Plasma Focused Ion Beam Research Articles

Development of a new, fully automated system for electron backscatter diffraction (EBSD)-based large volume three-dimensional microstructure mapping using serial sectioning by mechanical polishing, and its application to the analysis of special boundaries in 316L stainless steel.

We report the development of a fully automatic large-volume 3D electron backscatter diffraction (EBSD) system (ELAVO 3D), consisting of a scanning electron microscope (ZEISS crossbeam XB 1540) with a dedicated sample holder, an adapted polishing automaton (Saphir X-change, QATM), a collaborative robotic arm (Universal Robots UR5), and several in-house built devices. The whole system is orchestrated by an in-house designed software, which is also able to track the process and report errors. Except for the case of error, the system runs without any user interference. For the measurement of removal thickness, the samples are featured with markers put on the perpendicular lateral surface, cut by plasma focused ion beam (PFIB) milling. The individual effects of both 1μm diamond suspension and oxide polishing suspension polishing were studied in detail. Coherent twin grain boundaries (GBs) were used as an internal standard to check the removal rates measured by the side markers. The two methods for Z-spacing measurements disagreed by about 10%, and the inaccurate calibration of the PFIB system was found to be the most probable reason for this discrepancy. The angular accuracy of the system was determined to be ∼2.5°, which can be significantly improved with more accurate Z-spacing measurements. When reconstructed grain boundary meshes are sufficiently smoothed, an angular resolution of ±4° is achieved. In a 3D EBSD dataset of a size of 587 × 476 × 72μm3, we focused on the investigation of coincidence site lattice ∑9 GBs. While bearing predominantly a pure tilt character, ∑9 GBs can be categorized into three groups based on correlative 3D morphologies and crystallography.

Effect of dentine site on resin and cement adaptation tested using X-ray and electron microscopy to evaluate bond durability and adhesive interfaces.

Glass ionomer (GI) cements and self-etch (SE) or universal adhesives after etching (ER) adapt variably with dentine. Dentine characteristics vary with depth (deep/shallow), location (central/peripheral), and microscopic site (intertubular/peritubular). To directly compare adhesion to dentine, non-destructive imaging and testing are required. Here, GI, ER, and SE adapted at different dentine depths, locations, and sites were investigated using micro-CT, xenon plasma focused ion beam scanning electron microscopy (Xe PFIB-SEM), and energy dispersive X-ray spectroscopy (EDS). Extracted molars were prepared to deep or shallow slices and treated with the three adhesives. Micro-CT was used to compare changes to air volume gaps, following thermocycling, and statistically analysed using a quantile regression model and Fisher's exact test. The three adhesives performed similarly across dentine depths and locations, yet no change or overall increases and decreases in gaps at all dentine depths and locations were measured. The Xe PFIB-SEM-milled dentine-adhesive interfaces facilitated high-resolution characterization, and element profiling revealed variations across the tooth-material interfaces. Dentine depth and location had no impact on adhesive durability, although microscopic differences were observed. Here we demonstrate how micro-CT and Xe PFIB-SEM can be used to compare variable dental materials without complex multi-stage specimen preparation to minimize artefacts.

How innovations in methodology offer new prospects for volume electron microscopy

Detailed knowledge of biological structure has been key in understanding biology at several levels of organisation, from organs to cells and proteins. Volume electron microscopy (volume EM) provides high resolution 3D structural information about tissues on the nanometre scale. However, the throughput rate of conventional electron microscopes has limited the volume size and number of samples that can be imaged. Recent improvements in methodology are currently driving a revolution in volume EM, making possible the structural imaging of whole organs and small organisms. In turn, these recent developments in image acquisition have created or stressed bottlenecks in other parts of the pipeline, like sample preparation, image analysis and data management. While the progress in image analysis is stunning due to the advent of automatic segmentation and server‐based annotation tools, several challenges remain. Here we discuss recent trends in volume EM, emerging methods for increasing throughput and implications for sample preparation, image analysis and data management.

