of the shuttle and presents potentially dangerous conditions to the Space Shuttle Main Engine. This paper describes the testing done to determine the impact tolerance of the Space Shuttle Main Engine nozzle coolant tubes to ice strikes originating from the launch pad or other parts of the shuttle.

Gradl, Paul R.↗

Performance of Waterless Concrete

The development of permanent lunar bases is constrained by performance of construction materials and availability of in-situ resources. Concrete seems a suitable construction material for the lunar environment, but water, one of its major components, is an extremely scarce resource on the Moon. This study explores an alternative to hydraulic concrete by replacing the binding mix of concrete (cement and water) with sulfur. Sulfur is a volatile element on the lunar surface that can be extracted from lunar soils by heating. Sulfur concrete mixes were prepared to investigate the effect of extreme environmental conditions on the properties of sulfur concrete. A hypervelocity impact test was conducted, having as its target a 5-cm cubic sample of sulfur concrete. This item consisted of JSC-1 lunar regolith simulant (65%) and sulfur (35%). The sample was placed in the MSFC Impact Test Facility s Micro Light Gas Gun target chamber, and was struck by a 1-mm diameter (~1.4e-03 g) aluminum projectile at 5.85 km/s. In addition, HZTERN code, provided by NASA was used to study the effectiveness of sulfur concrete when subjected to space radiation.

Toutanji, Houssam↗

Enthalpy-Based Thermal Evolution of Loops: II. Improvements to the Model

This paper further develops the zero-dimensional (0D) hydrodynamic coronal loop model "Enthalpy-based Thermal Evolution of Loops" (EBTEL) originally proposed by Klimchuk et al (2008), which studies the plasma response to evolving coronal heating. It has typically been applied to impulsive heating events. The basis of EBTEL is the modelling of mass exchange between the corona and transition region and chromosphere in response to heating variations, with the key parameter being the ratio of transition region to coronal radiation. We develop new models for this parameter that now include gravitational stratification and a physically motivated approach to radiative cooling. A number of examples are presented, including nanoflares in short and long loops, and a small flare. It is found that while the evolution of the loop temperature is rather insensitive to the details of the model, accurate tracking of the density requires the inclusion of our new features. In particular, we are able to now obtain highly over-dense loops in the late cooling phase and decreases to the coronal density arising due to stratification. The 0D results are compared to a 1D hydro code (Hydrad). The agreement is acceptable, with the exception of the flare case where some versions of Hydrad can give significantly lower densities. This is attributed to the method used to model the chromosphere in a flare. EBTEL is suitable for general use as a tool for (a) quick-look results of loop evolution in response to a given heating function and (b) situations where the modelling of hundreds or thousands of elemental loops is needed. A single run takes a few seconds on a contemporary laptop.

Cargill, P. J.↗

Simulating Damage Due to a Lightning Strike Event: Effects of Temperature Dependent Properties on Interlaminar Damage

A multidirectional, carbon fiber-epoxy, composite panel is subjected to a simulated lightning strike, within a finite element method framework, and the effect of material properties on the failure (delamination) response is investigated through a detailed numerical study. The numerical model of the composite panel consists of individual homogenized plies with user-defined, cohesive interface elements between them. Lightning strikes are simulated as an assumed combination of excessive heat and high pressure loadings. It is observed that the initiation and propagation of lightning-induced delamination is a significant function of the temperature dependency of interfacial fracture toughness. This dependency must be defined properly in order to achieve reliable predictions of the present lightning-induced delamination in the composite panel.

computational mechanics↗

Porous silicon based anode material formed using metal reduction

A porous silicon based material comprising porous crystalline elemental silicon formed by reducing silicon dioxide with a reducing metal in a heating process followed by acid etching is used to construct negative electrode used in lithium ion batteries. Gradual temperature heating ramp(s) with optional temperature steps can be used to perform the heating process. The porous silicon formed has a high surface area from about 10 m.sup.2/g to about 200 m.sup.2/g and is substantially free of carbon. The negative electrode formed can have a discharge specific capacity of at least 1800 mAh/g at rate of C/3 discharged from 1.5V to 0.005V against lithium with in some embodiments loading levels ranging from about 1.4 mg/cm.sup.2 to about 3.5 mg/cm.sup.2. In some embodiments, the porous silicon can be coated with a carbon coating or blended with carbon nanofibers or other conductive carbon material.

