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At least 55 records · Page 3
All sourcesNASA NTRSDOE OSTI
DOE OSTI2020

Mechanocatalytic Ammonia Synthesis over TiN in Transient Microenvironments

Environmentally friendly and energy-efficient ways to produce ammonia are essential to meet global food demands. In this study, a new approach for ammonia production at nominally ambient conditions is introduced. As proof of concept, ammonia is synthesized mechanocatalytically by ball milling titanium in a continuous gas flow. The ammonia synthesis reaction is proposed to follow a transient Mars–van Krevelen mechanism under mechanically activated conditions, where molecular nitrogen incorporation into the titanium lattice and titanium nitride hydrogenation occur in thermodynamically distinct environments. X-ray powder diffraction and X-ray absorption spectroscopy confirm the formation of titanium nitride from titanium and N2. The reactivity of nitrided titanium supports that lattice nitrogen plays a role in ammonia formation. The in situ formed titanium nitride is catalytically active, and the nitride regeneration reaction is determined to be the rate-limiting step. A preliminary technoeconomic analysis shows that this approach could be feasible for distributed ammonia production.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2022

Nanoporous Titanium (Oxy)nitride Films as Broadband Solar Absorbers

Broadband absorption of solar light is a key aspect in many applications that involve an efficient conversion of solar energy to heat. Titanium nitride (TiN)-based materials, in the form of periodic arrays of nanostructures or multilayers, can promote significant heat generation upon illumination thanks to their efficient light absorption and refractory character. In this work, pulsed laser deposition was chosen as a synthesis technique to shift metallic bulk-like TiN to nanoparticle-assembled hierarchical oxynitride (TiO x N y ) films by increasing the background gas deposition pressure. The nanoporous hierarchical films exhibit a tree-like morphology, a strong broadband solar absorption (~90% from the UV to the near-infrared range), and could generate temperatures of ~475 °C under moderate light concentration (17 Suns). The high heat generation achieved by treelike films is ascribed to their porous morphology, nanocrystalline structure, and oxynitride composition, which overall contribute to a superior light trapping and dissipation to heat. These properties pave the way for the implementation of such films as solar absorber structures.

14 SOLAR ENERGY↗
NASA NTRS1962

PYROLYTIC GRAPHITE ROCKET THRUST CHAMBER INVESTIGATION PROJECT. MONTHLY LETTER

This is the Monthly Letter Progress Report for the eighth month of a twelve month technical study directed toward the following objectives: A. Determining analytically and experimentally the feasibility and attractiveness of using free-standing pyrolytic graphite for a radiation cooled liquid rocket thrust chamber and exit nozzle for space application. B. Establishing through analysis and experimental demonstration, a set of design principles to facilitate the design of a reliable pyrolytic graphite thrust chamber assembly for a specific range of operating conditions. C. Demonstrate by means of test firings of complete thrust chamber assemblies, the validity of the design data and principles developed during the program. Preparations have been completed for test firing the two 100 lb. thrust Boron Pyralloy chambers at Marquardt during the first week in March 1962. These two chambers will first be static pressure checked with water to a pressure of 135 psig. The chambers will then be test fired with N204/N2H4-MMH propellants . Test samples of eleven different pyrolytic carbide and nitride materials have been ordered for high temperature oxidation tests and should be delivered by the end of March for evaluation in the plasma torch facility. The specific materials ordered in free- standing condition in thicknesses from 0.030 inch to 0.065 inch were as follows: (a) Pyrolytic graphite (on hand) (b) Pyrolytic graphite-boron alloy (on hand) (c) Pyrolytic graphite-tungsten alloy (d)Boron nitride (e) Titanium nitride (f) Silicon carbide (g) Titanium carbide (h) Zirconium carbide (i) Hafnium carbide (j) Niobium carbide (k) Tantalum carbide (l) High density (1 1-90) graphite (m) High density graphite (heat treated) These materials were ordered from Raytheon, HTM, and American Meta 1 Products . A summary of the available data on the oxidation rates of pyrolytic materials under slow air and rocket motor conditions is shown in Figure 1. High Temperature Materials, Inc. has been contacted relative to providing Pyrographite thrust chambers with extra-thick walls . They believe they can deliver chambers with substantially thicker walls than were possible a short time ago. Such a configuration, with acceptable residual stresses, would provide a longer firing life since it is ultimately limited by the oxidation rate of the chamber wall material. Stress and structural studies have continued. The analytical stress studies point out some of the problems associated with the experimental determination of the elastic constants of this highly anisotropic material. Further analysis may shed light on improved techniques for making these experimental determinations. The large potential weight saving available with the use of pyrolytic graphite as a thrust chamber wall material in a radiation cooled rocket motor has been calculated and is shown graphically in Figure 2. Figure A presents the program progress schedule and the actual expenditures as of 7 February 1962.

