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At least 91 records · Page 5

Revealing the Correlation between the Solvation Structures and the Transport Properties of Water-in-Salt Electrolytes

Water-in-salt (WIS) electrolytes containing 21 m lithium bis(trifluoromethane sulfonyl)imide (LiTFSI) have been considered as a safe and environment-friendly alternative to common organic electrolytes used in lithium-ion batteries. However, the relation between the solvation structures and transport properties of these materials remains elusive. Here, for this paper, we performed small-angle X-ray scattering (SAXS), small-angle neutron scattering (SANS), and X-ray pair distribution function (PDF) measurements of LiTFSI aqueous solutions at a wide range of concentrations. Combined with molecular dynamics simulations, the detailed solvation structures from long to short length scale were resolved. We found that the TFSI– solvation structures consist of TFSI– solvated structures and TFSI– networks; the former corresponds to solvent separated ion pairs, while the latter corresponds to contact ion pairs and cation–anion aggregates. In addition, we found that the relaxation time in the q range associated with the anion network structure exhibits the same concentration dependence as the viscosity. By combining the results from the experiments and simulations, this study revealed a correlation between the solvation structures of LiTFSI and the transport properties of the solutions, which is critical to understand the relation between the transport properties and the dynamics of the ions for imide-based lithium-ion salt aqueous electrolytes.

36 MATERIALS SCIENCE↗

Localized Hydrophobicity in Aqueous Zinc Electrolytes Improves Zinc Metal Reversibility

The rechargeability of aqueous zinc metal batteries is plagued by parasitic reactions of the zinc metal anode and detrimental morphologies such as dendritic or dead zinc. To improve the zinc metal reversibility, hereby we report a new solution structure of aqueous electrolyte with hydroxyl-ions scavengers and hydrophobicity localized in solvent clusters. In this work we show that although hydrophobicity sounds counterintuitive for an aqueous system, hydrophilic pockets may be encapsulated inside a hydrophobic outer layer and a hydrophobic anode-electrolyte interface can be generated through the addition of a cation-philic, strongly anion-phobic, and OH - -reactive diluent. The localized hydrophobicity enables less active water and less absorbed water on the Zn anode surface, which suppresses the parasitic water reductions; while the hydroxyl-ion-scavenging functionality further minimizes undesired passivation layer formation, thus leading to superior reversibility (an average Zn plating/stripping efficiency of 99.72% for 1000 cycles) and lifetime (80.6% capacity retention after 5000 cycles) of zinc batteries.

25 ENERGY STORAGE↗

Does Confinement Mediate Cerium Exchange and Its Impact on Ionomer Properties?

Thin-film ionomers, pivotal in the function of fuel-cell catalyst layers (CLs), are undercharacterized compared to their bulk membrane counterparts, especially with respect to cation effects. Cerium cations, used as an additive in fuel-cell membranes, tend to migrate from the membrane into the CL ionomer during operation. Further, this study investigates whether cerium doping of perfluorinated sulfonic acid ionomer changes under confinement (to a nanometer thin film) and affects the hydration behavior. Confinement has a negligible effect on the ionomer’s cerium partitioning, yet it reduces the ionomer water uptake. Thus, cerium replaces protons similarly in a membrane or CL ionomer; however, its presence affects the thermodynamics of hydration differently.

36 MATERIALS SCIENCE↗

Local structural distortions drive magnetic molecular field in compositionally complex spinel oxide

