Intercalated layered materials offer distinctive properties and serve as precursors for important two-dimensional (2D) materials. However, intercalation of non-van der Waals structures, which can expand the family of 2D materials, is difficult. We report a structural editing protocol for layered carbides (MAX phases) and their 2D derivatives (MXenes). Gap-opening and species-intercalating stages were respectively mediated by chemical scissors and intercalants, which created a large family of MAX phases with unconventional elements and structures, as well as MXenes with versatile terminals. The removal of terminals in MXenes with metal scissors and then the stitching of 2D carbide nanosheets with atom intercalation leads to the reconstruction of MAX phases and a family of metal-intercalated 2D carbides, both of which may drive advances in fields ranging from energy to printed electronics.

Out-of-plane chemically ordered transitionmetal boride(o-MAB) phases, Ta4M & DPRIME;SiB2 (M & DPRIME; = V, Cr), and a structurally equivalent disordered solidsolution MAB phase, Ta4MoSiB2, are synthesized.DFT calculations are used to examine the dynamic stability, elasticproperties, and electronic density states of the MAB phases. We report on the synthesis of computationally predictedout-of-planechemically ordered transition metal borides labeled o-MAB phases, Ta4M & DPRIME;SiB2 (M & DPRIME; =V, Cr), and a structurally equivalent disordered solid solution MABphase Ta4MoSiB2. The boride phases were preparedusing solid-state reaction sintering of the constituting elements.High-resolution scanning transmission electron microscopy along withRietveld refinement of the powder-X-ray diffraction patterns revealedthat the synthesized o-MAB phases Ta4CrSiB2 (98 wt % purity) and Ta4VSiB2 (81 wt% purity) possess chemical ordering with Ta preferentially residingin the 16l position and Cr and V in the 4c position, whereas Ta4MoSiB2 (46wt % purity) was concluded to form a disordered solid solution. Densityfunctional theory (DFT) calculations were used to investigate thedynamic stability, elastic properties, and electronic density statesfor the MAB phases, confirming the stability and suggesting the boridesbased on Cr and Mo to be stiffer than those based on V and Nb.

Structural defects are detrimental to the efficiency and quality of optoelectronic semiconductor devices. In this work, we study InGaN platelets with a quantum well structure intended for nano-LEDs emitting red light and how their optical properties, measured with cathodoluminescence, relate to the corresponding atomic structure. Through a method of spectroscopy-thinning-imaging, we demonstrate in plan-view how stacking mismatch boundaries intersect the quantum well in a pattern correlated with the observed diminished cathodoluminescence intensity. The results highlight the importance of avoiding stacking mismatch in small LED structures due to the relatively large region of non-radiative recombination caused by the mismatch boundaries.

c-TiAlN/h-Cr2N multilayer thin films, with modulation period lambda of 10 nm, 20 nm, and 30 nm and different Cr2N/lambda thickness ratios (25 %, 50 % and 75 %), were deposited on c-plane sapphire using reactive DC magnetron sputtering. All multilayers exhibited preferred orientation [Cr2N(0001)/ TiAlN(111)](x), regardless of the modulation period and thickness ratios. X-ray diffraction f-scans revealed an influence of the Cr2N layer thickness on the overall orientation quality of the multilayer, where the thicker the Cr2N layer the higher orientation quality. Atomically resolved high-angle annular dark-field scanning transmission electron microscopy revealed well defined and homogeneous atom stacking in the Cr2N layers. In contrast, the cubic TiAlN layer was found to be composed of coherent cubic AlN-rich and TiN-rich regions. Additionally, the TiAlN layers were found with a higher density of grain boundaries compared to the Cr2N layers. Mechanical properties evaluation revealed that the film with a 20 nm period and 75 % Cr2N thickness ratio exhibited the highest hardness of 27.11 +/- 0.72 GPa and an reduced elastic modulus of 349.1 +/- 6.84 GPa. The hardness increased as the thickness of Cr2N increased, until reaching 10 nm, after which it remained at a high level (similar to 25 GPa).

Studies of single crystal artificial superlattices (SLs) of transition-metal (TM) diborides, which is instru- mental to understand hardening mechanisms at nanoscale, is lacking. Here, CrBx/TiBy (0001) diboride SLs [x,y E 1.7-3.3] are grown epitaxially on Al2O3(0001) substrates by direct-current magnetron sputter epitaxy. Growth conditions for obtaining well-defined SLs with good interface quality are found at 4 mTorr Ar pressure and 600 degrees C. 1 -mu m-thick SL films deposited with modulation periods A between 1 and 10 nm, and A=6 nm SLs with TiBy-to-A layer thickness ratios F ranging from 0.2 to 0.8 are studied. SLs with A=6 nm and F in the range of 0.2-0.4, with a near stoichiometric B/TM ratio, exhibit the high- est structural quality. The effects of F and stoichiometries (B/TM ratio) on the distribution of B in the SL structures are discussed. By increasing the relative thickness of TiBy, the crystalline quality of SLs starts to deteriorate due to B segregation in over-stoichiometric TiBy, resulting in narrow epitaxial SL columnar growth with structurally-distorted B-rich boundaries. Moreover, increasing the relative thickness of under-stoichiometric CrBx enhances the SL quality and hinders formation of B-rich boundaries. The SLs are found to exhibit hardness values in the range of 29-34 GPa.(c) 2023 The Author(s). Published by Elsevier Ltd. This is an open access article under the CC BY license (http://creativecommons.org/licenses/by/4.0/).

Nanocomposites have been long exploited for achieving balanced material properties. Here, we synthesized nominal (Mg2Sn0.85Sb0.15)1-x-(Mg3Sb2)x (x = 0-0.15) nano-composites, achieving a significant reduction of the lattice thermal conductivity of Mg2Sn0.85Sb0.15 from 2.03 Wm-1K-1 to 1.38 Wm-1K-1 due to phonon scattering by VMg point defects, Mg3Sb2 nanoparticles, and heterogeneous interfaces. Hence, a significantly enhanced thermoelectric figure of merit, ZT, is achieved. At 773 K, the sample of x = 0.075 reaches a ZT of 1.4, corresponding to a 14% enhancement compared to the Mg2Sn0.85Sb0.15 (x = 0) sample. The strategy of introducing heterogeneous structures has important implications for reducing thermal conductivity for other solid-solution thermoelectric systems.