(Digital Presentation) Advances in Cryo-Atom Probe Tomography Studies on Formation of Nanoporous Metals By Dealloying

The selective removal of a less noble (more chemically active) metal from a mixture of 2–3 metals can yield a bicontinuous, open-pore, 3D nanoporous metal (NPM), that is rich in the more noble metal(s)1. NPMs have been successfully developed by the intelligent use of the conventionally-undesired dealloying corrosion. The excellent properties of NPMs are attributed to the surface area-to-volume ratio, and high curvature of nanoligament surfaces 2,3 . Experimental work on NPMs revealed the formation of uniformly nanoporous structure by dealloying AgAu alloy in nitric acid, a method still widely used until today for making nanoporous gold (NPG). This dealloying process is complex: the selective dissolution of the less-noble element should lead to the creation of surface vacancies or adatoms, which migrate across the surface to form surface roughening features, and thus assisting the migration of the residual more-noble atoms, leading to island growth4.Ex-situ characterization cannot fully explain some intricate details at the dealloying interface and at the surface of the formed nanoligaments. Gaining insight into initial stages of dealloying, and the inherent competition between surface roughening from the dissolution of silver atoms, and surface smoothening from surface diffusion of gold atoms5, can only be done effectively by monitoring the changes occurring at the surfaces of alloys in-situ. Several notable in-situ methods were used to characterize formation of NPMs, such as TEM 6, often limited by the 2D nature of the analysis. Also, synchrotron-based methods such as X-ray nanotomography 7 and neutron scattering 8 were limited by resolution and lack of compositional contrast. APT is a powerful technique that provides 3D characterization9 and near-atomic-scale compositional analysis of materials, and could complement the abovementioned suite of techniques, yet the analysis of nanoporous structure comes with challenges.Aiming to develop a universal method for probing corrosion systems by APT, the concept of embedding frozen solutions in corroded systems was developed and reported in a recent reporting 10 of analyzing NPMs along with frozen water-based solutions. This involved the joint use of an ensemble of equipment and techniques that connect the frozen liquid to the atom probe, including a plasma-focused ion beam (PFIB) where the preparation of APT specimens uses a cryostage, and transfer of the frozen sample through ultra-high-vacuum suitcase11. This paved the way for many advances in characterization of corrosion processes, as the possibility of freezing corrosion reactions for APT (now known as cryo-APT) arises. Here, we further develop cryo-APT to probe into the mechanisms of dealloying in AgAu and how that leads to the formation of NPG using our in-situ approach. Nanoligament structure will be correlated with dealloying conditions by making observations at the solid-liquid interface in 3D. References Newman, R. C. 2.05 - Dealloying. in Shreir’s Corrosion (eds. Cottis, B. et al.) 801–809 (Elsevier, 2010).Zielasek, V. et al. Gold Catalysts: Nanoporous Gold Foams. Angew. Chemie Int. Ed. 45, 8241–8244 (2006).Xue, Y., Markmann, J., Duan, H., Weissmüller, J. & Huber, P. Switchable imbibition in nanoporous gold. Nat. Commun. 5, (2014).Forty, A. J. & Rowlands, G. A possible model for corrosion pitting and tunneling in noble-metal alloys. Philos. Mag. A Phys. Condens. Matter, Struct. Defects Mech. Prop. (1981) doi:10.1080/01418618108239399.Erlebacher, J., Newman, C. & Sieradzki, K. Fundamental physics and chemistry of nanoporosity evolution during dealloying. RSC Nanosci. Nanotechnol. 11–29 (2012) doi:10.1039/9781849735285-00011.Liu, P. et al. Dealloying Kinetics of AgAu Nanoparticles by In Situ Liquid-Cell Scanning Transmission Electron Microscopy. Nano Lett. 20, 1944–1951 (2020).Chen-Wiegart, Y. C. K. et al. In situ imaging of dealloying during nanoporous gold formation by transmission X-ray microscopy. Acta Mater. 61, 1118–1125 (2013).Corcoran, S. G., Wiesler, D. G. & Sieradzki, K. An in Situ Small Angle Neutron Scattering Investigation of Ag0.7Au0.3 Dealloying Under Potential Control. MRS Proc. 451, 93 (1996).Gault, B., Moody, M. P., Cairney, J. M. & Ringer, imon P. Atom Probe Microscopy. vol. 160 (Springer New York, 2012).El-Zoka, A. A. et al. Enabling near-atomic–scale analysis of frozen water. Sci. Adv. 6, eabd6324 (2020).Stephenson, L. T. et al. The LaplacE project: An integrated suite for preparing and transferring atom probe samples under cryogenic and UHV conditions. PLoS One (2018) doi:10.1371/journal.pone.0209211. Figure 1