Understanding how local distortions determine the functional properties of high entropy materials, containing five or more elements at the same crystallographic site, is an open challenge. We address this for a compositionally complex spinel oxide (Mn 0.2 Co 0.2 Ni 0.2 Cu 0.2 Zn 0.2 )Cr 2 O 4 (A 5 Cr 2 O 4 ). By comparatively examining extended X-ray absorption fine structure on A 5 Cr 2 O 4 and its parent counterparts, ACr 2 O 4 , along with density functional theory calculations for multiple configurations, we find that the element-specific distortions go beyond the first neighbor. Specifically, the strong Jahn-Teller distortion present in CuCr 2 O 4 is found to be completely suppressed in A 5 Cr 2 O 4 even locally. Instead, there is a broad distribution of Cu-O and Cu-Cr bond distances, while other A-O distances acquire certain specific values. This study demonstrates the additional flexibility of a cationic sublattice in maintaining a uniform long-range structure, in contrast to previous reports showing only the accommodative anionic sublattice. The mean-field magnetic interactions of A 5 Cr 2 O 4 exhibit a striking resemblance to those of NiCr 2 O 4 , despite the presence of multiple magnetic ions and variable bond lengths. This originates from the comparability of bond lengths around Cr in both materials. Our study paves the way for a deeper understanding of the impact of local structural distortions on the physical properties of compositionally complex quantum materials.

36 MATERIALS SCIENCE↗

tert-butoxides as precursors for atomic layer deposition of alkali metal containing thin films

Alkali metal containing materials have become increasingly attractive in a world hunting for sustainable energy materials and green functional devices. Lithium- and sodium battery technology, lead-free piezo- and ferroelectric devices, and record-breaking alkali doped tandem perovskite solar cells are among the applications where alkali metal-containing thin films get increasing attention. Atomic layer deposition (ALD) is one of the enabling thin film deposition techniques that offer chemical and geometrical versatility to realize the implementation of such thin films on an applicable scale. The drawback has until recently been a lack of available precursor chemistry that offers self-limiting growth that is fundamental to ALD. The alkali metal tert-butoxides have been shown to exhibit the necessary properties to facilitate saturating growth for Li-, Na-, K-, and Rb-containing compounds. However, the behavior of the tert-butoxides in ALD-growth has been considered difficult to unravel, with processes exhibiting limited control and low reproducibility. Very little has been reported on trends in reaction mechanisms as the mass of the alkali metal increases. Herein, we summarize the existing literature on the use of alkali metal tert-butoxides as precursors in ALD. We consider differences in the structure and behavior of the tert-butoxides as the alkali metal cation becomes heavier. In addition, we present precursor synthesis routes and key information on precursor structure, stability, and mechanistic behavior. Finally, we provide the first ever report of Cs-containing films by ALD to complement previous work on its lighter counterparts.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Stable, Efficient Iron Electrodeposition via Anion-Directed Control of Fe(II) Coordination

Traditional steelmaking processes consume about 7% of the world’s energy supply, with reduction of iron oxides into iron via blast furnaces representing the most energy-demanding and capital-intensive step. To economize and modularize iron reduction processes, we aim to develop an electrodeposition technique to reduce aqueous iron ions to metallic iron. However, the hydrogen reduction reaction (HER) occurs at a more positive standard reduction potential than the iron reduction reaction. In addition, aqueous Fe(II) cations easily precipitate at mildly acidic conditions (pH ≥ 3), which limits the deposition efficiency and degrades deposit quality. To address these challenges, we first search for anions that have intermediate coordination strength with Fe(II) based on the hard-soft acid-base theory, trading a slightly more negative Fe(II) reduction potential for a considerably broader pH stability range. We select citrate with predicted intermediate coordination strength, in combination with more weakly coordinating anions (e.g., SO 4 2- , Cl - ) to control the coordination structure of Fe 2+ for improved electrolyte stability and electrodeposition behavior. We find that citrate coordination stabilizes Fe 2+ -based electrolytes at higher pH conditions (4.8–5.5), significantly extending their shelf life while also suppressing HER during Fe electrodeposition by orders of magnitude. To measure Faradaic efficiencies (FE), we developed a straightforward, titration-based methodology to quantify the amount of deposited iron regardless of the rate of concurrent HER. Although coordination between citrate and Fe 2+ decreases the reduction potential of Fe(II), high FE (≥98%) was achieved at 10 mA cm -2 . FE and achievable deposition rates are tunable by both concentration and the ratio of Fe 2+ to citrate. In all cases, Raman spectroscopy and X-ray diffraction (XRD) reveal that iron deposition in citrate-containing electrolytes suppresses iron oxide/hydroxide precipitation, in contrast to deposits generated in citrate-free electrolytes. Altogether, this work demonstrates that citrate-mediated anion coordination enables high-purity iron electrodeposition with increased FE, high current density, and improved electrolyte stability. This multi-anion coordination strategy provides a versatile framework for designing stable electrolyte and efficient metal electrodeposition.

