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At least 343 records · Page 19

The synthesis and characterization of Mg-Zn-Ca alloy by powder metallurgy process

Known for its biodegradation and biocompatible properties, magnesium alloys have gained many interests to be researched as implant material. In this study, Mg-3Zn-1Ca, Mg-29Zn-1Ca, and Mg-53Zn-4.3Ca (in wt%) were synthesized by means of powder metallurgy method. The compression strength and corrosion resistance of magnesium alloy were thoroughly examined. The microstructures of the alloy were characterized using optical microscopy, Scanning Electron Microscope, and also X-ray diffraction analysis. The corrosion resistance were evaluated using electrochemical analysis. The result indicated that Mg- Zn- Ca alloy could be synthesized using powder metallurgy method. This study showed that Mg-29Zn-1Ca would make the highest mechanical strength up to 159.81 MPa. Strengthening mechanism can be explained by precipitation hardening and grain refinement mechanism. Phase analysis had shown the formation of α Mg, MgO, and intermetallic phases: Mg2Zn11 and also Ca2Mg6Zn3. However, when the composition of Zn reach 53% weight, the mechanical strength will be decreasing. In addition, all of Mg-Zn-Ca alloy studied here had better corrosion resistance (Ecorr around -1.4 VSCE) than previous study of Mg. This study indicated that Mg- 29Zn- 1Ca alloy can be further analyzed to be a biodegradable implant material.

36 MATERIALS SCIENCE↗

The use of a directional solidification technique to investigate the interrelationship of thermal parameters, microstructure and microhardness of Bi–Ag solder alloys

Bi–Ag alloys have been stressed as possible alternatives to replace Pb-based solder alloys. Although acceptable melting temperatures and suitable mechanical properties may characterize such alloys, as referenced in literature, there is a lack of comprehension regarding their microstructures (morphologies and sizes of the phases) considering a composition range from 1.5 to 4.0 wt.%Ag. In order to better comprehend such aspects and their correlations with solidification thermal parameters (growth rate, v and cooling rate, T-dot), directional solidification experiments were carried out under transient heat flow conditions. The effects of Ag content on both cooling rate and growth rate during solidification are examined. Microstructure parameters such as eutectic/dendritic spacing, interphase spacing and diameter of the Ag-rich phase were determined by optical microscopy and scanning electron microscopy. The competition between eutectic cells and dendrites in the range from 1.5 to 4.0 wt.%Ag is explained by the coupled zone concept. Microhardness was determined for different microstructures and alloy Ag contents with a view to permitting correlations with microstructure parameters to be established. Hardness is shown to be directly affected by both solute macrosegregation and morphologies of the phases forming the Bi–Ag alloys, with higher hardness being associated with the cellular morphology of the Bi-2.5 and 4.0 wt.%Ag alloys. - Highlights: • Asymmetric zone of coupled growth for Bi–Ag is demonstrated. • Faceted Bi-rich dendrites have been characterized for Bi–1.5 wt.%Ag alloy. • Eutectic cells were shown for the Bi-2.5 and 4.0 wt.%Ag solder alloys. • Interphase spacing relations with G × v are able to represent the experimental scatters. • Hall-Petch type equations are proposed relating microstructural spacings to hardness.

36 MATERIALS SCIENCE↗

Influence of Local Inhomogeneity of Thermomechanical Treatment Conditions on Microstructure Evolution in Aluminum Alloys

The influence of local inhomogeneity of the stress–strain condition on structure and texture evolution during thermomechanical treatment of aluminum alloys is studied in this work. For this purpose, laboratory rolling and plane strain tests that simulated roughing mill thermomechanical modes were performed. For all processes, the local inhomogeneity of structure evolution was estimated. For this purpose, x-ray texture analysis, EBSD and optical microscopy were used. Additionally, the calculations which allow to evaluate local inhomogeneity of stress–strain conditions for the each process were performed. The experimental results were compared with mathematical simulation output. They indicated structure and texture evolution inhomogeneities, especially during the plane strain and industrial rolling processes. In the plane strain test, typical local deformation zones occurred with different resulting grain size and texture effects than those observed in both rolling processes. This difference was mainly associated with different stress states, strain intensity and strain rate distribution throughout the deformation zone. This study demonstrated that the inhomogeneity of these parameters has a strong impact on structure and texture evolution in the first stage of thermomechanical treatment. In the center layer, laboratory rolling could adequately generate the structure and texture effects observed during rolling of ingots in a commercial mill. Plane strain tests can generate useful results only in the case of adequate choice of sample geometry.