Plasma Focused Ion Beam Tomography for Accurate Characterization of Black Silicon Validated by Full Wave Optical Simulation

AbstractBlack silicon (BSi) is a branch of silicon material whose surface is specially processed to a micro/nanoscale structure, which can achieve ultra‐low reflectance or ultra‐high electrochemical reactivity. The diversity and complex surface structures of BSi make it challenging to commercialize BSi devices. Modeling and simulation are commonly used in the semiconductor industry to help in better understanding the material properties, predict the device performance, and provide guidelines for fabrication parameters’ optimization. The biggest challenge for BSi device modeling and simulation is obtaining accurate input surface morphological data. In this work, the 3D models of challenging BSi textures are compared as obtained by atomic force microscopy (AFM) and plasma focused ion beam (PFIB) tomography techniques. In previous work, the PFIB tomography workflow toward the application of surface topography is optimized. In this work, the 3D models obtained from both AFM and PFIB are comprehensively compared, by using the surface models as inputs for finite‐difference time‐domain‐based optical simulation. The results provide strong evidence that PFIB tomography is a better choice for characterizing highly roughened surface such as BSi and provides surface 3D models with better reliability and consistency.

Advanced characterisation of 3D structure and porosity of ordinary portland cement (OPC) mortar using plasma focused ion beam tomography and X-ray computed tomography.

The visualisation and quantification of pore networks and main phases have been critical research topics in cementitious materials as many critical mechanical and chemical properties and infrastructure reliability rely on these 3D characteristics. In this study, we realised the mesoscale serial sectioning and analysis up to ∼80 μm by ∼90 μm by ∼60 μm on portland cement mortar using plasma focused ion beam (PFIB) for the first time. The workflow of working with mortar and PFIB was established applying a prepositioned hard silicon mask to reduce curtaining. Segmentation with minimal human interference was performed using a trained neural network, in which multiple types of segmentation models were compared. Combining PFIB analysis at microscale with X-ray micro-computed tomography, the analysis of capillary pores and air voids ranging from hundreds of nanometres (nm) to millimetres (mm) can be conducted. The volume fraction of large capillary pores and air voids are 11.5% and 12.7%, respectively. Moreover, the skeletonisation of connected capillary pores clearly shows fluid transport pathways, which is a key factor determining durability performance of concrete in aggressive environments. Another interesting aspect of the FIB tomography is the reconstruction of anhydrous phases, which could enable direct study of hydration kinetics of individual cement phases.

Using Xe Plasma FIB for High-Quality TEM Sample Preparation.

A direct comparison between electron transparent transmission electron microscope (TEM) samples prepared with gallium (Ga) and xenon (Xe) focused ion beams (FIBs) is performed to determine if equivalent quality samples can be prepared with both ion species. We prepared samples using Ga FIB and Xe plasma focused ion beam (PFIB) while altering a variety of different deposition and milling parameters. The samples’ final thicknesses were evaluated using STEM-EELS t/λ data. Using the Ga FIB sample as a standard, we compared the Xe PFIB samples to the standard and to each other. We show that although the Xe PFIB sample preparation technique is quite different from the Ga FIB technique, it is possible to produce high-quality, large area TEM samples with Xe PFIB. We also describe best practices for a Xe PFIB TEM sample preparation workflow to enable consistent success for any thoughtful FIB operator. For Xe PFIB, we show that a decision must be made between the ultimate sample thickness and the size of the electron transparent region.

A novel pathway for multiscale high-resolution time-resolved residual stress evaluation of laser-welded Eurofer97.

The plasma-facing components of future fusion reactors, where the Eurofer97 is the primary structural material, will be assembled by laser-welding techniques. The heterogeneous residual stress induced by welding can interact with the microstructure, resulting in a degradation of mechanical properties and a reduction in joint lifetime. Here, a Xe+ plasma focused ion beam with digital image correlation (PFIB-DIC) and nanoindentation is used to reveal the mechanistic connection between residual stress, microstructure, and microhardness. This study is the first to use the PFIB-DIC to evaluate the time-resolved multiscale residual stress at a length scale of tens of micrometers for laser-welded Eurofer97. A nonequilibrium microscale residual stress is observed, which contributes to the macroscale residual stress. The microhardness is similar for the fusion zone and heat-affected zone (HAZ), although the HAZ exhibits around ~30% tensile residual stress softening. The results provide insight into maintaining structural integrity for this critical engineering challenge.