ROCKET ENGINE↗
NASA NTRS2023

Tribological and Radiation Shielding Response of Novel Titanium-Boron Nitride Coatings for Lunar Structural Components

Aluminum (Al) and titanium (Ti) lightweight alloys play a crucial role in space systems due to their exceptional strength-to-weight ratio. However, their premature failure in the presence of lunar regolith and their lack of neutron shielding ability are significant challenges. To address these issues, we have developed air and vacuum plasma-sprayed hBN (hexagonal Boron Nitride) -reinforced titanium coatings with 2 and 10 vol% of hBN. Tribological studies conducted with JSC-1 A lunar regolith simulant revealed a 90 % reduction in wear volume for the Ti/2 vol% hBN coatings compared to conventional materials due to the synergistic action of harder secondary phases and solid lubrication effect of hBN. Additionally, a 27 % enhancement in radiation shielding is obtained based on the mass absorption coefficient (radiation absorbed per sample density and thickness) for VPS Ti/2 vol% hBN coatings.

Wear↗
NASA NTRS2003

Thin Thermal-Insulation Blankets for Very High Temperatures

Thermal-insulation blankets of a proposed type would be exceptionally thin and would endure temperatures up to 2,100 C. These blankets were originally intended to protect components of the NASA Solar Probe spacecraft against radiant heating at its planned closest approach to the Sun (a distance of 4 solar radii). These blankets could also be used on Earth to provide thermal protection in special applications (especially in vacuum chambers) for which conventional thermal-insulation blankets would be too thick or would not perform adequately. A blanket according to the proposal (see figure) would be made of molybdenum, titanium nitride, and carbon- carbon composite mesh, which melt at temperatures of 2,610, 2,930, and 2,130 C, respectively. The emittance of molybdenum is 0.24, while that of titanium nitride is 0.03. Carbon-carbon composite mesh is a thermal insulator. Typically, the blanket would include 0.25-mil (.0.00635-mm)-thick hot-side and cold-side cover layers of molybdenum. Titanium nitride would be vapor-deposited on both surfaces of each cover layer. Between the cover layers there would be 10 inner layers of 0.15-mil (.0.0038-mm)-thick molybdenum with vapor-deposited titanium nitride on both sides of each layer. The thickness of each titanium nitride coat would be about 1,000 A. The cover and inner layers would be interspersed with 0.25-mil (0.00635-mm)-thick layers of carbon-carbon composite mesh. The blanket would have total thickness of 4.75 mils (approximately equal to 0.121 mm) and an areal mass density of 0.7 kilograms per square meter. One could, of course, increase the thermal- insulation capability of the blanket by increasing number of inner layers (thereby unavoidably increasing the total thickness and mass density).