36 MATERIALS SCIENCE↗

Controlling potential barrier height by changing V-shaped pit size and the effect on optical and electrical properties for InGaN/GaN based light-emitting diodes

The internal quantum efficiency (IQE) of InGaN/GaN multiple quantum wells (MQWs) with blue light emission was improved by inserting an InGaN/GaN superlattice (SL) beneath the MQWs. While the SL technique is useful for improving the light-emitting diode (LED) performance, its effectiveness from a multilateral point of view requires investigation. V-shaped pits (V-pits), which generate a potential barrier and screen the effect of the threading dislocation, are one of the candidates for increasing the light emission efficiency of LEDs exceptionally. In this research, we investigated the relationship between the V-pit and SL and revealed that the V-pit diameter is strongly correlated with the IQE by changing the number of SL periods. Using scanning near-field optical microscopy and photoluminescence measurements, we demonstrated the distinct presence of the potential barrier formed by the V-pits around the dislocations. The relationship between the V-pit and the number of SL periods resulted in changing the potential barrier height, which is related to the V-pit diameter determined by the number of SL periods. In addition, we made an attempt to insert pit expansion layers (PELs) composed of combination of SL and middle temperature grown GaN layer instead of only SL structure. As a result of the evaluation of LEDs using SL or PEL, the EL intensity was strongly related to pit diameter regardless of the structures to form the V-pits. In addition, it was clear that larger V-pits reduce the efficiency droop, which is considered to be suppression of the carrier loss at high injection current.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Vibrational exciton nanoimaging of phases and domains in porphyrin nanocrystals

Much of the electronic transport, photophysical, or biological functions of molecular materials emerge from intermolecular interactions and associated nanoscale structure and morphology. However, competing phases, defects, and disorder give rise to confinement and many-body localization of the associated wavefunction, disturbing the performance of the material. Here, we employ vibrational excitons as a sensitive local probe of intermolecular coupling in hyperspectral infrared scattering scanning near-field optical microscopy (IR s-SNOM) with complementary small-angle X-ray scattering to map multiscale structure from molecular coupling to long-range order. In the model organic electronic material octaethyl porphyrin ruthenium(II) carbonyl (RuOEP), we observe the evolution of competing ordered and disordered phases, in nucleation, growth, and ripening of porphyrin nanocrystals. From measurement of vibrational exciton delocalization, we identify coexistence of ordered and disordered phases in RuOEP that extend down to the molecular scale. Even when reaching a high degree of macroscopic crystallinity, identify significant local disorder with correlation lengths of only a few nanometers. This minimally invasive approach of vibrational exciton nanospectroscopy and -imaging is generally applicable to provide the molecular-level insight into photoresponse and energy transport in organic photovoltaics, electronics, or proteins.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

Cryogenic Treatment of CoCrFeMnNi(NbC) High-Entropy Alloys

The effect of cryogenic treatment on the microstructure and mechanical properties of CoCrFeMnNi and CoCrFeMnNi(NbC) high-entropy alloys was investigated during annealing. The heat-treated samples were characterized by optical microscopy, scanning electron microscopy–wavelength-dispersive x-ray spectroscopy, x-ray diffraction technique, differential scanning calorimetry, Vickers hardness testing and tensile testing. The results showed a single-phase FCC crystal structure matrix in both alloys during cryogenic treatment and annealing. Cryogenic treatment altered the recrystallization behavior of CoCrFeMnNi high-entropy alloy, while it did not influence the recrystallization of CoCrFeMnNi(NbC) high-entropy alloy. It was also found that cryogenic treatment changed the precipitation behavior of CoCrFeMnNi(NbC) high-entropy alloy during annealing. In both studied high-entropy alloys, the mechanical testing indicated that the cryogenic treatment can effectively reduce the yield strength of cold-rolled samples after annealing. This was primarily attributed to the effect of cryogenic treatment in enhancing crystalline defects annihilation. Furthermore, the cryogenic treatment increased the ultimate tensile strength of CoCrFeMnNi(NbC). A lager plastic deformation and precipitates were considered as the main reasons for the higher ultimate tensile strength.