Direct Observation of PFIB-Induced Clustering in Precipitation-Strengthened Al Alloys by Atom Probe Tomography.

The effect of sample preparation on a pre-aged Al–Mg–Si–Cu alloy has been evaluated using atom probe tomography. Three methods of preparation were investigated: electropolishing (control), Ga+ focused ion beam (FIB) milling, and Xe+ plasma FIB (PFIB) milling. Ga+-based FIB preparation was shown to introduce significant amount of Ga contamination throughout the reconstructed sample (≈1.3 at%), while no Xe contamination was detected in the PFIB-prepared sample. Nevertheless, a significantly higher cluster density was observed in the Xe+ PFIB-prepared sample (≈25.0 × 1023 m−3) as compared to the traditionally produced electropolished sample (≈3.2 × 1023 m−3) and the Ga+ FIB sample (≈5.6 × 1023 m−3). Hence, the absence of the ion milling species does not necessarily mean an absence of specimen preparation defects. Specifically, the FIB and PFIB-prepared samples had more Si-rich clusters as compared to electropolished samples, which is indicative of vacancy stabilization via solute clustering.

Large volume tomography using plasma FIB-SEM: A comprehensive case study on black silicon

The xenon plasma focused ion beam and scanning electron microscopy (PFIB-SEM) system is a promising tool for 3D tomography of nano-scale materials, including nanotextured black silicon (BSi), whose topography is difficult to measure with conventional microscopy techniques. Advantages of PFIB-SEM include high material removal rates, precise control of milling parameters and automated slice-and-view procedures. However, there is no universal sample preparation procedure nor is there an established ideal workflow for the PFIB-SEM slice-and-view process. This work demonstrates that specimen preparation, including the orientation of the volume of interest, is critical for the quality of the final reconstructed 3D model. It thoroughly explores three unique configurations incrementally optimized for higher total throughput. All three sampling configurations are applied to a resin-embedded BSi sample to determine the most favourable workflow and highlight each approach's advantages and disadvantages. The reconstructed 3D models of the BSi surface obtained are shown to be qualitatively closer to the topography measured directly by SEM. The height distribution data extracted from the rendered 3D models reveal a higher structure depth compared to that obtained from an atomic force microscopy measurement. Furthermore, the work demonstrates how samples with different rigidity react to long-term ion-beam interaction, as both amorphous (resin) and crystalline (Si) material is present in the tested specimen. This study improves the understanding of sample-beam interaction and broadens the utility of the 3D PFIB-SEM for more complicated sample structures.

Coatings for Core–Shell Composite Micro‐Lattice Structures: Varying Sputtering Parameters

Magnetron sputtering has garnered increased attention as a versatile deposition method for generating novel core–shell composite nano‐ and micro‐lattice materials spanning a wide range of properties and functionalities. Sputtering offers an expansive material workspace consisting of a wide range of ceramics, single‐element metals, and alloy systems. However, achieving uniform coatings on such fine‐featured structures remains a challenge. Thus, herein, a foundational assessment of various sputtering configurations, cathode geometries, and deposition parameters is carried out to investigate their implications on the coating thickness and uniformity of 3D micro‐lattice scaffolds. Specifically, tetrahedral‐truss structures fabricated via direct laser writing are coated by leveraging planar and inverted cylindrical magnetron cathodes at select deposition rates, sputtering powers, and Ar working pressures. Both plasma focused ion beam and microtome sectioning techniques are employed to evaluate the cross section of individual struts and assess overall uniformity. Overall, the influence of key sputtering factors on the design and development of core–shell composite nano‐ and micro‐lattice materials is highlighted and a pathway for future sputter coating optimization on these complex structures is provided.