coordination↗

Exfoliation of Cu-Containing Poly(triazine imide): From Three-Dimensional to Two-Dimensional Particle Morphology

Controlling the morphological parameters of extended covalent organic frameworks remains challenging and represents an important yet often elusive metric of consideration. Typically, carbon nitride materials possess local ordering but remain largely amorphous in terms of their long-range order and orientation. This study probes the synthesis of a crystalline carbon nitride, poly(triazine imide) lithium bromide which possesses an atomically-precise extended structure, and demonstrates its exfoliation into a two-dimensional hexagonal sheet-like morphology. Furthermore, a previously unreported carbon nitride material, poly(triazine imide) copper bromide, or PTI-CuBr, was developed through an additional flux-assisted cation-exchange process and is shown to retain its internal Cu cations during solvothermal exfoliation. Characterization by dynamic light scattering and high-angle annular dark-field scanning electron microscopy reveals the morphological changes and captures the high aspect ratio of the thin carbon nitride sheets with <10 nm thickness while maintaining hundreds of nm in width. Additional characterization by energy-dispersive spectroscopy and X-ray photoelectron spectroscopy confirms that the Cu:Br:N molar ratio was maintained within the extended layers throughout the exfoliation process. This top-down synthesis approach differs from typical methods that isolate thin sheets for subsequent metal−cation coordination and illustrates the importance of maintaining oxygen-free conditions to minimize copper clustering. Thus, this new approach is demonstrated to provide a consistent and more homogeneous occupancy of the PTI pore spaces throughout the carbon nitride framework.

Exfoliation↗

Influences of Alkali Metal Cation Interactions on N2 Coordination to Iron(I) Beta-Diketiminate Complexes in Electrolyte Solutions

N2 functionalization reactions often use stable, isolable N2-bound complexes and low temperatures or highly activated reagents. However, little work has focused on systems where N2 binds weakly, and the N2 binding equilibrium can be modulated. Here, we describe analysis of surprising trends in alkali metal cation solvation on the formation of an anionic iron(I) beta-diketiminate complex and the subsequent N2 binding equilibrium. Variable temperature UV-vis spectroscopy shows that increased ionic strength in the coordinating solvent tetrahydrofuran promotes N2 coordination. Additionally, less solvated alkali metal cations in noncoordinating 2-methyltetrahydrofuran (MeTHF) stabilize N2 coordination, likely through the formation of contact ion pairs in solution that have enhanced N2 binding. Ionic strength has little effect on the energetics of N2 coordination to these proposed contact ion pairs in MeTHF. When the electrochemical analysis is done at –78 °C, there is an irreversible reduction of iron(II) and an anodically shifted oxidation, which is attributed to the formation of the spectroscopically observed N2 complex. Finally, bulk electrolysis is used to verify the electrochemical formation of the N2-bound anionic iron(I) complex. These studies demonstrate a new strategy for promoting N2 coordination by changing solution properties, which is relevant to homogeneous electrochemical N2 reduction methods.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Cations Enhance Hydride Transfer to Noncatalytic Metals in Concentrated Alkaline Electrolytes