36 MATERIALS SCIENCE↗

Crystallization of belite–melilite clinker minerals in the presence of liquid phase

Crystallization of belite–melilite clinker minerals was studied from the view point of a high temperature equilibrium. Ca{sub 2}SiO{sub 4}–Ca{sub 2}Al{sub 2}SiO{sub 7} and Ca{sub 2}SiO{sub 4}–Ca{sub 2}AlFeSiO{sub 7} clinkers were synthesized at 1330 °C–1650 °C. The constituent phases were determined by X-ray powder diffractometry and optical microscopy. Chemical compositions of the individual clinker minerals were determined using an electron probe microanalyzer. We established the two types of P{sub 2}O{sub 5}-bearing pseudobinary phase diagrams in the systems Ca{sub 2}SiO{sub 4}–Ca{sub 2}Al{sub 2}SiO{sub 7} at 1505 °C–1650 °C and Ca{sub 2}SiO{sub 4}–Ca{sub 2}(Al,Fe){sub 2}SiO{sub 7} at 1330 °C–1550 °C. In the latter system, the liquid phase appeared at 1390 °C, which is approximately 150 °C lower than the temperature of liquid formation in the former system. The melilite phenocrysts larger than 50 μm were observed not only in the slowly cooled Ca{sub 2}SiO{sub 4}–Ca{sub 2}(Al,Fe){sub 2}SiO{sub 7} clinker but also in commercial belite–melilite clinkers. These crystals would be nucleated and grown from a liquid phase which was formed at relatively low temperatures.

36 MATERIALS SCIENCE↗

Anandamide and analogous endocannabinoids: a lipid self-assembly study

Anandamide, the endogenous agonist of the cannabinoid receptors, has been widely studied for its interesting biological and medicinal properties and is recognized as a highly significant lipid signaling molecule within the nervous system. Few studies have, however, examined the effect of the physical conformation of anandamide on its function. The study presented herein has focused on characterizing the self-assembly behaviour of anandamide and four other endocannabinoid analogues of anandamide, viz., 2-arachidonyl glycerol, arachidonyl dopamine, 2-arachidonyl glycerol ether (noladin ether), and o-arachidonyl ethanolamide (virodhamine). Molecular modeling of the five endocannabinoid lipids indicates that the highly unsaturated arachidonyl chain has a preference for a U or J shaped conformation. Thermal phase studies of the neat amphiphiles showed that a glass transition was observed for all of the endocannabinoids at {approx} -110 C with the exception of anandamide, with a second glass transition occurring for 2-arachidonyl glycerol, 2-arachidonyl glycerol ether, and virodhamine (-86 C, -95 C, -46 C respectively). Both anandamide and arachidonyl dopamine displayed a crystal-isotropic melting point (-4.8 and -20.4 C respectively), while a liquid crystal-isotropic melting transition was seen for 2-arachidonyl glycerol (-40.7 C) and 2-arachidonyl glycerol ether (-71.2 C). No additional transitions were observed for virodhamine. Small angle X-ray scattering and cross polarized optical microscopy studies as a function of temperature indicated that in the presence of excess water, both 2-arachidonyl glycerol and anandamide form co-existing Q{sub II}{sup G} (gyroid) and Q{sub II}{sup D} (diamond) bicontinuous cubic phases from 0 C to 20 C, which are kinetically stable over a period of weeks but may not represent true thermodynamic equilibrium. Similarly, 2-arachidonyl glycerol ether acquired an inverse hexagonal (HII) phase in excess water from 0 C to 40 C, while virodhamine and arachidonyl dopamine exist as an isotropic L{sub 2} phase, even at very low temperatures. Due to their preferential conformation and lipid self-assembly behaviour, all five endocannabinoids constitute high curvature lipids that can impart membrane stress within a cell membrane which has been linked to a number of membrane and membrane protein associated processes.

59 BASIC BIOLOGICAL SCIENCES↗

Microstructure characterization of the stir zone of submerged friction stir processed aluminum alloy 2219

Aluminum alloy 2219-T6 was friction stir processed using a novel submerged processing technique to facilitate cooling. Processing was conducted at a constant tool traverse speed of 200 mm/min and spindle rotation speeds in the range from 600 to 800 rpm. The microstructural characteristics of the base metal and processed zone, including grain structure and precipitation behavior, were studied using optical microscopy (OM), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). Microhardness maps were constructed on polished cross sections of as-processed samples. The effect of tool rotation speed on the microstructure and hardness of the stir zone was investigated. The average grain size of the stir zone was much smaller than that of the base metal, but the hardness was also lower due to the formation of equilibrium θ precipitates from the base metal θ′ precipitates. Stir zone hardness was found to decrease with increasing rotation speed (heat input). The effect of processing conditions on strength (hardness) was rationalized based on the competition between grain refinement strengthening and softening due to precipitate overaging. - Highlights: • SZ grain size (∼ 1 μm) is reduced by over one order of magnitude relative to the BM. • Hardness in the SZ is lower than that of the precipitation strengthened BM. • Metastable θ′ in the base metal transforms to equilibrium θ in the stir zone. • Softening in the SZ results from a decrease of precipitation strengthening.

