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NASA NTRS1987

Stability and rheology of dispersions of silicon nitride and silicon carbide

The relationship between the surface and colloid chemistry of commercial ultra-fine silicon carbide and silicon nitride powders was examined by a variety of standard characterization techniques and by methodologies especially developed for ceramic dispersions. These include electrokinetic measurement, surface titration, and surface spectroscopies. The effects of powder pretreatment and modification strategies, which can be utilized to augment control of processing characteristics, were monitored with these technologies. Both silicon carbide and nitride were found to exhibit silica-like surface chemistries, but silicon nitride powders possess an additional amine surface functionality. Colloidal characteristics of the various nitride powders in aqueous suspension is believed to be highly dependent on the relative amounts of the two types of surface groups, which in turn is determined by the powder synthesis route. The differences in the apparent colloidal characteristics for silicon nitride powders cannot be attributed to the specific absorption of ammonium ions. Development of a model for the prediction of double-layer characteristics of materials with a hybrid site interface facilitated understanding and prediction of the behavior of both surface charge and surface potential for these materials. The utility of the model in application to silicon nitride powders was demonstrated.

Feke, Donald L.↗

NASA NTRS2018

Friction and Wear of Unlubricated NiTiHf with Nitriding Surface Treatments

The unlubricated friction and wear properties of the superelastic materials NiTi and NiTiHf, treated by either gas nitriding or plasma nitriding, have been investigated. Pin on disk testing of the studied materials was performed at sliding speeds from 0.01 to 1m/s at normal loads of 1, 5 or 10N. For all of the studied friction pairs (NiTiHf pins vs. NiTi and NiTiHf disks) over the given parameters, the steady-state coefficients of friction varied from 0.22 to 1.6. Pin wear factors ranged from approximately 1E-6 against the NiTiHf and plasma nitrided disks to approximately 1E-4 for the gas nitrided disks. The plasma nitrided disks provided wear protection in several cases and tended to wear by adhesion. The gas nitrided treatment generated the most pin wear but had essentially no disk wear except at the most severe of the studied conditions (1N load and 1m/s sliding speed). The results of this study are expected to provide guidance for design of components such as gears and fasteners.

friction↗

DOE OSTI2011

Use of additives to improve microstructures and fracture resistance of silicon nitride ceramics

A high-strength, fracture-resistant silicon nitride ceramic material that includes about 5 to about 75 wt-% of elongated reinforcing grains of beta-silicon nitride, about 20 to about 95 wt-% of fine grains of beta-silicon nitride, wherein the fine grains have a major axis of less than about 1 micron; and about 1 to about 15 wt-% of an amorphous intergranular phase comprising Si, N, O, a rare earth element and a secondary densification element. The elongated reinforcing grains have an aspect ratio of 2:1 or greater and a major axis measuring about 1 micron or greater. The elongated reinforcing grains are essentially isotropically oriented within the ceramic microstructure. The silicon nitride ceramic exhibits a room temperature flexure strength of 1,000 MPa or greater and a fracture toughness of 9 MPa-m.sup.(1/2) or greater. The silicon nitride ceramic exhibits a peak strength of 800 MPa or greater at 1200 degrees C. Also included are methods of making silicon nitride ceramic materials which exhibit the described high flexure strength and fracture-resistant values.

36 MATERIALS SCIENCE↗

DOE OSTI2016

Liquid flow cells having graphene on nitride for microscopy

This disclosure provides systems, methods, and apparatus related to liquid flow cells for microscopy. In one aspect, a device includes a substrate having a first and a second oxide layer disposed on surfaces of the substrate. A first and a second nitride layer are disposed on the first and second oxide layers, respectively. A cavity is defined in the first oxide layer, the first nitride layer, and the substrate, with the cavity including a third nitride layer disposed on walls of the substrate and the second oxide layer that define the cavity. A channel is defined in the second oxide layer. An inlet port and an outlet port are defined in the second nitride layer and in fluid communication with the channel. A plurality of viewports is defined in the second nitride layer. A first graphene sheet is disposed on the second nitride layer covering the plurality of viewports.