Choi, Michael K.↗
DOE OSTI2021

Methods for tuning plasmonic and photonic optical resonances in high surface area porous electrodes

Abstract Surface plasmons have found a wide range of applications in plasmonic and nanophotonic devices. The combination of plasmonics with three-dimensional photonic crystals has enormous potential for the efficient localization of light in high surface area photoelectrodes. However, the metals traditionally used for plasmonics are difficult to form into three-dimensional periodic structures and have limited optical penetration depth at operational frequencies, which limits their use in nanofabricated photonic crystal devices. The recent decade has seen an expansion of the plasmonic material portfolio into conducting ceramics, driven by their potential for improved stability, and their conformal growth via atomic layer deposition has been established. In this work, we have created three-dimensional photonic crystals with an ultrathin plasmonic titanium nitride coating that preserves photonic activity. Plasmonic titanium nitride enhances optical fields within the photonic electrode while maintaining sufficient light penetration. Additionally, we show that post-growth annealing can tune the plasmonic resonance of titanium nitride to overlap with the photonic resonance, potentially enabling coupled-phenomena applications for these three-dimensional nanophotonic systems. Through characterization of the tuning knobs of bead size, deposition temperature and cycle count, and annealing conditions, we can create an electrically- and plasmonically-active photonic crystal as-desired for a particular application of choice.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Toward high laser power beam manipulation with nanophotonic materials: evaluating thin film damage performance

Nanophotonic materials enable unprecedented control of light-matter interactions, including the ability to dynamically steer or shape wavefronts. Consequently, nanophotonic systems such as metasurfaces have been touted as promising candidates for free-space optical communications, directed energy and additive manufacturing, which currently rely on slow mechanical scanners or electro-optical components for beam steering and shaping. However, such applications necessitate the ability to support high laser irradiances (> kW/cm 2 ) and systematic studies on the high-power laser damage performance of nanophotonic materials and designs are sparse. Here, we experimentally investigate the pulsed laser-induced damage performance (at λ ∼ 1 µm) of model nanophotonic thin films including gold, indium tin oxide, and refractory materials such as titanium nitride and titanium oxynitride. We also model the spatio-thermal dissipation dynamics upon single-pulse illumination by anchoring experimental laser damage thresholds. Our findings show that gold exhibits the best laser damage resistance, but we argue that alternative materials such as transparent conducting oxides could be optimized to balance the tradeoff between damage resistance and optical tunability, which is critical for the design of thermally robust nanophotonic systems. We also discuss damage mitigation and ruggedization strategies for future device-scale studies and applications requiring high power beam manipulation.

36 MATERIALS SCIENCE↗
NASA NTRS1997

Diamond Composite Films for Protective Coatings on Metals and Method of Formation

Composite films consisting of diamond crystallites and hard amorphous films such as diamond-like carbon, titanium nitride, and titanium oxide are provided as protective coatings for metal substrates against extremely harsh environments. A composite layer having diamond crystallites and a hard amorphous film is affixed to a metal substrate via an interlayer including a bottom metal silicide film and a top silicon carbide film. The interlayer is formed either by depositing metal silicide and silicon carbide directly onto the metal substrate, or by first depositing an amorphous silicon film, then allowing top and bottom portions of the amorphous silicon to react during deposition of the diamond crystallites, to yield the desired interlayer structure.

Ong, Tiong P.↗
DOE OSTI2026

Confinement of quasi-atomic structures in Ti 2 N and Ti 3 N 2 MXene electrides

Metal carbides, nitrides, or carbonitrides of early transition metals, better known as MXenes, possess notable structural, electrical, and magnetic properties. Analyzing electronic structures by calculating structural stability, band structure, density of states, Bader charge transfer, and work functions utilizing first principle calculations, we revealed that titanium nitride MXenes, namely Ti 2 N and Ti 3 N 2 , have excess anionic electrons in their lattice voids, making them MXene electrides. Bulk Ti 3 N 2 has competing antiferromagnetic (AFM) and ferromagnetic (FM) configurations with slightly more stable AFM configuration, while the Ti 2 N MXene is nonmagnetic. Although Ti 3 N 2 favors AFM configuration with hexagonal crystal systems having 6/ mmm point group symmetry, Ti 3 N 2 does not support altermagnetism. The monolayer of the Ti 3 N 2 MXene is a ferromagnetic electride. These unique properties of having non-nuclear interstitial anionic electrons in the electronic structure of titanium nitride MXene have not yet been reported in the literature. Density functional theory calculations show TiN is neither an electride, MXene, or magnetic.

