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In-Pile testing of CrN, TiAIN, and AlCrN coatings on Zircaloy cladding in the Halden reactor - 2016-0011
CrN coating came out as superior and remained completely intact after the irradiation, as evidenced by SEM analysis. Based on these promising results, an in-pile experiment with coated Zircaloy claddings (containing fuel) was performed in the Halden reactor in PWR conditions in 2014. The experimental rig contained four Zircaloy-4-clad fuel rods-three coated (CrN, TiAlN, and AlCrN) and one uncoated. Due to a mechanical deformation of tubes for cooling water within the rig, the fuel rods were insufficiently cooled, resulting in a higher-than-normal cladding temperature. Nevertheless, an SEM examination showed that the CrN coating largely remained intact apart from several local spots where the coating had cracked or disappeared. Underneath the cracked coating, oxide formation was observed in the Zircaloy-4 cladding. The TiAlN and AlCrN coatings both disappeared after the irradiation. (authors)
Novel concept of functional oxide coatings providing enhanced oxidation resistance to Ni-based superalloys
Graphical abstract: - Highlights: • New concept for providing extended oxidation resistance to Ni-based superalloys. • Oxygen-defective nanostructured oxide coatings reduce the oxygen partial pressure at the substrate interface. • Pre-oxidation of the substrate during annealing with the formation of alpha-alumina. • Growth of CeAlO{sub 3} perovskite enhancing the adherence of the ceria top coat. • Microstructural stability of the coating system with no SRZ formation upon exposure. - Abstract: Aluminide-coated Ni-based superalloys are prone to microstructural instabilities during long-term exposure at high temperature with the growth of a secondary reaction zone (SRZ) detrimental from a mechanical viewpoint. This has been since overcome by the use of thermodynamically stable coatings (γ-Ni/γ′-Ni{sub 3}Al). However, additions of Pt and Hf are required to provide the formation of an exclusive α-Al{sub 2}O{sub 3} scale and improved oxidation resistance in cyclic and isothermal regimes. The present work proposes a new coating system that relies on the use of a superficial nanostructured functional oxide providing the establishment of a stable alumina while avoiding SRZ formation. Tailored oxygen-defective and multi-cracked coatings were designed for 2nd generation Ni-based superalloys and generated by electrosynthesis using a water-based solution. Cyclic oxidation tests were carried out at 1100 °C in air and the oxidation properties and the microstructural stability of the coating system were demonstrated.
An elasto-plastic solution for channel cracking of brittle coating on polymer substrate
Not Available
Systems and methods for application of stress corrosion cracking resistant cold spray coatings
Systems and methods for application of stress corrosion cracking resistant cold spray coatings include a method of forming a partial coating on a canister having a perimeter wall with a surface. The method may include identifying a compromised region on the surface of the wall of the canister, and impacting a substantially linear flow of particles of a powder against an area in the compromised region of the surface in a manner effective to cause the particles of the powder to bond to the surface of the wall to produce a coating on the area of the compromised region. The method may also include moving the substantially linear flow in a direction substantially parallel to the surface of the wall to cause the particles to impact an additional area of the compromised region to cause the particles to bond to the surface of the additional area.
The study of crack resistance of TiAlN coatings under mechanical loading and thermal cycle testing
The effect of preliminary ion bombardment of 321 stainless steel substrate on crack resistance of TiAlN coatings at uniaxial tension and thermal cycling is studied. The ion-beam treatment of the substrate is shown to substantially improve the adhesion strength of the coatings that prevents their delamination and spalling under uniaxial tension. The resistance to crack propagation and spalling by the thermal shock is higher in the TiAlN coating deposited onto the substrate subjected to Ti ion bombardment as compared to that in the TiAlN coating deposited onto the initial substrate.
