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At least 127 records · Page 7

Photodriven Ammonia Synthesis from Manganese Nitrides: Photophysics and Mechanistic Investigations

Ammonia synthesis from N,N,O,O-supported manganese(V) nitrides and 9,10-dihydroacridine using proton-coupled electron transfer and visible light irradiation in the absence of precious metal photocatalysts is described. While the reactivity of the nitride correlated with increased absorption of blue light, excited-state lifetimes determined by transient absorption were on the order of picoseconds. Furthermore, this eliminated excited-state manganese nitrides as responsible for bimolecular N–H bond formation. Spectroscopic measurements on the hydrogen source, dihydroacridine, demonstrated that photooxidation of 9,10-dihydroacridine was necessary for productive ammonia synthesis. Transient absorption and pulse radiolysis data for dihydroacridine provided evidence for the presence of intermediates with weak E–H bonds, including the dihydroacridinium radical cation and both isomers of the monohydroacridine radical, but notably these intermediates were unreactive toward hydrogen atom transfer and net N–H bond formation. Additional optimization of the reaction conditions using higher photon flux resulted in higher rates of the ammonia production from the manganese(V) nitrides due to increased activation of the dihydroacridine.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Epitaxial integration of superconducting nitrides with cubic GaN

Epitaxial combination of transition metal nitrides and group III-nitrides holds significant potential for novel device architectures, given their wide array of properties and similar lattice constants. However, the mixture of hexagonal and cubic crystals limits structural quality and has stymied development. This work will discuss the molecular beam epitaxy synthesis of metastable cubic GaN on 3C-SiC templates and its integration with cubic ZrN and NbN superconductors in single and multilayer heterostructures. The fully cubic nature of GaN and the epitaxial nature of all layers are confirmed via in situ and ex situ techniques. The electrical transport properties of transition metal nitrides on cubic GaN (001) are compared to those grown directly on 3C-SiC (001) and c-plane hexagonal GaN templates. The determination of a similar growth window for cubic wide-bandgap and superconducting metal nitrides creates a platform for new epitaxial device architectures and potential applications in metamaterials, quantum information science, and condensed matter physics.

Condensed matter physics↗

Synthesis of LaWN 3 nitride perovskite with polar symmetry

Perovskite structured materials have a variety of uses as photovoltaics, capacitors, and micromechanical actuators, along with other applications. Oxides, halides, and chalcogenides all have large numbers of perovskite structured materials. Examples of perovskite nitrides are conspicuously absent, but Talley et al managed to synthesize one (see the Perspective by Hong). Lanthanum tungsten nitride in the perovskite structure turns out to be piezoelectric, which is ideal for a variety of applications. Perovskite structured nitrides are very attractive because they could easily integrate with the large number of nitride-based semiconducting devices already in use.

36 MATERIALS SCIENCE↗

ZrN Phase Formation, Hardening and Nitrogen Diffusion Kinetics in Plasma Nitrided Zircaloy-4

Plasma nitridation was conducted to modify the surfaces of Zircaloy-4. Scanning electron microscopy (SEM), transmission electron microscopy (TEM), and Raman analysis were used to characterize microstructures and phases. Surface indentation and cross-sectional indentation were performed to evaluate mechanical property changes. Nitridation forms a thin layer of ZrN phase, followed by a much deeper layer affected by nitrogen diffusion. The ZrN phase is confirmed by both TEM and Raman characterization. The Raman peaks of ZrN phase show a temperature dependence. The intensity increases with increasing nitridation temperatures, reaches a maximum at 700 °C, and then decreases at higher temperatures. The ZrN layer appears as continuous small columnar grains. The surface polycrystalline ZrN phase is harder than the bulk by a factor of ~8, and the nitrogen diffusion layer is harder by a factor of ~2–5. The activation energy of nitrogen diffusion was measured to be 2.88 eV. The thickness of the nitrogen-hardened layer is controllable by changing the nitridation temperature and duration.