36 MATERIALS SCIENCE↗

DOE OSTI2018

Transformation enabled nitride magnets absent rare earths and a process of making the same

A process for producing an ordered martensitic iron nitride powder that is suitable for use as a permanent magnetic material is provided. The process includes fabricating an iron alloy powder having a desired composition and uniformity; nitriding the iron alloy powder by contacting the material with a nitrogen source in a fluidized bed reactor to produce a nitride iron powder; transforming the nitride iron powder to a disordered martensitic phase; annealing the disordered martensitic phase to an ordered martensitic phase; and separating the ordered martensitic phase from the iron nitride powder to yield an ordered martensitic iron nitride powder.

36 MATERIALS SCIENCE↗

DOE OSTI2020

Transformation enabled nitride magnets absent rare earths and a process of making the same

Matthiesen, David↗

DOE OSTI2012

Additive-assisted synthesis of boride, carbide, and nitride micro/nanocrystals

General and simple methods for the syntheses of borides, carbides and nitrides are highly desirable, since those materials have unique physical properties and promising applications. Here, a series of boride (TiB{sub 2}, ZrB{sub 2}, NbB{sub 2}, CeB{sub 6}, PrB{sub 6}, SmB{sub 6}, EuB{sub 6}, LaB{sub 6}), carbide (SiC, TiC, NbC, WC) and nitride (TiN, BN, AlN, MgSiN{sub 2}, VN) micro/nanocrystals were prepared from related oxides and amorphous boron/active carbon/NaN{sub 3} with the assistance of metallic Na and elemental S. In-situ temperature monitoring showed that the reaction temperature could increase quickly to {approx}850 Degree-Sign C, once the autoclave was heated to 100 Degree-Sign C. Such a rapid temperature increase was attributed to the intense exothermic reaction between Na and S, which assisted the formation of borides, carbides and nitrides. The as-obtained products were characterized by XRD, SEM, TEM, and HRTEM techniques. Results in this report will greatly benefit the future extension of this approach to other compounds. - Graphical abstract: An additive-assisted approach is successfully developed for the syntheses of borides, carbides and nitrides micro/nanocrystals with the assistance of the exothermic reaction between Na and S. Highlights: Black-Right-Pointing-Pointer An additive-assisted synthesis strategy is developed for a number of borides, carbides and nitrides. Black-Right-Pointing-Pointer The reaction mechanism is demonstrated by the case of SiC nanowires. Black-Right-Pointing-Pointer The formation of SiC nanowires is initiated by the exothermic reaction of Na and S.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2010

Impact of temperature increments on tunneling barrier height and effective electron mass for plasma nitrided thin SiO{sub 2} layer on a large wafer area

Thermally grown SiO{sub 2} layers were treated by a plasma nitridation process realized in a vertical furnace. The combination of a pulsed-low frequency plasma and a microwave remote plasma with N{sub 2}/NH{sub 3}/He feed gas mixture was used to nitride the thermally grown SiO{sub 2} gate dielectrics of MIS structures. Temperature dependency of effective masses and the barrier heights for electrons in pure thermally grown SiO{sub 2} as well as plasma nitrided SiO{sub 2} in high electric field by means of Fowler-Nordheim regime was determined. It is frequently seen from the literature that either effective electron mass or barrier height (generally effective electron mass) is assumed to be a constant and, as a result, the second parameter is calculated under the chosen assumption. However, in contrast to general attitude of previous studies, this work does not make any such assumptions for the calculation of neither of these two important parameters of an oxide at temperature ranges from 23 to 110 deg. C for SiO{sub 2}, and 23 to 130 deg. C for nitrided oxide. It is also shown here that both parameters are affected from the temperature changes; respectively, the barrier height decreases while the effective mass increases as a result of elevated temperature in both pure SiO{sub 2} and plasma nitrided SiO{sub 2}. Therefore, one parameter could be miscalculated if the other parameter, i.e., effective mass of electron, was assumed to be a constant with respect to variable physical conditions like changing temperature. Additionally, the barrier heights were calculated just by taking constant effective masses for both types of oxides to be able to compare our results to common literature values.