Anionic electrons↗
NASA NTRS1983

Nitriding of titanium and titanium: 8 percent aluminum, 1 percent molybdenum, 1 percent vanadium alloy with an ion-beam source

Titanium and Ti-8Al-1Mo-1V alloy were nitrided with an ion-beam source of nitrogen or argon and nitrogen at a total pressure of 2 x 10 to the minus 4th power to 10 x 10 to the minus 4th power torr. The treated surface was characterized by surface profilometry, X-ray diffractometry, Auger electron spectroscopy and microhardness measurements. The tetragonal Ti2N phase formed in pure titanium and Ti-8Al-1Mo-1V alloy with traces of AlN in the alloy. Two opposite processes competed during the ion-beam-nitriding process: (1) formation of nitrides in the surface layer and (2) sputtering of the nitrided layers by the ion beam. The highest surface hardnesses, about 500 kg/sq mm in titanium and 800 kg/sq mm in Ti-8Al-1Mo-1V, were obtained by ion nitriding with an ion beam of pure nitrogen at 4.2 x 10 to the minus 4th power torr at a beam voltage of 1000 V.

Gill, A.↗
DOE OSTI2022

Metal–ceramic composite structures for fabrication of high power density plasmonic devices

The recent decade brought many advances to plasmonics, but high power density plasmonic antennas designed to behave as heaters or operate in high temperature environments are still facing material stability challenges preventing their ultimate use. Gold has been the optimal choice among plasmonic materials but experiences morphology changes at temperature that result in device efficiency reduction and failure. Bulk titanium nitride has been explored as a solution but has deal-breaking tradeoffs in device quality factor. In this paper, we explore via proof-of-concept the use of a metal–ceramic composite structure to determine whether a bulk Au nanorod can provide strong plasmonic resonances while coated with an ultrathin conformal layer of titanium nitride or silica to provide morphological stability and sufficient plasmonic activity without excessive resonance quality degradation. We show SEM-level morphological stability for temperatures up to 500 °C with coatings below 4 nm. Computer modeling suggests the ultrathin titanium nitride has detrimental effects on the strong plasmonic resonances of a Au nanorod. Here, we then looked into other possible coatings for solutions to stabilize high power density plasmonic antennas including plasmonic oxides, metal adhesion layers, and silica, the latter appearing to be the best option while lowering the overall peak electric field intensity, the silica increases the electric field intensity at its boundary.

36 MATERIALS SCIENCE↗
NASA NTRS1997

Simulation of Gas Mixtures in RF Discharges for Nitride Deposition

Tungsten and titanium nitride films have long been grown by chemical vapor deposition (CVD) methods. However, there has been recent interest in low temperature growth using plasma enhanced CVD. For the present work, we focus on the radio frequency (BE) discharge characteristics of gas mixtures used in nitride deposition (for example, WF6 and ammonia). Because the radial variations for a standard 200 mm, parallel plate reactor are limited to a small zone near the edges of the electrodes, a 1-D (one-dimensional) analysis is considered. This model consists of a self-consistent, 3-D (three-dimensional) moment fluid simulation that solves the continuity, momentum, and energy equations for neutral and charged species. The results in terms of plasma structure, radical concentrations, and local deposition rate will be presented. We will also compare the 1-D results with those obtained from a 2-D hybrid plasma equipment model (HPEM) developed at the University of Illinois.

Hwang, Helen H.↗
DOE OSTI2023

A Study of a Surrogate Nuclear Thermal Propulsion Fuel Element

We report a surrogate fuel, Zirconium Carbide/Titanium Nitride has been prepared using a simple method to obtain a more uniform distribution of titanium nitride in the zirconium carbide matrix. Powders were sintered using Spark Plasma Sintering at 1750oC and 1850oC using a modified sintering profile. This resulted in a fairly uniform distribution of titanium nitride in the zirconium carbide matrix with a density of 95% of theoretical at 1850oC. Scanning electron microscopy, indentation hardness and x-ray diffraction results are given.