Impact of polymer additives on crack mitigation of rod-coated fuel cell cathode catalyst layers
Cracks in catalyst layers (CLs) are a potential source of long-term failure in a fuel cell membrane electrode assembly (MEA). While modifications to the CL ink formulation can affect the degree of cracking, these changes may lead to lower initial performance than their cracked analogues due to the established link between formulation and performance. In this work, we explored the use of polymeric additives to mitigate CL cracks. Small quantities of poly (acrylic acid), poly (ethylene oxide), poly (methyl methacrylate), or poly (vinyl alcohol) - 5 wt% relative to ionomer mass - were added to the ink prior to its final mixing. Poly (vinyl alcohol) resulted in crack-free CLs, whereas the other polymers resulted in CLs with similar crack percentages as the control CL. Through a combination of transmission electron microscopy, X-ray computed tomography, and infrared spectroscopy, we ascribed the crack-mitigating mechanism of poly (vinyl alcohol) to its ability to hydrogen-bond with Nafion, the ion conducting polymer binder in the catalyst ink. Initial performance of this non-cracked electrode exhibited nearly identical electrochemical behavior to its cracked counterpart, demonstrating that PVA additives successfully reduce cracks while maintaining cell initial performance.
Study of the Crack Resistance of Microarc Oxidation Coatings after Laser Doping with Zirconium Oxide
In this paper we present the results of a study of crack resistance of a microarc oxidation coating (MAO) after laser doping with zirconium oxide. Crack resistance was determined by indentation with imprint imaging using atomic force microscopy. Laser doping with zirconium oxide was established to lead to a significant hardening of the MAO coating. The stress intensity factor increases by a factor of 2.7 while surface damage decreases by a factor of 2 compared with the initial MAO coating.
Intense pulsed light annealing of copper zinc tin sulfide nanocrystal coatings
A promising method for forming the absorber layer in copper zinc tin sulfide [Cu{sub 2}ZnSnS{sub 4} (CZTS)] thin film solar cells is thermal annealing of coatings cast from dispersions of CZTS nanocrystals. Intense pulsed light (IPL) annealing utilizing xenon flash lamps is a potential high-throughput, low-cost, roll-to-roll manufacturing compatible alternative to thermal annealing in conventional furnaces. The authors studied the effects of flash energy density (3.9–11.6 J/cm{sup 2}) and number of flashes (1–400) during IPL annealing on the microstructure of CZTS nanocrystal coatings cast on molybdenum-coated soda lime glass substrates (Mo-coated SLG). The annealed coatings exhibited cracks with two distinct linear crack densities, 0.01 and 0.2 μm{sup −1}, depending on the flash intensity and total number of flashes. Low density cracking (0.01 μm{sup −1}, ∼1 crack per 100 μm) is caused by decomposition of CZTS at the Mo-coating interface. Vapor decomposition products at the interface cause blisters as they escape the coating. Residual decomposition products within the blisters were imaged using confocal Raman spectroscopy. In support of this hypothesis, replacing the Mo-coated SLG substrate with quartz eliminated blistering and low-density cracking. High density cracking is caused by rapid thermal expansion and contraction of the coating constricted on the substrate as it is heated and cooled during IPL annealing. Finite element modeling showed that CZTS coatings on low thermal diffusivity materials (i.e., SLG) underwent significant differential heating with respect to the substrate with rapid rises and falls of the coating temperature as the flash is turned on and off, possibly causing a build-up of tensile stress within the coating prompting cracking. Use of a high thermal diffusivity substrate, such as a molybdenum foil (Mo foil), reduces this differential heating and eliminates the high-density cracking. IPL annealing in presence of sulfur vapor prevented both low- and high-density cracking as well as blistering. However, grain growth was limited even after annealing with 400 flashes. This lack of grain growth is attributed to a difficulty of maintaining high sulfur vapor pressure and absence of alkali metal impurities when Mo foil substrates are used.
Stress corrosion cracking mechanism of cold spray coating on a galvanically similar substrate
Here, the chloride-induced stress corrosion cracking (CISCC) mechanism of cold spray (CS) coating on a galvanically similar substrate is investigated. Arc welded 304L stainless steel (SS) specimens are loaded into four-point bend fixtures, cold sprayed with 304L SS, then immersed in boiling MgCl 2 . Interconnected porosity forms through crevice corrosion along CS splat boundaries, allowing corrosive species to penetrate through the CS layer. Nevertheless, the substrate is resistant to CISCC likely because of compressive stress introduced by peening during CS particle impacts. These findings underscore the importance of residual stress in the environmental degradation of CS coatings or repairs of engineering structures.