36 MATERIALS SCIENCE↗

Phase-Controllable Synthesis of Ultrathin Molybdenum Nitride Crystals Via Atomic Substitution of MoS 2

MXenes are emerging members in the two-dimensional (2D) material family and are highlighted by their high electrical conductivity. Among different MXenes, molybdenum-based MXenes, especially molybdenum nitrides (MoN x ), are rarely accessible through the common synthetic approach of selective etching due to the absence of stable MAX phase precursors. In this work, we apply the atomic substitution approach to synthesize two phases of ultrathin nonlayered molybdenum nitrides (i.e., Mo 5 N 6 and δ-MoN) from 1.6 to 42.9 nm thickness by converting layered MoS 2 under different temperatures. The morphology and 2D nature of MoS 2 are well remained in both phases. These newly created 2D materials are further characterized using Raman spectroscopy, high-resolution transmission electron microscopy, and electrical measurements, suggesting that both phases are highly crystalline and highly conductive down to the thickness of a few nanometers. Moreover, Ohmic contacts are formed between the ultrathin nitrides and Cr/Au electrodes, suggesting the great potential of the obtained nitrides for nanoelectronic device applications. The stability test shows that the Ohmic contact is well maintained after 4 weeks under ambient conditions with a slight degradation in conductivity. Furthermore, this study extends the 2D family by providing highly conductive members, offering desired building blocks for solid-state nanoelectronic devices.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

Synthesis and Physical Properties of Manganese Chromium Nitride Thin Films Grown via Molecular Beam Epitaxy

Here, we demonstrate the ability to grow epitaxial thin films of manganese–chromium nitride (Mn x Cr 1–x N) across the entire composition range on magnesium oxide (MgO) (1 0 0) surfaces by molecular beam epitaxy. By independently controlling the ratio of the atomic fluxes of manganese and chromium, the compositional dependence of structural and electrical transport properties is determined. Soft X-ray absorption shows that the valence states of Cr( 3+ ) and Mn( 3+ ) remain identical among these MnCrN epitaxial films. The metallic transport behavior of binary manganese nitride (MnN) and chromium nitride (CrN) is suppressed in the ternary alloys. Changes in room temperature electrical resistivity of up to 100 times and 5 orders of magnitude at cryogenic temperatures are observed. This work expands the variety of nitride compounds available for epitaxial integration and could provide additional flexibility for the development of metal–semiconductor–insulator junctions for spintronic devices.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Twisted-layer boron nitride ceramic with high deformability and strength

Moiré superlattices formed by twisted stacking in van der Waals materials have emerged as a new platform for exploring the physics of strongly correlated materials and other emergent phenomena. However, there remains a lack of research on the mechanical properties of twisted-layer van der Waals materials, owing to a lack of suitable strategies for making three-dimensional bulk materials. Here we report the successful synthesis of a polycrystalline boron nitride bulk ceramic with high room-temperature deformability and strength. This ceramic, synthesized from an onion-like boron nitride nanoprecursor with conventional spark plasma sintering and hot-pressing sintering, consists of interlocked laminated nanoplates in which parallel laminae are stacked with varying twist angles. The compressive strain of this bulk ceramic can reach 14% before fracture, about one order of magnitude higher compared with traditional ceramics (less than 1% in general), whereas the compressive strength is about six times that of ordinary hexagonal boron nitride layered ceramics. The exceptional mechanical properties are due to a combination of the elevated intrinsic deformability of the twisted layering in the nanoplates and the three-dimensional interlocked architecture that restricts deformation from propagating across individual nanoplates. The advent of this twisted-layer boron nitride bulk ceramic opens a gate to the fabrication of highly deformable bulk ceramics.