We report the synthesis of three out-of-plane chemically ordered quaternary transition metal borides (o-MAB phases) of the chemical formula M4CrSiB2 (M = Mo, W, Nb). The addition of these phases to the recently discovered o-MAB phase Ti4MoSiB2 shows that this is indeed a new family of chemically ordered atomic laminates. Furthermore, our results expand the attainable chemistry of the traditional M5SiB2 MAB phases to also include Cr. The crystal structure and chemical ordering of the produced materials were investigated using high-resolution scanning transmission electron microscopy and X-ray diffraction by applying Rietveld refinement. Additionally, calculations based on density functional theory were performed to investigate the Cr preference for occupying the minority 4c Wyckoff site, thereby inducing chemical order.

Gallium nitride (GaN) epitaxial films on sapphire (Al2O3) substrates have been grown using reactive magnetron sputter epitaxy with a liquid Ga target. Threading dislocations density (TDD) of sputtered GaN films was reduced by using an inserted high-quality aluminum nitride (AlN) buffer layer grown by reactive high power impulse magnetron sputtering (R-HiPIMS) in a gas mixture of Ar and N2. After optimizing the Ar/N2 pressure ratio and deposition power, a high-quality AlN film exhibiting a narrow full-width at half-maximum (FWHM) value of the double-crystal x-ray rocking curve (DCXRC) of the AlN(0002) peak of 0.086° was obtained by R-HiPIMS. The mechanism giving rise the observed quality improvement is attributed to the enhancement of kinetic energy of the adatoms in the deposition process when operated in a transition mode. With the inserted HiPIMS-AlN as a buffer layer for direct current magnetron sputtering (DCMS) GaN growth, the FWHM values of GaN(0002) and (10 1‾ 1) XRC decrease from 0.321° to 0.087° and from 0.596° to 0.562°, compared to the direct growth of GaN on sapphire, respectively. An order of magnitude reduction from 2.7 × 109 cm−2 to 2.0 × 108 cm−2 of screw-type TDD calculated from the FWHM of the XRC data using the inserted HiPIMS-AlN buffer layer demonstrates the improvement of crystal quality of GaN. The result of TDD reduction using the HiPIMS-AlN buffer was also verified by weak beam dark-field (WBDF) cross-sectional transmission electron microscopy (TEM).

Realizing stress-free inorganic epitaxial films on weakly bonding substrates is of importance for applications that require film transfer onto surfaces that do not seed epitaxy. Film-substrate bonding is usually weakened by harnessing natural van der Waals layers (e.g., graphene) on substrate surfaces, but this is difficult to achieve in non-layered materials. Here, we demonstrate van der Waals epitaxy of stress-free films of a non-layered material VO2 on mica. The films exhibit out-of-plane 010 texture with three inplane orientations inherited from the crystallographic domains of the substrate. The lattice parameters are invariant with film thickness, indicating weak film-substrate bonding and complete interfacial stress relaxation. The out-of-plane domain size scales monotonically with film thickness, but the in-plane domain size exhibits a minimum, indicating that the nucleation of large in-plane domains supports subsequent island growth. Complementary ab initio investigations suggest that VO2 nucleation and van der Waals epitaxy involves subtle polarization effects around, and the active participation of, surface potassium atoms on the mica surface. The VO2 films show a narrow domain-size-sensitive electrical-conductiv ity-temperature hysteresis. These results offer promise for tuning the properties of stress-free van der Waals epitaxial films of non-layered materials such as VO2 through microstructure control (C) 2023 The Author(s). Published by Elsevier Ltd. This is an open access article under the CC BY license (http://creativecommons.org/licenses/by/4.0/).

The development of abundant, cheap, and highly active catalysts for the hydrogen evolution reaction (HER) and oxygen evolution reaction (OER) is important for hydrogen production. Nanolaminate ternary transition metal carbides (MAX phases) and their derived two-dimensional transition metal carbides (MXenes) have attracted considerable interest for electrocatalyst applications. Herein, four new MAX@MXene core-shell structures (Ta2CoC@ Ta2CTx, Ta2NiC@Ta2CTx, Nb2CoC@Nb2CTx, and Nb2NiC@Nb2CTx), in which the core region is Co/Ni-MAX phases while the edge region is MXenes, have been prepared. Under alkaline electrolyte conditions, the Ta2CoC@Ta2CTx core-shell structure showed an overpotential of 239 mV and excellent stability during the HER with MXenes as the active sites. For the OER, the Ta2CoC@Ta2CTx core- shell structure showed an overpotential of 373 mV and a small Tafel plot (56 mV dec-1), which maintained a bulk crystalline structure and generated Co-based oxyhydroxides that formed by surface reconstruction as active sites. Considering rich chemical compositions and structures of MAX phases, this work provides a new strategy for designing multifunctional electrocatalysts and also paves the way for further development of MAX phase-based materials for clean energy applications.

As a single-phase alloy, CrFeCoNi is a face centered cubic (fcc) material related to the archetypical highentropy Cantor alloy CrFeCoNiMn. For thin films, CrFeCoNi of approximately equimolar composition tends to assume an fcc structure when grown at room temperature by magnetron sputtering. However, the single-phase solid solution state is typically not achieved for thin films grown at higher temperatures. The same holds true for Cantor alloy-based ceramics (nitrides and oxides), where phase formation is extremely sensitive to process parameters such as the amount of reactive gas. This study combines theoretical and experimental methods to understand the phase formation in nitrogen-containing CrFeCoNi thin films. Density functional theory calculations considering three competing phases (CrN, Fe-Ni and Co) show that the free energy of mixing, Delta G of (CrFeCoNi)(1-x)N-x solid solutions has a maximum at x = 0.20-0.25, and AG becomes lower when x < 0.20 and x > 0.25. Thin films of (CrFeCoNi)1-xNx (0.14 >= x <= 0.41) grown by magnetron sputtering show stabilization of the metallic fcc when x <= 0.22 and the stabilization of the NaCl B1 structure when x > 0.33, consistent with the theoretical prediction. In contrast, films with intermediate amounts of nitrogen (x = 0.22) grown at higher temperatures show segregation into multiple phases of CrN, Fe-Ni-rich and Co. These results offer an explanation for the requirement of kinetically limited growth conditions at low temperature for obtaining single-phase CrFeCoNi Cantor-like nitrogen-containing thin films and are of importance for understanding the phase-formation mechanisms in multicomponent ceramics. The results from the study further aid in making correlations between the observed mechanical properties and the crystal structure of the films.