Alkali metal cations are known to influence the kinetics of the hydrogen evolution reaction (HER), acting as either promoters or inhibitors to the rate-determining step depending on the metal surface, local pH, and cation concentration. Despite the importance of concentrated electrolytes for commercial electrochemical cells, the impact of cations on the HER in concentrated alkaline environments (>1 M) and in mixed cation systems remains poorly understood. Here, this study quantifies the HER kinetics at polycrystalline metal surfaces (Pt, Au, Cu, and Fe) and the equilibrium solvation environment in pure and mixed alkali metal hydroxide electrolytes at concentrations up to 3.0 M. Kinetic analyses of Au, Cu, and Fe revealed a positive cation-concentration-effect that was primarily driven by changes to the charge transfer coefficient. Multinuclear NMR spectroscopy examined the solvation of H 2 O/OH – species and the alkali cations as a function of (mixed) alkali cation concentration(s), and demonstrated rapid exchange between solvent, hydroxide, and solvated cations. Together, these findings support models where HER kinetics on noncatalytic metal surfaces in strongly alkaline conditions are primarily governed by the average polarization and polarizability of the metal/solution interface and that increasing cation activity continues to increase the transfer coefficient at metal-hydroxide concentrations up to 3.0 M. Electrolytes and additives which can outcompete weakly hydrated cations and disrupt the interfacial water structure are expected to suppress parasitic HER at electrodes for energy storage and electroplating.

Cations↗

A redox-active organic cation for safer high energy density Li-ion batteries

Ni-rich layered cathode materials are at the forefront to be deployed in high energy density Li-ion batteries for the automotive market. However, the intrinsic poor structural and interfacial stability during overcharging could trigger violent thermal failure, which severely limits their wide application. To protect the Ni-rich cathode from overcharging, we firstly report a redox-active cation, thioether-substituted diaminocyclopropenium, as an electrolyte additive to limit the cell voltage within the safe value during overcharging. The organic cation demonstrates a record-breaking electrochemical reversibility at ~4.55 V versus Li + /Li and solubility (0.5 M) in carbonate-based electrolyte. The protection capability of the additive was explored in two cell chemistries: a LiNi 0.8 Co 0.15 Al 0.05 O 2 /graphite cell and a LiNi 0.8 Co 0.15 Al 0.05 O 2 /silicon–graphene cell with areal capacities of ~2.2 mA h cm -2 and ~3 mA h cm -2 , respectively. With 0.2 M addition, the LiNi 0.8 Co 0.15 Al 0.05 O 2 /graphite cell survived 54 cycles at 0.2C with 100% overcharge. Moreover, the cell can carry an utmost 4.4 mA cm -2 (2C) with 100% overcharge and a maximum capacity of 7540% SOC at 0.2C.

25 ENERGY STORAGE↗

Investigation of Key Electronic States in Layered Mixed Chalcogenides With a d 0 Transition Metal as Li-Ion Cathodes

Lithium-rich transition metal chalcogenides are witnessing a revival as candidates for Li-ion cathode materials, spurred by the boost in their capacities from transcending conventional redox processes based on cationic states and tapping into additional chalcogenide states. A particularly striking case is Li 2 TiS 3-y Se y , which features a d 0 metal. While the end members are expectedly inactive, substantial capacities are measured when both Se and S are present. Using X-ray absorption spectroscopy, it is shown that the electronic structure of Li 2 TiS 3-y Se y is not a simple combination of the end members. The data confirm previous hypotheses that, in Li 2 TiS 2.4 Se 0.6 , this behavior is underpinned by concurrent and reversible redox of only S and Se, and identify key electronic states. Moreover, wavelet transforms of the extended X-ray absorption fine structure provide direct evidence of the formation of short Se–Se units upon charging. The study uncovers the underpinnings of this intriguing reactivity and highlights the richness of redox chemistry in complex solids.