36 MATERIALS SCIENCE↗

Ion-beam assisted sputtering of titanium nitride thin films

Abstract Titanium nitride is a material of interest for many superconducting devices such as nanowire microwave resonators and photon detectors. Thus, controlling the growth of TiN thin films with desirable properties is of high importance. This work aims to explore effects in ion beam-assisted sputtering (IBAS), were an observed increase in nominal critical temperature and upper critical fields are in tandem with previous work on Niobium nitride (NbN). We grow thin films of titanium nitride by both, the conventional method of DC reactive magnetron sputtering and the IBAS method, to compare their superconducting critical temperatures $$T_{c}$$ T c as functions of thickness, sheet resistance, and nitrogen flow rate. We perform electrical and structural characterizations by electric transport and x-ray diffraction measurements. Compared to the conventional method of reactive sputtering, the IBAS technique has demonstrated a 10% increase in nominal critical temperature without noticeable variation in the lattice structure. Additionally, we explore the behavior of superconducting $$T_c$$ T c in ultra-thin films. Trends in films grown at high nitrogen concentrations follow predictions of mean-field theory in disordered films and show suppression of superconducting $$T_c$$ T c due to geometric effects, while nitride films grown at low nitrogen concentrations strongly deviate from the theoretical models.

36 MATERIALS SCIENCE↗

On the mechanism of intermolecular nitrogen-atom transfer from a lattice-isolated diruthenium nitride intermediate

Catalyst confinement within microporous media provides the opportunity to site isolate reactive intermediates, enforce intermolecular functionalization chemistry by co-localizing reactive intermediates and substrates in molecular-scale interstices, and harness non-covalent host–guest interactions to achieve selectivities that are complementary to those accessible in solution. As part of an ongoing program to develop synthetically useful nitrogen-atom transfer (NAT) catalysts, we have demonstrated intermolecular benzylic amination of toluene at a Ru 2 nitride intermediate confined within the interstices of a Ru2-based metal–organic framework (MOF), Ru 3 (btc) 2 X 3 (btc = 1,3,5-benzenetricarboxylate, i.e., Ru-HKUST-1 for X = Cl). Nitride confinement within the extended MOF lattice enabled intermolecular C–H functionalization of benzylic C–H bonds in preference to nitride dimerization, which was encountered with soluble molecular analogues. Detailed study of the kinetic isotope effects (KIEs, i.e., k H /k D ) of C–H amination, assayed both as intramolecular effects using partially labeled toluene and as intermolecular effects using a mixture of per-labeled and unlabeled toluene, provided evidence for restricted substrate mobility on the time scale of interstitial NAT. Analysis of these KIEs as a function of material mesoporosity provided approximate experimental values for functionalization in the absence of mass transport barriers. Here, we disclose a combined experimental and computational investigation of the mechanism of NAT from a Ru 2 nitride to the C–H bond of toluene. Computed kinetic isotope effects for a H-atom abstraction (HAA)/radical rebound (RR) mechanism are in good agreement with experimental data obtained for C–H amination at the rapid diffusion limit. These results provide the first detailed analysis of the mechanism of intermolecular NAT to a C–H bond, bolster the use of KIEs as a probe of confinement effects on NAT within MOF lattices, and provide mechanistic insights unavailable by experiment because rate-determining mass transport obscured the underlying chemical kinetics.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Computational discovery of a novel double transition metal nitride MXene and its applications as an anchoring and catalytic material in Li–Se batteries

Double transition metal (DTM) nitride MXenes offer enhanced electrical conductivity and tunable catalytic properties compared to conventional carbide-based MXenes. In this study, we employed first-principles density functional theory (DFT) calculations to discover and computationally validate a novel DTM nitride MXene, Nb 2 TiN 2 , derived from its MAX phase precursor and investigated its potential as an anchoring material (AM) for Li–Se batteries. This newly proposed MXene expands the compositional landscape of DTM nitrides and opens new avenues for functional material design. We performed a comprehensive analysis of the thermodynamic and electronic properties of Nb 2 TiAlN 2 , and the MAX phase precursor to Nb 2 TiN 2 to assess its structural stability and exfoliation potential. Exfoliation energy calculations confirmed the feasibility of synthesizing Nb 2 TiN 2 from Nb 2 TiAlN 2 . We then explored the functionalized form, Nb 2 TiN 2 S 2 , evaluating its capability to serve as an effective anchoring material (AM) in Li–Se batteries by analyzing the reaction mechanisms and kinetics of the selenium reduction reaction (SeRR). Our results indicate that Nb 2 TiN 2 S 2 exhibits a strong binding affinity for lithium polyselenides (Li 2 Se n ), effectively suppressing the shuttle effect. Gibbs free energy calculations for the rate-limiting step of the SeRR reveal favorable kinetics and reduced reaction barriers. Overall, this study provides a detailed evaluation of the structural and electronic properties of a newly proposed DTM nitride MXene and its S-functionalized derivative and the catalyzing effect of Nb 2 TiN 2 S 2 in accelerating the reaction kinetics in Li–Se batteries. These findings underscore the potential importance of the further exploration of MXenes to address current challenges in high-performance Li–Se batteries.