36 MATERIALS SCIENCE↗

Thermal Hydraulics Safety Analyses of TRIGA Reactor Upon Fuel Reconfiguration

Safety analyses of the Training, Research, Isotope, General Atomics (TRIGA) reactor at Kansas State University(KSU) is performed using thermal hydraulic simulations based on changes to reactivity or the volumetric heat generation rate due to changes in the positioning of the enriched fuel elements in the reactor core. If the reactivity or neutronics parameters are known, then they can be used to simulate the thermal energy state of the material which is crucial to assess the safety of the nuclear fuel inside a nuclear reactor. Several thermal hydraulics models and codes have been developed in the past to assess reactor safety. RELAP (Reactor Excursion and Leak Analysis Program) is one such tool widely used throughout the world for safety analyses. Although RELAP is considered a reliable tool by regulators, vendors, and operators, it lacks the numerical fidelity provided by 3-D computational fluid dynamics (CFD) models. This work involves the critical task of assessing safety of a research reactor upon fuel reconfiguration based on models developed in RELAP and comparing them with a commercially available 3-D CFD program. The TRIGA Mark-II reactor, designed by General Atomics and located at Kansas State University, is a class of small pool type inherently safe research reactor licensed to operate at steady state power of up to 1.25 MW. It has a cylindrical core measuring 0.45 meters diametrically and 0.38 meters axially positioned in a tank measuring 1.98 meters diametrically and 6.25 meters axially. It has uranium zirconium hydride (UZrH) fuel rods housed in stainless steel cladding material arranged in five concentric rings (B,C,D,E and F rings, in that order, moving outwards from the center). TRIGA fuel is nominally 20% enriched, but the reactivity of the fuel can be changed by using burnable poisons (not used at KSU), or by varying the total weight percent of uranium in the UZrH fuel meat. The TRIGA reactor is designed to be an inherently safe reactor and is designed to be cooled by natural convection. Thus it is of paramount importance to avoid the film boiling regime; failing to do so will subject the fuel to severe conditions, possibly resulting in its failure due to fuel/clad interactions. A high DNBR ratio is a primary consideration in the reactor core design and thus any modification in the core should ensure that this criteria is always met. In order to fully utilize the capabilities of KSU TRIGA reactor facility, it should be operated at its full capacity, i.e. 1.25 MW, which requires increasing the fuel loading in some of the E- and F-ring elements from 8.5% U (nominal) to 12.0% U (nominal). Only four elements are to be switched to 12% loading, causing local power peaking in these elements. The degree of power peaking to be expected in these 12%-loaded fuel elements was calculated based on a detailed MCNP (Monte Carlo N-Particle code) model of the reactor core. Some preliminary results of the calculations are presented in this paper based on changes in peaking factors and power levels. To predict reactor thermal behavior, axial changes in the peaking factors obtained from MCNP models were used to calculate volumetric energy density functions for a single channel one dimensional RELAP model and a three dimensional COMSOL model of the TRIGA MARK-II reactor. (authors)

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Computational Thermodynamic Study to Predict Complex Phase Equilibria in the Nickel-Base Superalloy Rene N6

