| 1. |
- Fazi, Andrea, 1992, et al.
(author)
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Characterization of as-deposited cold sprayed Cr-coating on Optimized ZIRLO™ claddings
- 2021
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In: Journal of Nuclear Materials. - : Elsevier BV. - 0022-3115. ; 549
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Journal article (peer-reviewed)abstract
- As-produced Cr-coated Optimized ZIRLO™ cladding material fabricated with the cold-spray (CS) deposition process is studied. Cross-sectional electron microscopy, nano-hardness profiling, transmission electron microscopy, transmission Kikuchi diffraction, and atom probe tomography (APT) were performed to investigate the nature of the CS Cr-coating/Optimized ZIRLO™ interface, the microstructure of the coating, and the effects of the deposition on the Zr-substrate microstructure. The former surface of the Zr-substrate was found to have a highly deformed nano-crystalline microstructure, the formation of which was attributed to dynamic recrystallization occurring during coating deposition. This microstructural change, evaluated with electron backscattered diffraction and nano-hardness profiling, appeared to be confined to a depth of a few microns. Through APT analysis, a 10–20 nm thick intermixed bonding region was observed at the interface between coating and substrate. The chemical composition of this region suggests that this layer originated from a highly localized shearing and heating of a thin volume of the outermost former surface of the substrate. The study of the intermixed bonding region's crystalline structure was performed with high resolution transmission electron microscopy and revealed a distorted hexagonal close-packed structure.
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| 2. |
- Fazi, Andrea, 1992
(author)
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Cold spray Cr-coated Optimized ZIRLO claddings: an option for accident tolerant fuels
- 2021
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Licentiate thesis (other academic/artistic)abstract
- Accident tolerant fuel development has started with the aim of providing nuclear fuels able to endure severe accident conditions. Research in this field has also sparked a wave of material renewal in the nuclear industry that had being delayed for the last few decades. Climate change is an ever-growing public concern, and policies about greenhouse gas emissions are becoming more stringent both at the national and international level. Nuclear energy produces very low carbon emissions and the successful development of new accident tolerant materials might play a role in making this technology a viable solution to this global issue. Cr-coated zirconium claddings are one of the most promising candidates as near-term response to the need for accident tolerant materials. These coatings can be produced via a range of different technologies, but the two main designs being currently developed are obtained with physical vapour deposition or cold spray (CS) deposition. In cold spray, high pressure gas is fed through a nozzle together with Cr powder. The Cr particles are accelerated up to 1200 m/s and directed to the substrate, in this case cladding tubes made of Optimized ZIRLO™ alloy. The resulting Cr-coated zirconium cladding is the subject of this work. As-fabricated samples and autoclave tested material are characterized with atom probe tomography and a range of electron microscopy techniques. The scope of the investigation is to evaluate the performances of Cr-coated claddings under operating conditions. Additionally, the nature of the adhesion in cold spray coating and the effects of this deposition method on the substrate are explored. A 10-20 nm thick intermixed bonding region was observed at the Cr/Zr interface of the as-fabricated cladding. This region is deemed to play an important role in the strong adhesion of CS coatings. When exposed to operating conditions, ZrCr2-Laves phase was found to nucleate in the intermixed bonding region. CS deposition involves severe plastic deformation of both coating and substrate. As a result, a 1-2 μm thick nanocrystalline layer can be found in the substrate adjacent to the Cr/Zr interface. After autoclave exposure, a Zr-Cr-Fe phase was discovered precipitating in this nanocrystalline layer at the Zr grain boundaries.
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| 3. |
- Fazi, Andrea, 1992, et al.
(author)
-
Cold sprayed Cr-coating on Optimized ZIRLO™ claddings: the Cr/Zr interface and its microstructural and chemical evolution after autoclave corrosion testing
- 2022
-
In: Journal of Nuclear Materials. - : Elsevier BV. - 0022-3115. ; 560
-
Journal article (peer-reviewed)abstract
- Cr-coated Optimized ZIRLO™ cladding material fabricated with the cold-spray deposition process is studied. Microstructure and chemistry of this material are investigated before and after exposure to autoclave corrosion testing with scanning electron microscopy, energy dispersive spectroscopy analysis, electron backscattered diffraction, transmission electron microscopy and atom probe tomography. The results are used to assess what changes have occurred upon autoclave exposure. The formation of a compact, 80 – 100 nm thick Cr2O3 layer is observed on the surface of the exposed samples. Nucleation of ZrCr2 intermetallic phase is discovered at the Cr/Zr interface. This Laves phase nucleates inside the intermixed bonding layer that can be found in both pristine and exposed samples, and decorates the interface in the form of small particles (less than 50 nm in size). Using transmission electron microscopy and atom probe tomography the growth of a Zr-Cr-Fe phase was detected. This phase is found in the region of the Zr-substrate immediately adjacent to the coating, up to a few hundred nanometres distance from the Cr/Zr interface. A small degree of recrystallization occurs upon autoclave exposure in the 1-2 µm thick nanocrystalline layer produced on the Zr-substrate by the cold spray deposition method utilized for the fabrication of the Cr-coating.