36 MATERIALS SCIENCE↗

Effect of rapid thermal processing on copper precipitation in p/p{sup +} silicon epitaxial wafers with heavily boron-doped substrates

The effect of rapid thermal processing (RTP) on the formation of copper precipitation in p/p{sup +} silicon (Si) epitaxial wafers was systematically investigated by defect etching and optical microscopy. After RTP preannealing at high temperature (1250 °C/60 s, with cooling rate 30 K/s) followed by the 750 °C/8 h + 1050 °C/16 h low-high (L-H) two-step annealing, it was revealed that the bulk microdefects were found only inside the p{sup +} substrate, manifesting no defects generated in the epitaxial layer. However, it was found that the width of denude zone (DZ) in samples only subjected to L-H two-step annealing was narrower than that of epitaxial layer, which meant that oxygen precipitation was formed in epitaxial layer. It can be concluded that RTP was beneficial to the formation of DZ. Additionally, it was found that the width of DZ has a sharp dependence on the introducing temperature of copper contamination, that is, the corresponding equilibrium concentration of interstitial copper in the Si influence the thermodynamics and kinetics process of the formation of copper precipitation significantly.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Constitutive Model for Hot Deformation of the Cu-Zr-Ce Alloy

Hot compressive deformation behavior of the Cu-Zr-Ce alloy has been investigated according to the hot deformation tests in the 550-900 °C temperature range and 0.001-10 s{sup −1} strain rate range. Based on the true stress–true strain curves, the flow stress behavior of the Cu-Zr-Ce alloy was investigated. Microstructure evolution was observed by optical microscopy. Based on the experimental results, a constitutive equation, which reflects the relationships between the stress, strain, strain rate and temperature, has been established. Material constants n, α, Q and ln A were calculated as functions of strain. The equation predicting the flow stress combined with these materials constants has been proposed. The predicted stress is consistent with experimental stress, indicating that developed constitutive equation can adequately predict the flow stress of the Cu-Zr-Ce alloy. Dynamic recrystallization critical strain was determined using the work hardening rate method. According to the dynamic material model, the processing maps for the Cu-Zr and Cu-Zr-Ce alloy were obtained at 0.4 and 0.5 strain. Based on the processing maps and microstructure observations, the optimal processing parameters for the two alloys were determined, and it was found that the addition of Ce can promote the hot workability of the Cu-Zr alloy.

36 MATERIALS SCIENCE↗

Development of a spectroscopic Mueller matrix imaging ellipsometer for nanostructure metrology

In this paper, we describe the development of a spectroscopic Mueller matrix imaging ellipsometer (MMIE), which combines the great power of Mueller matrix ellipsometry with the high spatial resolution of optical microscopy. A dual rotating-compensator configuration is adopted to collect the full 4 × 4 imaging Mueller matrix in a single measurement. The light wavelengths are scanned in the range of 400–700 nm by a monochromator. The instrument has measurement accuracy and precision better than 0.01 for all the Mueller matrix elements in both the whole image and the whole spectral range. The instrument was then applied for the measurement of nanostructures combined with an inverse diffraction problem solving technique. The experiment performed on a photoresist grating sample has demonstrated the great potential of MMIE for accurate grating reconstruction from spectral data collected by a single pixel of the camera and for efficient quantification of geometrical profile of the grating structure over a large area with pixel resolution. It is expected that MMIE will be a powerful tool for nanostructure metrology in future high-volume nanomanufacturing.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

Nondestructive Evaluation of Alkali-Silica Reaction in High-Strength Concrete for Aging Structures Sustainability