Nitrogen-polar III-nitride heterostructures offer advantages over metal-polar structures in high frequency and high power applications. However, polarity control in III-nitrides is difficult to achieve as a result of unintentional polarity inversion domains (IDs). Herein, we present a comprehensive structural investigation with both atomic detail and thermodynamic analysis of the polarity evolution in low-and high-temperature AlN layers on on-axis and 4 degrees off-axis carbon-face 4H-SiC (000 (1) over bar) grown by hot-wall metal organic chemical vapor deposition. A polarity control strategy has been developed by variation of thermodynamic Al supersaturation and substrate misorientation angle in order to achieve the desired growth mode and polarity. We demonstrate that IDs are completely suppressed for high-temperature AlN nucleation layers when a step-flow growth mode is achieved on the off-axis substrates. We employ this approach to demonstrate high quality N-polar epitaxial AlGaN/GaN/AlN heterostructures.

This study presents a novel approach to forming low-resistance ohmic contacts for AlGaN/GaN HEMTs. The optimized contacts exhibit an outstanding contact resistance of approximately 0.15 & omega;& BULL;mm. This is achieved by firstly recessing the barrier of the heterostructure to a depth beyond the channel. In this way, the channel region is exposed on the sidewall of the recess. The coverage of the Ti/Al/Ti ohmic metalization on the sidewall is ensured through tilting of the sample during evaporation. The annealing process is performed at a low temperature of 550 & DEG;C. The approach does not require precise control of the recess etching. Furthermore, the method is directly applicable to most barrier designs in terms of thickness and Al-concentration. The impact of recessed sidewall angle, thickness and ratio of Ti and Al layers, and the annealing procedure are investigated. Structural and chemical analyses of the interface between the ohmic contacts and epi-structure indicate the formation of ohmic contacts by the extraction of nitrogen from the epi-structure. The approach is demonstrated on HEMT-structures with two different barrier designs in terms of Al-concentration and barrier thickness. The study demonstrate large process window in regard to recess depth and duration of the annealing as well as high uniformity of the contact resistance across the samples, rendering the approach highly suitable for industrial production processes.

Refractory high-entropy protective coatings are of interest for nuclear fuel cladding applications due to their corrosion resistant properties and irradiation resistance at elevated temperature. Here, TiZrNbTaV metallic and (TiZrNbTaV)N films were deposited by magnetron co-sputtering. The metal elemental contents of both films were nearly equiatomic. These films were irradiated by Xe ions at room temperature and 500 degrees C, and examined by X-ray diffraction and transmission electron microscopy. The as-deposited (TiZrNbTaV)N film showed a single NaCl-type fcc phase and a pronounced columnar growth structure, which could remain intact after irradiation treatments. In contrast, the as-deposited TiZrNbTaV film exhibited an amorphous structure and formed a bcc phase structure after irradiation at 500 degrees C. The TiZrNbTaV film after irradiation at 500 degrees C composed of depth -dependent size of grains. This distribution of grain size is consistent with simulated displacement damage. The stable structure of (TiZrNbTaV)N film under high temperature irradiation indicates that these materials have potential for use as protective coatings for nuclear fuel claddings.

The recent discovery of chemical ordering in quaternary borides offers new ways of exploring properties and functionalities of these laminated phases. Here, we have synthesized and investigated chemical ordering of the laminated Mo4MnSiB2 (T2) phase, thereby introducing a magnetic element into the family of materials coined o-MAB phases. By X-ray diffraction and scanning transmission electron microscopy, we provide evidence for out-of-plane chemical ordering of Mo and Mn, with Mo occupying the 16l site and Mn preferentially residing in the 4c site. Mn and B constitute quasi-two-dimensional layers in the laminated material. We have therefore also studied the magnetic properties by magnetometry, and no sign of long-range magnetic order is observed. An initial assessment of the magnetic ordering has been further studied by density functional theory (DFT) calculations, and while we find an antiferromagnetic configuration to be the most stable one, ferromagnetic ordering is very close in energy.

Compositionally graded channel AlGaN/GaN high electron mobility transistors (HEMTs) offer a promising route to improve device linearity, which is necessary for low-noise radio-frequency amplifiers. In this work, we demonstrate different grading profiles of a 10-nm-thick AlxGa1-xN channel from x = 0 to x = 0.1 using hot-wall metal-organic chemical vapor deposition (MOCVD). The growth process is developed by optimizing the channel grading and the channel-to-barrier transition. For this purpose, the Al-profiles and the interface sharpness, as determined from scanning transmission electron microscopy combined with energy-dispersive x-ray spectroscopy, are correlated with specific MOCVD process parameters. The results are linked to the channel properties (electron density, electron mobility, and sheet resistance) obtained by contactless Hall and terahertz optical Hall effect measurements coupled with simulations from solving self-consistently Poisson and Schrodinger equations. The impact of incorporating a thin AlN interlayer between the graded channel and the barrier layer on the HEMT properties is investigated and discussed. The optimized graded channel HEMT structure is found to have similarly high electron density (similar to 9 x 10(12) cm(-2)) as the non-graded conventional structure, though the mobility drops from similar to 2360 cm(2)/V s in the conventional to similar to 960 cm(2)/V s in the graded structure. The transconductance g(m) of the linearly graded channel HEMTs is shown to be flatter with smaller g(m) and g(m) as compared to the conventional non-graded channel HEMT implying improved device linearity. (c) 2023 Author(s). All article content, except where otherwise noted, is licensed under a Creative Commons Attribution (CC BY) license (http://creativecommons.org/licenses/by/4.0/).

MXenes are electrically conductive 2D transition metal carbides/nitrides obtained by the etching of nanolaminated MAX phase compounds, followed by exfoliation to single- or few-layered nanosheets. The mainstream chemical etching processes have evolved from pure hydrofluoric acid (HF) etching into the innovative "minimally intensive layer delamination" (MILD) route. Despite their current popularity and remarkable application potential, the scalability of MILD-produced MXenes remains unproven, excluding MXenes from industrial applications. This work proposes a "next-generation MILD" (NGMILD) synthesis protocol for phase-pure, colloidally stable MXenes that withstand long periods of dry storage. NGMILD incorporates the synergistic effects of a secondary salt, a richer lithium (Li) environment, and iterative alcohol-based washing to achieve high-purity MXenes, while improving etching efficiency, intercalation, and shelf life. Moreover, NGMILD comprises a sulfuric acid (H2SO4) post-treatment for the selective removal of the Li3AlF6 impurity that commonly persists in MILD-produced MXenes. This work demonstrates the upscaled NGMILD synthesis of (50 g) phase-pure Ti(3)C(2)Tz MXene clays with high extraction yields (>22%) of supernatant dispersions. Finally, NGMILD-produced MXene clays dry-stored for six months under ambient conditions experience minimal degradation, while retaining excellent redispersibility. Overall, the NGMILD protocol is a leap forward toward the industrial production of MXenes and their subsequent market deployment.