Fracture properties of porous yttria-stabilized zirconia under micro-compression testing

Micro-compression tests were carried out on pillars of 60 μm in diameter, milled by plasma focused ion beam in porous Yttria-Stabilized Zirconia (YSZ) pellets. The fracture properties were determined over a wide range of porosities (33 %–63 %) for 8YSZ and at a given pore volume fraction of 63 % for 3YSZ. The mechanical properties determined from testing were reproducible thanks to the homogeneity of the microstructures. The Young’s modulus was estimated as a function of the porosity from the unloading curve of tests stopped before fracture. The experiments conducted until the total rupture allowed measuring the compressive fracture strength, which was found to decrease when increasing the porosity. Specimen tested and unloaded just before the total fracture were cross-sectioned by focused ion beam - scanning electron microscope. A transition was detected from a brittle behavior, with macro-cracks parallel to the direction of solicitation, to a diffuse damage with micro-cracks, when increasing the porosity.

Recent Developments in Femtosecond Laser-Enabled TriBeam Systems

Streams of multimodal three-dimensional (3D) and four-dimensional (4D) data are revolutionizing our ability to design and predict the behavior of a broad array of advanced materials systems. Over the last 10 years, a new 3D imaging platform consisting of a femtosecond (fs) pulsed laser coupled with a focused ion beam scanning electron microscope (FIB SEM) has been developed by UC Santa Barbara in collaboration with Thermo Fisher Scientific (formerly FEI). The femtosecond-laser-enabled FIB SEM, called the TriBeam, has become one of the only 3D serial sectioning methods available that can gather millimeter-scaled multimodal datasets at sub- $$\mu $$ m voxel resolutions; these length scales are critical for many materials problems. Multimodal chemical, crystallographic, and morphological information can be gathered rapidly on a layer-by-layer basis and reconstructed in 3D. Large (gigabyte to terabyte scale) 3D datasets have been generated for a broad array of materials systems, including metallic alloys, ceramics, biomaterials, polymer- and ceramic-matrix composites, and semiconductors. The research tasks performed have resulted in a completely new design, operating with a dual-wavelength femtosecond-pulsed laser on a plasma focused ion beam (PFIB) platform.

3D electron backscatter diffraction characterization of fine α titanium microstructures: collection, reconstruction, and analysis methods

3D electron backscatter diffraction (3D-EBSD) is a method of obtaining 3-dimensional crystallographic data through serial sectioning. The recent advancement of using a Xe+ plasma focused ion beam for sectioning along with a complementary metal-oxide semiconductor based EBSD detector allows for an improvement in the trade-off between volume analyzed and spatial resolution over most other 3D characterization techniques. Recent publications from our team have focused on applying 3D-EBSD to understand microstructural phenomena in Ti-6Al-4V microstructures as a function of electron beam scanning strategies in electron beam powder bed fusion additive manufacturing. The microstructures resulting from this process have fine features, with α laths as small as 1 μm interwoven in a highly complex fashion, presenting a significant challenge to characterize. Over the course of these fundamental works, we have developed best-practice 3D-EBSD collection protocols and advanced methods for 3D data reconstruction and analysis of such microstructures which remain unpublished. These methods may be of interest to the 3D materials characterization community, especially considering the lack of standard commercial software tools. Thus, the current paper elaborates on the methods and analysis used to characterize fine titanium microstructures using 3D-EBSD and presents a detailed description of the new algorithms developed for probing the unique features therein. The new analyses include algorithms for identifying intervariant boundary types, classifying three-variant clusters, assigning grains to variants, and quantifying interconnectivity of branched α platelets.

Degradation Diagnostics from the Subsurface of Lithium‐Ion Battery Electrodes

Despite the long‐established rocking‐chair theory of lithium‐ion batteries (LIBs), developing novel characterization methodology with higher spatiotemporal resolution facilitates a better understanding of the solid electrolyte interphase studies to shape the reaction mechanisms. In this work, we develop a Xenon ion plasma focused ion beam (Xe+ PFIB)‐based characterization technique to probe the cross‐sectional interface of both ternary cathode and graphite anode electrodes, with the focus on revealing the chemical composition and distribution underneath the electrode surface by in‐depth analysis of secondary ions. Particularly, the lithium fluoride is detected in the pristine cathode prior to contact with the electrolyte, reflecting that the electrode degradation is in the form of the loss of lithium inventory during electrode preparation. This degradation is related to the hydrolysis of the cathode material and the decomposition of the PVDF binder. Through the quantitative analysis of the transition‐metal degradation products, manganese is found to be the dominant element in the newly formed inactive fluoride deposition on the cathode, while no transition metal signal can be found inside the anode electrode. These insights at high resolution implemented via a PFIB‐based characterization technique not only enrich the understanding of the degradation mechanism in the LIBs but also identify and enable a high‐sensitivity methodology to obtain the chemical survey at the subsurface, which will help remove the capacity‐fade observed in most LIBs.