A previous study by Ritzert et al. on the formation and prediction of topologically closed packed (TCP) phases in the nickel-base superalloy Rene' N6 is re-examined with computational thermodynamics. The experimental data on phase distribution in forty-four alloys with a composition within the patent limits of the nickel-base superalloy Rene' N6 provide a good basis for comparison to and validation of a commercial nickel superalloy database used with ThermoCalc. Volume fraction of the phases and partitioning of the elements are determined for the forty-four alloys in this dataset. The baseline heat treatment of 400 h at 1366 K was used. This composition set is particularly interesting since small composition differences lead to dramatic changes in phase composition. In general the calculated values follow the experimental trends. However, the calculations indicated no TCP phase formation when the experimental measurements gave a volume percent of TCP phase less than 2 percent. When TCP phases were predicted, the calculations under-predict the volume percent of TCP phases by a factor of 2 to 8. The calculated compositions of the gamma and gamma' phases show fair agreement with the measurements. However, the calculated compositions of the P Phase do not agree with those measured. This may be due to inaccuracies in the model parameters for P phase and/or issues with the microprobe analyses of these phases. In addition, phase fraction diagrams and sigma and P phase solvus temperatures are calculated for each of the alloys. These calculations indicate that P phase is the primary TCP phase formed for the alloys considered here at 1366 K. Finally, a series of isopleths are calculated for each of the seven alloying elements. These show the effect of each alloying element on creating TCP phases.

Copland, Evan H.↗

Influences of Quench Cooling Rate on Microstructure and Corrosion Resistance of Al-Cu-Mg Alloy Based on the End-Quenching Test

To investigate the effects of the quench cooling rate on corrosion resistance of Al-Cu-Mg alloy, an end-quenching test was conducted and the microstructures at different cooling rates were observed by SEM and TEM. Additionally, the corrosion resistance was characterized by an intergranular corrosion test and electrochemical test. Moreover, the finite element method was applied to simulate the end quenching process. The results indicate that the actual end quenching process can be approximated as one-dimensional heat transfer, and the cooling rate varies at different cooling distances. By affecting the microstructures, decreasing the cooling rate leads to a decline in the corrosion properties. Low cooling rates coarsen the constituent particles and grain boundary particles, resulting in a wide precipitation-free zone and an increase in the intensity of corrosion reactions. A high cooling rate concentrates on the intragranular precipitant, which can reduce the pitting depth and represents a conversion from localized corrosion to general corrosion.