Production and characterization of TRISO fuel particles with multilayered SiC
Three distinct composite architectures of silicon carbide (SiC) and pyrocarbon (PyC) were incorporated into the SiC coating layer of tristructural-isotropic (TRISO) nuclear fuel particles. The composite architectures are meant to increase the resistance of SiC coating layer to cracking and fission product attack during operation and accident scenarios. All composite layers were produced using the existing fluidized bed chemical vapor deposition apparatus that is used for production of TRISO fuel particles without modifications. Detailed characterization of the composite microstructure was carried out via optical and electron microscopy. Nano-indentation examination confirms that mechanical properties of the SiC phase was not affected in the composite architectures, however, the resistance to crack propagation in this coating layer was greatly increased in all cases when compared to the reference monolithic coating layer. The stress required to debond the SiC-inner PyC interface in the reference TRISO particles was determined to be ~1 GPa using micropillar compression technique. The high strength may explain the ease of crack propagation from the inner PyC to SiC in the reference design. In the composite architectures, the means of crack deflection were effectively incorporated at this interface. Lastly, finite element analysis of stress evolution in the fuel particles during normal operation with the reference and composite SiC coating layer architectures did not show any significant differences between the variants.
The Effect of Titanium Dioxide (TiO{sub 2}) Nanoparticles on Hydroxyapatite (HA)/TiO{sub 2} Composite Coating Fabricated by Electrophoretic Deposition (EPD)
Composite coatings of Hydroxyapatite (HA) with ceramics, polymers and metals are used to modify the surface structure of implants. In this research, HA/TiO{sub 2} composite coating was fabricated by electrophoretic deposition (EPD) on 316 stainless steel substrate. HA/TiO{sub 2} composite coatings with 5, 10 and 20 wt.% of TiO{sub 2}, deposited at 40 V and 90 s as an optimum condition. The samples coated at this condition led to an adherent, continuous and crack-free coating. The influence of TiO{sub 2} content was studied by performing different characterization methods such as scanning electron microscopy (SEM), energy dispersive x-ray spectroscopy (EDS), corrosion resistance in simulated body fluid (SBF), coating’s dissolution rate in physiological solution and bond strength to the substrate. The results showed that the higher amount of TiO{sub 2} in the composite coating led to increase in bond strength of coating to stainless steel substrate from 3 MPa for HA coating to 5.5 MPa for HA-20 wt.% TiO{sub 2} composite coating. In addition, it caused to reduction of corrosion current density of samples in the SBF solution from 18.92 μA/cm{sup 2} for HA coating to 6.35 μA/cm{sup 2} for HA-20 wt.% TiO{sub 2} composite coating.
Crack mitigation and wear performance of high-strength steel coatings deposited by high-speed laser cladding
This article investigates the fabrication of defect-free Rockit® 606, a high‑carbon, vanadium- and chromium-enriched precipitation-hardening martensitic steel coating, using high-speed laser cladding (HSLC). Compared to conventional laser cladding, HSLC offers higher deposition efficiency, improved coating quality, minimal thermal distortion, and a reduced heat-affected zone. Various HSLC parameters—including laser power, travel speed, powder feed rate, and overlap distance—were optimized to achieve superior coating properties. Microstructural analysis revealed solidification cracks in coatings deposited on carburized steel, regardless of processing parameters. However, preheating the substrate to 250 °C effectively eliminated cracking by reducing thermal gradients. The coatings exhibited a columnar dendritic microstructure, with coarser dendrites near the substrate and finer dendrites towards the surface. Hardness measurements confirmed that all coatings significantly exceeded the industry-specified threshold of 60 HRC, with preheating having minimal effect on overall hardness distribution. Reciprocating sliding wear tests demonstrated a substantial improvement in wear resistance for the defect-free HSLC coatings compared to baseline carburized steel. These findings underscore the potential of HSLC for producing high-performance, wear-resistant coatings suitable for industrial applications.
Tensile cracking of a brittle conformal coating on a rough substrate
This note examines the effect of interfacial roughness on the initiation and growth of channel cracks in a brittle film. A conformal film with cusp-like surface flaws that replicate the substrate roughness is investigated. This type of surface flaw is relatively severe in the sense that stress diverges as the cusp-tip is approached (i.e., there is a power-law stress singularity). For the geometry and range of film properties considered, the analysis suggests that smoothing the substrate could substantially increase the film’s resistance to the formation of the through-the-thickness cracks that precede channel cracking. Furthermore, smoothing the substrate’s surface has a relatively modest effect on the film stress needed to propagate a channel crack.