25 ENERGY STORAGE↗

Elucidating the speciation of extracted lanthanides by diglycolamides

Many studies over the past few decades have been devoted to addressing the application of diglycolamides (DGAs) for hydrometallurgical-based, f-element separations. Work to date has shown the molecular structure of a DGA derivative can have a significant impact on intra-lanthanide partitioning patterns. More recent studies have pushed towards probing the structure function relationship of the lanthanide-DGA complex to enable the design of more efficient lanthanide separation systems. Spectroscopic techniques, such as UV–Visible, Fourier Transformed Infrared Spectroscopy (FT-IR), Nuclear Magnetic Resonance (NMR), and Extended X-ray Absorption Fine Structure (EXAFS), provide information regarding the inner-sphere coordination of a given lanthanide-DGA complex. Scattering techniques, such as Dynamic Light Scattering (DLS), Small-Angle X-ray Scattering (SAXS), and Small-Angle Neutron Scattering (SANS), address nanoscale structures including aggregate sizes and morphology. Here, this review assesses the current state-of-knowledge regarding lanthanide-DGA hydrometallurgical (i.e., solvent extraction systems) interrogated using spectroscopic and scattering techniques to characterize the extracted Ln 3+ DGA species. Of particular interest to this review is the impact of varied diluents, inclusion and variation of phase modifiers, and DGA derivatization on system characteristics. While there has been extensive literature on the application of DGAs for f-element separations, the literature lacks a collective assessment of the speciation of Ln 3+ in the organic phase. This review provides new insights into the field of DGA separations, explicitly with an application to intra-lanthanide separations. Specifically, this review illustrates the importance of both the co-extraction anion (Cl - , NO 3 - , or ClO 4 - ) as it pertains to both the aggregate size and Ln 3+ distribution coefficient. It is evident the ability of the anion to disrupt the hydrogen bonding network limits both aggregate size and distribution coefficients according to the Hoffmeister series. This suggests the importance of the large, softer anions with a low charge-to-surface area ratio on encouraging hydrogen bond interactions. In addition, the co-extracted cation (H + vs Na + ) is important for mitigating transfer of Ln 3+ from the aqueous to the organic phase through extensive hydrogen bonding networks. These networks are responsible for forming supramolecular aggregates where a change in morphology is observed with increasing concentrations of H + and/or Ln 3+ in the organic phase.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Impact of Ion–Ion Correlated Motion on Salt Transport in Solvated Ion Exchange Membranes

The influence of dynamical ion-ion correlations and ion pairing on salt transport in ion exchange membranes remain poorly understood. In this study, we use the framework of Onsager transport coefficients within atomistic molecular dynamics sim- ulations to study the impact of ion-ion correlated motion on salt transport in hydrated polystyrene sulfonate membranes and compare with the results from aqueous salt so- lutions. At sufficiently high salt concentrations, cation-anion dynamical correlations exert a significant influence on both salt diffusivities and conductivities. Anion-anion distinct correlations, arising from the imbalance between the concentration of free (mo- bile) cations and anions, and the retarding effect of the fixed charge groups on cations, proves to be an additional important feature for polymer membranes. Furthermore, our results demonstrate that dynamical correlations should become an important consideration in experimental measurements of salt diffusivities and conductivities for non-dilute salt solutions in polymer membranes.

36 MATERIALS SCIENCE↗

Phosphine/Photoredox Catalyzed Anti-Markovnikov Hydroamination of Olefins with Primary Sulfonamides via α-Scission from Phosphoranyl Radicals

New strategies to access radicals from common feedstock chemicals hold the potential to broadly impact synthetic chemistry. Here, we report a dual phosphine and photoredox catalytic system that enables direct formation of sulfonamidyl radicals from primary sulfonamides. Mechanistic investigations support that the N-centered radical is generated via α-scission of the P–N bond of a phosphoranyl radical intermediate, formed by sulfonamide nucleophilic addition to a phosphine radical cation. As compared to the recently well-explored β-scission chemistry of phosphoranyl radicals, this strategy is applicable to activation of N-based nucleophiles and is catalytic in phosphine. We highlight application of this activation strategy to an intermolecular anti-Markovnikov hydroamination of unactivated olefins with primary sulfonamides. A range of structurally diverse secondary sulfonamides can be prepared in good to excellent yields under mild conditions.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Stabilizing Ru-Formyl CO 2 Reduction Intermediates by Formation of Lewis Acid–Base Adducts: A Combined 2DIR and NMR Study