25 ENERGY STORAGE↗

Solar-Thermal Ammonia Production Via a Nitride Looping Cycle [Slides]

Solar Thermal Ammonia Production has the potential to synthesize ammonia in a green, renewable process that can greatly reduce the carbon footprint left by conventional Haber-Bosch reaction. Ternary nitrides in the family A 3 B x N (A=Co, Ni, Fe; B=Mo; x=2,3) have been identified as a potential candidate for NH 3 production. Experiments with Co 3 Mo 3 N in Ammonia Synthesis Reactor demonstrate cyclable NH 3 production from bulk nitride under pure H 2 . Production rates were fairly flat in all the reduction steps with no evident dependence on the consumed solid-state nitrogen, as would be expected from catalytic Mars-van Krevelen mechanism. Material can be re-nitridized under pure N 2 . Bulk nitrogen per reduction step average between 25 – 40% of the total solid-state nitrogen. Selectivity to NH 3 stabilized at 55 – 60% per cycle. Production rates (NH 3 and N 2 ) become apparent above 600 °C at P(H 2 ) = 0.5 – 2 bar. Optimal point of operation to keep selectivity high without compromising NH 3 rates currently estimated at 650 °C and 1.5 - 2 bar. The next steps are to optimize production rates, examine effect of N 2 addition in NH 3 synthesis reaction, and test additional ternary nitrides.

14 SOLAR ENERGY↗

Gallium nitride optoelectronic devices

The growth of bulk gallium nitride crystals was achieved by the ammonolysis of gallium monochloride. Gallium nitride single crystals up to 2.5 x 0.5 cm in size were produced. The crystals are suitable as substrates for the epitaxial growth of gallium nitride. The epitaxial growth of gallium nitride on sapphire substrates with main faces of (0001) and (1T02) orientations was achieved by the ammonolysis of gallium monochloride in a gas flow system. The grown layers had electron concentrations in the range of 1 to 3 x 10 to the 19th power/cu cm and Hall mobilities in the range of 50 to 100 sq cm/v/sec at room temperature.

Chu, T. L.↗

Method and apparatus for stable silicon dioxide layers on silicon grown in silicon nitride ambient

A method and apparatus for thermally growing stable silicon dioxide layers on silicon is disclosed. A previously etched and baked silicon nitride tube placed in a furnace is used to grow the silicon dioxide. First, pure oxygen is allowed to flow through the tube to initially coat the inside surface of the tube with a thin layer of silicon dioxide. After the tube is coated with the thin layer of silicon dioxide, the silicon is oxidized thermally in a normal fashion. If the tube becomes contaminated, the silicon dioxide is etched off thereby exposing clean silicon nitride and then the inside of the tube is recoated with silicon dioxide. As is disclosed, the silicon nitride tube can also be used as the ambient for the pyrolytic decomposition of silane and ammonia to form thin layers of clean silicon nitride.

Cohen, R. A.↗

Rolling-element fatigue life of silicon nitride balls

The five-ball fatigue tester was used to evaluate silicon nitride as a rolling-element bearing material. Results indicate that hot-pressed silicon nitride running against steel may be expected to yield fatigue lives comparable to or greater than those of bearing quality steel running against steel at stress levels typical rolling-element bearing application. The fatigue life of hot-pressed silicon nitride is considerably greater than that of any ceramic or cermet tested. Computer analysis indicates that there is no improvement in the lives of 120-mm-bore angular--contact ball bearings of the same geometry operating at DN values from 2 to 4 million where hot-pressed silicon nitride balls are used in place of steel balls.