Formation and 3D morphology of interconnected α microstructures in additively manufactured Ti-6Al-4V

Three-dimensional characterization methods, such as 3D electron backscatter diffraction (3D-EBSD), have been used to reveal phase transformation and microstructural evolution mechanisms in multi-phase materials such as steel or titanium alloys. While 3D techniques have enabled many findings in steels, fine dual phase microstructures in titanium alloys such as the basketweave structure have been challenging to resolve. Now, advances in 3D-EBSD methods using sectioning with a plasma focused ion beam have allowed in-depth analyses of fine α microstructures. We apply 3D-EBSD to investigate the microstructures formed in Ti-6Al-4V by electron powder bed fusion (E-PBF) using different scanning strategies. Basketweave, acicular, and colony microstructures are produced from linear, Dehoff, and random scanning strategies, respectively. Different types of 3D interconnectivity were revealed in each microstructure including within clusters of platelets in the basketweave microstructure, within a grain boundary allotriomorph in the acicular microstructure, and between platelets in colonies. These observations are discussed in terms of the formation mechanisms of interconnectivity, including sympathetic nucleation, impingement, and morphological instability. Morphological instability was found to potentially play a role in both the basketweave and colony structures while the interconnectivity in the acicular structure likely forms via sympathetic nucleation or impingement. This information allows for a more complete description of the phase evolution of Ti-6Al-4V during thermal cycling in E-PBF than previously available and represents new insights into the complex branching reported in different titanium microstructures.

Expanding the Capability of Xe Plasma Focused Ion Beam Sample Preparation for Transmission Electron Microscopy

Expanding the Capability of Xe Plasma Focused Ion Beam Sample Preparation for Transmission Electron Microscopy

Fracture of Porous Ceramics: Application to the Mechanical Degradation of Solid Oxide Cell During Redox Cycling

Solid Oxide Cell (SOC) is a high-temperature electrochemical device that can be operated in both fuel and electrolysis modes. It is constituted of a dense electrolyte in Yttria Stabilized Zirconia (YSZ) sandwiched between two porous electrodes. The hydrogen electrode is classically made of a cermet composed of Nickel and YSZ (Ni-YSZ). Because of system failures in operation (e.g. a fuel shortage or air re-introduction during the system shutdown), the Nickel is liable to be re-oxidized inducing its volume expansion. The Ni swelling within the cermet leads to a mechanical damage in the YSZ backbone [1] resulting in a degradation of the overall cell performances [2]. Therefore, it is still required to enhance the hydrogen electrode robustness for a higher redox tolerance. For this purpose, it is essential to predict accurately the formation and distribution of micro-cracks in the YSZ network during the re-oxidation. Nevertheless, the modeling of the initiation and propagation of cracks in complex microstructures of porous ceramics is still a subject of investigation. Moreover, there is also a lack of data on fracture properties for the porous YSZ material. In this frame, the present study was focused to propose a relevant model for the initiation and the growth of cracks in porous ceramics in order to simulate the fracture induced by Ni re-oxidation. For this purpose, a coupled experimental and modeling approach has been adopted (Fig.1). For the experimental part, the mechanical characterizations have been performed on thin YSZ membranes of different porosities representative of SOC microstructures. The compression test has been chosen as it generates a quasi-uniform stress field in the tested samples. To this end, micro-pillars of few tens of micro-meters in section have been milled in the YSZ membrane using a xenon plasma focused ion beam. For each investigated porosity, the compressive fracture strength has been measured on several pillars. The tested samples have been carefully characterized to assess the damage in the microstructure. As expected, the compressive strength was found to decrease with increasing the porosity. Moreover, a transition has been observed from a brittle behaviour at low porosity towards a local damage at high porosity [3]. All these experimental data have been used to validate a numerical tool to simulate the fracture in porous microstructure. In this study, a model based on the Phase Field Method (PFM) has been developed. In this approach, the crack is modeled implicitly through a smooth scalar damage variable and its width is controlled by a length scale parameter. Therefore, this method is well adapted to solve the fracture problem in complex and heterogeneous materials since it is mesh independent. The implemented model corresponds to the one proposed by C. Miehe et al. [4] who proposed a staggered scheme for the numerical resolution. A special attention has been paid in this work to evaluate the model capability to accurately predict the crack initiation for porous electrode material. For this purpose, the results of the PFM simulations have been compared to the mixed criterion proposed by D. Leguillon [5]. The study has been conducted on notched samples with different opening angles and for macro-cracks blunted by different cavity sizes. It has been highlighted that the two approaches provide consistent predictions for the crack initiation. Moreover, it has been checked that the PFM model is able to reproduce accurately the expected decrease of the fracture toughness when increasing the material porosity. Once these studies completed, the PFM model has been used to simulate the micro-compression test using a multiscale approach. It has been found that the model is able to reproduce correctly the decrease of the measured compressive fracture strength with the sample porosity. Moreover, the distribution of cracks in the simulations has enabled analysing the transition from a brittle to a local damage detected during the experiments. The validated model has been applied to simulate the fracture induced by the Ni re-oxidation. The repartition and density of micro-cracks in the YSZ backbone has been computed during the Ni reoxidation and the results have been confronted with an available tomographic data set. Finally, the impact on the cermet redox tolerance of the Yttrium content in YSZ has been discussed thanks to the modelling. [1] Faes, A. et al. J. Power Sources 193, 55–64. [2] Laurencin, J. et al. J. Power Sources 192, 344–352. [3] Meille, S. Et al . J. Eur. Ceram. Soc. 32, 3959–3967. [4] Miehe, C. et al. Comput. Methods Appl. Mech. Eng. 199, 2765–2778. [5] Leguillon, D. J. Mech. – A/Solids 21, 61–72. Figure 1