Two-dimensional (2D) materials offer advantages that their 3D counterparts do not. The conventional method for the bulk synthesis of 2D materials has predominantly been through etching layered solids. Herein, we convert - through a bottom-up approach - 10 binary and ternary titanium carbides, nitrides, borides, phosphides, and silicides into 2D flakes by immersing them in a tetramethylammonium hydroxide solution at temperatures in the 25-85 degrees C range. Based on X-ray diffraction, density functional theory, X-ray photoelectron, electron energy loss, Raman, X-ray absorption near edge structure spectroscopies, transmission and scanning electron microscope images and selected area diffraction, we conclude that the resulting flakes are carbon containing anatase-based layers that are, in turn, comprised of approximate to 6 x 10 angstrom(2) nanofilaments in cross-section some of which are few microns long. Electrodes made from some of these films performed well in lithium-ion and lithium-sulphur systems. These materials also reduce the viability of cancer cells thus showing potential in biomedical applications. Synthesizing 2D materials, at near ambient conditions, with non-layered, inexpensive, green precursors (e.g., TiC) is paradigm shifting and will undoubtedly open new and exciting avenues of research and applications.

Gadolinium chelates are employed worldwide today as clinical contrast agents for magnetic resonance imaging. Until now, the commonly used linear contrast agents based on the rare-earth element gadolinium have been considered safe and well-tolerated. Recently, concerns regarding this type of contrast agent have been reported, which is why there is an urgent need to develop the next generation of stable contrast agents with enhanced spin-lattice relaxation, as measured by improved T-1 relaxivity at lower doses. Here, we show that by the integration of gadolinium ions in cerium oxide nanoparticles, a stable crystalline 5 nm sized nanoparticulate system with a homogeneous gadolinium ion distribution is obtained. These cerium oxide nanoparticles with entrapped gadolinium deliver strong T-1 relaxivity per gadolinium ion (T-1 relaxivity, r(1) = 12.0 mM(-1) s(-1)) with the potential to act as scavengers of reactive oxygen species (ROS). The presence of Ce3+ sites and oxygen vacancies at the surface plays a critical role in providing the antioxidant properties. The characterization of radial distribution of Ce3+ and Ce4+ oxidation states indicated a higher concentration of Ce3+ at the nanoparticle surfaces. Additionally, we investigated the ROS-scavenging capabilities of pure gadolinium-containing cerium oxide nanoparticles by bioluminescent imaging in vivo, where inhibitory effects on ROS activity are shown.

Electrochromic (EC) materials that change color with voltage have been widely studied for use in dynamic windows. However, colorless-to-colorful switching with high contrast ratio is generically unattainable, especially for colorless-to-black electrochromic materials with an ultrahigh contrast ratio over the entire visible region. In this work, we developed Nb1.33C MXene-based dynamic windows with colorless-to-black switching of up to 75% reversible change in transmittance from 300 to 1,500 nm. By exploring the electrochromic effects of different electrolytes through in situ optical changes and electrochemical quartz crystal microbalance (EQCM), it is found that electrochromic behavior is greatly influenced by the extent of reversible Li+ insertion/deinsertion between the two-dimensional Nb1.33C MXene nanosheets. In addition, a colorless-to-black EC device based on Nb1.33C with an overall integrated contrast ratio over 80% was successfully constructed by a solution-processable spin coating method. This work enables a simple route to fabricate MXene-based high-performance electrochromic smart windows, which is important for further expanding the application of MXenes to optoelectronic and photonic applications.

Photoconduction (PC) properties were investigated for ternary indium aluminium nitride (InxAl1-xN) nanorods (NRs) with different indium compositions (x) from 0.35 to 0.68, as grown by direct-current reactive magnetron sputter epitaxy. Cross-sectional scanning transmission electron microscopy (STEM) reveals single-crystal quality of the vertically aligned InxAl1-xN NRs. Single-rod photodetector devices with good ohmic contacts were fabricated using the focused-ion-beam technique (FIB), where the In-rich In0.68Al0.32N NR exhibits an optimal photocurrent responsivity of 1400 A W-1 and photoconductive gain of 3300. A transition from a positive photoresponse to a negative photoresponse was observed, while increasing the In composition x from 0.35 to 0.57. The negative PC was further enhanced by increasing x to 0.68. A model based on the coexistence and competition of deep electron trap states and recombination centers was proposed to explain the interesting composition-dependent PC in these ternary III-nitride 1D nanostructures.

i-MXenes, a new family of 2D transition metal carbides with in-plane ordered vacancies, have shown great potential in aqueous supercapacitor (SC) applications due to their high volumetric capacitances and energy densities. However, how vacancies affect their electrochemical performance, in general, and their self-discharge (SD) behavior in particular, remains unexplored. Herein, we compare the electrochemical performance of vacancy rich, ordered Mo_1.33CT_z i-MXene to that of Mo₂CT_z (with much less vacancies) in a 1 M sulfuric acid (H₂SO₄) or 15 M of lithium bromide (LiBr) electrolyte. The Mo_1.33CT_z exhibits higher volumetric capacitances and energy densities, but at the cost of a higher SD rate. Specifically, the Mo_1.33CT_z symmetric SCs deliver an energy density as high as 25.4 mWh cm(-3) at 152.4 mW cm^-3, with 65.4% voltage retention after 10 h in 15 M LiBr. In comparison, the Mo₂CT_z symmetric SCs have a maximum energy density of 20.8 mWh cm^-3 at 124.9 mW cm^-3, with 73.1% voltage retention after 10 h in the same electrolyte. The SD rates in the H₂SO₄ electrolyte are quite rapid.

We report structure, vibrational properties, and weak antilocalization-induced quantum correction to magnetoconductivity in single-crystal Bi₂GeTe₄. Surface band-structure calculations show a single Dirac cone corresponding to topological surface states in Bi₂GeTe₄. An estimated phase coherence length, l_Φ ~ to 143 nm and prefactor α~-1.54 from Hikami-Larkin-Nagaoka fitting of magnetoconductivity describe the quantum correction to conductivity. An anomalous temperature dependence of A_1g Raman modes confirms enhanced electron-phonon interactions. Our results establish that electrons of the topological state can interact with the phonons involving the vibrations of Bi-Te in Bi₂GeTe₄.