36 MATERIALS SCIENCE↗

A Study of Nucleate Boiling with Forced Convection in Microgravity

The ultimate objective of basic studies of flow boiling in microgravity is to improve the understanding of the processes involved, as manifested by the ability to predict its behavior. This is not yet the case for boiling heat transfer even in earth gravity, despite the considerable research activity over the past 30 years. The elements that constitute the nucleate boiling process - nucleation, growth, motion, and collapse of the vapor bubbles (if the bulk liquid is subcooled) - are common to both pool and flow boiling. It is well known that the imposition of bulk liquid motion affects the vapor bubble behavior relative to pool boiling, but does not appear to significantly influence the heat transfer. Indeed, it has been recommended in the past that empirical correlations or experimental data of pool boiling be used for design purposes with forced convection nucleate boiling. It is anticipated that such will most certainly not be possible for boiling in microgravity, based on observations made with pool boiling in microgravity. In earth gravity buoyancy will act to remove the vapor bubbles from the vicinity of the heater surface regardless of how much the imposed bulk velocity is reduced, depending, of course, on the geometry of the system. Vapor bubbles have been observed to dramatically increase in size in pool boiling in microgravity, and the heat flux at which dryout took place was reduced considerably below what is generally termed the critical heat flux (CHF) in earth gravity, depending on the bulk liquid subcooling. However, at heat flux levels below dryout, the nucleate pool boiling process was enhanced considerably over that in earth gravity, in spite of the large vapor bubbles formed in microgravity and perhaps as a consequence. These large vapor bubbles tended to remain in the vicinity of the heater surface, and the enhanced heat transfer appeared to be associated with the presence of what variously has been referred to as a liquid microlayer between the bubble and the heater surface. The enhancement of the boiling process with low velocities in earth gravity for those orientations producing the formation of a liquid macrolayer described above, accompanied by "sliding" vapor bubbles, has been demonstrated. The enhancement was presented as a function of orientation, subcooling, and heated length, while a criterion for the heat transfer for mixed natural/forced convection nucleate boiling was given previously. A major unknown in the prediction and application of flow boiling heat transfer in microgravity is the upper limit of the heat flux for the onset of dryout (or critical heat flux - CHF), for given conditions of fluid-heater surfaces, including geometry, system pressure and bulk liquid subcooling. It is clearly understood that the behavior in microgravity will be no different than on earth with sufficiently high flow velocities, and would require no space experimentation. However, the boundary at which this takes place is still an unknown. Previous results of CHF measurements were presented for low velocity flow boiling at various orientations in earth gravity as a function of flow velocity and bulk liquid subcooling, along with preliminary measurements of bubble residence times on a flat heater surface. This showed promise as a parameter to be used in modeling the CHF, both in earth gravity and in microgravity. The objective of the work here is to draw attention to and show results of current modeling efforts for the CHF, with low velocities in earth gravity at different orientations and subcoolings. Many geometrical possibilities for a heater surface exist in flowing boiling, with boiling on the inner and outer surfaces of tubes perhaps being the most common. If the vapor bubble residence time on and departure size from the heater surface bear a relationship to the CHF, as results to be given indicate, it is important that visualization of and access to vapor bubble growth be conveniently available for research purposes. In addition, it is desirable to reduce the number of variables as much as possible in a fundamental study. These considerations dictated the use of a flat heater surface, which is rectangular in shape, 1.91 cm by 3.81 cm (0.75 x 1.5 inches), consisting either of a 400 Angstrom thick semi-transparent gold film sputtered on a quartz substrate which serves simultaneously as a heater and a resistance thermometer, or a copper substrate of the same size. The heater substrate is a disc which can be rotated so that the heated length in the flow direction can be changed from 1.91 to 3.81 cm (0.75 to 1.5 inches). The fluid is R-113, and the velocities can be varied between 0.5 cm/s and 60 cm/s. For a sufficiently low velocity the CHF can be modeled reasonably well at various orientations by the correlation for pool boiling corrected for the influence of bulk liquid subcooling, multiplied by the square root of q, the angle relative to horizontal. This arises from equating buoyancy and drag forces in the inverted positions where the vapor bubbles are held against the heater surface as they slide. A distortion of the measurements relative to pool boiling occurs as the flow velocity increases. In modeling this effect at different levels of subcooling it appeared appropriate to estimate the volumetric rate of vapor generation, using measurements of bubble frequency (or residence time), void fraction and average bubble boundary layer thickness. These were determined with the use of a platinum hot wire probe 0.025 mm in diameter by 1.3 mm long, applying a constant current to distinguish between contact with liquid or vapor. Two-dimensional spatial variations are obtained with a special mechanism to resolve displacements in increments of 0.025 mm. From such measurements it was determined that the fraction of the surface heat transfer resulting in evaporation varies inversely with the subcooling correction factor for the CHF. The measured inverse bubble residence time is normalized relative to that predicted for an infinite horizontal flat plate at the CHF, and is correlated well with the CHF normalized relative to that for pool boiling, for various orientation angles and subcooling levels. This correspondence is then combined with a normalizing factor for the energy flux leaving the heater surface at the CHF and the computed bubble radius at departure, determined from the balance between the outward velocity of the interface due to evaporation and the buoyance induced velocity of the center of mass of the bubble. The product of the CHF and the corresponding residence time was determined to be a constant for all orientations at a given bulk flow velocity and liquid subcooling, and must be determined empirically for each velocity and subcooling at present. It then becomes possible to predict the CHF for the different orientations, velocities, and subcoolings. These are compared with normalized measurements of the CHF for velocities ranging from 4 cm/s to 55 cm/s, subcoolings from 2.8 to 22.2 K, over orientations angles of 360 degrees.