Parker, R. J.↗

Fatigue life of high-speed ball bearings with silicon nitride balls

Evaluation of hot-pressed silicon nitride as a rolling-element bearing material. Two grades of hot-pressed silicon nitride balls were tested under rolling contact conditions in a five-ball fatigue tester. A digital computer program was used to predict the dynamic performance characteristics and fatigue life of high-speed ball bearings with silicon nitride balls relative to that with bearings containing steel balls. The results obtained include the finding that fatigue spalls on silicon nitride balls are similar in appearance to those obtained with typical bearing steels.

Parker, R. J.↗

Improved reaction sintered silicon nitride

Processing treatments were applied to as-nitrided reaction sintered silicon nitride (RSSN) with the purposes of improving strength after processing to above 350 MN/m2 and improving strength after oxidation exposure. The experimental approaches are divided into three broad classifications: sintering of surface-applied powders; impregnation of solution followed by further thermal processing; and infiltration of molten silicon and subsequent carburization or nitridation of the silicon. The impregnation of RSSN with solutions of aluminum nitrate and zirconyl chloride, followed by heating at 1400-1500 C in a nitrogen atmosphere containing silicon monoxide, improved RSSN strength and oxidation resistance. The room temperature bend strength of RSSN was increased nearly fifty percent above the untreated strength with mean absolute strengths up to 420 MN/m2. Strengths of treated samples that were measured after a 12 hour oxidation exposure in air were up to 90 percent of the original as-nitrided strength, as compared to retained strengths in the range of 35 to 60 percent for untreated RSSN after the same oxidation exposure.

Baumgartner, H. R.↗

Variations in pore structure of reaction-bonded silicon nitride /RBSN/

A discussion is presented relating the observed pore structures (sizes) to the reaction mechanisms in reaction-bonded silicon nitride (alpha- and beta-Si3N4) on the basis of information available from the literature. While the techniques for reducing the residual macroporosity are quite well-developed for reaction-bonded Si3N4 (RBSN), it is important to be aware of three other orders of magnitude for porosity present in RBSN as a result of the nitriding process itself, and how these types of nitridation-induced porosity can be controlled. For ease of description, these types of nitridation-induced porosity are called micropores, nanopores, and picopores in order of their decreasing size. A scanning electron micrograph is presented, showing nanopores isolated in the unreacted Si and picopores in the alpha-matte Si3N4. The assumption that an alpha-matte growth mechanism is active explains the occurrence of nanopores and their partial filling with alpha-Si3N4, leaving behind very fine-grained alpha-matte and picopores.

Danforth, S. C.↗

Development of silicon nitride of improved toughness

The application of reaction sintered Si2N4 energy absorbing surface layers to hot-pressed Si3N4 was investigated. The surface layer was formed by in-place nitridation of silicon powder. It was found that reaction sintered Si3N4 layers of 1 mm thickness, fabricated from either -100, +200, -200, or -325 mesh Si powder and nitrided in 96% N2/4% H2 so that approximately 20-25 vol % unnitrided Si remained in the layer, resulted in a sevenfold increase in ballistic impact resistance of a 0.64 cm thick hot-pressed SI3N4 substrate from RT 1370 C. Both NC-132 SI3N4, with MgO additive, and NCX-34 Si3N4, with Y2O3 additive, were evaluated as substrate material. The finer grain size -200 and -325 mesh nitrided Si layers were for their smoothness and relatively high density. It was found that nitriding in N2/H2 mixtures, rather than pure N2, resulted in a microstructure that did not substantially degrade the strength of the hot-pressed Si3N4 substrate. Thermal cycling tests on the RSSN/HPSN combinations from 200 C to 1370 C for 75 cycles in air did not degrade the impact resistance nor the interfacial bonding, although a large amount of internal silica formation occurred within the RSSN layer. Mach 0.8, 5 hr, hot gas erosion tests showed no surface recession of RSSN layers at 1200 C and slight surface recession at 1370 C.

Brennan, J. J.↗