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| 4. |
- Fazi, Andrea, 1992, et al.
(author)
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Comparing CrN and TiN Coatings for Accident-Tolerant Fuels in PWR and BWR Autoclaves
- 2022
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In: Journal of Nuclear Engineering. - : MDPI AG. - 2673-4362. ; 3:4, s. 321-332
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Journal article (peer-reviewed)abstract
- The development of coatings for accident-tolerant fuels (ATFs) for light water reactor (LWR) applications promises improved corrosion resistance under accident conditions and better performances during operation. CrN and TiN coatings are characterized by high wear resistance coupled with good corrosion resistance properties. They are generally used to protect materials in applications where extreme conditions are involved and represent promising candidates for ATF. Zr cladding tubes coated with 5 µm-thick CrN or TiN, exposed in an autoclave to simulated PWR chemistry and BWR chemistry, were characterized with SEM, EDS, and STEM. The investigation focused on the performance and oxidation mechanisms of the coated claddings under simulated reactor chemistry. Both coatings provided improved oxidation resistance in a simulated PWR environment, where passivating films of Cr2O3 and TiO2, less than 1 µm-thick, formed on the CrN and TiN outer surfaces, respectively. Under the more challenging BWR conditions, any formed Cr2O3 dissolved into the oxidizing water, resulting in the complete dissolution of the CrN coating. For the TiN coating, the formation of a stable TiO2 film was observed under BWR conditions, but the developed oxide film was unable to stop the flux of oxygen to the substrate, causing the oxidation of the substrate.
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| 5. |
- Fazi, Andrea, 1992, et al.
(author)
-
CrN–NbN nanolayered coatings for enhanced accident tolerant fuels in BWR
- 2023
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In: Journal of Nuclear Materials. - 0022-3115. ; 586
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Journal article (peer-reviewed)abstract
- The accident tolerant fuel (ATF) concept has emerged in the years after the 2011 Fukushima accident as part of a renewed effort in research for light water reactors. The primary focus is to further improve safety measures under and beyond design basis accident conditions, and to improve fuel cladding performance in normal operation. The application of a coating on zirconium claddings can achieve both these aims without extensive changes to the reactor design. Metallic chromium coatings have been profusely studied as solution for pressurized water reactors, but the search for an effective ATF coating able to withstand the environment inside boiling water reactors (BWRs) is still ongoing. In this work, two different versions of a novel nitride coating composition were studied. Zirconium claddings coated with 8 µm thick layers of superlattice CrN–NbN and a nanolayered CrN–NbN were tested in autoclave under BWR operating conditions for 60 days. Scanning electron microscopy, transmission electron microscopy, energy dispersive x-ray spectroscopy, electron back-scattered diffraction, x-ray diffraction, and atom probe tomography were employed to characterize as-deposited and autoclaved samples of these two materials. During exposure, both coating versions formed a stable, dense and passivating oxide scale (200–300 nm thick) on the surface, demonstrating improved oxidation protection under operating conditions. Some differences in the oxide growth mechanism were observed between the superlattice and the nanolayered CrN–NbN coatings, which allowed to glimpse at the effect of the layer thickness on the oxidation protection provided by these coatings. The nano-structured morphology of both coatings remained unaffected by the autoclave test, but a 35 nm thick Zr-Cr-N phase was found at the coating-substrate interface of the superlattice CrN–NbN coated cladding.