36 MATERIALS SCIENCE↗

DOE OSTI2016

Effect of substrate nitridation temperature on the persistent photoconductivity of unintentionally-doped GaN layer grown by PAMBE

The surface roughness and defect density of GaN epitaxial layers grown on c-plane sapphire substrate are investigated and found to be dependent on nitridation temperature. GaN epitaxial layers grown after nitridation of sapphire at 200°C have a higher defect density and higher surface roughness compared to the GaN layers grown at 646°C nitridation as confirmed by atomic force microscopy (AFM). The persistent photoconductivity (PPC) was observed in both samples and it was found to be decreasing with decreasing temperature in the range 150-300°C due to long carrier lifetime and high electron mobility at low temperature. The photoresponse of the GaN films grown in this study exhibit improved PPC due to their better surface morphology at 646°C nitrided sample. The point defects or extended microstructure defects limits the photocarrier lifetime and electron mobility at 200°C nitrided sample.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2011

Nitride chemical passivation of a GaAs (100) Surface: Effect on the electrical characteristics of Au/GaAs surface-barrier structures

The effect of chemical nitridation of GaAs substrates in a hydrazine-sulfide solution on the electrical characteristics of Au/GaAs Schottky structures has been studied. In nitridation of this kind, a solid passivating gallium nitride film with a monolayer thickness is formed on the surface of GaAs, providing almost direct contact between the semiconductor and the metal deposited on its surface. Au/GaAs structures fabricated on nitride substrates have ideality factors close to unity and are characterized by a narrow scatter of potential barrier heights. Prolonged heating of these structures at 350 Degree-Sign C does not change these parameters. The data obtained show that the nitride monolayer formed on the GaAs surface upon treatment in hydrazidesulfide solutions effectively hinders atomic migration across the metal-semiconductor phase boundary.

36 MATERIALS SCIENCE↗

DOE OSTI2013

Mesoporous TiO2 spheres with a nitridated conducting layer

Nitridated TiO2 mesoporous spheres have been synthesized by hydrothermal processing followed by post-nitridation with NH3. Characterization data reveal a nitridated conducting layer, in addition to a mesoporous, and nanosized building-block morphology resulting in a large surface area. The samples have an average pore size and surface area of, respectively, 10 nm and 87 m2/g. The nitridated TiO2 mesoporous spheres exhibit a high capacity of > 200 mAh/g with good cyclability and high rate capability, as the nitridated conducting layer and favorable morphology of nanosized spheres provides good electrical contact, accommodates cycling induced strain smoothly, and facilitates lithium-ion diffusion.

anode↗

DOE OSTI2017

Laser Nitriding of the Newly Developed Ti-20Nb-13Zr at.% Biomaterial Alloy to Enhance Its Mechanical and Corrosion Properties in Simulated Body Fluid

Despite the widespread application of Ti alloy in the biomedical field, surface treatments are typically applied to improve its resistance to corrosion and wear. A newly developed biomedical Ti-20Nb-13Zr at.% alloy (TNZ) was laser-treated in nitrogen environment to improve its surface characteristics with corrosion protection performance. Surface modification of the alloy by laser was performed through a Nd:YAG laser. The structural and surface morphological alterations in the laser nitrided layer were investigated by XRD and a FE-SEM. The mechanical properties have been evaluated using nanoindentation for laser nitride and as-received samples. The corrosion protection behavior was estimated using electrochemical corrosion analysis in a physiological medium (SBF). The obtained results revealed the production of a dense and compact film of TiN fine grains (micro-/nanosize) with 9.1 µm below the surface. The mechanical assessment results indicated an improvement in the modulus of elasticity, hardness, and resistance of the formed TiN layer to plastic deformation. The electrochemical analysis exhibited that the surface protection performance of the laser nitrided TNZ substrates in the SBF could be considerably enhanced compared to that of the as-received alloy due to the presence of fine grains in the TiN layer resulting from laser nitriding. Furthermore, the untreated and treated Ti-20Nb-13Zr alloy exhibited higher corrosion resistance than the CpTi and Ti6Al4V commercial alloys. The improvements in the surface hardness and corrosion properties of Ti alloy in a simulated body obtained using laser nitriding make this approach a suitable candidate for enhancing the properties of biomaterials.