This work demonstrates how the stability of a Ru(II) formyl complex (cis-[Ru(bpy) 2 (CO)(CHO)][PF 6 ]), which is known to decarbonylate to form the metal hydride complex, is greatly enhanced by the addition of a Lewis acidic cation (Li + or Mg 2+ ). Multinuclear NMR is used to measure equilibrium constants of adduct formation, and then ultrafast 2DIR spectroscopy is applied to determine how the electronic structure and local molecular dynamics change upon complexation of the formyl ligand with the Lewis acid. We attribute the stabilization of the complex to the formation of a carbene-like structure where the bond strength between the Ru and the formyl group increases. The change in electronic structure is evidenced by steady-state NMR spectroscopy and DFT calculations. 2DIR measurements further confirm both the complexation of the formyl ligand with the Lewis acid and the change in electronic structure, where changes in vibrational frequency, relaxation kinetics, and a slowdown in the time scale of rotation about the metal-formyl bond are observed in the presence of Lewis acids.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Plant defensin MtDef4–derived antifungal peptide with multiple modes of action and potential as a bio–inspired fungicide

Chemical fungicides have been instrumental in protecting crops from fungal diseases. However, increasing fungal resistance to many of the single-site chemical fungicides calls for the development of new antifungal agents with novel modes of action (MoA). The sequence-divergent cysteine-rich antifungal defensins with multisite MoA are promising starting templates for design of novel peptide-based fungicides. Here, we experimentally tested such a set of 17-amino-acid peptides containing the γ-core motif of the antifungal plant defensin MtDef4. These designed peptides exhibited antifungal properties different from those of MtDef4. Focused analysis of a lead peptide, GMA4CG_V6, showed that it was a random coil in solution with little or no secondary structure elements. Additionally, it exhibited potent cation-tolerant antifungal activity against the plant fungal pathogen Botrytis cinerea, the causal agent of grey mould disease in fruits and vegetables. Its multisite MoA involved localization predominantly to the plasma membrane, permeabilization of the plasma membrane, rapid internalization into the vacuole and cytoplasm, and affinity for the bioactive phosphoinositides phosphatidylinositol 3-phosphate (PI3P), PI4P, and PI5P. The sequence motif RRRW was identified as a major determinant of the antifungal activity of this peptide. While topical spray application of GMA4CG_V6 on Nicotiana benthamiana and tomato plants provided preventive and curative suppression of grey mould disease symptoms, the peptide was not internalized into plant cells. Our findings open the possibility that truncated and modified defensin-derived peptides containing the γ-core sequence could serve as promising candidates for further development of bio-inspired fungicides.

54 ENVIRONMENTAL SCIENCES↗

Is the Chemisorbed CO 2 in Ionic Liquid Electrolytes Active for Electrochemical Utilization? A Case Study on Carboxylate and Carbamate Speciation

This study examines the activity of chemisorbed CO 2 species in the microenvironment formed by bifunctional ionic liquids (ILs) in the reactive capture and conversion (RCC) of CO 2 to CO on silver. Comparative electroanalytical measurements with imidazolium based ILs were performed to probe the impact of electrostatic interactions, anion and cation basicity, and hydrogen bonding on RCC. Particularly, ILs with 1-ethyl-3-methylimidazolium ([EMIM]+) and 1-ethyl-2,3-dimethylimidazolium ([EMMIM]+) cations and aprotic heterocyclic anions of 2-cyanopyrrolide ([2-CNpyr]) and 1,2,4-triazolide ([124-Triz]) were examined for RCC. It was found that anion–CO 2 carbamate complexes facilitate RCC at significantly lower overpotentials compared to cation–CO 2 carboxylate complexes. Additionally, [EMIM]+ was found to better stabilize anion–CO 2 complexes at the interface than [EMMIM]+. Furthermore, it was found that 2-CNpyrH that naturally forms during CO 2 absorption competes for electrode surface adsorption with the anion–CO 2 carbamate complex, thereby reducing the electrochemical activity of the anion–CO 2 complex. These results highlight the importance of IL structure in tuning the interfacial interactions and suggest that ILs with anion-dominated CO 2 chemisorption enhances CO 2 utilization in RCC applications.