CaMnO3 is a perovskite with attractive magnetic and thermoelectric properties. CaMnO3 films are usually grown by pulsed laser deposition or radio frequency magnetron sputtering from ceramic targets. Herein, epitaxial growth of CaMnO3-y (002) films on a (112 over bar 0)-oriented LaAlO3 substrate using pulsed direct current reactive magnetron sputtering is demonstrated, which is more suitable for industrial scale depositions. The CaMnO3-y shows growth with a small in-plane tilt of <approximate to 0.2 degrees toward the (200) plane of CaMnO3-y and the (1 over bar 104) with respect to the LaAlO3 (112 over bar 0) substrate. X-ray photoelectron spectroscopy of the electronic core levels shows an oxygen deficiency described by CaMnO2.58 that yields a lower Seebeck coefficient and a higher electrical resistivity when compared to stoichiometric CaMnO3. The LaAlO3 (112 over bar 0) substrate promotes tensile-strained growth of single crystals. Scanning transmission electron microscopy and electron energy loss spectroscopy reveal antiphase boundaries composed of Ca on Mn sites along and , forming stacking faults.

The hot-wall metalorganic chemical vapor deposition (MOCVD) concept, previously shown to enable superior material quality and high performance devices based on wide bandgap semiconductors, such as Ga(Al)N and SiC, has been applied to the epitaxial growth of beta-Ga2O3. Epitaxial beta-Ga2O3 layers at high growth rates (above 1 mu m/h), at low reagent flows, and at reduced growth temperatures (740 degrees C) are demonstrated. A high crystalline quality epitaxial material on a c-plane sapphire substrate is attained as corroborated by a combination of x-ray diffraction, high-resolution scanning transmission electron microscopy, and spectroscopic ellipsometry measurements. The hot-wall MOCVD process is transferred to homoepitaxy, and single-crystalline homoepitaxial beta-Ga2O3 layers are demonstrated with a 201 rocking curve width of 118 arc sec, which is comparable to those of the edge-defined film-fed grown (201) beta-Ga2O3 substrates, indicative of similar dislocation densities for epilayers and substrates. Hence, hot-wall MOCVD is proposed as a prospective growth method to be further explored for the fabrication of beta-Ga2O3.

High-entropy (HE) ceramics, by analogy with HE metallic alloys, are an emerging family of multielemental solid solutions. These materials offer a large compositional space, with a corresponding large range of properties. Here, we report the experimental realization of a 3D HE MAX phase, Ti1,0V0.7Cr0.05Nb1.0Ta1.0AlC3, and a corresponding 2D HE MXene in the form of freestanding flakes of average composition Ti1.1V0.7CrxNb1.0Ta0.6C3Tz (T-z = -F, -O, -OH), as produced by selective removal of AI from the HE MAX phase in aqueous hydrofluoric acid (HF). Initial tests on HE MXene "paper" electrodes show their high potential as electrode materials in supercapacitors through volumetric and gravimetric capacitances of 1688 F/cm(3) and 490 F/g, respectively, originating from a combination of diffusion- and surface-controlled charge storage processes. The introduction of the HE concept into the field of 2D materials suggests a wealth of future 2D materials and applications.

InxGa1-x N is a strategically important material for electronic devices given its tunable bandgap, modulated by the In/Ga ratio. However, current applications are hindered by defects caused by strain relaxation and phase separation in the material. Here, we demonstrate growth of homogeneous InxGa1-x N films with 0.3 < x < 0.8 up to similar to 30 nm using atomic layer deposition (ALD) with a supercycle approach, switching between InN and GaN deposition. The composition is uniform along and across the films, without signs of In segregation. The InxGa1-x N films show higher In-content than the value predicted by the supercycle model. A more pronounced reduction of GPC(InN) than GPC(GaN) during the growth processes of InN and GaN bilayers is concluded based on our analysis. The intermixing between InN and GaN bilayers is suggested to explain the enhanced overall In-content. Our results show the advantage of ALD to prepare high-quality InxGa1-x N films, particularly with high In-content, which is difficult to achieve with other growth methods.

The impact on the performance of GaN high electron mobility transistors (HEMTs) of in situ ammonia (NH3) pre-treatment prior to the deposition of silicon nitride (SiN) passivation with low-pressure chemical vapor deposition (LPCVD ) is investigated. Three different NH3 pre-treatment durations (0, 3, and 10 min) were compared in terms of interface properties and device performance. A reduction of oxygen (O) at the interface between SiN and epi-structure is detected by scanning transmission electron microscopy (STEM )-electron energy loss spectroscopy (EELS) measurements in the sample subjected to 10 min of pre-treatment. The samples subjected to NH3 pre-treatment show a reduced surface-related current dispersion of 9% (compared to 16% for the untreated sample), which is attributed to the reduction of O at the SiN/epi interface. Furthermore, NH3 pre-treatment for 10 min significantly improves the current dispersion uniformity from 14.5% to 1.9%. The reduced trapping effects result in a high output power of 3.4 W mm(-1) at 3 GHz (compared to 2.6 W mm(-1) for the untreated sample). These results demonstrate that the in situ NH3 pre-treatment before LPCVD of SiN passivation is critical and can effectively improves the large-signal microwave performance of GaN HEMTs.

The crystal reorganization of the IrMn thin film was observed by the in situ thermal annealing in the X-ray diffraction (XRD) and electron energy loss spectroscopy. From room temperature to 700 degrees C, the in situ annealing measurements identify the different Mn diffusion effects in three temperature ranges. First, between room temperature and 300 degrees C, the XRD profiles show the reorganization of Mn atoms from interstitials to IrMn lattice points. Second, between 300 and 400 degrees C, we observed the diffusion of Mn atoms from the IrMn thin film to the surface, causing the atomic Mn/Ir ratio to drop from 10 to 7. The MnO appeared on the film surface in this temperature range. Third, from 400 to 700 degrees C, the O content in the IrMn thin film increases to 8%, while the Mn/ Ir ratio continuously decreases from 7 to 5. The scanning transmission electron microscopy images also show that the crystal structure of IrMn thin film completely degrades to another structure.

Structural defects in Mg-doped GaN were analyzed using high-resolution scanning transmission electron microscopy combined with electron energy loss spectroscopy. The defects, in the shape of inverted pyramids, appear at high concentrations of incorporated Mg, which also lead to a reduction in free-hole concentration in Mg doped GaN. Detailed analysis pinpoints the arrangement of atoms in and around the defects and verify the presence of a well-defined layer of Mg at all facets, including the inclined facets. Our observations have resulted in a model of the pyramid-shaped defect, including structural displacements and compositional replacements, which is verified by image simulations. Finally, the total concentration of Mg atoms bound to these defects were evaluated, enabling a correlation between inactive and defect-bound dopants.