36 MATERIALS SCIENCE↗

DOE OSTI2018

Studies on Enhancement of Silt Erosion Resistance of 13/4 Martensitic Stainless Steel by Low-Temperature Salt Bath Nitriding

Low-temperature salt bath nitriding of heat treated and tempered 13/4 Martensitic stainless steel (13/4HTT) was carried at 450 °C (N450) and 500 °C (N500) for 10 h each. The nitrided samples were characterized by using x-ray diffractometer, field emission scanning electron microscope and optical microscope. The nanohardness and elastic modulus of the cross section of nitrided specimen were measured by nanoindentation test using Hysitron TI950 triboindenter. The nitrided 13/4HTT (N450 and N500) and 13/4HTT specimens were subjected to slurry erosion test in a slurry pot tester. The test was conducted for 48 h, and weight loss was measured after every 6 h. The relative speed of slurry with respect to specimen was 4.55 m/s. It was found that the weight loss due to erosion of the N450 is 83% less than that of 13/4HTT and that of N500 was 92% more than that of 13/4HTT. The erosion mechanism is correlated to the phases present in the specimens. The improvement in the slurry erosion resistance of N450 is due to presence of expanded martensite (α{sub N}-Fe). Increasing the temperature of nitriding to 500 °C led to the decrease in the slurry erosion resistance of N500 due to the formation of brittle CrN phase.

36 MATERIALS SCIENCE↗

DOE OSTI2018

Influence of Laser Nitriding on the Surface and Corrosion Properties of Ti-20Nb-13Zr Alloy in Artificial Saliva for Dental Applications

Ti alloys have been used for dentistry due to their lower density and improved compatibility. However, the resistance to corrosion and surface hardness of Ti alloys need to be improved to avoid the formation of debris, which affects the long-term biocompatibility. In the present work, the surface characteristics and corrosion protection in artificial saliva produced by laser nitriding of a new biomedical Ti-20Nb-13Zr at.% alloy have been investigated for dental applications. The laser nitrided and untreated alloy surfaces were examined using XRD, FE-SEM, x-ray photon spectroscopy, Vickers microhardness measurements, atomic force microscopy, scratch measurements, Raman spectroscopy, and surface energy measurements. The susceptibility of the laser nitrided TNZ alloy to corrosion in an artificial saliva medium was investigated by electrochemical corrosion tests, which were performed by utilizing open circuit potential monitoring, electrochemical frequency modulation, and electrochemical impedance spectroscopic methods. The findings revealed that a TiN layer formed on the alloy surface after nitriding. The surface hardness of the treated alloy was 2.4 times that of the as-received samples. Moreover, the results showed improved friction coefficient and hydrophilic surface characteristics. The corrosion analysis revealed that the compact and dense TiN layer produced during laser nitriding improved the corrosion resistance of the Ti-20Nb-13Zr sample in artificial saliva medium.

36 MATERIALS SCIENCE↗

DOE OSTI2022

Capture of novel sp 3 hybridized Z-BN by compressing boron nitride nanotubes with small diameter

Experimental synthesis of new sp 3 hybridized carbon/boron nitride structures remains challenging despite that numerous sp 3 structures have been proposed in theory. Here, we showed that compressed multi-walled boron nitride nanotubes (MWBNNTs) and boron nitride peapods (C 60 @BNNTs) with small diameters could transform into a new sp 3 hybridized boron nitride allotrope (Z-BN). This strategy is considered from the topological transition point of view in boron nitride nanotubes upon compression. Due to the increased curvature in compressed small-diameter MWBNNTs, the uncommon 4- and 8-membered rings in Z-BN could be more favorably formed. And the irreversible tube collapse is proved to be a critical factor for the capture of the formed Z-BN, because of the competition between the resilience of tube before collapse and the stress limitation for the lattice stabilization of Z-BN upon decompression. In this case, Z-BN starts to form above 19.0 GPa, which is fully reversible below 45 GPa and finally becomes quenchable at 93.5 GPa. Consequently, this collapse-induced capture of the high-pressure phase could also be extended to other tubular materials for quenching novel sp 3 structures.