Merte, Herman, Jr.↗

Thermal-Fluid and Thermal-Structural Response of the T-Tube Modular Divertor to Spatiotemporally Varying Heat Loads

Tungsten (W) is the leading candidate for divertor target plates because of its high melting point (>3000°C), thermal conductivity, and ultimate tensile stress. While W and its alloys are the only solid materials that can survive the high heat fluxes incident on the divertor, W’s low-ductility high ductile-to-brittle transition temperature of ~600°C and relatively low recrystallization temperature (RT) of ~1300°C pose structural (among other) challenges. The objective of this work is to estimate the thermal-fluid and thermal-structural performance of the helium (He)-cooled T-tube divertor, which was originally developed by the Advanced Reactor Innovation and Evaluation Study (ARIES) using numerical simulations. Here, predictions of temperature distributions across the plasma-facing structural component and surface pressures from computational fluid dynamics simulations are used to determine stress distributions using commercial structural finite element modeling software over a range of fusion-relevant conditions. The maximum allowable incident heat fluxes are determined based on the temperature limits imposed by the ITER elastic Structural Design Criteria for In-vessel Components (SDC-IC) and the maximum RT over a range of He mass flow rates and presented in the form of performance design charts. Our recent work found that thermal- structural criteria accounting for the low ductility of W in a finger-type modular divertor constrain the maximum incident heat fluxes to values well below the ITER specifications, and those based on considering only the RT demonstrate that integrated thermal-fluid and elastic structural performance evaluation are required for accurate assessment of divertor performance. This novel analysis of the T-tube considers how nonuniform and transient incident heat fluxes affect its thermal-fluid and thermal-structural performance, as well as the effect of volumetric heating, which can be as great as 27% of the power incident on the divertor surface. The W tile of the T-tube, with its relatively large plasma-facing area of ~15 cm 2 , will likely experience significant spatial variations in incident heat flux. This work therefore assesses whether steady-state incident heat flux profiles with a peak of 10 MW/m 2 and maximum heat flux gradients of 200 MW/m 2 per m exceed the structural limits imposed by the ITER elastic SDC-IC and the maximum RT over a range of fusion-relevant conditions. The effect of transient heat fluxes typical of plasma detachment and reattachment from the target plate due, for example, to gas injection are also evaluated

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

Solvothermal hot injection synthesis of core-shell AgNi nanoparticles

Silver-nickel core-shell nanoparticles (NP) were prepared by solvothermal hot injection synthesis by simultaneous thermolysis/reduction of AgNO 3 and Ni(acac) 2 precursors in the hot mixture of octadecene and oleylamine. Oleylamine decreases decomposition temperature of AgNO 3 to that of Ni(acac) 2 thus ensuring favorable reaction conditions. The prepared AgNi NPs with different Ag/Ni ratios were completely characterized. Dynamic light scattering (DLS) and small angle X-ray scattering (SAXS) were used for particle size characterization of as-prepared AgNi colloids. There is no dependence of the particle size (13–21 nm by SAXS) on the Ag/Ni stoichiometric ratio, but the ultraviolet–visible spectroscopy (UV–vis) reveals that the intensity of the surface plasmon (SPR) decreases with increasing Ni content. Transmission electron microscopy (TEM) verified the results of DLS and SAXS and showed spherical nanoparticle shape. Distribution of individual elements in the nanoparticles was mapped by high resolution scanning transmission electron microscopy and energy dispersive X-ray spectroscopy (STEM-EDS) and revealed their core-shell structure where an Ag nucleus is covered by a thin amorphous Ni layer. Upon heating to 400 °C, Ni crystallization is substantiated by appearance of diffractions in the high-temperature X-ray powder diffractograms (HT-XRD) and of a magnetic moment. Ultimate phase separation was proven by scanning electron microscopy and energy dispersive X-ray analysis (SEM-EDS) in samples heated to 1000 °C. The reaction course and nanoparticle formation studied by DLS, UV–vis, and Ag and Ni elemental analyses reveal an initial Ag seed formation with subsequent Ni overlayer deposition after 180 s.

36 MATERIALS SCIENCE↗

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