Concrete is a multiphase geo-material, which is utilized extensively in passive supporting and shielding structures at nuclear facilities. Chemo-mechanical degradation of concrete in old structures is a challenge to sustainability of aging commercial light water reactors. Alkali-silica reaction (ASR) is a common slowly evolving chemo-mechanical damage mechanism of concrete, which could take tens of years to reach the threshold stage when visible cracks appear in a concrete structure. In ASR, concrete constituents react with each other, namely the alkalis in the pore solution of hydrated cement paste (mostly K{sup +}OH{sup -} and Na{sup +}OH{sup -}) react with non-crystalline silica (SiO{sub 2}) of the aggregates to form highly hydrophilic gel. At sufficient levels of ambient relative humidity (typically above 85%), imbibition of water causes expansion of the ASR gel, which results in cracking of constrained reinforced concrete and ultimate structural weakening below safety margin levels. Stability and functional performance of concrete structures potentially suffering from chemo-mechanical deterioration due to ASR is evaluated in a multi-stage process involving material evaluation and structural engineering analysis. Existing methods used by industry for concrete material evaluation are based on extrusion of cores from multiple locations in a structure, and destructive laboratory tests on cores. Because each destructive test requires separate core extrusion, the total number of cores taken from the structure at once could be numbering in hundreds. Laboratory tests include petrography (high resolution optical microscopy of core sections) to develop damage rating index (DRI) score of concrete cores. Another test may involve chemical pore solution extraction from cores, and solution speciation analysis using inductively coupled plasma and mass spectroscopy (ICP/MS). Other tests may consist of mechanical evaluation of cores strength and fracture toughness. The DRI score of concrete material as well as other information obtained from the laboratory tests is subsequently used in structural engineering calculations, where stresses in the entire structure are modeled to evaluate its safety and mechanical stability. Extrusion of a large number of cores is highly undesirable for evaluation of nuclear facility concrete structures. The amount of destructive material testing could be minimized by developing methods for in-situ NDE of ASR to quantify the amount of deterioration that is occurring in the structure, and to identify areas in the structure where more deterioration may be occurring.

36 MATERIALS SCIENCE↗

Evolution of the substructure of a novel 12% Cr steel under creep conditions

In this work we study the microstruture evolution of a newly developed 12% Cr martensitic/ferritic steel in as-received condition and after creep at 650 °C under 130 MPa and 80 MPa. The microstructure is described as consisting of mobile dislocations, dipole dislocations, boundary dislocations, precipitates, lath boundaries, block boundaries, packet boundaries and prior austenitic grain boundaries. The material is characterized employing light optical microscopy (LOM), scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD) and electron backscatter diffraction (EBSD). TEM is used to characterize the dislocations (mobile + dipole) inside the subgrains and XRD measurements are used to the characterize mobile dislocations. Based on the subgrain boundary misorientations obtained from EBSD measurements, the boundary dislocation density is estimated. The total dislocation density is estimated for the as-received and crept conditions adding the mobile, boundary and dipole dislocation densities. Additionally, the subgrain size is estimated from the EBSD measurements. In this publication we propose the use of three characterization techniques TEM, XRD and EBSD as necessary to characterize all type of dislocations and quantify the total dislocation densty in martensitic/ferritic steels. - Highlights: • Creep properties of a novel 12% Cr steel alloyed with Ta • Experimental characterization of different types of dislocations: mobile, dipole and boundary • Characterization and interpretation of the substructure evolution using unique combination of TEM, XRD and EBSD.

36 MATERIALS SCIENCE↗

Characterization of a Messer – The late-Medieval single-edged sword of Central Europe

Metallurgical characterization of a sword blade fragments dating from the second half of the 15th century found in central Slovenia was performed in order to determine its chemical composition, microstructure, microhardness, and to obtain insight into the methods of manufacture of a late-medieval Messer sword. As the artefact was broken, examinations were limited to six very small fragments that were allowed to be removed from the cutting edge, core and the back of the blade. Light optical microscopy, scanning electron microscopy, energy dispersive X-ray spectroscopy, energy dispersive X-ray fluorescence spectrometry, differential scanning calorimetry, thermodynamics approach and Vickers micro-hardness tests were employed to analyze the microstructure and mechanical properties. The results show that the sword was manufactured from a single wrought iron billet. The surface of the sword was carburized. No evidence of quenching was found. The ferritic microstructure is concentrated in the core, and the pearlitic in the outer layer of the blade. All metal fragments contained non-metallic inclusions that were derived mostly from slag and some from hammer scale. - Highlights: • A metallurgical characterization of a medieval sword blade has been performed. • The carbon content decreased from the surface to the core of the blade. • The dominant microstructure in the outer layer is pearlite and in the core is ferrite. • The presence of lump shaped and elongated non-metallic inclusions was observed. • The sword was manufactured from a single wrought iron billet.