36 MATERIALS SCIENCE↗

DOE OSTI2018

Influence of hydrogen peroxide in enhancing photocatalytic activity of carbon nitride under visible light: An insight into reaction intermediates

Carbon nitride is a known photocatalyst that can be activated under visible light irradiation. In this study, the combined effect of carbon nitride and hydrogen peroxide in photocatalytic degradation of methylene blue (MB) in water was investigated under visible light. Carbon nitride was synthesized by thermal polymerization of dicyandiamide and characterized by x-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM), Energy dispersive x-ray (EDX), Fourier transform infrared spectroscopy (FTIR) and pore textural properties. The kinetic study of degradation of MB with carbon nitride and in presence of hydrogen peroxide showed complete degradation of MB before 45 min of time interval. The kinetic studies were also performed by varying the dose of photocatalyst and initial concentration of MB and it was shown that higher dose of photocatalyst and lower concentration of MB resulted in higher rate of degradation. The dual role of hydrogen peroxide can be related to the generation of additional highly reactive hydroxyl radicals in presence of photocatalyst and prevention of recombination of holes and electrons of carbon nitride thereby improving its photocatalytic activity. The pH study revealed that neutral pH of the solution results in the highest rate of degradation. Lastly, analysis of liquid chromatography–mass spectroscopy (LCMS) results helped to reveal the reaction steps of photocatalysis of MB and it was found that the four stages of photodegradation of MB were demethylation, ring shortening, ring opening and complete mineralization.

36 MATERIALS SCIENCE↗

DOE OSTI2015

Supramolecular intermediates in the synthesis of polymeric carbon nitride from melamine cyanurate

The adduct of melamine and cyanuric acid (MCA) was used in past research to produce polymeric carbon nitride and precursors. The reaction yield was considerably incremented by the addition of sulfuric acid. The polymeric carbon nitride formation occurs around 450 °C at temperatures above the sublimation of the adduct components, which occurs around 400 °C. In this report the effect of sulfuric acid on MCA was investigated. It was found that the MCA rosette supramolecular channel structures behave as a solid solvent able to host small molecules, such as sulfuric acid, inside these channels and interact with them. Therefore, the sulfuric acid effect was found to be close to that of a solute that causes a temperature increment of the “solvent sublimation” enough to allowing the formation of polymeric carbon nitride to occur. Sulfate ions are presumably hosted in the rosette channels of MCA as shown by simulations. - Graphical abstract: The blend of melamine cyanurate and sulfuric acid behaves like a solution so that melamine cyanurate decomposition is shifted to temperatures high enough to react and form polymeric carbon nitride. - Highlights: • The adduct of melamine and cyanuric acid behaves as a solid solvent. • The blend of sulfuric acid and melamine cyanurate behaves like a solution. • Melamine cyanurate decomposition is shifted to higher temperatures by sulfuric acid. • The formation of polymeric carbon nitride occurs for these higher temperatures.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2010

Moessbauer spectroscopy study on the corrosion resistance of plasma nitrided ASTM F138 stainless steel in chloride solution

Plasma nitriding of ASTM F138 stainless steel samples has been carried out using dc glow discharge under 80% H{sub 2}-20% N{sub 2} gas mixture, at 673 K, and 2, 4, and 7 h time intervals, in order to investigate the influence of treatment time on the microstructure and the corrosion resistance properties. The samples were characterized by scanning electron microscopy, glancing angle X-ray diffraction and conversion electron Moessbauer spectroscopy, besides electrochemical tests in NaCl aerated solution. A modified layer of about 6 {mu}m was observed for all the nitrided samples, independent of nitriding time. The X-ray diffraction analysis shows broad {gamma}{sub N} phase peaks, signifying a great degree of nitrogen supersaturation. Besides {gamma}{sub N,} the Moessbauer spectroscopy results indicated the occurrence of {gamma}' and {epsilon} phases, as well as some other less important phases. Corrosion measurements demonstrate that the plasma nitriding time affects the corrosion resistance and the best performance is reached at 4 h treatment. It seems that the {epsilon}/{gamma}' fraction ratio plays an important role on the resistance corrosion. Additionally, the Moessbauer spectroscopy was decisive in this study, since it was able to identify and quantify the iron phases that influence the corrosion resistance of plasma nitrided ASTM F138 samples.

36 MATERIALS SCIENCE↗