36 MATERIALS SCIENCE↗
NASA NTRS1996

Low Temperature Unbalanced Magnetron Deposition of Hard, Wear-Resistant Coatings for Liquid-Film Bearing Applications

The original program for evaluating the tribological properties several different hard coatings for liquid film bearing applications was curtailed when the time for the program was reduced from 3 years to 1. Of the several different coatings originally planned for evaluation, we decided to concentrate on one coating, carbon nitride. At BIRL, we have been instrumental in the development of reactively sputtered carbon nitride coatings, and we have found that it is a very interesting new material with very good tribological properties. In this program, we found that the reactively sputtered carbon nitride does not bond well directly to hardened 440C stainless steel; but if an interlayer of titanium nitride is added between the carbon nitride and the 440C, the adhesion of the dual coating combination is very good. Statistically designed experiments were run with the dual layer combination, and 3 variables were chosen for the Box-Benken design, which were the titanium nitride interlayer thickness, the nitrogen partial pressure during the reactive sputtering of the carbon nitride, and the carbon nitride substrate bias voltage. Two responses were studied from these three variables; the adhesion of the dual coating combination to the 440C substrate and the friction coefficient of the carbon nitride in dry sliding contact with 52100 steel in air. The best adhesion came with the thickness interlayer thickness studied, which was 4 micrometers, and the lowest coefficient of friction was 0.1, which was achieved when the bias voltage was in the range of -80 to - 120 V and the nitrogen partial pressure was 3 mTorr.

Sproul, William D.↗
NASA NTRS1993

Application of hard coatings to substrates at low temperatures

BIRL, the industrial research laboratory of Northwestern University, has conducted unique and innovative research, under sponsorship from the NASA Marshall Space Flight Center (MSFC), in the application of hard, wear resistant coatings to bearing steels using the high-rate reactive sputtering (HRRS) process that was pioneered by Dr. William Sproul, the principal investigator on this program. Prior to this program, Dr. Sproul had demonstrated that it is possible to apply hard coatings such as titanium nitride (TiN) to alloy steels at low temperatures via the HRRS process without changing the metallurgical properties of the steel. The NASA MSFC program at BIRL had the specific objectives to: apply TiN to 440C stainless steel without changing the metallurgical properties of the steel; prepare rolling contact fatigue (RCF) test samples coated with binary hard coatings of TiN, zirconium nitride (ZrN), hafnium nitride (HfN), chromium nitride (CrN), and molybdenum nitride (MoN), and metal coatings of copper (Cu) and gold (Au); and develop new alloyed hard coatings of titanium aluminum nitride (Ti(0.5)Al(0.5)N), titanium zirconium nitride (Ti(0.5)Zr(0.5)N), and titanium aluminum vanadium nitride.

Sproul, William D.↗
DOE OSTI2022

Fabrication of ultrathin suspended membranes from atomic layer deposition films

In this report, ultrathin films suspended as freestanding membranes are critical to many microelectronic and materials science applications. However, fabrication methods are currently limited in either their flexibility, due to material selectivity issues during the final membrane release, or their scalability. Here, we demonstrate a novel fabrication process for suspending ultrathin films with thicknesses as low as 4 nm and lateral dimensions up to 20 x 1000 μm from a variety of materials grown by atomic layer deposition. A silicon nitride membrane serves as the support for a sacrificial polymer layer and an ultrathin atomic layer deposition film which, after plasma etching, will form the membrane. The high chemical selectivity between atomic layer deposition-grown transition metal nitrides and oxides and the sacrificial polymer means that ultrathin films of a variety of materials can be released without damage using a single process. Electrically conductive titanium nitride membranes can be produced by this method and are of significant interest for electron microscopy applications. Electron transparency of titanium nitride membranes was found to be ~14% higher than silicon nitride of the same thickness, and of similar conductivity to graphite, meaning that ultrathin, conductive, and electron transparent membranes can be fabricated at scale. These membranes are ideal supports for electron and photon characterization techniques, as well as microelectromechanical system applications that require a conductive membrane.

36 MATERIALS SCIENCE↗