Strong magnon–photon coupling with chip-integrated YIG in the zero-temperature limit

The cross-integration of spin-wave and superconducting technologies is a promising method for creating novel hybrid devices for future information processing technologies to store, manipulate, or convert data in both classical and quantum regimes. Hybrid magnon–polariton systems have been widely studied using bulk Yttrium Iron Garnet (Y3Fe5O12, YIG) and three-dimensional microwave photon cavities. However, limitations in YIG growth have, thus far, prevented its incorporation into CMOS compatible technologies, such as high-quality factor superconducting quantum technology. To overcome this impediment, we have used Plasma Focused Ion Beam (PFIB) technology—taking advantage of precision placement down to the micrometer scale—to integrate YIG with superconducting microwave devices. Ferromagnetic resonance has been measured at milliKelvin temperatures on PFIB-processed YIG samples using planar microwave circuits. Furthermore, we demonstrate strong coupling between superconducting resonators and YIG ferromagnetic resonance modes by maintaining reasonably low loss while reducing the system down to the micrometer scale. This achievement of strong coupling on-chip is a crucial step toward fabrication of functional hybrid quantum devices from spin-wave and superconducting components.

Microstructural optimization and anti-wear performance of supersonic atmospheric plasma sprayed nickel based self-lubricating coatings under heavy load

The aim of this work is to explore high-property nickel based self-lubricating coatings to meet the challenge of the increasing demand of heavy load wear condition. Thus, a series of Ni-MoS2/graphite coatings were designed and prepared by supersonic atmospheric plasma spraying. The microstructural evolution of lubricating phases was systematically studied by plasma focused ion beam (FIB) and field-emission transmission electron microscopy (FE-TEM). The results suggested that the lubricating phases, such as graphite and MoS2, can transform into some independent lamellar structures due to their low binding energy. MoS2 phase was easy to decompose into nanoscale Mo with preferred (110) crystal plane at high temperatures, leading to the decrease of self-lubrication property of coatings. Due to the rapid formation of the graphite-dominated debris transfer layer, the coating with approximately 19 vol% graphite showed the longest friction time and the lowest wear rate. The graphite with a large size range (1–60 μm) not only effectively compensated the loss of MoS2 caused by the thermal decomposition, but also improved the density and fracture toughness of coatings. In addition, the content of monoclinic β-MoO3 was significantly decreased with the addition of graphite, which further improved the tribological properties of the coatings. This work provided an in-depth understanding for the development of composite coatings with high anti-wear performance under heavy load.