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| 6. |
- Fazi, Andrea, 1992
(author)
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Development and performance evaluation of accident-tolerant coated fuel claddings for light water reactors
- 2023
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Doctoral thesis (other academic/artistic)abstract
- The development of accident tolerant fuel has the aim of providing nuclear fuels able to endure severe accident conditions. Research in this field has also sparked a wave of material renewal in the nuclear industry that had been delayed for the last few decades. Climate change is an ever-growing public concern, and policies about greenhouse gas emissions are becoming more stringent both at the national and international level. Nuclear energy produces very low carbon emissions and the successful development of new accident tolerant materials might play a role in making this technology a viable solution to this global issue. Coated zirconium claddings are one of the most promising candidates as a near-term response to the need for accident tolerant materials. These coatings can be produced via a range of different technologies, but two main techniques are being currently employed for the development of such coatings: cold spray deposition and physical vapour deposition (PVD). In cold spray, high pressure gas is fed through a nozzle together with a powder. Powder particles are accelerated up to 1200 m/s and directed to the substrate, in this case cladding tubes made of zirconium alloy. In PVD, the coating material is evaporated from a target and sputtered onto the substrate as atoms or ions. The resulting coated zirconium claddings are the subject of this work. As-fabricated samples, autoclave tested material, and specimens tested under simulated accident conditions are characterized with atom probe tomography and a range of electron microscopy techniques. The scope of the investigation is to evaluate the performance of the coated claddings under operating conditions and in simulated accident conditions. Metallic Cr has emerged as the best candidate for accident tolerant coatings for pressurised water reactors. In this work, the focus was on Cr-coatings deposited with cold spray, which performed well in both tested environments. A passivating layer of chromia formed during autoclave exposure, and a protective scale of chromia prevented any oxidation of the Zrsubstrate for up to 40 min in 1200 C steam. The nature of the adhesion in cold spray coatings and the effects of this deposition method on the substrate were studied. The formation of a Cr2Zr phase at the Cr/Zr interface was observed both under autoclave and simulated accident conditions. The search for an effective accident tolerant coating for boiling water reactors is more challenging and many coatings have been tested in autoclave, where PVD (Cr,Nb)N coatings showed the best performance under operating conditions. A 200 nm thick passivating oxide film composed of an outer Cr, Nb, Ni phase and an inner layer of oxidised coating was found after exposure.
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| 7. |
- Fazi, Andrea, 1992, et al.
(author)
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Multiple growth of graphene from a pre-dissolved carbon source
- 2020
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In: Nanotechnology. - : IOP Publishing. - 1361-6528 .- 0957-4484. ; 31:34, s. 345601-
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Journal article (peer-reviewed)abstract
- Mono- to few-layer graphene materials are successfully synthesized multiple times using Cu-Ni alloy as a catalyst after a single-chemical vapor deposition (CVD) process. The multiple synthesis is realized by extracting carbon source pre-dissolved in the catalyst substrate. Firstly, graphene is grown by the CVD method on Cu-Ni catalyst substrates. Secondly, the same Cu-Nicatalyst foils are annealed, in absence of any external carbon precursor, to grow graphene using the carbon atoms pre-dissolved in the catalyst during the CVD process. This annealing process is repeated to synthesize graphene successfully until carbon is exhausted in the Cu-Ni foils. After the CVD growth and each annealing growth process, the as-grown graphene is removed using a bubbling transfer method. A wide range of characterizations are performed to examine the quality of the obtained graphene material and to monitor the carbon concentration in the catalyst substrates. Results show that graphene from each annealing growth process possesses a similar quality, which confirmed the good reproducibility of the method. This technique brings great freedom to graphene growth and applications, and it could be also used for other 2D material synthesis.
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| 8. |
- Fazi, Andrea, 1992, et al.
(author)
-
Performance and evolution of cold spray Cr-coated optimized ZIRLO™ claddings under simulated loss-of-coolant accident conditions
- 2023
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In: Journal of Nuclear Materials. - : Elsevier BV. - 0022-3115. ; 576
-
Journal article (peer-reviewed)abstract
- The performance of Cr-coated Optimized ZIRLO™ as accident tolerant fuel cladding material for pressurized water reactors (PWRs) is assessed. The coating oxidation mechanisms, oxide stability, and the transformation of the Cr-coating/Optimized ZIRLO™ interface are among the studied phenomena. For this purpose, samples were exposed at 1200°C in steam for 3 min, 20 min and 40 min. As-fabricated coated claddings, plus specimens tested in autoclave at 415°C for 90 days in simulated PWR water chemistry were employed for comparison. Characterization techniques such as scanning electron microscopy, energy dispersive x-ray spectroscopy, electron backscattered diffraction, and transmission electron microscopy were used to determine the chemistry and crystalline structure of the various phases formed during the different exposures. When exposed to loss-of-coolant accident (LOCA) conditions for 40 min, a layer of Cr2O3 up to 8 µm thick was measured on the outer surface of the Cr-coating. No significant oxidation of the underlaying Optimized ZIRLO™ alloy occurred, and the applied coating appears to be very effective at delaying the cladding degradation under accident conditions. At the coating-substrate interface, a 1–2 µm thick layer of (Cr,Fe)2Zr Laves phase was found. The presence of this phase appears to have no detrimental effects on the coating performance, and it might play a role in slowing down the dissolution of the coating into the substrate. ZrO2 particles were frequently found at grain boundaries in the coating after exposure to LOCA conditions. For longer exposure time, these particles are expected to grow into a ZrO2-network, creating a fast diffusion path for O, and compromising the oxidation protection offered by the coating.