The hot-wall metal-organic chemical vapor deposition (MOCVD), previously shown to enable superior III-nitride material quality and high performance devices, has been explored for Mg doping of GaN. We have investigated the Mg incorporation in a wide doping range ( 2.45 x 10( 18) cm(-3) up to 1.10 x 10(20) cm(-3)) and demonstrate GaN:Mg with low background impurity concentrations under optimized growth conditions. Dopant and impurity levels are discussed in view of Ga supersaturation, which provides a unified concept to explain the complexity of growth conditions impact on Mg acceptor incorporation and compensation. The results are analyzed in relation to the extended defects, revealed by scanning transmission electron microscopy, x-ray diffraction, and surface morphology, and in correlation with the electrical properties obtained by Hall effect and capacitance-voltage (C-V) measurements. This allows to establish a comprehensive picture of GaN:Mg growth by hot-wall MOCVD providing guidance for growth parameters optimization depending on the targeted application. We show that substantially lower H concentration as compared to Mg acceptors can be achieved in GaN:Mg without any in situ or post-growth annealing resulting in p-type conductivity in as-grown material. State-of-the-art p-GaN layers with a low resistivity and a high free-hole density (0.77 omega cm and 8.4 x 10( 17) cm(-3), respectively) are obtained after post-growth annealing demonstrating the viability of hot-wall MOCVD for growth of power electronic device structures. (C)2022 Author(s).

Aqueous asymmetric supercapacitors (AASCs) can have high voltages and high energy densities. However, the rational design of AASCs with proper negative and positive electrodes remains a challenge. Herein, we report on an AASC using Mo1.33CTz MXene films as the negative electrode, and tetramethylammonium cation intercalated birnessite (TMA(+)-MnO2) films as the positive electrode in a 21 mol kg(-1) lithium bis(trifluoromethanesulphonyl)imide (LiTFSI) electrolyte. Benefiting from a high, stable voltage of 2.5 V, an energy density of 86.5 Wh L-1 at 2 mV s(-1) and a power density of 10.3 kW L-1 at 1 Vs(-1) were achieved. The cells also exhibit excellent cycling stability (>98% after 1,0000 cycles at 100 mV s(-1)) and a 51.1 % voltage retention after 10 h. This good performance is attributed to the high stable potential window and high volumetric capacitances of both Mo1.33CTz and TMA(+)-MnO2 electrodes in highly concentrated electrolytes. This work provides a roadmap for developing high performance AASCs with high voltages and high energy/power densities, with relatively slow self-discharge rates.

Planar defect structures appearing in transition metal diboride (TMB2) thin films, grown by different magnetron sputtering-deposition approaches over a wide compositional and elemental range, were systematically investi-gated. Atomically resolved scanning transmission electron microscopy (STEM) imaging, electron energy loss spec-troscopy (EELS) elemental mapping, and first principles calculations have been applied to elucidate the atomic structures of the observed defects. Two distinct types of antiphase boundary (APB) defects reside on the {1(1) over bar 00} planes. These defects are without (named APB-1) or with (APB-2) local deviation from stoichiometry. APB-2 de-fects, in turn, appear in different variants. It is found that APB-2 defects are governed by the films composition, while APB-1 defects are endemic. The characteristic structures, interconnections, and circumstances leading to the formation of these APB-defects, together with their formation energies, are presented.

We investigate the interfaces and polarity domains at the atomic scale in epitaxial AlN and GaN/AlN grown by hot-wall metal organic chemical vapor epitaxy on the carbon face of SiC. X-ray diffraction, potassium hydroxide (KOH) wet chemical etching, and scanning transmission electron microscopy combined provide an in-depth understanding of polarity evolution with the film thickness, which is crucial to optimize growth. The AlN grown in a 3D mode is found to exhibit N-polar pyramid-type structures at the AlN-SiC interface. However, a mixed N-polar and Al-polar region with Al-polarity domination along with inverted pyramid-type structures evolve with increasing film thickness. We identify inclined inversion domain boundaries and propose that incorporation of oxygen on the & lang;40-41 & rang; facets of the N-polar pyramids causes the polarity inversion. We find that mixed-polar AlN is common and easily etched and remains undetected by solely relying on KOH etching. Atomic scale electron microscopy is, therefore, needed to accurately determine the polarity. The polarity of GaN grown on mixed-polar AlN is further shown to undergo complex evolution with the film thickness, which is discussed in the light of growth mechanisms and polarity determination methods.

Direct-current magnetron sputtering (DCMS) and high-power impulse magnetron sputtering (HiPIMS) were used to deposit understoichiometric Ti(1-x)Al(x)B(2-y )diboride coatings by sputtering from a segmented TiB2-AlB2 target using Ar and Kr as sputtering gas. For films with a fixed Al/(Ti + Al) ratio of x = 0.1 (Ti0.9Al0.1B2-y), the B content was varied with y & ISIN; (0.1, 0.6 and 0.7). For films with a fixed y = 0.7 (Ti1-xAlxB1.3), the Al content was varied with x & ISIN; (0.1, 0.4 and 0.7). Evaluation of the mechanical properties of the Ti1-xAlxB1.3 samples showed a reduction in both hardness and elastic modulus with increasing Al concentration, while the Ti0.9Al0.1B2-y samples showed a hardness increase with decreasing B content. Thus, Ti0.9Al0.1B1.3 films exhibited a superior hardness of 46.2 +/- 1.1 GPa and an elastic modulus of 523 & PLUSMN; 7 GPa, compared to the values for Ti0.9Al0.1B1.4 and Ti0.9Al0.1B1.9, showing a hardness of 44 +/- 1 GPa and 36 +/- 1 GPa, and an elastic modulus of 569 +/- 7 GPa and 493 +/- 6 GPa, respectively. The oxidation behavior of the mechanically most promising Ti0.9Al0.1B2-y sample series was investigated through air-annealing at 600 C for durations from 1 h to 10 h. All films formed a mixed non-conformal Al2O3-TiO2 oxide scale which acts as an inward and outward diffusion barrier, significantly reducing the oxidation rate compared to TiBz films, which form an oxide scale consisting of porous TiO2. The thinnest oxide scale after 10 h was found in the B-deficient samples, Ti0.9Al0.1B1.3 and Ti0.9Al0.1B1.4, at ~200 nm, which is significantly below that for Ti0.9Al0.1B1.9 at 320 nm. The enhanced oxidation resistance of highly understoichiometric films is due to the elimination of the B-rich tissue phase that is present at the grain boundaries for higher B content, where the latter has been shown to enhance the rate of oxidation in borides.