Coskun, Oguz Kagan [Case Western Reserve Univ., Cl↗

MOCVD Growth and Characterization of ZnSnN 2

Since the first few reports of its synthesis in 2011 and 20121-3, interest in ZnSnN 2 for diverse applications, including photovoltaics1,3,4, visible light photocatalysis5, and optoelectronics, has been growing. Novel nitride-based LED device designs promise high gains in efficiency at emission wavelengths into the green, amber and even red.6-8 Their realization requires the precise insertion of an ultrathin layer of ZnGeN 2 or ZnSnN 2 into the active region of an InGaAs-GaAs LED structure. While thin films of ZnSnN 2 have been synthesized by RF sputtering1,9 and by MBE 2,10,11, and thin films of ZnGeN 2 , ZnSiN 2 and their alloys by MOCVD, the synthesis of ZnSnN 2 thin films by MOCVD has not yet been reported. It is a challenging goal, given the narrow temperature window between efficient activation of ammonia and the thermal decomposition of ZnSnN 2 at near-atmospheric pressures. We report here the results of studies of ZnSnN 2 films grown on r- and c-plane sapphire substrates, GaN templates on sapphire, and In 0.15 Ga 0.85 N templates on GaN-on-sapphire, at temperatures from 500 °C to 560 °C, using tetramethyltin (TMSn), diethylzinc (DEZn), germane and ammonia. Chamber pressures were varied between 200 and 500 torr. In addition, the ratios of the cation precursors and the total cation-to-anion precursor ratios were varied. Single crystal growth, as evidenced by 2θ-ω x-ray diffraction scans, was achieved on all of these substrates. Wurtzitic (0002) ZnSnN 2 diffraction were observed at 2θ ~ 32.90 for the samples grown on c-sapphire, GaN (0001) and InGaN (0001) templates, and wurtzitic (11-20) peak at 2θ ~ 54.80 for the films grown on r-sapphire. Higher pressures and higher temperatures promoted better crystallinity and more continuous films, as revealed by scanning electron microscopy (SEM) images and 2θ-ω x-ray diffraction peak widths and intensities. Crystal quality was observed to be highly dependent on growth temperature. For example, in one series a 10 °C change in growth temperature resulting in a factor of 15 increase in diffraction peak intensity. SEM images show that films grown on the GaN templates had better uniformity in nucleation than those grown on sapphire. The presence of satellite peaks around the Bragg peak in the XRD 2θ-ω scan for a film grown on a GaN template, and the absence of satellite peaks for the films grown simultaneously on c- and r-sapphire, also indicate superior quality for the film grown on GaN. HAADF-STEM images of films grown on these templates showed smooth interfaces at the film-substrate boundary and show growth rates as high as 167 nm/h, considerably higher than reported previously for MBE growth.9,10 Electron diffraction patterns show single crystallinity. Rocking curves show FWHM as low as 0.100. RMS surfaces roughnesses, measured by atomic force microscopy, are of the order of 3 nm for 1µm x 1µm areas. Current work is focusing on optimizing growth on InGaN templates. These templates are promising for their relatively lower lattice mismatch with ZnSnN 2 . Their use is a next step toward producing LED device structures.

Jayatunga, Benthara Hewage Dinushi↗