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| 9. |
- Jabir Hussain, Ahmed Fardan, 1996, et al.
(author)
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Fine-Tuning Melt Pools and Microstructures: Taming Cracks in Powder Bed Fusion—Laser Beam of a non-weldable Ni-base Superalloy
- 2024
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In: Materialia. - : ELSEVIER SCI LTD. - 2589-1529. ; 34
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Journal article (peer-reviewed)abstract
- Powder Bed Fusion – Laser Beam (PBF-LB) of high γ’ strengthened Ni-base superalloys, such as CM247LC, is of great interest for high temperature applications in gas turbines. However, PBF-LB of CM247LC is challenging due to the high cracking susceptibility during PBF-LB processing (solidification cracking) and heat treatment (strain age cracking, mostly caused by residual stresses). This study focuses on understanding the impact of process parameters on microstructure, residual stresses and solidification cracking. Laser power (P), speed (v) and hatch spacing (h) were varied while the layer thickness (t) was fixed. The melt pool size and shape were found to be key factors in minimizing solidification cracking. Narrower and shallower melt pools, achieved using a low line energy density (LED = P/v ≤ 0.1 J/mm), gave low crack densities (0.7 mm/mm2). A tight hatch spacing (h = 0.03 mm) resulted in reduced lack of fusion porosity. Electron backscatter diffraction investigations revealed that parameters giving finer microstructure with 〈100〉 crystallographic texture had low crack densities provided they were processed with a low LED. Atom probe tomography elucidated early stages of spinodal decomposition in the as-built condition, where Cr and Al cluster separately. The extent of spinodal decomposition was found to be affected by the LED and the hatch spacing. Samples with low LED and small hatch spacing showed higher degrees of spinodal decomposition. X-ray diffraction residual stress investigations revealed that the residual stress is proportional to the volumetric energy density (VED = P/(v. h. t)). Although low residual stresses can be achieved by using low VED, there is a high risk of lack of fusion. Hence, other parameters such as modified scan strategy, build plate pre-heating and pulsed laser mode, must be further explored to minimize the residual stresses to reduce the strain age cracking susceptibility.
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| 10. |
- Patnaik, Sobhan, et al.
(author)
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Crystallographic characterization of U 2 CrN 3 : A neutron diffraction and transmission electron microscopy approach
- 2023
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In: Nuclear Materials and Energy. - : Elsevier BV. - 2352-1791. ; 35
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Journal article (peer-reviewed)abstract
- In this study, neutron diffraction and transmission electron microscopy (TEM) have been implemented to study the crystallographic structure of the ternary phase U2CrN3 from pellet to nano scale respectively. Recently microstructural evaluation of this ternary phase has been performed for the first time in pellet condition, overcoming the Cr evaporation issue during the conventional sintering process. In this work for the first time, the crystallographic structure of the ordered ternary U2CrN3 phase, stabilized in pellet condition, has been obtained by implementing neutron diffraction. For this study, pellets of the composite material UN with 20 vol% CrN were fabricated by powder metallurgy by mixing UN and CrN powders followed by Spark Plasma Sintering (SPS). TEM was used to investigate the nanoscale structure with a thin lamella of the order of 100–140 nm produced by focused ion beam (FIB). The neutron data revealed the phase composition of the pellet to be primarily 54(8) wt.% U2CrN3, in good agreement with the stoichiometry of starting reagents (UN and CrN powder) and metallographic analysis. Neutron data analysis confirms that all the crystallographic sites in U2CrN3 phase are fully occupied reinforcing the fully stoichiometric composition of this phase, however, the position of the N at the 4i site was found to be closer to the Cr than previously thought. TEM and selected area electron diffraction rendered nano-level information and revealed the presence of nano domains along grain boundaries of UN and U2CrN3, indicating a formation mechanism of the ternary phase, where the phase likely nucleates as nano domains in UN grains from migration of Cr.
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