Solid-state precipitation can be used to tailor material properties, ranging from ferromagnets and catalysts to mechanical strengthening and energy storage. Thermoelectric properties can be modified by precipitation to enhance phonon scattering while retaining charge-carrier transmission. Here, unconventional Janus-type nanoprecipitates are uncovered in Mg3Sb1.5Bi0.5 formed by side-by-side Bi- and Ge-rich appendages, in contrast to separate nanoprecipitate formation. These Janus nanoprecipitates result from local comelting of Bi and Ge during sintering, enabling an amorphous-like lattice thermal conductivity. A precipitate size effect on phonon scattering is observed due to the balance between alloy-disorder and nanoprecipitate scattering. The thermoelectric figure-of-merit ZT reaches 0.6 near room temperature and 1.6 at 773 K. The Janus nanoprecipitation can be introduced into other materials and may act as a general property-tailoring mechanism.

High entropy alloys are multielement materials exhibiting enhanced properties compared to their binary or ternary equivalents. Here, the authors investigate the influence of microstructure and elemental distribution on the transport and superconducting properties of (TaNb)(1-x)(ZrHfTi)(x) thin films. Superconducting high entropy alloys (HEAs) may combine extraordinary mechanical properties with robust superconductivity. They are suitable model systems for the investigation of the interplay of disorder and superconductivity. Here, we report on the superconductivity in (TaNb)(1-x)(ZrHfTi)(x) thin films. Beyond the near-equimolar region, the films comprise hundreds-of-nanometer-sized crystalline grains and show robust bulk superconductivity. However, the superconducting transitions in these nanocomposites are dramatically suppressed in the near-equimolar configurations, i.e., 0.45 < x < 0.64, where elemental distributions are equivalently homogeneous. Crystal/glass high entropy alloy nanocomposite phase separation was observed for the films in the near-equimolar region, which yields a broadened two-step normal to superconducting transition. Furthermore, the diamagnetic shielding in these films is only observed far below the onset temperature of superconductivity. As these unusual superconducting transitions are observed only in the samples with the high mixing entropy, this compositional range influences the collective electronic properties in these materials.

Organic electrochemical transistors (OECTs) have the potential to revolutionize the field of organic bioelectronics. To date, most of the reported OECTs include p-type (semi-)conducting polymers as the channel material, while n-type OECTs are yet at an early stage of development, with the best performing electron-transporting materials still suffering from low transconductance, low electron mobility, and slow response time. Here, the high electrical conductivity of multi-walled carbon nanotubes (MWCNTs) and the large volumetric capacitance of the ladder-type pi-conjugated redox polymer poly(benzimidazobenzophenanthroline) (BBL) are leveraged to develop n-type OECTs with record-high performance. It is demonstrated that the use of MWCNTs enhances the electron mobility by more than one order of magnitude, yielding fast transistor transient response (down to 15 ms) and high mu C* (electron mobility x volumetric capacitance) of about 1 F cm(-1) V-1 s(-1). This enables the development of complementary inverters with a voltage gain of >16 and a large worst-case noise margin at a supply voltage of <0.6 V, while consuming less than 1 mu W of power.

Titanium boride, TiBx, thin films were grown by direct current magnetron co-sputtering from a compound TiB2 target and a Ti target at an Ar pressure of 2.2 mTorr (0.3 Pa) and substrate temperature of 450 ?degrees C. While keeping the power of the TiB2 target constant at 250 W, and by varying the power on the Ti target, P-Ti, between 0 and 100 W, the B/Ti ratio in the film could be continuously and controllably varied from 1.2 to 2.8, with close-tostoichiometric diboride films achieved for P-Ti = 50 W. This was done without altering the deposition pressure, which is otherwise the main modulator for the composition of magnetron sputtered TiBx diboride thin films. The film structure and properties of the as-deposited films were compared to those after vacuum-annealing for 2 h at 1100 ?degrees C. As-deposited films consisted of small (?50 nm) randomly oriented TiB2 crystallites, interspersed in an amorphous, sometimes porous tissue phase. Upon annealing, some of the tissue phase crystallized, but the diboride average grain size did not change noticeably. The near-stoichiometric film had the lowest resistivity, 122 mu omega cm, after annealing. Although this film had growth-induced porosity, an interconnected network of elongated crystallites provides a path for conduction. All films exhibited high hardness, in the 25-30 GPa range, where the highest value of similar to 32 GPa was obtained for the most Ti-rich film after annealing. This film had the highest density and was nano-crystalline, where dislocation propagation is interrupted by the off-stoichiometric grain boundaries.

Recently, we presented a family of in-plane chemically ordered transition metal borides of the general formula (M-2/3M-1/3")(2)AlB2. Here, we investigate incorporation of magnetic rare earth (RE) elements into this structure by synthesis and analysis of Mo4/3RE2/3AlB2, where RE = Ho, Tb, and Er. The crystal structure is verified by X-ray diffraction and scanning transmission electron microscopy, while the composition is derived from energy dispersive X-ray analysis. Through magnetization measurements, we also show that Mo4/3Ho2/3AlB2 orders antiferromagnetically below 9 K. We suggest that (M-2/3M-1/3")(2)AlB2 could potentially be a versatile platform for new magnetic materials, in 3D as well as 2D. [GARPHICS] IMPACT STATEMENT This paper introduces magnetic elements to i-MAB phases family with a formula of Mo4/3RE2/3AlB2 (RE = Ho, Er, and Tb), which opens a venue for further exploration of chemically ordered magnetic materials.

A new family of 2D transition metal carbo-chalcogenides (TMCCs) is reported, which can be considered a combination of two well-known families, TM carbides (MXenes) and TM dichalcogenides (TMDCs), at the atomic level. Single sheets are successfully obtained from multilayered Nb₂S₂C and Ta₂S₂C using electrochemical lithiation followed by sonication in water. The parent multilayered TMCCs are synthesized using a simple, scalable solid-state synthesis followed by a topochemical reaction. A superconductivity transition is observed at 7.55 K for Nb₂S₂C. The delaminated Nb₂S₂C outperforms both multilayered Nb₂S₂C and delaminated NbS₂ as an electrode material for Li-ion batteries. Ab initio calculations predict the elastic constant of TMCC to be over 50% higher than that of TMDC.