ORNL Analysis of Leach-Burn-Leach Round-Robin Test Samples
An international round-robin test to examine the consistency in leach-burn-leach (LBL) analysis of tristructural-isotropic- (TRISO-) coated particle fuel was conducted by three research organizations from the Generation IV International Forum member countries of the People’s Republic of China, the Republic of Korea, and the United States of America. Two sets of round-robin test samples were exchanged for analysis. One set of samples consisted of a series of nonuranium-bearing, TRISO-coated zirconium dioxide particles seeded with up to four depleted uranium-bearing, TRISO-coated uranium dioxide (UO 2 ) particles, which had intentionally damaged coating layers to simulate either particles with either exposed-kernel defects (i.e., particles with a cracked TRISO coating that should be detected during preburn leaching) or particles with silicon carbide (SiC) defects (i.e., particles with an intact pyrocarbon coating and a hole in the SiC layer that should be detected during postburn leaching). These simulated samples also contained added powder with known quantities of impurities from a coal standard. The other sample set consisted of representative sublots of UO 2 -TRISO particles fabricated in a production-scale coater, except they all contained depleted uranium instead of enriched uranium. In this report, the methodology used at Oak Ridge National Laboratory to conduct LBL analysis of the round-robin samples is presented, and the general results are summarized.
Butt Laser Welding–Brazing of AZ31 Mg to Nickel-Coated Ti-6Al-4V
Mg and Ti alloy are hard to be bonded due to their huge discrepancy in physical and metallurgical characteristics. As an intermediate element, Ni is feasible for joining of Mg and Ti. The interfacial microstructure and mechanical properties of laser-welded–brazed AZ31 Mg/Ti-6Al-4V joints in butt configuration were investigated with different thicknesses of electrodeposited Ni interlayer. The interfacial reaction products evolved from an ultra-thin Ti{sub 3}Al layer to Ti{sub 2}Ni layer mingled with Ti{sub 3}Al, and more Mg{sub 3}AlNi{sub 2} compounds were produced in the fusion zone (FZ) as Ni coating thickness increased. Slag inclusions and cracks were observed in interfacial layer when coating thickness exceeded 2.5 μm. The quantity of Mg{sub 3}AlNi{sub 2} and the thickness of interfacial layer decreased from the top to bottom of groove of the same joint owing to high thermal gradient during laser welding. The chemical potential of Al and Ni indicated that Al-Ti reaction product was produced more easily than Ni-Ti in 0.001Mg-(Ni-Al-Ti) system. The thermodynamic calculation results of Gibbs free energy suggested the preferential formation Ti-Al phase and Ti-Ni phase along the interface while the Mg-Al-Ni ternary phase in the FZ. Fracture loads of joints increased first followed by a decline with the increase in coating thickness. The joint fractured at the Mg base metal, reaching a maximum value of 3900 N with the Ni coating thickness of 1.5 μm. In the case of using thinner or thicker Ni coating, crack propagated along the interface due to the insufficient metallurgical bonding or defects existed in the interfacial layer. The characteristic of fracture surface changed from the tear ridges and terraces to river pattern when interfacial failure occurred.
A comparison of He and Ne FIB imaging of cracks in microindented silicon nitride
Highlights: • Silicon nitride was successfully imaged with helium and neon ion microscopy. • Indent-induced cracking was resolved on conductively-coated and uncoated samples. • Cracking was found to be primarily intergranular in nature. • The grain microstructure was most visible on the carbon-coated sample. • For the carbon-coated sample, localized charging was observed along crack pathways. - Abstract: Helium ion microscopy (HIM) offers potential as a high spatial resolution technique for imaging insulating samples that are susceptible to charging artifacts. In this study helium and neon ion microscopy are used to image cracking in microindented samples of the non-conductive ceramic silicon nitride. The crack morphology of radial cracks emanating from the microindentations has been characterized for two different compositions of silicon nitride, with and without conductive coatings. Gold coating enhances crack edge contrast, but masks grain contrast for both He and Ne ion-induced secondary electron (ISE) imaging. Carbon coating enables the crystalline and glassy phases to be distinguished, more clearly with Ne-ISE, and the cracking pathway is found to be primarily intergranular. Zones of <100 nm diameter depleted ion-induced secondary electron emission along the crack paths are identified, consistent with charging ‘hotspots’.