36 MATERIALS SCIENCE↗

Effect of cold rolling on the microstructural evolution of new β-typed Ti–6Mo–6V–5Cr–3Sn–2.5Zr alloys

A Ti–6Mo–6V–5Cr–3Sn–2.5Zr (wt.%) alloy was designed as a new metastable β-Ti alloy. The effect that cold rolling had on the microstructural evolution of the material was investigated via optical microscopy (OM), X-ray diffraction (XRD), electron back-scattered diffraction (EBSD) and transmission electron microscopy (TEM) measurements. A single β phase formed in the alloy after solution treatment at 780 °C for 30 min followed by water quenching. The solution-treated alloy was cold rolled with thickness reductions of 10%, 30%, 50% and 70%, and the hardness values increased as the thickness of the specimen decreased. The textures of the cold rolled specimen were characterized according to the 〈110〉 partial parallel to the rolling direction as the rolling reduction increased. The crystallographic orientation showed principal α-fiber textures for (111)〈110〉 and (112)〈110〉. The cold deformation led to the appearance of martensite α″ phases, particularly stress-induced martensite (SIM) α″ phases. - Highlights: • Effect of cold rolling on new β-typed Ti-6Mo-6V-5Cr-3Sn-2.5Zr alloy was studied. • A single β phase was obtained after solution treatment at 780 °C for 30 min. • α-Fiber textures became dominated with the increase in cold rolling reduction. • A stress-induced α″ martensite was caused by cold rolling.

36 MATERIALS SCIENCE↗

Microstructure development and texture evolution of aluminum multi-port extrusion tube during the porthole die extrusion

Aluminum multi-port extrusion tube is processed by the porthole die extrusion and the internal tube walls are welded through the solid state metallurgical bonding. In order to observe the development of grains and their orientations under severe plastic deformation and solid state welding, the extrusion butt together with the die is quenched immediately after extrusion to preserve the grain structure in the processing. The forming histories of selected material points are obtained by analyzing the optical microscopy graph. The evolution of the microstructure along the forming path is characterized by electro backscattered diffraction. It is found that geometrical dynamic recrystallization happens in the process. Grains are elongated, scattered at the transition zone and shear intensive zone, and then pinched off when they are pushed out from the die orifice. The shear-type orientations are predominant at the surface layer on the longitudinal section of the tube web and have penetrated into the intermediate layer. The rolling-type orientations are formed at the central layer. Texture gradient through the thickness of the tube web is observed. And cube orientated grains are found at the seam weld region. - Highlights: •Microstructure of extrusion butt is preserved after the micro scale porthole die extrusion. •Grain morphology history along forming path is investigated. •Texture evolutions on three material flows are present. •Texture gradient exists on the longitudinal section of the internal wall of profile. •Rolling-type and cube textures are found at the solid state welding region.

36 MATERIALS SCIENCE↗

Evaluation of Aluminum-Boron Carbide Neutron Absorbing Materials for Interim Storage of Used Nuclear Fuel

The objective of this work was to understand the corrosion behavior of Boral® and Bortec® neutron absorbers over long-term deployment in a used nuclear fuel dry cask storage environment. Corrosion effects were accelerated by flowing humidified argon through an autoclave at temperatures up to 570°C. Test results show little corrosion of the aluminum matrix but that boron is leaching out of the samples. Initial tests performed at 400 and 570°C were hampered by reduced flow caused by the rapid build-up of solid deposits in the outlet lines. Analysis of the deposits by XRD shows that the deposits are comprised of boron trioxide and sassolite (H 3 BO 3 ). The collection of boron- containing compounds in the outlet lines indicated that boron was being released from the samples. Observation of the exposed samples using SEM and optical microscopy show the growth of new phases in the samples. These phases were most prominent in Bortec® samples exposed at 570°C. Samples of Boral® exposed at 570°C showed minimal new phase formation but showed nearly the complete loss of boron carbide particles. Boron carbide loss was also significant in Boral samples at 400°C. However, at 400°C phases similar to those found in Bortec® were observed. The rapid loss of the boron carbide particles in the Boral® is suspected to inhibit the formation of the new secondary phases. However, Material samples in an actual dry cask environment would be exposed to temperatures closer to 300°C and less water than the lowest test. The results from this study conclude that at the temperature and humidity levels present in a dry cask environment, corrosion and boron leaching will have no effect on the performance of Boral® and Bortec® to maintain criticality control.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