We recently showed that sputter-deposited Zr_1-xTa_xB_y thin films have hexagonal AlB₂-type columnar nanostructure in which column boundaries are B-rich for x < 0.2, while Ta-rich for x ≥ 0.2. As-deposited layers with x ≥ 0.2 exhibit higher hardness and, simultaneously, enhanced toughness. Here, we study the mechanical properties of ZrB_2.4, Zr_0.8Ta_0.2B_1.8, and Zr_0.7Ta_0.3B_1.5 films annealed in Ar atmosphere as a function of annealing temperature T_a up to 1200 °C. In-situ and ex-situ nanoindentation analyses reveal that all films undergo age hardening up to T_a = 800 °C, with the highest hardness achieved for Zr_0.8Ta_0.2B_1.8 (45.5±1.0 GPa). The age hardening, which occurs without any phase separation or decomposition, can be explained by point-defect recovery that enhances chemical bond density. Although hardness decreases at T_a > 800 °C due mainly to recrystallization, column coarsening, and planar defect annihilation, all layers show hardness values above 34 GPa over the entire T_a range.

Extensive research has been invested in two-dimensional (2D) materials, typically synthesized by exfoliation of van der Waals solids. One exception is MXenes, derived from the etching of constituent layers in transition metal carbides and nitrides. We report the experimental realization of boridene in the form of single-layer 2D molybdenum boride sheets with ordered metal vacancies, Mo4/3B2-xTz (where T-z is fluorine, oxygen, or hydroxide surface terminations), produced by selective etching of aluminum and yttrium or scandium atoms from 3D in-plane chemically ordered (Mo2/3Y1/3)(2)AlB2 and (Mo2/3Sc1/3)(2)AlB2 in aqueous hydrofluoric acid. The discovery of a 2D transition metal boride suggests a wealth of future 2D materials that can be obtained through the chemical exfoliation of laminated compounds.

This work reports on sputter depositions carried out from a compound (Ti,Zr)(2)AlC target on Al2O3(0 0 0 1) substrates at temperatures ranging between 500 and 900 degrees C. Short deposition times yielded 30-40 nm-thick Al-containing (Ti,Zr)C films, whereas longer depositions yielded thicker films up to 90 nm which contained (Ti,Zr)C and intermetallics. At 900 degrees C, the longer depositions led to films that also consisted of solid solution MAX phases. Detailed transmission electron microscopy showed that both (Ti,Zr)(2)AlC and (Ti,Zr)(3)AlC2 solid solution MAX phases were formed. Moreover, this work discusses the growth mechanism of the thicker films, which started with the formation of the mixed (Ti,Zr)C carbide, followed by the nucleation and growth of aluminides, eventually leading to solid state diffusion of Al within the carbide, at the highest temperature (900 degrees C) to form the MAX phases.

MAX phases are gaining attention as precursors of two-dimensional MXenes that are intensively pursued in applications for electrochemical energy storage. Here, we report the preparation of V2SnC MAX phase by the molten salt method. V2SnC is investigated as a lithium storage anode, showing a high gravimetric capacity of 490 mAh g(-1) and volumetric capacity of 570 mAh cm(-3) as well as superior rate performance of 95 mAh g(-1) (110 mAh cm(-3)) at 50 C, surpassing the ever-reported performance of MAX phase anodes. Supported by operando X-ray diffraction and density functional theory, a charge storage mechanism with dual redox reaction is proposed with a Sn-Li (de)alloying reaction that occurs at the edge sites of V2SnC particles where Sn atoms are exposed to the electrolyte followed by a redox reaction that occurs at V2C layers with Li. This study offers promise of using MAX phases with M-site and A-site elements that are redox active as high-rate lithium storage materials.

Two-dimensional (2D) Mo1.33C MXene renders great potential for energy storage applications and is mainly studied in the sulfuric acid (H2SO4) electrolyte. However, H2SO4 limits the electrode potential to 0.9 V for symmetric devices and 1.3 V for asymmetric devices. Herein, we explore the electrochemical behavior of Mo1.33C MXene in LiCl electrolyte. In comparison to H2SO4, LiCl electrolyte is a neutral salt with high solubility at room temperature and low hazardousness. The analysis shows a volumetric capacitance of 815 Fcm(-3) at a scan rate of 2 mVs(-1) with a large operating potential window of -1.2 to +0.3V (vs. Ag/AgCl). This is further exploited to construct MXene-based asymmetric supercapacitors Mo1.33C//MnxOn, and the electrochemical performance is evaluated in 5M LiCl electrolyte. Owing to the wide voltage widow of the Mo1.33C//MnxOn devices (2V) and high packing density of the electrodes, we have achieved a volumetric energy density of 58 mWh/cm(3), a maximum power density of 31 Wcm(-3) and retained 92% of the initial capacitance after 10,000 charge/discharge cycles at 10 A g(-1). One of the main value propositions of this work, aside from the high energy density, is the outstanding columbic efficiency (100%), which ensures excellent cyclic stability and is highly desirable for practical applications.

This review celebrates the width and depth of electron microscopy methods and how these have enabled massive research efforts on MXenes. MXenes constitute a powerful recent addition to 2-dimensional materials, derived from their parent family of nanolaminated materials known as MAX phases. Owing to their rich chemistry, MXenes exhibit properties that have revolutionized ranges of applications, including energy storage, electromagnetic interference shielding, water filtering, sensors, and catalysis. Few other methods have been more essential in MXene research and development of corresponding applications, compared with electron microscopy, which enables structural and chemical identification at the atomic scale. In the following, the electron microscopy methods that have been applied to MXene and MAX phase precursor research are presented together with research examples and are discussed with respect to advantages and challenges.

Enhancing both the energy storage and power capabilities of electrochemical capacitors remains a challenge. Herein, Ti3C2Tz MXene is mixed with MoO3 nanobelts in various mass ratios and the mixture is used to vacuum filter binder free, open, flexible, and free-standing films. The conductive Ti3C2Tz flakes bridge the nanobelts, facilitating electron transfer; the randomly oriented, and interconnected, MoO3 nanobelts, in turn, prevent the restacking of the Ti3C2Tz nanosheets. Benefitting from these advantages, a MoO3/Ti3C2Tz film with a 8:2 mass ratio exhibits high gravimetric/volumetric capacities with good cyclability, namely, 837 C g(-1) and 1836 C cm(-3) at 1 A g(-1) for an approximate to 10 mu m thick film; and 767 C g(-1) and 1664 C cm(-3) at 1 A g(-1) for approximate to 50 mu m thick film. To further increase the energy density, hybrid capacitors are fabricated with MoO3/Ti3C2Tz films as the negative electrodes and nitrogen-doped activated carbon as the positive electrodes. This device delivers maximum gravimetric/volumetric energy densities of 31.2 Wh kg(-1) and 39.2 Wh L-1, respectively. The cycling stability of 94.2% retention ratio after 10 000 continuous charge/discharge cycles is also noteworthy. The high energy density achieved in this work can pave the way for practical applications of MXene-containing materials in energy storage devices.